1
SRI Instruments
r: ,
Operation Manual and Reference Guide
•
.. •• ,.
-
•
~:::::; : :
....... "
e
.
"" 'w
.. 4'.4. -'
-L
.; ..: : : .: .: :":.:; : : : : : ; :. ... , ,~
.,
---
-
:;;:; .... : :': :"fi': :; ;: ,: ..~; :~ : ;;:;; , "?;:. ~
, .".. : .
Model 310 Ultra-
_
"
'
~~
.--, .'- .-
• .2£;::I."WU
Model 110 Standalone
.
-f
...
,
"
,
QA
Mode l 8610C Compact GC
compact GC
Detector Chas sis
SRI Instruments 20720 Earl si. Torrance CA 90503
t-:
"""'~'C"i:::k Model H2-50 Stand-alone Hyd rog en
Generator
Phone: 310-214-5092 Fax: 5097 Web: http:/ /www.sngc.com i_~-
E-mail:
[email protected]
~nt
\ "
January:.lUU!:J
M oue l ZOJ Oingle
Channel Data System
Ill
~~-
..•-'4> -1 . _ .: " .,
bff
-_..
" ~ _ " _ ' .' -_ ""• . , .' ..~~ , .,;.".., .,-~----'.---
-
c nenner Chromatography Data
M ooel ZOZ Four
System
Manl lll.pub
1 (of 550 ) 2006(-2016)
2
INJ ECTORS Heated Stat ic Headsp ac e Inject o r
Overview
r==~~""'""'=~ ~
The Hea ted Static Headspace Injecto r is installed o n the left side of the GC
chassis
-.
The Heated Static Headsp ace Injector is useful for anaylsis ofthe light volatiles that can beparti tioned into the beadspace ora vialcontainingeither-a liquid or a solidmatrixsample. Itcan be used withdirty or complex samples, suches blood. urine, powders. food.'> and flavors. The SRIHealed Static Headspace Injector is built into the 86 IDC Ge , on the left side of the chassis, eliminating the need for transfer lines and reducing dead volume. Thermostatted fromambient to 9Cl"C, a beater body accepts a 40mL VOA vialcontaining IO-2Om L of sample. Covered with a protectiveheat shield, the heater body is hea led and mechanically agitated under control of the PeakSimple data system. Two needles puncture the vial's septum top uponinsertion into the hea ter body. Purge gas to pressurize the vial is delivered through one needle. The other needle carries the headspace vapors to the sample loop on the 10pa n gas sampling valve. located in the valve oven. On the downstream end of the loopis a solenoid shut-off valve, also controlled through the data system. This solenoid shut-off valve opens to fill the sample loop with thesample headspace from thepressurizedvial. A syringe port allows the addition of internal standards. spikes: etc. into the vial without exposing the sampleto ambient air.
Heated Sta tic Headspace Inj ector
r' -
j i
Solenoid shut-off valve
I
2 (of 550 ) 2006(-2016)
3
INJ ECTORS Heated Stati c Heads pace Inj ector
..
tS
..
Theory of Opera tio n The SRI Heated Static Headspace Injector uses a mechanically agitated hearerbody for sample equilibration.a 10 port gas samp ling va lve witha ImL sample loop, and a sample loop shutoff solenoid valve. The headspace anal ysis begins with the sam ple equilibration period. curing which the
Valve in LOAD Position
,f\. _-";cc-,,,~, ..... ~ , 5 0 ~
Cartier gas In from
earner EPC and po lish ing filter ~
'~ 1ml sample
'...!J\
r~, jocp ;,J
Pucoegosm froms"" ",e EPC_,
~~vv
2 ' l (). V .,
Heater- bod y
~~
I
JillTI
-=tj
.
Tocolumn
---7 vent to
~
a!rnOsphere
Sample loop
"'" s."ll:t-off valve
VOAvial
eer-ier gas in from carrie r EPC and po Jish ir.g filter ~ 4
I I from sparge EPC
1
-
100
v:
~?
I y~7<::G_/
I I
Hea:"'body-,!JW~ Hee: :
1ml samp l e ~ I
: : : \.
l~lQ.t) ~1 . P rgv
PlJrge gas in
m~ !
. ij ~
'0
To column
J"
Vent 10 atmosphere
Sernpe lccp
iii
VOAvi al
position. A40mLVOA vial containing I0- 20mL of sample matrix is inserted into the heater body. the n hea ted and agitated (the time it takes to achieve equilibration depends on the sample matrix and dee target anal ytes) . Two needl es in the upper part of the heater bod y puncture the septum top of the via l in order to deliver p urge ga s into and m ule the sample out ofthe viel. After the equilibration period, the vial is pres surized so that the sampl e wilI
escapewben the solenoid shut-offval ve is opened. Th e amoun t of purge gas neede d to pressurize the VOA vial
Valve in INJECT Position
•
gas sampling valv e is in the LOA D
sh:t-off valve
depe nds upon the type of sample. A sample v,vith high liqu id content can c reat e sufficient pressure during the cqiulibration period to fill the sample kop withbcadspace. A dry sample will require that the pu rge gas be turned ON, up to IOpsi, to pressuri ze the sample vial. The solenoid shut-off valve
at the downstreamend of the l mL loop is th en open ed bri efly, and t he pressurized headspace sample fills the loop as it exits through the valve. After the sh ut-off va lve cl oses. the gas sampling valve i~ actuated 10 the lXJECT pos ition, placing the sam ple loop in the carrier gas stream to sweep the headspace sampl e into the GC column, and on to thedetectorts).
3 (of 550 ) 2006(-2016)
4
INJECTORS Heated Static Headspace Inj ecto r
Genera l Operating Procedures
I. The Headspacc injection technique requires little sample preparation. sincejust thesample headspace, not the sample itself, is run through the Gc. Insert I0-20mL of sample into a clean VOA vial and seal it. 2. The p urge gas pressure is contro lled wi th an Electronic P res sure Controller (E Pe). Sci the purge gas to 0J Dpsi, depending on the liquid content of jhesample. SRI recommends helium purge gas .
3. Using the trimpo t on the top edge of the GC's front control
Hdspace.M
panel, set the heater body temperature betweenambient and 90"<:.
Pressure builds as the vial is hea ted. The temperature setting d epend s upon the target enalyt es and the liquid co ntent of tbe sample .
4 . Create or load an event table. Hcspaee.evt, shown at right and on the Expected Performa nce page, is inc luded in versio n 2 .66 (an d h igh er) o f the PeakSimple so ftware. A typica l e vent
table heats and agitates the vial for 20 minutes; it may take more or less time to achieve beadspace equilibration. 5. Create or load a temperature program. The column oven is typically held at the initial tempe ratu re (ususally 40"C) for the
duration ofthe sample equilibration period, plus 2.-4 more minutes.
EVENT TlItE
, em ' n>
EV'"
EVE NT "'U ~ C T (lN
ZE RO
Zero 1'l:1'If1
r RO N"
V O'" Vial M.. ,.,. ,
D " (IN"
S halt... ' Ooltl'lO id "ON"
1 ~.
D ROrr'"
S ..... 5O·.. I'IO ... - O" I' -
11i1.9Xl
r -crr-
V O"' \I\a IH.. _ ,
taeco
E "ON"
P>IVl!-OH"
,. ""
E " OFF"
P ..gI "O Fr R
10S00
A"ON"
111.1lOD
A " ~'"
Zl DOQ
e "ON"
V. I ,n NJ ECT
"' DOQ
C·O FF'"
Va"" .. L.OAJ)
' '''''
S n~lI loop " lilt
so luClId opln SI ~1I
loo"" .. >11 s o_Ill dOSed
6 . Set the valve oven temperature to 100°C or higher to avo id water condensation ( 120"( is a typical setting]. 7. Activa te andeoergize yoer derectors asnecessary Consuh themanual sections foryourparticulardctector(s).
8. Insert a VOA vial filled with IO-20mL of sample into the headspace heater body: slide the vial into the heater body from the bottom. You will feel some resistance as the needles meet the vial septum lid, and once the needles have penetrated the septum. the vial will stop against the top of the heater body interior. The needles will hold the vial in place. Beginthe analysis by pressing the RU":'ol burton on the GC or the spacebar on your computer keyboard.
4 (of 550 ) 2006(-2016)
5
INJ ECTORS Heated Static Headspace Injector Expected Performan c e P..-r
"
BeJEl
• •
•
~
"
,"; "
!i
~ ~
ffi
•
<
.s
1
,"-
8 " g
•"
.~ -E
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
--'
-
sample: 1IJl1OOppb BTEX Plus (vial 25% full er sernc'e sonn'on with 10IJL c f
Events:
1OOppb BTEX Plus) VOA vial s et to heat from ambient te mperature to 5 0"(;
Time 0.100
Event F ON ( VOA vial heater) 0.200 DON (sIl a ;';er solenoid ) 19.400 DOFF
Cclumr x15mMXT-VOL CatTier: l1e1Jum @ 10mUm in
FID gain: HIGH FID temp: 3OO"C FlO ignitor : -400 V~veten1P:
...c ,-
[ Ie "
,~
120"(;
-,
~ 5l " !6
E!Ql:I"'''''''' ~:J t
Column 0Yef1 tencereure program (Hd spa ca .t em): Initial Hold Ramp Fiilal 5O'C 23.00 10.00 160'C
~
"
19.800 AON (sample loopcx:t ,- I .~
.~
"l,,:E e:
r-&01
, •, •
19.500 F OFF 19.600 E ON (purge s;as) 19.700 E OFF
"
'~<'O H"'-l.T.CO N
The carryover p pb of O rthc Xylene is ce termm ed
by com par ing th e two res :Jltil"g ere e counts:
-l... __ x_
BTEX st:rrJ#e re $l' js'
307 "tcoooe 307x =30pplJ
X:= O.9nppb
~-
--
-
-
--
or 1%
--
I j
r, -31m
i
~
(I\'':): e: th iS C.'XltnatCl\jra.71 was geee -ated in our tactory lEIS: ia;" wtldl nss T e E co1'!tami !'!3lion )
11 0 ••0
•A
I ~ :..a ;~
-
:::J
~
Retel'l l iOl'l Area
Scivoe":
20 .35C
~,..,Z@<" e
21483
"rs.ace ®
7332.C8:S 256 2780
TtE 2 1.91 6 23.266 To!uene 24.216 FCE Ethy; Benzene 25.~8S
298 6540
cr~~
306. 6 11~
Xylene 26.333
3romolcr.n
u
l'i
J
sOO~d )
19.900 A OFF 20.000 G ON (valve eduator) 27.000 GOFF
26,616
T,,,,,
119,664 5
2B5.23 10
98671 0 2L ~ 1 5
8731.6720
Wale<" blan k re sou s : Relen tior. Area
Co:':l;)()nOm!
LC.3SC
137J}385
2 1.91 6 0 11\0 Xyle:-e 25.350
10_0no 3.13CS
~'en:
TCE
T='
15C USO
5 (of 550 ) 2006(-2016)
6
INJECTORS
Purge & Trap Overvie w Built-in to the 8610C gas chromatograph.the SRI Purge & Trap is designed for compliance wi th EPA Methods5030 andJor5035forthe extraction ofvolatileorganic compounds from waterorsoil samples. The purge and trap technique is applicable to arange ofmolecules from C3 to C11. ThePurge & Trap bardware consists of a 10 port valveina heated, ductedvalve oven, two traps, a coolrngfan,and tbe purge head(s). The unique dualtrap design enables thesimultaneous trapping of compounds with different boiling points. Each trap has its own heater, andthe ends ofthe traps are enclosed in the v-alvc oven ducts to prevent cold spots. The coolingfan maintains the adsorption temperanrrc and rapidly lowers trap heat afterdesorption. The trap in the lowerposition (TRAP I) is usuallypacked with TenaxlM_GR at the factory,\\Me the upper trap (TRAP 2) is left empty forfheuser topackwith the desiredadsorbear. A Carbosievet" packed trap is also shipped with the GC for optional installation in the TRAP 2 position. The Carbosieve trap is used only when the analysis includes light gaseous VOC's, the most common being vinyl chloride. The Method 5030 Purge & Trap is the standard model with a fixedpurge bead that uses disposable 16mm test tubes forambicnttcmperature purging. Tbere is a bu ilt-in septum port on this purge head through 'which Basstandards may be spiked. The Method 503015035 Purge & Trap fea tures intcrcbangcablepurge heads. The 5035 purge head is a thermostarred heater body (from ambient to 50"C) which accepts standard 40mL VO A vials. Ins ide the heater body are two needles which puncturethe septum: thelonger one bubbleshelium purge gus through the sample. while the shorte r needle exhausts sa mple-laden gas to the adsorbent traps. In compliance with EPAMethod 5035. thepurgc head is mechanically agiteicdwhile the S3D1ple is being purgcd Tbcrc isa syrmgeport on the Mcthod 5030,'5035Purge & Trap that allows wa ter and internal standard to be added to the sample in the vial wirhoutpuncturing the septum again. Opcrarion of the Purge & Trnp is automated by the PcakSimplcdata system.
Method 5030/5035 Purge & Trap --=-~ --
Purge head on a Method 5030 Purge & Trap
6 (of 550 ) 2006(-2016)
7
INJECTORS Purge & Trap
Theory of Operation Purge & Trap Valve in the LOAD Position
The SR I Purge & Tra p uses a l Oport gas sampling valve and dual adsorbent
traps. Each trap has independent adsorption and desorption serpoicts to optimize the analyte trapping and releasing
earner gas in from carrier EPC
~~
~,
~ s . ~~
Oulto On-cclumn injector and column
, 4
,~
I
Purge gas in
frompurge ~ ~~!
~'
(i').
'''''' \T~
atmosphere
traps with sample at the adsorption
.? , ) \
~ ~ 3'~ e ;
~
EPC a nc:l sdenoid
:....
< 1-.'"''\0 q, "7 Vent to
temperature (30-4O"C). In this po sition. the carrier gas merely enters and exits the
\~:i=?
't....--: .,
tl'...--'"":
valve,
10 PORT VALVE
After a period oftime sufficient for the traps to reach desorption temperature (200"C). the valve is actuated to the INJECTposition. In theINJECf position.
SAM PLE Helium or nitrogen purge gas bubbles through the sample in Ihe tube
VIAL
i: ':
from each adsorbent. When the valve is in the LOAD position, the sample-laden purge gas from tbctesttube or VOA val isdirectedthrough the two traps, then out to vent, loading the
the carrier gas flows through the traps in
the direction opposite to the sample-laden purge gas flowwith w hich the traps w ere
loaded, The carrier gas backflushes Purge & Trap Valve in the INJECT Position Carrier ga s in from
camer EPC
"-:
dcsorbed analytcs into the column. while the purge gas flows out to vent
The valve remains theLNJECf position for the optional bake cycle. during which the respective desorption temperatures of
both traps are raised an add ftional Str'C, and the purge gas polishing filter is
~
-9
reco ndi tione d. A relative ly high flow of
->. ~"':""'"\!:0
Out to On-column injector and column <-
v-
4 ,, ,-:/
'- V
'0
~
Purge gas in : I ,.::> I \ PURGEGAS 0 ..i 7]i;;;:;-.. :~ ~ frompurge ~ POUSHIHG RlTER \ I........:... EPC and ~. solenoid V '--I- ~ .-/ ~ 10PORT YAlVE
ViP'15f/ sy /:
SAMPLE VIAL r· •
Helium or nitrogen
•
purgegas buot:res
:
ttlfO'JSh lhe sam ple in the lu~
'0.
It
-..::;, ~ ~i'W Imosp en 0 .._ ' S' a nere
purge gas sweeps throughthe hotpolishing filter. .....hich heats whenever TRAP I beats. Th is purge gas flow sweeps contam inants fromthe polishing filterand out to vent. The va lve is then acrtatedback into the LOADpositioo, TRAP I and thepolishing filter hea t are turned OFF, followed by
TRAP 2. rhea the purge gas (see the Event Table on the General OpeI'ating PrDcadures page.) Trap h ooting, vuJ..-c rotation, and purge gao; control are automated through the Peak Sirnple data ~)':)ll."IIL
7 (of 550 ) 2006(-2016)
8
INJECTORS Purge & Trap
.Sample Preparation
Sample preparation depends on the sample type. concentration. amount, etc. The third editionofSW&46 fromthe EPA isacccssibleontheInternet Go to http ://www.epa.gov/epao5werlhazwasteJtestfmain.htm and click on the 5000 series link to down load Methods 5030 and 5035. Method 5030 Method 5030 style purge and trap is for-the analysis ofVOCs in aqueoussamples. This purgeand trap technique is limited to analyres tbat purgeefficientlyfrom water. 10mL of thcsample is placedin a clean test tube. The test tube headspace willcontain ambient air.so ifyour laboratory or work areais not free of solvent fumes. they will showup in yourchromatogram. F OJ" aqueous samples:
I. Inserts 10mLaliquotoftbe aqueoussample into a clean test tube. 2. Plug the test tube opening with your thumb andshake it untilthe contents are evenly dispersed.
3. Quickly slide the test rubcovcr thepurge gas tubing and into the purge head, and tighten it in p lace with the knurled retaining nut.
Test fube
VQAviai
4. Immediately begin the analysisby pressing the Rtf!': buttonon the front of the GC or by pressing thespacebaron yourcomputer keyboard.
For medium concentrationsoilsamples, doa quickmethanol extraction: I. Place 109ofsampleinro a clean glass container, Add 2OmLofmetbanol
and shake it for 1-3 minutes, 2. Allow the soil toscttlc, then pull l 00~ of th e liquid solution into a glass syringeand inject it into the testtubecontaining 10m.L oforganicfreereagent water.
3. Plug the test rubeopeningwith your thumb and shake it until the contents are evenly dispersed,
Always use ceen
sample containers
4 . Begin the analysis. You may need to dilute the sample more or less. depending on the concentration.
Method 5035 Method 5035 style purge and trap is forthe analysis ofVOCs that are purgeable from soil at4O'-C. This method docs not allow the VOC's to escape the VOA vial until it is punctured by the 5035 purge head needles. Approximately 5g ofsoil, weighed in the field at the time of collection, is sealed in a pre-weighed, septum-sealed, screw-top VOA vial containinga preservative solution There is no needto inserta magnetic stirring bar -since the SRl purge and trap mechanically agitatesthe VO A vialduringthe analysis. Organic-free rcagentwarcr; surrogates, and internalstandards(if applicable) are added through the syringe port immediately before beginning theanalysis.
1. Insert the VOA vial containing 5g ofsoil and 5mL ofrea gcnt water into the Method. 5035 purgehead. 2. Using thesyringe port, inject5mLof organic frccrcagcmwater,internalstandards, and surogarccompounds into the VOA vial. 3. Begin the analysis by pressing the RL"X button or the computer keyboardspacebar.
8 (of 550 ) 2006(-2016)
9
INJECTORS Purge & Trap
General Operating Procedures The following are genernlized operating guidelines for the SRIPurge& Trap system I. The purge gas flow is contro lled with an Electronic Pressure Controller (EPC). Setthe purge flow (measurable at the trap vent at the rear of 'tbe purge an d trap system) . 40mUmin is a typical purge flow. The pressure required for 40mUmin through . single Tenax trap is printedoo therightpanel of the GC. Ifyouinstallthe optional Carbosievc trap or anotheradsorbent trap in the TRAP2 position, you will need to raisethe pressure to maintain the flow. N EVER use hydrogen as apurgegas. SRI recommends helium purge gas, 2 TRAP I is in the lowerposition in thePurge & Trap, and lRAP 2 is in tbeupper position. The tra p temperatures are factoryset al 200"C for desorption and may be adjusted using the trimpot
setpoiats on the top edge of the GC's front control panel. For adsorption temperatures. trap 1 is set at 3Q>C and trap 2 is set at 35"C. Trap heating will be controlled by th e timed E vent Table during the run. Note: the actual trap temperatures typi cally run S"C over the setpoint. See the information and instructions on the following 2 pages for adjusting tb e trap adsorption temperature
settings,
Typlcal50:1liS035 Evett Table EVE HTn"'E
m '"
EVENT FUN CT 011
0.lD>
zseo
.... . g
0 .100
EO' "
P.. ~ ~('V
0,,"
sig ....
( D "CfI")
S~ « "'GN"
,.roo
(D " OFF")
ShWlt.">:o n "
s.""
E "OFF "
Pwglt "OF F"'
B.lD>
C " C·f/'"
TUIl:!:(huOc"VH"
B""
r " ON'"
Tr.. I ( h0U9"Off'"
e.ece
GO'"
v...... ifI " tu ECl"
raccc
EO'"
P.. ge "&
12. Q:Q
S"ON'"
"em
G" OFF"
fr. .. nl"CoN" (+5:10:) v. ~
""L.OMI"
,.""
F "'O rr"
T,..., 1 "OfF"
15 .100
C 'O Fr
Tf..., a "OFF"
E" OH"
Puge "':f"F"
B ' OfT"
Trap n t" Cf F" (+0)
,,,"" ,..co
3. Set the valve OVcD temperature to lOO'Cor higberto avoid water conde nsation. If you're using Method 5035, set the purge head heater body temperature to 4O"C. It is factory set to 4O"C but is user adjustable. 4 . Load or create an event table tha t is appropriate to the sample to be analyzed, or that is designed for compliance with a particular EPA Method The valve ov en in your Purge & Trap system is labe led with a typicalPurge& Trap eventtablefor asingle Tenax trap. The event table shown above isanexample for both methods; the only difference is that Method5030 does not use Relay D (the sample vialshaker).
S. Load or create an appropriate temperarure programforthc cohunn oven Epap<erTl is a typical Purge& Trap tem perature program file provided with the PeakSimple software. As a basic rule forgoodsepar:rtioo, thecolumnoven should bekept: at4O"C for 10- J2 minutes: thefirst 8 minutesoftherunplus24 more minutes after thevalve actuates to the JNJECT position.
6. Activate and energize the detectors asnecessary. For instance, if'you harlan Environmental GCsystem, you wouJd tum on thePID lamp current, light thc FID flame, and set lhc D ELCD reactortemperature. Choose the detector gain settingsaccording to the analysis. Consult the manual sections for your particular d.etectot(s) operating procedures.
7. When the system is at temperature and displaying a stable signal . insert the sample test tube or VOA vial
intothepurge head and beginthe analysis.
....-...
9 (of 550 ) 2006(-2016)
10
INJECTORS Purge & Trap
General Operating Procedures Continued Using Two Traps The SRI dual Imp design givesthe Purge & Trap user manyopticns to effectively Imp and release analytcs froma particular adsorbent, Due to its lowaffinity for water;Tenax™-GR is especiallyuscful forthepmging of VOCs from aqueous samples. making it a goodg eacral purpose trap for EPA style purge and traptechniques. The Carbosiev el" packed trap is very rete utive, Because it lends to retain a large water peakand smear the otherpcaks, it sbouldonly be used when vinyl chloride is amongthetarget: anal ytes, This tendency to smear may be reducedby manipulating the desorption times forthe two traps. lithe CaTbosievenl: trap (TRAP 2) is desorbedwhile the Tenax™-GR trap CIRAP I) is still cold, the components will refocuson the TenaxTM_ OR. The TenaxTM"(]R trap is then heatedto desorb the components in a more narrowband, which results 10 sharper peaks o n the chromatogram.
TenaxTII·GR Properties Composite of Tenax TA and 30% graph ite
Low water affinity 3SO"C temperature limit 200 nm average pore size 60180 mesh size Available from A1ltech 2051 Wau kegan Road Deerfiekf, Il 60015 USA 908-78lh$5O
www_aBted1v
Dual Trap Event Tabte lEpap&t2c.e.rt)
eve vr zaec
e VENT FUNCTION
c.'"
,.....
P\lll ' - OW'
S.'"
e -o r-
P.. ~e -OrF"
EVENT TIMe
nrco
' .000
0 · ....
Trap 2 (C. bo. ioe....) "u ! "ON'"
7. 1])0
G " CM"
Va"," in ". U ECl"
'000
G - OFF'"
V. "' in""l.O.:lD-
F - ON'"
T'.. ~ 1 (TBWlO GoR) __ - ow-
.'"
'"000
CarbosieveT1ll 5111 Properties Carbon m olecu lar sieve Moderate wa ter affinity 4OO'C temperature limit 15-40 angstrom averag e pore size 60/80 me sh size Ava ilable f rom Supelco
a 'Os '8 ~1
G· ....
VaM. '" "NJ Ec r
' 2lDO
,·W
P"'lI, "ON"
" 000
G "OFF'''
V..lvttin "LOAD "
' 4 llXl
F "OFf -
T",p1 "CKr"
"mo
E "OFF"
P"'l, "OFF'"
'U,.
S- ON"
T, ~
set"etr (+5l"C)
15.1!Xl
C "or r-
T,apZ "a r-
tsscc
S "OFF"
Tra p uot "OFFO
S Upieco Pari<
Bellefonte PA 16823 800-247-6628 VNIW,sig ma-aldrich .co m
Version 2 .66 at the PeakSimple software indudes Epap&t1 e.evt for a singl e trap, Epap&t2c.evt for rwo traps.
am
10 (of 550 ) 2006(-2016)
11
INJECTORS
-
Purge & Trap General Operating Procedures continued Adjusting Trap Ad sorption Temperatures During the purge and trap process, the purge gas carries significant amounts of wa ter into the traps. The Tenaxnl trap is unaffected, due to its low affinity for water. The Carbosicve'?' packing tends to retain the water,resulting in a large water peak at desorption. Adsorption settingscan be adjusted by the user-to set the Carbosicvetrap at a high enough temperature to avoid water-retention. However; this temperature may be too hot to trap target analyres. Therefore, experiment to find the adsorption temperatures that work best for your eralyses. Oncepinpointed, they usually requ ire no further adjustment GC Chassis Interior
1. Removethe 6 screws that secure the bottom panel to the rest oftheGC chass is. Supportthc panelwhile yougently rock the GC onto its back. then lowerthe panel to your-work ing surface to access the chassisinterior.
2. Locate thePurge & Trap board; it is one of a group of similar-looki ng boards installed along the back and top walls ofthe GC interior. The Purge & Trap board has two trimpots rigbt next to each other, and it is marked wi th an upsidedo\\'Tl "P&T"" on the lower outer -comer;
The PtIrge & Trap board is installe d in this area inside the GC chassis
The Purge & Trap Board 3. The two trap trimpot sctpoints are on the outer edge of the board. The
trimpot for Trap I is on the bottom. and the top rrimpot is for Trap 2. T:J.m the trimpot while press ing: the
TOTAL button a nd observing thebrightred LED displ a y to set the t rap
adsorption temperature.
4. When youare finished adjusting bo th trap adsorption temperatures, place the bottom panel on the GC chassis. Support the panel while you gently rock the GC onto its base. Secure the base with its 6 S('Te\\'S .
11 (of 550 ) 2006(-2016)
12
INJ ECTORS Purge & Trap Swi tching / Replacing Traps Three traps are included with your SRI Purge& Trap: a Tena:~n.f-GR trap and a Carbosicvc'Y trap. both
permanentlypackcd, and a blanktrap. The blanktrap may be packed with anadsorbent of the user's choice or left blank, depen ding on the analytical situation. Follow the instructions below to access the traps for switchingor replacement.
1. With the red protective GC covet -raised, remove the Purge & Trap cover plate by loosening the four brass thumbscrews at its comers. 2. Care fully removethe t\VO squares of white insulation from each valve oven duct to exposethe fittings that secure the traps ends 10 the 1/16 ' O.D. tubing leading to the 10 port valve.
3. Gentlyslide the trap assemblyout of the slots in thevalveovenducts(thereis enoughslack in the heater and thermocouple wires to pull either trap about I inch outside the duct). 4. Use two wrenches to loosen the 1/8" Swagelok type nuts that secure the traps ends to stainless steel 118"· 1/16" reducing unions.
S. The trap heater is a clamshell design, consisting of'two halves. To rem ove the heater from the trap, loosen butdo not remove the two securing hex heed screws. The two halves of the clamshell heater will open enough to let the trap drop out. 6. Attach th e replacement trap to the reducing un ions w ith th e trap's two 1/8" nuts. Use stainless steel nuts
and brass ferrules when replacing traps. DO SOT usc graphite ferrules. as grap hite has some adsorption propertiesand may interfere with your analysis. 7. Slip thetrap into the clamsbcll heater and tighten the two hex head screws.
s. G ~J y push the trap ends back into the slots in the two interior d uct walls. making sure that the black spacers arc between the duct walls and the trap heater. TO AVQIDDAMAGE, ARRAKGE TlI E TR.-'\PS SO TI IAT O!\"E TRAP' S HEATER WIRES DO KOT LAY AC ROSS TIlE OTHER TRAP'S HEATER.
9. Repesrthe process wi th the ether trap ifnecessary, Replace the white duct insulation squares. then replace and secure the Purge & Trap cover plate.
SRI Trap Assembly Reducing
~ , :r-1V~::'
'lJ: 4:
valve oven duct wall / ' (soned 10eccomccate the Impends)
1/B"SWagelok type nut
Trap heater J-lex-hft~
,/
screws
~
Black spa cer
cartr~ge ~
Heale r wire, r hermcccope Wire (conne cted to the
hex head screws by screw term inals)
.1-.
,
II
~I
n--
1116- 0 .0. tub :ng to the valve
}eadi ~
12 (of 550 ) 2006(-2016)
13
INJECTORS
Purge & Trap Metho d 503015035 Purge & Trap: Changing the Purge Heads 1. To change the purge heads. first disconnect the two purge gas lines at their fittings on the top of the front valv e 0 \ en duct
2. Ifyou are removing the 5030 purge head, pull it out tow ard tho: front ofthe GC. and unplug the 5-pin
>
Xl.R dmrnny plug.
5035 Purge Head
>
3. Ifyou are removing thc 5035 purge bced, squeeze the protruding tail ofthe spri ng toward the heate r body with your thumb as
you pulltbc purge head out towardrhe front oftheGC. Unplug the cord from th e socket on the Gc. 4. To install the 5030 purge hea d, line up the securi ng rod with the bo le. and gentlybut firmly push it in until it locks intoplace. Connccttbepurge gas in and o ut lines to the fittings on the top of the front valve oven duet. Connect the dummy S·pin XLR plug to the socket on the GC.
5. To install the 5035 purge head, hold the spring tail in a downward direction against the heater bod y as you slide th e securing rod mrothehole until it locks (the shakerwill Dot work ""ilhoutthespring). Connect the
-~ ""fF~ .'~-.
:.~'~~ .::::::e , -- ...I l" _ • ;:mmn>i Illliiil ~
- r,1I1111
;~~
~ -~- . ~J. ~
The spring lail (encircled in white) protrud es from the botto m o f the fro nt
valve ovenduet.
5035 Purge Head Sewring rod
I Spring Ia'i
p urge gas in and out lines to the
fittings on the top of the front
valveoven duct. Connect the 5·p in XLR plu g to the socket
S-pln XlR plug
5i:in Xl R sock et
on the Gc.
13 (of 550 ) 2006(-2016)
14
INJ ECTORS Purge & Trap
.Expected Performance
The followingtwoscts ofchromatogramsare from an Emironmenral GC systemequippedwith aMethod 5030 compliant Purge & Trap, a PID detector; and a FID/D ELC D combination detector. First, a lOppb BTEX PhIS sampl e was analyzed usingthe 5030 event table on the GeneraJOperating Procedures page and the Epap&t.tem temperature fi le. Second, a w ater blank was run through the system under-identical conditions to show thc componentcarry-ovcr lcvcl ofthe Purge & Trap system. Toluene is used as a representative of the carryover in the Purge & Trap system; ifthe carryover level ofToluene is bclowu.Sppb. then it willnot affect subsequent analyses. NOTE: The TeE ghost peaks in the water blank chromatograms are augmented or C3USCd by our factory test laboratory contamination. p rust d i[l; s o lved in 1CmL of Sample: 11.li.. 10 0ppm BTE X walf!1' to yield 10ppb BTEX Plus
FJ~ReWlts '
i
CQl11PQrJ
f':!... ~n
Area
Sutvent
10616 15 .0 33 15 .883
921.09 00 1019 9260 A41 8700
S-z_
rrs
R:E 18 ,700 To!IJl1ne 17683 EIDyt Ber=e 20.016 Ortho Xyle ne 20 ,800 Bromoform 21 .166 Taral
f~~!e~'~i~§i~~~~~~~~~~~~~~~~~~~~~~~~ -·-£-'-'''' -.- '-M -'-*- - - - - - - - - - - ----;,- - - - . ----;, - - , Ia , i ., I :e -' :~~~~~~~~~~~~~~~~~~~~~~~~~~~~
"; ::r ;-e~t "' -". " ,...,
''''.... C·-....
I
Ie:'
!
T
~
"
"
3833770 1195. 3320 "''"';;',:' ~''iil.'''' 5'' U e", 124 7,3420 1258.9260 78.9360
;\
d
6M 6. B080
I -
!l ,
PIO Res u~s :
-.
Cunponent
Re'Mnfion
Are3
BelUe....
15 01 6 15.866 17.666 18 683
311.1630 25843S0 353 2 100 233.4750
Ethyl Benzene 20 .000 Ortho Xylene 20.783
343 ,9640 350 .7040
TeE
reaeee
R:E Brornotorm
21 .133 101<11
DELCOR....w1li; Con~l Ro.kffltiun TO:' 15.883 R:E 18.883 ~ 2 1.150 To:..l
32 ,3470 1863.3080
,
, ~ i A I ".IOI:l===:::==:::========~=====::!'~====~:d -.,.. " ..... _-!
~,
\
~
.±CJ
At",..
192. 1020
,,.= 527.11160 209-"6IJ
res
1S.BS3
T~
17 .566
::thyl 8ellzene 20 0 16 oreo Xylene 20 800 PID Rel>ur.s.: COI .gonen:, TCE
r......
Ortt1OX~
~
,
,,• ,\
~
N"
15.866
258.':'360
17 .533 20.783
T='
4 ,340
Rete ntion 15 .750
Are a 46 .034 0
-
~
,j.
,
-I
--J
!
i
~
,
350 7()40J 600. 1300
DELCO l-lMUrS :
ccm cc neet TCE
f
,.
Re~
!
~
i,
To ta l
f:
.
;\
...- "" ~-.:ion
,
, i
e
fn ~'tS:
..
::: 1ill',"_ 81 '\ :t r. -, •
T
Compaoetlt
~ ,. ~
J
~, G: P'
"
:
"
i .==-.J
~
14 (of 550 ) 2006(-2016)
15
INJECTORS
Purge & Trap Troubleshooting and Maintenance Carryover Carryover is a slightcontamination of the purge and trap system by analytes (especially high boiling components), and is a nonnal condition ofoperation. All purge and trap systemsexhibit some carryover. An organic free reagent water blank is analyzed aftersample runs to determine thecarryover level. as shown on the &pectedparlortnant;&page. Most regulatory QualityControl rcqulremcnts ullow carryover that is either less than the Minimwn Detectable Limit (MDL) or less than I00/0of the reportcd anaJyte concentration. For example, ifthe reported analytc conccntration is I 00ppb, then IOppb is acceptable carryover. lfthe carryover is greaterthan an acceptable level, subsequent water blanks are run until the carryover is sufficiently low,or untilthe user has determined that there is system contamination that requires further cleaning.
Thecarryoverlevel of tile lOppbBTEX sample on the Expected pedonnance page was determinedby comparing the areas ofthe resulting PID Toluene peaks, where x is the ppb coccenrration ofthe carryover. ....1... = _ x_ 353 10pp b 353x = 40ppb x = O.1133ppb
The IOppb BTEXsample analysis resulted in a Tolueoepeak withan areacount ofapproximately 353. Thevvater blankanafysisshows a To1uenepeak. with an area countof approximately4. Since thecanyoverof Toluene is less than 10010 or O.Swb. subsequen t analyses may be resumed.
Most carryover problems occur while enelyziug sam ples of unknown concentration. Because the user cannotassume therewill be no carryover in this type of analyticalsituation,a cleanwater blankshould be run betweeneach sampleanalysis to ensure that carryover will not affectsubsequent sample analyses. Avoid carryovercontamination problems by screeningyour samplespriorto purge and trap GC analysis. SW·846 containstwoappropriatescreening tec hniques :
•
Method 5021, in w hich an automated hcadspacesampler isusedwitha PIOandDELCD
cqu ipped GC
• Method3820. in which a hexadccane extraction of tbc sample is analyzed by a FlO and! or BCD equipped Oc. Segregate the screened samples according to concentration, then run the highly concentrated ones first, Clean the purge and trap system after the high concentration samples have been NIl., then analyze the low
cooccntration samples.
15 (of 550 ) 2006(-2016)
16
/
Chapter:
PURGE AND TRAP CONC ENTRATOR
Topic:
HARDWARE ORIENTAT ION
Cooling fan for traps
maintains selected adsorbtion tem perature and rapidly lowers trap emperature from desorblion tempe rature ( typicall y 200 C )
Pu rge and Trap Sample Concentrator Opt ion is mounted in the special du cted heated valve ov en located on the left side of the B610C Gas Ch romatograph. The Purge and Trap opt ion is not available on the Model 310 GC.
Purge vessel uses d isp osable 16mm test tu bes and rugged needle sparg ing tube. Sparge head all ows gas standards o be spi ked in th rough built-in septum port .
he SR I Purge and Trap concentrator allows low levels of org an ic compounds in water to be automatica lly extracted from the water ma tri x and collected on one or two series mounted adsorbent traps. The purge and trap tech nique is applicable to a broad range of m olecules from about C3 to e 12. Molecules hea vier Ihan e 12 do not purge we ll from water nor do po lar molecul es which resist purging due to their sol ubility. The SR I Purge and Trap is unique because of the dual trap design wh ich allows two different aoscrtient trapping ma terials to be used, and each material can be adsorb ed and desorbcd at Indiv idual temp erat ures and different lim es. Th is flexibility all ows for tighter des orbtion bandwidths, and greater wate r rejection than other Purge and trap designs which have only a sing le mixed adsorbe nt bed trap. Additionally, the disposable test tubes wh ich hold the water sample are ine xpe nsive ( 5 cents each U.S ) so they can be thrown away in the event of contamination. A 10 position autosampler can be easily added to the Purge and trap fo r un-attended ope ration. HOl l .doc
16 (of 550 ) 2006(-2016)
17
Chapter:
PURGE AND TRAP CONCENTRATOR
Topic :
HARDWARE ORIENTATION
Co lumn oven
The purge and Trap option Is mounted on the GC chassis in a special ducted heated valve oven j ust 10 the left of the column ove n
To cfl ange traps this cov er plate mu st be rem oved by loosening the four brass thumbscrews located at the com ers.
Traps are located between d ucts so that t he ends of the traps are enccsed within the heat ed duet area while the body of t he tra ps arc suspended in the trap heal ers between the duets . A protect ive grill keeps fingers and too ls out of the trap hea t zone while all owing hot air to
10 port electri call y ope rated Valco valve mounted in the heated valve ove n is the heart of the purge and trap ha rdware. The va lve ov en is typically set to 150 degrees C so water will not con dense.
escape.
A vent tube is located at the
back of the P &T va lve ove n. The sparge gas exits from thi s vent tube atte r passing through the traps.
Dud s enclose ends of traps within heated valv e ov en to prevent co ld spots.
17 (of 550 ) 2006(-2016)
18
Chapter:
PURGE AND TRAP CONCENTRATOR
Topic:
HARDWAR E ORIENTATION
Remove the protective wire grill from the top of the valve oven for better access to the raps
Remove the two squares of
wh ite insulation from each duct to expose the fitti ngs which secure the trap ends to the H 16th inch O.D. tUbing leading to the Valoo valve.
-
.
To accessthe traps for melnten ence or replacement: 1)
Rem ove the left side plate from the purge and trap valve oven by loosening the 4
brass thumbscrews at the comers. 2)
Remove the protectiv e grill from the top of the valve oven by loosening the two
screws. 3)
Carefully remove the two squares of white insulation from the duets at the ends of the traps.
H023.doc
18 (of 550 ) 2006(-2016)
19
Ch apter:
PURGE AN D TRA P CONCENTRATOR
Topic:
HARDWARE ORIENTATION
1/8th to 1I16th reducing fitting at end of trap
Clamshell type trap heater halves can be separated by loosening two hex head type
screws.
There is enough slack in the neetemnerrro-coupre wires to pull the trap about 1 inch beyond the duct . To rem ove the trap : 1)
2)
Loosen the 1/8th inch swage /ok type nuts wh ich secure the trap ends to stai nless steel 1/8 to 1116l h reducing unions using tw o wrenches . The trap healer is a Clamshell design wh ich w ill separate when the two hex head screws holding the heale r together are loosened . With the trap heater apart the trap itself can be remo ved .
H024.doc
19 (of 550 ) 2006(-2016)
20
I
PURGE-AND-TRAP
Chapter:
Diag nostic FlowChart Pag e 1 of 2
Troubleshooting Purge and Trap Contamination
Topic:
IS th e t o-rx>n: gas sampling valve even tenperarure ~ng
Use this troubleshooting lIowcI1art ff you are experiencing difficulty with
sa: and
a!XM! 15O"C? Set valve oven t em perature
above 150"C ana perform 2 blank runs.
Det ermine th e conca"ltTatia1 at the cootamination. its area to the area obtained from a , 0 Pf:tI
compare
standard analysis. Is tne concentration of contamination significant (> 1120 at '0 ppb {0.5 ppbl )1
contamination when perfonning purge and trap
I
Does the
contaminarlon persist?
onaJyses. Tum off the sparge gas pressure (set to 0 psQ. After perform ing two blank analyses, are the contamination peaks stiD
a pn:bIem?
Tum me sparg e gas pressure back to normal setting (4-5 psQ. Bake out me polishing
I
filter. Then run 2 clean wereIs contamination still a
blanks.
proCIem?
The contaminarion,
reduced to an acceptable level, appears to have been I1(M'
The concentration is below 0.5 p~ (1120 01 ttl e area obtained from a 10 ppb stanaard). This level at background is acceptable ana ilsignifi cant and wiJJ I'lIX adversely affect yaJf
Proceed to pege:2 of the diagnostIc flowchart.
Clean the sparge head. baddlow trap and all gas lines
in between. Then make rwo blank runs. ts the contamination still a problem?
I I !
Contamination p rob lem has
been resolved.
ana¥is.
Repeat th e cleaning of the complete Spar!J!ng apparatus, including the water trap. This should e!m inale the problem
R~
Contact SRI Instruments for technical assistance in diagnos ing this
cenCition.
the ernre sparging
appara%us wM a section of clean tubing. Atter p;rlorrning two more blank runs, is the contaminati on
still
a problem?
accum utal:ed on tne polislling tilter. 1lle
poUshing filter shoukl be
baJ
--
perio
The contamination, insigniF.eat1t was
now
jocared
in me area ex
tne sparge! backtlow heads aroJor related
tubing.
Using a heat gun. heal the entire spar!Je head assembly with the sparge head's injection pen nut removed while sparge gas is flowing. After petfOlllling a blanI< ana/r-iis, is the comamination still a prctllem?
LocaliZed
heat cleaning resolved the
prOOlem.
20 (of 550 ) 2006(-2016)
21
Chapler. Topic:
I
PURGE-AND-TRAP
Diagnostic F _
Troubleshooting Purge and TI1Ip Contamination (continued)
C Use this troubleshooting flowchart ff)'Ou are experiencing difficulty v.ill1 contamination when performing purge and
trap analyses.
From page'
I
• pi::lr ID removing lI'l8 rtl lOf, rote the posIbon C! a. eee- stamped on one el'ld 01 tnll metal tin pwlXling the lOP. T1'is Iet:ef lI'l8 rotIY 19mperann raung. bLA: a.tso essss i't onenting ee rI'l trOperIy osng rein5:allaoon cf IIl!I rolOr after c:18aRng. Ml,CfI lik8 a ~ CIiSlJ'tMDl'. In! l'O1O' can be rercsooeo 180'" wrtlI'll;. ~ In vaNe lallle.
oean
rrom
meatllS
Begin on page 1.
traps and the column. the fittings. Look for graphite shavings in trap and column endS. R""""" shaving ff foom Then petom a blank analysis. Are
I
=:>
Bemove trap heating events (relays C and F on) from event table. Perform two mere blank runs. Is the corICel l[J a1ion of contamination stiD a prOOfem?
ReplaCe the graphite teruee securing the
Page 2 of 2
With a clean test tube, sparge and carrier gas flowing and the gas sampling valve in the INJECT position. bake out the traps for 15 minutes. ActivaIe relays C and F with trap secpoints of 3OQO C. In the INJECT posjtion. the traps will exhaust to the column (raise the column temperarure). Perform 2 blanl
the contamination pea.ks stiU a prClb'em?
Set the trap temperature to 250° C. ts the contamina1ion stilt a
The traps were
Remove- and clean the gas sampflt'lQ valve rotor. Clean the rotor seat. ReinstaJI the rota. Is contamination stiU a proOIem?
Replace the stainless steel nbng around the gas sampling valVe. Is "'" cmtaminafJcn SliD a problem?
retaining anaJyte.
Graphfl:e is adSOrbenL It is possible tha1: tne ferrules couJd adSortl
Spent uaps may tend to retain anaIyte. Replacement
anaryte if ecceec to a higtl concentra1ion.
maybe
New ferrules e liminated the high contamination level.
The sampling valve mOl' and I
or rotor Seal: appear to have been contalT'inaIed. Oeaning trIe area eliminated the CCIllaminaIiOO prcOlem.
indiCated.
j:rObIem?
Replace the traps with blank tubes. Pertcm 2 mae blank runs. Is the contamination still a problem?
Remove" and clean the sampling valve rotor. Clean the rcJlor seat. Perlorm 2 blank runs. Is contaminaIia'l
still a prcbIem?
It appears that the traps
thai
Dirty SRI
to< teen, support
tubing. N"" tubing
was !he fix.
in use are
contaminams. Replace the traps to eliminate the problem
Replace all 1116"
Call
were
detective and retaining
The sampling varve rotcr and I or seat was cooraminared. Cleaning the rttor area surfaces eliminated the prOblem. Further cleaning may be necessary as contamincnion works through the valve body.
stainless steel purge and trap IUbing around the gas sampling valve. Is
contamination prOOIem?
still
a
Gall SRI ret further
assistance. Diny tubing. New tubing was the fix.
21 (of 550 ) 2006(-2016)
22 Mal Chrm. 1996 . 66 , 3(31 - 34 33
Effectiveness of Purge-and-Trap for Measurement of Volatile Organic Compounds in Aged Soils Minoa D. F. Askari.1 Michael P.
Maskarinec. ~
Stacy M. Smith,~ Paul M. Sea""t and Curtis C. Travis·';'
University of Tennessee, Knoxville, Tennessee 37996, EM-4S1, 1000 Independence Avenue, U.S. Depanment of Energy, Washington, D .C. 20585, and Chemical and AnaIytJea! Sctences and Hsafttl Sciences Res8a rc;tl Divisions, Oak Ridge National tsoomtones. Oak Ridge, Tennessee 37830
The Il.S, EPA-reannmended meth od for measurement of trace levels ofwllltile organic compounds (VOC5) in soil.
pJU'2e-and-trap,measures the readil).' desorbabk organic C01l1am;naots from 50iI pore spaces and external soil
surfaces. It does not. however, measure contamination that has diffw:;t!d into internal micropon:s of soil matrix. Thus, the purge-aod-trap method m easures only 8 small fraction of total soil contaminants. especially in kmgcontaminated soils, where -90-99",1; of con tamination may be in the interior of th e soil matrix. We compared three methods for determination of " OCs in ae-ed field
sampJes : purge-aud-trap, methanol immersion, and hot solvent extraction. Hot solvent extraction proved to be much more effective than the U.s. EPA -approved purgeaad-trap ltdlJIique. For tI:uff Jont-eontaminated soils con taining su ch VOU as tricbJoroethwe, benzen e, tolu-
ene . chloroform. methylene chloride. and cu.l,l -dicbJo. roetbylene.l'eCOVft'Y from purge-and-trap ranged between
1.5 and 41.3% that of bot solvent extraction. Our data show that purge-and-trap may oot be the best methodol~ for mcasUJ'in£ so il " OCs ccnceatraticus, parti cu1Rrly in aged lOOils. it is dear frottJ this and prn10uS studies that the best O\~ ch oice for soil VOCs meas.unmeulS is hot solvent extrnetioo. These resuns also indicate the inefficiency of purge-and-crnp as a method for t!\-aluatina' vapor extraction remediation technology. Our results suggest that th e EPA sbould review the use of the purge-and-trap method for measUl'int Voc.s concentrnti.ons in so ils .
.Ii crilQl require-m=l in th~ cleanup of conwninated soi: sites is an accurate determination of the naturt and extent of soil contamination 'Ibe primary U.s. EPA-r«Offill'lt"ndl"d method (EPAlS'W-84&5030A and 826OA) for measurement of volatile organiccompounds (Voes) in soils ispurge-and·trap.l.2U'>foUowed b)' gas chromatography/mass spectroscopy. Under this protocol organic-frN. ....rarer containing internal standards and surrogates is mixed with J. soil sample and he.led 10 40 "C. An inert gas is bubbled thro ugh the solution at ambient temperature. and the v:zpor is passed throu.rh a sorbenl coiumn. wbere the volatiJt. components are adsorbed. After purging is completed. the scrbent column is heated and backflushed with inert gas to desorb · UIIlW'l"Slt'l· 0: TtM~¥t. ' Clwmirat _
' r .s • (Il
" ...lyt ical
~I'lmm '
~
DWlsior.. OR."L
0: t:.~.
fi~¥.h ~~ ~ardl
Di\=on. OR.\·l.
C«' vi FN:~I ktp1JJ!Jrnn. Pan $~ : Tl:.Jt «~ U.s. ~'fl<"/:~ Prin:ial/ Off...... w..q .lI'.r'GlI. DC. ~'J'<4. C!wollT ElI,"tl'Ollr.otr:W Proledoc
: . App. III. I' b. O~ ll'
,\,rtol c)·
r. l
the components onto a gas chromatographjc cohrmn.! Use of purge-and-trap to measure VOCs in soil is based on tht assumpucc that sen VOC, rapidly equilibrate with soil water. Recent studies.~-~ however, strongly question this assumption and indicate that soil desorption is a biphasic process with an initial rapid surface desorption followed by a much slower. diffusion· limited. desorptive phase from the interior of the soilm:aoiL~-I""' : : The biphasic nature of desorption casts doubt on the widely used. EPA~ mrnen ded purg ~an d-trap method. wh en soil has been in contact with VDes fl)f a long time peri od (~t'd soils). VOCs diffuse into soil mkropores, where they are unavailable for purgt"-alld-rrap measurement Except for a single studt involving l .2-dibromoethant' (EDB), the impact of soil aszinR on the effectiveness of VOCS measurement techniques is Witly unexplored, Th e present study focuses M. the dfecriveoess of three common!)' usedtechniques tor ~ \'OCs concentrations in aged sells. purgNnd-tJ'2p. methanol immersion, and ho i
methanol extraction, Since"APOf extraction is a currently popular technique for removal ofV OCs from soils. we subjected one soil sample 10 air stripping to evaluate the effect of vapor extraction on tht' extraction dfidency of putg e-and-trap measurements. EXPERIMENTAL PROCEDURE Soils . Soil samples were obtained b"om three ~PhiCaJlY disl:ribut~d sites with a l o-20-}'E'af history of VOCs conwnination. The Kentucky soil had hii"h cla~' content. with 100 ppb of trichloroethylene . The Louisiana soil was a silty loam, w ith 3000 ppb of ro.l.1-dichloroethylen~ and 6OCO JIJIb oftrichloroethylelle. The Florida. soil was silty, fine to ver). fiIl e sand, conlaining m~thylene chloride al 240 ppb. benzene at 2 ppb. toluene at 190 ppb, and ch lOT'Dform at 2 pp b.
Sample eonection. Soil samples we'~ extraetl'd with .II hollow-stem auger and spirt-spoon sampler. Undisturbed soil S. M..; Pirnatdlo. J ].; ~whM'Y. B. L E..~ ...... XI Ttr/n: oJ. 19.'17. 2J . 12l:l1-L.""J8.. 0 , Pa.l...rarl\is. S. G.: /roUlho;..-4Il. <:t. /'00 . f u m.... Sci Tid"",. 1992. 26. 532(21
S1~inbo-q:.
saa
(tl
Kz:1.. A. T~ f ll.. G
0'
F,",,," "- KiJwl<"I. D. T~
E~ .. ",~
so. THIt.,,[
1..&"""""
f'~
1994 . lA. 859- 801 . I' crT1Il'I'I. C . 1'. £~n"9'l. $n'.
T~~J
199 5 . 29. 1 564- 1~. (6) Pi!:"alt llo,]. J. E~ ";",~ T",,;<<>1 Clw~. 1990, 9. 11 l1i ~ 1115 (7) I'Ignall'ItO. J. J.; fri nk. C. It: Marin. P. A.: Dor:o;tt . £. X- j. CO"/Q",;~. H.wt"'l. 1990. 5.1lJ5- 21(, ( 8) ~~"Y. B. L ; r'~ttlk>. l. J ~ Srl'MbtTg. S M.). t:- "'.... Qw l. 19 68 . J7.
](!>- 1~
I~ \\-r.kO'Oo~i. P. l~
Gaf. P. R.: ftrran. R. A
J-
(.(JOW,,, ......
11."'''''-
1988. 2.
:M -:!69 (IV) Plrv~:h ~ S G.: J~.a: K. l (Il l T", ..... C C : Madnn l&, J. t.:.. .!:.m
A n(llytiC:l1 Cl'lcm'(try,
Xi T..ittttll. 1991.25. :7,f-?/'< 5n 7...Jo"*". 1992 . ~'t . 199,, - I R~ ~
Vol. 68. No. 19, (ktOOP.f 1. 199 6 3431 22 (of 550 ) 2006(-2016)
23
Table 1. Comparison of Th r" Method$ fo r
compounds
.....il lypt". component
trichloroethylene
Kentu cky (c!3yJ Louisiana lsil,,' loam) florida
(silty. lin~
rne.a~ring
w very tine ~..,d)
ee-Ll -dichloroethylene trich loroe thylene mWl)'ie ne chlo:lde
",,-
"."....,
chiorolorm
VOC.. in Soib purj.:"E'-an ri·tTa;r'" (mg/ kgl 100 ± 57 3070 ± 351 5900 ± 1210 ZW±63 2::: I 190 ::: 41 2::: 0
met!-.anol
immcrsioll" lrr.!:/ kg) 140::: 15 26 000 ± 43590
85000 :: 13 115"
530 ::: 31' 110 = S' 240 ::: Il' 110 = S'
hot me-dumol extrac tion" (ml:/ kg l 240 = 31' 41 700 = 2082' 121700= 11 719"' 630 .:~
I SO :: Z5' 270 .: 3"" 130 % 25"
• A~ of three "" il umple measu rements. I Sip:nificlUltly hig her mean than PUll\'Mnd-trap aI 95'i level of con fidence. ' SiKDifjcan tiy higher mean than pur~an d'!TlIp al9O% level of confid~ce .
T.-ble 2. Comparison of Extractton Mnhods for L.out.-.. Soil after 1 Week of Air Stripping
,......,,-
C'Ompotmd rnethvlen e chlorid e
hot methanol
inunersiort4 (mglkst:J
extr.l.ctIo~ (mg/k~O
94 ± 5O
I SO:;; 43 390 :;; t nt 5400:: 91t¥
160 ± 110 2110 ± 1688' 5500 ± roai'
86 ± 39 310 :: 60
ee -i. i-dichloroclhylt'ne m eI'lloroeth"lene-
~.hanol
(m g/kg)
• A~·en.ge or tnree soil sample measu~rs. • SiJ:nifiamtly highe:- mean than pmg't...al:lf;l..~ .3t 95\ leee l of C'O rdHienc:e t SiRl\ificantiJ.· higher mean th an Ptrge-ar.ci-Irop at 90\ It-Yd If. confdence ,
cores were sealed in glass jars with minimum headsp ece an d stored at 4 °C on anivaI. At the start of each experiment the sample core was plu2led and subdivided to obtain three 5-g subsamples.. Subsamples were extruded directly mtc VOA vials (1»-natech. Bat on Rol/i't . LA) and mixed with 5 ml of weeconla:in:ine lnlermJ standards and surrogates before capping. l'oIeas~enlS on'OCs. Contaminan ts ....t!""e extracted from soil samples by meth ods of purge-and..t rap. methanol immersion, and hot methanol extra ction. Contaminant concentrations were expressed as micrograms per kilogram of soil . PrtrgNJ7Ui-Trup. SamplealiquoLS were purged using a D)nal. ech PTA-SO -.uto:;ampkr" and :II Tekmar (Cincinnati. om l.SC-2 pu~ci"lnP device. Soil 5lIIIlpIes of 2 g each were PW'ied at 40 ·C. The trap was desorbed. and measurement WlIS perfumed with a Hewle tt-Packard Mood 5lNl/S971 GC/ MS. using and EPA metho d 8260, I~.lJ AD quality assurance measures given in the method were followed. MnhQM l lmmm;itm Five milliliters of purge-and-tnilp rrade methanol wa s added to sample aliquots.. The vial was c:apped as fn'\'KJ usly described and yjzoro usly shaken for 30 s to facilitate we1ting of th e soil ecrrace. A 5O-oIL aliquot of the methanol was the n remov ed and added 10 5 mL of wate r conWning Internal standard s and surrogates. The water ""<15 then subjected tu purgt" and-trap and analyzed for the concentration o f chemicals by GC. Hor MrtAallOl E.rtta.ctJDJl. Hot methan ol extraction wa s per.. formed in th e same manner as mettlanol imme rsion except that. prior to withdrawal of the aliquot of methanol the VQA vial was placed in a 40 °C ultrasonic"wa ter hath tor 3D min. The methanol was drawn and analyzed as described above.
&troctiO'7l Following Air StriPPillK. The Louisiana sample was mixed in a 7:3 ratio with calcium oxide to prevent solidification during air soippinK. Th e sam ple
"1"'35
then placed in a Buch ner
c. L 1'lr,s",,,,,J r,.i... 1M~I b:'< G
..
funn el with a vacuum running from the bonom of the funn el thI"Ough a flask. Ambient elr was passed through the sample using a vacuum of 450-675 mmHg for 1 week. Occasional mixing of th e soil was perionned throughout this time. The soil sample was divided into three subsamp&es. and each sebsample was then subjected to one- of the three methods as Pl"C'\,ously described. All of the above extractions was performed as wri tten in EPA! SW-846 me th odology , Internal standard s w ert' add ed , and surrogate recovery '0\'3.5 within th e limits of the method for all extractions. All quality assu ranc e procedures were applied .
RESULTS Measuretl1eItt results from the three dtfferent snes-Kt:ntucky. Louisiana. and Florida.--are preseJlled in Table I. Trichlorcethylene was the only contamin ant detected in the Kentucky soil (Table 1). w ith a purge-and-trap re covery only 42% as compared to hot methanol extra ction. Both tU-l.l-dichloroethyie ne and rric:hloroethe:ne were detected in the Louisiana soil Purge-andtrap recovery of these two con taminants ';lo"JJ.S only 7.4 and 4.S\.. rnpectiv~·. when co~ to ho t methanol extl"'3Ction method. Four compounds were identified in the florida soil methylene chloride. benzene. toluene, and ch lorofonn. with purge-and-trap recovery 38.0, 1.5, 71.2, and 1.5%. re spectively, in comparison to hot methanol extracti on. Effect of Air Strip~ Contamin ant concentrations for a jrS'J'ipped Louisiam !lOiI are presented in Table 2. Purg('-and-trnp detected levels of methylene chlori de. cis-Ll -dichbroeth)iene. and TCE at 58. 4.1. and 5.6\, respt."Ctively. tha t of hot melhanol extraction. ComparisoD of these results v.ith those in Table 1 for Louisiana soils indicates that air stri pping does not appear to affect the distri bution of contaminants between the accessible and inaccessible phases .
------.
DISCUSSION f>u:-ge-and-:np is tht EPA-recommended method
23 (of 550 ) 2006(-2016)
24
protocol. organic-free water is mixed with a soil sample and heated to 40 0(' An inert gas is bubbled through the water, and the concentration of chemicals in the gas is measured with a gas chromatograph. This method is effective only if 'laCs in soils rapidly desorb from the soil surface into surrounding water. Laboratorycontrol samplesusing sea sand in place of soilsindicate that for nonadsorptive solids. purge-and-trap recovery is acceptable. Recent studies2- U H •IS on the physical inaccessibility of contamination in soils sugges t that this may not be th e case, particularly in lone-contaminated soils. It has been hypothesized that aginginvolvesdiffusion into soilmicropores, partitioning into soil organic matter, strong surface adsorption, or a combination of these processeS.2.l Wi.l 7 Previous studies6.18 indicate that 2090% of contamination may be located in the interior of the soil matrixand thusinaccessible for purge-and-trap measurement The purpose of the present study was to compare the effectiveness of three commonly used techniques for measuring' VOCs in soils: purge-and-trap, methanolimmersion,and hot methanol extraction. We found that purge-and-tnIp consistently underestimated the concentration ofVOCs in aged soils by factors ranging from 2 to -100. This consistent underestimation of soil concentrations undermines the EPA's attempt to remediate contaminated soils to levels consistent with health-based cleanup standards. The soil desorption process is known to involve two distinct phases:
HalZioger. P. B.; Al exa~Mr. M. Eft~jrmt. Sd Tit"'"I . 1995, 29. 537
(151
P;i'Il~tel i
F.-.r.mdillU. f . J~
Huan~.
'-45.
1.. O. £><. St;;. Tt (i,,,
27, 156:3-1571. (161 Brussea u. M. L: JeSsup. R. E.: Rao. P. S. C. Eft"",,,," $n. Tuir""r 1991, 25.134- 1C Il l} Wu. S. C,: G.rn""'~d. P. M. E."".,,,,. Sci. T_,,<>L 1986, 20 . 717- 725. ( 8) SmiUl.. J. A.; Ch,QU. C. l.; Kr-..."mer.J A; lGle-. D. E. E""i""" 56. Tw"wl. 1990,24,676 -663.
WI) ),1~tk3y. D. M.: Cherry. J. A Eft"",,,,,, 56. Ttcknd 1989,2J. 63(\-636. (:!OJ Di TOr<>. D. M ~ Hone-rnpa, L M. E..vmm. Sd.
'"'
T~ch""l.
1982,16.594-
(:?l) Ce>at... , J, T.; Elzerman. A W.J- Umr.o...ift_ Hyd."L 1986, 1. 191-210 r.!2) Pignatello. J. 1.. Hu;/.Slg. L Q. J. £'''~''}ft . QwaJ. 191:11, so. :1:.::1- 228. (23) Scribner . 5. L : Benzi ng , T. R: Sun. S.. Boyd. S, A i . £,,<~""'. QI,,,1. 1992. 21.115-120, (24) TeS! mcth od$ toe evaJu~ti ng ""li d w~Slc. EPA/600- SW--8-t6. 3m I'd_ \2:;) Heertt, A D. Cold Ref:lons Regem-e1tand Enginernng Laoonl1OT)'. ~l
-- '.
R~n ~ o.
93-5. 1\-by 1993.
Arsenal wee found 10 be 1-3 orders of magnitude greater than predicted using soil-gas concentrations and equilibrium conditions, n The present study found that the purge-and-trap method, as compared to hot solvent extraction. recovered only42and 4.8%. respectively. of TCE in long-contaminated clays and silty loam soils. Even in freshly spiked soils. desorptionrates of pollutants can be 1-3 orders of magnitude smaller than equilibrium-predicted rates: Cleansoils spikedwithhalogenated aliphatic hydrocarbons for 24- 72h resisted desorption after 16 extractions of 24- 72 h each." These observations bring into question the OCOJITellce of desorption equilibrium necessary for validity of the purge-andtrap measurements in the freshly spiked and aged soils. Previous analysis oIEDB in long-contaminated soils has shown that purge-and-trap is less effective than extraction at 75°C with organic solvents such as methanol, acetonitrile, and acetcee.w recovering less than 11%of the total EDB found by hot solvent extractionS Ourpurpose in the present studywas to extend these results to a larger class of VOCs in aged fi eld samples. Hot methanol extraction proved to be more effective than the EPAapproved purge-and-trap technique. For three Jong-contaminated soils containing such VOCs as trichloroethylene, benzene, toluene, chlorofonn, methylene chloride, and cs-Lf-dichloroethylene. recovery from purge-and-trap ranged from 1.5 up to 41% that of hot methanol extraction. Slow desorption is recognized as a serious obstacle to soil remediation technologies. IW .2l>-2: For such technologies as pumpand-treat, vaporextraction, and bioremediation to be effective, soil contaminants must be accessible. To simulate the effect oivapor extraction on the efficiency of the purge-and-trap methodology. we subjected the louisiana soil to a week of air stripping. Purge-. and-trap recovered only 58% of the methylene chloride. 4.1% of the cis-l.l-dichloroethylene, and 5.6% ofthe TeE that hot methanol extraction y..as able to recover. These results indicate that the purge-an d-trap method is not a reliable method for evaluating vapor extraction as a remediation technology. It is dear from the resuhs of this and previous studies that the best overall choice for measurement of soil VOCs is hot methanol extraction, since this method yields a more accurate analysis, regardless of the age of contaminated soil. The VOC data from three differenl soil types clearly demonstrate the limitations ofthe EPA-approved purge-and-trnp method, which can bias analytical results by several orders of magnitude. depending on soil type and chemical properties. We suggest that the EPA review the use ofpurge-and-trapas a method formeasuringVOCs in soils. ACKNOWLEDGMENT
Oak Ridge National Laboratory is managed by Lockheed Martin Energy Research Corp. for the U.S. Department of Energy under Contract DE-AC05-960R22464.. Received for review January 3, 1996. Accepted June 17, 1996." AC96 0009C • Ab-str3ol:t
ptl bli~
in MO~I"~ ACS Absrmc:.. AuI':'J5I 1. 199ti.
Ana/yfiCdI ChemiSTry V",r 68. No. 19. DcfObe: t , 1996
3433
24 (of 550 ) 2006(-2016)
25
GC AC CESSORIES 10 Positio n Meth od 5030 Purge & Trap A utosampler Retrofit The purge & trapautosampler retrofit kit contains everything youneed to add a 10 Position M ethod 5030 Purge & Trap Autosampler to yo ur existing SR I purge & trap equipped GC. The kit includes a new purge & tra p cover .nlatc (A), a transfer line to valve connectiomls), ar.d a .purge gas line(C).
.
A . Purge e trap cov er plare:
I. Remove the existing purge & trap cover plate from the GC by :.:DSCTe'.'<-!ng rtc four thumbscrews that hold it in place.
----: :- --
,~
4. Feed rhe autosampler's red heat transfer line through its cover plate hole, then secure it with the hose clamp
includedwith tte aurosampler; B. Transfer line to valveconnection: I. Remove thevalve even lid by unscrewing thebrassthumbscre...-onthe frontedge of the lid. tilt ing the front ofth e lid up, then sliding hack slightl y to free it from the screw in th e back. Carefull y remove the white ins ulation padding, and set it secure ly aside with the oven lid 2. Connectthe Valco fitting to PORT #2 ofthe gas sampling valve (the Valco fitting is labeled " CO:;\X ECT TO PORT #2"'). 3. Feed the transfer lin e completely throegh the Swag elok fitting and 1I16"'tubing (th is fittmg
is iabded"I"SERTX-FER LINF"l. 4. Use a wrench to securely tighten the fitting until it is SIlUg against the graphite ferrule; donot o....er-tightea. C. Purge gas line:
1. Remo ve the glass test rube from the purge & trap.
2. Connect the brass union on the purge gas line to the purge gas rube(formerly inside the ~' ess test tube). TbedurableTeflonTv. ferruleic the brassunion allows this operation to be perform ed many tim es.
3. Connectthe 1/8- nut on tee purge gas fmcto "P URGE NO> on theeutosampler;
See the S RI manual for rel ay beard insrulluuon in structions: " AUTO S A..c\1PLE RS ; Installation of the Relay Board fe r the 10 Posit ion Me thod 5030 Purge & Trap
Auiosampler fandother Autosampters)"
25 (of 550 ) 2006(-2016)
26
A UTOSA MPL ERS In stallation of the Reley Bo ard for th e 10 Position Method 5030 Pu rge & Trap Autosampl er (and other Autosemplers) "i
m "
,
I
"
$
,
,
a •
B¥"
A relay board is provided with theautcsampler for connecting it to en SRI 86 i 0 GC. This relayboard supplies the additionalrelaysrequired to operatethe autosampler, and must be installed inside the GC by the user. The relay board comes with the necessarywiriag. andno soldering is required. 4 holes fOf Relay 3card screws The four holes in the right side panel of the Gncbassis, under the "Relay Functions " table, correspond with th e rel ay board securing screws. The relay board is installedon the inside cf thispaneL
it
.c,
-
.- .0
,' .:.:......-
.:!- • ;;;
Hole 70r at:".csampler con trol cable
AD beard
Aut.csaI"l".pIer corrtrol caale rwtingh de
1. Remove- the six screws holding the bottom pane-Ion1±:e GC chassis. Supportthepanel while you gently rock theGC onto its back, then lower the panel to your working surface to access the chassisinterior. 2. Secure tbefour , -- - - -- ----, GC chassis aluminum stand::;; / pa"" offs in th e relay
"- I
board hob . use
venow
Connect the green & relay board wire to the chassis ground stu d screw
- >: ~-oE,, I' , ,
the four hex-bead screws provided, and sec ure the
stan d-offs fro m the outs ide of the Ge panel. Insert the relay board into position sotharthe compoacnr side taresoutward. Secure it in placeon the aluminum stand-offs withthe fourphilips headsere...."Sprovided.
i Phili ps
:
I i
Hex-
head
;j
head
,
screw - > ='=']<-
SCfflW
4. Connect eachofthe fcuryeliow wires. differentiated by color stripes, to the appropriate TIL relay outputs GC cha ssis panel o n the _~'D(Law son) boani All I eight of the TIL outputs are N O 9QAR:> (lAWSON) Identicakase any available ones. Connect the blueand red wireto the Amp board 12V terminal.
Re:ey outpcts A-H; ¥e!!O'N rela y coe-c vires co-s-ect ~ ere
5. Remove aileofthe plast ic hole plugsfor the autosempler control cable. Rou te the control cable through the bole. and L"O.c...nec t eachwire to the appropriate relay circuit on the relay board (see aut osam p ler con t ro l ca bl e labeling).
26 (of 550 ) 2006(-2016)
27
(
l
Chapter:
PURGE-ANn-TRAP
'\
Topic:
10 Station Purge -and-Trap Au tosampler
j
The SRl 10 Station Purge-and-Trap Autosarnp ler permits the unattended sparge, concentration, and analysis of up to 10 separate water and I or soil-in-water samples, when used in conjunction with the SRI EPA-Style Automated Purge-and-Trap Sample Concentrator option available as a built-in option for all SRI 8610C gas chromatographs. The Peakximple data system (or other data system offering timed event control of external events via relays) is required for automated operation of this system. Manual controls are also provided for direct, manual control by Manual remote cootrol with digital position display and momemary stepping I home
__SJ'.. .0 l!.l C
•
toggle switch
... .. ........
@ ...
='W=~J! i!l il l !I I I I I I I! I : -:
-
Left bank of S sparge beads
\
•
.....
G~ remote control
<,
wand
Right bank of
5
spaTgte'
beads
the analyst, including a remote cabled sample position stepping control that features a digital LED display of the
sample position in use. The toggle switc h on this control has two momentary-on positions. Pushing the
toggle switch to the up momentary-on position causes the automated sample stream selection valve to step to the
next sample in order. Pushing the toggle switch down causes the sampling valve to return to the home (sample sparge head 1) position. The
sample sparge heads are numbered according to their sampling order. A stainless steel knurled fitting holds the disposable glass sample tubes in place. Teflon ferrules in the knurled fitting seal the sample tube s in place,
preventing gas leaks . to STATION PURGE-A.'D-TRAP AlITOSAMPLER SIDE VIEW Only two gas connections are needed to supply the autosampler with sparging gas, and to deliver the sample-laden sparge ga s to the purge-and-trap sampler's dual trap concentration system. These two gas lines re place the sparg e head
assembly on the EPA-style purg e-and -trap system. A remote control signal cable connects the autosarnpler valve control electronics to the data system external event control circuitry. This simple cable requires only three connections to the data system event control relays, common, step, and home. The data system must provide a mo me ntary closure between the common wire and one of the two action wires to move the stream selection valve to the desired position. Any of the 10 sample vessels may also be used to contain a clean water blank (o r air) for use between analyses for blank runs. The stream selection valve must be stepped to this blank position, and then to the desired sample position for blank operation. A large volume headspace sample may also be introduced into the system for concentration onto the dual adsorbent traps, as each sparge head is equipped with a gas injection port for manual syringe injections. In this manner, a SOcc, IOOcc, or larger volume headspace sample can be passed through the traps, in order to acheive low sample detection lev els unattainable by regu lar headspace inj ection on -column using standard microliter to milliliter volumes. The sparge gas supply should be turned on to assist the injected sample to flow through the traps when this feature is used. D:\96EPDOCS\lllSTAOI .FPO
27 (of 550 ) 2006(-2016)
28
Chapter:
PURGE-AND-TRAP
Topic:
10 Station Purge-and-Trap Autosampler (continued)
As illustrated below, the SRI 10 Station Purge-and-Trap Autosampler is configured in a symmetrical, space-saving bilateral design. Located along each side of the unit are 5 sparge heads with respective headspace injection ports. The autosampler should be located to the left side of the SRI 8610C GC for ease of operation and access to the sample tubes. The gas transfer lines provided with the autosampler permit separation between the auto sampler and GC of up to 24 inches. This
Insulated heated transfer line jacket
/
Gas injection
port
--+'1 -~~___
Sparge gas inlet ~ (from spargt: gas outlet on
16mm x 250mm disposable / sample sparging tube
SRl 8610C GC)
A C power outlet box and leads <,
Sparge bead and disposable glass sample tube
W ide-bot-e fused silica -lined metal capillary transfer line to 8610C GC purge-and-trap inlet (replaces GC sparge bead)
<,
SRl IO STATION PURGE-AND-TRAP AUTOSAMPLER FRONT VIEW
allows the analyst to have access to each sample sparging head and injection port, and to move the autosampler around on the lab bench as needed, while maintaining all connections and operability. As the autosampler is a stand-alone unit, it does not require a hard attachment or bracket for GC mounting. A 3' length of 1/16" stainless steel tubing carries the sparge gas from the GC's EPA-Style Purge-and-Trap Sampler sparge gas outlet (previously supplying gas to the single sparge head), and an insulated, electrically-heated capillary transfer line returns the sample -laden gas to the purge-and-trap system ' s dual adsorbent traps via the GC-mounted purge-and-trap plumbing and sampling valve hardware . The glass sample tubes are low-cost disposable 16mm x 250mm (2Occ) straight-mouthed test tubes available in bulk packs from SRI or any laboratory supplier. The sparge head assemblies are stainless steel hardware that is heated by the valve oven that they are mounted to, eliminating cold metal condensation of sparged analytes. The bilateral configuration of sparge heads with respect to the stream selection valve, located inside the heated, insulated valve oven, permits the use of the minimum amount of valve plumbing. This ensures efficient and complete transfer of sample-laden gas through the autosampler system, for delivery to the GC and purge-and-trap concentrator. The headspace gas injection ports use the same 1/8" molded silicon septa that are used in the GC's direct on-column injector, minimizing the need to maintain a variety of consumable replacement parts . Unlike the on-column injector, the headspace injection ports accept needle sizes larger than 26 gauge , such as those commonly found on large volume gas sampling syringes. D: \96EPDOCS\ I OSTA02.EPD
REV. Jt).Jt).96
28 (of 550 ) 2006(-2016)
29
Chapter:
PURGE AND TRAP
Topic:
Connecting The Free-Standing Hl-Station Purge and Trap Autosampler
The physical appeannce and configuratiOll
of the to-station purge-and-trap is subj ect to change without notice due to continuing improvements in hardware design
-.........•, - .•...- .
..,.,.,.,....."' ...
Nul o:ull
fenule
Valve control cab le*
/
Black
SIDE VIEW SHOWING CONNECTIONS
FRONT VIEW OF lo-STATION
• r... infortnlbon
~ nililow nllboa cable remooo COdnlI . . .00 scIcctica. lICe rN1ECTOR &.GAS VALVE x:etioo of this 11lIIIfAl.
used for
PURGE-~TRAP
AlITOSAMPLER REV . 11..(13...06
29 (of 550 ) 2006(-2016)
30
1 0 PORT
REMOTE CONTROL CABLE
AUTOSAMPLER
m% 0
~~
", •
i..."" - ~ ~ ~
~
~
.
~
•
~
•
:.!! ! ~ 5:: ! J~ -!-. '..-
'IE
'1
~-
! c :;,
s
~~
•
< 0
<
,
~n
",
,O•• N
•i
.~ rm
~
nn
~,
~CD •
-
~>
>~
A '• en ~~ A
n
e
[;
~ ~
=~ ~> on
~ 90
•• .." !
i
. .filii! ! si
oo
n
• n
~
•
0
•"
...•
• I<
0
%
~ eil~cj 0
• ~
'J -s
•n0
•"z
H
• Z
'1
n
•
r J$
•" ~
• "J
~
iqi
•
;'1l
e
n
•
C! ~
0
;
<
e e
~o
~ .
0
g ~Cl
;; ~ " ~~g
0
,
-t
0
"
tH>-
"
2
,
~
I !
2 1464
17
30 (of 550 ) 2006(-2016)
31
,,
I
Chapter:
PURGE-A.'ID-TRAP
!
Topic:
Connecting The On-Line Liquid Sampler To An Existing SRI Purge-and-Trap
I
!
,~--------------------' The on-line Liquid sampler accessory for the SRI purge-and-trap sampling system is an external unit designed to deliver, purge , and evacuate a liquid sample from the SRI purge-and-trap sample concentrator, on a repetitive basis, under data system automation. This permits the unattended monitoring of any fluid effluent or stream on a continuous basis. In order to operate this acce ssory , the following installation steps are required: 1. Locate the three cables exiting the rear of the on-line liquid sampler. Find and connect the AC supply cable to an available AC wall outlet. A second cable terminates in a remote control wand for the optional manual operation of the liquid sampling valve. Operation of this control is by means of the toggle switch provided. Make sure that the valve is in the LOAD position before proceding. The third cable is the control cable for the sampling valve actuator. Of the 5 wires in this cable, only three are used (green, black, and red) for control of the valve loading and injection. Connect these wires to an unused relay (or relay s) in your data sy ste m (green is common). 2. Four ports are located 00 the front panel o f the on-line liquid sampler. The upper left JX>r1 is the liquid sample .inlet, where the inco ming sample flow is connected. The lower left port is the sa mple outlet for liquid that has pas sed through the Sec sampling loop to the drain line. Route the drain away from the GC and any electrical devices and connections. TIle upper right port is the sparge gas inlet Disconnect the sparge gas supply line from the GC to the original p urge-and-trap sparge head, and connect it here. The lower right port is the sparge gas outlet from the internal liquid sampling valve. 'This outlet is directed to the inlet of the modified sparging head provided with this unit.
3. Remove the original purge-and-trap sparging head from the GC purge-and-trap sampler, and replace it with the sparging head provided with the on-line liquid sampler. Note that it is equipped with two lines that enter the sparge head through the top. From woilified From spuge eas One line delivers the liquid sample , propelled by the flow outlet of on-line sparging bead to of sparge gas through the liquid sampling valve. The second sampler (carrier solenoid-ccorrolled drain line line is the drain line that C3IT'ies spent sa mple from the sample into ~ ----,.sparging head to the drain line, after passing through a modified purge-.and-uap solenoid-controlled valve that controls draining. .-.:>0.....
sparging bead)
Liquid
~-
sample inlet
Sparge gas
WI" (f~GC)
:-:<::::':~::::::::::::':%:':::::':::::::::::::<-';:;""; ;$;':';:;:';:::':~;::;;:;:;;;::$::::::~;;::;:::;:::::::::::; .:.·.·.·.·.v.·.w.·. "'......... .......... w.'" .·.·~
.,
· .::~::: ; ;:,, ;:: : ; :: :: ,;~ ; ·<,,;:;»: ,· ::»:« :>i« ~
Sparge gas " Wid =
sample-1aden gas to purge-and-trap
coecenaaror
·.- .w .-~ -.-. -.w., ·_ ·~., ·.w.·. · .·.·.·.·.·. ·.·.
Liquid sample ourle (drai n)
r \
Sparge gas outlet (to sparge bead)
........ ·;~x:;::;::::::::" :::;'::' ::'::::: :::: '':' :' ':::;:': ., ,-
FRONT VIEW OF ON-LINE
U QUID SA.\1PLER ACCESS ORY
:\10DrFlE D SPARGE HEAD FOR
PL"RGE·AND-TRAP SAMPLER
o,,\97E1'0c:>c5\ONLINEI .fJ'D
31 (of 550 ) 2006(-2016)
32
, - - -- --
-
-
-
-
-
- -- - -- - - - - -' .
Chapter:
PURGE-AND-TRAP
Topic:
Connecting The On-Line Liquid Sampler To An Existing SRI P-&-T (can't. )
4. Once the on-line sampling accessory hardware has been connected to the SRI purge-and-trap
sampling system, edit the purge-and-trap timed event table in order to control the on-line sampler as an integral part of the purge-and-trap system. The event table used should be similar to the timed event table that follows, making note that events H and D specifically control the liquid sampling valve rotation and the sparge head drain valve, respectively. Once the event table has been input and saved, the system is ready for operation. TIMED EVENT TABLE FOR ON-LINE LIQUID SAMPLING ACCESS ORY TIME
EVENT
DESCRIPTION
0.100 0.200 4.500 5.100 5.300 5.400 6.000 6.100 8.000 12.000 13.000 13.100 14.900 15.050 15.100 15.200
EOn HOn DOn E Off DOff HOff COn F On GOn E On GOff BOn F Off E Off C Off B Off
Sparge Gas Activation (Gas On) Rotate Liquid Sampling Valve T o INJECf Pos ition Sparge Head Drain Valve Open To Drain Sparge Gas Activation (Gas Off) Sparge Head Drain Valve Closed Rotate Liquid Sampling Valve To LOAD Position Heat Trap #2 Heat Trap # 1 Rotate Purge-and-Trap Sampling Valve To INJECT Position Sparge Gas Activation (Gas On) Rotate Purge-and-Trap Sampling Valve To LOAD Position Add 50 Degrees To Trap Temperature Setpoint (For Bakeout) Heat Trap #1(Heat Off) Sparge Gas Activation (Gas Off) Heat Trap #2 (Heat Off) Add 50 Degrees To Trap Te mperatu re Setpoint (Back To Normal)
SIMPLIFIED PROCESSION OF OPERATION - O N-LINE UQUID SAMPLING ACCESSORY
1 At 0.2 minutes, the sparge gas forces liquid sample from th e. sample loop in the on-we liquid sampling accl'ls,<;ory into the sparging bead for analysis .
D:\97EPDOCSIONUNE2.EPD
2 Through 4.5 minutes, the sparge gas pas ses through the measured VONmC of liquid in the sparging bead, and the. sparge gas passes to the purge-and-trap concentrator.
3 At 4.5 minutes , the sparge gas forces the liquid in the sperging bend out of the VC43CI a:I the drain solenoid valve opens, allowing the sample to be drained completely. REV. 00-26-97
32 (of 550 ) 2006(-2016)
33
Stream Flow using Standard Vacuum Pump
3/16103
Stream Flow· 118"' Tubing 1IS-Tubing Length (ttl 50
100 150 200 250 300
Flow (mUmin)
570 420
240 150 80
60
The flow was measured from theeldt port of a standard Rena Vacuum Pump.
600 500
ace 300 200 '00 0
,
2
3
•
5
•
33 (of 550 ) 2006(-2016)
34
Chapter.
CUSTOM MODIFICATIONS
Topic:
Custom Val ve Configuration Diagram
Mas! of the gas chromatographs manufactured 01' SRl that employ multi-port gas valv es follow a standard gas line connection and flow path scheme tha t is specific to the user 's applica tion and/or dictated by the anaIyticaJ test method. The majoriry o f these gas valv e schemes have been diagrammed and are included in the Injector and Gas Valves secti on of the unit' s manual . Th e page header info rmation will quickly identify the di ffe rent application diagrams for the user 's refe rence. In certain cases, the ren-port valve must be plumbed differently in order to perform a unique function as required by the use r of the instrument. If man ual entries have been made on this diagram page, the SRl gas chromatograph that accompani es this manual has been equipped with a ten pail valve that has be en custo m-configured to the speci fications o f the use r.
All custom plumbing of this ten-port valve will be documented on this page by the build er for the user's reference. Pleas e not e tha t there are TW O dia grams shown o n this page . The first diagra m represents the relationship between port connec tions and flo w scheme when the valv e is in the LOAD positio n (rotated counter-clockwise}. The second diagra m represents the relationship between port connections and flow sc heme when the valve is in the ll\"JECT pos itio n (rotated cloc kwise). These diagrams ar e applicable to both manually-operated valves and automated valves built into this chromatogra ph.
AP PUCATION OF VALVE :
_
10 PORT GAS VALVE
10 PORT GAS V A..L VE
o 0-0 CQ
CiJ000
,
o
0
~ @-
~~ <,
Valve
III
;
LOAD posmc n
Valve
III
INJECT position
DESCRIPTION OF CONNECTIONS MADE AT EACH PORT OF GAS VALVE 1
_
2
6 7
3
8
_
4
9
_
5
10
C ,\EP2\ OOCS'.[ :-.'JCUST I. EPD
- -- - - -- - - REV 0'2-08-9;
34 (of 550 ) 2006(-2016)
35
,"----------------------~~~-----~~~~Chapter:
INJECTORS AND GAS VALVES
Topic:
Custom Dual Valve Con figuration Diagra m
Most of the gas chromatographs manufactu red by SRI that employ multi-port gas valves follow a standard gas line connection and flow path scheme that is spec ific to the user's applica tion and/or dictated by the analytical test method. Th e maj ority of these gas val ve
schemes have been diagrammed and are included in this section of the unit's manual. The page header information will quickly identify the different application diagrams for the user' S reference . In certain case s, the ten-port valve must be plumbed differently in orde r to perform a unique function as required by the user of the instrument In some applications. dual valves are required and utilized. If manual entries have bee n made on this diag ra m page , the SRI gas chromatograph that accom pan ies this man ual has been equ ipped with dual ten port valve s tha t have been custom-configured to the spec ifications of the user.
Ali custom plumbing of these ten-port val ves will be docu mented on this page by the builde r for the user' s reference. Plea se note tha t there are TWO diagrams shown o n this page. The first diagram represents the relationship betwe en port connections and flo w sc he me when the valve s are in the LOAD po sition (rotated counter-clockwise). The second diag ram rep resents the relationship between port connections and flow sche me whe n the val ves are in the INJE CT position (rotated clockwise). These diagra ms apply to both manua lly-operated va lves and automated valves buil t into this chromatograph.
I
APPUCATION OF VALVES: - --
-
-
-
-
-
-
-
-
-
-
-
-
-
-
to PORT GAS VALVES
10 PORT GAS VALVES
V A
l V
E 1
V
A l V E 2
Valves in LOAD position C;\ EP2\DOCS\INJDUAL I.EPD
Valves in INJECT position REV. 11-1 6-93
35 (of 550 ) 2006(-2016)
36
Chapter: INJECTORS & GAS VALV ES
To pic:
REV. 9-7-91
LOOP SAMPLING 6 PORT MODE
SRI has plumbed the valve in
LOAD POSITION - TURI'/ SHAff CCW
your GC according to the
accompanying schematic. In the LOAD position:
CARRJER - ,
Carrier gas flows onto the col umn while sample gas flow s
through the sample loop. In the INJECT position: Carrier gas flow s through the sample loop and then onto the
column.
L
o o
valco's ten port valve catalog SAMPLE has a large assortment of IN plumbing applications. You can order Valco's catalog from :
VALCO BOX 55603 HOUSTON, TX 77055 (800) 367-8424
P
OUT
_ 0~
1'9Y -,;
~~-~TO
COLUMN
INJECT POSITION - TU RN SHAfT CW
(713) 688-9345 CARRJER - - ,
Your Valve was plumbed by: Date:
GC serial number:
OUT SAMPLE IN '---"::;" TO COLUMN
36 (of 550 ) 2006(-2016)
37
,- - - - - - -- -- - - - - - -- - - - - - - - I
Chapter: INJECTORS & GAS VALVES Topic: ALTERNATE LOOP SAM PLING OF TWO DIFFEREl'.'T STREAMS
SRI has plumbed the valve in your GC according to the
, I
REV . 9-7-91
LOAD POSm ON - TURN SHAFT CCW
accompanying schematic.
In the LOAD position:
CARRlER -~
sample loop A is in position
IN
to be loaded while sample loop
B has carrier gas flowing through it onto the column.
SAMPLE B
In the INJECT position:
Sample loop B is in position to be loaded while sample loop A has carrier gas flowing through
it onto
the column.
r+-;> OUT OUT
SAMPLE A ~;X"-"''t~~ IN
Valco's ten pen valve catalog
'---~TO
has a large assortment of plumbing applications. You can order Valco's catalog
CO LUMN
from: VALCO BOX 55603 HO USTON, TX 77055
INJE CT POSITION - TURN SHAFT
ew
(800) 367-8424 (713) 688-9345
CARRIER IN
Your Valve was plumbed by:
SAMPLE A
Date: GC serial number:
OUT
OUT
IN
'-""::> TO COLUMN
37 (of 550 ) 2006(-2016)
38
,~--------------~ Chapter: INJECTORS & GAS VALYES Topic:
THERMAL SOIL DESORBER
SRI has plumbed the valve in
your GC according to the accompanying schematic. In the LOAD position:
REV. 9-7-91
LOAD POSmON - TURN SHAFT CCW
CARRJER - - ,
Carrier gas flows onto the
column while the desorber is isolated. In the INJEcr position:
Carrier gas flows through the desorber and then onto the column.
'""'
(~~/
valco's ten port valve catalog has a large assortment of
~TOCOLUMN
plumbing applications. You can order v alco's catalog
from: VALCO BOX 55603 HO USTON, TX 77055 (800) 367-8424 (713) 688-9345
INJECT POSmON - TURN SHAFT CW
CARRJER - ,
Your Valve was plumbed by:
Date:
GC serial number:
'--;> TO COLUMN
38 (of 550 ) 2006(-2016)
39
, I I
1
Chapter: INJECTORS & GAS VALVES
Topic:
SIMULTANEOUS INJECDON OF THE SAME SAMPLE INTO TWO SEPARATE COLUMNS
REV. 9-7-91
,------=-=~:....:::..:..::::..-=-:..:..:::~:.:..:-==:....::===------------
SRI has plumbed the valve in
j
LO AD POSITION - TURN SHAFI CCW
your GC according to the accompanying schematic.
In the LOAD position:
CARRIER B -
-
' - 7>"- TO CO LUMN B
Both sample loops are in the load position while carrier A flows onto column A and
carrier B flows onto column B.
In the INJECT position:
Carrier A flows through loop A onto column A while carrier
OUT
r-»;
B flow s through loop Bonta column B.
8
1"9cv -
SAMPLE
~~-~
IN
Valco's ten port valve catalog
'
has a large assortment of plumbing applications. You can order Valco' s catalog
TO COLUMN A
CARRIER A
from: VALCO BOX 55603 HOUSTON, TX 77055 (800) 367-8424 (713) 688-9345
INJECT POSmON - TURN SHAFT CW
,- -)-3> TO COL UMN
CARRIER B
,Gs
Your Valve was plumbed
by:
0-jLOOP B
Date:
GC serial number:
B
-E---t-I. 2
OUT
SAMPLE A IN
1-f--3>"TO COLUMN A
-="F CARRIER A
39 (of 550 ) 2006(-2016)
40
Chapter: INJECTORS & GAS VALVES Topic: LOOP SAMPLING WITH BACKFLUSH TO DETECTOR
SRI has plumbed the valve in your GC according to the accompanying schematic.
REV. 9·7·91
LOAD POSITION · TURN SHAFT CCW
In the LOAD position:
CARRJER -
The sample loop is in position be loaded while carrier gas flows through the column and onto the detector. to
-
, C
DETECTOR
In the INJECf position:
7 H--
Carrier gas flows through the OUT sample loop and then on to the column. however the direction of flow through the column is SAMPLE opposite from the direction in IN the LOAD position .
--";>
0 L U
M N
Valco's ten port valve catalog has a large assortment of plumbing applications. You can order Valco's catalog from: VALCO BOX 55603 HOUSTON, TX 77055 (800) 367-8424 (713) 688-9345
INJECT POSITION· TURN SHAFT CW
CARRJER
Your Valve was plumbed by:
C DETECTOR 0
Date:
GC serial number:
1-+_..:<::;,, OUT
SAMPLE
L U M N
9
IN
40 (of 550 ) 2006(-2016)
41
/~---------------
I
Chapter:
Topic:
REV. 9-7-9 1
.-SRI has plumbed the valve in your GC according to the accompanying schematic.
LOAD POSm ON - TURN SHAFf CCW
In the LOAD position:
CARRIE R -
The sample loop is in position for loading. Column I has carrier flowing through and out the vent. Column 2 has flow from carrier 2.
,
,
0-cv r-./\ L
o
In the INJECT pos ition :
o
O lIT Carrier 2 is venting while carrier 1 flows through column 1 and 2. The direction of flow SAMPLE through column 1 in the IN INJECf position is reversed from the LOAD position.
COLUM N 2
C
o L
P
) -j+ _ CARRIER 2 r--;
8
I~~=tTO VENT
___
Valco's ten port valve catalog has a large assortment of
plumbing applications. You can order valco's catalog
INJECT POSmON - TURN SHAFf CW
from: VAL CO BOX 55603 HOUSTON. TX nOS5 (800) 367 -84 24 (7 13) 688-9345
CARRIER - -
~
Your Valve was plumbed by:
0:(
COLUMN 2
L
o o
Date : GC serial number:
OUT
L
7
CARRIER 2
P
SAMPLE IN
TO VENT
41 (of 550 ) 2006(-2016)
42
Chapter :
INJECTOR S & GAS VALV ES
Topic :
D ual Loop Injec tion of Two Sepa rate Streams Onto One Column
The fol lowi ng is a description of the 10 port gas sa mpling valve plumbed to permit the loading of dual loo ps fro m separate strea ms fo r injec tion as a sing le sample on to a sing le an a lytical colu mn .
ThIS gas sam pling valve configuration permits two sepa rate loo ps to be loaded simultaneo usly from two stream s and injected togethe r onto the ana lytical column.
-
.
10 Port Ga s Sa mpling Va lve in LOAD Position
Carner
ga~
in _ ....._'-~
~
In the LOAD position: T wo se parate loop circ uits exist in this configu ration . Sa mple loop # 1 rec eives sample through por t # 1. and vents through po rt #2. Sample loop #2 receives sample through port #8 and vents through port #7. Meanwhi le the ca rrier gas is rou red into port #4 from the mjecto r. through the valve. and ou t through port #5 to the analytical co lumn an d detector.
Sample loo p I ou t -
+---+-f:
Sample loop I in - ......./." Sam ple loop [ sample: stream
To colum n
Sam ple loo p 2
9
Fig. 1
OUI
'-_<-_ Sample loop 2 in Sample loo p 2 internal standa rd
10 Port Gas Samp ling Valve in lNJECT Pos ition
In the INJECT position: When the val ve is rotated to the Ll\IJECf position . both sam ple loop inlets an d outle ts are isolated (ports #1 and #2, and #7 and #8) . T he carrier Sample loop 1 out -+-1-{" gas entering the vaJve at port #4 is diverted into loo p #1 through port #3. Loop #1 is Sample loop I in now in series with loop #2 and the contents of both Sample loop 1 loops is swept out by the sample stream carrier gas flow , to exit through port #5 to the
analytical column for analysis. At no time is the carrier gas flow to the col umn interrupted, pro tecting both the co lumn an d the detector. C:'.97EnDOC\ \OPORTDI... EPD
To col umn
>+.....- Sample loop 2 o ut '--~- Sampl e loop 2 m
Fig. 2
Sample loop 2 internal stan dard
This configuration is convenient for applications where an internal standard must be inserted into the sample prior to analysis. Both samples are then merged and deposited on-column for analysis when the sampling valve is rotated to
the INJECf position. REV. 04-14-97
42 (of 550 ) 2006(-2016)
"'----- - - - - - - - - - - - - - - - - - - - - - - - -'\
43
.
Chapter: L'"JECI ORS s: VALVES Topic:
Liqui d and l oo p Sampling wi th Backflush o f Pre -co lumn to Ve nt {Using Extern a l Liq uid Samp le Valve I
' '--- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - // S RI has pl um bed th e val ves in
LOAD POSITIO:-J
your GC according to the accompanying schematic.
,.~
v
In the LOAD position: Th e liquid sample valve (LSV) :in in position for loading wh ile the gas sample valve is in inj ect position .
In the f:\-JECT position:
Carrier gas flows through the liqu id sam ple slo t in LS V and the IO-port valve then on to the col umn.
f):JECT POSITIO:-J
The IO-pon valve remains in the iinjecI position throughout the [inj ection procedure and then switches to load position for vent.
I
Valco's ten porr va lve catalogue has a large assortment o f plumbing app lications . You can order Valcos catalogue fr om:
VA LCO BOX 55603
HOli STOK. TX 77055 (800) 36i· 8424 (713) 688-93-lj YOW" Valve was plumbed by :
Date:
GC serial number:
C: \ W~ WORD\ DOCJ...rQVA L.DOC'rJ
REV. 06·26-97
43 (of 550 ) 2006(-2016)
44
TUBE VOLUME SELECTION GUIDE INT ERN AL
DIAMETER
0.001 0.002 0.003 0.004
0.005 0. 006 0.007 0. 008 0.009
MICROLITERS PER INCH
INCHES PER MI CROLITE R
0.0129
77.6979
0 .0515 0 . 1158 0 .2059
19. 0:2 45
0.3218
3.1079 2. 1583 1.5857
0 .4633 0.6306
8.6331 4.8561
1.2140
0 .8237 1. 0425 1.2870 1.5573 1.8533
0.6421 0.5396
2. 175 1
0.4598
0.014
2.5226
0.015
2.8958 3.2948 3 .7 195
0.3964 0.3453 0.3035 0.2889 0.2398 0.2152
0 .0 10
0.011 0.012 0.013
0.016 0.017
0.018 0.019 0.020 0.021
0.022 0.023
4. 1700 4.6462 5 . 1481 5 .6758
6 .229 2 6.8084 7. 4133 8 .0440
0 .9 59 2 0 .7770
0 .1942 0.1762
' 2.3684
0.032
13 .1792 14.0158 14 .878 1 15 .7662 16.6799 17 .6195
0.035 0.036 0.037 0.038 0 .039 0.04 0 0.()41 0.042 0.043
0.044
18 .584 7 19.5758 20 .5925 21.6350
22. 7032 23.7972 24 .9 169
33.4757 34 .8014
0 .0299 0 .028 7
36. 1527 37 .5299 38 .9327 40 .3613
0.02n
41.8 157
0.023 9
43.295<1
0.0231 0 .0 223 0 .0 2 16
0 .054
0.055 0.056 0 .057 0.058 0.059
0 .060 0 .061
0 .062 0 .063 0 .064 0 .065 0 .086 0 .067 0 .068 0.069 0 .070 0 .071 0.073
54.3no 56 .0630 57.n47 59.5122 61.2754
83.0643
0 .0 248
0 .0209 0 .0202 0 .0'96 0 .0190 0 .0184 0.0178 0.0173 0 .0168 0.0163 0 .0159 0 .0 1$40 .0150 0 .01 46 0 .0142
0 .0138 0 .0135
0.0759 0.0713
0 .062
84 .4417 86 .5395
0 .083
88.6631
0 .0113
0.0672
0 .084
90 .8124
0.0634
0 .085 0.086 0 .087 0.068 0.089 0 .090 0.091 0.092 0 .093
0 .01 10 0.0108
0.0600 0.0568 0.0538 0.0511 0.0486
0.0462 0.0440 0.0420 0.0401 0.038 4 0.0 367
0 .078 0 . 079
0 .080 0 .081
0.094
0.0352
0.095 0 .096 0 .097
0.048 0.049
29.6532
0.0337
0.098
JO.9017
0.0324
0 .099
o.oso
32..1758
0.0311
0 .1 00
0.046 0.04 7
47.890 5 49.4735 51.0822 52.7167
0 .0266
0 .0257
0.013 1 0 .0128 0.0124 0.0 12 1 0. 01 18 0.01 16
28.0624 27.2336 28.4306
0.045
44 .801 6 46.3332
76.JOn
0.0809
0.03 4
0 .051 0 .052 0.053
o.on
11 . 5833
0 .033
MIC ROLIT ER.
0 .074 0.075 0 .076
10.8239
10.0903
8.7003 9.38 25
PEA IN C H
0.072
0.0 29
0.025 0 .026 0 .027 0.028
DIAMETER
0.1605 0.1469
0.030 0.031
0.024
p,
M I C ROLI T ERS
64 .8790 66.7195 68.5858 70.4n5 72. 3952 74 .3386
0 .1349 0.1243 0.1 149 0. 1066 0. 0991 0.0924 0.0863
IN CH ES
INTERNAL
78 .3026
80.3232 82.3696
92 .9875
95.' 882 97 .4148
99.6670 101.9450
0 .0 105 0.0103 0 .0100 0.0098
104 .2488
0 .0096
108.5783
0 .0094 0 .0092 0.0090 O.OOBB
108.9335 111.3145 113.7212 116 . 1537
118.6119 121.0958 123.6055 126 .1409 128 .7 020
0 .0086 OJJ084
0 .0083 0 .0081 0 .0079 0 .0078
44 (of 550 ) 2006(-2016)
45
Chapter. ~. I nj ect_ors EPC ( electr<:mic'pressure control) operation ,
,._, :-'-1,i.:; ,
. :"' ~;:--
'
';:"
.,
~,~ :;
,
,:' ,~
' " ,-,
SRI GCs are equ'ppeo wtttI electronic pressu re control of all system gases. Detector support gases suc h as hydrogen and air are controlled by the screwdriver adj ustable local setpcmt on the GC , and once set are seldom altered. Th e carrier gas pressure may be co ntroll ed by either the local setpoin t screwdriver adJustment or by the chan nel two pressure program in the Peak Simple data sys tem so ftware. The ma in benefit of carrier gas pressure programming { ramping} is to speed up the flow rate th ro ug h the column at the end of the run in o rd er to elute hig h boiling peaks more quickly.
Most cnromatocracners choose to set the carrier gas press ure using the screwdriver local setpoint adjustmen t rather than the channel two pressure prog ram for the follow ing reasons: The screwd river adjustment is simpler, and once set is 1) not likely to be altered unintentiona lly. 2) Th e benefits of ramping the carrier gas pressu re are often not worth the extra operatio nal complexity.
Local setpofnt adJustmtlnts for te mperature s and pressures USing small screwdriver
-..._.,, _._-
.'
--
Set the 'Contro l By' rad io button in the Cha nnel 2 Deta ils
scree n to Pressure.
sure Channel 2 Thenprogram enter theinto desired presby selecting the Pres sure screen from the Edit/Chan nel menu
_1~~~~~~~~~~~~9~MM'P :i-..:t~ . _ _ ~
• (" 101
r ,.. .-,-- ,.
[~~ ~~;£~=:T':.~~~:?Jt;~:j?C': ~~.f~
!r:-: ..~:-'-'.I' ~~t~~. ~o;;:'r;:_ ,~ ..
.
~
fiIl · _
_ -- . . • ~ . ~ - . - - .
::~ ...::~~
--- - _ ~
Manl 49.pub
45 (of 550 ) 2006(-2016)
46
Chapter: Injectors '. .. "."--. Topic::J : Enabfin-gthe~can:iergas EPC ' ... "' !;;
.
". "
. - •.. , , ~- -= ~ ~ . ~ .
-';. ',"-
:~=~)~.,.._ ~
-
,-r~-~--··,
it'=-" ;__ ==-:~,;- :"'-~~;='" -; ,~:';'
1)
U n-p lug the GC power cord. Remove the six screw hold ing the bott om cover to the GC cnassis. Ti lt the GC on its back and expose 3) the interior. 4) Locate the AJD board which is mounted on the right hand interior wa ll. Locate the earlier gas EPC wire S) ( green wit h white stripe and labelled carrier EPC ) This wire is attached to a Ground ( G D ) termmal on the NO board before shi pment from the SRI factory. Atta ching
2)
,-
--
=.
-
- .'
this wire to Ground disables the computer control of the EPe. 6) Use the screwdriver provided with the GC to loosen the screw securing the WIre and re-a ttach the WIfe to the termina l labelled TP2. The pressure control signal from the PeakSimple data system is now connected to the carrier gas EPC .
7)
Re-assemble the botttom cover and
screws . 8) Plug the GC power cord back in. Use the screwcrwer to adjust the 9) ca rrier gas local setpcmt to 0.00 . T he local setpoint is sum med with the EPC co ntrol signal from PeakSim ple, so if the local se tpoint is not set to 0.00, the carrie r pressure wi ll be the sum of the loca l and co mputer se tpomts . Enter a pressure program in Pea k10) Simple's channel 2, and verity that the GC pressure fo llows the prog ram.
\
. :~
.-=""
'1111111111111 ~
Some WIllchann be equipped with theGCs single el Model 203 AID board . Other GCs will be equipped wit h the 4 channel Model 202 AID board.
The procedure IS identICal on either bea rd.
~an l.50 . pub
46 (of 550 ) 2006(-2016)
47
The On-column injector is designed for .53mm ( w ide-bore) capillary columns and 1/8" packed col um ns. One or two on-colum n injectors can be mounted on the 861 0C GC , while a single on-co lumn injector can fit on the Mode l 310 GC. The photo at right shows a single on-column injecto r mounted on the 86 10C GC . The on-col umn injec tor is not separa tely thermostatted because it closely follows the temperature of the column oven due to its low mass design and mounting location on the wall of the col umn oven,
Because the insulated allen wall on SRI GCs is only . 7 5~ thick , sample is injected onto the co lumn well ins ide the co lumn oven, so no cold spots can trap the sample, even if the sample consists of high boiling analytes .
For most applications, the oncolumn injector is the best way to inject a liquid sample because the syringe deposits the sample into the bore of the column itself. The column is usually the most inert surface available ( more inert than glass injector liners ), and unlike heated injectors, the sample does not undergo a flash vaporization which can broaden peaks and result in peak tailing. Also, because the entire sample is deposited on-column, boiling point discrimination can not occur as it can wHh split/split/ess injection techniques.
Septum nut with silicone rubber septum seals ca rrier gas in. but allows syringe to penet rate into column
60 meter .53mm metal capillary co lumn shown connected to on-column injector
Vlan111.pub
47 (of 550 ) 2006(-2016)
48
Chapter: -Jnjectors .. .. ,--
-'
-.
..-
"~.-
c_
~
Topic:'-- :::;Oii.:column Injector' Operation- .. . :.
.,.
Th e On-column inj ector consists of 1) The s eptum , ( pa rt#8670- 1353) which is a plug of si licone rubber which allows the syringe to penetrate but wh ich preve nts the ca rrier gas from escaping. The se ptum u sed on SRI GCs is sometimes called a "snirn aczu pluq" type septu m an d is widely available fro m GC supply ca talog s
2) The special septum n ut ( part#8 6709090 ) for 26-27 gauge sy ringe needl e s. T he extended s nout on the septum nu t helps guide the syringe need le stra igllt o nto the colu mn. 3) The wid e-bore capilla ry co lumn adapter ( pa rt#8690- 90 93 ) whdl a ligns the syring e needle and the column Insid e the on-column injector bod y. 4 ) Th e injector body titti ng ( pa rt#867Q9094 ). T his is a stainless steel swagelok typ e titting modifJed INith the addition o f a earner ga s inlet tube which is welded into the side .
5) A 1 /a ~ to 0.8 mm graphite red uc ing fer rule se cu res the wide- bore ( .53m m ) ca pilla ry column into the injector body frtting. Either so ft o r hard graphite ferrules may be us ed with capi llary co lumns. 6) A 1/8 " swag elok type nut ( sta inless or brass) is used to compress the graphite ferru le a round the co lumn . Stai nless is recommended for oven temperatures above 2 000C. 7) A wide- bore capillary col um n ( .53 m m i,d. ) of an y length . The on-column injector is normally used with woe-bore capilla ry o r 118- packed col um ns . not with columns whose insid e diameter is les s than .ssmm since mat IS tne smallest 0 1ameter into whic h a standard 26 gaug e syrmqe wi ll fit.
As srcwn above , the 26 gauge need le on the standard 10 ul GC syringe fits perfectly into the bo re of
Manl f Zpub
48 (of 550 ) 2006(-2016)
49
:.,:... ...:.. i ,"_ .. .
.. '-.,_ ';'-
,
To install the column in the injector: 1) Feed the column end through the 1/8 swagelok type n ut and graphite red ucing ferrule , If the ferrule has been previously used , inspect it carefully to make sure it is sM Intact Sometimes used ferrules will break inSide the nut and a part of the ferrule will fall ou t What's left inside the nut may not seal correctly. Try to avoid shaving bits of graphite from the ferrule into the bore of the colu m n as th is can cause peak tadlng and absorption.
-i ;::;_l.i
2) Push the column all the way through the injector fitting and out the front Then slip the wee-cere adapter over the end of the colu m n. Be sure that the conical end of the adapter is fa ci ng out towards the operator. The gash in the adapter allows carrier gas to enter the co lum n even if the end of the adapter is plugged off. 3) If you are uSing a metal capillary as shown in the photo . use a sharp file m ake a score ma rk an inch or two from the end of the column. Holding your thum bnail under the score mark , snap the column end off 10 make a cl ean break . If you are using a polyim ide coated fused silica ca pil lary column, a razor or sharp k nife edge is used to make the score ma rie The end of the col umn is removed to ensu re that no graphite particle s or other debris which may have entered th e column bore during the install atio n process rem ain s in the column .
HINT. Some chro matographers use a small reamer ( Dremel tool bit ) to clean up and smooth the end of the metal capjflary column bore hole. The smoother hole aflows the syring e to enter the colum n with less chance of snagging on the lip of the column. The syringe itseff should be III good colldition with no butTS or kinks. SRI supplies a syringe wi th a con ical needle tip ( part#86 7G-9550 ) In your choice of 5. 6, or 7 em needle lengths
As shown above, a sharp lr iangle file is used to score the m etal cap illary column a few inches from the end which may have p icked up graphi te or other debris during the installatio n process.
Manll j.pub
49 (of 550 ) 2006(-2016)
50
4) Pull the column and wide-bore adapter back into the injector fitting through the partially tightened nut and graphite ferthe column will gradurule. As you ally disappea r from view inside the injector fitting, Pull the column until the open end is about halfway Into the fitting. The exact distance is not Clitical so loog as the syringe needle ends up depositing the liquid samp le in the bore of the column itself. If the column is pulled too far towards the oven, the syringe needle may deposit the sample in the adapter where it w ill gradually diffu se into the column caus ing wide or tailing peaks. If the column is positioned too tar out towards the opera tor, the syringe needle may snag on the lip of the column as it is inserted.
pun.
W ith the column positioned. tighten the nut and graphite ferrule. You should feel the ferru le squish slightly as you tighten the ferru le. and the column should feel snug and immov able. A property lightened ferrule can be re-used 5-10 times, wture a ferru le which is over-tightened mus t be replaced every time the column is cha nged. NOTE: Metal cap illary columns are easier to install than polyimide coa ted fused SIlica columns because as the syringe enters the column entrance it can ch;p away bits of the fused sifk;.a unless it is perfecL'y per smoned The metal columns are more forgiving since the COlumn will not fracture when in contact with the syringe needle.
A
7/16~
wren ch is used to snug up the nut and graphite ferrule sec uring the column to the injec tor.
Manl 14.p ub
50 (of 550 ) 2006(-2016)
51
Chapter; Injectors "
,-" ,
-
,-."",;",
Topic: " ' :~ On:coiumn Injector Operatiori ·,,
5) Tighten the septum nut until it conta cts the one or two ru bber o-ring s on the injector body. The a- rings act as a helpfu l guide to avoid over-tiqhter nnq the septum . When the soft silico ne rubber of the septum is over-compressed , the syringe has to fight its way through often plugging with septum material in the process. A properly tightened septum cleaves easi ly to let the syringe need le pass, the n self-heals itself when the syringe is withdrawn. Properly tigh tened, a plug type septum as us ed on the SR I GC will las! u p to 300 injections, wh ile an over-tightened one will leak after 10-20 injections.
The photo above shows tile injector fitting w ith two a-ring s ins talled on it, and the septum nut tightene d up so it just con tacts the a-rings, If the syringe snags on tile edge of the colum n as it is ins erted, loosen the swagelok nut and ferrul e an d p ull the col umn anothe r few millim eters further towards the inside of the colum n oven. Tighten the nut and retest by inserting tne sy ringe .
Test you r installation by inse rting a s yring e int o the co lumn as far as it will go. The syringe should glide into the column bore smoothly w itho ut snagging or feeli ng rough.
Man l 15.puh
51 (of 550 ) 2006(-2016)
52
(
Chapter:
INJECTORS AND GAS VALYES
Topic:
INJEcnON PORT
Location of ~jcctioo port in typical FID system
Septa nut with needle guide 26 gao needle
SRI model 8610 injection port assembly
Black rubber O-rings (2)
~ I [D Silicone 'SEPTA"*
CRSl23n40 Beveled
Side-port
R_
Syringe ncedJc tip styles
~J
The 8610 gas chromatograph is shipped equipped with a direct injection-type injection port, This port permits on-column manual injections with traditional chromatography syringes. The injection port is simple and highly efficient by design. Swagelok stainless steel hardware is used in the assembly of the injection port. Injection of gas and liquid samples is performed using standard syringes equipped with a 26 gao needle. Beveled (medical-style), straight, and hooked tips are available from many suppliers in this needle size. For larger needles, such as a side-port, blunt-tipped needle, a liS- Swagelok stainless steel nut is used in place of the supplied septa nul Although several needle tips are available. booked-tip oeedles promote septa life by slicing through the septa without "coring" the silicone, as do medical and straight-tipped needles. liS- bulkhead 0.53mm capillary fitting column adapter
I
/
liS- to O.Smm graphite ferrule
liSnut
O.53mm. a
I ===< ~~=
Connection of O.53mm. fused silica column to injection port
VeIII: DOlch CUI inle oolumn
~
liS- 5.S. fronl!back ferrul es
1/S~
~
0 085- S S ~umn "
I
i
CODOeCtioo oeO.OSS- I.D. stainless steel packed co/umn to injection port
ther
Therefore, are recommended. "Coring" punches shards of septum into the injection port and may result in pluggmg of the syringe needle and failure to deliver sample. Over an extended period of time, these shards could migrate into the column. In a packed column, this accumulation of septum shards increases the exposed surface of silicone available to produce silicone or septa bleed. In a capillary column, these shards could plug the column completely. Routine maintenance of the septum prevents this from occuring. A bad septum may bleed excessively or pemtit carrier gas to leak out of the system, affecting retention times. It may visibly bulge or show numerous slices or shards of silicone protuding in toward the injection port. This usually occurs when the septum nut has been over-tightened and the physical characteristics of the septum have been altered due to compression of the silicone. If a septum is extremely bad. the user might see a puff of smoke blowout from the injection port after injection. This is the volatized sample blowing back out through the leak. on a continuous stream of carrier gas. Septa may become tacky and unusable after extended service. The septa. nut should be finger-tight. Once the user feels the septum seat snugly against the bulkhead fitting. the septa nut has been tightened sufficiently. Use the two black rubber O-rings on the injection port as a guide - the nut should barely make contact with the outer O-ring when the nut is properly tightened. NEVER use a wrench to tighten the septa nut. An over-tightened septum will have a markedly decreased lifetime. Larger side-delivery needles also tend to reduce septa life due to the size of the puncture created during injection. This requires more frequent servicing of the septum. Please note that when septum replacement is required during use of the thermal conductivity detector (TeO), the filament current should be turned off at the electrometer located on the right side control panel of the chromatograph, prior to removing the septa nut. Failure to do so could result in the desttuetion of the detector filaments due to lack of carrier gas flow through the column and into the detector. It
C :\EPl\DOCS\ INJPOO! .EPD
It
REV. 06-24-92
52 (of 550 ) 2006(-2016)
53
Chapter:
INJECroRS AND GAS VALVES
Topic:
Manual Direct Injection Technique
A dow injectioo will result in broad,
tailing peW "'"' ~y ccehse.
When perfonning analyses using manual direct injection, the method or technique used to prepare the syringe and perform the injection can mean the difference between obtaining chromatograms that are either poorly resolved or clean and sharp. Reproducibility can also be affected if the amount injected varies from injection to injection. This is why it is imperative that a consistent. reproducible method or technique of manual injection be used when performing direct injection.
A quick. properly
performed iIljectiOIl will result in sharper peaks,
r®
--....-
t@ ,
Ru- the
lhurougbJy ill 0 - , ....,..I::ing lbc plllllgCl'. lbco dmtl' ~Ic in,
_. J.. ...
microliter
vial, and
cje<:1
""""
needle, an;!
tina
10
prime
syri._
....
lb~
Orawoi>o 0(
orvial wipe
-e--,
Ioedcd. illllCn
•
~-"
"""'-"
""'" ...
syrillfC i5
air irto
""
I
~
microliler ut :s&a:;llc
"'" ... "" ~'" ""'"
lbc.....ae ;me:> \be inja;tion port quic;.Idy. .....".
,-, .......
-_ .
irmD:diueIy.
.....d.., """""
_.....
le
1>.. 2
Properly prepared. the syringe needle is inserted completely into the injection port in one smooth, quick motion. Then the plunger is driven borne immediately. As soon as the plunger tip hits the end of the sample chamber, the syringe needle is withdrawn from the injection port in a quick, smooth motion. This will prevent any sample remaining in the needle from having time to vaporize into the injection port before or during withdrawal (if this were allowed to occur, it would result in peak broadening and tailing). You may currently be using a different technique for direct injection. As long as the method being used is consistent and reproducible, you will obtain reliable. consistent
rep roducibility from your direct injection analyses of gases and/or liquids. O:\fl'200CS\IN1I'ECHI .EPD
REV. 05-17-94
53 (of 550 ) 2006(-2016)
54
Chapter:
lNJECfOR & GAS YAL YES
Topic:
SRI Septa Overview
In order to place a sample into the column of a gas
chromatograph without de-pressurizing the injection port and column or interrupting the carrier gas flow. some type of penetrable, resealable membrane must be used. Tbe membrane must be penetrable to permit the introduction of the syringe needle into the injection port, but must also have the ability to re-seal itself. If it could not re -seal itself, each injection would leave a leak that would permit carrier gas to escape from the system. Each subsequent injection would worsen the condition, adversely affecting retention times and sensitivity. Silicone rubber is commonly used to produce injection port septa. Silicone, due to its formulation, is soft yet maintains the ability to seal puncture wounds created by syringe needles. Although septa differ in formulation, proper care will prolong the life of any septum, A silicooe septa (CRS 800-327-3800, pan number 23TI40) is installed in all SRI inj ection ports when shipped. This septum is very soft and rescalable. It demonstrates low silicone bleed and does not affect sample co mponent elution times. Additionally, this septum exhibits
negligible "coring" for better durability and performance. This septum seals well in the tapered interior of the 118" modified Swagelok injection port.. 10e example at right illustrates the difference in
Side view
Front View Sepwm with added coating
Mokled septum used by SRI
Side view
Front view
physical appearance between this septum and the standard cut septa machine-stamped fro m silicone sheets. Coated septa are manufactured this way. The coating is intended to reduce septum bleed and increase
reseaIability. All septa are made of silicone rubber that contains polymerized silicone gums. A catalyst is used to obtain the polymerization that produces the elasticity sought from the septum material. Unfortunately, some silicone oils remain unpolymerized in the septum and freely diffuse out of the silicone septum. These oils vaporize into the injection port and are known as septa bleed. Some manufacturers insert additional oils, making the septa softer and easier to remove from their molds. This increase s the amount of septa bleed in those pieces. M ost low bleed septa are manufactured by extending the duration of polymerization , resulting in a harder silico ne with less bleed. The septa used by SRI exhibit extremely low bleed while remaining soft and highly resealable.
When silicone oils bleed into the column over time, the efficiency and performance of the column is degraded. Columns with a silicone liquid phase, such as OY·l or SE-30 types, will not display the effects of septa bleed as readily as would a phase such as Carbowax 20M, which would be adversely affected by the effects of silicone bleed. In other columns, the condition may go unnoticed initially. especially during isothermal operation until the development of a high unsteady baseline occurs, accompanied in some instances by increased noise. When the column temperature is ramped as occurs during temperature-programmed operations, the silicone oils begin to elute as they are heated to their respective boiling points. These silicone components will elute through several runs, producing spurious peaks with often reproducible retention times. This can influence componen t identification and measurement negatively. In some work, where sensitivity is not great, septa bleed is not a concern. To identify septa bleed, especially where temperature programming is employed. cool the uni t to ambient temperature and hold for ten to fifteen minutes. Then ramp the temperature up to the maximum running temperature normally used, with the sensitivity set to high. Any peaks or baseline drift can be attributed to septa bleed. One method to minimize bleed is that of baking septa in an oven prior to insertion into the injection port in order to volatize the silicone oils. The septa may also be baked in the injection port overnight, as long as the column oven is maintained at the same temperature as the injection port to avoid the accumulation of bleed products. Regardless of septum type, septa should never be handled except with tools. Finger oils may appear on chromatograms as additional peaks. C:\EnlOOCS'-SEPTAJ"Gl. EPl)
54 (of 550 ) 2006(-2016)
55
Chapter: "Injectors
';'
-
-.
-;.'
Topit; ·"_" •.Heilited Splitl~plit less Injector "· . " -""':. '; " ,'~"-::', .:;
i?,~,!- '~;'::L""'-'£-i ;'
,;"~;
- ,,'; '.; "":
The Heated SphVSpJitless Injector can be
mountedonthe8610C or3 10GC.lt is shown in stalled on the 8610C GC at rig ht.
When mounted on the 8610C GC Chassis. the precision needle valve wh ich adj usts the split flow rate IS mounted In th e heated valve oven alongs ide the column oven . The split flow is adjusted by rotating this knob.
The lid on the valve oven has bee n removed to expose the SplitlSplitless hardware wh ich is installed in the valve oven .
Septum nut mounted on front of Sp lil/Sp litless Injector.
The plumb ing schem atic shown at left illustrates the hardware comprising the Heated Sp litlSphtless Injecto r
Manl 16.pub
55 (of 550 ) 2006(-2016)
56
T he Heated SplitiSplitless Injector parts are shown at left removed from the GC for clarity. 1) Injector purge restrictor. A few m Vmin of canier gas continuously exit the inj ector through this restrictor tubing to prevent high boiling point anelytes from diffusing back. into the injector.
~~'§1~2) Precision needle valve for adjustment of split flow rate. 3) Spill flow solenoid turns split on/off under control of the PeakSimple data system . 4) Column is secu red Into injector using nut and graphite ferrule. 5) Aluminum heater block conta ins heate r cartridge and Type K thermocoup le
The injector liner is strewn at light removed from the aluminum heater block for clarity.
1) Carner gas inlet tubing .
2)
Septum nut and septum.
3) SRI sta inless steel injector liner.
4) End fittin g where col umn co nnccts and $plit flow px ik to (lurg '"
vent and need le valve
Man l1 7.pub
56 (of 550 ) 2006(-2016)
57
A variety of injector liners can be used with the Split! SplitJess inject or depending on the colu mn and application.
SRI stainless liner with wide-bore COlumn adapter.
Supelco glass liner
SRI designed the SplitJSplitless injector to use the same size liner as HewlettPackard 5890/6890 ser ies GCs. A hu ge variety and se lection of suita ble injector jner types can be purch ased from chromatography catalogs . such as AJltech . Restek. Supe lco and others. The liner supplied with the SRI GC is an unbreakab le stainless steel type which also adapts for
on-column injection onto w ide-bo re capil-
Iary co lumns ,
The SRI stain less steel in-
jector liner supplied w ith the GC as standard equ ipment is shown at right with the
wide-we column adapter slipped ove r the colu mn in preparation for final adjust ment fo r on-co lum n injection ( see on-col umn injector Instructio ns ). Wid e-bore column
( .53mm ) adapter identical to that used In on -column injector fits perlectly into recess in sta inless steel injector liner.
Manl 18.pub
57 (of 550 ) 2006(-2016)
58
To rem ove the inj ect or liner from the SplitlSplitiess injector:
1) l oosen the brass trurmbscrew holding the 1116" stainless union in the carrier gas supply line .
2 ) Using two 114" wren ches. loosen the nut and ferrule on the down stre am side of the union and discon nect the tUbing leading to the injector.
3) Using a 7/ 16" and 112" w rench, loosen the nut and grapl"ute ferr ule securing the co lumn to the oven side of the injector.
Man l19 .pub
58 (of 550 ) 2006(-2016)
59
Chapter; ~ lnIectOr5 ..
..
.
t~~Ji~~~f!~~~Jgl~,iif~~I2~~~4tf~f,r"i~~~ .;~ )~:; ~ To rem ove the injector liner from th e SplitiSp littess
injector:
4) Using a 112" and 9/16- wrench remove the swage lok type nut securing the end fitti ng .
5) The end fitting is shown here removed fro m the GC for clarity. Notice the hard 1/4" hard gra phite ( m ixture of graphite and vesper ) fe rrule on this end o f the liner. If you are using a glass liner instea d of
stainless, a soft graphite ( 100% gra phite ) ferrule may be a better choice. A graph ite ferrule is used on this end of the liner so the nut can slide off the line r.
6) The injector liner and carrier inlet fitting can then be removed from the GC by pullrng stra ight out towards the ope rator.
Man I20_pub
59 (of 550 ) 2006(-2016)
60
Chapter:
,;-: '.=-- .
Inj~ctors ..
-, -
To replace the injection liner:
7) USing a 112" and 9/16- wre nch remove the swagelok type nut securing the end fitting The stain less stee l liner provided as standard equipment WIth the spliVsplit less injector uses a brass ferr ule on the septum end of the liner, but if you replace the stainles s liner With a g las s line r, you wi ll need to use a 1/4" soft graphite ferru le instead .
Align the flat surfaces of the nut and fitting
8) The glass liner and end fitting is shown here partially inserted into the heater block and rem oved from the GC for clanty. Be sure to align tile flats on the nut and the frtting so that the carrier gas Inlet tube will adopt the same onentaton once me IlOe f is funy inserted Into the heater block .
9) The injector liner and ca rrier inlet fitti ng can then be insta lled into the GC by sliding straight in towards the co lum n oven
Man l2 J.pub
60 (of 550 ) 2006(-2016)
61
chapter: ',InjectorS ": ,,:' "- ~. ~7-O::-·"::
_.
.~-
..
;\'- ' . :_~;;.~ ::-~~::.~ :.~
:r<5Pic:~ -~~ :i:;feat~"SPtitJsplittes~ Injector .
'-E.::- ,.
=_.. :-:. -":~.~; ~_ "':'..:- ~ .';,.._..:~: ;- .:~-:-:"' ~ -' -:-':'f' ....;.......
To install a narrow bore (.25mm ) capillary column :
10) Use some wh ite correction fluid to mark the column ap proximately 1.5" ( 4cm ) from the end . Slip a 118- swagelok type nut and 1 /8~ to .5mm graphite redu cing ferrule over the colu mn . You can use soft Of hard graphite ferru les .
11) Using a 7/16" and 112: wrench secure the col umn into the injection liner so that the white ma rk on the co lumn is ju st visible . The intent is to pos ition the end of the co lumn upstream of the split vent exit tu be which rs we lded into the side of the end fittin g.
12) Adjust the sp lit flow rate using the needle valve
loca ted on the front of the valve oven .
I ~
./iiia
Ma n l 22.pu h
61 (of 550 ) 2006(-2016)
62
Chapter;-lnjeCtors..· '.-" , , ... .' ., :, : ~.
> ,. ~-, > .
'-:'~:\:
+~PtC~·.~i~·~ '~~led:~p;lttSPlitleS~.lnjector ,:;';Ui<
, ;;i~~ '2~;j~i, cr" ::, ~~ ;~'f::" '·'G;,:;,;~=?':~n.;r'; '±:n:i:.
':;~i!; ;:
To install a narrow bore (.25mm ) capillary column :
- ..
--i :j§:0 . ............... I
13) The spli t ve nt must be opened by activating one
-.;..;.
of the relay outputs from the PeakSimple data sys-
,
~:i~
!
tem . Typically Re lay A is use d to act ivate the split vent solenoid. If an other relay has been allocated to this func tion , it will be annotated in the rela y assignment chart located on the rig ht hand side pane l of the GC . Rela y A can be turned onloff by d isplaying the relay w indow and then usi ng the mouse 10 click on the letter A.
_--
.....
.-..... ,,:i., ,"-f '-,:~ ''' ~: '' ;-;';
~,: ':J$ti-:;:j'f'og",,; .,~
14) The relay can be tumed on/off automatically during an analysis by entering the relay commands in the PeakSimpJe event tab le.
~ . ,-,
,
15) Carrier gas will only ex it the sp lit vent when Relay A is activated. Connect your bubble-meter or other flow measuring device to the spli t vent exit tube , Activate Re lay A. Make sure the red lid of the GC is down ( lid interlock disables solenoid fu nction ). Adjust the needle va lve to obtain desired flow .
Manl 23.pub
62 (of 550 ) 2006(-2016)
63
INJECTORS PTV - Programmed Temperature Vaporization Injector
Overview
..
Injector body
,•
Standard SplrtfSplitless capillary adapter & liner •
~ ~ _ ·~ ··h
=40. 44
,_ ..
~~_
. .<.
The Programmed Temperature Vaporization (PTV) injector is composedof the same parts as the Heated Split/S p lit lcss injector: the injector body. a SilcoSleeve'> liner. an injector purge restrictor, a precision needle valve for adjustment of split flow rate, a split flow solenoid that turns on & off from
the PeakSimple datasystem.and an alumi numheater
Sucosleeve' .. liner paCKed witt! adsorbent
block containing a heat er cartridg e and Type K thermocouple. Contrasted with the Spl it/Spli tless injector, the PIT inj ector has a removable insulating. PTV and SplitlSplitless Injector components slee ve, a large r (250 watts) heater cartridge wi th ballistic heating capab ility, and carrier flow ON/OFF control. The Si lco'Slccvc'v lincr can be packed with a variety of optional adsorbents, depending on the applicatio n. The SR[ PTV injector has three modes o f operation: 1) large volume liquid injector. 2) an offline thermal desorbcr, or 3) an online thermal desorber in conjunction wi th a gas sampling valve.
Aluminum heater block Column Ovenwa ll Tubing to gas sampling valve
Septum nut and septum
•
Front of vafve Oven and Column Oven - top view ._
Tenax-GRTU pecked $ ilcoSleeve lll liner. partially slid out for VISibility
1-;::'1 ~~
..t
-. .
~
Split flow ex its to purge
vent and needle valve
!
I
."'"
Sample loop inlet (top) and purge vent (bottom)
Needle valve precision control
63 (of 550 ) 2006(-2016)
64
INJECTORS PTV - Programmed Temperature Vaporization Injecto r
Theory of Operation The Programmed Temperature Vaporizat ion injector is basically a Heated Split/Splitless injector with the abi lity to rapidly heat to 3 00~C. This ballistic heating capability enables large volume liqu id sample injections. The PTV injector can be used us a thermal desorber for volatiles and semi-volatiles, online or a mi ne. Multiple liners with different adsorbent packings may be in terchanged in the SRI PTV injector. The adsorbent used depends on the compoun ds of' interest, as each has its own selective retention
properties. 1) Large Volume Liq uid Inject or
Largevolume injections allow analysis ofsamples withIowconcentrarionoftargeearatytes. Liquid samples from I ul, to 200j..lL may be injected using the SRl PTV injector. A. To begin.hoth the Colwnn Oven and the PTV injectorure held at 40-60"C. Prior to injection. the split vent is opened. Thus. the large volume liquid samp le is inject ed into the Pl V inj ector at 4O-6QOC with the split wide open. Introducing the sample at a low tempe rature allows the solvent to vent while the inj ector liner packing retains higherboilingpoint analytcs.
A
.
B. The split vent is then turned OFF, the PTV inj ector is ramped to 2()()" 3OCY'C. and the carrier flow
~
~----- To oc lumr.
I V
Glass
~lO o l
~ nie eto ~
Purge
p:.rrse
,~
ex it
transfers the an alyt cs omo o~
thecolumn, which is still cool at this po in t. The coo l column tempera ture
.l.--...J
Ii
W
--... '
Pre cision ne edle veve
promotes condensation and
h
Spll: vent
U~ "" )
Split tlew !:lOi,:!!'rIOJd (Re ia y -A- O N)
focusing ofthe analytes and
helps prevent smearing and excessive tailing. Each of these ev'ents is automatically contro lled t hro ug h th e
B S.m=:> . "
PeakSimple da ta system, so
ope rato rs can pr eci se ly control their tim ing. The
operator sets [he PTV
inje c tor
~;;TI''lax-G'< --: ~J.:- ~
;:O ~
Glass wee!
inj e cto r te m pera ture by adjusting with a screwdriver the appropriately labelled serpoint on the GCs front
panel.
car"," ~
rP1 r-t ---:'1
LJ ~
,
)
L
~:~~~
]"jeetor Purge..j... ,---. Purge restn'eto'. .. te a -"' ~ .....:;.. ;xJrw:e ~
h
;:>:'e~ sior:
Sa mple '
nee dle ve've
;-;;:=='U -
Spl it now soie noic
ex it
Sp " ve nt
eKit
(R;;.:ay ";.." OFF)
64 (of 550 ) 2006(-2016)
65
INJECTORS PTV - Programmed Temperature Vaporization Inj ector
.-.~.
Theory of Operation continued 2) Offline Thermal Desorber For oflline thermal desorption. the Silcoxleeve liner packed with adsorbent such as Tenex-Gk'" is loaded with sample outside of and separate from the GC. Althoughthe best analys is isobtained from a fresh sample, theendsofthc liner may be plugged after loadin g sample w ith rubbe-r septa or capped with rubber end caps for storage or transportation. Tum offthe flow before removing the inject or liner by ac tivating relay B, which stops the carrier gas flow. Leave the EPC flow offunril the beginningof the analytical run (see the event table at right). To replace theliner, unscrew the septum nut and septum protruding from the frontofthe Column Oven wall. Remove the rubber septaor caps from the liner and slide it in Yo.ith the gash to....ani the operator. Replace and closetheseptumand nut. 'With the carrie-flow still turned OFF. start the run. Wh en the PTV inject or reaches tem pe rature, the carrier flow is tumed ON and the analytcs arc swept onto the
",,-
Uner plugged with rub ber septums for storage or tra nsport
ett"§}
><,
=-
Example PTV as offline thermal dese rter event table
~ ~
_ I - :-1 ---c:.. ~I
~j
""
~ f ~I
~
I
column. 3) Online Therma l Desorber For -online lh..-rmaldesorpticn. the ?TV canbe plumbed with agassamplingvalve. In this mode ofoperation, the PTVfunctions
LOAD
as a sample loo p. trapping and conc entrating compounds for
~;"
analysis.
;p-'~~Co'"n"
LOA D Position: (Relay "G " OFF)
When the gas sampling valve is in LOAf) position. the PIT injector can be loaded wi th sample through the sample inlet and
Sa"'l)le
-~
In
Sample
r=+"'"_
outlet. The P'IV injector is at 40-60"C. Anelytcs arctrapped in the injector's liner packing.
INJE CT Position. (Relay "G" ON )
INJECT
~ A)
Inthe INJEC r position. thefrv injector ramps 10 300"C.
."
vap orizing the sample. Th e carrie r gas flow then flushes the desorbcd components onto the columrus). The valve should he rotated back to the LOAD position after the components are transferred to the column to avoid smearing and peak tailing.
y
cur~~
~CO I"m" s _~
I,
S a mple
o,
65 (of 550 ) 2006(-2016)
66
INJ ECTORS PTV - Programmed Temperature Vaporization Injector
General Operating Procedure Large Volume Liquid Injection Steps I. The split vent must be opened manual ly prior to the run by activating one of the relay outputs from the PeakSimpJe data system. Relay A is typically used to activate the splitvent solenoid. If anotherrelay has been allocated to thisfunction. it \...'ill he noted in the relayassignment chartlocatedon the right hand side panel ofthe Gc. Enterthe desired relay commands in the Peakximple Events table. The split vent can also be turned ON (or OFF)by opening the relay windov....then clicking on the letter A. -- 1. 1
t- I:W , .... ;: $--
- -_.
. . !~ ! _ -- . -.
. . .. , - ,
-. -.
-
- ~-
I
-
.-
""' ", no
•
-;
-.0""
.. .. -_._ ~
..,
•
........... ....,7'"
, ""' ..."',
•
••
-
~I
~'o:l
'' eF:~~"=1 '''' ~'I.C/Io·QI< ''''''1
~"'"
' ''''' P''''I'I''~"q.,.''''.v1I
1211:
~ ""'r.o·_1
•
'-~
fii -
Open the Relay window in PeakSimple by clicking on the Yiew c rop-down menu and choo sing Relay/pump ~ndOw
il~
-- ;;z ! "p;,;:.;,;. r -~- r
-- ~
l
-.. J
__ J
~
~
:::::E:J
... "'"
~
Example PeakSimp le PlY event table
3. Carrier gas exits the split vent only when Relay A is activated. Connecratlowmeasuring de\'lcc to thcsplit vent exit tube. Lower -the GC lid (when open. lid interlock disables the solenoid function), activate Relay A, and adjusttheneedle valve to the desired flow. For most liquid injections using a PTV, the sp lit vent should be wide open. This allowsthe trapping material to retainthe compoundsofintcrcst and quicklyflush the solvent to vent If the split ratio is set too low, some of the solvent and analytes may enter the column befbre the PTY injecto r is hC3tOO up, resulting in smeared or double peaks.
2. Type in an e\ en t program as [0110\V5: Tun: 0.00 3.00
Event ZERO A OFF (split vent closed; if you get too large a solvent peak, keep the split vent open
longer) 3.10 B O~ ( carri e r O FF) 3.20 C OK (PTV inj ect o r h eat) 5.0 0
IJ OFF (carri cr O~)
4. Injec t 1ul, to 200,u L of liq uid sample into the: PTV injector. In the "Expected Performance" example. 1OOIlLof C1O-C28 hydrocarbon mixture was injected. 5. Hit the RUN button on your GC or press the spacebar on your computer keyboard.
66 (of 550 ) 2006(-2016)
67
INJ ECTORS PTV • Programmed Temperature Vaporizati on Injector Expected P erformance The followingthreechromarograrns are from the FID ina SRI GC wi th a PTV injector upgrade. The liner
was packed with 0.1 grams ofTena.x·GRP.-t adsorbent All three 25 minuteruns utilizedthesame temperature andevent programs. Inthe first one, a IJlL 2000ppm C 10-e2~ sample ""'3.<> injected through thePTV injector. In thesecondchromatogram. the samesamplewas diluted. I:100, then 1DOp.l injected. achieving results consistent with the first run. and demonstrating the high volume liquid injection capability of
the PTV inj ector. In the third chromatogram. IOOIlL ofmethanol was injected. asa blank, resulting ina small hump between the 4 and 7 minute marks and miniscu le peaks which correspond to
f 'tt i f
, fiIo
~
0.866
84953.1370
C1Q
5.366
5299,9150
e12
7.300
5034(l960
C14 C 16 e1 8
10.233 12,450 14 2 16
48 14.21XXJ 4&X1.C300 4436.1180
C20
15.750 17,150 18.483 20.033
4528 2890 4570.0975 4778.9380 4863.4290
222 16 10'.a!
4135,4760 132013.7875
~
J
!
!
I
0'
i
- -
j
••
~
~
- =.
SoIYer:1 CI O
5.433
2258 5340
7. 366
26 140640 38138985
C 12 C 14
O. ~
C20
10 266 12 <183 14.266 1~ sec
3924.8340 3939 .9080 3933.0400
C22
17200
4660.5ll6O
C24 C26
18516 20.083
C28
22,256
473 7.3130 4174.2920 32ti0 1120
C16 C 18
Total
536 789.4<1 :1:'
'" =
" "'"
.
,
•
"e,
H
~
~
!!J
~
~
/,i
. 0
i,~. ~Q
-
lEa
•
499472.8740
'"
.
2
~
'"
J 0
C9 C poce;!!
"''''
rr .I!:EED
.1. =-
Chromatogra m 2 Resu lts :
i
I elf
-
!'I
f
,
!
!
I
j
I'
,
i!!0 1
liP"
......~ _, -
,. ~
... :;'-"Od ...... r
""~
I
3
Tempera ture p.-ograms & events fo r all 3 runs: E..-en'.s : (A '" sclit rerrl) T~ PTV ~
11O"C (3m;nllo 27 5'C
Temperatu re program Inititl /-IoI::j ~
11 O"C 27O'C
700 2(jJX
15.:>0 000
0 00
E."'" 2ERO
3.00
AOF'
3,10
B ON C ON
3.20 5.00
i
!-
- -
JA-
B OFF
.E"!Y!
27lJ'C 27lJ'C
,
,",,'
~
1
~
Retention
Solverrt
C26
_._10 14 _
. . -:.7'~~e~ ..-."... . _t""'"
Chromatogram 1 Results: Com ponem
C24 C26
"""""
.::r;t; g llll l
contaminants in the methanol blank and bleed fromthe Tenax-Gk? '.
en
I
_
-:!=t"""
iF
-
I
I
-
-
I J I
•
I
I
'*! 67 (of 550 ) 2006(-2016)
68
Chapter:
INJECfORS & GAS VALVES
Topic :
SplitiS plitless Injector
CONVERTING TO COLD ON-COLUMN MODE: To set up the unit into a cold on-column mode, rai se the red lid and adjust the injector temperature setpcint to 20° C. This will ensure that the injector does not heat itself but will be at the oven temperature. Thi s temperature setpoint can be displayed on the digital display by turning the readout selector switch to INJECTOR SET. When the injector and oven are cool, remove the oven lid. Remove the injector nut and 9.5mm septum (All teeh # 15428). Use a 7/16 inch wrench to loosen the nut that secures the column in place while holding the split vent fitting with a 1/2 inch Mench. Slide the column all the way through the injector until it is protruding out the front of the injector. Remove the 0.53mm J.D. capillary column adaptor from the holder in the oven lid and slip the column through the adaptor. Insert the 0.53mm I.D. capillary column adaptor all the way into the injector sleeve. The colu mn should be inserted midway into the adapter. The adapter is then inserted into the injector so that the "funneled" end of the adaptor facing the needle is near the septum. The adaptor is vented so that carrier gas will flow to the column even if the adaptor is installed against the septum. This end toward
Tighten the nut to secure the column in place while holding the split vent fitting with a 1/2 inch wrench. Replace the injector nut and 9.5mm septum making it finge r tight. Use the toggle switch to select the flow controller to regulate carrier gas. ~
COLD ON-COLUMN OPERATION: The GC is shipped configured in a cold on-column mode. This mode is the simplest to operate. The heated injector temperature setpoint is set to 20 degrees C. 'The flow controller is used to regulate the flow of carrier gas. A packed column can be directly connected to the back of the injector by removing the so lvent expansion chamber. H a 0.53mm capillary column is used. it will be mounted in a capillary column adaptor (part # 867(),,9095) which will allow direct injections onto the column. The adaptor is stored in a special holder in the back right corner of the red lid when not in use.
Unlike the split methods where much of the sample is lost, a cold on-column injection places all of the sample directly onto the column, therfore no sample is lost. Cold on-co lumn injection method is idea l for samples of low concentration and gives the best sensitivity and sharpest peaks. The split vent is never opened for the cold on-column method.
CORRECf PLACEMENT OF COLUMN AND CAPILLARY ADAPrOR FOR COW ON-COLUMN MODE:
C:\EP2\DOC$\ S P'U'T1N04.EPD
REV. 08-17-9ol
68 (of 550 ) 2006(-2016)
69
Chapter:
lNJbCJ'ORS AND GAS VAL VES
Topic:
Near -Ambient Tempera ture Sep tum Nut Assembly For Heated Injectors
All SRl Instruments heated injection ports are equipped with a specially-designed septum nul which dissipates any heat that could be tran sfered from the heated injection port body (including split-splitless configurations), to the septum nut and septum by contact. Experience indicate s thai when injection ports are permitted to tran sfer hea t to the silicone septum, that septum bleed can and does occur. Septum bleed is the volatization under heat of silicone oils used in the manu facture and formu lation of today's high-performance, resealing silicone septa. Column oven ....all (86 IOC)
Insu lated inject ion port liner bear ing a sse mbly
ij~1I13~~~I~IIIIIIIIII~~~(~~
temperature se ptum ___ n ut assembly Spec ial near-ambient
':i
.I .,
Silicone bleed produces numerous interference peaks in chromatogra ms when the septum exce eds lSO"C and oil vapors are swept into the column and quantitated. This situation is undesirea blc and easily avoided when the special septum nut is used.
View of fully-assembled heal ed injection port
"<,
Split vent (on split'splitJess
mjec tor -equipped models )
G lass injection port !mer (user-supplred)
Special capillary col wnn ada pte r for on-co lumn injectioo
H eatsun k septum nut
extension
Exploded view of disassembled
Capillary analytical co lumn
heat ed injection port assem bly and special septum nut hardwa re
Not e the position of the an.tlyticill coluuw
within the capilla ry column adapt er and its posit ion with re lation to the septum an d injt'CtClr liner
Only th e injecti on port hardw are ""';thiD the column oven is heated direc tly
/ "-
The special septum nut asse mbly illustrated abo ve keeps the septum at an adequate CUt-away VIew of assembled heated inj ~oo port assembly distance from the heated injector assembly to maintain the septum at or near ambient temperature with the assistance of the additional mass of the septum nut extension. This prevents any silicone oils prese nt in the septum from volatizing and being earned into the column . This feature may be retrofitted onto earlier versions of the SRI GC heated injectio n port, as onJy two new parts are required. The following page contains chromatographs that illustrate the effect of this new injector design D: W~Ef'DOCS\A,..tBSEPrI. EPD
REV . 05-QS-9'7
69 (of 550 ) 2006(-2016)
70
,(
i
"'I
Chapter:
INJECTOR S
Topic :
THERMA L DESORBER OPERATION
T he SRJ T herma l Su il Desorber accessory is useful for the analvsis ofvolatile and especially semi -volatile co mpounds in soi l or ot her granular so lids . Because the analyte can be ext racted fr om the soi l by heat alone. with little or no sample preparation. field analyses can be performed wit hout liq uid solven t extraction. In ad dition. ve ry high sens itivit y for semivol ati le compo und s such as diese l fuel can be o btaine d because essentially all t he an alyte is e xt ract ed from up to a gram of so il and de po sited on colum n.
' ---r?...~ ~; r,
H007.doc
,
~"
. _.
, . . $- . .
-
\
. -....... .'. , .. . •
\
Valeo v alve hand le rotates to inj ect sam ple
The SRI Th ermal Soi l Desorber accessory is mounted In a heated va lve oven on the left hand side of the 86 1OC Gas Ch romatog rap h. The g lass tube which contains up to a gram o f so il is inserte d into the ho t ( 2 50 C ) desorbc r ce ll through an opening in the top of the Ges red lid , and then secur ed by tightening th e nut and 3/8" graphite ferrule. Th e handle of the man ua lly ope rated Valco 10 port valve ex its from the left rear of the heated valve o ven, and is rotated to d irect the carrier gas flo w down and through the hot soil. transporting an y hydrocarbons with boiling points below 3 00 C ont o the GC column. The stai nless ste el tubing leading from the Yaleo valve to the eolwnn is routed and insulated to maintain a h igh tem perature all along the path to the column oven to prevent high boiling compo unds from condensing or tailin g .
.
.'
~ :l ·" ....Ii -~''',~x(, : - ~. -._- - :j
.
~
-.
Heated Valve Oven conta ins Therma l Desorbcr
1i='T."
,r
Transfer line from valve to column must be kepi as hot as possible to avoid sample condensation. Arrange insulation to create "hot pocket" in this area.
70 (of 550 ) 2006(-2016)
71
(
l
Chapter:
INJECTORS
Topic:
THERMAL DESORPTION fl'<7C:0:-X-- Gas Inlet
With the SRI 8610 Thermal Desorption unit, samples of soil or other solids can be analyzed for organic compounds without any extraction or other special sample preparation. The sample being tested is placed directly into the 3/8" a.D. machine glass desorption tube. The bottom end of the tube is plugged with glass wool. This holds the sample in place without restricting gas flow. A one gram sample weight is adequate. The open end of the tube is then packed with glas s wool to secure the sample and inserted into the opening of the 3/8" stainless steel Swagelok" hardware attached to the pigtailed gas tubing. This hardware is the desorber tube cover and seals the organics in until desorbed. The gas tubing supplies the carrier gas. The sample tube is then inserted into the heated desorption chamber and secured by the 3/ 8" Swagelok't nut. When the sample is in place, the injection valve is rotated (either manually or automatically. if so equipped) , and the volatized organics flow info the column on the carrier gas. Historically, samples in soil have required solvent extraction with methlyene chloride, hexane, carbon disulfide or others prior to injection into a gas chromatograph. Unfortunately, solvent extraction often dilutes the sample and adversely affects detection limits. The detection limit for diesel fuel in soil by extraction is typically 10 ppm. When thermal desorption is employed, 10 ppb is attainable. With the phasing out of the use of CFCs such as freon and the ever-increasing scrutiny of laboratory solvent usage, the stripping of analytes from the soil by and into the column by thermal desorption is a practical (and sensible) alternative.
In the past, direct thermal desorption of average soil samples had been difficult due to the massive amounts of water liberated. This tended to extinguish the flame of the Fill detector (typical detector for hydrocarbon analysis). Water elutes along with the early gasoline components and may interfere with the quantitation of benzene and toluene. Water does not interfere, however, with diesel quantitation because the diesel components elute well after the water.
T HEMIA L DESORBER DETAIL
Deso rber tube ~cover hardware
r-·'-\.- (CRS 3.18" graphite ferrule pan # 211600)
" .._._"
-of- Glass woo l
. - 3/8"
Fo r replacement rubes, contact:
SANDFIRE SCIENTIFIC LTD.
D.D. glass
desorption rube
(604) 826-5355
.. :~. -
part no. S·9 1OO
Sample
(pa ck of 10 tubes)
+- Glass wool (
~
Desorber o pening. Located on top left side , of chromatograph. HOT .
Carrier in _ _\.-_~_
Tubing
"pigtail----* Desorbe-r~
To column
10 PORT VALVE DIAGRAM -LOAD- POSITION
Carrier in - - \.-_ _--/...
Tubing
-pigtail" -s-
The Fill detector-equipped SRl 8610 gas
chromatograph is supplied with an advanced design ceramic ignitor which can be run hot continuously,
thus re-igniting the FlO flame should it momentarily be affected by the passing water vapor. This minimizes
the water interference and flame-out difficulties normally experienced with high moisture content samples analyzed with an Fill detector. C:\EP2 IDOCSITIU1U.1OES.EPD
Desorber -Joo
r' L
':::f-:::'-':::>';~
'-'.
To column 10 PORT VA LV E DIAGRAM -INJECT- POSITION
REV. 01-05-94
71 (of 550 ) 2006(-2016)
72
Chapter:
INJECTORS
Topic:
O PERAT ION OF THE THERMAL DESORBER
To operate the SRl model 8610 thermal
desorption unit. the following steps are required:
1. Place a clean desorption tube with a glass wool plug at one end on a scale of known accuracy. The tare weight is obtained. Thi s is done by either weighing the clean, empty tube and recording the weight , or by placing the tube on the weighing platform and zeroing the balance . 2. Load the sample into the desorption tube and place the tube back on the balance. The gross or sample we ight is recorded. The actual sample weight is obtained by subtracting the tare weight from the gross weigh t. A sample of solid we ighing be tween 0. 1 and 1.0 gm is recommended for best results. It is pre ferable to use a small sample d ue to the moisture
that average samples contain. A small sample is less likelv to interfere with the FID detector flame. A large r sam ple will permit the user to attain lower
detection limits, but water content must be co nsidered . 3. The tube co ntaining the weighed sample is plugged with glass wool to hold the sample inside an d the tube is inserted into the 3/8" opening of the S wagelok'" hardware co mprising the desertion rube cover. The end of the plugged tube is slid into the opening with the nut loosened . O nce the tube has bee n inserted, the nut is tightened to seal the sample
in the assembly. 4. Verify that the injection val ve is in the "LO AD" position. Insert the sealed de sorption tube assembly into the de sorption chamber opening on top of the chromatograph and quickly sec ure it in place by tightening the Swagetok" nut at the opening. Care should be exe rcised when performing this step. as the desorption chamber is typically maintained at 350 degrees C and a burn potential exists. 5. Initiate the c hromatogram either by keyboard o r foot switch. 6. As soon as the desorption tube assembly has been secured into the desorption chambe r. the injection valve is rotated 10 the "INJECT" position, and the sample is allowed to flow into the column. After the sample has desorbed completely. the valve is returned to the "LOAD" position. The tube may then be removed from the desorption chamber and
The co lumn is co nnected to the inj ection valve inside the valve oven using a 111 6" to 1/8" adapter and 0.040" J. D. stainless steel tubing (11 16" 0 .0. ). This ensures a uniform sample tempe rature while en route to the column and eliminate s any possible co ld spots. The ignitor element may be set to
6OO"C (a dull red glow) for the duration of the run in orde r to avoi d any possibility of FlD flame-out should the sample have a high moisture content. The ignitor eleme nt can operate continuouslv at this high temperature without a ffecting its normal life expectancy.
Replaceme nt de sorber tube s may be ordered directly from Sa ndfirc Sc ientific Ltd . in M ission, B. c., Canada a t phone (604) 826-5355 (part no. 5-9100 ).
- ....--E .....
- I
EXAMPLE OF TEMPERATURE PROGRAM FOR DESORPTIOK
-
---_.-_._.
"""-
cleaned. The contents of the tube should be removed and discarded. Once the tube has bee n thoroughl y cleaned, it may be returned to service. If in doub t, a blank run should be used to verify tha t the tube has been cleaned adequately. Once the blan k chromatogram is acceptable, the tube may be re-used for a subsequent sample. Users may make their o wn tubes if so desired. C:\EP2\DOCS\1 lIFJU.fDS::!.EPO
EXAM PLE OF TIMED EVE ~J TABLE FOR CONTROL OF AUTO .\1ATED N JECTIOr;
REV. Ol ~ .""
72 (of 550 ) 2006(-2016)
73
~----------------~--------~---------, ,
Chapter:
INJECTORS & GAS VAL VES
Topic:
Thermal Desorber Soil Sample Preparation
1) To ensure that the soil sample analyzed is representative of the site sample, mix the soil in the sample container compl etely. Then weigh 10 grams of soil from the sample containe r into a 150 ml beaker. 2) Add 10 grams of granular sodiu m sulfate (Na2S04) to the beaker and mix wi th a stirring rod or spa tula. The granular sodium sulfate ,
when mixed with the soil, absorbs most of the moisture from the soil, allowing c lay soils to be
~ ----
-------------_. -----
"60 10 gms.
70
NA~S04
60
so
ground into smaller particles. This is important bec ause dense clay will not fully desorb . The
"
mixture of soil and NA2S04 should be of a granular co nsistency with small uniform particles . 3) Roll a small a mo unt of glass wool into a ball with your fingers , then insert it into one end of the glass desorption tube so that it remains in place. Then plac e the tube on a tared balanc e. Record the tare weight.
4) Load approximately 0.5 grams of the soil -sodium sulfate mixture into the desorption tube.
;::...i.l
10 gms . / soil sample
t-
2S
Sample preparation in beaker
(6.35cm)
I=;;:::::::==~ /
Borosilicate desorption tube
5) Insert another plug of glass woo l into the de sorption tube to hold the sample in plac e. Do not compact the sample when insertin g the glass wool or the sample may not de sorb thoroughly . 'When properly loaded and plugged, the tube should resemble the diagram to the right. 6) Place the loaded desorption tube on the balance and record the undesorbed we ight After desorption, allow the tube to cool and re-weigh to obtain the de sorbed weight. The hydrocarbon content can then be calculated based on either the desorbed weight of the sample or the undesorbed weight (wet weight) of the sample. The difference between the two weights represents the amount of moisture left in the sample following the mixture with sodium sulfa te.
C :\ EP3\ DOCS\IDPREPl. EPD
Glass woo l plug
Placement o f glass wool in desorp tion tube prior to sa mple insertion
00 Nar COMPAcr SAMPLE!
Sample mixture
Glass wool plugs
Diagram of assembled sample desorption rube containing 0. 5 gms of soil -
N~ 04
sample mixture
REV _ 06-2 1-93
73 (of 550 ) 2006(-2016)
74
DETECTORS
'------------ ] Topic:
Operation of The Methanizer Accessory
o
o
METII
"""""'' ' ' -F--.=,. ::..-~:-----+_
=
-
do""""
Fill assembly
o WP VIEW OF ME1HANIZER-EQUlPPED TCDIFID CHROMATOGRAPH
Carbon dioxide and carbon monoxide can be catalytically reduced methane if passed through a nickel-packed trap heated to 375° C with the use of hydrogen either as
10
carrier or make-up gas. Methane can be detected to 1ppm using the FID detector, permitting lower detection limts than obtainable with unmethanized CO and C02 using the TCD detector. With the SRI design, the methanizer is placed in series between the TeD and the FlO. This enables the user to quantitate the sample firs t through the TCD as CO and C02 and then through the FID after methanization. In this manner. high concentrations (l % and DETAIL· LOCATION OF METHANlZER ON FRONT OF greater) are quantitated by the TCD and COLUMN OVEN ABOVE CARRIER GAS POLISHING FILTER low concentrations by the FID. The methanizer is held in place by liS- Swagelo~ nuts. A metal ferrule is at the left end of the methanizer tube. A graphite ferrule is installed on the right end (Allteeh # SF-2
r
C;\EP2\DOCS\).IEJlK)l . EPD
R.£V. Ol -W-9'2
74 (of 550 ) 2006(-2016)
75
In the combo mode. the DELCO is operated after the FlO. The FlO
s~nal
is usually con-
nected to Channel 1 on the PeakSimple data system . The DELCO signal ma y be on Channel 2 or 3. Each detector ampfif.er is labeled at the factory with the data channel to which it has been connected. Detector signals may of course be connected to any ava ilable data channel by simply attad"ling the white and black signal wires to the screw terminals on the AID board inside the GC. 1) Set the FlO hydrogen and airflows for norma l FlO operation. This is typica lly 25 mVmin hydrogen ( corresponds to 25 psi ) and 250 rnVmin air ( typically 6 psi ). The exact pressure required for each flow is labeled on the GC 's right hand side. 2) Set the DELCO temperature setpoint to 260 using the front panel adjustments. This number actually represents 1OQ()DC. The DELCO will heat up to about 254 and stabi lize. The quartz collector electrode will appear a bright red color due to the 1000c temperature. 3) In the FIOIOElCO combo mode. the FlO is nonnally operated on high gain or on hifilte red gain if the peaks are mo re than 10 second wide at the base . The hi-filtered gain position is identica l to the high gain except that extra noise filtering results in a quieter baseline. The DELCO amphfier is nonnally operated on low gain . In this conf~uration the FlO and DELCO produce approximately the same response to chlorinated peaks such as TeE ( same peak area counts). The FlO will generate approximately 4 area counts per nanogram injected on column while the DELCO will generate 2-4 area counts per nanogram of chlorinated hydrocarbon. ( see example chromatogram below ).
~~ - f---.• I
'I
•V •
ll
l-
i !!
'j-
/--......
l!
, •
•
J I-
•• .
:•
i
•
i
I
•
i
l-
\'\
--
.-
- .. FlO shows 500 area counts tor 100 nanograms of Perchlorethylene -
~
..
s;
i
DELCO shows 250 area counts for 100 nanograms of PerchlorethyJene ~
•
K
,
-, ·•
"-
~-
~ -.
---
\.
Manl04.pub
75 (of 550 ) 2006(-2016)
76
DElCO peak cwerlaid on FlO peak for PCE. then expanded for clarity.
The smaller peak is the DELCO re-
sponse.
1) As shown in the chromatogram above. the DELCO peak for PeE occurs at the same time as the FlO peak for peE. Notice that the DELCO peak exhibits a little bit of ta iling compared to the FlO response. 2) In the FIDIDElCD combo mode, the min imum de tectable amount is approximately 1 nanogram. Assuming a 1 microliter injecti on. this translates into approximately 1 ppm. The exact detection limit will depend on the analyte molecule ( how much ch lorine! bromine in the compound) and the chromatographic conditions. A sharp peak is always more detectable than a short fat peak. 3) The detection limit will be worse when using the built-in air compressor for FIDIDELCD flame combustion instead of clean dry tank air. While the built-in air compressor is useful and convenient, low levels of halogenated compounds in the ambient air ( even levels below 1 ppm) cause the DELCO to lose sensitivity, and fluctuations in the level of organics in the ambient air may cause additional baseline noise.
4) In the FlO/DELCO mode the DELCO response is useable from 1 to 1000 nanograms with a slightly quadratic calibration curve . EPA and other regulations allow the use of detectors with ncn-nnear response as long as the operator calibrates with sufficient data points to accurately model the detector response CUNeo Where a 5 point calibration would normally be required , the DELCO may demand a 6 point calibration. The DELCO calibration curve shown at light illustrates the quadratic response from 11000 nanograms of TCE in-
JOCled
-
"
M an205.pub
76 (of 550 ) 2006(-2016)
77
1) The DELCO can be operated in a high sensitivity mode by eliminating the hydrogen from the reactions which lead up to the detection of the CI02-Br02. Because the chlorinelbromine atoms prefer to react with hydrogen to form non-detectable HCI-Hbr, than with oxygen to form detectable CI02~Br02 by a factor of 100-1000 to 1, eliminating the hydrogen improves the DELCO sensitivity by at least 100 times. Water must also be eliminated as at the high temperatures inside the DELCO, hydrogen becomes dissassociated from the H20 molecule and available as a reactant. In practice, this means turning off the hydrogen and using clean dry tank air ( not the built-in air compressor). 2) Remove the hydrogen supply from the GC by disconnecting the hydrogen supply at the ec'e inlet bulkhead on the left hand side of the instrument. Reduce the air flow to the DELCO to 50 mUmin by turning the air pressure setpoint down to 1-2 psi . An add itional airflow restrictcr-ccneietinq of 12" of .067 tubing ( 1/16', 1.58mm) with an intemal diameter of .010 (.25mm) can easily be added 10 the air supply immediately below the detector to enable the flow to be controlled more precisely at higher pressures. With the extra restrictor installed a pressure setpoint of 10 psi will deliver an air flow of approximately 50 mUmin. 3) If using a capillary column, push the column through the FlO jet until it just enters the ceramic tubing of the DELCO. This will improve the peak shape somewhat because the column effluent will be discharged into the flowing airstream and will be immediately swept into the DELCO detector volume. When switching back to FlO/DELCO combo mode remember to pull the column back into the FlO jet. 4) Remove the FlO collector electrode and replace it with a 1/4' cap fitting . The FlO collector electrode allows some gas to escape from the FlO combustion area , and this is not desirable when operating in the high sensitivity mode.
The DELCO chromatogram shown at right illustrates the response to 10 picograms ( 1ul of 10 PPB ) ofTCE in the high senstivity mode. Note that in high sensitivity mode, there is some response to the methanol solvent.
Ten picograms ( 10 PPB) of Trichloroethylene
.7 ,
-- -
Man206.pub
77 (of 550 ) 2006(-2016)
78
Chapter: Detectors .
Topic:-~ l-:Opeiati;'gtfilFIDIDELCD in the high sensitivity : ..:
"' DEL,CD onIY:rTl0d~ ~~:;:>L) ~< ' i;:.~; j
,
. :.
," .,
The FlO/DELCO detector is shown at right confi gured for the hig h sensitiv ity m ode .
The collector electrode is removed and a 1/4" cap installed instead.
1) Just as the DELCO response curve is quadratic in the FIDIDELCD combo mode, the response is also quadratic in the high sensitivity mode, but sensitivity is increased by 1001000 times. In the high sensitivity mode the DELCO is most useful in the range of 11000 pfcograms which assuming a 1 microliter injection translates into 1-1000 PPB. 2) In the high sensitivity mode , the DELCO can perform much like an Electron Capture Detector ( ECO ) except that the DELCO is more se lective for ha logens and blind to oxygen. 3) Although the DELCO will not be damaged by large quantit ies of chlorine/bromine, there is a short term loss of sens itivity fo r an hour or so fo llowi ng th e injecti on of 1 ul of Methytene Chloride for example. 4) When possible quantitate by the Internal standard method, usi ng a chlorinated! brominated compo und for the internal standard peak . Us ing an internal standard will correct for Changes in the DELCO detector's respo nse.
DELCO linearity in high sens itivity mode is s hown
at right from 10 to 1000 plcograms ( 10-1000PPB ).
Ten to 1000 picoqrams of Tri c hloroethylene ( TCE )
At leve ls above 10 nanograms the detector is saturated .
J Man207.pub
78 (of 550 ) 2006(-2016)
79
Chapter: ., Dete.ctors " :~-'C, . :
' ''-' ' ' : '_'0:-"
_,." ..,. .,~_-_.
4~~ic;~;~;P!:¥~~~1~\~~b6_d~d4~~~D~f~do~:( rlEbc6';- ~ - : - ~;a:c::
_. ,
-
-o-:c,_-,
'';
.~_.
The DELCO detectoris only available in combination with the FlO detector.
The F rO/DE LCO combo detector is mou nted to a therm ostatted aluminu m hea ter block on the right hand side of the col umn oven.
The FIDfDELCD combo detector is shown at right removed from the GC.
FlO body The DELCO part of the detector is the large black cylinder which mounts into the right hand port of the FlO detector body . It ca n be separated from the FlO bOdy by loosening the 1/4 · Swagelok nut and graphite ferrule wtIich secures It In place
Man l34.pub
79 (of 550 ) 2006(-2016)
80
C ~a p~er:i Detect_or:s ~._, . - - -
JO~i~~-;~;~fr6~J$~;6rYtic ¢~ridt;ity'Detecl~r (DE~~DJ> :-, -' _. ';-'"" ~.
::.-: :-;1- ':": ~?1E ~~ ~:r;~-,-,
-0; 0'",",-_ -_~ ::':;'_..;~t; :-:. _:q~1 ~ - ·~t~ ··:k: :-:,.:
o_~:-' ~~O:.·~f
-
.. -.
The DELC O co llector electrod e ( part# 867Q..1028) can be rem ove d from the hea ter. Becau se the heater ope rates at close to 10000C, it wi ll fail eventually. A new heater ( part # 867 0-1 027 ) is Jess expensive than the complete heater/collector assembly (part# 8670-1029), so it may make sen se to rem ove the collector from the bad heater and re-mstan it into a new heater .
--:"'
_. ",, ' ~
-:.:"-
Dis-connect the three sm all plati num wires from the screw termina ls and gently mov e them aside.
Using two wrenches to avoid rotating the fitting, loosen the 118- Sw agelok nut and graphite ferrule which secures the co llec tor electrode into the heate r.
Co llector
The collector can then be withdrawn from the healer.
ManI35.pub
80 (of 550 ) 2006(-2016)
81
Chapter: DeleCtcirs
·;.~'t" ~ct_ ''''_: ' - .'.
I:pj-~~j-:Bt/i;~;~~~'6t=-~~~d~~"~c~et~eto({ DELCO ) :' : ..: l:_".'
~:;~~ ~-:-~-,,:-:::::f~~L:' ~~~~-=~~ ~} .:~;-t=-:;-;- ~ ~ _±~~~r ~'::
W hen the collector electrode is re-in stalled in the new heater, it is important that the tip o f the electrode is positioned in the cen ter of the heater.
:~- - ~._
Tip of electrode centered in heater
Use a file, rod . scre wdriver or oth er long th in object as a gauge to verify that the electrode tip is centered in the ne w heater body. Gently re-position the electrode by sliding it through th e graphite ferrule to get the prop er adjustment Fina lly. look down the bore of the hea ter and check to make su re that the hp of the eectrode is centered in the bore of the heater. and is not bent to one side , touc/"ung the heater wa ll.
Connect the heater/collect or assembly back onto the FlO body. The heater/co llector assembly should be inserted as far as POSSIble Into th e FlO body.
The two DELCO heater wi res are connected to the push termmais on the dec k of the GC which are labeled DE LCO heate r.
-. Man l 36.pub
81 (of 550 ) 2006(-2016)
82
The red , white and yellow wires are inserted into the labe lled screw term ina ls on the deck of the GC.
Se l lhe DELCO heate r setpoint tem perature to 250, Th is is an arbitrary num ber which actu ally corresponds to a temperature of 1000"C. Bette r sensitiv ity can be obtained by raising the setpoint to 26 0 or 270 , but at the cost of red uced heater lifetimes.
The actu al temperature o f the DELCO heater WIll equilibrate to about 7 degrees less than the setpoint with in 10 m inute s
Verrty that the FID flame is fit by hOlding a Shiny wrench or mirror above the F lO co llector electrode and looking for droplets of water condens ation .
Manl3 7.pub
82 (of 550 ) 2006(-2016)
83
[
~r.
DETECTORS
Topic:
FPD - Theory ofOperatioo and General Information
The Flame Photometric Detector, or FPD, as it is referred to, is typically used to analyze for sulfur or phosphorus-containing compounds, as the photomultiplier tube is extremely sensitive to a broad portion of the visible light spectrum, including those specific wavelengths emitted by the combustion of sulfur and/or phosphorus molecules in a hydrogen flame. Specific filtration inserted in the light path allows only the specifically desired wavelengths to pass unimpeded into the photomultiplier nthe for quantitation, Specificity for sulfur and phosphorus is obtained by the used of precision optical filters designed for use at 393 and 525 nanometers, the wavelengths of light that are emitted as the sulfur or phosphorus compounds elute from the analytical column and enter the flame of the detector. The hydrogen flame in the detector is invisible to the unaided eye because it does not give off any visible light, yet permits the photomultiplier tube electronics to establish a reference as a baseline or background value. When a sulfur molecule, for instance, enters the flame, a measurable quantity of blue light is emitted by the flame and this specific frequency of light is allowed to pass unimpeded through the filter and onto the measuring surface of the photomultiplier nthe (PMT). The electrically-operated photomultiplier nthe converts the quantitated emission of light into an analog signal that can be delivered to, and used by a data system for display and integration. The in-line optical filtration eliminates any interference from odw:r compounds present in the sample-bea.ring carrier gas stream.
SlUIlple-1aden carrier gas exiting column
into FPD detector
~~~~~~~!;;,;=~~~~ , aUt r+ Comp",s"",,
flamepoet
10
fuel hydrogen flame
/ Oplic.J filter (393 or 525 am)
BASIC flAME PHOTOMETRIC DETECTOR DIAGRAM
Ceramic ignitor clement 10 light FPD flame)
(...d
t
....
Secondary hydrogen inlet (used to
PMT
enrich flame. iDcreasio2
sensitivity and prevent moisture buildup on filter surface
tubo
SigoaJ 00fiU to detector electronics for processing
In addition to the standard single FPlJ detector configuration that may be used to quantitate either sulfur or phosphorus compounds with the appropriate in-line optical filter, SRI offers a Dual Flame Photometric Detector that permits the user to analyze a single sample simultaneously for both sulfur and phosphorus compounds. Two photomultiplier tubes, equipped with filters for 393 and 525 nm, face each other across the flame and produce simultaneous analyses from the same sample injection. SRI offers the only Dual Flame Photometric detector (DFPD) available today. O: \EP2OOCS'H'DDET.EPD
REV_ 04--(J8...94
83 (of 550 ) 2006(-2016)
84
[
Chapter: Topic:
DETECTORS DFPD - Theory of OpeI1llion and General Infunnation
The Dual Flame Photometric Detector, or DFPD, as it is referred to, is typically used to simultaneously analyze for sulfur and phosphorus-containing compounds. The photomultiplier rubes employed are extremely sensitive to a broad portion of the visible light spectrum. Specific filtration inserted into the light paths permits only the desired wavelengths to pass into the photomultiplier tubes and be quantitated, Specificity for sulfur and phosphorus is obtained by the used of precision
optical filters designed for use at 393 and 525 nanometers, respectively. the wavelengths of light that are emitted as the sulfur and phosphorus compounds elute from the analytical column and enter the flame of the detector. The hydrogen flame in the detector is invisible to the unaided eye because it does not give off any visible light, but establishes a background value for the photomultiplier tube to
reference as the baseline measurement When a sulfur molecule, for instance, enters the flame, a measurable quantity of blue light is emitted by the flame and this specific frequency of light is allowed to pass through the filter and onto the measuring surface of the photomultiplier tube (PMT). The electrically-operated photomultiplier tube converts the quantitated emission into an analog signal that can be delivered to the data system for display and integration. The process is similar for phosphorus-eontaining compounds. Each photomultiplier tube is equipped with full amplifier and data acquisition electronics to permit the simultaneous acquisition of both signals by a data system or other device. The SRI Dual Flame Photometric Detector (DFPD) permits the user to analyze a single sample injection simultaneously for both sulfur and phosphorus-bearing compounds, reducing the normally required analysis time to half.
Two separate photomultiplier tubes, equipped with filters for 393 and 525 nm, face each other across the flame and produce concurrent signals that may be analyzed by the data system. SRI offers the only Dual Flame Photometric detector (DFPD) available
today.
r-+
Signal output to detector elecrrceics for processing
Secondary hydrogen inlet (used
PMT
to enrich flame. increase sensitivity and prevent moisture buildup on filter surface
tube
SULFUR
DETEcnON
Optical filter
(393 mn) Primary hywogell inlcl (needed to mainlllin flame) -----ill'-
../ rrr,:
~
..........
Exhaust vent
:]
>
Ceramic ignitor element
Sample-laden carrier gas eXiting column
(used to light DFPD tlame) Optical filter (S95nm )
into FPD detector flameport Secondary hydrogen inlet (used to enrich flame. increasing: sensitivity and prevent moisture buildup on filter surface
PMT tube
4
PHOSPHORUS DETECTION
Signal ourpUl to detector electronics
.•.
for processing
BASIC DUAL FLAME PHOTOMETRIC DETECTOR DIA.GRAM
D:\EP2DOCS\DFPDD£!.EPD 84 (of 550 ) 2006(-2016)
85
Chapter:
DETECTORS
Topic:
Operating The Flame Photometric Detector
o
o FPD voltage control knob
Ignitor element and FPD flameport
assembly
o
Ignitor current control knob
/ . Primary hydrogen AirreguIator
\
regulator
/
Carrier regulator
and flow controller
FPD flameport exhaust tube
The flame photometric detector (FPD) is primarily used for the analysis of compounds
containing sulphur or phosphorus. The FPD consists of a flameport similar to a flame ionization detector (FID), but it lacks the collector electrode used to quantitate ionization. In the FPD detector, a photomultiplier tube (PMl) is positioned beneath the flameport for the purpose .of monitoring the spectra emitted from the flame. A narrow wavelength optical bandpass filter is located. between the flame and the photomultiplier tube window in order to selectively permit the passage of specific
wavelengths of light into the photomultiplier tube. When testing for phosphorus-based components, a 525 nanometer filter is utilized. This filter appears as a yellow disk. When testing for sulphur-based components. a 393 namometer filter is utilized. This filter appears as a blue disk. When a sample component containing one of the specific chemicals elutes from the column and into the flame. the specific spectrum sought is emitted and is permitted to pass through the appropriate filter and strike the photomultiplier rube. This produces a quantitatable signal into and response from the detector electronics. which is relayed to the data system to be interpreted as a peak. The SRI FPD incorporates several innovations: a compact PMT which can be mounted in a very small space, digital display of the PMT voltage being used, a variable output high voltage power supply and a secondary hydrogen inlet for purging the light path and enriching the flame boundary
region with extra hydrogen. It is important to note that the photomultiplier tube may be damaged by exposure to stray light when energized. De-energize the chromatograph prior to performing any maintenance that requires exposing the photomultiplier tube to ambient light. C: \EP2 IDOCSIFPOOI.EPD
REV. OI.Q4..92
85 (of 550 ) 2006(-2016)
86
i
Chapter:
OETEcrORS
1 i
Topic:
Operating The FPD Detector
\,-
- -- - - - -- - - -- - - - - - - - - -- - - -
-.
The flame photometric detector (FPD) is similar to a flame ionization detector in that the sample exits the column into a flame. A FID would then measure ions produced as a result of the combustion, finding any organic compounds. A FPD analyzes the spectrum of light emitted by the compounds as they luminesce in the flame. By selecting a specific band pass filter, the FPD may selectively detect compounds containing sulfur or phosphorus . When compounds are burned, they release photons of discrete wavelengths. The bandpass filter will only allow Primary H;J. injected photons to move through that are into carrier gas within the range of the filter stream nourishes the specifications .
~ "'---* Exhaust tube
~
Ignitor
flam';'~~-.;~~~
Sample-laden ::-.. By selecting a 52Snm carrier gas filter (yellow in appearance), from column phosphorus-eontaining compounds can be quantitated. A 393nm filter (blue in appearance) permits sulfur-containing compounds to be quantitated.
A secondary hydrogen supply is
Secondary H2 ~ :
sweeps the
directed toward the ftlter and has two functions - making the flame hydrogen-rich, which makes the FPD more sensitive, and by directing it towards the filter, keeping the filter free from water which is formed in the flame and would tend to condense on the filter. Moisture is vented through the exhaus t outlet.
=nE~~IT--
til""
DIAGRAM OF FPD
n ::
.:I
.,
Bandpass filter
Photomultiplier rube
n,. :1-""': "
n
""'"
DETECTOR
Light must be kept out of the detector chamber so that only light from the flame will be analyzed.
FPD PRELIMINARY TESTING: Verify that all gases are set to the proper flows. The primary hydrogen that feeds the flame is set to 30 ml/min (30 psi ). The secondary hydrogen that sweeps the filter surface, and enriches the atmosphere over it, is set to 30 mlImin (psi). The flame's air supply is set to 100 mlImin. (Spsi), and the carrier gas is set to between 20 and SO m1Jmin. Before the FPD is operated, perform a few simple tests. With the voltage to the PMT off and the flame unli t, remove the FPD exhaust tube. Look directly down into the FPD detector body. You should see the reflection of your eye deep in the center of the detector cavity. This verifies that the bandpass filter is properly aligned. If the reflection of your eye is not visible, realign the bandpass lilter. The next test is to check for possible light leaks. Replace the FPD exhaust tube . Set the FPD gain switch to LOW . With the flame unlit, set the FPD voltage to 500 volts. The voltage will read negative on the GC's LCD display. Lower the red protective oven cover. Take note of the millivolt reading produced by the FPD. The millivolt signal should be close to zero. Now raise the red protective oven cove r and observe any change in the millivolt signal. When the detector is light-tight, the millivolt signal should rise no more than 10 millivolts. If the millivolt signal rises above this amount, inspect the FPD detector assembly for light leak sources . C \95EPDOCS\FPDQ2.EPD
REV. 12-18-95
86 (of 550 ) 2006(-2016)
87
I
Chapter:
DETECTORS
Topic:
Servicing The FPD Detector
\_ - - - - - - - - - - - - - - - - - - - - - - - - - - - - - As has been stated before, the flame photometric detector (FPD) is similar to a flame ionization detector (FID) in that the sam ple exits the column into a flame. It differs in that the FID measures ions produced by organic compounds during combustion, while the FPD analyzes the spectrum of light emitted by the compounds as they luminesce in the flame. One of two filters available determines whether the detector "sees" sulphurous or phosphorous compounds. Regardless of which filter is in use, it is important that the filter be properly installed, clean, and free from dust, debris, and particulate matter. The bandpass filter Jot will only allow photons within the bandpass of the ~te:r specifications ~a~j~i to pass, but sensrtrvrty may be "reduced if the filter is Sample-laden _:::0 """"'--i~~~~~ > improperly installed or dirty. ca rrie r- ga s inl et
Fi~~~''''''E:~=1
. ,- -~J~~(..
from column
rube
r,---" Ignitor
?
As illustrated in the Compressed diagram at right, either of the filters (393nm or air inlet 525nm) installs into the lower e xtension of the FPD assembly with the mirrored Secondary filter surface of the lens facing the flame (up). The H, inlet ---i>-=IJ;"':~t=~ Bandpass Rubber O-ring blue (sulphur) or yellow (phosphorus) side of the filter should face the lens of the Photomultiplier photomultiplier tube (down ). A rubber O-ring is "----_ - - - " / tube inserted j ust below the lens in the lower assembly extension to secure the lens in the / ' Rubber- a-ring stainless steel body. The lens should seat fully in the stainless steel body, so that if the c::::iE3-- Split Teflon operator temporarily removes the FPD exhaust to-pin socket _ ferrule tube assembly and looks down into the FPD body, the reflection of the eye should be clearly seen in the visible mirrored surface. A misaligned lens will not permit viewing the ! .. eye' s reflection. ..~." -_:::~
I;; rl--s~~~~ S::I
The miniature photomultiplier tube
(PMn is connected to its lu-pin socket, and a
DIAGRAM OF
FPD
\ \
Photomultiplier- - signal cable
DETECTOR rubber Ocring is slid over the PMT body until it is j ust above the point where the photomultiplier tube body meets the soc ket. Just beneath this O-ring, a split Teflon ferrule is mounted so that it sits on the socket, just below the point where the tube body meets the socket. This is also j ust below the rubber Ocring. Inspect the lens of the photomultiplier tube for dirt or debris. Use care in cleaning this lens, if cleaning is necessary .
The tube / socket assem bly is then inserte d into the lower FPD assembly body and held in place by the knurled stainless steel retaining nut. When the FPD detector assembly is fully reasse mbled, pack any excess signal cable from the socket back into the FPD chassis orifice. Th is discussion of the servi cing of the FPD detector will be especially useful for users who must change filters on a regular basis to switch fro m sulphur mode over to phos phorus mode and back again. The FPD detector is provided with one user-specified filter. Replacement and secondary filter s are also available from SRI Instruments. 0: \9 ~ EP[X)CS\ FPD03 EPD
REV.
r-se-ss
87 (of 550 ) 2006(-2016)
88
Chapter:
DETEcrORS
Topic:
Demonstration of The Detection Limit of The FPD Detector
The flame photometric detector, or FPD, as it is commonly referred to, is capable of extreme sensitivity and selectivity. The selectivity is obtained by the use of optical filters placed in the light path to the photomultiplier tube. These filters permit the specific passage of 393 and 595 nm wavelength light emitted when either sulphur or phosphorus-containing compounds are burned in a hydrogen flame. The sensitivity of the detector is the product of the combination of the design of the pbotomultiplier tube and the SRl detector electronics design coupled with the optimization of gas flow through the detector. The SRl design is simple and readily permits being coupled with an FID detector or a second photomultiplier tube for simultaneous sulphur/phosphorus analysis. Although the one ppm (l nanogram) carbon '._0_ ,...,,,_ disulfide (CSU peak shown at left is a clean, crisp peak, it is by no means close to the limit of detectability of the SRl FPD detector. Carbon disulfide produces the following calibration curve when concentrations. as in this example (shown in the screen illustrated below) of 0.1 to 3.0 ppm cs" are plotted on the data system screen. 1 wrn (l ngm) of c:arboo disulfide via FPD detector
The lowest level detection limit acbeived by SRl for carbon disulfide using the flame photometric detector, as demonstrated in this example, was O. lppm (0. 1 nanograms) of sample. Detection of concentrations beneath this level could not be reliably obtained, as the component peak area fell within the background noise leve l at
smaller concentrations. For the calibration curve shown at right, a seven point curve was COOSb'UCted, using six data sets generated by analyzing ~ at concentrations of 0.1, 0.25, 0.5. 1.0, 2.0, and 3.0 ppm via FPD. Points below 0. 1 ppm could have been determined if the noise level did not obscure
-_. _.. _-' ... .-......- "....__ - .. -... _._.-...._ ................_ ........ ._--_._--
_
,,--
.."
•._ . . . .._
0._ 0._
_ _
~
,
-::'-1.. · ;---;. / ~; I
-- _.- .-
..- ..
~
1 -I
]
I _I
_
(
._J
I _
le'- ]
I
C ........
PeakSimple calibratim CUJ"Ve for CS 2 via SRI FPD
the peak areas, preventing integration. The 0.1 ppm peak is at a level approximately twice the background noise level It is not recommended to attempt to establish detection limits below this level, As can be see n in the screen at left, the CS2 peak clearly stands out above the background noise even at the one-tenth of one nanogram level (0.1 ppm or 100 ppb), facilitating quantitation of
the carbon disulfide. Comparable detection limits can he expected for other similar compounds when operating the flame photometric de tector in the sulphur or phosphorus mode. 0 .1 ppm
or CS 2 delecta ble well above background
D:\EP2DOCS\FPDDTUM .EPD
REV. 12-14-93 88 (of 550 ) 2006(-2016)
89
-
/
I I
Chapter:
DETECTORS
I,
Topic:
Proper Photomultiplier Tube Operating Voltage For FPD
The photomultiplier rube employed in the SRI flame photometric detector (F PD ) is a new compact design that offe rs optimum performance and a long service period when operated at the recommended operating voltage. Photomultiplier tubes used by different manufacturers require
distinct voltage levels to drive the tube for proper response. The SRI version requires a drive voltage that is lower than many, and in fact, is lower than the operating voltage used in earlier FPD detectors manufactured by SRI prior to use of this compact photomultiplier tube .
[I] . r/b
o
•
o
Setpoint display and trimpoc
adjustments for the FPD PMT tube are located on the frunl
§E) I@l
•
•
•
control panel
•
•
0
D \9 7F.POOCS\FPD04 . EPO
FPD ce ramic ignitor
0
FPD detector amplifier
®
gain control
•
FPD detector assembly
TOP VIEW OF FPO DETECfOR LOCATION ON 86IOC GC CHASSIS
The Ha mamatsu compact photomultiplier tube (PMT) used 'in current SRI FPD detectors has a recommended ope rating voltage of 300 volts. At no time is it necessary or advisable to operate this PMT tube at a voltage higher than this . Operation of the PMT tube at voltages higher than 300 volts will result in re duced PMT tube life, and a conseq uential loss of analysis time. The FPD tube voltage may be displayed and adjusted from the GC front control panel and the associated setpoint trimpot. The PMT tube is a consumable part, like septa and photoionization lamps, and is not covered by an SRI warranty. Any photomul tiplier tube warranty issues or concerns must be communicated directly to Hamamatsu. A conservative PMT drive voltage is inherently more beneficial than any perceived gain to be obtained at higher drive voltages. Replacement photomultiplier tubes are available for purchase from SRI Instruments and directly from Hamamatsu.
FPD exhaust vent tube
and PMT tube
DO NOT EXCEED 300 VOLTS
Compact
photomultiplier tube used in current
SRI FPD
detector design (side view, / shown with Ocring and Teflon seat on tube body)
./
'C:::J1E3
Top view of () P\ 1T robe , with _ .:: :. lens visible .
REV. 07-25-97
89 (of 550 ) 2006(-2016)
90
Chapter: DETECTORS Topic:
FPD Nonlinear Sulfur Resp onse
The FPD sulfur response curve is extremely nonlinear even over very small ranges (see diagram below). Thorough calibrations must be developed with multiple data points and limited range in order to accurately quantitate desired components. FPD 0, I ml of 92 ppm H,S Standard Response 1) Air at 100 mlImin
""
~dK
Helium carrier at 10 mlImin Column:3' PoraPak QS, Teflon tubing Gain on high FPD set at -400 V 10 minute, 60 degrees Celsius isothermal temperature program 8) Direc t on col umn injection of 0.1 ml of 92 ppm H,S 9) Expected area counts a minimum of
~
"~
~Il'm
I' 'I
II,
-
I'I
•••-S Hil L
..
150 mVsec
C;\Mi\.;.'JUAL\cHAPTER3\FPD:-fUlR DOC rni
.
1'64 mV Full Scale
3) 4) 5) 6) 7)
FPD 1 0 mI of 92 ppm H;::S Standard Response I) Air at 100 m1/min 2) Hydrogen at 30 ml/min each 3) He lium carrier at 10 ml/min 4) Column.S ' PoraPak QS, T eflon tubing 5) Gain on high 6) FPD set at -40 0 V 7) 10 minute, 60 degrees Celsius isothermal te mperature program 8) Direct on column injection of 1.0 mI of 92 ppmH,S 9) Expected area counts a minimum of 10000 mVsec
'" "
iuo.
2) Hydrogen at 30 mVrnin each
FPD 0 .5 ml 0[92 ppm HlS Standard Response 1) Air at 100 m1/min 2) Hydrogen at 30 ml/min each 3) Helium carrier at 10 ml/min 4) Column:3' Po raPak QS , Teflon tubing 5) Gain on high 6) FPD set at -400 V 7) 10 minute. 60 degrees Celsius isothermal temperature program 8) Direct on column injection of 0.5 ml of 92 ppmH2S 9) Expected area counts a minimum of 1500 mVsec
...'"
"",,",un H<"
~
I .,j..t U PPW f Pll
B" .
--Ait x! )-"'-9w';'; i - ,--
... -- ""'........
h·" 9:Z·:0~ l~ U IO
- -EA--- ->++l d ffil 111.GOll *'t
l:j " •
1.i l .. l.
.
.
~ 1024 mVFuIl Scale
, ', .,'~ ~Il'm
.....•
r \
Ii
.
·' 0Z.~ U
8134-1)·?:<-,,'22:< W<' mm»J\ } ; ' ·,%&@It·",HUD O.N O
r.
r~
....
.,.loIn_
--
'
,~
..
...
,
FTlPH1SJ. t
~""U""
~,+mI3
,
~f4U L r. COIO
4096 mY Full Scal e
""
1
~Il'm
II
i
,
·•.,un
rWt,.;:t , c. 0.1a0
,',. '
..., . , . ,
" ..4 ,,,
»@
.)" ii-lil
lEA
1C.OIlO
REV. 07. 23-96
90 (of 550 ) 2006(-2016)
91
[
Chapt~:
DETECTORS
Topic:
FPD - Expected Performance
]
FPD Expected Performance
FPD Flame Off Noise t) Air supply turned oft'
Hydrogen at 30 ml/min each Helium carrier at 10 mlImin Gain on high FPD set at -400 V 10 minute, 60 degrees Celsius isothermal temperature program 7) No injection 2) 3) 4) 5) 6)
if"""
..
0
,,;;,;;;;""",9,. ,
. . .. .
,
.
FPD Flame onNoise 1) Air at 100 ml/min 2) Hydrogen at 30 ml/min each 3) Helium carrier at 10 ml/min 4) Gain on high 5) FPD set at -400 V
6) 10 minute, 60 degrees Celsius isothermal
temperature program 7) No injection
FPD 0.1 ml of 9~pm HJ.S Standard Response I ) Air at 100 ml/min 2) Hydrogen at 30 ml/min each 3) Helium carrier at 10 mlImin 4) Column:3' PoraPak QS, Teflon tubing 5) Gain on high 6) FPD set at -400 V 7) 10 minute, 60 degrees Celsius isothermal
~.
'64 mV luU Scale
12J ~
f
temperature program
8) Direct on column injection of 0.1 ml of 92 ppm H,S 9) Expected area counts a minimum of
150 mVsec C:'.MANL'AL'CHAPTE.R3'fl'DEPDOCT\4:
1\
. . ... REY 07-23-96
91 (of 550 ) 2006(-2016)
92
Chap:tJ!r: FPD DETECTOR ,, -
Topic: "R~irofit ~i~i; p~i-g;d PMT tube h~~i~g~~;:-~ -
-,-
---
_ . _ ', _
•
- 'C- '
-"-
To prevent PhotoMultip lier Tubes { PMT ) fro m ma lfunctioning due to per meation of helium and/or hydrog en through the PMTs glass wi ndow. an airpurged PM T housing is Installed on FPO detectors manufactured after June 1998. Earl ier FPD detectors can be retrofitt ed with the purged PMT housing by ordering retrofit kit part # 8670-0084 . The FPO housing moun ts on the ex isting FPO detector in place of the un. purged housing. When installing the new housing , adjust the distance the hOUSing inse rts into the FPO bod y so that sufficient clearance will ex ist below the detector to allow the PMT tube to fit co mfortably. Only then snug up the brass ferru le w hich secures the new purged hous ing into the FPD body The new purged PMT housing has a tube wh ich directs a 10-3 0 mllmin flow of air across the face of the PMT tube. The air purge prevents helium and/or hy· drogen moecues from comJrlg into con tact with the PMT tub e's wi ndow. Th e purg e air is vented to atmos phere through a Shorter tube which is coi led to prevent light fro m reaching the PMT. The filter in
th e pu rged ho us ing is not remo v able. An add itiona l 1 /1 6~ brass bUlkhead fitting is installed in a 3/ 16- hole which must be drilled into the chassis alongside the exiSting 3 bulkhe ad fittings which sup. ply H2 and A ir to the FPD. The purge air tube will be connected to this 4th 1116- bulkhead fitting. -
_
On the inside of the GC chassi s, loca te the 1/16" stainless steel tube wh ich supplies air to the FPO cetect or. This tube acts as a rest rictor so that 3-4 PSI results in approximately 100 ml/m inute of air flow to the FPD flame. Install the 1/16 " brass tee on the upstream side of this restnctor tube. One leg of the tee will be con nected to the unrestric ted air supply, the second leg of the tee will be co nnected to the existing FPD restricto r tube. and the third leg of the tee will be con nected to a new restnetor tube ( 20" x .007 i.d. ) fo r tne air purge. The downstream side o f the purge resbictor is con nected to the underside of the brass bulkhead fitting described above . When the air supply is reg ulated to 3-4 psi. the air purg e should now at 1Q..30 mjtum. tk ca reful to route the stemless steel tube WNay from electronic or mechanical components wh ich cou ld be shorted out or dama ged by contact Insulate the tub ing with tace or Varglass siee vinq as necessary. Manl 40.pub
92 (of 550 ) 2006(-2016)
93
Chapter: FPO DETECTOR Topie.:Retrofit·of air purged PMT tube housing~L
.
_
••
_
_
__
, _
"-
;;'~.:
'"
Con tents of air purged PMT housing re trofit kit for FPD detector. SRI Part# 8670·0084.
1)
Purged PMT housing ( specify sulfur or phosphorus filter ) filter is not removable.
2)
1 /16~
brass tee
3)
11 1 6~
brass bulkhead fitting
4)
20· x _007 i.d . restnetor tUbing with va rglass insulation
5)
6- x .040 i.d. unrestricted tubing with varqrass msutaton for connecting the lee to the air supply
M anta Lpub
93 (of 550 ) 2006(-2016)
94
DETECTORS Helium Ionizati on Detector - HID
Overview The Helium Ionization Detector is a universal detector, responding to all molecules except neon. It requires
only heliumcarrierand make-up gas, and is sensitive to the low ppm range. The HID is particularlyuseful for volatile inorgan ics to which the FlO and other selective detectors will nor respo nd, like NOx , CO, CO: ' 0 :. N,. HS and H~ . It is a robust detector that. unlike the TeO. has no filaments to burn out. The SRI HID cdnsi;ts of a detector body. a collector electrode, an arc electrodeassembly.anda thcrmostaued heater block which can be heated to 3750(. In SRI GCs. the HID is mounted on the right-hand side ofthe Column Oven.
HID detector removed from GC and heater block CoJIecta -- ~ectt_
I
-
Pointed el ectrode
U.
~
Sam ple-laden carri er gas inlet
"
.
i~- ~ ~
~
;~ )< WIIldON
f~' ~_, -:i:: '- ,~ ' . - """=~= ...,;,.",. _. . :---- Makeu p
---:...0
-~
HIDdetector betwcan TCD e nd A D detectors an an SRr GC
Detector 00dy
Close-u p otthe same HID detector
Support brace-
-
-
!
.tJ
J. ,~
gas inlet
~s
Flat " ele ctrode -
--.
' ~
\
.
-
94 (of 550 ) 2006(-2016)
95
DETECTORS HID · Helium Ionizat ion Detecto r
Theory of Opera tion The SRI UfOdetector uses two electrodes which suppon a low current arc through thehelium make-up gas flow. The hel ium molecules betweenthe electrodes are elevated from ground state 10 form a helium plasma c loud. As the hel ium molecu les collap se back to ground sta te, they gi ve ofTa photon . The sample molecules
are ionized when they collide with these photons. All compounds having an ionization potentiallower than 17.7eV are ionized uponcontact with photons from the belium cloud. The ionized component molecules are then attracted to a collector electrode. amplified. and output to the PeakSimple data system.
Gro
Colleda electrode
electrode
A
~ uJ ' H
Sample-laden
carrier flOw
Photon s in the make-up gas stream Helium plasma dood
L9
q
-----~_····i--..········-r==""i;.,~··,~,. -,~·±;,j· '·l·::.:·=,·=,·=-=..·J·}.._'_.·_ . ·_. :-±~~- [3----<---" J.
" C' '
: 'keupgas
Purple ere
roo izatior. reacti on: photons aJl liding
_sample rrojeenes
Arc electrode
NOTE: If the arc electrode is covered with Tef1on™ (translucent) insulation, it should leave Imm of'its tip exposed . If the flat electrode is covered with ceramic (w hite) insulation, then the tip should be flush wi th the edgeofthc insulation sleeve. There should be a 1-2mm gap between the arc electrodes, and this gapshould be centered in the arc cross.
95 (of 550 ) 2006(-2016)
96
DETECTORS Heli um Ionization Detector - HID
Expected Performance :-Gl..-r-- - -.- - - - -
x-
- -. --. - - - - - -
.
--~.
, , a • -,I ~ bbl",'bbbNfrltr-
a=-.- 1Ie!11 ' D l6' g :J, §! '>". If !i:1 f?a' t
D~
Columns : 1m Mol. Sieve, 2m Hayeseo-D Carrier: Helium @ 10mU min HJD gain: HIGH HIDcurrer.t': 70
,
~
HID noise run
UllO ":\U 'le:>l' "'" _'IoU.T.C"WI
HID temp = 200"C
Ii(
r
~
s
~
Tem pe ratura Program: Hold Ramp 15.00 0.00
Initial 8O"C
ti
Final
8O'C
HID noise averages less than 100J;V from peak to peak
Cf~C6
Test A nalysis of 1cc 1000ppm ~: valve injedXxl CoIUm.1; 1m (3 ') Silica Ge l Carrier: He6um ~ 10mUrnin
HIDgain= HIGH HIDtemp =1 5O'C HID make-up = 29 psi @
»_.- - -
...
----
.
-~-_.
II
I'IB'"
"' . &: , , , • cq; bbfr..l[!l b ft. b ifr\ ~ ..., It I' "
1& V- ~ I!et> t::~W. ;~
eo f lllt PP
HI::
SlUOO
A: ~' ,
, ' ''00
".<;';l
.., ~ :<
40m U m in ~
tenoereaeeproqrarrt Inroaf
soc
22O'C
Hold
Ramp
1.CO
10.00
10.00
Fltal 22O'C
~ r g
0.00 22UC
r '~-
Results: Co mponent
0 200
Rele" hoo 0.766
M""""'"
t
oee
"',,'" Prow_
3.550 8.08 '3
9t.1an., Perrtarte
12 .850
16.9 50
He~C'ne
2D.800
tol:.11
A rIJa
3350.0970 1163. Hl€S 2~61 .0940
3001 6;>00
39$B.Xi'SO '849.9155 5023.::1105 2350 7.3185
-
~,
-
...x
i!!ElJ ux
~ ~
-
!!FlOJ>ME
If- A
-
- -
~
,
1\ ~
-
-
- ~
96 (of 550 ) 2006(-2016)
97
DETECTORS HID - He lium Ionization Detector
General Operating Procedure
1. Set the HID amplifier gain sw itch to HIGH for most app lications from the ppm level to 1%. Use the MEDIUM gain setting for slightly moreconcentratedsamples.
2. Set the helium make-up gas flow to 40mL'min. and thehelium carrier gas flow to 10mUmiD. Clean. high purity helium is best; moisture, air,and other contaminants can cause problems. 3. Set the HID temperature to 2000c. This temperature will help prevent moi sture accumu lation in tile detector 's arc assembl y.
4. Zero the data system signal. then switch ON the HID current; the switch is located on the Ge's front control panel under "DETECTOR PARA.\1ETERS." Set the HIDcurrentat l00 using the trimpot setpoint onthe top edge ofthe front contro l pan el.
5. When the 1110 is OFF and the signalzeroed, and the HID is then turned ON, the milliVolt offsetat HIGH gain setting should be 200-8OOmV. A higheroffset means more sensitivity, but less dynamic range. If theoffset is less than 200. the arc a nd ground electrodes are probably too close. 6. Observe the arc window; if you can see the purple arc betw een the ground and arc electrodes, proceed to step 7. Ifthe arc goes sideways to the detector body instead ofdo wn to the ground electrode. then the gap be tween the electrodes is too large. If you cann ot see the arc, A. Us e a mu ltimete r to check the voltage between the arc and ground ele ctrodes. With the HID current at 100, the voltage reading should be greater tha n 200VDC (our read ings average around 240YDC).
B. Look through the arc window at the arc and ground electrodes. If they appear to be touchin g, disconnect the red electrode lead wirethencheck the oontinuitybetweenthe electrodes using a multimctcr; the reading should be open or infinite.
C. Ifthe continuity between the electrodes is not open, re-gap the electrod es. 7. Let the milliVoltreading stabilize,then begin the analytical run.
97 (of 550 ) 2006(-2016)
98
DETECTORS Helium Ion izat ion Detector - HID
Clean ing the HID If your HID baseline seems noisy, try cleaning the electrodes following the steps below. Over time. the HlD
electrode" can develop a coating of soot, which can cause thearc to flicker o r c hange position. resu lting in sudden ba se line j umps. Green wire
,'-
.... Redwire
1. Urtclip the amplifier lead and slide it off the collector electrode. Uncl ip and remove the leads from the pomtcdand flat electrodes (note that the green wire is co n necte d to the pointed e le ctrode, and the red wire is
co nne c te d electrode).
to
the
fl at
2. Remove the the arc and
-
ground electrodes by loosenin g
th e liS" fittings th a t hold th e
electrodes in the arc cross.
J. Remove the collector electrode by loosening the 1/4" fitting that secures it in the detector body. 4. Use a piece of 100-400 grain sandpaper to clean the surface of the collector electrode and the point ofthe ground electrode. Sand the tip of the arc electrode so that it is flush against the ceram ic insulation. and 10 remove any residue. Whilehandlingthe electrodes, try to minimize hand contact by holding them \....ith a clean paper towel. 5. Remove any sanding re..idue from the electrodes using a paper towel optionally moistened with methanolor another quick-cvaporaung solvent.
I
Saew damp stop _:",,--:
6. Rep lace the electrodes and check for proper alignment. Th e collec tor electrode should ex tend ab out 4mm into the detec tor body. An existing scre w cl am p stop on the
Use the arc window
to check arc and grou nd electrode
positioning .
Il
collector electrode should allow replacement without readjustment, Should adj ustment be required, loosen
the screw clamp to position the
1-2mm gap -i:~~
e lectrode, then tighten it ro hold
the position. Topositionthe arc Arce.eccooe and ground electrodes. remove the arc cros s from the detector body by loosening th e ] /4" fining connecting the two parts of the detector (this fittine also secures the support brace). The ground and arc electrodes should have a gap of about l-Zmm (0.040-0.080") between them, with the gap centered in the arc cross. Hold me arc cross up to the light and verify the electrodes ' positions by looking through the arc window. Once the electrodesare positioned, tighten them securely with a wrench.
-.
98 (of 550 ) 2006(-2016)
99
[
Chapter:
]
DETECTORS CleaningtheHID Topic:
The Nitrogen I Phosphorus Detector, or NPD. as it is commonly referred to, is specified for the analysis of organic compounds containing nitrogen and/or phosphorus. The NPD detector is ideal for the analysis of pesticides and herbicides such as Parathiorrt, which contains nitrogen, phosphorus and sulfur. Minimum detectable quantities are in the 10 picograrn range for this compound.
In principle, when organic compounds containing either nitrogen or phosphorus are introduced into a hydrogen plasma induced around a saIt, charged particles or ions are generated. either by thermal ionization or oxidation. In the case of the NPD detector, ionization occurs as each sample component is eluted into the hydrogen plasma glowing around the NPD bead which is located directly at the exit of the analytical column. Ions freed in the plasma are then collected by a positively-charged collector electrode immediately adjacent to the gas plasma, and the electrical current produced by the passing of each component is carried to the electrometer/amplifier for processing and routing to the data system. The SRI NPD design exhibits extremely linear response. Hydrogen gas NPD ionization assembly Analytical column
Thermionic NPD bead
Sample-laden carrier gas exiting column into jet
Positively-charged collector electrode (carries signal to electrometer/amplifier) BASIC NITROGENIPHOSPHORUS DETEcrOR DIAGRAM
5 ppm concentrarioc of target component in nitrogen
D:\EP2DOCS\NPDDEr. EPD
The illustration at left shows a 5ppm concentration of a proprietary gasoline additive in nitrogen. The operation of the NPD detector was adjusted to permit display of the gasoline peaks immadiately preceding the internal standard and target peak. If the detector response was optimized, the selectivity of the derecror wonld have eliminated the gasoline peaks from the chromatogram. In this case. it was desireable to show the gasoline peaks, and the NPD H 2 gas and bead were adjusted according. REV.
~-94
99 (of 550 ) 2006(-2016)
100
Chapter:
D ETECTORS
Topi c:
Preparation of The Nitrogen-Phosphorus Detector For Operation
The majority of gas chromatographs manufactured by SRI Instru ments tha t offe r the Nitroge n-Phosphorus Detector option are equipped with a flame ionization detector as standard equipment. The Nitrogen-Phosphorus Detector is config ur ed for use by a conversion (hardware modification) to the Fill system in the field . The modification of the FID detector is minimal and may be performed in a matter of minutes . Reversion back to the standard Fill detector configuration may be performed as needed with out any major interruption to the throughput of analyses through the chromatograph. In some specific cases, the gas chromatograph is eq uipped with a permanent configura tion of the nitrogen-phosphorus detector (NPD). On such mood s, the hardware modifi cations indicated on this page are not applicable, as the detector is already co nfig ured and not converti ble.
330 ohm 114 wa lt NPD limiting resistor (EIA color coded ORANGE-QRAN GE-BROWN)
Location of NPD c urrent limiting resisto r inside of GC chassis (must be inse rted to operate N PD bead).
Loosen this nut to adjust the penetration pos ition of the FID jet with relation to the NPD bead as p reviously Illustrated
NPD bead inserted in FlO - NPD clel9Ctor body (pull FlO jet back to msort NPD bead)
21· of II W 0 .0 .• 0.005· 1.0 _5.S. tubiRi Flow should t... 3 rnIitnin or H, • 10 pr;i of p I1:Ml.lfe.
NPD hyd rogen gas flow restrictor (fo r redu cing hydro gen gas flow to proper level for NPD operation)
The thermionically-heated alkali bead used in the NPD detector must be positioned perpendicular to both the I detect or jet and the collector electrode on - . obc ;"""'~..od the lateral edg e of the hydrogen - air '- "~plioe~_ plasma generated by the application o f ""' electrical current. W'hen converting an FID This cap nut truly he detector to NPD operation. the FlD j et removed 10 view pos ition sho uld be repositioned back toward the ofj et tip. Jet should ~~ totaled 90 ~:"eeI1'mrn. column oven to permit proper insertion of protrude into flamc=port ~I for vialal flush with lead ing (left) the ?\''PD bead . The current is set as low as ""'rily edge of cap nut orifice possible while maintaining the plasma . N PD hydrogen restr jctor tubing must be inse rted Once these hardware mod ifications are in into hydrogen supply line to FID bod}' to ope rate place as indicated. adjust the NPD detector NPD detector as instructed on the previ ous page .
......
--.
""""'" ....,
D:I9SEP'2DOC\.>';PD02 .EPD
REV _01-29-9~
100 (of 550 ) 2006(-2016)
101
Chapter:
DETECTORS
Topic:
Operation Of The Nitrogen - Phosphorus (NPD) Detector }I,'PD bead pos iriooed in flameport
FlO jet pos ition , pulled back
The SRI design FID
from normal FlO position for use with NPDbead
detector converts quickly into a
nitrogen - phosphorus detector by the simple replacement of the FlD ignitor element with the Det ector inlet electrically-heated thermionic \ NPD bead element. The hydrogen flow is then manually reduced to between 1 and 7 mI. per minute by the installation of a flow re strictor prior to the FID detector :-;oac that the ~ hydrogen bulkhead fitting Fill air W )' hi s hec:n TOl&ICd (between I and 3 ml. per minute ~a rd 10 a hurimr&al is optimum) . With the heated pocitioa for iUIJWalI<>a }\ ' PD head installed directly in the FlD hydrogen po;rposes ocIy , carrier gas flow exiting the FID jet orifice, the sample components NPD de tector assembly (mod ified Fill de tector) are directed toward the area of the head, where any molecule containing a nitrogen or phosphorus group is prompted to release an electron in the hydrogen-air plasma generated by the bead. The liberated electron is attracted to the charged collector electrode and it creates a current that is delivered to the FlO electrometer for processing . Note that the AD jet should be relocated (pulled away) from the NPD bead and collector electrode, as illustrated, for proper operation. Return the A D jet to its original position when returning to FID operation.
-,
The nitrogen - phosphorus head is extremely selective. providing 10,000 times higher response to nitrogen - phosphorus compounds than to hydrocarbons. Whe n using the l\rpD detection method, nitrogen is the ca rrier gas of preference although helium carrier gas may be used . The bead must be operated with the minimum current required to maintain the hydrogen-air plasma. If more current
than necessary is applied. the detector will show greater sensitivity, but the life and subsequent sensitivity of the NPD bead will be greatly reduced. The NPD should only be operated with the 330 ohm NPD current-limiting resistor in place in the circuit. AT NO TIME should the NPD voltage be operated above 4.4 volts. Nitrogen - phosphorus compounds increase the current in the plasma as they collide with the surface of the thermionic heated alkali metal bead.
,I!
Hydrogen - air plasma created arou nd therm ion ically-heated NPD bead cl emen t
------L l '. J ~. " e1~trOO~i.:·::~·:~~~~.:.·.:. J~"PD
Fill collector
:: ::
!i FID jet
,.I
bead e1cmem
Curre nt to thermionic bead neces sary to maintai n gas plasma
===~~~ =
~ Electrons liberated from nitrogen > phos phorus sample components attracted by collector
i
d~liv~ring. sa mple
compon ents onto NPD bead
In order to operate the NPD detector. verify that the hydrogen flow rate is in the vicinity of 3 ml per minute by using a bubble flow meter capable of accurate measurement in that range. The hydrogen flow rate is normally maintained at 20 to 25 mI per minute. The air flow must be adjusted to approximately 80 ml per minute. This is much lower than the 250 - 300 ml per minute flow rate that
is typically used for flame ionization detector operation. D:~EPWOC'JI,l'DOI .i:1'D
REv . 01.J0.9S
101 (of 550 ) 2006(-2016)
102
OxygenalB Selective Detection for GC
OxygenalB Selective Detection for GC
ETHANOL In GASOLINE
CARBOXYLIC ACIDS
Negative tontzation on a cerarnIc TlD-1 . urfllca detects OxygenatM wtth good H IKtIvtty on. Hydroc:arbon-.
TJD· 1 d e te c ti on provides a simple
aoaly. i,
for
the
ETHANOL In GASOUNE
Ethanol additive in gasoIno. CWy a silgIe
AD
gas "'PP'ylN_> sumces for both GC camer and detector
121 nA fuIl..::ale
gases. Short analysis times can be . used
because Ethanol is easily detected' amidst many overlapping Hydrocarbon components . T1D-1
.-
T10 - 1 su rface ionIZation with an />Jr de....... gas gMls b;g slgna~
for Carboxyl ic Adds relative to oIher Oxygenates like Alcohols. n O-l detection indudes FonnicAeidwhldl ill: oot detected by an FlO. TID·1 detection is elso non-d••tructlve so componen t aromas can be sensed at the
detector exit. ~O
also detects Phenols, GIyco'-o and other
is also detectable
to ppm levels
Oxygena ted
,-
.._-
~ AaD INvnd. ~
.
._-
---.,--n~ _
•
A-
,- , .., -:""u::=,
•
,
•
I
compounds.
TRIHALOMETHANES
Pb-Sn- P-SI (Lead, Tin, Phosphorus, Silicon)
T1D-3 surhlce catalyzed negatlw Ionlzatlon procas
selective delBctlon with a DET Innovation
Selective Detection for GC
•
M
T
~
~.-
...
II
...
n~.
~"-
•
Lr""
J
•
•
HALOGENATES
.Q!:sanlcally-Fueled Remote FlO
response PCeeding 8 range of
A polanzer and Ion coIIectot located several c:entim8ters downstream of a flame jet detect long-lived Ion species that originate In a flame fueled
Vo la tile
detected with a _ o f l pgIsec. seleclMtyof 100,OCIO:1 vs. hydroc arbons. and li near
10,000 In sample weight Unlike other halogen detectors, TID-3 response to Br Is signl flcantly more than Cl. Detector ga8 may be Nitrogen or AIr with no requirement for ultra high purity . This detec:lDr Is mLlCh easier and less cosUy to operate and maintain than an 8ectrolytic
Conductivity Detector.
Sample anal)Dd: 140 pg nch: 1-eHCI, 2-CH~ 3-CHClBr, 4
RBIlIEFIl
by H.z - CH•• Air. Ionization from Hydrocarbon oombustion at the jet dissipates before reach ing the downstream collector. Detectivlty of 1 pglsec fof Pb.
-, g_.
Sn, P wiItI a selectivity 500,000:1 versus Carbon.
12
ppm
tetrabutytUn
ot
In
DETector Engineering & Technology, inc. 486 North Wiget Lane, Walnut Creek, CA 94598 USA ph: 925-937-4203, fx: 925-937-7581, www.det-gc.com
102 (of 550 ) 2006(-2016)
103
CHEMICAL DETECTION by DET featuring novel applications of the principles of THERMIONIC SURFACE IONIZATION and FLAME IONIZATION Selective Detecllon for GC
Selective Detection for GC
NPD • BEST N DETECTIVITY
PHOSPHORUS COMPOUNDS Very Big Signals with a New PTID
--lless than 70 femtograms Nlsec) The combnatioo of an
PMtickHi &le:
Agilent 6890 NPO and a DEl TID-4 ceramic
1-Mevlnph:>s (P)
....
600 femtograms Nicotine
T1D-4 in 6890 NPD
;on source ( ) provides stat8-of.the.. art N-&&I~ty fer trace detection of dnJgs of abuse, pesticides. expl osive s , en d
~
Nicotine
porllutants.
6890
T he
NPO hardware faatlres II concenbic cyl inder ion
source
j J.
COllectD~,
-
• I
lJ
electrode geometry for stntam-lr.ed gas
now
efficient
end
lon
coIIecIion. Simiar DET equipment Is available
for HP5890, Varian 3400-3800, and SRI 8610 GC models.
Tandem Thennlonlc Detection for GC
COCAINE· HEROIN
-
e_.....cc.
TAND.M
NPD and TIO·1 are two d ifferent modes of thermionic ionization.
N~,n~) 2 _ _• •
1oI_'n(H)
:O.OOA
_
...,
_
u
"..s_. "
T1O· '1oN. . . . . . .
..... 0,.,
-
Ceramic T1D-l surface operates at 4QO-60O"C in
f •••
~'I>A:~ r
! I
gas environment of Nitrogen or Air. TlD-1 is
. a
oon-destnJclive so it can combined In series with another detector like the NPD . Ceramic
NPO
,
2-Trifluralin (N)
3-Si'nazine (N) ....Methyl ParathiOn (NP)
2 pA f.s..
eurtece
operates at 6OCJ..8OO"C in \- an Ignned, dilute mix of Hydrogen in Air.
sample analyzed: NPD detects both Cocaine (C) and Hltroin (K). no.1 .ataets HwoIn and Heroin Impurity (U) Tandem comblnaUOn gJw•• imultan~1TIo·1 and NPD I lynm for ItCh NfIlphllnJKUon.
NPD detKtS both P Ind N. mo ct.tec;;ta only P algnals 10 UrMS b igger than the NPD.
wi"
..-no
" .......... r
,
A Phoaphoru.a Themlionic
Ionization Detector (PTIO) oombines su1'ace Ionization principles wiI;h high ftows of Hydrog en a nd Air for PI C seIec:tiviIy of 100.000:1. PIN selectiv ity of 1 00 : 1. detoctivity of 70 Ig P/sec. and a dynamic response range more than 100.000.
soe_
_ _ _Id_ _
i NPD
0.- ......' ...
•
•
r
•
1\
• Femtogram GC Detection · NITRO·COMPOUNDS like TNT, 2,4-Dinltrotoluene, DNPH-A1dehydes, Methyl Parathion, 4-Nltrophenol, etc. Unique TIO · 1 scrtsee ionization provides better selecli\lity than ECO and NPD. andneeds only AIr or N 2 as the detector g •• with n o requirement fo r high purity.
NPD (TlD-4)
.12pAU.
~-a~
T10-1 detoctlon I, an Inexpenslve mod ifICation of Agllent 6890 NPO equipm ent. DET NPDn"I[).1 equipment is also available to fit HP 5690.
T" ~
T10-1-Nttrogen .12 pA f.-.
Varian 3400-3800. and SR I 8610 GC mode ls.
TNT 0.2tI "ll
EXPLOSIVES Silmp": NPO
has • big r-.pon•• to RDX 4-Nftrctofuene. nO·1 has • much larger ....pons. to TNT. and
-
~:----
,
~
DETector Engineering & Technology, inc. 103 (of 550 ) 2006(-2016)
104
================
Dlnvited Paper'c.1
Recent Advances in Thermionic Ionization Detection for Gas Chromatography P.L. Patterson Detector Engineering & Technology, Inc .• 2212 Brampton Road , Walnut C reek , Cal ifornia 94598
Abstract Thefrrlionie Ionlutlon d.t.c;to~ .... mOS! wld.,y uMd tor the apedfle delKtlon of n1~lPrtoruIcompou~ In ga chromatography. n. ....... till5l mechanism of the.. deleeto... is. aurteee iortizatlon FOC'''N In which the key pallllmetltl'S Ire the work function of lh. thermionic emlslion 1lUr1-.. , the tempe""u'" of the trt.nnlonlc surfaee, and 1M compoaltlon of the gas env ironment In the namedlatll vicinity of the thermionic:: Il.Irf-ee. By .,stemltic verietlona of each of the. . three key paramelerw, th" tedlnlqu. of thermionic lon/Zatton detKtIon has ~n grNtl, expanded 10 eneompau I number of dlffel'Mll modes of response••U of which use similar ctetector hIIn:l. ••,. and -'ec:tfonlc: components.
prOCCSJ; was operative, it was possible 10 identify thr ee key operat ing parameters which ccmrot th e ionization pr oduced. Theseparametersare:: the: elecrrcnlc work function of the thermionic emission surface which is determined by the chemical composition of the surface; Ihe temperature of the thermionic surface; a nd the chemical composition o f t he gas environment immedialely surro undin g the therm ionic surface. The identification of these parameters has led to a clearer understanding of the complex chemistry active in NP detection, and has provided an important guide for expanding the applications of !hermionic ionization techniques. Through systematic: variations iD each of the key parameters, man y different modes of detector resp onse ha ve been achieved (3-6). Hence, the technique o f therm ionic ionization dereenon now correctly refers to a number ofOC detector responses which are related through the use of many common hardware and electronic components. This anic le reviews the present state of development of the members o f this unique group of detectors.
Intro duc tion Thermionicionization detectors (TID) an: C>Ql known in gas chromatography (GC) for their application to the specific detectio n of nitrogen (N) or phosphorus (P) compounds. All modern TIDs are essentially deriva tions of a basic desi&n first described by Kolb and Bi5choff(l) in 1974. The main component in th is type of detector ii an electrically-heated ther mionic emission source in the form of a bead or cylinder which is usuaUy composed o f an alkali-metal compo und impregnating a glass o r ceramic matrix. In the TID. the thermionic so urce is positioned so that sample compounds may impinge upon its sur face, a nd any ionizatio n produced is measured by an adjacen t collect o r electrode . Kclb and Bisdioff were the lim to repo rt thai a thermionic source compr ised of a Rb-sil icate glass bead produced ~ery specific NP respo nses when the bead was operated at high tem peratures in a gas enviro nment o f dilute H , in air. Since Ihe o riginal wo rk of Kolb an d Bilochoff . t he r e ha".. be
Types of Thermionic Emission Sources All commercially avai lable T IDs use thermionic emission sourc es formed aet:ordin , to one of the following four general methods: ( A ) homogeneous .ilkali_glass bead formed on a loop of bare platinum wire (I); ( 8 ) alkali salt aetivalor coated on a ceramic cylinder core containing an embedded heater coil (7); (C) homogenrous alkali-ceramic bead formed on 8 coil of nichrome heater wire (2,8,9); (D) mullipk: layers of cylindrically-shaped ceramic coatings, with a non-corrosive, electr ically-conducting sub-la yer of Niceram ic c:ompieteJy co vering a loo p of mcnrcme wire, and. a surface layer comprised o f alkali and/ or other additives in a c<'Tamic manix (S , I O). Thermionic sources represenling all four categories died above have been used in NP detectors available from different manufact urers. Generally. those sources formed from ceramic materials provide greater flexibility for varyin g the chemical compositio n of the source. Th is is beca use the ceram ic compositio ns are formulated and coated from a slurry at roo m tem perature (9), whcrCilS t he glll:i~ compo sitions are formed in
41 104 (of 550 ) 2006(-2016)
105
a process that proceeds lhrough a molten gla5s sta te {Ill. T he det ailed chemical compositions of the rmion ic emission so u rces arc usually rega rded U I,;onfiden tial pro prietar y informati o n by t he ma nufactu rer . Since the first alkal i-glass bead repor ted by I(olb and Bischo ff used Rb as tilt' alkali compound, the re existed for ma ny years a bel ief t hat Rb was an essent ial co m ponent for optimu m NP respo nses. However. in recent yea rs. NP detectors with state-of-the-art: performance specificatio ns have been report ed. in which Cs rat her than Rb is used ali the alkali componen t (5) . Also , anot her recent report (12) has described an NP detector whic h uses a LaB, fSiO, bead and no alkali additive. In accordance with a mechanism of surface ionizatio n prtvailing in t he TID, the most important characterist ic of the the rmio nic emission surface is its electronic work fun ction (i.e., the amount of energy requi red to em it a unit of elect rica l charge from the sur face ). Alkali-metal com pounds have been especiall y successful additives because they lower the work function o f the glass or cerami c matrix , thereby facilitating the emission of charged pa rt icles from the heated thermion ic surface. The ma themat ical relationsh ips between work runelion , surface tempera ture. and thermionic emission current have been d iscussed (2. 12). The development of multiple-layered, ceramic-coated therm ionic em ission sources has allowed examination of coatin gs of many different chemical compositions without the risk of materials in the surface layer corroding the heat er wire . In the search for expanded app lications for t hermionic ionization rechnlq ues, the basic task is to define a specific match of a thermionic sou rce type with an openu ing gas envi rc nrnent and a rang e of o perating source tempe ra tures. To dale, three c1ifferent chemical co mpos itions of thermionic sources have been shown (5,6) to have useful applications in differing modes of thermionic detection. These source com po sitions are shown in Table I. Data obtained using these three types o f thermionic emission sou rces are presented in the follo win g sections.
(D) an etecrro meter that meas ur es negative io niza tion currents arri .... ing at the co llecto r elect rode. T he TID hardware u sually mounts onto an FID-type det ector base th at is res ident o n a GC, so t hat IwO different de tecto r gases may be supplied in ad dition to Ihe GC effluent. ThereFore, changes in the modes o f detector res ponse that co rrespo nd to the schemat ics of F igures I th roug h 4 ar e accomplished by changes in the type o f th ermio nic so urce. ch a nges in the compo sition o f gases sup plied to t he detector, o r by changes in the o~rating temperat u re o f th e therm ionic surface. Most o f the TIDs availab le com mercially function by the collection o f negati ve ioniza tion ra ther than positive ionizat ion. In the discussion t ha t follow s, it will be sho wn that the concepts of negative ion chemist ry provide a logical pattern for corre lating the responses of the different modes of thermicmc detecti on. TlD-1-N 2 : Nltro/el ectroneg8thle specific respon..
The simplest mode o f thermio nic detect ion is represented by the schematic in Figure I . In th is mode, the lo w work function thermioni c so urce d esignat ed by the TID-I nomenclature is operated in a detector gas environment of N" Because the detector gases ar e inert, sample compounds interact directly with th e TID-I surface, which is typically hea ted to temperatures in the range of 400° to 6OO"'C. The ioniza tion process in this case is direct transfer o f negative charge from the TID-I surfa ce to
TJD-l -N 2 [A IR) THE RMIONIC
HfATiNG
SOURCE
CUUENT
IOCl;!~
SU....AC!
l l .AS VOLTAGE
K
~
Schematic illustrations of four differenl verstcn s of thermo ionic ionization det ection equ ipm ent are shown in Figur es I through 4 . Common components in each version are as follows: (A) an electncally-heated, therrmcnic/caralytic source con structed of mu ltiple layers of ceramic coalings; lB) a cylindrical couectcr electrode surrounding the cylindrically sha ped thermionic sou rce; (C) a source power supply that provides heating curr ent to heat t he source to typical temperatures o f 400'" to SOO"C. and a bias voltage 10 polarize the source structure at a negativ e voltage with respect to the collector;
r-,
r-,
.. , 1
, I
Table I. Thermionic Source Surface Layers
TIO-1 TlD·2
CFID
High
concent r~ion
Wort IIlnetion
Cs
l ow concentrallDn CslSf
lo. MeOium
HICJh
GAS
N,
(.4. I R)
,
/
V
,
!lECTROM!T! C
+
I,
~COtlf:CTOR
..... """'r:
I AllllltITt
f-'-
~
'-
+
·J-11
I"-
I
SlMIl'll' typ' "
r-
l-
~ \ I
1
I I
I
, I
I
SAMPLE
+
GAS 1
"2
(A"
I
Figure 1. Schemalie itluslrallon 01file detectIOn confiQUration for II\e thermiOniC crazancn modes Tl0-1-Nz ane TIO· l ·31r. ueiectcr gas 1cFIO·H, inlet line: detector gas 2:R[)·air inlet hne.
42 105 (of 550 ) 2006(-2016)
106
JOu,~
ct Chrornalograolloc seeeee . Vol. 2. , Fellruary 1986
the sample molecule. Consequently, Ihis mode o f response provides exceptionally high specificity and sen sitivi ty to many com pounds containing the nitro (NO.) functional group (5, 13), as as to certain other electronegative compounds te.e.. pentachlo rophenol, diazepam, and. methaqualone). This mode of detection is very sensitive to the detailed elecrrenegadvn y o f the sample's molecular srructure.as has been illustrated by the observation thai a larger signal is ob tained for th e z.a-tscmer of dinnroroluene in comparison to the 2,6·isomer (5). The TlD-I-N, mode is superior 10 a conventional NP detect or or an electron caprure detector (ECD) for detection of trace level nuro- ccmpounds such as nilro-PAH, nitro-explosi ves, nitropesticides (e.g. , parathion, methyl parathion) , nitro-drugs, nitroderivatives. For many nitro-compounds. the specificity vs. hydrocarbons is an astonishing 10", and detect ivity is in the 0.1· to I.Q-pg range (5).
wen
~.tlc "..,onae When the TID-I thennionic source is operated in an oxygenco ntaining gas environment rath er than one of N h specific respo nses to halogenated compounds are enhanced while responses to nitro-compounds are decreased somewhat (14). The TlD.I-air mode of cerecucn is generally nOI as sensinve as an ECD or HaU detector for chlorina ted compounds. but it provides halogen specificity .11 higher concentrations where ECD and Hall are saturated. Typical specificity is 10' and detecr:ivity
Tlo.1·elr: HetogttnInltm
is 0.1 to 1.0 ng. Thi s is an especially simple mod e of detecuon fo r ethyle ne dibrom ide (EDB) in the headspace vapo rs of food products. T1D-2·H2felr: Nltrogen/phosphorua specjflc rupon..
The schematic illustration o f Figure 2 represents the situation that prevails in an NP detecuoe mode. For this mode , H, and air gases are supp lied to the derectcr, and a therm ionic so urce of modera te work functi on TID-2 ) is operated hot enough ( 600~ 10 8OO C ) to cause t hermal/chem ical decom positio n o f the H, and 0 , gases. A cri tical parameter in this NP mode is the restriction of t he H z10 lo w flo..... s (e.g .• 3 to 6 m1/m in ) which are nOI su fficient 10 maintain a self-sustaining flame al the sampie co nd uit [i.e.• jet structure) depicted in Figure 2. Instead. a flame-like gaseous boundary layer is created in the immediate vicinilY of the nor therm ionic source. Since this boundary layer is very reactive chemically, sample compounds are decomposed by the active gas phase chemistry, and electronegative products of decomposition are selectively ionized by surface ionization o n the ther mio nic source. N or P compounds are ionized with especially high specificity by this process . An essenlial ccndiricn for the onset of NP detection is that the thermionic source mUSI be her enough to "ignite" the boundary layer chemistry. Under these ecncmcns, a thermionic so urce: o f moderate work Iunclio n provides me optimum compromue of sample response signal vs. detector background signal. A low work function therm-
u.e.•
C
CFID TI-IEIlMIONIC
H~ATlNG
SOURCE
HEATING
CURRENT
~
.OOT~
SUlfAC~ \
\
\nl-J;;:-j
lIAS
CArAlYT Ie
sousee
r-, r-, r---
-, r-, '
, f'.-
I .
,.-
"'-
I
r-, r-,
~COLLECTOIl:
I
U R~ACTIVE , ' ~~;A"" Y --~80UNDARY ,, , , , , , ,
I
tAYER
I
I
AI,
SAM'LE
+
f-
"
ElECT.Oio'En.
,
,
SAMPLE CQNOU I r
GAS 1
H,
FiQure 2. Scnemanc lIlUsIraton or II'Ie detectIOn c(lfl~ratl on lor ee nD·2~u or NP mOde of lI\erm,omc IOnI.utlon.
+
I, t--..."-..i I
'--- 1
I
+
r-, I r-, I' \,
I
;~ i"--
~
"- r-, I'
ELECn:OMUEIl:
G AS 1
liAS VO LTAO f
VOLTAGE
~, I
CUAUNT
+ ,
,, ,
AI,
\
•, ,
/
I
~CO~~ECTO.
~ FLAME
,,
'..
11-1, 0 . 0 1-1 1
I
SAMItLE
H,+
FiQure J, scnemaeeIllustration01 me cetectce connqurauon lor the catilylic flame loniu bon defector (CfID) mode of response,
43 106 (of 550 ) 2006(-2016)
107
io nic sou rce te. g., TID-I) operated undcT these conditions would pr oduce an I)\'Cf'o'helmingl) large backv ound signal. Conversely. :a nigh ....or k funct ion IhermiOnlCsou rce te .g., calalYtic flame io nizat ion detlXtion} opcrataj under these condiliolU ...o uld pr odu ce smaller NP signa ls and less spcri ficily than the moderat e wor k fun ction Ihermionk sourc e. Typi~ performance spea flca uoru fo r !'lip det ectors ar e dettct i\; (ies in th e rang e of 1 to 10 Pi. and speci ficity wi th respect 10 hydrocar bons in the ran ge o f 10" 10 10' . CFJD: UnI......... reapen.. 10 all organics
Figure) depicts a mode o f rn polUe achiev ed whe n t he H . flo w 10 lhe cereece is sufficien t 10 produce a true self-sustaining flame bu rning at the jet structu re. This mode of operaucn has been designaled (~) catalytic name ionization detection tCFIO ) because of Iu close similarilY 10 a convennonal FlO. The CFIO is essentially an FlO which bas been mod ifial. b y inserti ng an erect r t -ally-heared catalytic so urce comprised of a Ni-impreg · nated ceram ic in to Ihe cen ter of the act ive flame regio n. In thi s detection mode , the cata lytic source structure serves the th reefol d fun ction o f flame ignitor. flame polarizer , and catalytic co m bustion mod ifier / ther mionic surface ionizer . In the CFID . IwO types of ionization processes are active: gas phase Io nlza-
fTlD T",IMIO"'l IC
c--
~UICI
HIAT'"G
IOo:,~
l iAS
~
~
r-, r-,
~"
~
,
~CO LL IC T O A
, I
I
I
l L
,
,,
,
I
(UCTlO lllfTlA
T
.~
I
+ '--
-, l-
~OLrAGf
~
I
[
/\ I I
,
t
t--i
bas ic co ncepl (6) o f Ihis flame thermionic io nization d etect ion ( FTI D) mode is 10 burn sample compounds in a sd f-sU$lain ing H . /air flam e a:t a flame jC1. and 10 sdeC1ivtly re-ic ruze elec n onesative com bustion prod ucts by means of the th erm ioni c a ion iwion compo nents Ioca led downstream. In the large ph ysical separation between the flame and the t berrmcnc soutcc/colk<:1oc- ekc-.rode pr ov ides minim:al col lectIo n o f ioniu· lion prodlKC'd in the flam e, but eece uem ccnecnce of ioniza tio n predueed at t he healed surface of Ihe thermio nic so urce. A \'l aUll:i1iary ion·suppress "oilage can be applied to further prevenr ionizatio n produced in the l1&me from rraching the jonuation col lector. This mode of detecl.ton provides specific responses to compounds containing N Dr halogen al oms wirh a speci fid l)· o f 10' and de la:ti"ily o f 1.0 ng . The precombu5lion of samples in the name minimizes mterterences from sample matrices and pro vides more uniform respo nses independeOl of the or igin al molecular struct ure of the sample com pound. Both the low work function (TID- I) and moderate work funct ion (TID-21 thermi o nic sources have been used in this FTID con figu ration . FTIO· I pr ovides good responses to both nnrcjen and halo gen compo und s. whereas FTJD-2 respo nds besr fer halogen compo unds wilh suppr essed nitrogen response.
Remot. fl O: Otglno-Med apecltlc ,etPOlIM
C OllltUSllO" ,IO DUCU
b
FTID: Nilrogen/helogen ap.cltlc rnpon.. Figure 4 depicts a further detecucn mode in which the thermionic SOUKe and col jecrcr electrode scucrure are po5itioned well downstream of the active region of a self· s.u.sla ining flame. Tbe
mo,
CUlll"T
SUIfACI
tio n proc esses identica l to rbos e which occur in a co nventional FlO, a nd sur face ioni za tion processes at the cara lyric so urce srr c crur e which espec ially enhance the io nizat ion efficiency of man) nerercarcm comp(Xl nds l C'S peeiaJJ)' haJogcn31ed and pho$p ho rus compo unds l. li ke a conventio nal FlO, 1M magnitude of th e gas phase ionization is determ ined prunarily by the mallnn udes o f H, and ai r f1o ","s and the size o f t he jet Ori fice. so t ha t ad di tio nal erecuical hea ting o f th e C FlO source has lill ie effect on the gas phase ion izat ion. Howev er, the magnitudes ef io niza tie n produced by sur face processes althe CFIO source is slrongl)' d ependem o n Ihe electrical heal inl! of Ihe so urce . Hence , in ma ny cases. res ponse facto rs for hetero.alom co mpounds ca n be en hanced [ 0 be comparab le to hydrocarbons by a j udicious setecnen o f source healing current. For this C FID mode o f detecnon, th e thermio nic/catalYticso urer o f h ighest work runeucn is most suitable because Ihe na me heat wou ld ot herwise cause an excessive thermionic emt uicn background signal, The C F ID p ro vides detectivities in the Ie- to 1000pg ra nge for mOSI Otllan ic compounds.
~
~
I
H4MI I O N I U.'IUS VO ltAGE fL41111 C OIIIIUlr lON
FlQLre 4 Sl;."ltmibt: I~ of "'e CetectJOl'l conliQu~ br :tie llame tnem -
io'1lt oOmutlOl'I ceteC\Gl" (fTlO] moce 01.noo::mt
This mode of detect ion is a sim ple variati on of tht' FTID in which no dectri~ heating is suppli('(! to lhe thermionic source, and the ion-suppress " olla&e depicted in Fi,ure 4 is not applied. In t his case, Ihe th ermionic so urce serves merel)' as a pol arizer 10 d ri ve negative ions in th e Ila me e ffluent 10 the TID collector elecn ooe. The ionization sensed in this mode correspo nds to Ioni·lived nep.ti' e ions origi nall y produced in th e flam e. Because Or t he large sep arat ion between the flame and the TID ecneetcr electrode, the bulk of the hyd rocarbo n ionizalion produced by the f1a.me is diuipa led [i.e., pesitive-ne gative ion re:combinat ion or ne:utralization il l iii "' all su rface) befo re reaching the TID cel lector , HowC"\'er, certai n heteroato m corn po unds appear 10 com bust to negalive ion prod ucts which an elpecially sta ble: and IOr\&· lived . The: outsta nding demOlUlnolIon
44 107 (of 550 ) 2006(-2016)
108
o f this e rreer is the spec ific detectio n of lead compounds in gasoline. Since the thennio nic source is not electricall y-hea ted an d is nOI used as a source of sur face Ienizatja n, any Iypc of thennion ic so urce ma y be employed in Ihis mode .
Experimental The applications data pr ncnl ccl in l.tt.is report were cbcained with tquipO\CJ1t previously described (:1.6, 1") . All the data WU"C' obtained usq . Modd 3740 IPS dlronwOJrlpb (Varian Ass0ciates) equ ipped wilh either a TIO/CflD detector aucmbly mD-I-N .. TID-l -air , TID-2-H ,/ air. and CFID modes) or an FTIDfTlO dctC(1.or uscmbly (FriO and remOTe FlD modes ) (Dctcaor Eqineering and Tcdtnoio£Y). lbeT~ J . 110-2, aod CFID th ermio nic emission sources were also manufac1ured by Detector Enp nceri na aDd Tcdlnok>gy. as Wti the Mood 4000 detector current supp ly. NCfw ve ionization siIn.als from the detector were measured usina: lb.e differential dcctromctc:r (Varian ) in a neptive polarity c:onli, uratioa . The deta,;l.or uscm blies mounled ome lhe FlO-base on the GC. 50 lhat diffC'Cenl detector ,as environments were impkmemed by p1umbinl in lb.e a ppropriale ps throush the two gas tines lhal nonnally supp ly H, and air to Il1 n D. Typical ps now s su pp lied for differcm modes o f dctcaion are dewled in Table II . Al tM data pracnlcd in this report we-c obtaiDed. using glus colullUU. 6 ft x 'ti in. x 2 mm i.d., packed with eilbcl- 3" SP-2250, 3.,. SP-2JOO. or I'" SP-J240 DA on 1001120 Supc~ pon (Supclco) or 80/ 100 Chromosorb 102. The GC camer gas in all cases _ as N, al a flow rate of 30 ml/min. For complex. SImples like gasol ine. Ihe c:hromatoJrilphic: separation was InIc:nlionall y vcry poor in order 10 produce a c:hallcnging detector environ menl 10 demcnsrrare specificity of response: in the simultaneous presen ce o f many ovc:rlappinl compounds. Sample min ures thal were analyzed included a TSD test sample (nlleYel! of azcbenzene, methyl para thion. aDd malathion) (Varian); 8aJe.Ncutral. I sample (Supdco); phenol mix (Supeko); DCMA PCB mixture (Supdco); and nitro aromat ic mixt ur e (Supelco) di luted in rcaaent -aradc: benzene. GasoUne, cologne, and diesel fuel samples were analYU'd by direct injection oro.s 10 1.0 III amounu ootO the column. Ot her samples cnrcmaroiraphed were a 1"- v/v each mixture o f a.celonc and carbon tetrachlor ide in water ; and an 11"- vlv each mixture o f methylcnc chloride. n-C.. benzene, i.e.. toluene. n·C" p-Xylene, e-c,.. an d n-C , I • •
..
T.ble II. Typa l Gas Flo_ Supplied for EKh Mode ot Delectlon
....
10 mlimln Nt
T!D-l'i1r
10 mllmln ar
""IIWI HI
TJl).2·HJI_
3
""
2S """"" ..,
flI)
Ilemcte FlO
20 mlll!Wl
Hz
20 mll'rrwt Hz
Spec:ially form ulated test samples arc of len employed to demonstrate the specificity an d sensitivity of NP detectors . The data in Filu re :I ccrresp ,d to such a tesl sample comprised of 2.2 n8 each o f azo benttne (N) and methyl parathion (N .P) • .. ... nl of malalhion (P), and 4400 ng o f n-C.. in a so lvent of isc-cctane. The: data illustrate clearly the substantial di fferences in responw bet Wteft lWO differenl moon of thermio nic deteclion, and lhe 'VCr)' high specificity of th e TID-I -N. mode for sc:nsinl the NO . il"OUP in meth yl parar hioe, The io nization signals in both chromat orrlms are VCf)' iargto, indica lina eeeetiYiti es in lb.e PI and sub-PI r&nie. Filure 6 shows another comparison o f tile TlD-I · N. mode 'IS. the NP mode o f detcroon for a sample consislinJ o f 1:1 PI am ou nts o f lhe 2.4. and 2.6-isomen o f dinirrcrc luen e in a relaLively i,mpurc. reagent grade benzene solvenr, Fo r man y nitro-c:ompounds, the: TID-J-N, mode prcMdcs substaotial imprO'Vt'lDmts in spcdnd ty an d sensi tivity in comparison to Il1 l'o"P mode. HOW('VCf, the NP mode (Le ., TlD-2-H./m) provides mort' uni vc:rsal detection for all N
.~_
..........
_._
....
T1D-2-H
2
lAIR
AlQ
••
..,
,
TIO-l -Nt
Applications ·
TID -1 -N
2
60 mfJrrwt Nt
OJ"'- '" IiO niImil air
..
2lXI rnII1TWt fir
""""" '"
2lXI rnrnW! . .
S. Chl1lfTlltOlll'llms S/'Il7ftl; l'IIIO modes 01 respol"5e 10 iI f $ wnJ* tar;e CI:ll'Qf1tfIliOl1 of 11 IlydrocIftIon ICl ifIll tra:c tcnb g l aml:Jeltlene (AlO). /TIClftJl P¥Ill"«ln IMp}. and /TI~ lMAlI. 80m crroFig~
QlR!uln,j •
m.lIO\lrMl'l$
~
recorllltG
It tne 5.iITI! SCftSIlMIy
of 128 x to- « IITItIS'mV_
CoUnn; SP-2250. JSOtrlCfTTYl V 21 a-c.
108 (of 550 ) 2006(-2016)
109
non p rovid es very specific responses on ly to a nitro-co mpo und (2,6-dinitrow luene) and a chlorinated compound 0,3 ' -dichlcrcbenaidene). The lack of significant TID- I-N , response to nitrobenzene, bj ~(2-(;hloroethyl)cther, bis(2-ch loroisopropyl)eth er . or 4-b romophenyl_phenyl-elher demonstrates thar th e TI D- I-N, response depends o n how the electronega tive fu nctionali ties are bound up in the molecular structu re of th e sample compound . Wh en th e detecto r gas environment of the TID-} source is chan ged from N. to 0 ., the TID..I-Q . mod e pr ovides enhanced relative responses 10 the chlorinated compounds and a diminlshed re lative response to me nitr o-compound. The TlD- I-O. mod e continues to provide good discrimination in favor of chlorinated compounds with respect to hydrocarbons , while exhibiting some low level responses to ph thalate com pou nds. The T ID-2·H ,/air mode responds to all the N-eompou nds , with some small interferences from chlori nated compounds. The FTlD- 1 mode uses a TID.I source and provides respons es to all the nit rog en and halogen compounds in the sample. The FrID-2 mod e uses a TID-2 source which produces responses to the halogenated compounds bu t supp ressed responses to nitrogen compounds in comparison to FriO-I. This set of six ch romatograms provides a good illustration o f how the detector response can be varied through simple changes in the composition of the detecto r gas environment. Figure 8 shews chr omatograms of a sample miluurc consistins o f 75 og each of 2-ehlorophenol, 2-nitrophenol, phenol, 2,4-dimethlyphenol, and 2,4 dichlorophenol; zzs ng each of 2,4,6-I:ri.. chlorophenol , and 2,4-di nitrOpheno l; and 375 ng each of 4chlcro-ei-crescl. 4 ,6odiniuo-o-cresol, pentachlo rophenol, and 4-nitrophenol. The CFIO provides a relatively uniform response o f 0.004 coul /gC for all these compo unds , (Note: The flame lip orifice for these CFIO data was 0.062 In. instead of 0.03 1 in., which is normally used. The srna.llc:r orifice WiuaJly provides im proved sensitivities of approximately 0.01 co ul/gC. ) The CF ID data provide a good nlustrancn of a principal difference in the responses of a CFID vs. a conventional FlO. It is well known that con ventional FIDs provide relatively un ifonn
respo nse to ma ny hyd rocar bo n compounds. However , when hereroaroms, such as O. CI, or P, arc present in the sample compo unds, the FlO response is frequently signific a ntly lower tha n its response 10 hydroc ar bons. In contr as t, t he CFIO appears to yield more unifo rm response to all or ga nic compounds ir-
BASE NEUTR ALS C FI D
·• ·;• i· i ·, ·•·e !;• : •
: •
e
\ til,
J~
·,• • : ,• •a ,• i , ! ,••• '.·-." ·•• ·•,• !•· •:; • • , i •• !• I ! ;" ·• ·•a ,••• ~ :• a • , • ! : '. i ·• •• • · ~
.~
i
'.
!• i
•
i
e
•:·
i
i
!
!L_~AL_
T10-:Z-H:z/AIR 10 >1 10-9
SOU l CE
Hf Ar
15 P9
"
P IN I Tl 0 10 1 UE NE 5
I X
, ~
cr
'0. 12
200"9
16.0; 10- 10
2. 6 A
C I. ..
.
'
FTIO -2
' .A
F'gure 8 Chromatograms companng 1lle responses of me TID·I -N, mode and me TID-2·Hz/air (Np) mode to traces of dmilrotoluenes. Coh,lmn: SP·2100. t60° to 200"(; af tOOlmlfl.
Figure 7. Chromatograms showlIlg six different roodes 01 defeCtor response to a sample ot tese oeutral com~una~ . In ,ncreasmgorder 01 retention time. the components 01the sample are bls(2·chlofl;>etllyl)eIMr: bis(2·chlorcrsopro· pyl)e!tler: rntreOenzene: acenaphtnylene. d,melhyt~!llhalale : 2.li-lliMtotoh.iene: 4-bromophenyt·phenyt ether: d,.,,·blJty1 phthaiale: bts(2-ell'lylhexy1l phlhalate; 3. 3 '-d ,dlI0l'0ben ruline. and benzo(b)ll00ratlthene. Colum n: 5",·2250: loo"C. held lor 4 min, men 100" to 270 "C at 18°/mln.
46 109 (of 550 ) 2006(-2016)
110
respect!."t otwhelher thC')' ;are bydroarbon or hcl:croatom com pounds. Ibis is t he result of the additio nal ionization precess
that occurs at the sur face of ttlt catalytic ( FlO source, As anticipated, Ihe TID·I ·N, mode in Figure 8 provides high
• s •0 :• § 0
;;
0
·- •
•
·- •,
• 0• 0 •• • • 0
;;
0
0
0
•0 • ~i i i 0 0 ~ • ; ;, • ;; • ui •
0
•
i
, • 0
u
• •a i
;;
-•
% 0
••
~
"• • · -•
" -·
-
-
• ? 0• 0
u
0
§
0
0
•
u
•
%
•
o·
110-1 -N 2
Jlt10- 8A
, Jl
specifiCity and sensitivity [0 certain nitro - and polychlorinatedphenols. The responses 10 peTllachl orophenol-.nd a-nirrcphenol ar e more than 100 times largel" thim the (FlO responses to th ese com pounds. Comparinj: the respo nse of 4-nitrophenol and 2· niuo pbeno! &pin illustrates a signi flCllltly greater TI D-J · N, tes pcnse for the lscmer wilh the nitrO grou p loafed al the 4pcsnion in the molecuJe. In the third chro mat ogram in Figu re 8, the low work fun ction thermionic source (TID-I ) was operlled in a detect or gas environment comprised of appro~mately equal flows of N. and air. This illustrates thai the composition o f the ps environment is an additional pa rameter wltich can be used to suppress th e respo nse 10 cmain compoulMh whili: enhanci ng the r esponse to e t hers. The bottom chromatogram in Figun: 8 shows the analysis o f th e phenol umpk for the case where ~h eet ectcr pses I and 2 Me air . RespOnKS are DOW obtained fl)lr a ll the chlori na ted and nitre-pheno ls, with the dinitro-eompound.5 continuing to ~ye the dom inant responses. The rl::!iPOJ15tS 10 2-nitrophenol and 4-nitrophmol are now comparable. in contrast 10 the TID-I -N, response in which there was siplificanl preference for the nitr o If"OUp in the ~IOCltion vs. the 2-location. Fi&:ure 9 demonstrates the hiP specifJcity for lead a1k yls in
TIC -l -N /A IR 2
3
10- 8
J;
•
u,
,s • ;;
~
,:
·,••
~
2
:
• ;;
•
-~ ij!-• •· •
I:U .I O- 12
,, • ;; • 2
,• • ,• ,• s ;;·• -· • ·, •• ,"• •• ,• ·· • •~
2
' HIll UG UlAI
2 2
,.i •; -' ·•
H] - I O
i
••
•
· , · ,-· ; ·-
,• !• ,,
T1D-1 -AIR
•
.. ..- ·
• • r• • •• • • :e •• ; • • ,
8
· · ·. • ,-
.0
GASOLINE
"-'-
\.
2 5 6.1 0 . 12
·•,
'--.
~ I . Orornat~ ~ drl!el$1l mooesalOl!tKtCt restalSE' 10 pI'lerd sample conlil 'fIInq 2·Chloropn@nor: 2-l11rophenol; pnt1lol: 2.4-CIme'Jl)oIDllenol, 2.4'1lid'lloroptlenol: 2.4,&-tnC:hloropl'tenOl. 4-(lI loro-m-erm , 2.4-dlotlropllltl'lOl:
4.6-dHlII11HI-etl!'SOl: Pentachlorophenol: aM 4·l1ItToph.nol ,n croer ol ,nil ~lenbOtl l!me COlUmn: SP-1240. 100° 10 2100C at SO/min,
TEXACO IlEGULAR
ln crn~
SHel L SU ' 1Il UNLt "OI O
~ 2;6 ~·;o- I~
-
Fig~ re 9. Chromatograms ilustratmg the SQl!CIfic dmClQrl 01 lead IIk.,.s on gaSd1ine using the remote FlO, Oilla correspond to samples f;anclomly ollt3,ned Irl)ffl local oaSOIln! smions. Col~mn : SP-2100. 50° 10 230"C al 15°lm'n
47 110 (of 550 ) 2006(-2016)
111
gasoline provided by the rem ote FlO mode of detection. Previous ly. GC/ a lo mic abso rplion spect roscopy (AAS) instrumentation has been described for t he specific detection of lead alkyls in p.5 oline or ot her umples (IS). By comparison wilh AAS. the: eeeore FlO provides excellent sensitivity and speci fici lY. and is conuderably simpler and less expensive 10 o per a te . The: dau shown in Fi!urc: 9 ...ere obtained by dired injections o fO.s-.J amoul1U of the !UOliflCli onto a temperatureprogrammed, packed column . The remere flO mode o f detection has some: confi gur ation sim ilarities to a hydrOllC'n atmosphc:rc: flame: io nizatio n ceector (HMID). whicb has also been reported to provide: specific detection o f lead alk yts in psoIioe (16). Both the: renoee flO and HAFID UK" a conector electrode wc:U removed from the name jet structure. Howcya-, the: sirnals in the remote flO are: largest with ~ olYim-ri<:b name• • ~ the HAf"lD req uires a hydrOJa:a-rich at mosphere doped with silanc. Gasoline is a readily available, compla: mixture: o f organic co m pounds wh id! is a pc:cially wdJ scit ed to demonstratina th e different responses obtained in the family of thermionic deiecuce modes. r .t8urc: 10 shows mulliple modes o f analysis of a ~ of rquW pKltinc The chronwOlf&Phic separation was performed. 0Cl . packedcohunn 10 purposel y create !be demandiDa situation in which many ovulappiDg compo unds are peesent in me dc:leaor volume: at the: ume lime:. This srruanou is shown to be lhe cas. by the CAD response. When the same lasoline sample is chromatosnPhc:d usinl; me rcmcne: AD mode, seleecve rC5QOO.scs arc: obtained only for the five lead a1kyls . The remote: flO data in Fi.un: 10 were obtained with an FrIO eeeeeee assembly and a TID-Z source mounted on a Model 3700GC (Varian). The dctc:d:aconditions wee H, - 30, air _200 mlImin; mo headna: CWTmtto the TID-Z source: and name ion·supprcss voltaIC disconnected. The FrID-2 dala in FiiUle 10 correspond to the followinl chanled detector cOlIdi· uces: H. = 30. air = 80 mVmin; source beating ccrreu = J.2 A: and ion-supprcu voltaic on . This change in conditions produced an fTJ().Z response which WIIS 5dectivc: for the: haJo&cnatcd Ic:ad sc;avenacrs. ethylene: didUoride (EDe) and ethylene dfbromide IEDB). Figure 10 sho .... Ihal selecnve responses [0 EOB and tetraethyllead (TEL) arc also obtained ill the TID-I·air mode:, while the TID-I·N, mode provides responses to an lhe lead a1kyls and lead scavenaers. Note the wae TID- I-N, response to TEL in comparison to letramethyllead (TMLl. thereby illustratina a greater elcclroncptivc: character for the TEL molecular strucrure vs . TML. Note also Ihat precombustion of all samples in the name o f the remote FlO mode provides a more: unifonn response fo r all Ic:ad alkyls irrespective of their original molecular nruct ures . Fi!ure II iIIustralCS six differmt detector responses in the analysis of diesel fuel COIllaining a Irate: mrrc-compcuod additive . It is dear from ttlc: CFID chromatogram thai: there ate many un resolved compon ent peak s in this packed column anaIy1is. A primary objective: o f Ihis partilCUlar SCI o f analyses WIIS to der.nc: the best method of measuring the amount of thc: nitroco m pou nd added 10 such s amp les . ThenD-I-N , modeclc:arfy gives the: bt$t spedficity and r.tC~lIenl ,cnsitivity to the nitrOaddit ive . The other specific modes o f detect ion illustrate seteclive enhancemen t of other sesmems of this complex sample in addit ion 10 the !tilro-additive. For example. the dUSIC':" o f peab at la te retention lima in the TID-Z·H,/ air chr omato.riilfll undoubledly corresponds to OIher N-i:ompou nds in the sa mple:. Thc: two FTID-I dvottWOit.IlnS i1Juslrate thar the: Hs-air mroLIrc: ratio is a funhC'l" means o f significantly allerin. t he FrID re -
MULT I-MOOE
0'
AEGUL~R
~ N ~L Y S E S
GAS OLINE
REM OTE
FlO
••
••
....
•s
•
_
lEAD
• s • Al KYlS
F'T IO-2 HAL OGENATE D
"••
LEAD
SC AVE NGERS
•
•• TID-1-AIR
•
-
•
-• --••• •..... ...-• -"
;
F.gl6t 10 Orom ~ ~ mll'bple lI'OGe$ 01 deIrc10r rCSllOll5C 10 I ~ of ~ lUdell 08lI'1le. CoIurM and progrim ",me 15in F9Jre 9.
111 (of 550 ) 2006(-2016)
112
spouse. The mixture of 20 mJlmin H I> 100 ml/mi n air represents an oxygen-rich name, while the mixtu re of 35 mJl min H" 70 mllmin air is it hydro gen- rich na me. Generally, stoichiometric o r oxygen-rich names are the most useful for the FTI D. Figu re 12 sho ws multip le mode ana lyses o f a commercial bra nd of co logne. T hese sets of chromatogr ams illustrate the ad vantageo us use of the specific dete ction modes 10 enhance responses for tra ce fragr ance components in colognes. The T ID- I-N, mo de is especially useful because it is non-destructive. Ther efore, T ID- j·N, emits exhaust gases that are characterized
N I T RO
AO O I TlV E r- ) IN
D IE S EL
b)' distinctt y different fragrances th a t cha nge with time as t he vario us segments of the chroma tog ram elute. For the cologne shown, as well as fo r other bra nds that have been exa mined. t he set of chroma tog rams obtained fro m the different modes of thermio nic detection provide a character istic fingerpr int th at distinguis hes o ne brand fro m another. AJl the modes of derecuo n described in this ar ticle measure negative ioniza tio n currents. T he magmrudes of these curre nts arc very dependen t on the elecrmnegarive char acter of th e chemic al species adjacent to the heated ther mion ic source.
F U EL
• C, J 0
e FID 6A X 10 -
CH ANE L 1'1 0 • .5
aa •
9
,,
10 · '
•
• • tID-I- N2
• T I D -l -N
1
2
I
3 2 X 10- 11
,
IH
• 10 - 1 0
•
Ik
tiD-I -AIR
'"
T I D-2-H 2 / A I R
•
• r '.0 • •
10- 11
•
.512 X 10-11
•
TID -I - A lII:
, FTlO- 1
•• X
10 - 1 2
",
•
'0 10 0
AI,
•
FT I D -I
FTlO-1
",
I 2'
35
AIR 70
••
x 10- 12
Figwe 11 Chromatograms sOOwlng Oillerent cetencr reSPOl15eS ttl a samgle
otdiesel fUel contalnlllq it \race nnro-oompQlJl1d am~e ~11ied by the asteflsk , CO~1Tlfl
SP·2HXi. 90" 10 V O"C at l 0"/ml/l.
a,
•
10 - 11
•
. '
FiQ ure 12. Chromatograms shO""';nll muhrple modes 0' oetector -esocose to a brand 01 cologne randomly obtaIned. Column. SP·2100, 100" to 270"C at IS"/mrn.
•• 112 (of 550 ) 2006(-2016)
113
Figure 13 i1Iunrales ho .... the respo nse to a s ro up of polychlorina ted biphenyl (P CB) compounds changes with precombustion of Ihe compounds. The du.a obtained with a T1D- 2 source in an air ewirceeem exhibit lar ge differences in response between the differcnt PCB compounds. similar 10 the known wracteriilics of an ECD. The FTI£>.2 da ta sho ... that the precombustion of th e PCBs yield negativc io niza tion currents. ....hich are larger in magn itudc as .... ell as more unifo rm per Cl at om, In t his caseof Peas, precomb ustion improYeS the detectab ility by producing chemical species more electronqative than th e original compounds. For ot her compo und types, precombustion sometimes causes the opposite erfect of prod ucing co mbcsuen products which are not as electronegative as the original compound. The data in Filu re 14 provide an illustra tio n of the reta uve electr on eprivtty o f phen ol compounds before (TID-I -air) and d"ter (FTlD-l) combustion. The FTlD-1 mode o f operation can
,
be easily con vened 10 Ihe T IO -I-&ir modc by simp ly turning off t he H. fuel 10 the fTtD flame . Figur e 14 shows thai the FTI O- I mode produces ~ much more uniform response for all t he cnlcro- md nilrophenols o f Ihis s.amp le. bu r the absolute magni t udes of FriO respo nse for th e diaitrcphencls, pen . tac hlorophenol. and 4-nitrophenol are subslan tiaUl' lower than the T ID-l-air reapcnse to these compounds. Figu re IS ilI u~r.r C5'he use of the T ID- I-air mode to detecr EOD in food products. A simple headspace technique was used for th e data. One of the advant a ges of the T ID- I-air mod e is Ih at it is insensitiv e to th e large air component in the injectio n hea ds pace vapors, Hence , all chromalograph ic peaks that are obtained may be: at tr ibuted to vapors emanating from the food product itself, In addi tion to EDB. Ihis cake mix a mple provided other WIC TID-l-.a.ir signab, thereby sugges tinr the presence of oth Ct" halogenat ed or e1cetronClatiYe constitue nts that may be of int eresl: in such produeu. With lo better optimization of GC colum n for lbe EDB 5q)at3.lion. Ihis a mp le technique sho uld be eapable of EDB detection in tbe I 10 10 ppb range o f concentration in thc food product. FilUTC 16 illustn. tn dat ODed ifrCt"e:nce between a CF JD and an flO is Ihal the CFID will provide silnificant respo nses 10 halogenated compounds. fi gure 17 furth er shows that the CAD
F Tl D -2
,
512 x
3. 10- 10 A
'flO
to - , 2
s••
s ;; • • ;z sz _, 0z •
,.
, • z ;; ;; z •, · · z s · • • · ·••• ·••• .z• •-• •• -• ,z ••·• ;• • • •• •• • • • , ii•i i ,
2
0;
0
0
• ••
-
0
~
0
ii
~
0
0
• .'· :• ••s • .'• ~.' • ........." 0
0
~~
-
~
0
0
0
~ .~
L..
" sz
• •0•
z
•
L-
• ,
FT IO _ 1
256 x 10- 12
S
T I D·2-A IR 14 a 5
t o- 1 2 , e
,
• •
II 110 -I-AIR 12 1
figUrl! 13 ClJromalOOrams illuSlrating detector ICSPonseS obtilintd betore mD--2·ul ~ al!tf lFTlD--2) comtlUstiOO 01 pOyd1IorlNltdlJphenyI compounds. pca peak identifications: 1. 1000 ng 2-etllofo·, 2_ 1000 no 3.3··c1lChloro-. 3_ 100 ng 2.4.5-tl'ICI'icJr&. ""00 rog 22'.4... ··lttI'~rt)- . 5_ 10009 2.3'.4.5'. 6-oentaetlloro-. 6=100 IICJ 21'.3,3·,6.&'·hex;K:IIl)'ObftlenYl. CcUnn: SP·22S0. 200" to 27C"C .II 10 "ltTWI
X. 10. 9
• F'Qurl! 14. Chroma1ll9rllntS iIlaslrating aetcetor responses oblillOed bercre lTll). l ·ullirld sner (FTI).11 com~ 01pI1cnol compoundS. seree , columtl. .1nc1 program WCfC rne ~ as Il'1 F'9urt II
50 113 (of 550 ) 2006(-2016)
114 Jou rniIJ ot Chromatogr apr"c SCience. VOl. 2~ . February 1986
response to halogenated compo unds can be selectively enhan ced by increasing the source heating current, while the CFID respo nses 10 hydroca rbo ns remain unc hanged. Cons equ ently . by judiciousl y adjusting the source heating curr ent , t he CFID response to halOjlen3ted and some other heeroarom com pounds can be:' tuned to yield about the same response factor as o btained for hydrocer bc ns,
T he development s of thermionic techniq ues in GC have also spa wned applica tions o f the rechnotogv in liq uid chrc marogt aphy cerecncn (17), thin la}er chromatography ( 18). and mass spectr ometr y ion so urces (19). Since there remai n [0 be: studied many differen t combinations of thermion ic sou rce compositions, thermi onic so urce tempera tures. and gas environment cc mposincns, it is proba ble that the techno logy will continue to evo lve in coming year s.
Summary
.-
The preceding data have demonstrated that thermionic ionization techniques and equipment have appl ications in gas chro matography that go well beyon d t he usual NP det ection, such as that ofTID-2-H ,/ air. To achie ve the best possible signalto-noise ratio and spec ificity for each mode of detection. the specific chemical composition o f the thermio nic emission SO~ needs to be matched with the temperature and gas phase environmen t in which the so urce is operated. From their extensive use in NP detect ion, ther mionic io nization detectors are known 10 often exhibit decreasing sensitivity with increasing ope rat ing time as a resulr of depletion o f the thermionic SOUI"«' activity. Co nsequently. the:the:nnionic source usually needs to be replaced at periodic intervals. O f the different modes o f detection described in this report, the: NP mode is the most demanding with regard to the operating life o f the thermionic source. Generally. in modes of detection {e.g •• TlD-I ·N,) where: the operating temperature is lower and the gas environment is less reactive. the thermio nic sources maintain their responses over longer periods o f tim e. For aU modes of detection. a practical guideline for achieving the longest possible source lifetime is to operate the thermionic source just hot eno ugh to achieve rhe response required.
c F ID
.'o
I
o
-1 Figure 16 . Com parison 01CFIOand FlO responses 10 a wale!"
CFIO
3x10- 8A
11 % v sv
EACH
..
''' '' •• - I'" ~ ...DDrD
"
%
V
COMPOUND
..
••
HE" T
_.• . v, I•
v •
,n o o.
cornilin·
12nOC.
• •,,,_11. c .. k!
samp~
ing ac:el00e aIltl cartlO" tetrachlonae. Column: ClJromosorll 102. Isothermal
•z • "z
wll
''0
. •., z
v
0
v• e•
·z ··• •
. • 0
v
.•" V
•
~
. .. r..
'" ., . 0 "( '
J
I
, ''' J ! , I
t
F'glif! 15. Example of TID-l ·3/I" applJcalion todetemuneEDB irl cake mlX. Sample: heaoSll ac~ vapors from 0 7 gm Duncan H;nes Deluxe YellowCalle M" in a sealed
2.ml VIal Sampling proceoure: neal sealed samplt' vial 10 12Q"C: e:ctra ~t 200
,,11lea
tempCfature program.
C~ u mn:
SP·2100. 40" to 110"C at It)°lrrnn
LJUL.--J'--
FigUle 17. ccn oaoscn 01CFIO responses to sample of mc:tnyte1le chlonde and vanous hydrocartlOtls al two differ enl magnitooes or hea~n\l currenllO 111. catalytic source. Column: $P·2100. 40° to 1800(; at 100 1mm.
51 114 (of 550 ) 2006(-2016)
115
References
source lor alka li flam. lonl zauon detectorS. J. Chromatogr. SCi.
16: 8 (1978). 1. 8 . Koltl and J. BisehOff. A new design of a thermiOnic nitrogen and pnosllhorus a.lector 101" GC. J. CIlromatogr. SCi. 12: 625
(19 7" ). 2 . P .L . Plnel'$On. Selectivt responses or a flameless ttHtrmiOnlC detector. J. Chromtltogr. 167: 381 (1978). 3. B. Kolb. M. Auer. and P. Pospisi. Reaction mec1'lanlsm in all ionizatIOn ae!eClOr With 1UnaD'&!letectMty tor carbon, nitrogen
and Pf'IOlIPf'IOrus. J . Chromatogr. Sci. 15: 53 (19m • . P.L Panerson. AA Gmt.,. a'lCI C. Onvveras. An ~ thefm. ionic IOI'IIZabOn ~ tor gu clTorl'lalcgJaph. J. OIn:ImlIkI!iJr. SCi. 20: 97 (1982) . 5. P.L Panerson. New- uses at 'lNrmIOI'IiC IOI'liZaIiOn Ol!ltllCl:on WI gas chrorn.llography. Chrometographia 11: 107 (1962). e . P.L. Pan~ . A name tl'lenniOnC iorliZ:ation lMtectol" lor GC. Presented a1 thlI Pmsburgh Conknnt:e on ~ Chemmry and AQQlied $pect~. AtIaIltic: City. JliJ. 1oI...-ch 19&4. Abstrae1 No. 372. 7. C.H . Burgeft, O.H. Smith. and H.8 . 8e",e. The nitrogenphc5phau,(leledDr.-cla~in gas~.
J. ChromtllOgf. 134: 57 (11il77). 8 P .L P 0IJt8f'SOl'l aI'ld RL Hc.e. Thermionic nrtrogen-pho5pho ctetec1lOf'l wrtl'I an aJkaI.-ram1C bud. J. Cllromarogr. sa. 15: 275 (' 1iI78). 9 . P.L . PanfHSOn. ThetmlotllC det.etor. U.S. Patent ".203.726. (1980)_ 10. P.L Pmerson. ThermioniC detector with mu~ layered ionizab on sou rce . U .S . Patenr 4.524.047. (1985). 11 _R . G.--n~ . J . MUlIfi , ..d W . Aue. It p,lre rubidium/quartz
12 . T. F'uji i atla M. k imolO. Tt!ermiomc ioni.z:ation a81~"'" with 11lIIIhAnvm hexaOOncleJSlllCOn diOxlOe 1I'lel'l'l'lionIC emrtlet matenal tor 9U ch roml log raphy_ AmJ I. Chem. 57 : 490 ( 1985 ). 13. C .M . WMe.A. RobOaI.Jr.• ancl R.M. Hoes. EvaluatlOn~a thetmIOnIC: ionlLallon clet.ClOt lo r ""raled polycyclic aromatic hydro-
caroons. AnaJ. Chii'm. 5&: 23211964). 14 . P.L . Palt.,son . New mOdes of response for thwmionic eereetors in GC. PnrsenteCl at the Pittsburgh Cottetence on Anatyticaf Cn.mistry and AQQtiect Spectroscopy. AtIan1lC City. NJ . March 1983. Abstract: No . 423. 15. V.K. ChaI.l, P.T.S. Wong. G.A.~. and J .L. Du,,". 0.1...• mmahOn 01 dialkyllead. lnaIkt'k-1 _aallr.yllead and lead fll) compouncls WI ledlmenl and tllOlogiCal samples. Anal. Chem. 56; 271 (19&4). 1&. .... D. DuPuIS and H.H . HI.,.Jr. AneIysIs 01 gasoline tor antlknodl
agenl5.,;tIl a hyaog«l Hmo5pherI 1~.lCrililbon det8C1Ol". Anal. Chern. 51: 292 (1979). 17 . V.I. McGvH ln and 101 . NoYotny. Thermionic: detection i n tnIctOC01l.WTln ~Cl chromalography . Anal. Chem. 55: 2296 (1983) 18 . P.L Pallerson. A speafic: 0BI8dOr b nrlrogen ancl halogen c0mpoundS WI n.c on COIled quartz: rodS . ~ 20: 503 ('985). 11i1. O. BorrOck. J.D. p..,ksIon.. and J . A.bon. F'ota5L.m ion d'IfIrnICaI ioniution andOlhef \,IS8I of an aIIaII thermiOniC emittw in mass SpeClJ'l)melry. ArIM. CMrn. S l: 3!Hi119&4). ""~I receiYed Odl:lbet 2. 1985 ; revis>on reclff«l NO\"efT1ber 18 . 1985.
52 115 (of 550 ) 2006(-2016)
116
DETECTORS Photo Ionization Detecto r - PIO
\ _ O/H
Overview ThePhoto Ionization Detector(pID) respondstoallmolecules whose ionization
f
" C- H \ c=c /
H- C
potential is below IO.6eV, including aromatics and molecules wi th carbon double bonds. The Pill is nonde structive. so the sample can berouted through the PIO and on to other detectors. It is oft en used in series with the Fro an d / or D ELCD . Pill detection limits for aromatics are in the ppb rarige: purge and trap concentration Benzene of the sample can lower det ection limits to the pp t range. Because of its selective sensitivity.use ofthe Pro is mandated in several EPAmethods. The PID detector cons ists ofa 10.6electron volt (eV) UV lamp mounted on a thermostaned, low-volume (IOO!lL), flow-through cell. The tem perature is adjus table frOI:1 ambient to 25O"C. Three detector gain levels (lOW, ~EDIUM and HIGH) are provided for a wide range of sample concentrations. The PID lamp is held in place by a spring-loaded plate . so tha t the lamp may be quickly removed for cleaning and replacedwithout any special tools. The Pill can run on air carrier for gesless operation. orfo r stream monitoring applications wherethe entire stream ofsample isdirected through the detector (no column is used).
/
\
110 PJD
star-o-etcne oetector
, ~;.-- PID in series with a DE LCD
ancenr rncn an SRI 861 0C
eeesere
.'...
Spring-loaded retaining plate
100lJl cetect or cell
I
(th e area i'1 the ce-ter ofthe Teflonn< sear ring}
-
High voltage bane! in bl ack plasti c hood over lamp ercoe ring ;
. ~
I
116 (of 550 ) 2006(-2016)
117
DETECTORS Photo Io nization Detector - PIO
Theory of Op eration 10.6eV PIO Lamp (SRI Part # 8670-1242)
ceecoe -
base
Partial PID Assembly Ex ploded View
The SRIPlDdesignuses a IO.6eVlamp with a high voltagepower supply, Sample laden carrier gasflows from the analytical col umn into
the PID sample inlet, where it is stream ed through a l 00J.lL flow-through cell. When sample molecules flow into the cell, they are bombarded by the UV light beam. Molecules with an ionization potentia l lower than IO.6eV release an ion when struck by th e ultravio let photons. These ions are attracted to a collector electrode, then sent to the amplifier to produ ce an analog signal. which is acq uired by the PeekSimpledata system. Unlike otherPill designs thaIheal. theentire lamp. only the lamp windo w ofthe SRl PIO is heated . This results in a longer lamp life for SRI PID detectors.
rezoo.....seal (SR I part # ' "
867o-1244)
Teflon'" seer
f errule
sarrce-eoeo carr ier g as
colu:nn oven i:lIet (fromthe on 861 0 310 GC's, or t h e he a te d
Analytical
ccaem
&--->::>
tra nsfer me en
110models l
Spri ng-loaded retainin g plate
detector cell
1
=
Simplif ied PIO Oaeratlcne ! Diagram
1 00 ~ l PI D
~:
'\...-
NOTE : The end of Ir-e coumn must be visible in tne dete ctor eel : when th e PIO lamp is rem ov ed from '!he retaining plate. It should be app-oxirnate!y 1mrn from the lamp wir:c:!ow when the PIO la:r.p is in place.
,. ~~t~~~~~ij~~~ :;7""
, 'I
Y £/'
,
_ ······· ·······
11- \1\ =' \, , eecrcoe
Th e PIO ceil effluent flows around the
I to tbe
col:Jmn back to the PID sar;.pie gas o:..lIet wn:c."I is ccemected to tte next detec t or i n ser ies or ve nted to
I collector
at:":lOS!'h ere i,,sid e tr-e column OIIen
I II :Ii
1=
:"'_--1_ " _,
r \ A \\
support unon
\~
/fIT
ColJectoc eiececce
I n CoIumn ~:"I ":2:1 -- L Heater b~ot:k.
"' ~'£ 7' r""''' r·I''~
.
i
,\
coaector
\~ \
electrode
\
CeI' _ " e ctor e.ectrcoe si;r.al ceo'e
Hig h volta ge band il":s:ce tr.e black crasuc hood (mu st make con tact w ;th th e la mp a node fo r P IO
operation : do net adj ust
unlessthe man GC po....'er is turned OFF) PIO high vo!tage
\-\- Ie""
117 (of 550 ) 2006(-2016)
118
DETECTORS Photo Ionization Detector - PtD
Expected Performan ce PJP"ol.N l
'"
t _ !'-
-
-
C ~5iiI. :.5 i'i ~ · LCI~ ":
, '
-~
I 2
"SEl
•
!
~ f!', f'!l fr.
!;r,. b I» /:0.1;y.. fr.. ..., <;- I h ,
. mD Ef l«. .CO:'!
PID Noise Run
,
CoIumr.: 15tl'l MXT-VOL Carrier; Hef.um@ 1frr. Um ir. , PiD gain: LOW PiD temp: 15O"C p rD carreot; 70
•s P!D n ois e averages less than SO}JV from peak t o pea k
-1.Jel1
I::ili] ....... """"" 11 w;,
-
--
,,_.
- " ~ :::r
- :!::EF.J ,~
PID STEX An alys is (in series with FlO and DELCO) Sample. 1iJL 100ppm STEX plus Column: 15m MXT-VOL
! fjjIo
l.
_
~
_
,' 0'" "..,..1... . ·".,' ..
Gamer. Helium @10 mLslm;n
~ b bfr;. ! b b b f!', ! fr\ fA ..., * lb l
PID ga in: LOW PIDtar.cp: 15O"C P ID
current
7C
"remceaase ~ram: If' itia! Hoic: Rarr.;:l F ine!! 4O"C 2.00 15.00 24O"C 24O"C 10.00 0.00 24O"'C
J- it -
Results: Co"p:)t ~
;; el!!!'t on
Sanze re T:::E
2A1S 3.06 5 4 .600
TclOle~ e
Ar ez. 3!3.~54J
2.31.51 20 309.2120
FGE
s.eas
Elh~ :
Berzeroe 6.70n
285.0000
O:':!1e Xylene 7.383 6roc'!lct"= 1.5 50
298.9190
'''''
11
2 16.62 3 0
559460 1711.J 5SC
L"~ " ~ " ~ "~ "~:::::.
A II, ~_~~
~~'-'
118 (of 550 ) 2006(-2016)
119
DETECTORS Photo Ionization Detector· PID
.
General Operating Procedure The capillary column enters the PID cell from inside the column e ven through the bulkhead fitting in the insulated oven well. The coiumnmay be installed .....' ith the lamp in place. Insert thecapillarycohzna iato the PID detector inlet until the column stops at the lam p window inside the Plf) cell, then pull it back about imm from the lamp window. Tighten the 1/8" nut with the graphite ferrule at the PID inlet to securethe column in pla ce. The collector electrode is positioned at the factory end should not touch the column under normal
circumstances.
1. Always ensure that the black plastic hood is in place on the lamp prior to operating me PID detector. The hood contains the high voltage band which is maintained ala high potential;never anempt to adjust the PID high voltage band unless the main GC power is turned off. 2. TumON thc GC. Turn Ol\ tbe PID lampcurrent with the flip swi tch 00 the GC 's front control panel.
The vcet iight is v eo e t-e-e w."le:'l lhe lam;>is on
3. Set Ute PID current to 70 (= O.70ma) wi th tile rrimpot se tpoin t on the rep edge ofthe GC '~ front control panel. Use the flat blade scr ewdriver provided with yo ur G C to adjust th e trim pot. The lamp should emit a violet-colored light visible do.. . . n the center of the tube 4. Confirm that th e lamp is operating at or near O.7Oma by pressing th e PID detector ACT UA L display button on the fron t control panel. The scasi ti..-ity of the lamp increases proportionally to the current applied, but operation at higher currents reduce s lamp life. The PID operating current range is 70· j 25. A setting o£1 0 should provide the user with sufficient sensitivityand lamp durability. Most PIDepplicaticas carl be performed using LOW gain. 5. Set the PID temperature to 1500c . 6. On ce the detector bas reached tem perature and the signa l appe ars stable, sample may be introduced.
!\OTE: Lamps arc aconsumable pertuf'the PID detector. It is recommended :'0 huve n :;pnre lcmp .rv eilaale ifcritic al ana lyses are being performed cr rercote f:eld sites . Spare end replac ement lO.6eV Pill lamps are
available unde-r SRI part number 8670· 1242. Teflon seals arc avai'able under SRI pll:: number 8670-1244.
119 (of 550 ) 2006(-2016)
120
DETECTORS Photo Ionization Oetector • PIO Troubleshooting an d Maintenance Cleaning the ? ID Lamp Tr.ePID lamp window
Overtime, during normal operation. G film ofcontaminants will condense on the PID 1arr.p wind ow. Typically, this film is a result of stationary phase column bleed. To minimize contaminant condensat ion and thus lamp window cleaning, avoidheating the column any higher than abso lutel y neces sary. C ontaminant condensation can bloc k
the photons, reducing lamp emissions and sensitivity. Therefore, the Pill lamp window
must be cleaned when an appreciable change in sensitivity has been observed by the op erator. Beca use the response change resu lting from cleaning the lamp window usually requires detectorrecalibrarion, frequentcleaningis not recommended. 1. Tum the PID current OFF w ith the switch on theGC's front control panel. Turn the (Ie Off am! let the PID detector assem bly cool enough to touch it without getting burned . 2. Disconnect the high-voltage band from the lamp anode by removing the black plastic hood. 3. Grasp the spring- loaded retaine r plate with the fingers of'one han d and push or pull it toward the PID lamp; it doesn' t take much force to move the plate enough forlamp remo...a!' Slide the PID lamp up and out of the P ID detector assembly. 4. Clean the lamp window using a mild abrasive cleanser like Bon Ami or Com et. Wet y OU! f inger; and make a peste with 3 small amount of cleanser. Scrub the lamp window clean in a circular-motion with your finger.
5. Rinse the lamp w-indow clean with water. Dry the lamp with a paper towel 6. Inspect the Teflon N seal for cutsor nicks. A damaged seal willnot affect~ PID response, but it may provide a leak site that will redu ce the amount of sample delivered to any subsequent detector. 7. With the lamp remo ved. the collector electrode is visible where it protrudes
The ccsectcreeceece p-otnoes into the cell
•
/
-
int o the cell. Ch eck.the collector electrod e fur any visible res idues. films, ~, . ~~ , discolorations,etc. Ifpresent, they may impedetbe flow of ions from thescmple molecules to the collecror electrode. Tocleaa the collector electrode, gently use TeflonTlol se al e small file to remove any residuesfrom its tip. Blow the residue Mak.e sure the Iai.lj) wnocwe centered offthe collector electrode and surrounding areas.
-
o....er u-s Tenor. seal and s....ug against it
8. Opea the spri ng-loaded reta iner plate and rep lace the P!D lamp snug against tbe seal . The lamp window bas a slightly larger diameter than the seal; try to center if against the seal. Replace
~~
1ft
the high voltage band I blac k p lastic lamp hood.
9. Recalibrate the Pill detector before returning it to service. •
A;1l.
120 (of 550 ) 2006(-2016)
121
DETECTORS Electron Capture Detector · ECD t.
OVERVIEW The ElectronCaptureDetector (EeD) is selective to electronegative compounds, especially chlorinated, fluorinated,or bmminatedmolecules. It is sensitive to some c fthese compounds in the parts per trillion (ppt) range. The ECD detector requires nitrogen or argon /5% methane (P5) to operate. The ECD detector is mounted immediately.. adjacent to tbcrightreer cclumn oven wall on your SRI GC chassis. Two BNe cables connect the anode end cathode,respectively, to the ECD amplifier. The ECD detectorcoosists of a stainless steel cylinder containing 5 millicuries ofradioactive Sickel 63 in an even enclosure that is thermostatically controllable from ambient temperature to 3 7)~C . Since the detecrorcontaius only 5 millicuries ofNickel-ed, the ECD is covered by a "General License" requiring a periodic wipe test and the filing oft! form with y OU! state's Department of Health. The documentation necessary [0 authorize your possession of a radioac tvie sourcei s includedinthe ECDmanual from valco, the manufacturers. This documentation transferspossession of tr.e ECD directly to youfrom Valco; SRI provides the ECD installation service andthe GC. There are four important documents to lookfor: 1) Certificationof Sealed Source. 2) Conditions for Acceptance of 8 Generally Licensed Device, 3) Test Specifications. and 4) Record of Source Transfer. Valco may printyour address {ID the multiple copies of the Reco rd of Sourc e Transfer, which ere 10 be completed by you and filed with the appropriate stareand local authorities. The other documents remain wi th the ECD detector; and Parts kit are necessary 10 proveauthorized possessionof the ECD. corTI:aini ng
_..--....
test res istor ~~?->~~-
•
.'
~
~~ :':"~ :..-:~-~..:=---:=
• :--- •:
0 ..
,
- ~ "":- . -
. .. .:"'- .,
ECD-€Qu ipped SRI GC
Trimpot setpoets
'e . ...
\"::=~
propcrau1:i:!orities, andtofumiliarizc \
• yourselfwith the requirementsof yO:lf ~ i : . .. -_. Cl· General L icense . You must also keep r~-A".: ~ I. I •• \. ..- • • • e .. · t on file the Ccrificetion of'Scalcd r-, ~ . •..y " . • •..', ,~ • • I '~ ':; " :~ .0' ~ ... _ : " Source and 'Icst Specifications, / ;~. ~~ - - 8 . 8 _. \ which are proof that your {-.. ;:= , \ :.:' • _.
• • • .. • ..
-
Ccse-up viewoaMe ECDcErtEc:o, or: an SRl GC
EeD det;c:or meers~--=- ,,:.::~ regu;at OrlS.. ./"
~
'Y< >,,-_ .~
__
,~ ~u
~. ~---
~_ ----L ... ........
~
~
__ _
...
-""~-<:_~_
..
:< ." '//$
_
...:..:d-/ ~,,:<
' v
--
.. _
. - , -!" " . ~!
•
...
Reco~ of ~-:.:-=~
Source Transfer and Iorwerd it to :.... ~l
_
__---
~::::::~~.~~ complete the
:"_.
- ...--..... /
-- ,... 2
•
-- -_ -
a:.::: .;:=~.::.:.::::.=-
-_
.-~o...... o o~
-H'
1
.
4
__
--.
......
~
~",,7.:..
ECD Detecl or
--.... ---_ ---- ----
--- -~~ , - --.- -- _ .....- --..~-- -
....
--. ----- ._ - ... ------ _. ~
- ~_
121 (of 550 ) 2006(-2016)
122
DETECTORS Electron Capture Detector - ECD
Theory of Op eration The rad ioactive Nickel 63 seal ed inside the ECD detector emits electrons (beta particles) which collide with end ionize the make-up gas molecules (either n itrogen or P5). This react ion forms a stable cloud offree electro ns in the ECD detector cell. The EC D electronics w ork to ma intain a constant current equal to the sta ndin g current through the electron cloud by applyi ng a periodic pu lse to the anode and cathode. The
standing current value is selected by the operator; the standing current value sets the pulse rate through the ECD cell. A standingCUt"Tent value of 300 means that the detectorelectronics will maintain.a constant current 0[03 nanoamperes through the ECD cell by peri odically pu lsing. If :'1 e current drops below the set standing CI!;'T:nt value, the mrnber of pulses per second inCI""....2.SCS to maintain the sta!:.6ng current
ECD Detector Operational Diagram Samp ie-iaden
ca rrier gas euet
Makeupgas inlet
I
•
V
I
• ---;:.. Gas outlet
When electronegative compounds enter-th e ECD cell from the column,they immediately combine with so me of the free electrons, temporarily reducing the number rema ining 10 the electron cloud. Wh en the electron popu la tion is decr eas ed, the puls e ra te is
increased to maintaina constant curren t eqU21to the standing current, The pulse ta te is convert ed to en
Example Pulse 'trans
JLJ~-ULJL Detecto r aectron'cs pulse to malrrtafn the sta"":ding CUfre:'t
increaseta signalrespcnse, the ECD dete ctor-electron ics
rJ1lfJlllfJLJl
meexure the pulsereteneeded to maintain the standing
esecrcnecetve ccmcccnoe
analog output, which is acquired by the PeakSimpl e data system. Unlike othercerectors which measure 2Il
The pulserate IS r- c-eesec in the presenceof
cu..'Te n!..
122 (of 550 ) 2006(-2016)
123
DETECTOR S Electron Capture Detector - ECD •
r-
"sa
I
•
Ex p ected Perform an ce ECD No is e Ru n
.
... ,
JII_
~.
-- -
" 0 1# g " ,M I '" GI e i ~ 1
Colum n: 15m M XT~5 capillary Carrier. Helium @ 10mU min Ma ~e up: Nitrogen @ 60mUmin FCD Ter:1P: 250"(; EGO standing cc rren r 30 0 O:'fsEt before Ze;:)i r.g L'1e ceta systen slgr.al: 28CmV
, ., , ec
1e.0Ul
~.
-
, , • '£..! ~ ft- b
~
"••VE'AJ\. '
•
,
"
. "D
fr-.. L!J!,. b f!J. I.~. ! fr\. f:.. ...., -if , b :
;!} '"
~
ECO noise ave rages less than 1mV fro m peak t o pea k
_1t.0lr.
~
~
~.
160 I .. Y- _ _
:!C r.HiUJ:. r....
'0
Eeo Pest icide An a lysis ~
::l!: ii ,! I 2: :t ..
;J;. ~~ hbtf:\ i !:c.. bI'~b !j.'Yo. b. ...., * [ ~ Sample : 1I-lL 200ppb cblorinated pesticides Column: 15m MXT·5 czli l1a ry Carrier: He:lur.-: @ , OmUmin
fo.'lckeu;J: Nitrogen@6Orr'. umn
ECD temp: 25O"C
,
ECD stinCing ~err..: 3CD
• Resu'ts
Cor.I;>or:err:
~~:ion
a -ea
F'e s:lOdes
2.850
"57e243~~
..
.·e2.,:ll! L - - - - - -- - - - - - - -- -- - - - - - -' .!..l!.EO ,
123 (of 550 ) 2006(-2016)
124
DET ECTORS Electron Capture Det ector - ECO
Genera l Operating Procedure The following suggestions are specific to your SRI ECD-eqlripped GC. Consult the Valco [ CD detector manual fo-cerrier gaspurityrequirements, carrier gas system configuration, and other general ECD detector informa tion. Keep in mind that the electronics shercetics in the Valco manual do not apply to your ECD· equipped SRI GC. <0
, I. Cap off the carrier inlet to the ECD cell (in the column oven). :::. Conn ect the makeup gas and let it flow through and purge the EeD cell.
Makeupflow is40-l00 mL; typically 60mL. 3. Hea t the ECD detector to 150
i I
DETECTOR
I• • • • • • • •
PARAMETERS
• • • •
••
• • • • • • •• •• • •, •, •• •"• <
••• ••,• •• •• ••• •, •• • • • ••,, ,•• ••• • ••• ••• ••• • •• ••• ,•, ••• • , • •
· ·· ,
,
· ••• ' -~"" I _ - ....... "' ' ' .... 1....~ ==.":"
(t 4. Tum on the [C D standing current (the ECD current ON / OF F switch is locat ed on the front contro l panel of the GC , under " DETECT OR ECO standing current P... \R..A..\.1ETERS'). As a rule ofthumb, an ECD detcceorreqcires enoughnitrogen ON/OFF swit'" ..h makeup now(40-I00mUmin) to significantly dilute thecarrier in order to help keep detectornoise down; the ECO can tolerate a 6:1ratio ofnitrogento helium. With the carrier and makeup gas connected and flowing, check the offset from zero. The millivoltreading should be between I00 and lti JECTOR-DU ECTOR-COl U,,",'" OVEN TEMPERATURES 5DOmY. lfthe signal offset is Jess than lOOmV, the standing current • •••••••• • • needs to be increased, Iftbe signaloffset i..higherthan 500mV, the • • • • • • • .' needs to be decreased. Once the signal is relatively standingcurrent • • • , • • • • quiet and stable, set the temperature to whatever is appropriate for < , , , ,, < < " yo ur analysis by adju sting the trimpot setpoint with the flat blade • • • : : ; ; ; ; ~ screwdriver provided. :~ :: : • • • 5, when the EeD detector cell reaches temperature, Iet tbe system I stand untilyouget astable milliVolt reading. Oncethesystem exhibits ECD C8'~ temperature display a stable baseline, reconnect the column. Observe the signal in the presence ofthe carrier flow. lf it is significantly higher, it indicates contamination introduced on thecarrier flow, If the millivolt reading is still relarively stable inthe presence of carrier flow, then sample may be injected. Avoid sam ples with high con centrations of electronegative compounds: theyw..ay effect ECD operation for some time thereafter, asthey could take toe long to dissipate. ~
• •
• .• . . . . . •• ••• • •
· ... .
·
...
0
·
6. You may need to adjust 11:.: Ee D standing current using its trimpot setpoint, The trimpot setpcin ts are located on the top edge oftile front control panel, directly above the display push-buttons for each controlled zone. Remember, increasing the standing current increasesthe ECD's sensitivity end raises the baseline offset.
124 (of 550 ) 2006(-2016)
125
DETECTORS Electron Capture Detector · ECD ECD Troubleshooting If you are experiencing baseline offset and noise problems witbyour EeD detector, try the following two diagnostic tests: 1. Veri fy that the ECD ampli fier electronic s are working properly by removing the detect or from tbecircuit and inserting a 1OOOMOhm test resistor in its place. The parts kit in the tackle box included with yourGC under the red lid contains a IOOOMOhm resistor for this test. Tarn the ECD current off. The anode and cathode connections are axe connectors located on the GC chassis near the base of the Ee D detector housing. Disconnect these two B~C connectors from the detector electronics, and install the IOOOMOhm tes resistor as a j umper betwee n the center conductor in the anode B::"C jac k and the center conductor in the cathode BNe jack, Z ero the d ata sys tem signal. Turn the ECD current bac k on, and check the signal offsetjobserve
the m V reading in the upper right areaof the Pe2kSimplechromatogram window. Withthe testresistor in the detector's place, the signaloffset should be 12o-15OmV with the standing current at 300. Ifthe signaloffset is pegg ed up or down (5()()()mV or 1500m V, respectively), there is a problem with your f eD detector electronics. Try turning offthe GC po....-erfor at least30 seconds. 'With the test resistor still in place, lhenruming it back on to see ifl he signaloffset stillindicatesa problem. lf the signal offset is at zero with the test resistor in place, check to make sure that you are lookingat the correct detectorchannel. Ifyou are observinga signal offset of zero in the EC D detector channel, call technical support. The ECD anode and cathode are conne cted to the ECD amplifier via BN C ca bles
Anode and cathode BNC co nnectors
ECD e lectronics test
" JA 1 :=:: . . : : i'~'~1 A
3NC cebies rrcm ECD
1illID)
"
i~!l uij 2:
Test resistor
,
L..._.
Ancoe i r
..
"
~
:
.1
caeoce
2. Operate the EeD 0 0 m ak e-up gas only by disconnecting the column from the Ee D. with the stan ding current still set at 300, observe the signal offset andaoise. Ifit drops. then the problem is being introdaced iatc the GC and EeD by the carrier gas thro ugh the column. Tip: In most siruatlons, the ECD will be used to detect S
CO I Ul'llilS :O help avoid
reactive sites arxi ghosrpeaks.
125 (of 550 ) 2006(-2016)
126
DETECTORS Dry Elec tro lytic Conductivity Detector - DELCO Overview The DIy Electrolytic Conductivity detector, or DELCO. is selective
to chlorinated and brominaredmclecules. It differs from the traditional wet El e D in that it does not use a solvent electrolyte, and the reaction products aredctccted in thegaseous phase. The SRI DELCO is available alone or in combination with theFlO detector, On its own, the detection limitsofthe DELCO are in the low ppb range. In combination with the FlO, its detection limits are in the low pp m range. The FID/DELC D
DE LCO on an 86 1DC GC
combination enables theoperator-to reliably identify hydrocarbonpeaks detected by the FID a<> halogenatedor not. Because the DELCO operates at 1000"<::, it can tolerate thewater-saturated FlO effluent, measuring the chlorine and brom ine content simultaneously with the Fill measurement ofthe hydrocarbon content. Allhydrocarbons are converted by the r ID flame to CO2 and H20 prior to reach ing the DELCO, thus preventing contamination of the DELCO by large hydrocarbon peaks.
FlO I DELCD C ombo Detecto r
DELCO - A la carte DE LCO
FrD FID collector
electrode , Close-up of the sa me
DE LCO detector
FlO f1ameport
.: "._- "
as~:", ;~ fl O heatsr block
DElCO reaction cnarroe- in sulation
'j,> /
~'r- . 1"10' ~
FID ignitor _ _--...,--'--_
.. Air supply
. ..,
FlO ignit or
&DEl CD
reee-
DELC O coll ector & thermocouple termina: a nd
ter:'Tli."'laI
gain swncn
DELCO collector & thermocouple
iecce
126 (of 550 ) 2006(-2016)
127
DETECT ORS Dry Electrolytic Con du ctivity Detector · DELC O
Theory of Operation The DELCO consists ofa small ceramic tube-
the DELCOreactor-heated to lOOO"C. Inside the reactor, a plat inum thermocoup le measures the detector temperature. and a nichrome collec tor e lectrode measures the conducti vity of the gases flowing through the DELCD. Thedetectorresponse is dependent upon its tem perature. Therefore . the
controlcircuitmustmaintain thetemperature, withina fraction of a degree, at lOOO"C. When combined w ith the FlD detec tor, the DE LCO is m o unted on the FlO exha ust. Column
effl uententers the FlD flame where hydrocarbons are
or bromine an d hydrogen forms HCl and Har, and the reaction of chlorine or bromine and oxygen forms CIO and BrC.,. - The D ELCO detects the oxidized species of chlorine a nd bromine, suc h as CI0 2 and Br02, It do es no t detec t the ac ids HCI or I lBr like the co nventio nal wet ELCD. In the hydrogen rich effluent from the FlO flame. the chlorine and bromine preferentially react with bydrogen (or the hydrogen in water) to make HCI-HBr. Given equal availability of hyd rogen and oxygen molecul es , a chlorine atom is 100 times mo re likely 10react with the hydrogen than theoxygen. Therefore, the FH1DELCD combination is lOO times less sensitive than the DELCO operated with the Fill off The SRl ,FIDlDELCD is operable as a combinat ion de tector, as a n FlO o nly. o r as a
,
ionized and combusted. Electrons freed in the ionization process are collectedby the flO collector DELCDonly.
electrode. which ha s a n internal diameter of l mm A DELCD only detec torreceivcs the sample laden (O.O4Ol . Due to its small LD..the collector electrode ca rrier gas directly from (he column o r from a no nacts as a restrictor; splitting the Fill exhaustgases so destructive det ector outlet, like the PID. it is mounted that it takesabout half of the flow, and the remainder on the hea ter block on th e c olumn o ven wall so that is di rected to the DELCO, The FlO exhaust gases consist of un-c ombusre d hydrogen and oxy ge n, ni tro gen. and w ater and carbon di oxide from the combustion ofhydrccarbons. The reactionof chlorine FlOcollector
FIDIDELCD Com bination
-
electrode ) }Flo smPlifier
q ,
Detector
I .-
th e co lumn effl uent is m ai nta ined at a temperature
ccnsistenrwith theanalysis. Thistype ofhigh sensitivity DELeD uses hel ium or nitrogen carrier gas and air make- up gas. DELCO ceramic electrode probe DELCO
eermccocpe f cathode
'"
Exhaust
""'" P~ tinum
tnerrro-
cccpe ard
co aectcr
ccseece Hydroge n suppty
"
~\
A ,.',
supply
DELCO insu lation
assembl y terminal
~
7
DELCO ccaecrcr, tnerrnccccc te. and he ater fi:ame nl leads
127 (of 550 ) 2006(-2016)
128
DETECTOR S Dry Electro lytic Conductivity Detector · DELCO
Expected Performan ce .
Fle l"" .W . . ._
_
c e a e.e :... II:< ,
-
- j¢l~li
.....
1r 1>
,,
,
I
•
DELCO Noi se Run
5. '
CoIt.mn: 15m MXT-VOL carne- helium@ 10mLJmir
,
DELCO gai n: l OW DELCO heater blo<;l( tem p : 15O"C
DE LCO reactor setpoin t; 260
~
T~lUre proJ;am:
Inrtial OO'C
;<
Hdc
R2nl>
20 00
0.00
FreJ OO'C
DELCO No ise averages les s t han 100I.lV from peak t o pea k " ~
nau ' ;:»0
~ .'~
:J
FlO I D EL CO Co mbo Test Run
l.. t .. X_ _
Sample: 1!Jl100ppm BTEX Pl us
.. . o<..... ... ~ an;
-
,
O;& " . <':i .... !
coumn. 15m MXT-VOl
!
,
•
<20"'" "'.'$",",;:;;:1("'-'-"$ ~-~
I
Final 24O'C
,"'
I
DELCO gain: lOW DElCO heater block temp: 15O"C DELCO rea ctor setpoint 260
"
cceccoent
Re!:erllion
Area
TeE PCE Bromoform
3 483 5.416 7.0 16
<63""""
-"
759.6650 1755.4 630
f, Ifj!!
...I
Rete ntion
..
~ o ";:[ " ~iJ j ~....-. t :1
5'__
..::a •
SoM
0.600 2850
3er.zene
»<,
TeE Toluene PCE Eth yl Benzene
3.500 4.766 5.416
Ort!'loXyie~
6 800
6.316
7.016 Total
II, .
i "iii!
..
!
l
•
<';
~
1:;. /::> 1-',
r~·
?20. 3325 149793. 350 5
~
~
.•.
I
\
I
+- .,
, · V :iT -' , ~
:!,. i"':"- ~ r .j"1 ~ if ' L
=
,,
I
,, •
,,, ~ ~
,
~ -
,
H I \j !I " :.UL--
.
\
",.
. h l. r
'. •
j A 'ea 144406.8420 1074 _0740 378.3505 1109.8590 364.5700 1103.6 3 70 1135.6855
\ I. ,\ , .
FlO Results: Co~"lt
j\
~ m
5322900
R D gain: HIGH FlO temp: 1500C FlO igr:itor.-4oo
'I
~"
DELCO Results:
Total
~
'::
Ca rrier: helium @ 10m Umin
Temperature program: Initial Hokl Ran"<> 4O'C 15.00 200
,-
~ '"
,
-
,"
rl,
i
.\
"
, ••) . J
".
128 (of 550 ) 2006(-2016)
129
DETECTORS Dry Electrolytic Conductivity Detector - DELCO General Operating Procedure The FIDIDELCD combination detector can be operated in the Combo Mode.the HighSensitivity Mode (DELCO only), or the FlO o nly mode.
Combo Mode In the Combo Mode, the DELCO is operated after the FlO; the FlD signal is usually connected to Channe l l on th e PeakSimple data system, w hi le the DELCO signal is on channel 2 or 3. Each detector amplifier is factorylabeled with the data channel to which it isconnected. The DELCO response in this mode
isuseable from I to 1000nanogramswitha slightly quadratic calibration curve. EPA andother regulations allowthe use ofdetectors with non-linear response if the operator calibrates with sufficient data points to accurately model the detector response curve. Therefore, the DELCO may require a 6 poinrcalibration where 5 poinrcalibrarion is normally required I . Set the hydrogen and air flows for normal FlO operation : set the hydrogen flow to 25mUm in and the air flow to 2SOmUm in . The pressure required for each flow is printed o n the right band side of the GC chassis. (1IiOTE: If you 're using a built-in air compressor, low levels ofbalogeoatcd compounds in ambient air-even levels below I ppm-s-can cause the D ELCD to lose sen siti vity, an d fluctuat ions in the level of orga n ics in am bientairmay cause additional baseline noise . To av oid this.use clean, drytank air. ) 2. Set the DELCO temperature serpoint to 26 0 by adjust ing the app ropriate rrimpot on the top edge o f the GC 's front control panel. The number 260 represents I OOO"C; the DELCO will heat to about 254 and stabilize. Theend ofthe ceramic tube will g low bright red due to the high temperature. 3. In this mode. th e Fill ampli fier is normally operated on HI GH g ai n or, if the peaks are more than 20 seconds wide at th e base, o n HIGH FILT ERED gai n for a more quiet baseline.
4. The DELCO amplifieris normally operated on LOW gain. High Sensitivity Mode The DELCO can be operated alone in thehigh sensitivity mode by eliminating hydrogen. With hydrogen eliminated, oxygen in the a ir will react with the chlorinated and brominatedmolecules at t OOO"C to fonn C10 2
andBJO , which arc detected hy the D ELCO. Water must a lso be e liminated; at the high tem peratures inside theDELtD, hydrogen disassociates from the H 20 mo lecule and becomes available as a rcectanrto form HCI and HBr, which the D ELCO will n o t detect The DELCO response curve is quadratic in the high sensiriviry mode as in theFIDJDELCD combomode, but sensitivity is increased by 100 to 1000 tim es. In this mode, me DELCO can perform much like an ECD, except that the DELCO is more selective for ha logens and blind to oxygen. When po ssible, quantitate by the internal standard method, usin g a chlorinatedlbrominated compound for the internal standard peak. Although th e DELCO will not be damaged b y large qu an tities ofch lorine1 bromine, there is a s ho rt tenn loss o f sensitivity for abou t an h o ur following the injection o f 1III of pure methylene chloride., forexample. I . Remove the hydrogen supply by turning itOFF, then di sconnecting it at the GCs inlet bulkhead on theleft
hand sideont einstrument. 2. Reduce the air flow to the DELCD to 25mUmin by turning the the air pressure trimpot setpoint down to 1 or 2psi. An additional 24" restricror made ofO .OO I " J.D. tubing would be useful for fin epressure adjustm ent. 3. lfyou're using a capillary column, push tbe column through the FlD jet until itjust enters the ceramic tubing o f the DELCO. This will improve p eak shape a s the co lumn effluent will be d ischarge d into the flo wing airstream and immediately swept into the DELCO detector volum e hy the air make-up gas. (When swi tching back 10 the FIDJDELCD com bo mode, remember to pull the colum n back into tbe FlO j et.)
4. TheFill collector electrode allows some gas to escape from the FlO combustion area, which is undesirable for the high sensitiv ity mode. Remove the FlD collector electrode and rep lace it with a 1/4" cap fitting.
129 (of 550 ) 2006(-2016)
130
DETECTORS Dry Electrolytic Conductivity Detector - DELCO
General Operating Procedure continued FIDIDELCD - FlO Only I. Remove the DELCO hea ter wires from the pus h terminals. Remove the three D E LC O collec tor and thermocouple wires (yellow,white and red) from the SCeYo' termina ls. 2. Disconnect the DELCO detector assembly from the FlO exhaust by using a wrench to loosen the 1/4"
Swagelok fitting securing the two detector parts together. 3. Use a cap nut to seal the DELCO connection on the FlO flameport. 4. Set theFID amplifiergain sw itch to HIGH for most hydrocarbon applications. Ifpeaks ofinrerest gooffthe scale (greater than 5000mV). set the gain to MEDIUM. When peaks of interest are 20 seconds wide or more at the baseand extra noise immunity is desired, set the gainswitch to m GH (filtered). This setting broadens the peaks slightly.
S. Set the FlO hydrogen flow to 25mL/rnin. and the FlO air supply flow to 250mUmin. The approximate pressures required are printed in the gas flow chart on the right-hand side of the GC.
6. Ignite the Fill by holding up the ignitor switch for a couple of seconds until you hear a small POP. The ignitorswitch is located on the front panel of yourSRI GC uode-the "DETECTORPARAMETERS" heading (it is labelled vertically: -FLAME IGNITE"). 7. VerifY that the FlO flame is lit by holding the shiny sideofa chromed \\TfDCh directly in front oftbe collect or outlet- Ifcondensation becomes visible on the \.'ITeOCb surface. the flame is lit
DELCO Only 1. Set the helium carrier gas flow to 1OmUmin and the air make-up flow to 25mUm in. Clean, dry tank air helps to obtain the best achievable DELCO sensitivity and signalstability. 2 . Set the DELCO reactor temperature serpoinr to 260 (= JOOO"C) by adjusting the trimpot on the top edge of thc GCs frontcontrolpanel. The DELCO willheat to about254 and stabilize. The ceramic tube will glow bright red from the heal 3. By adjusting the appropriate trimpot, set the thcrmostaucd D ELCO heater block temperature to 2S"C higher than the "Hnalr tcmperauue yuuhave CUI Cfcd inthe temperatureprogram.
4. The DELCO amplifier is normally operated on LO' ''' or MEDIUM gain.
130 (of 550 ) 2006(-2016)
131
DETECTORS Dry Electrolytic Conductivity Detector· DELCD
Troubleshooting and Maintenance
Installing the Spare DELCO Cell
Each SRI DELCO detector is shipped with a spare DELCD cell. Because the DELCO heater operates close to IOOO"C, it will bumout and fail eventually. Follow the instructions below to remove the old celland install the new one. I. WiththeGC power OFF, remove theDELCD heater wires (2) from the push terminals and the DELCO thermocouple and collector wires (3) fromthe screw terminals.
2. Remove the DELCOcell by using a wrench to loosen the 1/4" fitting that secures it on the FID exhaust port or on the heater block. You may have to hold the insulation aside to freely access the fitting; it is soft and may becompressed by hand. 3 . Position the new cell on the fitting with the label fac ing up, as the DELC Ds are shown on the Overview page. Be sure to push the DELCO ceUall the way into the FlO.
4. Secure the new DELCOcell into place by tightening witha wrench the fitting that holds it onto the FlO exhaust or the heater block. 5. carefully lower the red lid to make sure that it does not touch the DELC O ceU; the cell will crack if the lid hits it, There should be at least 0.5.... o f clearan ce between the red lid and th e edge o f the DELeD cell
6. Sensitivity may improve for the first 24 hoursof operating time with the new cell installed,
131 (of 550 ) 2006(-2016)
132
DETECTORS Cata lytic Combustio n Detector - CCO
,..- ..
Overview .1
-
r]
Iii
111111i! Iij!II [iiii !I IiIi; ; : ;.. :IIIii 11 11111t il l iII! II iI
IM.,I
leM 11
I
2:
. :
I
31
4i
5,
I
61
Oil
I
: I I ' i I ! ! ! 11 ' I j [ i I I il !
CCD Detector and protective cap (cap is removed prior to inslallatioo)
--. -
The Catalytic Combustion Detector responds to allhydrocarbons with
the selectivityofan FIDand the sensitivityof'aTeD. The entire detector's diameter is merelyonecentimeter. Its sensor element consistsofa tiny coil ofplatinum wire embedded in acatalytic ceramic bead Each CCDdetector hasa pair of sensorelements. The sensorsare housed in high-grade, flame-
..... \
CCO on Column Oven
' II
=== _ "' ~
1~~~~=' II i
,::
'i~~~~ ~
'. I
--",
'
procfnylon.and protecti vely capped with a fine steel mesh. In SRI GCs , the CCD detector is mounted on the wall of the ColumnOven in a brass housing,as500\0\n in the topleft picture. The analvtical column residingintheColumnOven is connected to the ddtectorthrough the oven wall; the example shownat
bottom left is an SRI Gas -less? ' Educational GC featuring a
CCDdck'Ctorand a Im (3·)HaYe:-e~D ~ked~lwnn. The ,\ ~.rL .... -- ~ CCD detec~rlsespecl~ly sulted forgas I ~~~ less operanon because It can operate on i ambient air, requiring no high pressure I ' cylinder gases suchashydrogen or helium. In theGC system pictured at. left, a built-in air compressor supplies the carrier gas for the CCD.
The CCD detector can also be used as a hydrocarbon monitor in non-chromatographic applications where the CCD
.,
senses the total hydrocarbon content of a flowingair stream. or as a hydrogen/hydrocarbon leak detector.
/
132 (of 550 ) 2006(-2016)
133
DETECTORS Catalytic Combustion Detector - CCD
Theory of Operation Top ViewofCCD Detector
~\ (
-
.
j
Sensors
The eCD sensor clementsarc thetinicstand mostimportant pan of'the detector. Each CeD detector contains two sensor ele men ts. but uses onl y one at a time. A ca talyt ic combu stion sensorconsistsofacoil of platinum wire around an aluminacore surrounded bynoble metal catalysts. Each sensor is s uspended betwee n a pair ofnickel pins. The detector is shipped with a protective nyloncaptopped with steel mesh. but is installedon a SRIGC witboia it During a chmmatogaphic run. a 150 milliamp
current heats thecatalytic ceramic bead to around 50tJ<'C, hot enough to combust hydrocarbon molecu les o n contact. The CCD is ma intained in an oxidative environment by using air as Sensor Eleme nt
the carrieror make-up gas. This combustion causes the increase in tcrnperatureand change in resistance that is measured by the sensor. This change inresistarce C311';:;es theCCDdetector output to change. which produces a peak that is recorded by the PeakSimple data system. To pro long the life ofyour CeD detec tor. use it in stri ct
accordancewithyour GC system's operating instructions. For
+- - -
Niocel p os
-- - +
instance, if youhavean SRI Mud-Logger GC, you should connect yoursamplestreams at IOpsi so that no more than 5mL'min of pure hydrcarbon flow reaches the ceD. In the event ofa sensor burn-out, simp ly remove the white and black wires from the top
two nickel pins, Sid e View 01 Sensor Elem ent
andrnovc them to
thebottompair of nickel pins to connect them to the second sensor. It does not matter which wire goes on which pin Toreplace the CCD detector. UJL<>Cre\'.' its brass fitting after removing the wires from the nickel pins. Pull out the old one and remove the protective cap from the replacement. Sensorside first. insert the replacement into the ~ fitting"'ithits half-moon shaped cut-our on the bottom. Repl ace the fitting and - - Fc;-'---,,-, HANi) TIGHTEN it. If the detector (
fining is screwed on too tightly. tilt:
)
iI
n
detector wi ll net receive propcr gas flow. Next slip the black and white wire plugs ~ ~ [) oyer the pins. and your replacement ce D detec tor is ready to use.
..
..."'; --
- -
133 (of 550 ) 2006(-2016)
134
DETECTORS Catalytic Combustion Detector · CCD
Expected Performance
ceo Detector Noise Run
_
'. [ Ic
toM Y-
Flow = 37mUmin
,,
Isothermal Temperature Program : Initial Hold Ramp Fina! 8O'C 15.00 0.00 8O'C
I
~ <:- , ,," . ,,"-
-,,
-,. .
-'
~
,,
,
,
a •
'......
_.,-~
,
!
~l
~
I
\
,-
ii S
..
I
-
• 1/
..
. :-:~
~
..:..l.!C1
.
...
r.. t * _ _ _
,-
:;- -,;;---.-.-~ -. ------~
,,
C: Z; g lf .s",, ! ! [
•
J •
~,
~ •
~
••i
• \
i
..,
!
~
h h ."". .~ :'!- I"'.~, i"', f"...
-
<")
" IISD
*
e,
.
".,..,
•
,
~
Factory Test Run of a Gas-less'" Educationa l GC System
-- -
.,=- ...
I
No ise level is app roximately 50"IV from peak to peak
/=
,,_.
x
~
,,
Enlarged for clarity
• '"
!.'o.
E:; ;S1ii156'. t
i1,,",aco ~N::I ,_
Colum n = 1m Hayesep 0
~
~
,Ji· .Vj
Sample = 1~ L 1000ppm Methanol/Acetone mix; erect injectio n
I
\ \
Isothermal Tem perature P rogram:
\
Initial Temp 13O"C
,
\,
'--~
Negative water peak
Hold 10.00
Ramp Final Temp 0.00 13O"C
RESULTS:
\
;gw:.J .~
Column = 1m Hayesep 0 Flow = 37m Umin
~ ;Wi-
Component Me thanol Acetone
Retention
Area
0.816
13.2030
2.000
6945 .3570 6958- 5600
134 (of 550 ) 2006(-2016)
135
DETECTORS Th erma l Conductivity Detector - TCD
Overview The ThcnnaI Conductivity Detector (TC D) is the most universal detector available. Depending on the
compound. the TeD responds with a detection range of 0.01% to 100% (1 00-1,OOO,OOOppm). The SRI TeD consists offour filaments housed in a stainless steeldetector block. The TeD detector block is installed in its own thermostatically-controlled ov en for stability. The TeD o ven is mo unted on the right rear ofthe coJunm oven. The TeD filamentcontrol switch and the bridge tenninaI block to whichthefi lament leadsare connected are located to the immediate righ t of the detector oven. Since the four Te O filaments can be damaged or destroyed if energized in the absence of carrier gas flow. a TeD filament protection circuit is provided in all TCD-<:quipped SRI GCs.
Teo Detector (pa ired with an
~1----- TeD Detector on
~
anSRI310 GC
.
~~' :'-' . • t ·-~ - -. - " "; :.:. ... . ,-
.
---_. .,,:" ... . . ...... - . ::::::::;' :, :
I
....
•
'~ i
FI D detector) on
• e.. _
an SRI 8610 GC
.
t:-"-·U :
-
.,:-- .~::~- ~ . n,; .- - . .
. .. • .........................
;, j .
-=.T 7·~
-""'''
1: ~,
~ :iiIIIflkt
. ..
~-:-;--- , - v,
\ .~~.;,. ~~: ~,-:-," ~~
.____
...
0- .1
TC D detector oven sercoot (trimpot)
TCD Detector on an SRI GC
Teo Detector on an S RI GC with detector cover and toptfront ms uietcn removed for clarity
Co lo r-coded T C D fttam ent leads ate co n ne cte d to the bridge terminal block
. . .....- . ............... _.
-
body
Insulation - -j --
Teo detector - - f-
.....,.
"""""'."." ...,.... .."'." ,._ _,..,r.
housing
""' ~
~,""'
TCDdetecto'~--
',~
"';;-
TCD filament current control switch
Color-ceded filament leads
135 (of 550 ) 2006(-2016)
136
DETECTORS Thermal Conductivity Detector - TCD
Theory of Operation The Teo detector measures the difference in thermal conductivity inthe carrier gas flow and the analytc peaks. Every compound possesses somedegreeof thermal conductivity, andmaythereforebemeasured with a TCD detector. Due10 its high thermal conductivityand safety.heliumcarrier is most often used wi th TeD detectors. However. other gases may be used such as nitrogen, argon. or hydrogen.
*
v. o-...,
On e of four TCD filaments
TU ":gste~rtIernUf!l
I
rsament
~
Teo filament bridge
Woven li bwl~ ass tes u atcn
d<,;
~
-
.
-·.; F:
. '
,"
/ ,-:.','
fi lament leads are
The Wheatstone Bridge circuit col or-coded for iderr:tflc;;;tJ cr. design in the SRJ Te D uses four general-purposetungsten-rhenium filaments for sample analysis. T\\0"0 of S i!T.ai • the filaments are exposed to the sample-ladencarriergas flow and provide S:gr:aJ + the actual chromatographicsignal. The other two filaments are provided wi th clean carrier flow. enabling them to be used as a baseline reference signal. When the effluent from the co lumn flows ove r the two sample stream filemeors, the bridge current is Simplificati on of filament interc onnection unbalanc ed with r espect to the reference signal. Thi s deflection is Reference gas in Sample gas in translated imo an anal og signal which Red Red ,• ( ! is sent to the datasystem for analysis. Blue Green REFERE NC E v The fourpairs offilarnent leads are SAM P LE I color-coded in two-color units; ea ch color is used on two differentleads. All eight v..ires arcconnected to the bridge curre nt supply via four setscrew- type y Blue , Green terminal connectors on the top control ! panelof the GC Silkscrecned labelling SAMP LE REFERENC E on the chassis indicates which color Black "'" Colo r-coded ",..ire connects to each terminal. fi lam l!nt leed s The TeD detectorblock is divided into W..o cells containing tvro filaments each. One cell holds the reference pair while the other cell holds the sample pair. AlI four TeD filaments are physically identical exccpl for their color-coding. The carrier gas is plumbed so that is exi ts the Electronic Pressure Controllermodule. flows through the polishing filter, through the reference side ofthe TCD bridge. then through the injection port to the co lumn, and from the column to the sample side of meTeD bridge. Aft er the flow passes through the sampl e cell. it is directed back out ofthe Teoovenand into the columnoven through the TeD detector outlet. where it may be routed to a subsequent detector or to vent All four TCD detector inlet/outlet tubes are IJl6" stainless steel.
"
"t
I
I
I
l
- "
1/813C'
Teo carrie r gas flow diagram
I EPC H Polishing f. lte r
Refere nce side
~ of Te D bridge
f.>!ry /"'\
Injection port
1r --;;cS em--;----,-,-----. ple s ide cf TCD br id ge
TC ::: r de t ector
oLtle:
136 (of 550 ) 2006(-2016)
137
DETECTORS Thenna l Cond uctivity Detector - TCD Expected Performance Teo No ise Run
£11.
£d~
y_
~
1;1....
o ~ iii t h§ ] ~l< ~ .. ii' 1 cr
Carner; Helium@ 10mU mi n TeO ga in = LOW TCD lemp = 100"C
O. I C~
..""., ,,,
Z 3
n
",
~ ~, ~
f0. In j'f\ Iin h b h !1""- fr... ") * !~ ii
co..:
Temperature program: Initial Hold Ramo
roc
15 00
0.00
Te D noise averages 1OiJV fro mpea k to peak
_!LH ·O L
-
-
-
-
-
-
-
-
-
- - - --
-
-
-
-
-
-
-
-
-
-
-'
±.L!..l ~ .x J
Factory Test Run of a TCD-equipped SRI GC Sample: natural gas sta ndard, 1mL samp le loop
.P_l·-
-
D ~ fiiil 1J ~ I ~ i!l .....T Go'3 STO
'00'
.. "••I , , , , ,,:.: !' ....t, t,-- ' [.--, f~
Colum ns: 1m M olecular Sieve, 2m Silica Ge l
_£I ,
f.<: .0 f.!' i~\
.-
~,
.~.,
-,I. '
.
fr.''' ..., ...t . ' ,. '" I
"'-l:;~ 21; ' O '~IQHAU.
t
z
• ,
~ .i;i B ~ , 8
I
~I
0 .050 6.00
§
w
•
•
~
•
,
I, \
~ z~
j1
/1 , \
J
l
,0
~
-lI SOO
~
""
~
-
G OFF
Inil ial Hold 4 00(; 5.00 2 20"C 16 .00
~i
,
I
Eypnt ZERO G ON (valve inject)
Temperature program
$
r~
,
Events: Time 0.00
-
- - _._.-
Ramp 10.00 0.00
Resu lts "
I•
~
~
In
I
.
-n 'r'] aeecc
Com2j?!!£Ol:
Rctert;!;m ~
Oxyge n N2 Methane Etl-riine
1.633
19.7500
2 . 150
12 1 08 80
3.033 7 .550 9.983 13 .6 83 18.150
563.6130 128.2185 119860 113 9220 G9.49GO
18 .766
6 7.4460
lso-p enta oe 22.550
20.14 90
CO2 P ropane lee- Bu tan e N -BuUilne
N-Pentane
22.800 Total :
19.15(10 1134 6145
137 (of 550 ) 2006(-2016)
138
DETECTORS Therma l Conductivity Detector - TCD Expected Performance I!I P_l ,~
EO'
- ,..
,- ...
•
Ci ~ rd " .5 !":l.. 1!1 ~ , fi'
, '" "" .. ..
z a
•
,
"
,
5 CC RCQM
"-,.~ ~
Teo Room Air Analysis
IIQ..
• I .' WLT CON
Column: 3' Silica Gel Carrier: Helium at 10mUmin Sample: room air, direct injection
B
c.scc
I
,,
TeD current l OW TCD temperature. 100'C
~
i3
, Tem perature Progra m:
B
. '00
Initial 80''C
A
\ .!lili..U coco
~'
..
--~v
Hold 4.00
Ramo 0.00
Final BO"C
'T'[;1
""
"
Res ults:
RetentiOn 0.716 2.766 Total
Com oonent ° 2 NZ CO,
The CO..content of the room air analyzed is approximately 35Cppm.
Teo Breath Ana lysis
IIPHIo:''''
• , o rS liI
..
-
,
,
8 : .a ! ~"
E
§
. , , , -2.. 1 I
us CC BP.E.O.T><
Column: 3' Silica Gel Carrier: Helium at 10m Umin Sample: O.5cc human breath . direct injection
" '"
>:J,
,~
I.
.,
.
......
.
,
Component
Retention
h ea
°2 N2
0. 700 2.700
1379 4 740 6 19540 144 1.4280
CO,
TeO tenceratare. 100"C
To,," Q
,
~.
s Final SOCC
'. 5060 1022.8890
Resu lts:
iB
TeO current l OW
Temperature Program : Ram p Initia! Hold 8O'C 24.00 0.00
.
Area 1021.3830
0 0
~
,
~
.0.800 • i•
""
!• , I
(\
I \
1'
) \
~ •.ut:.
138 (of 550 ) 2006(-2016)
139
DETECTORS Thermal Co nductivity Detector • TCD
General Operating Procedure I. Check to make sure that the TeO filament current is 5\\ itched OFF. Plug in and tum on yo ur Oc. Allow the TeO detector ovento reachtemperature ( I OO"C) and stabilize . With the "Display Select" switch in the UP posi tion, press on the TeO Temperature A ctual button on the fro nt control panel to read the TeO cell
temperature. The Te O oven block is set to lOOOC atthe factory, but is adjustable by turning the trimpot with asmallblade screwdriver w'hile obscrving the TeO BWCK setpoint temperature on the digital display. The trimpot is located on the top edge ofthe GCs front control panel. under the red lid . 2. All TCD-equipped SRI GCs are tested wi th a 1m. 1/8'" stainless steel silica gel-packed column. The carriergas head pressure is preset at the factory to IOmUminfor this type and size column. Look on the right side ofthe GC for the carrier pressure th at correlate s to a flow o f 1OmUmin. Because d ifferent oolumns requi re different flow rates. the carri er head pressure may be adjusted by the user with the trim pot above the " CARRIER 1" buttons. 3. Make sure that the setpoint and actual pressures are within lpsi. 4-_ Damage ordestruetion ofthe Te D filaments will occur if current is applied in the absence of flowing carrier gas. . '. \LWAYS verify that carri er gas can be detected exiting the TeD carrier gas outlet BEFORE energizing the TeD filaments. The carri er gas outlet tube is located on the o utside of the Co lumn Oven on the same side as the detector. Place the end o f the tube in liquid and observe (a little sp it on a finger can su tlice). If there are no bubbles ex iting the tube, there is a flow problem. 00 NOT tum on the TeD current if carrier gas flow is not de tectable. A filament protection circuit prevents filament damage if carrier gas pressure is not detected arthe GC , but it cannot prevent filament damage und er all circumstances. Any lack ofcarrier gas flow should becorrected before proceeding .
5. With the Te D filaments switc hed OFF, Zt'W the data system sign al. Switch the fil ament s to LOW. Th e signal's deflect ion should not be more than 5·) OmV from zero for a brand-new TeD detector. Any more than a 5-1Om V d flectio n ind icates partial or complete oxidation o f the TeD filaments; more deflection means more oxidation. Therefore. it is a good habit to use th e data system signal to check the \vorking order ofthe TCD filaments.
6. In PeakSimple. set anisotheermal column ove n temperature ramp program as follows: Hold Rmnp Final Temp. Initial Temp. 80°C 7.00 0.00 80' C 7. Zero the da tasysrcm signal (clicking on the Auto Zero butto n at the left edge o f the ch rom atogram window is one way to do It), then start the run (hit the computer keyboard spacebar o r hit th e " R U:-';'- buno n on the Ge).
8. Injectsample, Injection volumes ofO.5mL forgas and Iul, for liquid is reco mmended
I-
AutoLero
:
button
to prolong TeO filam ent lire.
139 (of 550 ) 2006(-2016)
140
DETE CTORS Thermal Conduct iv ity Detector - TCD TCD Filamen t Protection Circuit All TCD detectors are susceptible to filament damage ordestruetion ifoperated at high current in the absence of carrier and/or reference gas Ilow, The filaments " i ll incandesce and bum out ifthe carrier or
reference gas flow is interrupted due to a variety ofpossible factors such as a column break, inadvertent colurrmdisconnection during columnchanges.removal ofthe septum nut for septum replacement, or when the carrier gascylinder runs dry during an analysis. The SRI TCD filament protection circuit is a current"ern-out" circuit that monitors the column head pressureduring GC operation. Under normal circumstances, there is no reason for the column head pressure to drop below 3psi, wi th most columns operating at 8psi or above. When the headpressuresensorlocated in the carriergas flow pathdropsbelow Spsi, the protection circuitis activated, and the current to the TeD filaments is interrupted immediately A red LED on the GC 's front control panel under " DET ECT OR PARAMETER S" will light to indi cate That the protection circui t has dete cted a gas pressureloss and shut downthe filament current The causeof the prot ection circuit activation should be immediately investigated and corrected. As an additional caution, use HIGH current on ly wi th helium or hydrogen carrier gases. Wit h nitrogen carrier. use LOWcurrent only. or the filaments may be damaged. The pressure at which the protection circuit activatesis user adjustable with the trimpot on the lop edge ofthe front
control panel above the label reading 'TCD PROTECT:" TCO protection circuit LED lit on an SR I model 8610 GC front control pane l
I
1 • •• • • •.. • •.. I:,• ·,• . ., •, •, .., ., II
DETECTOR PARAMETERS
e
81. .
Bright red LED di splay TEMPERATURE ("C) PRESSURE (PSI)
1· LOCAL SETPOINT button
. 2..
LED pa nel crsptays control: data corresponding to tne button pressed
2· TOTAl SETPOINT button
e
• JoG
r;
3- STATUS LED
. 4- ACTUAL button
•
e
e, •, c • , , c • , , , c •c c • , ,c •,• • ,, ,• •,r ,c, ,•• ,e ,•e c A
A
A
v
• •,• , ,, I ................. on
~
~
~
lit
@!l (it
~
~
~
_ ~ It.
UQ _
"
;~> OISPLAY SELE CT COI..'J>l>lO'i'!.. \
n . ~ Hl"' nl R~
,
•r
_.. - -.~
TI;;C ~ "-" T
~~
~ ,~
A
0
START RUN
T he DISPLAY SELECT switc h allows the user to ch oose between d isplaying the control zon es us ing the buttons or the column oven temperature
1- Pressing the LOCALSETPorr-rr button displays thefilament cut-offsetpoint value (factory set at Jpsi) in the bright red LED di~"p lay in the: upper right corner ofthe GC's front control panel. If the carrier gas pressure reaches or falls below this value. the filament current wil l imm ediately be interrupted. 2- Pressing the TOTAL S ETPOL'IT button displays the carriergas pres sure present in the GC system. Under normal operation.this value will bewellabove the Spsicut-offsetpoint.
-.
3 ~ The ST.ATUS L ED glows bri ght red only when the Teo protection circui t has been activa ted. 4- Pressing the ACTUAL button displays the voltage present acrossone halfof the TeD bridge. A v-aluc of 3.5 to 4.5volts is typical \....hcnusing high current: low current will display 2 .5-3 .5 volts (note : the LED disp lays 4 vol ts as ' '400:" 3.5 as - 350: " etc.). A ny value lower than these indicates a potentia l problem in the TeO
de tector bridge.
140 (of 550 ) 2006(-2016)
141
DETECTORS Therma l Co nd uct iv ity Detector - TCD
TeD Troubleshooting When the Ten fails to perform normally; reviewoperatingconditionsto ensure
that carrier gas flo w to the detector is uni mpeded. and that the column oven temperature, carrier gas flow rate, and carrier gas EPC pressure are al l within the desired operating parameters. If all conditions are properly met and the detector
continues to perform poorly or fails to perform at all.check the TeO filam en ts for damage. The main diagnostic test is to measure the resistanceofcach filamentusing the ohmctcrfunctionofa multimeter or volt-ohmctcr (YOM). At roomtemperature, the resistanceofeach filament should be 32-34 ohms. At 1OO"'c. the filaments are around 40 ohms each. Ifany filament is significantlydifferent from the others, the
Te n bridge vvill be unbalanced, no isy and drifty. All ei ght filamcnt vvires m ust be disco nnected and tested. Since aU the leads arc bundled together as the)" exit the
TeD detector assembly, you mayneedto use themuhimerer or VOM to determine the actual pairs. It is normal for each filament to have a sligh tly different read ing within the appropriate operating range. so match the readings to determine the lead pairs. With the power tu rned offand the power co rd unpl ugged from the electrical outlet, raise the red lid to access the Te D detector. Exiting the right side ofthe TeD detector oven is the bundle 0[8 insulated, color-coded wi res in pairs. Each pair ofwires represents one filament and is connected to the approp riately labeled terminal for its paired colors. One filament has red/green, one rod/blue, one black! green. and one black /blue. The red/green and black/blue are the sample side filaments, and the UIK."S which typi cally deteriorate first. Remove the 8 wires from the bridge terminal by loosening the retaining setscrews w ' ith a small blade screwdri ver; Mcas...ure the resistance across the filament leads using an ohmeter, making sure the correct pair ofcoloredwires is tested together foreachfilament. An infini tereading is an indication that the filament isopen.or bumed out If'any ofthefilaments hasa signi ficantly different resistance than the others (which sho uld be in the ranges mentioned above), it sho uld be replaced Replacement filaments. o-rings,and TeD blocks wi th four new filaments arc available from SRI. In addi tion to the standard filame nts, optional go ld-plated filaments for improved corrosion resistance are also available.
Many mummeters are available; the se two are from Fluke Corporation: USA 1-800-44-F LUKE EU, (31 40j 2 6 78 20 0 VtMW fluke .com
SRI TeO detector rep lacomont parts Standard Te D filament "lith robber O -ring gasket
High temperature TeD filament with copper gasket
8670-9 120 8690-9 123
(filam en t part #s are also listed on the top ofthe Te D oven in your Skl GC)
141 (of 550 ) 2006(-2016)
142
DET ECTORS Thermal Conduct iv ity Detector - TCD
Replacing the TeD Filaments SRJ Ten deteetors are made to last a long time without ever replacingthe filaments. However; anyTeO filaments that failthediagnostic ohmeter testmentioncd previouslywillhaveto bereplaced. Whilethey share the same outer assembly, there are a few differences between the high temperature Te O detector block and the standardTeD block. Both designsare discussed. All filaments are fragile; handle them with care. Have colored ink pens, electrical tape , whatever you will use for color coding close at hand before you begin. It is best to go slowly, color-coding then replacing each filamentone at a time. IF YOU MIX UP THE FILA\ffiNT LEADS. YOUR TeD WILL NOT WORK! A. Standard TeD detector block access I. With a small blade screwdriver. free the filament leads from the bridge terminal by loosening the setscrews.
2. Remove the detector assembly cover by unscrewing the thumbscrewthen sliding the cover off toward the right-hand edge ofthe GC; gen tly remove the white insulation to rcvca1 thedetector block. 3. Disconnect the detector block gas inlets and outlets. Thereference gas inlet is disconnected at the polishing filter immediately behind the column oven. The reference gas outlet is disconnected inside the colum n oven. Disconnect the sample gas inlet at the fitting onthe colu mn. The detector block sample gas inlet tubing has a copper sheath for identification. The sample gas outlet is usually routed out the right side ofthe column oven. Exp loded view of the standard Te O detector assemb ly Outer T C D detector assembly case permanently mounted to ccnenn oven waH
Insulated padding
Outer TC D detector asse mbly case cover is rem ovable fa' access to inn er metal d am shell case
ene heeree wrep
Carrier ga ~ in from polishing filter. and back to injector
Filament leads to bndg e electronics
i.·.·.·
«x. :
Sample ga s in rrcm a:"lalytical
ccumn. ene 0lJ: to nex detec tor
0'_
Column ev e-r
1f!===
=
-3>
TC D det ector block
In ne r clam shell case is heat-wrapp ed v:ith tbe-mcstatted electrical he aon; eemen; and protects Te D d etector block
2 hex -head screws
secure inner
c1 am s.:H~!
142 (of 550 ) 2006(-2016)
143
DETECTORS The nnal Conductivity Detector - TCD Replacing the TCD Filaments continued (Standard TeD detector block access continued)
4. Cut the fiberglass tapewrappedaround thedetector blockand peel it off. Unwrapand remove the heater rope from the detector block (it is probably affixedto the thermocouple wires with more fiberglass rape). 5. Disconnect the thermocouple by loosening the small philips head screw which holds it on the detectorblock clamshell. NC?.t removetheclamshell by unscrewing the two small philipshead screws that hold its halvestogether. Gently remove the white insulation to reveal the detector block. 6. The Ten filaments are secured in the detector block by two plates, eac h of wh ich is held in place with three hexagonalhead screw'S. Holdingthedetector blockwith one hand, use an Allenwrenchto
unscrew and remove the hexagonal head screws from oneofthe filament securing plates. Then. slide the filament securing plateoff the filaments and leads. SCi it securelyaside. 7. Once the securing plate is removed. the filament and rubber Ocring that seals it can be gently p ulled out ofth e detector block cell. When replac ing a f ilament, its rubber O-ring should a lso be replaced . Check the lip of thc detector block ceil for fragments of the old O-ring and ifany are present, remove them as they " i ll interfere with proper sealing ofthe cell. If yo u're replacing one reference or sample filam ent, replace the other at the same time . If'you d idn 'I have fun disassembling the TeD detector block, replace all the filaments \....hile you have it open . It's a goo d idea 10 remove then replace one plate an d corresponding pai r o f filaments; at u time to avo id mixing up their connections.
Exp loded view of t he standard TeO detector block
8. To install a new fi lam ent. color-
£!!!!! it the: same as the filament you are replacing. then slid e it, leads first, through the appropriat e hole in the filament .securingp lare. An existing or replacement filament shou ld occupy the other hole , Place a new rub ber O-ring against the rim ofthc detector block cell which will acc ept the new filamcnt. Place filament securing plate
ani filamernsagainst tbe detectcr block with the filaments inside the detector block cells. Replace and tighten the 3 hex-head screws. Repeat thisprocess on other s id e to rep lac e the corresponding filament. 9. Reverse you r st eps fo r Te O detect or reassem bly, Steps 7- 10 of the high tem perature TeD detector block acce ss instr uct ions d etail reassembly of the inner clamshell and outer detector ho using.
Detector block
Reference cell
Sample cell
R u~erO.;r.gs
Filament Filament secunnq plate
Hexagonal hea d screws
-, ,
Insulated filament le ad s
143 (of 550 ) 2006(-2016)
144
DE TECTO RS Th erm al Conduct ivity Detector · TCD
Replacing th e TCD Filaments con tinued B. High tem pe rature TeD detector block access The high tempe rature TeO assembly is the same as the standard: outer housing around an inner clamshell case. The high temp detector block uses glan d nuts and copper gaskets to secure the fo ur
filaments in it." 1"'00 cells. Insteadofthe heaterropc. it employs a heating cartridge, which is inside the inner clamshell case with the detector block. I. WIth3 smallbladescrewdriver.disconnect the filament leadsfrora the bridge terminal by loosening the setscrews. 2. Rem ove the de tecto r ho using by unscrewi ng the thumbscrew then slid in g the ho using co ver off toward the righ t-hand edge ofthe Gc. Gently remove the whi te insu lation to revea l the d etector block. 3. D isconncctthcdetector b lock gas inlets and outlets. Thereference gas inlet is disconn ected. at the polishing filter immediately behindthe column oven. The reference gas outlet is disconnected inside
the column O\ "CO. Disconnect the sample gas inlet at the lining on the column. The- detector block sample gas inlettubing has a copper sheath for identificat ion. The sample gas outlet is usually routed out the right side ofthe column oven. Once these three fittings are loosened and the detector block tubing freed. gently pull the detector blockaway from the housing.
Exoloded view of hig h tempera ture TCD detector block and inne r clam shell
Installed/secured filaments
Detector block
r
~-
_
Insulated
Insulated _ _ padding
padding _ _
-_._>+ - ---=--~/
:- ~ /
H.:IJf nf inner damshelJ case
-
.
: A1 r Glandnuts~ \
,~--.::===;====--~/ ~---
Copper gasKets
I
Half of i nner clamshell case
144 (of 550 ) 2006(-2016)
145
DETECTORS Th ermal Co nd ucti vi ty Detector - TeO
Replacing the TeD Filaments continued (High temperanae TeD detector block access continued) .1. Open the inner clamshell case by unscrewing the two small philips head screws that hold the two halves together, Gentlyremove the white insulation to access the detector block.
5. The f ilaments are held in place by gland nuts; loosen these nuts to removethe filaments andcopper gasket". Color-eode the new filament the same as the one you are replacing (y o u can use colored marker pens, electrical tape. etc.) before completely removing the old one . Slide the gland nut offthe existing filament, toward the ends ofthe
i
,-
Slide the gland nut down and off te remove the filame nt
f l
filamcrnlceds, 6. Put the new filament 's leads throu gh the gland nut. Slide the glandnut up thcfilament's leads untilit
rests against the base of the filament. Place the copper gasket against the rim ofthe detector block cell opening. Carefully insert the filament and gland nut together into the cell opening. lighten the gland nut to secure the filament in the cell.
7. When you 're finished replacing filaments. place the re-assembled deu.e. ctor block inside the inner clamshell with the insulationand heater cartridge. Makesure the gas inlet und o utlet tubes are numingthrough the cut-outs in the clamshell. Secure the clamshell with its two screws .
8. Reconnect the Teo detector gas inlets and outlets.
9. Replace theInner clamshell and its insulation inside tbedetectorhousing that is permanen tly mounted on the column oven wall. Replace the housing cover and secure with its thumbscrew
10. Reconnect the filament leads to the bridgecurrent terminal block. u se the colorgui de labels on the terminal blocktc insert the coJor-coded leads into the appropriate terminal.
145 (of 550 ) 2006(-2016)
146
As illustrated by the table below, Helium and Hydrogen have the highest thermal conductivities of any gases. The TCD detector responds to the difference between the thermal conductivity of the carrier gas and the analyte peak. The greater the difference, the better the sensitivity. For this reason, Nitrogen is only used as a carrier gas when hydrogen or helium is the target analyte. Argon is sometimes used as a carrier gas, but would have little sensitivity towards ethane or propane, for example, because the thermal conductivity of the argon ( 39 ) is very close to that of ethane ( 43 ) or propane ( 36 ).
THERMAL CONDUCTIVITIES OF SOME COMMON GASES Air 58 Argon 39 CO 53 C02 34 H2 419 HE 343 N2 57 02 58 109 Neon Methane 73 Ethane 43 Propane 36 Butane 32
Man200.pub
146 (of 550 ) 2006(-2016)
147
DETECTORS Flam e Ionization Detector - FlO
Overview The Flame Ionization Detector responds to anymolecule withacarbon-hydrogen bond, but its response is either pooror nonexistent to compounds such as H."S. eel,. or NfL. Since the FlO is mass sensitive, not " concentrat ion sensitive. changesin carrier gasflow rate have littleeffect on the detector response. It is preferred for general hydrocarbon analysis, with a detection range from 0.1ppm to almost 100010. The FJD's response
.
.
is stable from day to day, and is not susceptible to contamination from dirty samples or column bleed. It is generally robustandeasyto operate. but because it usesahydrogendiffusion flame to ionize compoundsfor
analysis. it destroys the sample in the process.
The SRI FlO features a un ique ceramic
ignitorwhichcan nul hot continuously, andprevent
•• FlO detector
(SRI Cap illary FlO GC with built-in Hydrogen Genera tor)
theflame from ex..r inguishingevenwithlarge water injections or pressure surges from column backflush. This ignitor is positioned perpendicular to the stainless steel detector jet and docs no t penetrate the flame. Oppo site this flame is the collector electrode. This positively charged metal tubeserves as a collector for the ions released as each sample componentelutes from the coJumn(s) and is pyrolyzed intheflame; it doublesas a vent for the FID exhaust gas. The FID is equipped with an electrometer amplifier wh ich has J UG H. HIGH(filtered), and MEDlli),1 gain settings. On an SRI GC, the hydrogen and air gas flows arc
controlled using electronic pressure controllers. Thermostatted Detector viewport
./ I .v ..
he ater block
~
~. / _'.
-.i ,~
t'l
Flameport
--
_10 ~
1
-
......
_
Collector
ii,;'-electrode
.
Ceramic
Elecuode lead to amplifier
~"'tor
FID. eliminatingbulky air cylinders. The built-in hydrogen generator is another option: the standard model ca n produce 20m U min for use as both carrier gas and FID combustion gas at p ressures
up to 25 psi.
e-
. ". -
, . ,, ~ -
AlrC . .
. ,~ · H 2 In
-lr"
which are user adj ustablcvia the GC's front panel. .'\.tbermostarred aluminum heater block main tains a sta ble detector tempera ture which is user adjustable up to 375"C. The optional built-in air compress or may be used to supply the air fix the
(rem ove S'N2gelok cap)
'J
Ampllfiergaln switch
147 (of 550 ) 2006(-2016)
148
DETECTORS FID - Flame Ionization Detector Theory of Operation In theSRIFlD. the carrier gas effluent from theGC columnis mixedwith hydrogen,then routed through an unbreakable stainless steel jet. The hydrogenmix supports a diffusion flame at the jet's tip whichionizes the analyte molecules. Positive and negati ve ions arc produced as each sample component is eluted into the flame. A collectorelectrode attracts the negativeions to the electrometer amplifier, producing an analog signal for the data system input. An electrostatic field is generated by the difference in potential between the positi vely
chargedcollector electrode and the grounded FIDjet. Because of the electrostatic field. the negative ions have to flow in the direction ofthecollector electrode. The FID hyd rogen diffusion fiame lnner flam e i py r:lly sis zone ,..:!
an d
carrier
.•.
~~~~:::~~t:t OUter I12.me ; cxi da bon zo ne
e f1\l.;e ~t
-" ' -
.
...-
:::Jectrostatic fieid
The ratioof air to hydrogenin the combustion mixture should beapproximately 10:1. Ifthe carrierflow is higherthan normal, the combustion ratio may need to beadjusted. Flowis useradjusted through the Electronic PressureControllers (EPe ): therates used to generate test chromatogramsat the factory are printed on the right side ofthe GC in the flow rate chart. The FID temperature must be hot enough so that con densation doesn' t OIXUC anywhere in the system: 150"C is sufficient [OJ" volati le analytes; for semi-volatiles, use a higher temperature. In addition musing the ignitor to lightthe flame, it may be le ft on ar an intermediate voltage level to prevent flameout (-75 0 or 7.5 volts). The ignito r is ve ry d urab le and will last a long time, ev en at high temperatures.
FlO detector schematic Hydrogen pee
F1e7l eport assemb'y
~_':_.o ,Y--FL%..Dt. =~
J
-_.-
Sample-laden earner pas
+
Pos tlVely charged
collector electrode I exhaust vent
),.Jli
ex"" . column Into jet
,If
;1
19n i!.:lr
_.
-
Compressed air
feeds nycrogen flame
148 (of 550 ) 2006(-2016)
149
DETECTORS Flame Ionization Detector - FlO
Expected Performance FID noise run C!
rs g
8
';
,!! : -h
ro
2 J
'f.
JI
RUt-:
Column: 15m MXT-l
Carner-Hefrum@ 10mUmin FlO gain = HIGH Fro tem p = l5O"C FlO ignitor = -400
I
;0(1
~ va~ c-=--- ~= =:::::;=:\/1 '
Temperatureprogram: Initial Hcld R
FID noise averages less than
100~V from
peak to peak
Final
roc
~IE'--------------------------_--J
±l!J a ce
C -C Hydrocarbon Test Analysis 1 6
r:-b ~ r;;rD _ a: ",, ~ s ,If~ lQOC P ~M
c
~.:l. :IOO
...
..
~
, z • '!\ r~· 1"\-
;l4 ~ ~. "'-'<.
3
}
Ar,fi>, .. . -
sur....- .f
!
ET"""'!
I I
f
.!ll.W..J 0.0"
r~
d
,
,
I\
I,
..
.:..;. ;
"
.-..
I,-, ,,
,I, ,
S-
-:F.<.aoa
/"!,,Ifr. ,.(I"... "l
('f\J'v:., '--_. ,.
II
"'l'K~.N E
!
D .'-
co"
~M1E
i
;
,
j
Sample: 1mLof 1000ppm C,.C6
.
.
Carrier: Hellum@ 10mUmin FlO H2at25psi = 25mUmin FID air at epei ... 250mUmin FlO temp = , 5O"C FlO ignitor = -750 FlO gain = HIGH Valve temp = 9O"C
R_u ~ '
Q;:mpon~!'It
\
-~ E""~
\
-~ ""'.~
",,"",0.
I
He xane
.850
A re a 69799260
2866 5 6<13
13623.7580 19535 8960
Rel
8200
10.283 12.916 Tot i!ll
26456 5980
330539680 394 19 0S7C 1390692330
.T·T·I 16.000
149 (of 550 ) 2006(-2016)
150
DETECTORS FlO· Flame Ionization Detector
Expected Performance
BTEX Test Analysis
The BTEX chemicals (Benzene. Toluene. Ethylbcnzcnc, and Xylenes) are volatile monoaromatic hydrocarbons fo und in petroleum products like gasoline. Due to indus1.r:iaJ sp ills andstorage tank leakage.the.y
are common environmental pollutants. Groundwater, wastewater, and soilarc tested for BTEXchemicals in m any everyday situations . The chromatogram below was obtained using an FID-equipped S RI GC.
!B Ve,','U El~
I
c:
..
i; CIl l!_
~!iiI IZl
4e
a , ':J, filT.'l
Ul, ~~ ~"'" llTErrti
S12.000 ,...-13"~
,.....
Z 3
4 '.co
I!!!IIiIEJ
•
~
~
h ft, 1'< f:to. /$>b f ~ ,Pi\. ~ . -") .;.r
fU
",-,- .
"
1IJL 100ppm BTEX sa mple 15m MXT-VOL capillary
column
, n <,
i\
, ~,
FlO S3in::: HIGH FlOlemp = 1 50~ FlO ignrtor = -400
1\
.St.lXL-- - - - - - - - - -- - - - - -- - - - - .J , ' '-F I I , ~
' 1' 1" ----ra
•
Re sults :
Component
Rete~tion
Solvent Benzene TeE
0.433 2083
2.700 4.183 PCE 5.000 Ethyl Benze ne 6.233 Ortho Xylene 6.900 7.150 Bromofonn total
TOluene
Nee 95879.7560 83 7.10 00 319.2450 1070.1060 34486.40 1200 .3320 1312.3070 225.2360 101188.9460
150 (of 550 ) 2006(-2016)
151
DETECTORS FlO - Flame Ionization Detector
General Operating Procedure 1. Set the FID amplifier gain switch to I-llGH for most hydrocarbon applications. Ifpeaks of interest go offthe scale (greater than 5000mV), setthe gain to MEDIUM. When peaksofinterestare 20 seconds wide or more at the base and extra noise immunity is desired. set the gain switch to HIGH (filtered). Thissetting broadens the peaks slightly.
..,-•
0" ,
I f,
;.,',' P• •FiER ~--==
•
FlO amp lifier ga in switch
2. Set the Fill hydrogen flow to 25mUmin, and the FID air supply flow to 250mL/min. The approximate pressures required are primed in the gas flow chart on the right-hand side of the Gc. 3. Ignite the FID by holding up the igni tor switch for a couple of seconds until you hear a smal l POP. "The ignitor switch is located on the from panel ofyour SRl GC WIder the"DETECTOR PARAMETERS" heading (it is labelled vertically:"FIA .i\ fE IG~.
4. ve rify that the FID flame is lit by hol ding the
.
.
shinvsideofa chromed wrenchdirectlv in front of the collecto r outlet/Ell) exhaust ven t. If condensation becomes visib le on the wrench
surface,the flame is lit
5 . Ifyou wi sh to keep the ignitor 0 7\'to prevent flameout. set th e igni tor vol tage to -750 by a djusti ng th e trimpot on the - FLAME IG~1TE" LOne with the supplied screwdriver.
151 (of 550 ) 2006(-2016)
152
DETECTORS Flame Ionization Detector - FlO FlO Troubleshooting \\ 'benever you experienceprnblems with your FID. review your operating procedures: check thedetector parameters, check to make sure )'OU are on the correct channel of the data system display,check the mixture of'hydrogen (25mU min) and air (250mUmin), check gas pressures and connecti ons, check the oven and detector temperatures. and all the other variables that compose your analysis. Having ru led out operating procedure as the source ofthe problem, there are [yvo simple diagnostic tests you can perform. Detector problems can be electrical or chemical in nature. Use-theFlame ON/OFF testto helpdetermineif the problem is ofchemical origin. Use the Wet Finger test to determine if the problem is electrical.
A. Flame ON/OFFTest
- -
-
1. Extinzuish the flame b... rumina off theair. 2. Usc the "Tench test to make sure the flame is OFF. If it is. o bserve the baseline in the chromatogram windowto see whether there isan improvement or no change at all. 3. lf baseli ne noise and high background disappear wi th the FID flam e OFF. the problem is chemical in nature.
4. Isolate the column by capping oil the: column entrance to th e detector with a swagelok-type cap or a nut and septum. Tumthe air back onand light the FID flame. If the detector noise is similar to the background that was observed wi th the flame
OFF, the column is suspect. B. Wet Fi nger Test
I . Make a V sign with the first rna fingers ofyour right hand.
2. Moisten those two fingers (you can achieve sufficient moisture by licking them). 3. Place one finger on the collector electrode. and placc the other on bare metal (like the Fill detec tor body or the column oven lid) (0 ground the co llector. Make your contact brief-yo u need only brush o~e/ finger here and these parts to perform the test. Be careful not to bum yourself; the . . column oven lid is probably cool er i~' - the cther fmger here than the FJD detec tor body.
1
{
tit
I ','
.
...
,:.,;,
5. Observi ng the milliVolt reading on the screen. If your
contact makesa significant change in the millivolt reading, then the FID detector electronics are working. The data systemsignalshouldjump fromzcroto themaximumvoltage (5.000mV). then come back dO\NTI whenvou . . remove .vour fingers,
152 (of 550 ) 2006(-2016)
153
DETECTORS FlO - Flame Ionizatio n Detector
Cleaning the FID The Fill detector rarely requirescleaningor servicing. It maydevelopa film or coating ofcombustion desposits in the Ilameport with extended use. Use the FlO detector vie wport to check for visible deposits. If you're experiencing problems with your FlD detector, try cleaning it. even if you can't see deposits through the viewport.
1. Unscrew the viewport capnutand examinethe flameport interiorfur coatings or films. Ifresidue is found. thecollcctorelectmde and the flameportwili needcleaning.
2. Remove flarneport assembly from the heater block a. Disconnectthe fl O air supplyline at the 111 6" bulkhead fitting.
_ c_ :=1 _
b. Using a philps headscrewdriver, remove the SlTC\N on the top
-~-£':EI'-
cf'the FID "s heater block and pull the aluminum cover up and
off.
[I
c. Gently pulloffthewhite insulation to reveal the detector's bulkhead fitting on thecolurnnoven wall. Loosenthisfitting to disconnect the flameport.
l-
m
-+) "1 -
I
._ -
1
~. _
-=~:ar-- =:=::
" l
3. Remove the collector electrode
a Undip the electrode lead terminal and slide it ofT the electrode.
b. Loosen and remove the nut and ferrule that hold the collector electrode in the flameport body.
c. Slide thecollectorelectrode out of the nut Once removed. spin it between your fingers in a piece ofsandpaper to clean the
stainless steel surface. A wire brushmay also be used to scrub the electrode. Once cleaned. set it aside with the ignitor.
153 (of 550 ) 2006(-2016)
154
DETECTORS Flame Ionization Detector - FlO Cleaning the FID continued 4. Removethe FIDignitorelement a. The ignitor element is brittle and will break \...'hen stressed, so hand le the ignitor carefully, mindful ofany torque on the blades. While holding the ignitor by the ceramic bod y with one han d. loosen the 1/4" sw agelok-type nut th at ho lds it in plac e. There is a g raphite fe rrule in sid e thi s nut that se cures the Ignitor body -
ceramic ignitor body whenthe nutis tightened.
b. Carefully pull the ignitor- down our o f the flameport. Disconnect the ignitor L from the spring-loadedignitor curreru source terminals. Set the ignitor securely aside.
-
-'
FID ignitor removed from the f1ameport asse mbly
5. U se a wire brush or a sharp obj ec t to remove any resid ue from the Ilameport interior. then rinse it with
so lvent (methanol or methylene chloride), and bake it o ut in the GC 's column oven at 2500C' for 10-1 5
---.....-
minutes.
Scrace. rinse, and ba ke out the FlO ftameport interior
a Once all the FID parts arc cleaned, reverse the disassembly process, starting with the replacement ofthe ceramic ignitor. Leaving out t he cleaning steps,yow last step should he reinstalling the flamcport assembly onto the heater block. Make sure to position the ignitor so that the blade is slightly below and angled 1O~ 15°toward the jet's tip so that th e ignitor wi ll not interfere with the flam e or creat e turbulence.
Fro ignitor removed from
ee flame port; note the
I
Use the v iewport to correctry position the FlO ignitor and collec tor e tectroce inside the narneport VIEW
I
slight angle of the blade
element
[Eli Ignitor blade must not
•
~
A~,
touch FlO jet
Positon the collector electrode SO mat about 1 18~ of It is visible through the viewport
I
154 (of 550 ) 2006(-2016)
155
Th ere are situations where it v.oold be helpful to 0pera te the FlO detector using j ust the built-in air compressor for carrie r gas and no other gases. SR I d istributo rs demonstra ting the GC and softwa re may find it usefu l to run live chromatograms without the inconvenience of providing hydrogen and hel ium . Service personnel troubleshooting other GC fu nctions may be ab le to test the GC witho ut gases, and under some circumstances . the response of the f1ame less ionization detector ( FliO ) may actuall y be useful for non-quanntauve applicatio ns. The Fl O detector is norma lly located on the right hand side of the column oven. The FlO normally requires a flow of 20-30 mrrrun of hyd rogen and 200·300 mVmrn of air to support a hydrogen flam e at the tip if the jet. The heat of the flame ionizes the analyte molecules, and the neg ative ions allow a sma Uelectric current to flow between the col lector electr ode and the grounded flame jet The ignitor normally se rves only to ignite the flame.
The FlO detector body is show n at right in the norma l configuration, but removed from the detector hea ting block on the GC for clarity.
Inside the FlO de tector body, the ignitor is norm ally positioned just below and behind the tip of the jet Notic e tha t the ignitor blad e is ti"ed at a 15 degree angle fro m the ceramic tube in which it is fabricated . In normal FID operation. the ignitor is posit ioned below an d behind the jet so it wi ll not disrupt or distort the flam e , yet clos e eno ugh to easily ignite the h ydrogen/air mixture.
Man l4 3.pub
155 (of 550 ) 2006(-2016)
156
In the FlID mode. the ignitor itself provid es the hea t nece ssa ry to ionize the sample molecules . Accordingly. the ignitor need s to be pos itioned directly in front of the jet The slight angle of the ignitor allows the ignitor tip to be located 1-2 mm in front and slightly a bove the je t The ignitor is held in place by a soft graphite ferru le and a swag elok nut Be careful when manipulating or twisting the ignitor beca use the ign itor bfade is very brittle ceramic. and wi ll snap if stressed. Replacement ignitors are available using pa rt# 8670-0150. The ignitor temperature must be raised so that it glows red hot set the FlO ignitor volts to at least 900 -1000 using the fron t panel FlO Ignitor control. A Chromatogram of gasoline is shewn below wh ich wa s run using the H ID mod e. Only the larger gasoline co mponents ( > 1000 ppm ) were detected. Se nsitivity is exponen tial due to the tem pera ture rise that occurs when the peak combusts on the ignitor surface . Large pea ks whi ch elute quickly may cool the ignitor resulting in spirt peaks .
1ul Gasoline injected onto 30 meter .53mm capillary column using air carrier gas from the bunt-in air compressor.
,
n
J Manl 44.pub
156 (of 550 ) 2006(-2016)
157
To convert the FID detector to NPD detector: 1) Th e Fl O and NPD detectors are almost identica l. Th e detector body is mounted on a heated aluminum block on the righ t hand side 01 the GC oven. Th e NPD body is slightly differe nt fro m the F lO in that the NPD flame j et does not protrud e as far into the detector body as it cces on the FIO_ Th is auows th e NPD tberrnc nc bead to be positioned directly in front of the je t Remove the FlO body from the heated aluminum block and repla ce it with the NPD body.
2) Th e photo at right shO'NS tne FID/NPD detector body and both the Fl O ignitor and NPD thermionic bead side by side for comparison. Both the FlO ignito r and NPD thermionic bead are inserted into the de tecto r body from the bottom. The ignitor is inserted until the tip of th e ignitor is just below the tip of the flame jet wh ile the NPD bead is in serted until the heated part of the bead is directly In front of the fl a m e jet For NPO operation , the sample molecules m ust co llide with the bea d In order to be ionized and detected.
3) T he gas flows to the NPD detector are different than the FID gas flows. The NPO hydrogen flow is normally about 3 mllmin while the FlO hydrogen flow is about 25mVmin. To obta in this lower H2 flow rate , an add itional restrictor coi l is attached to the hydrogen bu lkhead fitting im med iately below the detector body. W ith this additiona l restnetor coil in place . 10 psi hydrgen pressure will result in a flow rate of abo ut 3mVm in. T he NPD air flow rate is typ ica lly about 100 mllm in, but this flow rate ca n be achieved by simply reducmg the air pressure from 8 psi to about 3 psi.
Man l 28 .pu b
157 (of 550 ) 2006(-2016)
158
.
.
~~-~~
~. r
"
.
~-
' . ~"",,~:,: .
'.""'~ ~--
ca.
-' -""~--
To convert the FID detector to NPD detector:
4) The NPD bead plugs into the push terminal block on the GC directly beneath the d etector. The te rrrunats are labelled FlO Ignitor because tI1is is where the FlO ignitor is normally connec ted.
5) Because the NP O bead can only tolerate a maximum vo ltage of --4.50 volts, be careful not to set the·-l~~~;i~ Fl O 'letts setpo int higher than -4.50. Be especially carefu l no t to flip the FlO ignite swrtch to the up posttion , as this will apply 10 'l o fts to the NPO bead and bum it out When an NPO de tector is ordered seperatel y from the FlO , the NPO 'letts are automatically limited to --4.50 volts ma ximum. But when the Fl O and N PO share the bead/ignrtor CIrcuit. the operator must be ca refu l not to apply more voltage than the bead ca n to lerate
Man l30 .pub
158 (of 550 ) 2006(-2016)
159
POPULAR CONFIGURATION GCs BTEX & Environmental System Overview YourSRl Environmental GCis equipped with eo.~)'OO need to gcacrarecertification quality data forEPA Methods 8010, 8015, 8021, andothers. It is configuredonthe 86 lOC chassis. and includes a built-in Method 5030 OJ"503015035 compliant Purge & Trap for concentration ofliquid end/orsoil samples. Also included is an on-columninjector tor direct liquidinjections. Todetectcommonly targeted pollutants, the Environmental GC uses a sensitive, non-destructive PID detector inseries 'With a combination FIn/DELCO detector. Th e Pill det ector responds to compounds whose ioniza tion po tential is below l O.6eV, including aromatics and chlorinated moleculeswithdouble carbonbonds. TheFIDdetcctorrcspondsto the hydrocarbons in the sample. The DELCOselectivelydetectsthe chlorinatedand brominated compounds in the FID exhaust Since the sample is pre-combusted in the FID flame. the DELCO is protected from contarnmation due to hydrocarbon overload. The PID is blind to certain
fiI
.....
,
methanol, and isrecommended by the EPA.. P eaks
on the FID chromatogramthat are obscured by the methanol peak are visible on the PID chr omatogram . Benzene and carbon tetrachloride arc common target analytes whichco-elute, TheFIDresponds to bolh. The PIDresponds only to benzene. while the DELCO responds on ly to carbon
r-
Mel:hcx:l 5030
Purge & Trap
.
~
teeachlcride.
!I l
The BTEXGC is the sameas the Environmental GC without th e DELCD detector; Both systems have a " whisper qui et" internal ai r compressor and can be used with an H 2 -50 hydrogen generator for tankless field operation.
.
lE~
On- Column Injector
compounds whichcancauseinterference. such as
80m CapHlary Column inside Co~Jmn Oven
Method 5030 Purge & Trap carbo s fe v e w trap positbn ed for shippirrg"
Method 5030/5035 Purge & Trap on an Environmental GC
(blan k: and Tenax ....GR traps are be hind
the f a n. un de r the prctect ve grill )
Syri nge Port
10 Port Val ve in thermostaUed
vevcoven
i~c ~lI!:I~'1
~~.
' \'~ .
. \ ... . -' '" '-, .... .\~ '\~ \'--,\'" ~ .'
~"-'- -
-- '"'"'"
Cooling fan
5035 Purge Head with 'tbe-rrcstanec Sleeve
159 (of 550 ) 2006(-2016)
160
POPULAR CONF IGURATION GCs BTEX & Environmental
Theory of Operation
PURGE & TRAP
I I
~
i FID/DELCD LIQUID PID "INJECTION f-~ CAPILlARY'r- ---:~ DETECTOR i----c7 ~: COMBO PORT COLUMN DETECTOR
I
The versatileBTEXiEnvironmental GC systemscan analyze gas, water, and soil samples. Four-types of injectiontechniquescan beused: purge andtrap, direct liquidinj ection, TQ-14 type gas sample concentration, and manual hcadspacc injection. The Purge & Trap concentrator m ay be used for gas, liquid, and sol id samples. For liquid samples up to Sul, and gas samplesupto ImL . direct injections can be made through the on-column liquidinjection port Larger gas samplescan be injected through the syringe port onthe 5030/5035 Purge & Trap concentrator or the septum port on the 5030 model.
Purge & Trap Injection
Designedfor -compliance with EPA Methods 5030 and/or5035, thePurge& Trap systemextracts volatile organic compounds from the sample solution in the rcstrubc or VOA vial. Using a dual trap design plumbed with a 10port gas sampling valve, the Purge & Trap system enables the use oftwo separate adsorbents with different desorption temperatures for a wide range of target anal ytes. Each trap is heated independently.
10 Port Valve in LOAD
10 Port Valve in INJECT
,
,
~ samPJe ~ '/
When the valve is in the LOAD position, thesample-ladenpurge gas from the test tube or VOA vial is directed through the two traps, then out to vent, loading the traps 'With sample at the adsorption temperature. The traps are heated to their respective desorption temperaturesshortly after purging is stopped. When the traps reach desorption temperature, the valve isactuatedtothe INJECf position. In this position. the carriergas backflushes through the traps in the direction opposite to the sample-laden purge gas flow with WhICh the traps were loaded The carrier gas flow sweeps desorbed anafytcs into the column. while flow from the purge vessel is stopped by the PeakS imple data system.
160 (of 550 ) 2006(-2016)
161
POPULAR CONFIGURATION GCs BTE X & Environmenta l
Theory of Operation continued Direct Injection Direct injection with the BTEX orEnviroemcntal GC systems is simple andstraightforward, This method uses the on -col umn injector to inject the sample directly into the column, bypass ing the entire purge and trap inj ection system. Sample size far this technique is ImL orless for gas, an d Sul, orless for liqu id Nocvenr
table is necessery.just a temperature programfor -the column oven. Gas Sa mple Conce ntra tion In this TO- I 4 type te chnique. a large volume o f gas is pushed by syri nge or pulled by vacuum p ump through the dual traps. The trapped analytes are then desorbed and swept into the column. Ifthe GC has the optional vacuum pwnp interface, the pump is plugged into it and may be controlled by the PcakSimplc da ta
system using anevent table,
Room Tem perature Manual Headspa ce Injection
When naking bcadspacc injectionswitbthe BlEX or EnvironmentalGC systems. thesample is equilibrated o ffline at room temperatu re. It is the n injected by syringe into the on-column inj ec tor. This technique is basically the directinjection ofsmallgassamples.
VOA vial and 1mL syringe with 27gauge need le for manu al headspa ce inj ections
--
Q
"' - - - _ -:-- '-=--'":';
<::
""
Q-- - . ,,,- ~
-~
-
'"'
~ ~_o
..
"" .,.
- -
~
~ --
161 (of 550 ) 2006(-2016)
162
POPULAR CONFIGURATION GCs BTEX & Environmental
General Operating Procedures EPA Style Purge & Trap Injection This technique is limited to volatile organic compoundsthat purge efficiently from water at ambient temperature and VOC 's that are purgeable from soil at 4&'C. Sample preparation depends on the sample type, concentration. amount, etc . 1be third edition ofSW-846:from the EPA is accessibleonthe Internet Go to http://www.epa.goYfepaoswe r/hazwasteJtestlmain.hbn and cl ick on theSOOOSeries link to dovm.load
Methods 5030 and 5035. Also, please see the "Sample Preparation" page in the SRI Purge & Trap manual section (available onlineatwwwsrigc.com). 1. The purge gas flow is controlled with an Electronic Pressure Controller (EPC). Set the purge flow (measurable at the trap vent at the rear of the purge and trap system); 40mUmin is a typical purge flow. The pressure required for 4Oml/min through a single Tenax trap is printed on the right panel of the GC. NEVER use hydrogen as apurge gas. SRI recommends helium purge gas .
2. TRAP 1 is in the lower position in the Purge & Trap, and TRAP 2 is in the upper position. The trap temperatures are factory set at 200"Cfor desorption. For adsorption temperatures, trap I is set at 3O"C and trap 2 isser at 35"C. Trapheatingwillbecontrolledby!hetimedEVCIll Table duringtacnm, NOTI:: theactual temperaturestypicallyrun5"Cover!he setpOint. Seethe instructions in the Purge & Trapsection ofthemanual for adjusting the trap adsorption temperature settings. 3. Load or create an Event Table that is appropriate to the samp le to be analyzed, or that is desig ned for
compliance with a particular EPA Method (such as Epap&t1c.evtfor a single trap or Epap&t2c.evt forduaI trapsincluded in version 2.66 or bigherofthe PeakSimple software). 4. Load or create an applopriate Temperature Program forthe column oven. Epap&uemis a typical Purge & Trap temperature program file provided w ith the PeakSimple software for your convenience. As a basic rulefor goodseparation using the purge and trapinjection technique. the columnoven should bekept at4O"C for 10-12 minutes: 6 minutes while tbe sample is purging, plus 4-6 more minutes whilethe traps heatand the gas sampling valve (in the INJECT position) transfers the sampleto the colwnn. EPlIp&l1c.tM EVENT
EVENT TIME
Dual Trap EV81t TatlIe t: Pap&l2l:.fI\I! 1
E "eM" E- O Ff'"
P .. g.-Of F"'
• COO
c-or-
T, ,,,, Z (I'lN t;I"O N"
e. DO
, "eM"
T,,,,, 1 (hu t) "Otr
E.COO
G " ON"
V.i Ml in "INJ EC T"
12Jl:lO
E "ON"
Pvrg. "W
" 010
G "Orr-
VI "'" W\ -LOol-D-
"DO
E " ON"
TI.. p,.et · CN' (...~ )
,.."
r -or r-
Tr"" 1 " OF"' .
"or r"
1" .0::0
I:
C -crr-
""'"
8
-c rr-
.=
P..-g." ClN"
'DO ' DO
15.100
EV'E ~n ' I~ E
EVENT FU NCTION
P"S _ "OF F" Tr~
Trap
2 -ce s-
~.t · Of ""
(+0)
.m ,m
Epap&t1c .cvt is designed klr onetrap, whi le Epa p&t2e.evt
is for two traps.
l:' ~J
,,= 13.0:1
EVENT f IJNCT!CN
~~
z.,. <. .. 1
, .~
~ uv
E- Q<1·
.= .= a.m
.= ,,=
~"
e 'eM' ,.~
,~"
G" O"'''
' "~
..
' "~
"'"w,.. ~
-crr-
~
. .,.·or'"
T.. , 2 CC " """""l '-~ "CIIl" "".... ,• .....n:;CT'"
T.. , I (T...... G R) Ioo~·O'I" V_
In'l.OAll "
va... I"
"f,lJ£ C"
P"I"~II' ·J_ Iro ·~ '
ft.
'01 .CH" ('o~ )
,.~
f
1!.CCO
E ' OW
I"UJC. " UH '
e-ere-
lI'u 2
1~
ee
,,=
S "Y , '
ft., , - ~ f"
-e»f"
T...... · <:f"F""
162 (of 550 ) 2006(-2016)
163
POPULAR CONFIGURATION GCs BTEX & Environmental General Operatlng Procedur es continued Direct Injection This technique is uscfuI forvolatileandsemi-volatilecompounds,butistypically usedfordiesel and other compounds that don't purge well from aqueous orsoilsamples. 1. Perform Det ector Ste ps 1-4, then proceed with step two below.
2. Load or create a Temperature Program forthe column oven. Youcan
P IDdelecto r bypass for co lumn oven temperatu res above l5O-'C
crea te an isothermal or ramped temperature program; deciding which to use depends on th e sample be ing analyzed. and thegoalsofthe analysis.
There are several preset .tern files. included with version 2.66 andhigher of the PeakSimple software. If the analysis requiresthe column to be hotter than 15O<'C, it is best to disconncctthe column from the PID detector. The PID represents a cold spot in which
-
higher bo iling auelytcs will become / trapped, never making it to the much ho tter (3000C) FlD f OT detection. The ooIumn is inserted d i~dly into lhe FID, bypassing the PID_ Also. when the column is healed over l 5O"C. stationary phase bleed wi ll adhere to the PID Iarnpvvindow The higher boiling analytcs and the colunm bleed will create a coatingon the Pill lamp window that will interfere with the analysis. The PID lamp window may be cleaned in the event of contaminant condensa tion, but the resulting change in the PID response u.~sually requiresdetector recalibrarion. To bypass the PID. turn its 13mI' current OFF. then disconnecr thc column from the detector by loosening the swegelok-type nut from the butkhcad fitting in the column oven waIl Remove the robing that connectsthe PID exit to the FIDID ELCD by loosening that nut. Place the end of the column into the FlO/DELCO bulkhead fitting instead and tighten it in place.
3. While the detectors are heating and stabilizing. prepare a diesel sam ple by shaking a known weightofthe sample with a measured volume ofrncthyJcncchloride for 1·3 minutes. Allow any particulates to setde before drawing the samp le into the syringe. 4. Usc a clean. standard glass lOJ.lLGC syringe witha 26 gauge needl e. Fill the syringe with sample. and work out any air bubbles. Depress thc phmgeruntiI IJlL ofsamp le remains inthe syringe. S. Zero the data system signal by clicking on the Auta Zero button on the left side ofthe chromatogram wi ndow. Or. mak e the first even t ZERO (at tim c O.OO) in your cv cnt table.
6. Beg in the analysis by pressing the Rl;'N button on the GC or the computer keyboard spacebar.
!iAut02ero bu!!Dn
7. Quick ly and smoothly insert the syringe needle into the on-column injection port, and imrncdietclydepress theplunger;
163 (of 550 ) 2006(-2016)
164
POPULAR CONFIGURATION GCs BTEX & Env ironmenta l
Gen eral Operating Procedures continued Gas Sample Concentration This TO-14 type technique injects a gas or air sample usingeither a large syringe (60mL) or a Tedlar bag ( IL). A vacuum purnp maybe used topull the sample throughthesorbenttraps. The amount of sampic that may be loaded onto the trap(s) is limited only by the capacity of the trap's adsorbent packings. The more gas that is loaded onto the traps, the lowe r the detection limit will be. ThevoJume andflowofsampleand carrier gasthat can be fro through thetrapswithoutadversely affecting the resulting chromatogram is known as the breakthrough volume. Different adsorbents have different breakthrough volumes. A breakthrough volume value is determinedby the sample and target analytes, the adsorbent packing (pore size, natural affinities for certaincompounds,etc.), the diameter ofthe trap, and the temperature at which the traps are loaded. Therefore, a given trap 'Willhave different breakthrough volumes in diffcrcntanalvtical condition". The SRl Purge & Trap concentrator is shipped with a blank trap and a Tenax™-GR trap installed, and a Carbosievel" Sclll packed trap for optional user installation. TheTenax-GR trap has a low affinity forwarer, making ita good ad...orbcnt forthcpurgc and trap technique. TheCerbosieve has a high affinity forwater, and is generallyhighly retentive; SRI recommends usingit only whenvinyl chloride is among the target analyres. The blank trap is provided forthe user to pack with the adsorbent ofchoice. Using a syri nges I. perform DetectorSteps 1-4. While the detectors are heating and stabilizing, load or create an event table. The valve (RelayG) must be in the LOAD(G OFF) positionwhile analytesarc being adsorbed onto the traps . The valve is rotated to the INJECT (G ON) position during desorption. See the valve diagrams on the EPA Style P urge & Tra p Injection Th eo ry of Operation page. Relays C (trap 2) and F (trap I ) a ctivate the traps ' heat The relaysmay also be activated bythe operator duringan analysis: open the Relaylpump window and click on the letter corresponding w ith the relay you want to rum ON or OFF. 2. Inject the sample into the 5030 septum nut or the 5030/5035 syringe port. Alternatively, the 5030 purge head may be removed by unscrewing nut b, allowingthesampleto be inj ected directly into the bulkhead fitting on the front ofthe valve oven duet (seethe photo. below right). Depending on the syringe you're using, you may have to make an adaptor for injection intothe purge head..
3. Loador createa temperature programfor the columnoven Oncethe detectors are activated andstabilized, beginthe analysis. Using a vacuum pump: 1. Connect the vacuum pump to the trap vent on the backside ofthe valve oven. 2, Ifyour GChas the optional vacuumpump interface installed, plugthe vacuum pump into that power socket on the left panel ofthe GC chassis. Enter events in the event table to tum the vacuum pwnp power ON and OFF as desiredduring the analysis. IfyourGC doesn't have the vacuum pumpinterface, plug the vacuumpump into a wall outlet instead, and control it's ONI OFF switch manuallyduringthe analysis. 3. Once the detectors are activated and stabilizcd, connect the Tcdlar bag to the purge head septum nut (a ), or remove the purge head and secure the TedIarbag to the bulkhead fitting in the front valve oven duct [To remove the purgehead: loosen the nut (b) that securesthepurse head to the bulkhead fitting in the valve oven duct wall. Loosenthe nut (c ) that securesthe purge head to thepurge gastubing. Leave th~ second fitting(c ) on the purge gas tubing and slide the purge head offof them bing. Sec the photo, above right ] Load or-create a temperature program. Begin the analysis.
164 (of 550 ) 2006(-2016)
165
POPULAR CONFIGURATION GCs BTEX & Environmental
-
General Operating Proc ed ur es continued Room Temperature Manual Headspace Injection L In this technique, thesample Isequilibratedoffline, Transfersamp lcintoa cleanVOAvial untilthevial is half full. Let it set at room temperature for 30 minutes to an hour to equilibrate.
2. Load or create a temperature program for the columnoven. 3. Perform Detector Steps 1~4. then proceed wi th thefollowing steps. 4. Filla plasticmedical syringe with the vial beadspece. Injectthe sample into the GC injection port. bypassing the Purge & Trap concentrator. 5. Begin the analysis by pressing the RUN button on the GC or the computer keyboard spacebar.
Nore: both the sample vialand the syringemay be heated for the injection of warm hcadspaccsamples.
40ml VOA vials are ava ilable from Eagle Picher under part nu mber 14Q-4OC/EPJES.
Disposable, sterile l mL syri nges are a va ilable in packages of 100 from Aldrich urder catalog number Z23072-3. 'Zl gauge preceon glide needles in packages of 100 are avajebe under catalog number Z 19237-6 .
1-800-331-7425
1-llOO-558-926O
Detector Steps I. With the black plastic lamp hood in place on the PID lamp, rum ON the PID lamp current with the flip switch on the GC 's frontcontroJpanel. Settbe PIDcurrent to 70 (= 0.7Omal by adjusting the appropriate trimpot setpoint on the top edge of'thc GC's frontcontrol panel. (Each detector zone is labeled on the front control panel under DETECTOR PARAMETERS, with the corresponding trimpot sctpoint directly above it) The lamp should emit a violet-colored light visible down the center of the lube. Set the PID temperature to 150"C. Set the PID gain to LOW. 2 Tum on the air compressorusing theswitch ontbc GCs front control panel. KOTE: since mostambient air will not cause interference with the DELCO. the built-in air compressor is appropriate for most analytical situations. However. if you aredoing analysesin a labenvironrnent with low lcvels ofhelogenated compounds in the ambient air, they can cause the DELCO to lose sensitivity, and f luctuations in the level oforganics in ambient air may cause additional baseline noise. To avoid this, uscclcan, dry tank air.
3. Set the FIDhydrogenflowto 25mUmin. andtheFIDair flow to 25OmUmin. The pressure required for eachflow is printcdon tbe righthandsideofthc GCchassis. Ignite the Fill by holding up the ignitorswitch for a couplc ofseconds until you hear a small POP. Ensure that the flame is lit by holding the shiny surface ora chromed wrench to thetip ofthe collector electrode: whenthe flame is lit, you should be able to seecondensation on the wr ench. Set the FID gain to HIGlL lf the pcaks are more than 20 seconds wide at the base, usc the mGH FlLnRED gain setting, Ifyou wish to keep the ignitor ON to prevent flameout. set theignitor voltagc to -750 by adjusting the trimpot on the FLAME IGNITEzone. 4. If a DELCO detector is installed, set the DELC O reactor temperatu re setpoint to 260 t- 1OOO"C) by acljustingthcappropriate trimpot. The DELCO will heatto around 254 and stabilize: the protruding end ofthe ceramic tube will glow bright red in the heat Set the- DELCO gain to LO\\'. 5. When the systcm bas reach ed tenperanrre andeach detector-is displaying astable signal. beginthcanalysis by pressing the RlJN buttonon the front of the GCor the spacebar on the computer keyboard .
165 (of 550 ) 2006(-2016)
166
POPULAR CONFIGURATION GC s BTEX & Environ ment al
Expected Performance - Purge & Trap Concentrator Thesechromatograms were producedfrom a 1Oppb BTEX Plusstandardanalyzed in anEnvironmental GC equipped with a Method 5030 Purge & Trap injection system. The simultaneous display ofall three detectorchannels illustrates their relative selectivity. The chromatogram on the next pageshows thecarry-over from th e Purge& Trapconcentratoron the subsequent analysis
_ra , st
I
,. •
t
•
j
•
i
I
!
"••
~
f
,
~
I
,
f
~
~
U ;S
., I •
H
FID Results:
PIC Resu lts:
Com pon ent
Rete ntio n Area
SoIv,m t Benzene
10.6 16 15.033
921.0990 1019.9260
TeE
15.883
441.5 700
Tolue ne pe E Ethyl Benzene OrthoXytene Bromoform
17.683 16. 700 20 .016 20.800 21.166 Tola:
1195.3320 383.3770 1247..3420 1258.9260 78.9360 5546.8080
Sa rrple: 'lJl100ppmBTEXPlusstanda:d
d:ssdved in 10mL cr.. .rate- to yield 10ppb of _ m l'iIl".<'Ilyte
Met"\Od: 5030 P&T injection
Column: 5O:n MXT-VOL Carrier: Helium@ 10rnUmir:
Com ponent Be nze ne
DELCO Results: Rtlte nlion Ivea 15 .0 16 3 11.1630 15 .866 2 58.436 0
TCE Tolue ne 17.666 p eE 18.683 Eltlyt Benzene 20.000 OrthoXylene 20.783 Brcmcfcrm
353.21 60 233.4 780
21.133
34 3.9540 350.7040 32-3470
Tota l
1883.3080
Temperature! Program: (E;:mp&Uem) Ini tial t**1 ~ Final 4O'C 10.Xl 10.00 18O'C
Component Rl! tention Area
TCE PCE
15.883 18.683 Bromoform 21. 150 To tal
192.1020 209.2260 120.2820 527.6100
Events (5030.evt); Everts Time
O.oeo
ZE.~O
0. 100 5.100 6.000
E ON (PURGE GAS)
E OfF C ON (TRAP 2 HEAT)
6. 050
F ON (TRAP 1 H EAT)
8,000 12.000 12.900 13.000
G ON (VALVE INJECT) EON BON {BAKE) G OFF (VALVE LOAD) FOFF
1~ .900
15.100 COFF 15.300 E OFF 15.500 B OFF
166 (of 550 ) 2006(-2016)
167
POPULAR CONFIGURATION GCs BTEX & Environmental
Exp ec ted Performance - Purge & Trap Concentrator This chromatogram was produced from analyzing a water blank immediately after the analysis ofthe BTEXPlus standard to showthe PUTgc & Trap carry-over. The blank was run under thesame conditions (everrrtable, tempcratureprogram,detectorsettings) as the sample. Acceptable carry-over-is a contamination level o f 1% or O.5ppb-whiche,,·er is lower-ofan ena lyte (especially high boiling components), and is a normal condition ofoperation. This I %of contamination from preceding analysesshouldnot be significant enough to affcetquantitarionunless a veryhighconcentration sample is followed by a very lowconcentration sample. It is standardlaboratorypracticeto run a blank aftera high concentrationsample. Toluene is used as a representative of the carryoverin the Purge & Trap system; if thecarryover levelofToluene is below 1% or O.5ppb on the PID chromatogram, then it will not affect subsequent analyses. (Note: thechromatograms are magnificdforcarryovervisibility). ",l iloLIloY... i¢4 !
Sample : clean water blank
__
0 3" Q " : " ' 1 5 e
l t J 4 ":'
~ h~ /....
bbbb,.f·.. . £....
~ H ~
.-".
Note: Te E is a ccntarransnt In our tac toey lasting lab.
e
FlO Results.: Cor."Ipcnerr.: TCE
reoene
?ID ReSlils:
Rctenbon ~5. 766
17.566 Ethyl Ben z6'1e 20 .033 Ortho Xylene 20.833 Tol il l
Area
58 _9'00 17. 4000 51. 9080 91 .5290 2 19.74 70
Compone nt R ele.'1tion TeE 15.750 Totue ne 17 .533 Ortho Xylene 20.650
Determine thecarryoverlevel by comparing the areas of the two PID Toluene peaks
resahingfrom the sampleandblankruns:
"'ea 58 .1920
DELCO Res../lts : Compcnent Rele ntioo Area TCE 15.750 4 6.0340
4.3400 20.8720
Tota l 609. 1300
-L __ ' _ 353 - ' Cppb 353x~ 4Cppb
x
( x repr es en ts the ppb corcenrrationofthccerryovcr)
~ C . 11 33Pf:b
167 (of 550 ) 2006(-2016)
168
POPULAR CONFIGURATION GCs BTEX & Environmental
Expected Performance - Direct Injection Th is chromat ogram is from an analysis of a diese l sample. Th e PID detector was bypassed, and the
columnwas connected directly to theFID detector inlet. The results areidentifiableas diesel because it shows therange of hydrocarbons that compose this fuel. A few retentionwindows are placed in the chromatogram to show the approximate ranges o f C ;o' e n ' C 2S' and C1O"
f I#llli8. 4' ~ t oe Y.i<'-
• ~
S.'4
l:"'
_ _ ---J
~
-
:
-
~
-
:
:
-
'
_
.
~~ ~I -'J±J..J ~ . c oo
Sample : diesel fue l #2 Method : dfred injecti on
CoI'JlTln; 60m MXT-VOL carre c hefium @ 10rr:U min
FIDgain: HIGH FfD tem p: 325'C F!O ignilcr:
-zoo
"lemperanrre p:-ogr:3m"
Ir.ilial 5O'C 3Z1C
3.000
Ram;::l Fir.al 10.000 32D'C
3).00
0.000
Hold
32IYC
168 (of 550 ) 2006(-2016)
169
POPULAR CONFIGURATION GCs BTEX & Enviro nmental
Expected Pertormence
»
Manual Headsp ace Inj ection
To ob tain the chromatogramsbelow,50ppb Japanese standard 'was placed into a VQA vial withwater. and allowed to equilibrate arroom temperature for 45 m inutes . The FID (top) chromatogram shows all the components andthe solvent The Pill (midd le) does rot detect the 1_ 1_1-TCA. 'wh ile the DELCO (bottom) does not respond to the solvent
r.''''l.dl Iff' !d •. :;
_
~ 1OOl' '' 3 ~ ''.1I ;;; ...
~~
..... '
'
2 ~ ' "
.~
C('N
I
e,
e
-v_ . . . . . . . .
.•. ~
/~
L >-
!
'Ulll
A
r lo_
••
r~
""
__
F lO ga in: HIGH i!F IDte mp: 15O
,I
~
~
""",-~
I
•
~,
.~
..
~
PIO current 80 P ID le mp: 1SOUC
~
T '\
-, ,'--" ""]
,-•, ...• s, i\
e'
,
P ID gam: l OW
•
s
r
- -, ~
~-
0
),
"
- ---_. Semple : 1ml reecscece from 50ppb Japanese stardarc in wa ter
Temperature program:
Method : ma nual headspace inject ion Column: 60m MXT-VOL
Initial 4O'C 22CTC
Ca rrier. helium @ 10mU m in
Fro Results :
Ccrrccoen
pr o Results : Ccmporl€l'll Retentcn
Sdverll:
2 .416
1_1~E
3933
T-1_2-DCE G-1_2-DCE
4 .833
Area 290.1100 39.6100 34.3780
5.966
18 .6020
C-1_2-DCE
2.183 3916 4.800 5.950
1_' _'-TCA TCE
G,GQJ 7 .850 10.083 Tetal
29.roLO 23.4490
TCC
7 .016
PeE
10.056 Telal
PCE
Re le nLoo
10.7560
Solvent
1_ 1-DCE T- 1_ 2-DCE
Area 22.7450 39.4070 45.0050 15.7380 33 .72 70 10.7780 1n.9000
Hdd
Ramp FInal
2.000
15.000 22O"C 10-00 0,000 22O"C
DELCO Results: Cc moonenl Retention 1_ 1-DCE 3933 T-1_Z-DCE 4.816 C-1_2-DCE 5.950 1_ 1_ 1-TCA 6.666 TeE 7,"'" Fe E 10.083
Tolal
"""
53.1700 38.0780 18.0560 53.22 10 30.6000 20.8340 233.0580
445.5370
169 (of 550 ) 2006(-2016)
170
POPULAR CONFIGURATION GCs Mu ltiple Gas Ana lyzer #1
System Overview Your SRI Multiple Gas Analyzer GC is pre-plumbedand ready to resolve H,. 0 ,. N" Methane. CO. Ethane. CO 2, Ethylene. NOx. Acetylene, Propane. Butanes, Pentanes, and C 6 through C s' The basic version of the Mu ltiple Gas Analyzer GC has a TeO detector only. A TeD-HID detector com bination is also available. A thi rd version. shown below. has 1:1 TeO. Methanizer; an d FID .
. ,
10 Port Gas Sampling Valve and 1mL Sample Loop
.~
.
•
~
-'i"
J r 0
~
- -Methan izer
-
-TCD Detector
----~
Valve Oven
3' Molecular Sieve Column -
~----FID
-/ ._ ~
:.
Detector
.........-- . :. ii
6' Silica Gel
Colu mn Injecto r
Column
Sample In and Out
Column Oven
The Multiple Gas Analyzer # 1 configuration allows you to obtain complete analyses of' the fixed and natural gases listed above with a singl e sample inject ion . This is achieved. using a 10 port gas sam pling valve'. a ImL sample loop. and two independent analyt ical columns-sa Silica Gel packed column and a Molecular Sieve packed column. The Silica Gel eolum n is locat ed in th e Co lumn Oven, while the Molecular Sieve column . lmL sample loop, and the gas sampling valve are located in the Valve Oven .
170 (of 550 ) 2006(-2016)
171
POPULAR CONFIGURATION GCs Multiple Gas Analyzer #1
Theory of Operation 10 Port Gas Sampling Valve Plumbing Connections The Multiple Gas Analyzer #1 configuration uses two analytical columns and one lO-port gas sampling valve to analyze hydro gen, oxygen, nitrogen, methane, ethane. propane. butanes, pentanes, carbon monoxide and carbon dioxide. r------.,."."..,.~~_c=~_c==-=..,....,,=--__, 10 PORT VALVE IN "LOAD ;" RELAY G: "O FF"'
LOAD Position
_.-
~. _
A one-milliliter gas sampling loop is connected to the to-port gas sampling va lve.
~.
When t he valv e is in load position, the sample may be
flow ed
thi~';S:IOO:P:un~ll:'I_b~;~=~~====~;~~~~~::::::::::::::::~
the moment injecti: n occurs. through
LOAD
InjectDf
-... •
Molecula r SIeVe In va.. CNen
~ loop
10 Pat Gas
s;r
Sampling vat.-e
INJECT Position
10 PORT VALVE IN '"INJECT;" RELAYG: ' 'ON''
At the beginning of the chromatographicrun, the valve is actuated to the INJE CT position, depositing the loop contents into the carrier gas str eam and direct ing it to the
two analyt ica l co lu m n s, connected in series through the
.....""
samplingvalve.
"Column sequence is reversed while the flow direction remains the same-
j' Inj9dDr
INJECT
. r >:
-e.m. ...
-,
.."
~
Silica Gel in
Cok.mn ""'"
~
....... I
MolecUar
V;
10 Put GiilS Sampli1g 'v'iiI~e
171 (of 550 ) 2006(-2016)
172
POPULAR CONFIGURATION GCs Mult ipl e Gas Ana lyzer #1 Theory of Operation 10 Po rt Gas Sampling Valve Plumbing Connections Continued
The sample is deposited first into the Silica Gel packed column, at4O"Cin the column oven, where the ethane. propane, butanes. pentanes and carbon dioxide arc retained. The remainder of the sample containing hydrogen or helium (whichever is not being used as a carrier), as we ll as oxygen. nitrogen, methane and any carbon mon oxide, continues on to the Molecular Sieve column. During a chromatographic run with the sampling valve in the INJECT position. the hydrogen or hel ium. oxygen. nitrogen and methane components are the first to elute through the columns and into the detector. This is due to the Silica Ge l column 's long retention time at 400C ore", CO 2 and higher hydrocarbons. Under programmed temperature and event control using the data system, the sampling valve is actuated back into the LOAD position immediate ly following the el ution of the carbon monoxide peak.
MUlti pl e Gas Analyzer TCD chromatogram with temperature programming and sample valve rotation
"
-
~~
;;or
•
.,.,
Ii
f 'H1.Illi ----7~=== ---"'--.J -"
•
s,
\
\
Ii
...
.~
i\
~
....1=...-! -2::..J
~
~
0._.
Peakgtmpl e te mperature prog ramm Ing:
IrllhalTemp t!.!: Gas sampling va lve rotates back into the load positton.
~
22O-C
5 00 15.00
~
15.00 000
This reverses the sequence of the columns prior to the detector, and sends the components prepari ng to elute from the Silica Ge l packed column (ethane, propane, crc.) to th e de tec tor without passing them thr ough th e Molec ular Sieve packed column. At the same time, the Silica Gel pac ked column is temperature ram ped to promote th e rapid elution of the rem aining components. LOAD
ucrecuar Sieve in Valve Oven
I
I Silica ce in Column Oven
Detector
172 (of 550 ) 2006(-2016)
173
POPULAR CONFIGURATION GCs
Multiple Gas Analyzer #1
General Operating Procedure I . Set the gas cylinder pressure 15-2Opsi higher than the head pressure (heliwn carrier) . The carri er head pressure used to generate the test chromatograms at the factory is printed on the right side of your Oc. Typical head pre ssure for a Multi-Gas instrument operating at 20mUmi n is about 20p si 2. Damage or destruction of the TeD filaments will occur lfcurrent is applied in the absence offlowing carrier gas. ALWAYS verify that carrier gas can he detected exiting the TeD carrier gas outlet BEFORE energizing th e TCD. Labelled for identification, the carrier gas outlet is located inside the Column Oven . Place the end ofthe tube in liquid and observe (a bit o f spit on a finger can suffi ce). If there are no bubbles exiting the tube, there is a flow problem. DO NOT tum on the TeO current i f carrier gas flow is not detectable. A filament protection circuit prevents filament damage if carrier gas pressure is not detected at the GC, but it cannot prevent filamentdamage under all circumstances. Any lack of carri er gas flow should be corrected before proceeding .
3. Set the Valve Oven temperature to 9O"C. (The Molecular Sieve column is in the Valve Oven.)
4. Tum the TCD current to LOW. Ignite FlO if present. Tum Methanizer to 380°C if present. Tum HID current on if present. 5. Determine the elution time of ethane so that you can set an event program that will rotate the gas sampling valve at the right time during the run . Ethane is the first peak to el ute from the Silica Gel co lumn after the .Hz, 2, N!. CH 4, and CO, which are separated by the Molecular Sieve column. If the valve is not rotated back to the LOAD po sition by turning relay G OFF prior to the ethane elution, then the ethane and CO 2 will get stuck in the Molecular Sieve column. Type in an Event Program as follows: 0.00 zero
°
0.1 0.3
G on Goff
This Event Progam will inject the sample loop contents into the Silica Gel column and then immediately reverse the columns so the sample wil l not enter the Molecular Sieve column. In this mode ofoperation, the elution time of ethane can be easily determined. 6. Set the Column Oven temperature program as follow s: 4O"C hold 6 minutes then ramp at IOO/min to 200°C
173 (of 550 ) 2006(-2016)
174
POPULAR CONFIGURATION GCs
Multiple Gas Analyzer #1
General Operating Procedure Continued
7. In PeakSimple, zero the Data System signal by clicking the Auto Zero button, then hit the spacebar or the run button on your GC . Inject a sample that contains ethane into the Gas Sampling Val ve through inlet on valve oven (do not inject sample into the O n-column Inj ector).
8. Rev'ise the eve nt table so that relay G turns OFF just before the ethan e peak begins to rise from the baseline. A typical event table foe this GC is: 0.00 zero 0.05 GON 5.05G OFF 9. If the ~. 0 2' N 2• CH 4• and CO do not elute from the Molecular Sieve column before the el ution of
ethane. increase the Valve Oven temperature (which will increase the Molecular Sieve column temperature) so that all peaks trapped on the Molecular Sieve co lumn elut e within the req uired time. Or, hold the Sili ca Gel column temperature at 4O"C for a lon ger time period to delay the e lution of
et han e. allowing more time for the M olecular Sie ve peaks to elute.
174 (of 550 ) 2006(-2016)
175
POPULAR CONFIG URATION GCs Multiple Gas Analyzer #1
Expected Performance
...c
~ -----
:r-
1'"
g 9!
~
~
er '=>" 8
Ii• :=
c
cc l CCJPl''''
, , , • e:
,
"'-'3~ :; ' l:{F. c ~ 'lO'JE ~ ; :x.T CC"<
O . ~ OXI
_D
--
TeD noise run Colum ns: 1m Mol . Sieve , 2m Heyese p-D, 30m MXT- 1 Carrier: Helium @ 10mUmin TeO ga in'" l OW
TeD temc
e
1OOOC
Valve temp e 1100C
i!
La ~
I Te o
I, ;
,
,,~
.
~
~c
noise averages less than 25~V from peak to peak/
I
. T. r ,d
...J
z:cT'"
Temperature Progra m: Initial !::i2.!Q Ramp 8O"C 15.00 0.00
Final 8O"C
.!.EEl -e oc.1
Factory Test Analysis o f Natural Gas Standard Tempe rature program: Initia l Hold Ramp
40"C 5,00 22O"C 16.00
10.00 0.00
.
-
IIr_Olf f' " 220"C D IOS~~ ; <§ ; ~ I!!! Final
22 0 Q C
-
NO.T o;.s STP
'"
,
€ 'T,
H Oo "'-'\34Z7 ~ 'Q ' N O E
Events: 'Time
0.00 0.050 6.00
_Is
Reten:ion k eG
"'-
1.633
""""'"
3.333
"' E:tt':anc
C0 2
"'-'"
"""""~ N·81.1ane ~r1tlI ~
N-Penlane
7.5:50 9.933
f2 i3
13.683 18-150
6S 4S6()
57 450 20 . 1490 22 .66 '5 19 15'50 Total: 1134 8245
E.
~.
.
c
•c
!
~. "f
I
,
~I
191500 121.0as0 563.5130
l Z5.Z11:l:l 11.9860 113.S220
18 766 22 550
•>0
" ~
:;
JI
4
~
Compolle t
2 150
i
,
~,
; t
o· ",,' c.
,.
~\
I ;
:---
,
'kI .~
...;;.,,-,
.:..ex
-~ -'-
i•
,
1\ r>; '-;,J
-~ -
.
IlEJD
~ ft, ft,f,,'ft,f!,b ff,'f-, f ', "" '"' .
,
H ,
Evenl ZERO G ON (valve injed)
G OFF
"'Ul-
, a • .q
.
l
~
B
"
i\
1\ -
~-
~
~
m ~
.-
16,)t.:;
Valve rotations
175 (of 550 ) 2006(-2016)
176
POPULAR CONFIGURATION GCs
Multiple Gas Analyzer #1 Expected Performance Factory Test Analysis of 1% Fixed Gas Standard on a TCD Multip le Gas Analyzer #1 :g"...un b it> f.
-:"!o l.3l
&:-aoi.r.""
Xi "",
t;~
! D ~ liI 6 ' ~ : ' S ~ ~ 1 a TC D current = LOW TCD temp = 100'C Valve Oven temp = 9O"C
, C'" ,, ,. ~~~ :U:lO
~,.- '
,I
'UOll<'IU.
0 :;!:
, • "! ~ b
,-
b J"-'ft. bbf:!. l/Ab '-'
-It ;"" ,
~ ~
RESUL.TS: Com:!oner(
Hyctogen Oxyge n ~Otlgel'l
Metha ne
CO Vallie Rotate CO2
II
Ii
Retimn A-ea. 0.916 0 4710 1.383 14.9530 1.700 1049....940 3.333 9 487 5 4.900 11 4460 7,200 0 6460
j
j' ,, -
-
0
~
-
•a ,"
-
~
A
z
•0
~
63B3 13.8000 tOlal 11 OCl-2n s
0
f\
j\
I
>
•
0
4"" ·tor., I ~ .~
.
--- .. ,
"
. ~
8
z
0
0
I\
~
l\
""
\
~
\
,
.101 ..,_' .
, ~
.
Factory Test Analysis of Room Air & C,C, Hydrocarbons on a dual-channel TCD- Methanizer-FID Multiple Gas Analyzer #1
Retention 1.650 3 866 7.316
0 "
I,
~
;
a
T.
I
.,,-.--"'0
. _._..
.
-I
A
l
:!
I
~
t
-1\ ,I '\
I
"50
12 .063
15 533 18.333 21,900
''''''
..
"'''''''''''' 1 56Q
~
"'-.
I
!
I
!
-i!'-
I
2166 3,783 7.216 9150 11.966 15433 " 2lJO 21816
ToloJ
Are. 4731.214 0 2008.6000 3854 .7300 31<2.1040 53 79.8755 7326.4440 9136 3340 10408.3160 45981 .6175
.,., 13 1.0650 675 1440 O.3B80
0.4070 0.6 780 0.8210 1 1210 1.2 7 10 1 64SQ
862.6;30
176 (of 550 ) 2006(-2016)
177
POPULAR CONFIGURATION GCs Multiple Gas Ana lyzer #2
System Overview The Multiple Gas Analyzer #2 is pre-plumbed and ready to reso lve ~. He.
°
, ~ 2'
Methane. CO , Ethane. COr Ethylene!Acetylene, :NOx. Water. Alcohols. Propane. Butanes. Pentanes. and C6 through C:w Separationofthis wide varie l)' ofpeaks is accomplishedusing a 10 portautomated GasSampling Valve\....ith dual Sample Loops and two, three. or four columns, It can beoptionallyconfigured with I) a TeO, 2}a Teo. Methanizer; FID. or 3) wi th Teo. IlID and FIDd...-tcctors. AIl three versions have a Im (3') Molecular Sieve packed column in the Valve Oven, anda 2m (6') Hayesep-Dpacked column in the Column Oven. The mode l shown below is customi zed with TeO, HID and FlO detectors. In addition to the Hayescp-D co lumn. it has an optional 30mMXT-I capillary cohnnn in the Colwnn Oven. 2
- --'--- - TCD Detect or
~l:'--- HID Detector
Molecular Sieve Column - --
..J
i - - +-;11
30m MXT-1 column On-Column Injector
Hayes ep-D column
Column Oven
177 (of 550 ) 2006(-2016)
178
POPULAR CONFIGURATION GCs MUltiple Gas Analyzer #2 Theory of Operation The Multiple Gas Analyzer #2 GC usesa single automated 10 portGasSampling Valve and multiple columnsto separate a wide variety ofpeaks. TIle system achieves this by turningthecarrier gas flowto each colwnnon at different times during the nm. This procedure allows the Molecular Sieve column in the Valve
°
Oven to completely separate ~. He. 2 , N2 , CH4 and CO before tbe carrier flow to the Hayesep-D column in the Column Oven is nnned on. TbeHayesep-D column then separates all compounds in the C 1-C 6 range. An optiona130m MXT-1capillarycolumn in the ColumnOvenseparatestheremaining hydrocarbons out through C • using the same carrier gas flow as the Hayesep-D colwnnand an FIDor HID detector; 20 Thisconfigurationusestwo carrier gas flows, cachregulatcd by Electronic Pressure Control(EPe ) using the PeakSimple data system. Carrier 1 flows to the Molecular Sieve column, then on through the "Teevto the TeD detector, and it is always on; if not, the lack of carrier gas flow triggers the TeD filament protection circuit Carrier2 flows to another"Tee" whereit splits to entertheHayesep-D columnand also the MXT-l column. The flow from the Hayesep-D column continues to the TCD detector. and. the flow from the MXTt goes to the FlO or HID detector. The carrier #2 flow (EPC 2) is turned on and o ff by Peako imple, controlled by the user. MULTl-GAS #2 VALVE IN "LOAO" POsmON (RELAY G: OFF) Carrier 1
r
--';l>---":.:m:.:Mo=lecular Sieve SA co lumn
optional
EPC ,
Detector
TCD 1'"-- ----,;0.1 Detector
TEE
EPC
HID
ON.Q FF by
When the 10 port Ga s Sampling Valve is in LOAD position, the two carrier gas flows bypass 1he Sample Loops through the Valve and travel on to the colwnns.
PeakSifTlll@
HID
EPC2
-00-
Detector
Car rier 2
FlO Detector
MULTI-GAS #2 VALVE IN " INJECr' POSITION (RELAY G: ON)
rCarner 1
-';l_ ---"" m:.:"""= e cular Sieve SA
co.. ~
HIO Detector
EPC'
EPC
TEE ~-----'3>J
TCO Detector
ON-OFF by Pea kSi mp le
opfiooal Metharuzer
EPC 2 Ce- ne r 2
HID De tecto r
-oR-
no
Detecto r
When the to port Sampling Valveis in INJECT position . the two
Ga s
carrier gas flows sweep through the Sample Loop s. se n d ing the ir contents to the columns and detectors.
178 (of 550 ) 2006(-2016)
179
POPULAR CONFIGURATION GCs
MUltiple Gas Analyzer #2 General Operating Procedure I. Set the gas cylinder pressure 15-2Opsi higher than the head pressure (heliumcarrier). The carrier head pressure used to generate the test chromatograms at the factory is printed on the right side ofyow GC. Typical head pressure for a Multi-Gas instrument operatingat 20mUmin is about20psi
2. Damage ordestruction of the TeD filaments will occur ifcurrent is applied intheabsence offlo",'ing carrier gas. AL\\~YS verifytharcarrier gasC3I1 be detected exiting the TCD carriergas outlet BEFORE energizing the TeD. Labelled for identification, the carrier gas outlet is located inside the Column Oven. Placethe endofthetubc in liquidandobserve(a bit ofspit on a finger cansuffice). lfthere arcno bubblesexitingthe tube, there is a flow problem. DO NOT turn on the TeD current if carrier gas flow is not detectable. A filament protectioncircuit prevents filament damage if carrier gas pressure is not detectedat the Ge. but it cannot prevent filament damage underall ci.rcumstances. Any lack ofcarrier gas flow should be corrected
before proceeding.
3. Set the VaJveOven temperature to 900c. (The Molecular Sieve colunm is in the Valve Oven.) 4. Turntbe TCDclUTent to LOW. Ignite Fill if prescnt. TurnM ethanizer to 38O"C ifpresent. Tum HID current on ifpresent
5. Setthe Column Oven temperature program as follows: Initial Temp Hold Ramp FinalTemp 7.00 10.00 220'C 5O"C 10.00 0.00 220"C 22O"C 6. Type in an event table as follows:
TJme Evl."Ill. 0.000 ZERO (auto zero data system signal at stan ofnm) 0.050 G ON (valve inject) 0.100 B ON (carrier #2flow OFF) 7.500 B OFF (carrier #2flow ON) EPC #2 controlsthe cerrie szflow. When the limiter (B) is turned ON, this flowis shut off. Theevent table should aIJowfortheelution ofCO from theMolecular Sieve colwnn before the limiter(B) is turned OFF and carrier #2 flow restored. The Valve Oven temperature may be increasedto speed the elutionofthe ~,02' N2, CH4, and CO.
7. Load your sample gas streamby connecting the flow to the sampleinlet port on the frontofthe Valve Oven. 8. Startthe analysisby pressing the RUN button on the front ofyourGC. or bypressing your PC keyboard's spacebar.
179 (of 550 ) 2006(-2016)
180
POPULAR CONFIGURATION GCs Multiple Gas Analyzer #2 Expected Performance . '::; "
FID noise run
I
I
FID noise averages Jess than souv rrom peak to pea k
I
,
Temperature Program:
Initial
Hold
Ramp
BO"C
15.00
0.00
I ..
HID noise run Colu mns: 1m Mol. Sieve, 2m Havesep-D. 3 0m MXT- l Carrier; Hel ium @10mU min HID gain'" HIGH HID c urren t = 70 HID temp = 2000c Valve temp = 11 COC
Temperature Program: Initial Hold Ramp
Final
8O'C
8O'C
.
15.00
, ,.. ""'"
~_
0.00
.-
::Jf; ;; Z 6 ·'·~ ii(;;:
-
1 ~2
J
( _~, ":.; 7":' !"'..'· r, /" ,·'",. /;:7;, 7"',f.'~ ' -' *
"" ,
TeD noise run C olumns: 1m MoL S iev e, 2m Hay esep-D,
30m MXT- l Carrier; Helium@10mUmin I T e D ga in = LOW TeOtemp = 1co-c
TeD noise averages less tha n 2 51N fr o m pea k to peak
, - - --
-
- --
-
I
Valvetemp = 110' C
I
Temperature Program: InitIal Hold Ramp 8O"C 15 .00 0.00
!
--' .±l!J . '" ;
180 (of 550 ) 2006(-2016)
181
POPULAR CONFIGURATION GCs Multiple Gas Ana lyzer #2 Expected Performance: FID & TeD Detectors These two factory test runs utilized the samecarrierflowand temperature program The fir.;t chromatogram resulted from a run with a l OOOppm C t -C 6 sample; the second. a 1% fixed gas standardsample.
,"- y• •
fi:~
td ~
~~
... ,
D~g~ :a : ' I!!!~ '
m -C1::el':O , ll:~~ :;,.,ju
.-- - - - - - - - - - - - - - .... --E1-' Test Run #1 a
t
•
"
<.
,I
It
~i
EPC #2 on
I
~
~
G ON (va lve inJ~) 8 ON (earn er #2 flow off)
0. 100 0 .400
GOFF
7 000
B OFF (carri e r #2 flow on )
FlDResults
'l
I
0050
Component Methane
.I
Pro;:a~
Bu: ane
J "-Ll-
~A
e.
•
,
•
t
...e
!
~ w
i
Events:
Iunlt
Elho~
m p....es-c co
""
li
(BOFF)
.'=-:.(0[)
Sample: 1000ppm C l -C~
J" 1'<. h !!'. !~. fr. fr.. ..., ,;+ .•c,
t ...._~ .......t eoN
,.~:n
' '''G ''~.
~ ~~
I """""'
~
-
He~an e
(\~ ,"
~.
N _
"~
~
-
.,'" .r.,.-o
8 38.3160 2066.2065 2953 3865
8.165 6.800
34 79 450¢.0 4C2 1.5 110
10.0 16
351 2.6800
Total
16871.5340
TC DResult
•'inJ
ecce
: l r..::::
Columns: 1m Mol. Sieve, 2m Havesec- o . 30m MXT-1 Carrier: Helium t; l OmUrnln through each column
7.73 3 7.78 3 7.88 3
Temperature Program: Hold Ramp
!DltI.>ll 50"C
7.00
10.00
22C7C
10.00
0.00
yQ!'T!(l()!'!enl
Retention A re a
Oxygen
1.25 0 2.116 3.116
PAe:l""'"le
7.71 6
Hayesep A ir
8.250 12.133
_. ~
Tot al
Fina l 2 20"C 2200c
Test Run #2
EvenJ G ON (va lve inject) B ON (ca rrier #2 flow off)
G OFF
EPC #2 on
B OFF (ea rner #2 flow on)
(B OFF)
_1~ 400l:::===============+========:J
I
H ~F1X£O::w.s~~~~~~;;!C========~:;;::======~ 4 C :lO !"·~"" "
.•
. v " =~
;;,.;
I :t
...».
t"
'.T.T' l-' ,=
\
z
L ~ ~l ~
F lO Results: Co mponent
""~"'"
Remnt>o n Area
8.233
12 144. 3770
Re~Ar~a
§
f\
1. 166
26.492'0
1 633 308 3
2251.7140 23 .09 75
6.566
22.2440
8.116
524 .2010 37730 63940 6 3 .0115
8.715 9750 Tota l
181 (of 550 ) 2006(-2016)
182
POPULAR CONFIGURATIO N GCs Multiple Gas Analyzer #2
- ,
Expected Performance: HID & Te D Detec tors These two factor): test runs utilized the samecarrier flow. temperature program. and event table. Tbe:first chromatogram resulted from a nul with a lOOOppm C l -C~ sam ple; the second, a 1% fixed gas standard
sample.
Test Run #1•
t.rJO PPIIICl · C
• Ei'
;.Q v
l ~~. _c cO
.... · " ";Ol d ' "ew AV• •
I
-
Retention Area
8 233 8.283 8 353 8650 9.216 10.316 Tota l
6249 33 20 30642580 3408.5720 22553520 2650.8955 : 2250 8 975 19899.30 7
EPC #2 on (8 OFF)
-
i
zt ~
,I t' l
P
~, ~
TCD Resulls ~n:ent
Retentio n A re a
Ollygen
12 50 2.116 3.115 8.216
Nitrogen
""""M
Hilynep Air
-~ ."""
40220 21.05 10 2.1900 22.4900
8.733
12.333 Total
o.saeo
~ I 51.1630 !
L-~
Col umns : 1m Mol. Sieve ,
Temperatu re Program: Initial Hold ~.aJll.P 5 0· C 7.00 1000 220"C 10.00 0.00
2m Hayesep-O. 30m MXT- l Ca rrier. Helium @ 1OmU rr.in tnro ug n each colum n
,-
Test Run #2
Ei"
_ _----:::--:--_~ -
,~
.-
...
A<>l~
O ~IiiI""~ i"",e: _~ i :l
II"' f~D 3AS s1 HIC
Sample: 1% fixed gas standard
, ;
AD Results : ~
"''''''M
.
TeD Results: ~~licfl ~
Methane CO
QC
, • l.. !: t{ b b
f>!oll G ON (valve inject) B ON (carrier #2 flow off)
GO FF B OFF (carrier #2 flow on)
• a •
It',!f!l , f~ f!> t:, i f\'I. fl'o<. <") :7
-,
A;t H l t lt
"I
.
~
Are;
~_1 56
~ 1.0260
1.616 3.050
2261.5430
• •oc
12.5240
Hayesep Air MeL'1ane
8.716
22.4410 542.5790 3%50
CO2
9 750
~
B 11E
'ota'
2680.7COO
.
EPC #2 on (B OFF)
G Q
;
"_
Final 220· C 22 0
e, Retentr.m 8266
I Ol
~ o"'.ooo
e
e vents: Time 0.050 0 .1 00 0 400 7.500
_I t:2.4:.1
.. r JoF.l ~S
,- .
H'OC ...."' H .:"1 ~
~ !QI
~
&.1 .
" 00
~
'.I ' F fl c.ccc
-
. -
,
~-
~
\),
.
~
~ ~
¥ =
8
fAll L~ A ~ l Z (W;;;
182 (of 550 ) 2006(-2016)
183
POPULAR CONFIGURATION GCs Mud-Logger
System Overview The Mud-LoggingGCsystem isdesigned to provide a continuousreading oftotaI hydrocarbons in a gas stream, whileperiodically perlOrming a cbromaJographic separationofthe sample to determine thecomposition ofthe samplegas stream. This is accomplished using a 10portGas SamplingValve with a 25~L Sample Loop in a thcrmostattedValve Oven. a lm (3 'J Hayesep D packedcolumnina temperature programmable Column Oven,aCCDdeteetor, anFIDdetector and a built-in Air Compressor. This GC canbemodified to incorporate a second FID instead ofthe ceD for totalhydrocarbonmonitoring. Themodel shewn below has CeD and FIDdetectors.
Therrnostatted YalveOven
Gas Sampling Valve Restnct crs. and Sample loop - - -- -f-jif
Sample In & Out -
-
~~~~-- CCD Detector ) --
--'
F lO Detector
-, Column Oven
1m Hayesep-O Co lumn
Speciation ofCI-e, hydrocarbons is handled by the GasSampling Valve, Hayescp-O column, and FID while the CeD provides contiuous, total hydrocarbon monitoring. Detectionlimitsforthis system areO.l % to 100'% forthe continuous total hydrocarbon monitor, and 0.005%to 1000/0 for spccietcd hydrocarbons using the FlD. The Air Compressorsupplies combustion air forthe FID. andthe air make-up for the CCD. The buill-inPeakfiimple data SY'1cmdisplays boththe continuous total hydrocarbonreading, using the Data Logger mode, and the separated peaks. When the system receives out-of-range readings, analarm function may alert the user;
183 (of 550 ) 2006(-2016)
184
POPULAR CONFIGURATION GCs Mud -Logger
Theory of Operation The samplegas stream is connected to a bulkhead fittingon the system'sthermostatted Valve Oven where it flo", through the sampling loop ofthe 10 port Gas Sampling Valve.and also to the CCD detector, The fitting labelled"Sample In" (pictured at right) onthe front ofthe Valve Oven isthe sample gas stream inlet. The use r must reg ulate the pre ssure o f the sample stream so that it enters thi s inlet at IOpsi. Th e
instrument is factory preset todeliver 5mUmin to the CeD at l Opsi. The remainder oftheflow, approximately l00mUmin. passes through theSample
SAMPLE
Loop. This relatively high flowrare gets the sample from the samp ling point into the GC with minimal delay.
Tota l hyc roca rtxxt
FlO Detector 'or Cl -C6 hydrocarbcna
monitoring Detector (C CO or FlO)
l'
l'
I~.
Gas Sampl:ng val....... o-s, ar:d' Sample Loop •
OOT ID s:a ir.Jess stee l Restnctcrs
IN
O UT
Once thesampleenters the inlet, its path is 1"d through two restricrors and on to the detectors. To avoid damaging the ceo. the maximum pure hydrocarbon flo wto reac h this detector is 5mU min. Th e resrrictors regulate the flow to the to 5mlJmin when thesample inlet pressure is lOpsi The remainderoflhe sample stream (approximately lOOmUmin) flo ws thro ugh the Gas Sampli ng Valve's loop and is periodically injected into t he Hayesep-D column. then detected by the FID.
ceo
LOAD POSITION Ccennn is back llushed to detector
Vallie Oven
1Sample In
W
,
"
Sample Out
at l Op si
10 Po rt Gas Sampling Valve At an automatically repeating time interval controlled by the
user wi th the built-in PeakSimple data system, the Gas Sampling Val ve injects the co n tents of its sample loop into the Hayescp 0
~.- --
- - - - -- -- - - -,
p a cked column where it is separa ted into the co nstit ue nt hy drocarbon (C 1·CJ peaks and detected by the FID de tec tor, Betvvccn automatic sam ple injections into the column, the 10 port Gas Sampling Valve is in WAD position (top right schematic). In this position, thecarrier gas flows into thecolumn"..hile sample gas flo ws through the 2 5J.1 L Sample Loop and to vem . When PeakSimple automatically moves the valve to the L\''JECT position (b ottom righ t schem atic). the carrier gao; 00\\'5 though the Sample Loop first. then sweeps the samp le into the Haye sep-D column.
184 (of 550 ) 2006(-2016)
185
POPULAR CONFIGURATION GCs Mud -Lo g g er
General Operating Procedure Part 1: Total Hydrocarbons Using th e CCD Detector 1. Connect zero gas to sample inlet at 1Opsi. Zero gas has no hydrocarbons. 2. Zero Ute CCD detector signal using the Auto Zero buttonfor its channel(typ icallychanncl Z). 3. Connect calibration gasstandard to the sampleinlet at IOpsi. Calibration gal; istypically 100% methane. 4. The CCD signal " i ll increaseapproximately 300 millivolts while running 1000/0methane. 5. In PeakSimple, open theCCD Channel Details dialog box by right-clicking in that charmers chromatogram window. Enter the ~ajn factorwhich will multiplythe 300 millivol t signalto produce the desired concentration unit. Forexample: 300 x .33 = 100 if the desired unit is percent. 300 x 3333 = 1.000.000 if the desired unit is parts per million 6. Also in the Channel Details dialog box, select Data Logge r mode by clicking in the appropriate checkbox. The CCD signal times the gain factor will be displayed on the screen in large numbers.
•
Chanod 2 delall$
~-=~:nIt'~1.!D_lOGU~R FO
{ncIlme: 15.000
r.s.. . IoIP-~
."_.. t
r.
~ Hz
r:
2 !'fz
r S" Hz I
C
Ir
- C~d: ~}"-
!
Ma:c I~aXl
rritI
t.4 Sot:I ·~~~_+
rr.V
nWJ .. - Cm!roI ~--
e .u~" 1
- rl;,; :er ~ -
: r. ~!en
I C All
~ C1-! z
2C Hz , (; 50Hz
.... Re':!Ol
£1,
r- T ~ Ir
t r p~
I I
r
GraOert
PeakS im ple C hannel Details dialog bo x
- D8~ogger mode -
I
C $obtilct.t~ment!'l~IC ! ~ !B 1 r: flveMJI ~.iUI ~~e ' IT: I Ot'$~ 10.00 I ~ _ I'-~' -- I ~ 'elenlion #1b Ift ~r.ed~lo.ooo _ . - mo'" 1 33 u ~ soUe t!Jle:la OO) rm _.- E ~~
~
I
~--
"' I ""'"
I
D~~
{-1 b
1
au!Ief~
Chrom atogra m w ith channel 2 in Data Logger m od e
--
~2,_ U_ .~Z, "
.
., ~
1-:.. /':.:~,
."':. ~. !';. .~.
f'r., ~"<..
..., ; "
' Il>
e;
i, 1~L :11 t, #.
;
-- $-~-
e•
.""'.Dr<
...._i= ;';;c;:::..._ ~ """
(.•-
.:.:.:.:.:l..J ".,
I
I
I
17.4
I • , li '
,-
185 (of 550 ) 2006(-2016)
186
POPULAR CONFIGURATION GCs Mud-Logger
General Operating Procedure Part 2: Speciated Hydrocarbons Using the FID Detector I. Connect the calibrationgasstandard to the sample inlet at l Opsi. 2. Set the valve Oven temperature to 9Q'>C.
3. Ignite the FlO.
4. Setanisothenna1 Column Oven temperature program as follows: Initial Temp Hold !9mP FinalTemp 20if'C 5.00 0.00 200"C 5. Type in aneventable as follows: Tnre Even 0.00
Zero
0.050
G ON G OFF
1.5
6. Set the FlO gain to MEDIUM. 7. Start the analys is by hittin g the spacebar on the computer keyboard. 8. In Peakfiimplc, input the retention windows to identify the individual hydrocarbon components (methane, ethane, propane, butane, etc). 9. Calibratethe individual hydrocarbon peaks.
10 . Th is instrument is plumbed for backflush, This gives the use r the option to set the val ve pro gram to backflush the heavier hydrocarbons after the desired peaks have been separated. For instance, ifyour application required separation ofhydrocabons up to C••you could set the valve to backflussh after the
elution of the C5 component(s),and all the heavier hydrocarbons wouldtogetherproduce one large peale.
186 (of 550 ) 2006(-2016)
187
POPULAR CONFIGURATION GCs Mud -Logger _
Expected Performance
.
~ ,,,, D ~l;I l3' ~ ' ';;., !! :;
_ 0
• e.
~ ~,
fu f~, ft· h b
1~ )~" ",IV:..
0:") .;;. :
•
CCO Noise
f!:!:
- lO'Jlo ~ ;j "SCh Ii5i§ ~
I
I ,OOCI :....'\3<1<01:. , ~~t§';;:JL f ::0'1
CcJumn: 1 m Hayesep--D
J'-40~V
I
~
'S ~
Carrier: Air @ 10m Umin
Air make-up v t unmtrmtn
remperab,;re prog ra m"
•
J!mI!
.t!ll!!;;!
R3mp
Final
8Q->C
5.00
0 00
8O'C
ceo noise level = approximately 401J.V from peak to peak
I
" .<00
,
' r.-,' !
:J
~ :l.C ~O
""
,.. , , ...... D;S"" • e, ;;
-
.
IIp••IlIJ
FlO Noise
,a
S ~ ! !l
,I'".. ~ ooo _ ~~FfuSE: ~
\000 ",-~,I)a1J' ~l!}'kJi t
Co lumn: 1m Hayesep-D Ca rrier. Helium @ 10mU min FlO gain = High FlO temp == 15O"C F lO ignitor= -4 00 valve tem p = 90<>(;
Temperat1.:re ::'~I'iI ~ : Ini:lI::l t:!2!s!: R.T.:o 3O'C 5 0C 0,00
F:na
i
,,,
coo
t.. .
!
I,,
-
.~
,/4
~s
~
-
-
-'"
ft- ff). f~ i h~ I':!, ,IV;, [,,:-, !p'\ ,fV':, "") if !
"!
I
-----··t 'ElX¥V
-
e,
"'. FlO noise level = approximately 100p.V from peak to peak
8O"C
I I
·U Oll
,T.T. ,
rz-
..1
~ lC~
187 (of 550 ) 2006(-2016)
188
POPULAR CONFIGURATION GCs Mud -Logg er
Expected Performance Factory Test Run of a Standard Mu d-Lo gging Sys tem (FlO and Ce O) , ,, -, _ ~--------, -~-r -' --------,"",E1
foIo f
!{lew
~
~
0 ,. ", ,, '" " " . , ' "
:: .:: , bbfr.: hhf!:.j' ,'fr' f.'..... ;t 10>
Backflush at 1.5 m inutes
_! _ fD
~_ <1
lr\
~
10.1 .~5IlJ. t::====================:::1 .!l!EL.J ~;
Sa m ple: Natural Ga s stan dard
Temperature program: Initial Hold Ramo 200cc 5.00 0.00
Method: Valve injection FlO H2 = 30, FlO a ir = 6 FlO temp = 15O"C FlO ignitor"" -750 FlO gam = MEDIUM Valve temp = 90<>(;
Events: Time Event 0.000 ZSro 0050 G ON 1.500 G OFF
Column: 1m Hay esep-D
Carrier Helium@1 0psi
Res ults:
Comoonent Metha ne
Retention
N ea
0.291
6664.14 10
Etha~
0 366
Propane
0 483 0.6 91 0 .750 124 1
2 770.3785 2762.6450 1754.0118
K;4
N-C4 Pentanes
1913.8415
1580.4310 Total 1744 5.4488
188 (of 550 ) 2006(-2016)
189
POPULAR CONFIGURATION GCs Educational TCD
Overview
Sys tem
Your educational TeD GC is configured on the compact 3 J0 chas sis. It is equipped w·i th a TeD
Detector, a temperatureprogrammableColumnOven, a 3' Silica Gel packed column. Electronic Pressure Control (E PC) for carrier gas, On-column Injector. and a built -in.. single channel PeakSimple Data System. The mode l sho....-n below is equipped with optional Fast COOI-dO'\\'fl fans.
Fast Cool-down Fans - - -- TCD Detector Column Oven with 3' Silica Gel Co lumn inside - -- -- - --{
.;
On-Column Injector
--
--.. .. · ..
\\ :~ --- t~..: :~::::: . . . -:. ·· __ .. .. ..
,
'1 : ! " l l t :
1
'i
•
i t r t• It ;, .. 'i... '; .
,
il!
•
;
.
" ---'.."
. .':.
~ ; i i r
. .-
.' _- /
~_ ...
.
''JI.
.
~J
-- ' ~~ I
,
TCD Detector temperatu re selpoint
Jif.
Regu lator The TeD Detector is located inside its o wu o ven. mounted on the righ t rear of the Column Ove n as sho e... n above. Its temperature is fac tory preset at 1Ol)-'c. but it may be heated up to 13O"C by udjua ring the trimpot wi th the small b l ade screw d ri ver
He lium gas cylinder
attac hed to the fron t right comer of your Gc. The trimpot looks like a small brass screw and is located inside the: labeledhole on the top edge ofthc front control panel. The TeD Detector requires helium to operate, which must be supplied by a gas cylinder and regulator. The helium cylinder pressure isnormally set at 3Opsi.....hich is I0-2Opsi higher than thecolurrm head pressure.
189 (of 550 ) 2006(-2016)
190
POPULAR CONFIGURATION GCs Educat ional TCD
General Operating Procedure 1. Check to make sure that the Te O filament current is switched OFF. Plug in and turn on your G'C. Allow the TeD detector oven to reach temperature (1()()<-'C) and stabilize. With the " Di splay Select" switch in the
lJPposition. press on the TeO Temperature Actual button on the front control panel to read the TeD cell temperature. 2. The carrier gashead pressure is preset at the factoryto 1000min for the Silica Gel col umn. Look on the right side o f the GC for the carrier pressure that correlates to a flo w oft OmUm in. Because differen t columns require different flow rates. the carri c-rhead pressure m ay be adjusted by the user with the trimpot above the '''CARRIER 1" buttons. For this GC. carrier cylinder p ressure is normally set at 3Opsi, whic h is 10-20mL higher- than the column head pressure. Th e column head pressure is the pressure developed by
thecarriergas as it flowsthroughtheanalytical column. 3. Make sure that the setpoint and actual pressures arc within 1psi. 4. Damage or destruction of the "I"CD filaments wil l occur if current isapplicd in the absenceofflowing carrier gas. ALWAYS verify that carrier gas can bedetected exiting the TeO carrier gasoutlet BEFOREenergizing the TeO filaments. The carrier-gas outlet tube is locate d on the outside of the Column Oven on the same side as the detector. Place the end ofthe tu be in liquid and observe (a little spit on a finger can suffice). If thcreare no bubbles exiting the tube. there is a flo w problem. DO t'OTnun on the TCD currenl ifcarrier gas flow is not detectable. A filame nt protection circuit prevents filament damage ifcarrier gas pressure is not detected at the Gc. but it cannot prevent filament damage under all circumstances. Any lack ofcarrier gas flow sho uld be corrected before proceeding.
5. With the TeO filaments switched Off, zero the Data System signal. Switch the filaments to LOW. The signal' s deflection should not be more than 5-1OmV from zero for a brand-new TeD detector. Any mo re than a 5- JOm V defl ection indicates partial or complete oxidation ofthe TeD filaments; more deflection means m ore oxidation . Therefo re. it isa good habit to use the D ata System signal to chec k the workin g order ofthe TeO filaments. 6. In PeakSimple, set an isothermal Col umn Oven temperature ramp program as follows :
Hold Bi!!!m Firnl Temp. 7.00 0.00 80.00 7. Click on the Zero button to the Iefl ofthe chromatogram window in PeakSimple to zeroout the Data Systemsignal. l lit the RUN bunon on your GC or hit the spacebar on your computer keyboard to begin the run. You may a lso open the 8.CQuisition pull-down menu and sekct,Bun, but this gets d ifficult unless yo u ha ve a partner, [nina] Temn. 80.00
since yo ur hands are occupied with the sample syrin ge.
- .. 8. Using the 1mL syringesupplied with your GC. inject sample into column through the On-Column Injector.
190 (of 550 ) 2006(-2016)
191
POPULAR CONFIGURATION GCs Ed ucationa l TCD
Expected Performance Every compound possessessomedegreeofthennaJ conductivityandthereforemay be measured with a TeD detector. TeO detectors are most often used wi th helium as a carrier gas because of belium 's high thermalconducti...- ity, but othergasessuchas nitrogen. argon, or hydrogen may also beusedasacarrier gas. A TeD detects all m olec ules in concentrations from 1()()01o dO\\TI to around l OOppm. and is especially useful for meas u rin g ino rg anic gases like Or N 1 , CO & CO.2"
Teo Detector No is e
:!'.IE! ' ! " ,E_
!
It- _ _
! t~ Ji g " . lo,. ;: li
I
,
¢: '= ''''' "110,~r:;"7 ~i' CH«S "'''''~'~
Col umn = 1m Silica Gel Ca rrier = Helium at 10mU min TeD current = LOW
%19'>
, , • s;
I• iI
I
I
II
Noise Level = Appro ximately 20!lV from peak to peak
TCD Temp = 100CC
Temperature Program: Initial Hold ~ OO'C 10 00 0.00
s
•.3 -. .......,
Final
8O"C
-'- _
9 .
"S..
, •
CC'... • .....
I.. . ~ .~ • ...... I~ ~ ' ~
• / lA, " )\ ....r----j ~. ..·1.....\
.'t,,')
..
....'""?".
I !
2OJ.1V
i,
-
•••
I
.;~i~~~~~~~~~~~~~~~~~~~~ - ~-~lirrIi
't-.'="
Educational TCD GC Factory test ru n of an Column = 1m Silica Gel Carrier = Helium at 10mU mi n Sample = O.Sec 10.000ppm CO2 TeO current = LOW TCD Temp = 100"C
f~
i
i
r
j
/
Temperature Proqram. Initi;a] Hold Ramp 8O"C 7.00 0,00
\. RESUlTS
CO!llIlOrJe!Jl
Reter:ti91'1
0 2 N2
0 .4 50
C02
2.500 Total
......
12 52 .>1980
13.64 50 1266.6440
191 (of 550 ) 2006(-2016)
192
POPULAR CONFIGURATION GCs Edu ca t ional TCD
Ex pecte d Performance
Te o Room Air Ana lysis
-
-
,. ,- ,.. ,,• t ce~:r:; ~,. ~'.Ul.c., ,
iiI..- .
~ :S ~ :!iI & "". ~
Co lum n: 3' Silica Gel Carrier: Helium at 10mUmin Sample: o.scc room a ir, direct injection Te D current LOW TeO temperature: 100"C
_._- ~
<
<.
I
2
B
~
3f
I
-.
---
Temperature Program:
Initial
roc
Hold 4 .00
Ramp 0 00
Final
8O'C
,
\
B
~
I
.a J l)!:I
...±.1.!..lJ ,= Results: Component ° 2 N2
CO,
Retentio n
0.716 2.766
~
"
Area 1021.3830 1.5060
Total
1022 .8890
The CO 2 content of the room air analyzed is aoproximate ly 350ppm.
192 (of 550 ) 2006(-2016)
193
POPULAR CONFIGURATION GCs Educational TeD Suggested Class Experiment: " Waiting to Exha le" CO2 isa natural by-product ofh wnan respiration. Our lungs get oxygen v.. .hen we inhale and release CO: when weexhale. Wben We' hoJdourbreath, the concentration ofCOz increases. In thisexperimerrtal gas chromatography analysisofhwnan breath.the students will supplythe samples. They will exhale into and trap their breath in the syringe, then it will be injected into the Educational Te D system and analyzed fore02 concentration, Have a contest for the highest CO2 concentration: the student with the most CO2 in his or her breath \\iII win. Whomeverpasses out is disqualified! I. f ollow steps 1-4 ofthe General Operating Procedure.
2. InPeakSimple, set an isothermalColumnOventemperaturerampprogram as follows: Initial Temp. Hold Ramp Finallewn 80.00 4.00 0.00 80.00 3. Locate the 3mL (3cc) syringe supplied wi th yourGC. remove its needle. and give both parts to a student. Instru ct the st udent to exhale into th e tip ofthe syringe whi le pulling back on the p lunger. Students need not touch the syringevvim their mouths forit to ...vork, Fill the syringe completely, then replace theneedle. Depress the ph.mger until the syringe contains O.5mL ofbreath, NOTE: For sanitation concerns. it may be prudent to have one new, sterile syringe for each participating student. Sterile 3mL syringes complete withneedles may beacq uired for about SO.18 each from:
VWR (800-932-5000): BD-309587 Syringe-Needle, 3mL Sub-Q 260 5/8 Luer-lok'" 4. Click the Auto Zero button in PeakSimple, then press the RUN button on your GC or the spacebar on your PC keyboard to begin the run.
5. Inject sample into the On-Column injector. 6. Save and print the resulting PeakSimple chromatogram with the student's name for the sample identification. Typical results are about 12- 14 area counts per 1% ofeO l . 7. Repeat steps 2-5 for each student. Compare chromatograms to find the v...inner.
Example TeO Breath Analysis
C ~Iiii'j1.g·"", g
Column: 3' Silica Gel Carner: Helium at 10mUmin sample: 0 5cc human breath, direct injection TCD current LOW TCD temperature: 100"C Temperature Program: I n ~1 Hold &!fig 8O"C 24.00 0.00
r.. r _ _ _ _ H 1 !!Iliftii ;: 1
Total
,
I
I
+
~
I
\
I
2.700
I
I
Resufts:
CO,
"""
•• i
8O"C
Retention 0.700
t:
me -~Ii-::>o»>I5Oi'%l:ItU
Final
Comoonent °2 N2
, , .-! .
Area 1379.4740 6 1.9540 1441.4280
,I
~,
I
±!:L.l ,~
\,
I
"
•
~_. ~-
r\
J\
I .:::.±J ,~
193 (of 550 ) 2006(-2016)
194
POPULAR CONFIGURATION GCs Gas-less T• Educat iona l System Overview YourSRIGas-less'>' EducationalGC is equipped with a Catalytic CombustionDet...'"Ctor (CCD). builtinAir Compressor, temperature programmable Column Oven, Haysep D pocked column,On-ColumnInjector and built-in. single channel PeakSimple Data System, and optionally, Fast COOt-dO\.V11 fans. It is designed to teach the principles of Gas Chroma tograph y wi thout the ex pense and safety hazards of compressed gas cylinders.
,...: ..- -~ ." -.......-... _ "'
. ,.
t
~ CCD Detector
-
I
- ~~~--~-~-;; .-: r, ;;~~~~ B>. ='~- - -
,-
,
"1
'
/ .
..:. •
•
,
3' Haysep 0 Column
-._ _-- .--._..... .II:f. !;"
...,
~
--~
..
.
..
. ,:
: :l tl ' !- j~ ~ '~ I I r !
.,. ".. . .'.t.. :' : . ~-
~:; ~
1o!-
,"..
,
_~ ~
On-Column Injector
The CCD is about as sensitiveas a TCD.but hasthe hydrocarbon selectivity of an FlO. It operates on air alone. which is supplied b)' the built-in Air Compressor at around 12psi. If you chose optional fast cool-
dO\\TI fans, they will automatically reducethe Column Oven temperature at the end of an analysis to theinitial temperature in less than five minutes. Most isothermal applications don't require fast cool-down fans; in these cases. the oven lid is simply manuallyraised for cooling.
194 (of 550 ) 2006(-2016)
195
POPULAR CO NFIGURATION GCs Gas-less™ Ed ucat iona l CCO
General Operating Procedure I. ConnectyourGC to your Windows PC with PeakSimpleinstaJ led. PluginyourGC and rumits power on. 2. Set the Column O ven temperature to 13O"C in PeakSimple as follo w-s: InitialTemp Hold Ramp Final Temp
130.00
10.00
0.00
130.00
In anisothennal operation like this. the Hold period determines the lengthoftheanalytical run. .\ 'OT£: The Haysep D packed columnis standard for this GC system becauseof its separation qual ities and durability. To avoid possible damage to the packin g, do not pro gram your Column Oven to heat abo ve 150°C.
3. Let the system stabilize for at least 10 minutes. allowing the CCD detector to adj ust to the inc rease in temperature.
4. Click on the Zero button to the left of the chromatogram window in Pcakgimple to z ero out the: Data System signal. Otherwise. the signal starts out at 10 00 m illivolts. Press the RUN button on your OC or the spacebar on your computer keyboard to begin the run .
I~'El. A~oZero o
button
5. Inject sample into the On-Column Injector. A I III IOOOppm methanol/acetone sample is the factory test standard for this configuration.
Column Notes ".
/_J'
, i
1m Hayesep 0 packed co lumn
Hayesep D packed columns are useful for analyzing gases
and low molecular weight compounds such as alcohols. aldehydes. and keto nes. Fo r heavier mol ecular weigh t liquids. use a 30m or6Om ),0\."1"-1 capillarycolumn,
~-----/
30m MXT·1 .53mm
.----
....
/"
/
/
• c;,pillary column
195 (of 550 ) 2006(-2016)
196
POPULAR CONFIGURATION GCs Gas-leas" Educational CCO
Expected Performance The CCD Detectorin your Gas-less>' Educational GC is mountedon thewallof the Column Ovenin a brass housing. It consists ofa tinycoilofplatinum wire embedded in a catalyticceramic bead. Thiscatalytic ceramic bead is housed in a plast ic shell. A 150milliamp current heats the bead to around 50O"C. The CCD is maintainedin an oxidativeen..ironmenrby the air beingused asa carriergas. Whena hydrogen or hydrocarbon molecule impacts the hot bead. it combusts on the surface, raising the temperature and resistance of the platinum wire. This change in resistance causes the CCD Detectoroutput to change, which producesa peak.
F·; ldi:,
CCO Detector No is e Run
I L5Io
0;.-
U , l!'_ ~ I C ~ IiiI !!J 8 ' ii E - f I l ,u l Q _ lEl t ::o .....ao~.,.......
Column = 1m Ha yesep 0 Flow = 37m Umin
' '-
I
'-" '
~~
. !~ I ,, 1
r
• • ",,
,
' .......7, ~
Isothermal Temperature Program: Initial Hold Bim1 Final 0.00 15.00 8O"C
eoc
'iii :0-
enlarged for clarity
"..
~'-
...'
I
.
~
-,
l
Noise level = approximately
50~JV
from pea k to peak
~
1/
'.
~ .~
I
V
·1 .(1000
.±..WJ
.!.l..<..EI
,~
If bt , "
, 1."0 U.
--
~_
Factory Test Run of a
.~
.
.
, e •• '-
.~
.
_ ~
~
I~
,~
•~
I
,
" I,
1
<"")
Educational GC System - !§l·t Colu mn =1m Hayesep 0 Flow = 37mU min Sample = 1~ L 1000ppm Methanol/Acetone m ix; direct injecti on
1+
"
\
Isothermal Temperature Program: Inibal Temp Ramp Final Temo H"d 130'<: 10.00 0.00 l3O'C
\ \
,
\,
•
I
il; b .~ :"''' ."!, ;'Y,r;. f't>.~l"'-
,
t
,
Gas ~less TM
--
F'
n~ ;i g " . i "' . €. "'1'; ....
1.00:.
,
RESULTS:
<;
, V)
•••~ , ~
Neg ative water peak
.
.ilil!.J
"
Component
Retermon
Area
Methanol Acetone
0.816 2.000
6~5 .3 570
Total
69585600
13.2030
196 (of 550 ) 2006(-2016)
197
Chapter: Installation: .
TOPi?: ,, \ ~iftin~th,e 86.10G,} pd310GCs
Lift here
As illustrated by the photo above, lift the 861 DC and 310 GCs by grasping the GC under each side. Befo re lifting, check to make sure the bottom cover is securely attached to the chass is with six screws, and that the power cord, gas line connections and serial port cable are disconnected.
M an201. pub
197 (of 550 ) 2006(-2016)
198
(
Chapter:
'I
INSTALLATION
I
l~~------------------~)i I
Topic:
Initial System Inspection And Setup
Upon receiving the chromatograph and data system from the freight carrier, immediately inspect the containers for visible signs of damage. If any external damage is observed, notify the delivery person immediately. If no external signs of damage are present, proceed to inspect the contents of the containers. If the materials appear to have been damaged in shipping , immediately contact the carrier and submit a written report describing the extent of the damage. All packing materials and containers should be retained if damage is discovered until the carrier has been able to inspect the damaged goods. If no damage is discovered, packing should be retained until proper unit operation has been established. The chromatograph, serial data interface cable and manual are shipped in one container, along with the GC accessory kit. This container is a reusable plastic shipping container. These containers are rugged and shipped easily via freight carriers. Most importantly, the plastic container protects larger, more complex and delicate instruments from costly damage to external accessories. Save the packing materials after removing the chromatograph, for future transportation. The contents of the containers should be checked against the packing slip accompanying the shipment Verify that all specified accessory items ordered such as columns, syringes and the like have actually been shipped. If any items have been omitted or are missing from the shipment, contact SRI Instruments for location and/or replacement of the item. The SRJ model 8610C gas chromatograph requires either 110 VAC at 60 Hertz or 220 VAC at 50 Hertz , dependent on which AC power supply was specified when ordered. Both AC power supplies support the Scprong grounded outlet Proper grounding is required to minimize AC line interference and eliminate ground loops. The 220 VAC plug is keyed so that it cannot be inserted into a 110 VAC receptacle . A generator or high-current inverter may be used for operation from a vehicular power source. If an AC power generator is used , as is done in the field, line voltage and/or current may fluctuate. Appropriate steps should be taken to minimize any inconveniences caused by line noise or an irregular AC waveform. A standard model 8610C gas chromatograph measures approximately 18.5" x 14.5" x 12.5" and require s a counter surface space of about 32" x 22". Eight inche s of clearance are needed in front of the left side control panel for the fan, gas line access and the AC power switch. Another six inches of clearance are suggested in front of the right control panel and to the rear of the unit for safe operation and ease of access during routine service. The red oven cover requires a clearance of at least 24" (measured from the counter top) in order to provide adequate access to the column oven for service. If the chromatograph is equipped with optional accessories such as the 10 station purge and trap auto sampl er for the optional built-in EPA Style purge and trap, the access to the left side of the chromatograp h must be increased by a minimum of an additional 12". The compact footprint of the system is economical on lab counter space and is ideal for mobile environmental installations.
..- .
Prior to placing the chromatograph into service, the gas supply and related plumbing should be insta.lled and routed. The gas cylinders should be located outside the Jab where possible, with only the lines plumbed inside to the chromatograph. Gas cylinders should be secured in place with chain or nylon strap to prevent a cylinde r from falling and snapping off the valve. A gas cylinder contains up to 2700psi and can become a deadly projectile if the valve stem were snapped off. A regulator should be used to set the supply a gas pressure reduced to a va lue appropriate for introducti on into the GC. Gas pre ssures at each cylin der pressure regulator should be maintained reasonably above the carrier gas regulator setting in order to provide a range of control (a supply pressure set to no more than 20psi greater than the EPC setpoint is recommended). A block valve should be inserted on the output side of the regulator to permit line service when needed, and to per mit immediate shut-off in case of emergency. D:IEP" ..DOCS\lNSTPG01.£PD
REV. 07-23-9(;
198 (of 550 ) 2006(-2016)
199
r
Chapter:
INST ALLAnON
Topic:
Initial System Inspection And Setup (continued)
,- -- - - - - - - -- - - - - - - - - - - -- - -
)
Refrigeration-grade copper tubing may be used for all of the gas supply lines to the chromatograph. Plastic tubing should never be used as it permits contaminants, includung oxygen, to permeate and this can cause damage to thermal conductivity detectors (TeDs) and capillary columns, in addition to degrading the performance of the electron capture detector (ECD) system . Except in the case of the ECD de tector. copper tubing destined for gas supply line s may be rinsed out with methyle ne chloride. followed by methan ol. If the tubing is destined for use with the ECD, do not use methylene chloride or any other halogenated. solvent as this would wreak havoc upon the detector indefinitely. It is preferrable to switch to 111 6- stainless steel tubing, if available, for the ECD gas lines. It is also a good idea to flame the tubing with a torch while running clean carrier gas through it so tha t any possible pre-existing contaminants will be eliminated from the tubing run. The tubing is heated until it changes color. In order to eliminate moisture from the gas supply lines, it is recommended that molecular sieve filters be installed in all of the gas supply lines. SRI 8610C gas chromatographs are factory-equipped with electrically hea ted 118" x 3 " molecular sieve-filters on the carrier and sparge gas lines. Although not indispensable, an oxyge n filter is a worthw hile optional addition to an ECD carrier gas supply line. Extremely pure ga s should be used exclusively on the ECD detector (99.9995% purity ).
When routing the gas lines, care should be taken to avoid creating spots where moisture can gravitate and accumulate. Also, gas lines should not be routed near electrical outlets due to the potential for short circuiting created if the bare tubing were to come into contact with exposed electrical contacts . instantly melting the tubing at the short circuit site and releasing gas into the area. If the gas were flammable, a torch-like flame might be produced. If the gas did not ignite immediately. an explosion hazard would be created. Once the gas line connections have been made and leak-tested. and the gas chromatograph has been located in the counte r-top position where it will. be used, plug the GC into a properly grounded A C outlet, and energize the unit. Gas pressures may then be adjusted to proper operating condi tions by means of the gas pressure setpoint trimpots located under the red pro tective oven cover. Please revi ew the section regarding the setting of these setpoints for specific information regarding the ir use. Connect the 6' DB-9 serial cable to the R.S-232 connector on the left side contro l panel of the GC, and connect the opposite end of the cable to the COM port to be used for co mmunications on the PC. At this point, start the PeakSimple program and wait for the main chromatogram sc reen to appear. Once the PeakSimple program is running, select the FILE- CONTROLS • CHANNELS menu (CONfROLS • CHANNELS - DETAll.S menu in the M S-DOS version) and observe what temperature the default temperature is programmed to. This temperature should also be displayed on the chromatograph's LED display when digital display has been toggled em to OVEN ACfUAL position. If these two figures do not march within two degree s after a few minutes, select the CfiAl'Ir.'NELS - TEl\1PERATURE menu again and verify that if there is a temperature program loaded into memory, that it meet your req uirements. Otherwise you may edit. replace or clear the displayed temperature program. Return to the main screen. If the temperatures match, then the data system is co mmunica ting with the chromatograph. If there is no response from trn: chroma tograph data system to the PC, the port address (and/or data acquisition type in the MS-DOS version) information may be set incorrectly in the OVERALL sc reen (DETAILS screen in MS -DOS) for each channel. This will typically produce the "Channel I not functioning- message. Verify tha t the proper hardware settings have been implemented. Once this has been done, communication between the chromatogra ph and the data system is typically established by activating the channel in the CHANNELS scree n. Now the system may be adjusted to operating conditions . D : \ ~OOCS'. ['IlSTPG02. EPD
REV. 07-21-96
199 (of 550 ) 2006(-2016)
200
lOul 26 gao liquid injection syringe
Contents of accessories krt shipped wrth new SRI GCs.
1)
6' 08-9 serial cab le for connection of GC to computer ( Student model without data system will not have th is item ).
easy install ation of 1/8" copper or 1/16" stain less steel tubing
2)
Tubin g cutter for
3)
3m lleak check syringe ( fill with alco hol/Water mix to check fitti ng for leaks )
4)
1ml gas syringe and needle for injection of gas samples into GC
5)
1 Oulliqu id injection syringe
Man l4 Spub
200 (of 550 ) 2006(-2016)
201
INSTALLATION: ELECTRICAL POWER REQUIREMENTS
Plug all SRI prod ucts
into a Ground Fault lnt eru pter ( GFI )
equipped electrical outlet. The GFI will trip before a electrical fail ure in the GC can
result in a dangerous Shock to the operator, an important safet y feature. If you r outlet is
not already GFl equipped , have your electrician install an appro ved GFI such as th e one shown which
sells for under $1O.
The GFI has a Test and Reset button. If the
GFI trips. you must reactivate the G FI by pressing the Reset
H031 .DOC
201 (of 550 ) 2006(-2016)
202
8610C Power Consumption
711 612002
Basal Power Wrth no zones heating, Power usage = SOW Wittl 2 Detecto r zones heating = 150W Wrth Detector Z ones Stabi lized, Total Basal Power = 100W
Column OVen Tempe rature Program 40C to 300C @ SCl min Average Temp
45 60 85 110 127.5 145 165 185 205 222.5
240 260 280 295
Colum Oven Power Consumption Watts Temp Range
30 50 70 90 110 130 150 170 190 210 230 250 270 290
40-50 50-70 70-100 10()..120
120-135 13 5- 155 155-175 175- 195
195-215 2 15-230
230-250 250-270 270-290
350 300 E
"go 250
"' 200
"
~ 1 50 !.
E 100
•
~
50 0
290-300
Sample PoInt5
Maximum Power Usage Ballistic Heating to 30De = 675W Total Power = (Basal + Detector + Column Oven) = 825W
Isathennal Power Usage Column Oven Stabil ized @ 300 e 2 detecto rs @ 150C Total Power = (Basal + Detect ors + Co lumn Oven) = 400W
202 (of 550 ) 2006(-2016)
203
Chapter: INSTALLATION Topic :
Power Supplies and Space Requirements
Once the equipment has been removed from aU the packing material, check the contents of the container against the packing
o
slip and make sure everything listed is included. If any item(s) have been omitted or are missing, contact SRI Instruments for location and or replacement of t he item(s).
•
n OVA C
The SRI model 8610C gas chromatograph requ ires AC power at either 110 VAC at 60 Hertz or 220 VAC at 50 Hertz, depending on the AC power ordered. Both AC power supplies are equipped with
•
a three prong grounded outlet (see diagrams to the right). Proper grounding is required for safe operation. Do not disable the ground prong under any circumstance . These plug configurations are for ElA standard U. S. outlets. It may be necessary to replace the plug provided with a local standard plug.
A standard SRI 8610C GC measures 18.5" X 14.5" X 12.5" and requires a minimum counter space of 28" X 22" X 23.S" for proper operation (see diagram to the right). Roughly 8" of clearance beside the left side control panel is needed for data cable, gas line and power switch access. 6" of clearance to the rear of the GC and 11" of clearance above the GC is required. This will provide adequate access to the column oven for maintenance and provide space for proper GC ventallation. To the front and right side, 1.5" of clearance should be adequate to prevent the GC from coming into contact with surrounding objects or falling off the counter. Th e right side of the GC does contain general information on your instrument and some operators may want additional clearance for easy reference. The front control panel of the GC should be easily accessible m order to properly monitor digital display and control operating conditions, as we ll as pro viding access to the injection port for sample inject ions. C:\.\fANUAL',.cHAPTER1'.lNSTPSSRDOCTIf
220VAC
Required Operating Counter Space 2S"
Top
>---
View
22"
18.5" -
-
---1
I
14 .5"
1 28"
Front View 1---\8.5"----1
2] .5" 12.5"
REV. os-os-ss
203 (of 550 ) 2006(-2016)
204
Chapter: INSTALLATION Topic:
Installing Gas Supply
Pressure Regulator r""'::,,\~
Exit Pressure (no more tban 20 psi greater than
:Totai Remaining C)'Under Pressure
required GC pressure with a maximum of 80 psi)
-ri-r-r-r-: valve Stem
l}:::{tl]i-h=n Flow Snubber FrU - - -.....~~::::I (Flammable Cases Only)
""==:::::::
SbutofTVaJ,,"e
-----I'
,
Commercial Gas Cylinder
ToGC
Once the necessary gas supply cylinders have been properly secured to a strong foundation (see previous page), related plumbing must be carefully installed and routed. Always use a pressure regulator on the cylinder to provide proper pressure regulation to the GC. A shutoff valve should be inserted on the output side of the regulator to permit line service when needed. A flow snubber on the output side of the regulator is also highly recommended for hydrogen and all other flammable gases. Unless you are utilizing an ECD, refrigeration grade 1/8" copper tubing is recommended for all of the gas lines from the cylinder pressure regulator to the GC. Due to the exceptionally high sensitivity of an ECD, GCs equipped with this detector require 1/16" stainless steel tubing to reduce the potential for gas line contamination. It is also advisable to flame the stainless steel tubing with a torch until it changes color while flushing with clean carrier gas. This will help to remove any potential preexisting contaminants from within the tubing. An oxygen filter is also a worthwhile option for ECD carrier gas supply lines due to the damaging effects of oxygen on the detector. Plastic tubing should never be used for the gas supply lines due to its permeability to contaminants such as oxygen which can cause damage to thermal conductivity det ectors (TeDs) and capillary columns as well as EeDs. Proper supply line routing is also very important. Avoid routing gas supply lines near electrical outlets to eliminate any potential hazards associated with electrical shorts and/or flammable gases . Metal gas lines can very easily fall across the two prongs of any plugged in electrical device and start a fire if routed near an electrical outlet. After gas supply lines have been properly installed, pressurize the lines and check all associated fittings for potential leaks. In order for electronic pressure control units to operate properly, do not set gas pressure coming from the cylinders any more than 20 psi greater than GC requirements. For example, if carrier gas head pressure is set to 10 psi at the GC, then set carrier supply pressure from the cylinder above 10 psi but no greater than 30 psi. C:'J.w..1JALICHAPTER1\ThSTGAS2.I)(XITM
-_
REV. 08.(J7·96
204 (of 550 ) 2006(-2016)
205
Chapter:
INSTALLATION
Topic:
Gas Supply Selection
Helium is the recommended carrier gas for all standard SRI installed
detectors. These detectors include: TCD, FID, PID, £CD, DELCD, FPD, and NPD. If helium is unavailable, nitrogen is an acceptable carrier gas alternative. If nitrogen is used with a TeD, the filament current switch must be set to low to avoid filament damage. Do DOt use hydrogen OC any other flammable gas as a carrier gas for any SRI 8610C GC. These units have electronic pressure control and a simple column or injection port leak could release dangerously high levels of flammable gases. Some detectors and accessories require additional gas supply types for proper operation. Argon/methane or nitrogen is required for ECDs as make-up gas. The recommended make-up gas is argon/methane which provides the best
Protective cap
-,
ContenI
aDd status
rag -
~
~
r> .. ..
sensitivity and largest dynamic range for the ECD, but nitrogen is a readil y
available, cost effective alternative (see the manual section on the ECD for more details) . FIDs, FPDs, and NPDs all require hydrogen and air in order to create the combustible fuel mixture for the detector flame. Hydrogen is an extremely flammable gas and must be handled appropriately. Always consult local safety regulatory agencies for proper procedures for handling compressed and/or flammable gases. An internal air compressor is an available SRI GC option as a SOW"Ce of air. GCs with a purge and trap accessory also require some type of sparge gas. -Generally helium can be used as both a carrier and a sparge gas supply. Mcthanizer accessories require hydrogen gas as a reactant in the catalytic reduction o f CO and Co,. to
CI4.
We recommend the use of medium to high quality gas sources for all required gases in order to prevent any operational problems associated with low quality gas. ECDs require an extremely pure carrier gas source of 99.9995% or higher. SRI GCs are equipped with smaIl internal molecular sieve polishing filters on the carrier gas plumbing only to filter low levels of contaminants. If the quality of gas available is questionable, an larger external filter may be necessary to filter excess contaminants such as moisture. Please call SRI technical support with any additional questions on gas supplies or specialized applications.
IMPORTANT SAFETY NOTE When handling gas cylinders, remember - never transport or move a gas cylinder without its protective cap securely in place. Gas cylinders can contain up to 2700 psi of compressed gas. If the cylinder were to suffer an acciden t causing the unprotec ted valve stem to be broken off, the force of the escaping gas could convert the cylinder into a lethal projectile capable of travelling hu ndreds of feet and penetrating structural wa.11s. Once the gas cylinder has been placed in the loca tion where it will be stored or utilized , it should be secured by means o f a chain or belt securely fastened to the wall or other foundation. One strap may or may not be adequate depending on the installation - consult local safety regulations. Once the c ylinder is in place and secured, the cap may be removed. so that the gas pressure reeulator mav be attached for use. C:\M ANUAL\CHPTER1\ lNSTGASl .EPP
Typica..I gas cylinder sboIMl.. Noce mat the protective cap is in place. protecting the valve from damage. Cylinders are clearly labelled and tagged wber:I de livered for use. In
some areas, cyliMers are color-ceded for haMLing safety
Gas V2Ive -
.'
\
Regula""
Strong bell cr chain
ro.. • =wing cylinder to
•
""""'" The protective cap is removed ooly after cylinder is in place and secured by aI
least one chain or belt REV. C8-06-96
205 (of 550 ) 2006(-2016)
206
[
Chapter:
INSTALLATION
Topic:
Checking for Gas Leaks
J
Once all of the appropriate gas supply sources and lines have been properly installed, along with all other GC columns and connections, the entire system should be systematically pressurized
and checked for possible leaks. Begin by opening all of the compressed gas cylinder valves and setting exit pressures to the appropriate value for each cylinder regulator. Remember that cylinder exit pressures should never exceed the required GC pressure settings by more than 20 psi and 80 psi is the maximum pressure that the GC can safely handle. First check for leaks in the lines and connections between the compressed gas cylinder and the GC flow control fluistors . With the system pressurized and the GC power turned off, close each of the compressed gas cylinder valves one at a time and closely watch the pressure indicator on the cylinder regulator to see if pressure decreases. If the system is leak free between these two points, the cylinder pessure indicator should not noticeably decrease for at least five minutes . If pressure does noticably decrease over this time period, then it indicates a significant leak somewhere between the cylinder output and the GC fluistor. Any leak. especially with flammable gases. must be immediately located and repaired. The best way to check specific connections for leaks is with a leak check solution (see section below on Using Leak Check Solution). If pressure test indicates that the system is leak free from the cylinder to the fluistor, then proceed to check the rest of the carrier gas system for leaks. If the system does have a leak. locate and repair prior to proceeding. Next check for leaks between the fluistor and injection port. Begin by disconnecting the column from the back side of the injection port. Next insert some type of pressure blocking fitting on the injection port where the column was attached. A standard Swagelok nut with an injection septum in place of the ferrule will work quite well. Turri the GC power and gas supply back 011. Use the control panel to see what the actual carrier pressure value is and write it down. Now turn off the carrier gas supply at the cylinder once again. Wait 5 minutes and then use the GC control panel to view the actual carrier pressure once again. If this value has decreased in the 5 minute time frame and the previous test results were negative, it indicates that there is a significant leak somewhere in the interal GC carrier gas lines between the fluistor and the injection pen. Once again immediately locate and repair any leaks using a leak check solution as described below. After all of the leaks upstream from the column have been eliminated and confirmed by the two pressure tests described above, properly attach your colwnn to the injection JXJrt. Use leak: check solution to check all of the fittings within the column oven for leaks and repair any that you find .
Following all the instructions above will assure the operator that the system is leak free. Any time fittings are changed or the GC is relocated, the system should be rechecked for leaks. Failure to properly repair leaks can cause safety risks as well as operational malfunctions.
n
"
A 3 ee medical syringe is excellent fur dispensing leak: check solution. An eyedropper. pipette or squeeze bottle may also be used.
the tubing enters the nut and at threaded fittings .
Gas line Swage lok bulkhead litting/
Leak Checking Solution SRI recommends that a solution of 50% water and 50% alcohol (methanol, ethanol, or propanol) be used as a leak. check solution. The water-alcohol mixture leaves no residue which could leak through the fittings and cause system contamination. Furthermore. water. when used alone and . due to its high surface tension, tends to bead rather than flow into spaces between the tubing and the connectors where leaks may occur. A leak will show up as a stream or froth of tiny bubbles. Inspect any lealcing fitting for damaged threads and reversed. missing, or damaged ferrules. C ;\MANUAllCHAPTE.R11L.EAKCHK.EPD\Th:I
REV.~-96
206 (of 550 ) 2006(-2016)
207
Chapter:
INSTALLATION
Topic:
Removing The Chromatograph From The Shipping Container
TQP view of container. lid closed
Top view. lid QPeI1. GC in container
112" nut and holts
TQP view, GC out of container Rounded
fastener edge
Strap -I--I-r'tmfastened
SRl gas chromatographs and stand-alo ne units are shipped in a sturdy, protective shipping container. The molded gray plastic container is reinforced and resistant to blows and crushing pressures typically encountered while en route to the customer or job site. Upon receipt, check to see that there is no obvious damage to the exterior of the shipping container. Notify the delivery person immediately of any such damage. The lid of the shipping container is secured closed by a 112" nut and bolt set each located on either side of the container. To open the lid of the shipping container, completely remove the two nut and bolt set and simply open lid . Screw the nuts back onto the bolts and place in shipping container for future use . Th e GC is held in place within the shipping container in custom packing material consisting of (1) rigid foam bottom packing base, ( 1) soft foam top plate, (2) cardboard corner protectors, and (2) straps with fasteners to bind GC within pncking material . Some SRI GCs can weigh more than 70 pounds, and care must be taken to prevent injury when removing from shipping container. To properly remove the GC from within the shipping container, firmly gras p the two visible strap s running across the soft foam top plate between the two cardboard corner protectors. Being careful to properly bend your knees, lift the entire GC, still contained within the packing material, straight up and out of the shipping container. To remove the packing material from around the GC, begin by removing the two straps holding it all in place. Place your fingers beneath the rounded strap fastener edge and pull up and back. When the strap loosens up, pull the free end of the stra p completely through the fastener. Once both straps have been unfastened, remove the two cardboard corner protectors along with the soft foam top plate and place back in the empty shipping container for safe keeping. Next, slide your fingers between the metal GC base plate and the rigid foam bottom packing base, and firmly grasp the bottom of the GC with both hands . Once again being careful to properly bend your knees, lift the GC up an d out of the packing base. Place the packing base , with straps still attached, in the shipping container with the other packing materials. Be sure to save all packing materials along with th e shipping container for all future shipping needs . O;\MANUAI.:\SHIPCTREPDITM
FEY. 7-24-96
207 (of 550 ) 2006(-2016)
208
Chapter: Installation Topic:
Repacking Your Gas Ghro matograph or Stand Alone Unit For Safe Shipping
Cardboard Comer Protectors
GC or Sta nd Alone Unit
Rigid Foam Packing
-===::c::=d
• 4
!
_
±.jUJ
_
"""~.-_-'\
Straps withFasteners~ G
When reshipping an SRI GC or stan d alone unit, be sure to use the original shipping container and all of the original packing material to minimize the potential for damage during shipment. First, make snre that you have all of the primary packing pieces : ( I) molded gray shipping container, (I ) rigid foam bottom packing base with (2) straps and fasteners, ( 1) soft foam top plate, and (2) cardboard comer protectors. To properly pack your GC or stand alone unit, begin by placing the bottom packing base flat on the floor with the straps coming up through the surface of the base as shown in the diagram. Place yo ur GC on top of the base with the legs inserted in th e appropriate cutou ts. Next, place the soft foam top plate on top of the GC and place the car dboard corner protectors over the soft foam top plate. Pull the straps corning through the packing bas e up and around the GC. as well as all the other packing material and secure the two strap ends together. It may be helpful to straddle the GC and use your knees to squeeze all the packing material together as you firmly tighten the straps. Be sure the straps firmly secure the GC or stand alone unit in the packing material to properly protect your instrument. When you are sure the straps are firmly and securely fastened, gra sp the two straps running across the soft foam top plate between the two comer protectors. Properly bend your knees and lift up the entire GC, contained within the packing material. and gently place into the molded gray shipping container. Place bubble-wrap in the remaining empty spaces within the container to prevent any pot ential shifting during shipment. Also. include a packing slip inside. as well as one on the outside of the container. and then close the lid. Lastly place the 1/2" bolts in the two holes each side of the top surface and properly secure the lid closed with the 112" nuts. It is also important to properly insure your GC with the shipping company due to its high value. You r GC is now ready for safe shipping.
.'-,
C;\MAl\"UAL\CHAl'TERI\REPACKGC.DOCIT\II
208 (of 550 ) 2006(-2016)
209
(~------------------~---~---------"
Il
Chapter:
INSTALLATION
Topic:
Tubing Cutter - For Facilitating Gas Connections
:
_
Included in the optional gas line installation kits that may be purchased with each SRl Instruments gas c hromatograph is a disposable tubing cutter. Thi s tool is capable of producing clean, fast cuts in chromatography tubing that rival more time-eonsuming tubing cutting methods. The hardened, beveled cutting surface of the tool enables the user to effect a through-and-through cut upon the tubing in one motion , cutting copper and stainless steel tubing with ease. The cu t obtained allows both metal and graphite ferrules-to slide onto the tubing without the normal filing or reaming necessary after cutting tubing using other methods. No smearing or burring is prod uced if this tool is used as directed. Users can make up to ten connections in the time that it took to cut, file, ream and connect one single tubing connection. Since the tubing is sheared and not twisted or stressed, the inside passage is not deformed or restricted, enabling the user to cut very small internal diameter stainless steel tubing (such as 1/ 16" O.D. x 0.005" I.D.) that would likely collapse or otherwise become restricted when cut by an y other tool. Cuts on very small tubing is seldom attempted du e to the difficulty encountered using ordinary methods. By using this tool, delicate tubing cuts become as easy and routine as larger tubing cuts. Tubing cuts in tight or hard-to-reach locations can be performed without difficulty with the use of this tool. Since the cutting head is practically flat and requires relatively little clearance , it can be inserted into otherwise difficult spots to perform high precision cuts. As an example, if gas tubing routed through a hard-to-reach area inside the gas chromatograph required cutting for the insertion of an adapter or oth er special fitting , the cutter head could be inserted to the location and the cut acheived without having to dissassemble and relocate or remove the adjacent hardware blocking acce ss to the robing. Once cut, the tubing ends could be reached with another tool, such a s a needle-nosed plier, and pulled to gain accessibility for the installation of the fitting .
_ ..
Whe n making c uts, the tubing sho uld be located between the two "jaws" of the c utter, making sure tha t the cutter grabs the tubing in the "V" notches located on the blades. The cutter should be held complete ly perpendicular to the tubin g at the time the c ut is made, to avoid obtaining a bad angle on the tubing end. Care should be exercised to avoid pinching the fing ers or hand when operating this tool, as with an y other hand-he ld cutting too l. O,\ E:P2IXlCS\TUBEC1.m.EPD
.
. ~~ -
-
TO USE: Locate the tubing to be cut between the beveled cutting surfaces while maintaining the cutter at an angle completely perpendicular to the tubing. Holding the cutte r steadily, cut the tubing in one quick. hard motion. Do not he sitate d uring the cut to prevent any possible twisting of the blades or the tubing. This cutter cuts 1/8" and 1/16" copper and stainless steel with ease . After extended use, especially when used to cut stainl ess steel tubing, the cutter blade will become dull. Discard and replace the tubing cutting too l when this occurs to pre vent damage to any future rube cuts.
= ==1 = = = =• Keep cutter in a perpendicular position when
cutting and cut in one quick, sharp motion.
RE V. 07_! \.'16
209 (of 550 ) 2006(-2016)
210
(
I
Chapter:
INSTALLATION
Topi c:
Setting and Adj ustment of Contro lled Heated / Cooling Zones on 86lOC GC
!
I '-----------~-------------------,
The 861DC gas chromatograph permits easy display and adjustment of all controlled -At-a-glancezone setpoints. To view a controlled zone, displa)' panel simply place the display selector switch in the also permits UP position, and depress the des ired feature viewing of pushbutton. Depending on the zone, the =1m
-
• •
•
should display 150 degrees). Most zones will only display the local setpoint and actual value. Each zone also displays its status via a light-emitting diode (LE D) that glows whe n the zone is active ,
Local serpoim pushbuttoas To
S
~ ~.
.
'-~''''mg
LE~
~
R - COLUMN OVE N TURES
TEWJERATURE
PRESSURE
------1100011011 II 0 0 0 II 0 II ~ 0 0 0 • 0 ~ II 0 0 0 II 0 II
Actual va lue pushbuttoos - - - - 0 E Ccerroljed -zoe e descriptions - - - l C
PET I C C
0 -
C C C OO H
DOL l
U U
DOOREESCDlTaBRADE
Toggle switch
PRESSURE'. psi
selects display of setpolDt and actual "IIIu.::s in UP
A
s
D F B B Of Of S P l l H N I With the display selector Dn:tAYSQ.tClH) I _ ' S tE'1F'QHTIICIUl"t. .,../ '-- posttJOfl_ or tugglc switch in the UP position, the FD g g O O 1 8 K KV V value corresponding to any panel OL E E ~ pushbutton will be displayed. Wh en 2 0 H H CQl,MI4(MJ1' I te mperature C 1 2 the button is released, the display display in K DOWN will clear the value and return to position Front view of column oven temperature display 000 units.
@
D:\96EPDOCS\86 I OCSET. EPD
co:amoven
REV. 04-2H 6
210 (of 550 ) 2006(-2016)
211
(---------------------~':
I
I
Chapter:
INSTALLATION
:
Pressure-Programmed Carrier Gas Operation Using EPC System (- - - - - - - - - - - - -- - - - - - - - - - - - - - - - - - - -- - - -- - ,j
Topic:
Carrier Gas Pressure-Programming via Electronic Pressure Control
SR I 8610C GC
COWMHOVEN
EPC MODULE
IHJECTlOH PORT
LOCAL PRESSURE CARRIER SETPOINT GAS
;-!i/-+-~DETEGTOR
PRESSURE PROGRAM
FROM OATAS'lSTEM
A·b-O
TO PC-BOSEO DATA S'lSTEM
100 ps i
50 psi
I~
I
I
I
I
I
II
r
I I
FLOW CHART ILLUSTRATING CARRIER GAS PRESSURE PROGRAMMING ON THE 8610C' GC
All SRI 8610C gas chroma tographs are equipped with Electronic (or Pneumatic) Pressure
Control (EPC) of all system gases. Each gas, from the carrier gas, to the specific detector gases, such as FID hydrogen and FID compressed air, in the case of an FlO detector, are controlled by a dedicated solid-state EPC module that electronically monitors and instantaneously adjusts the pressure being supplied to the particular feature. This electronic control facilitates extreme precision of gas flo ws to the various functions. Each EPC module features a local, user-adjustable setpoint accessed by a trimpot (variable potentiometer) located just above the particular function on the "at-a-glance" panel display. The carrier gas is among these adj ustable setpcints. The term "local" refers to the fact that the "local" setpoint is set manually at the trimpot on the GC chassis. As in the case of the column oven temperature setpoint, the carrier gas pressure setpoint may be set "locally" (manually on the GC chassis), or from the computer via a pressure program. Created in the same format as a PeakSimple temperature program, the program signal is sent to the data system interface and converted to a control voltage that can increase, maintain, or dec rease the carrier gas pressure automatically at the user' s comman d. The PeakSimple serial data system interface offers two rampable voltage outputs - one to program the column oven, an d the other to program carrier gas pre ssure. Outputting a 0 to 5VDC va riah le signal , the EPe modul e will permit an output pressure of from 0 to lOOpsi (the carrier pressure shown is actually the column head pressure). Please note that any local serpoint value will be summed to this signal , resulting in the "total" setpoint value on the panel display . The carrier gas pressure regula tor at the gas cylinder should be set IOpsi higher than the highest programmed carrier ga s head pressure de sired for prope r control. Ramping permits the head pressure to be varied, to speed or slow the elution of pea ks from the analytical column as needed by the application or user. D~ \96EPDOCS\EPCFLOW l .EPD
REV. 05-17-96
211 (of 550 ) 2006(-2016)
212
(
l
Chapter:
INSTAliATION
Topic:
Analytical Column Installation
]
~
Location of
rearlr----_4__
polishing filter (at
of column oven)
0
rn •
Analytical column
•• •
~
1I- - -_
Oven heating
elem....
.... ....
Detector inJet
•
4!@@ @l oSl~«I8
Injection port
@
TOP VIEW OF 86 10C GC \VITH COLUMN INSTALLED
The column oven in the SRI 8610C GC measures approximately 7.8" x 8.0· x 3.0" (19.8 x 20.3 x 7.2cm). A column wound into a coiled form with a maximum diameter of 7" and a height of 3" may be installed in the interior space available. Standard 6" diameter or 3" diameter SRI-wound columns are installed with ease . Either capillary type (0 .25 to O.53mm I. D. ) or packed co lumns (118" to 1/4") may be used, depend ent on the application. Capillary columns may be made of either fused silica or stainless steel, and are coated on the inside with a fine film of stationary phase between 0.1 and 5.0 micron s thick. This phase , specific to the application, permits the sample components to be properly separated for analysis. The packing material in a packed column serves the same purpose. For wide-bore capillary applications, metal capillary columns are recommended , as they are virtually indestructible and can withs tand much physical abuse, unlike the fused silica variety, which can be broken with ease if handled improperly. SRI recommends the use of me tal capillary columns when
available for the application.
0 .25 to O.32mm I.d fused silica tub ing coated on inside surface with stationary phase film 0.1 to 1.0 microns thick
0.53 mm 1.0. fused silica or fused silica-lined stainless steel tubin g
coated. on the inside surface with a stationary phase film 0. 1 to 5.0 micron thick
1IS" to 1I4~ 0 .0 . seamless sled or glass tubing packed with granular support particles. These support part icles may nave a stationary phase coating. Glass tubing is specified for pesticide anlLlys is. as some pesticide components react with stainjess steel. A metal hit or glass plug retains the pack..iDg inside the tubing
won
D;-.EP:!DOCS\I~STCOU _ EPO
212 (of 550 ) 2006(-2016)
213
Chapter:
INSTALLATION
Topic:
Analytical Column Installation (continued)
The injection port of the SRI chromatograph is designed specifically for direct injection onto a 0.53mm 1.0. wide-hore capi1lary column. A sample, injected using a chromatography syringe equipped with a 26 gauge needle, is deposited. directly into the column. The injector IS supplied with a 1/8" 0.0. stainless steel 0.53mm capillary column adapter that guides the syringe needle into the capillary column entrance. The sample is then injected onto the column. The user's sample injection technique (sample loading, needle insertion and injection) should be quick, precise and reproducible.
1\ Conical / needle orifice
Typical chromatography syringe
[.!
I
I Capillary column adapter
(located inside iD,iection port)
0.53mm J.D. fused silica column
DIRECT INJECTION INTO A CAPll.tARY COLUMN
The wide-bore capillary column adapter is machined from 118" stainless steel and accepts the insertion of 0.8mm 0.0. tubing (the outer dimension of 0.53mm 1.0. capillary column tubing). The injection end of the adapter is conical and "funnels" the needle into the column tubing inserted into the adapter from the column end. A slot cut in the adapter prevents carrier gas flow restrictions caused by overtightened septa. By guiding the injection needle well into the analytical column tubing, the sample may be deposited as a liquid onto the stationary phase of the column without exposing the sample to contact with. hot metal or glass surfaces. The capillary column adapter is located within the assembly that forms the injection port when
a 0.53mm 1.0. column is in use. The injection port is constructed from a liS" stainless steel Swagelok'" hulltltead fitting that has heen modified to permit the connection of a gas source directly into the fitting through the hexagonal flange at the bulkhead. This modification permits the introduction of carrier gas into the injector. The end of the injector bulkhead fitting located in the oven compartment accepts a 118" Swagelo~ nut and graphite reducing ferrule (Allteeh RF200/0.8-G) used to secure the capillary column in the injector. At the other end of the bulkhead fitting, facing the user. a 118" septum nut is used to secure a formed silicone septum in place in front of the column, sealing the injection port. The septum nut should be finger-tightened. Two rubber O-rings are installed on the injector where the septum nut is attached. The septum nut should never be tightened beyond the point where the nut contacts the outer O-ring. Oven wall
Septum nut
Septum
~dJ
Rubber O-rings (2)----
Carrier gas supply
~
-:
I
~"''''''''",,,,,,,f
I
lIS~
Capillary column ....pter
10 O.8mm.
l iS"
graphite reducing
fenule
nut
./
/'
--<~
liS" Swagelok* bulkhead fitting
Swagel~
" O.53mm I.D. fused silica column
SRI CAPILLARY COLUMN/INJEcrION PORT DETAIL
The injection port is compact and has a low thermal mass. Since most of the injector body is located within the column oven, the injector and oven temperatures are always equal (the standard injector is not supplied with any provision for independent heating. Heated on-column injection is available as an option). Resultant sample component peaks are sharp and exhibit minimal or no tailing. This is due to the injection of the sample directly onto the column and at a temperature below the sample solvent boiling point. Decomposition of thermally-sensitive sample compounds does not occur and artifact formation is minimized because the sample is not subjected to vaporization and recondensation, as occurs in high temperature injectors. c :\EP2\DOCS\INSTC012.EPD
REV. 01-12-93 213 (of 550 ) 2006(-2016)
214
(
l
Chapter:
INSTALLATION
T opic:
Analytical Column Installation (contin ued)
-
-
-
- -- - -- --
-
) -
-
- - - --
-
-
!
,
Capillary column cubing Grnphite reducing ferrule
G
?':
hi rap: te
118" Swagelok retaining nut
Cutting 1001
- - (sapphire column cutter shown)
'ba~'
C1JF=§J~~~~
=
Proper cut
=
Unacceptable
Co lumn end should be inserted half-way into adapter
Injector assembly
" Column end and adapter inserted into proper position within injector
1 /8~
Anti
re taining nut
flow restriction slot
=
/
118" stainless s teel packed column
Syringe deposits sample on-column
Colwnn end is inserted into injec tor and secured into po sition with retaining nut
C ;\En lDOCS \ INSTC OLJ .EPD
Installation of a packed colu mn in the chromatograph is simpler . With 118" stainless steel col umns, standard metal ferrules are used to secure the column at the retaining nur. The ferrule s a re placed onto the column end as shown, and then the column end is inserted into the injector. The capilla ry column adapter is not used with packed column s and should be stored in the adapter h ol der under the red protective oven cover for future use. Columns manufacrured by SRI include a slot in the injector end for carrier gas flow ass urance . REV. O] · ll .9 j
214 (of 550 ) 2006(-2016)
215
r;::;-~--- _. _--- ---- - -- - - ~- _ . _. _ - - - - - - -_.
I
Cha pter :
INSTALLATIO N
I
Topic:
Analytical Column Installation (continued) '
__._ _.__._.- ..._--
Me tal ca pillary c olumn
....-n,..._==~ ~_9R
.o(_ •.•
G rap hite reducing ferrul e
tubing
t:::iJ
r.....v -
liS " Swage10k retaining nul
c utting tool ___
C1JF§l~
\
' shavings typ icall y lodge Graph ite in tip of colwnn ....hen pas sing th rough graphite red ucing ferrule
Sco re the meta!
tubing with !he me
When installing a metal capillary column in the chromatograph, a graphite redu cing ferrule must be used to secure the capillary tubing in the 1/ 8" retaining nut (..\ Utech RF200/0 . 8~G for 0 .53mm I.D tubing, RF200/0.5-G for 0 .32mm LD. tubing and RF200/0.4-G for O.25mm LD. tubing). The column is inserted first through the nut, and then through tile ferrule. Note the orientation of these pans in the accompanying illustrations . The insertion ofthe tubin g through the f errule will cause graphite
shavings to accwnulate in the column entrance. Graphite is adsorbent and may cause peak tailing or a flow restriction if left in the column. For this reason, an inch or so of column tubing s hould be CUt from the column tip after it has been passed throu~h
a graphite ferrule. A fine-cut triangular metal fi le 1S provided with all SRI metal capillary columns. Normal column cutting tools designed for use on fused silica will not work with metal columns. Metal After scoring lhc metal column, wipe away any shavings columns are coated inside with fused silica and and app ly fo rce to the tubing at the sco re column phase . The y offer the same perfo rmance. and are practically immune to breakage or rough handling damage . Score and cut the co lumn tubing as l2: indicated and the tubing snaps apart cleanly. Check the cut end prior to use; it should be Oat-ended , not j agged or with metal covering the col umn ori fice . The capillary column may now be inserted half-way into the capillary column adapter for installation into the injector . Once that the adapter and column end have been located in the injector as shown. the ferru le and nut are connected and tightened to secure the col umn in the injector. x ore that the adapter does The front piece of tub ing shou ld break aw-4Yc leanly Dot contact the septum. If the septum nut were overtightened, the septa would be forced deeper into the inje ction pert, sealing against the adapter. Th e zslot cut in the adapter permi ts carrier gas to reach the column even if the septum is overtightened, so that Insert a syringe needle into the column lip. This 'kill debur column fl ow is unaffected. Of corse, sep ta sho uld the lip and pe rm it the needle to slide in duri ng injection never be overtightened. A finger-tight sept um nut is adequate for proper sealing or the silicone against the injection port. Wbe n the column is properly installed, a head pressure reading of between 4 and CoIwnn end properly locat ed in capillary column adapter 12 psi should be observed. If there is little or no head pressure, the system should btl inspected for leaks . If the head pressure rises to a level equal to the carrier gas supply pressure, suspect a flow Inj ecto r assem bly restriction or plug either in the column (typically caused by an accumulation of cored septum slices in ~ the e ntrance to the column) or at th o: c utle t o f the CJJI=- = column (at the detector inlet). When plugged column inlets are encountered. cut off another inch or two of Column end and adapt er inse rted into proper the column and reinstall the column in the inj ector. position wi th in injcC(or The capillary column adapter is not used with packed columns and should be stored in the adapter holder under the red protective oven cover for future use .
t
"
D: ·~S0'2DOCJ :-;STt.:Ol. ~ ..E PD
-
REv . 06-08-9S
215 (of 550 ) 2006(-2016)
216
Chap ter:
MODEL 110 GC CHASSIS
Top ic:
FRONT PANEL OR IENTATION
Heated transfer line runs about 200 degrees C and has a thick layer of insulatio n co vered by red co lored ven tubing . A length of .53m m 1.0. sitco-ste et tubing carri es the carri er gas fro m the host GC to the detector mo unt ed in the 110 chassis.
On/off swncn for optional buitt-in air compressor
H0 14 doc
Detector parameter on/off switches for FlO ignitor, NPD bead voltage. PIO lam p curren t, etc.
-At a gl ance · LED display shows status 01 all de tector pa rameters
Dig ita l panel meter reads out detector empe ratures , voltages. etc . when a specific button on the front pan el is depressed .
The SRI Model 110 chass is is used primari ly as a mount ing platform for stand-a lone GC detectors. Th e heated transfe r line makes it easy to con nect the d et ect or to the host G C since only a small ope ning into the host GC's co lumn oven is requ ired . Use r's sho uld note that because th e heated transfer li ne ope rat es at 200 C. some high boiling po int a na lyt e ~ may cond ense before rea Ching the detector. Where high temperature analyses are envisioned , it m akes sense to m ount the detect or on the GC itself instead of on the sta nd- alone chassis.
216 (of 550 ) 2006(-2016)
217
Chap ter:
MODEL 110 GC CHA SSIS
Topic:
RIG HT SIDE PANEL ORIEN TATION
Screwd river m ounted in ha nd y "holster" for adj usti ng detector
parameters or te m perature setpolnts
Gas flow rate table is used to record the flow rates and pre ssures used for detect or support gases. Fact ory te ch nicians record ypical flow rates and press ures used to test detectors before shipment during fina l test at the manufactu ring faci lity.
Zero and atten uatar co ntro ls for detector outp ut signals. The ze ro cont rol is a ten tum potentiom eter which allows the output from the d etector to b e offs et to 0.00 . The artenuator divides the sign al by selectable powers of 2 ( 1.2,4 ,8 etc .) so that the peak rema ins on sca le en using a strip chart recoroer wttn a fix ed span ( i.e. t nmnuvor ts full scaie ). When used w ith a computer data syste m or integreator t he attenuator control is norma lly set and lett on max imum sensitivity (" =1 ).
Detector signal cable output wire. This cable containing two
wires is necked up
to your strip chart recorder or data system.
H015.doc
217 (of 550 ) 2006(-2016)
218
Chapter:
MODEL 11 0 GC CHASSIS
Topic:
LEFT SIDE PANEL ORIENTATION
Chassis cooling air exit
slots. Air expelled from th e chassis by the cooling fa n exits th rough these slots.
Do not obstruct the slot openings .
Main powe r switch, circu it breakers, and chassis cooling f an .
This fan cycles on and off to maintai n the selected int erior chassis t em peratu re .
Heated transfer li ne for
connecting column outlet from host G C to sta nd-a lone d etector on M ode l 110 chassis. Transfer li ne operates at 200 d eg rees C. T ake c are to route transfer line awa y from h eat
sensitive surfaces.
Po we r cord . On 220 von m od el s It may be necessa ry t o replace the plug o n the end of
this cord to match the plug type fo r th e cou ntry or region.
G as inlet bulkheads f or connection of d etector support ga ses ( t ypically hydrogen an d air ). Us e 1/ath inch 0 .0. co pper tUbing to connect gas cyl inder to stainless ste e l bulkh ead, not teflon or other plastic t Ubin g t ypes. Use brass ferru les for
good sealing.
IHOI6.dOC
218 (of 550 ) 2006(-2016)
219
Chapter:
MOD EL 110 GC CHASSIS
Topic:
TOP PANEL ORI ENTATION
Heated transfer line connects from host GC t o detector m ounted on Model 110 chass is..53mm 1.0 . sileo-steel tubing runs insid e heated tran sfer lin e so sample on ly cont acts inert fused sili ca surfaces for m ost at the le ngth.
Detector heated bloc k and cov er terminat e tran sfe r li ne in a hot
loca tion to avoid sample condensation H017.doc
Red lid hi ng es up t o allo w access to detectors
Detector shown above is the SRI DE LCO det ector , b ut any of 13
detector types or com binati ons of de tect ors m ay be mount ed .
Spare parts sto rag e container is con veni ent for
keeping extra nuts, fe rru les. etc.
Detector parameter and t empe ratu re adjustmen ts are done by using the pr ov id ed screwdriver to adjust he setpclnts th rough the holes in t he forward edge of the chassis
Detector gain controls are located here in the exact same la yout as the 3 10 a nd 8610C G Cs.
219 (of 550 ) 2006(-2016)
220
Chapter:
MODEL 11 0 GC CHASS IS
Topic:
HEATED TRANSFER LINE
This photo shows the dete ctor end of the heate d transfer line as it attaches to the heater block and
enclosure. When removing and reatt aching the heated transfer line be careful to eliminat e any
cold spots which could cause sample
condensation.
This photo shows the typical installation of the Model 110 to the right of the GC with the heated tran sfer line connecting the two units. Be careful to route the transfer line
so it does not rest on heat sensitive surfaces. In some ca ses , the lid or the GC may ne ed to have a small notch cut-o ut of the right side pa nel to allow the transfer line to exit
cleanly from the GC when the red lid is lowered. HOl8 .doc
220 (of 550 ) 2006(-2016)
221
Chapter:
MOD EL 110 GC CHASSIS
Topic:
CONNECTING TRA NSFER LINE TO GC
If you are connecting the Model 110 detector to a SRI Model 8610C or 310 GC the right hand side of the Ge 's column oven has 4 identical detector mounting locations.
locations where no detector is insta lled are
supplied with blank cover plates.
FJD detector installed
Replace one of the blank
cover plates with the Transfer Line Mounting Plate ( SRI part# 86709836 ) by removing tI1e two screws at the base of the plate. The nuts on the unders ide of the chassis must be accessed by removing the bottom plate of the GC . The heated
transfer line is then lightly secured to the plat e with he hose clamp so that the heated portion of the line penetrates into the column oven so that cold spots are eliminated H019.doc
221 (of 550 ) 2006(-2016)
222
Chapter:
MODEL 110 GC CHASSIS
Topic:
COLUMNrrRANSFER LINE CONNECTION
The .53mm 1.0 . sileo-s teel tubing which ru ns down the center of the transfer line is conne cted to the end of the analytical column inside the Ge's co lumn o ven . A special 1/8th inch sta inless steel bulkhead union and insert are provided to ensure a low dead volume butt type connection . Th e un ion may be mounted on a fla nge or bracket, or just left hanging in the oven.
e separate parts of the union and column to transfer line conn ection hardware consist of: GC co lumn Nut with graphite ferrule ( 2 )
Stainless Steel bulkhead Interna l alignment guide which ho lds th e transf er line and column butt to butt inside the bulkhead un ion
h020.doc
222 (of 550 ) 2006(-2016)
223
Chapter:
MODEL 310 GC CHASSIS
Topic: Liq uid or gas inj ecti on port fo r 26 gauge syringe needle
Therm o-co uple out of rang e alarm LED ind icat es
Meter selector switch allows con sta nt display of column oven temperature ( down position ) or display of any zon e setpo int or actual whe n a specific button on the fron t panel is pushed ( up position ).
Polishi ng filte r bake out switch hea ts built-in
hen any heated zone is reading lessthan 5 or more
carrier gas
than 400 degrees Centigrade. Wh en alarm is activated all AC power to heat ers is shut off by de-
fil ter for 5 m inut es to elim i nate c ontaminants.
Digital Pan el Meter d isplays co lumn oven temperature, detector temperatures , gas press ures, and detector parameters such as F lO ignitor volts, PIC lamp curre nt, FP C PMT vonage, etc.
Optiona l built-in internal air compressor onloft switch. Air compressor is usee to supply air fo r FlO, FPDand DELCO detectors
D etecto r c ontrol switches enable on/off of various detector parameters seen as p rD la mp current, FP C PMT volts or F lO ignitor.
energ izing ma in powe r relay.
HOO8.doc
223 (of 550 ) 2006(-2016)
224
Chapter:
MODEL 310 GC CHASSIS
Top ic:
RIGHT SIDE PANEL ORIENTATION
Screwdriver in convenient "holster" for adjustment of temperature and pressure setpolnts
Gas fl ow rate l able is used to reco rd the flow rates and pressures used for detector support gases . Factory echn icians record ty pica l flo w rates and pressures used to test detectors before shipment
Rel ay functio n ta ble shows wh ich function each of the 8 ( A-H) data system re lays is assigned. Depending on GC configurati on, some relays ma y hav e no functi on.
Mounting location fo r optional detector "zero" and atte nuatcr knobs when suc h controls are install ed. These contro ls are normally not required When the GC is suppl ied with the buitt-m PeakS imple Data system. but are inst all ed when no data system is provided.
Signa l cable access holes are prov ided for opt ional situatio ns req uiring wi ring 10 exit G C.
Optional location for mounting of quick discon nect jack for remo te start foot switch.
HOO9.doc
224 (of 550 ) 2006(-2016)
225
Chapter:
MO DEL 310 GC CHASS IS
Topic:
LEFT SIDE PANEL ORIENTATION opuonaucceuon for vacuum pump intertace socket. If this
Main Power SWitdl, circuit
breakers and C powe r cord.
option is installed a IEC422 type receptacle "]I be m ou nted in th is
space. Power to the receptacl e wi ll be controll ed by the data system
DB-9 serial port
connector to host c ompute r. The includ ed serial port
cable attaches here to ena bl e the PC to co ntrol and collect data from th e GC.
Opnc nal air compressor outlet. Typically co nnected to air inlet bulk.hea d filling with copper tu bing
Chass is cooling fan.
This fan cycles on and off to main ta in the preselected chassis interior temperature setpcmt. The chassis setpoint can be adj usted via front panel controls
Ch assis venitilation slots. Do not obstruct hese slots, as cooling air exits the GC through these openings .
Sta inless steel l I S" swagelok t yp e bulktlead fitting s fo r gas inlet connections . Depending on GC configuration, th ere may be inlets for H elium. Hyd rog en, A ir or EGD m ake-up gas . Gases are t ypica lly connected here using 1fBt h Inch 0 .0. copper tUbing from the gas cylinder.
HOI O.doc
225 (of 550 ) 2006(-2016)
226
Chapter:
MODEL 310 GC CHASSIS
Topic :
TOP PANEL ORIENTATION
400 degree C insulated tem perature progra mmable col umn ove n for packed or capillary col umns.
High speed cool-
Syring e
Spare parts
P IO detector.
down fans engage
injection
storage
Up to fo ur
at end of
pM
temperature
for liquid or
con ta iner is co nvenie nt for hol ding ext ra nuts, f erru les and sm all acce ssory
detectors may be m ounted alongside the right hand edge of th e column oven.
programmed run to bring column oven temperature back down to starting
gas inj ection
parts.
temperature.
Local setpoint
Heater block for
Com bina tion FlO.
adj ustment screws for temperautes. pressures and detector parameters.
each det ecto r is
CELCD detect or.
indiv idually tn erm ostatted and adjustable from front panel setpotnt co ntrols.
Other de tect ors may be mo unted in this tccatton depend ing of GC configuration.
F lO ignnor, NPD be ad
and
Detector amplifier ga in
OELCO
control
heater co nne cti on.
switch es and SNe signa! con nectors
HOJ2.doc
226 (of 550 ) 2006(-2016)
227
Chapter:
MODEL 310 GC CHASS IS
Topic:
COLUMN OVEN INTE RIOR
60 meter .53 mm . 1.0. capill ary col um n shown m ounted in col umn
oven.
Duct for coo ling air from oven coo ling fa ns .
Circulation fan and heate r coils on botto m of colum n oven. All heater ci rcuits and circulation fa n are disabled by interlock; switch wh ich is deactivated when red lid is raised .
The column ove n on the SRI Model 310 GC is designed fo r column diameters up to 4( 10 em.). Whi le this column diameter is smaller tha n a verage, m ost pacxec and capillary columns can be ordered with the reco mmend ed 3.5" coil d iameter. Metal cap illa ry columns are suggested because of their ruggedness and long life .
HOI3 .doc
227 (of 550 ) 2006(-2016)
228
(- -
-
-
Chapter: (, Topic:
- - --
-
-
-
-
-
-
- - --
-
-
- - --
-
-
-
INSTALLATION FRONT PANEL ORIENTATION - 86IOC GC CHASSIS
Space under red
On-column direct protective cover reserved injection port for injector accessories
Colwnn oven
OJtional
second
on-column direct injection port
Detectors mounted under red pr otective cover on right side of column oven
• 0ETEClCl'l · OClWMH 0'iEN 00N11'l0lS
Carrier gas filter bake-cia switc h
~£1'EI'lS
TEMPERAT\J RES
- * O * * O $ O O @O O . O O • • • • O OOO • • • OO*O* -*O • • O&OO&OO@OO@ • • • O OOO& • • OO&O+
Bright red LED digital display
- 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
- . 0 • • 0 . 00 . 0 0.00 • • • • 0 00 0 • • • 0 0 . 0 .
, ,
-v-
...-......
""-~
000 0
Detector control switches
LED valve status indicators
t -Di>play selector switch
"Al-a-glance" LED status
indicator panel
"AT-A·GLANCE" STATUS INDICATOR PANEL - All controlled zones on the gas chromatograph are displayable on this panel. Multicolored light-emitting diodes (LEOs) indicated when zones are active (on), or are being thermo statically-con trolled (heated zones - pulsin g). DISPLAY SELECTOR SWITCH - This switch toggles between constant display of the column oven temperature, and display of zone setpoints and actual valueswhen a specific button is pushed. Each "at-a-glance" status panel zone LED is accompanied by push-buttons that permit display of local and total setpoint values, and actual zone values on the digital LED panel meter. DIGITAL PANEL METER - A high-visibility, bright red j-digir panel meter displayed either the current column oven temperature, or the temperatures, voltages, and pressures of all controlled zones. Zone value display is momentary, and is shown as long as a button is depressed. VALVE STATUS INDICATORS - On gas chromatographs equipped with optional sampling valves, an LED glows to indicate the valve' s current position. Up to two valves may be displayed. INJECTOR PORT - A direct on-column inject port is provided, and supports the use of both packed and capillary analytical columns. A capillary column adapter is provided for installation of wide-bore GaP.illary columns. ~tiona1 heated injection ports and heated split-splitless injection ports are available. A second injection port may be installed on the same column oven. DETECTOR CONTROL SWITCHES - All detector control switches are located on the front control panel. including FID ignitor and PID current, and FPD voltage.
ADDmONAL SWITCHES - A carrier gas filter bake-out switch is provided to bake impurities from the gas polishing filter. If the GC is equipped with an optional built-in air compressor for FID or DELeD use, a swi tch is also provided on the lower left comer of the front control panel.
228 (of 550 ) 2006(-2016)
229
( Chapter:
INSTALLATION
, Topic:
LEFT SIDE PANEL ORIENTATION - 8610C GC OlASSIS
Red proeecrive
ECD
ovea cover
make-up gas
Carrier gas #2 inlet
o
•
TbermostaricalIycontrolled chassis cco hn g fan
0··· Carner gas
•
o (L~_I''I--advisory notice . . (see te xt) o• ....;---, ____ Sparge gas
Three conductor
groomded AC power-
~
coni
@
WI" Carrier gas #1 inlet
Buill-in air compressor Olalet
Compressed
Hydrogen
air inlet
inlet
FID I DELCD air inlet
FIn I DELCO hydrogen inlet
MAIN POWER SWITCH: A rocker switch provides control of the AC power for the e ntire gas chromatograph. When the GC power switch is turned off, the built-in serial data acquisition interface is also inactive, and communications with the computer cease.
COMPUTER SERIAL PORT INTERFACE: This port, a standard RS-232 serial interface , connects the gas chromatograph to any ffi M PC-eompatible desktop or notebook computer serial port. The computer collects the da ta and contro ls the gas chromatograph. No darn. storage occurs in the chromatograph. A six-foot DB-9 type serial cable is provided for connection to the PC. CARRIER GAS INLETS (I AND 2): The 8610C GC may be equipped with up to two independent carrier gas systems for independent injectors. columns. and detectors. An important advisory message, regarding the use of helium carrier gas only, is printed on the chassis and refers to all 8610C models. A dangerous condition could occur if hydrogen carrier gas were being used and a leak (such a break in the column) occured downstream of the pressure control circuitry. The leak would not be detected by the sys tem , and gas would be continuo usly vented at the set pressure, permitting explosive gas to accumulate in the vecinity of the chromatograph. GAS INLETS: Stainless steel gas bulkhead fittings are provided for connection of all system gases. Separate inlets are provtided for sparge, FID , DELCD. and ECD gases. If the GC is equipped with a built-in air compressor, a compressed air outlet is also provided.
CHASSIS COOLlNG FAN: This fan is thermostatically-controlled and draws ambient air into the chassis electronics compartment to maintain the internal electronic and pneumatic components at a stable, controlled temperature. The temperature setpcint is pre-set at the factory. PO\VER CORD: A permanently-attached six foot, three-conductor cord is provided for connection to a gro unded I IOVAC powe r outle t. 220VAC models are supplied with the appropriate plug for standard grounded 220V outlets. Neve r defeat the safety feature inherent in the grounded cord by
connecting it to a two-pro ng, ungrounded ourlct. o.\% £PDCK:S ,U-;SLFI'3. EPD
REV . 1)4.23·%
229 (of 550 ) 2006(-2016)
230
( Chapter.
I
l
Topi c:
INSTALLATION RIGHT SIDE PANEL ORJENTATION - 8610C GC CHASSIS
Red protective oven cover
Relay function table for bum-in da.t& sysem-coctrolled relays
Table of all GC system gas flow rate settings
Relay default seuicg is
underlined
Sparge gas setting for purge-and-trap
_-11-.. C=:=-;::=:;-:-;==;::=--.
opersnon
•
A
. . n _I
B C D
...... ~ (J4IOaol_
E F G
Auxiliary fcsture setting for custom GC systems
•
•
H
Flow equrvejecce
~~T(CIn'IQII)
_ _ to
-..... ,..,.._
....( _ '0001 (-
-
)
'I,I,I,\lI;'I _ _ ( l ~
_ "".....--o_1ID:!')
•
Relay letter 8 relays A-H
••
•
Auxiliary cable outlets for custom con figurations
•
Valve positions
may be ooofinnOO ~
FuDction descnption
front panel LED display
GAS FLOW RATES TABLE: A table of all of the 8610C gas chromatograph's detector and special feature gas flow rates is provided on the right chassis panel of the GC . This table bears the recommended gas flow rate settings for every fea ture that the particular gas chromatograph is equipped with . All detectors requiring supportive gases, such as hydrogen and compressed air (in addition to carrier gas) for Fill, FPD. NPD, and DELCO operation will have their suggested flows printed here for easy reference. Any special purpose gases requiring spec ific flow settings, such as the ECD make-up gas flow, will be printed here also. A pressure figure is given adjacent to each gas, and this value should be used when initially setting up the chromatograph for operation. These settings will ensure proper operation. Once the detectors and other accessories are operating normally. the gas flow rates may be adjusted for optimization. The values printed on this tab le have been tested with the particular chromatograph in the SRI quality con trol laboratory . Flow equivalences for each pressure setting are also provided for your convenience. The indicated pressure setting should provide you with the flow rare shown to its right on the tab le. For precise flow measure ments . a bubble or digital flowmeter should be used. RELAY FUNCTIONS TABLE: Adjacent to the gas flow rate table, yo u will find a rela y functions table that lists each of the eight data system-co ntrolled relays (labe led A through H) available within the gas chromatograph. These rela ys may be operated by means of either a timed event table within a ny of the PeakSimple software programs, or directly by keyboard control. When using event table control , each relay called in the event table will activate or dea ctivate at the exact same time during each run . This makes these event table-controlled relays perfect for operation of solenoids, autosampler injector control, and rotation of automated gas sampling and stream selection valve s. A de scription of the function of each relay is printed on the table. The default setting for each relay is identified by underlining of the desc riptive text Special purpose relays. such as the trap te mperature toggle implemented via relay B, permit you to increase your trap temperatu res from the ir normal desorption temperature, to a bake-out temperature fifty degrees above the desorb setpoint, when pe rforming purge-and-trap analyse s. D:'.96EJ'l)()("SIL"'SRD. Em
REV.
~23-96
230 (of 550 ) 2006(-2016)
231
Chapter:
INSTALLATION
Topic:
Top Control Panel Orientation - 8610C GC Chassis
Optional gas sampling valve or purge-and-trap valve oven
Location of carrier gas polishing filter
Grey elec tric bigh-ourpur
Fast-cool booster fan
VIEW OF TOP CONTROL
column oven cooling fan
PANEL - 8610C
Teo detector am plifie r gain switch and bridge fiJameor
FID deeecec
cceeecnoes
t$J
heated blOCk
•
Fast-cool co lum n oven heat exhaus t
o
•
veer
"""".T--~-=---
•
•
valve cover (if so equipped) is secured in place by two thumbscre ws
• •
•
I, 24 3,
o
On-column direct injection port
I
:=:;;f'Rl~;:;;:•, ~I ":~:~~in
•
I;;t:!j
electrode
coanecnons
FID """""
I
PID dcscctor
-it- amplifier and gain switch
--ff-~l= I,t~~~~~
amplifier and FID gamdetector switch
- -ff--
FPO detector amplifier and gain swrte b
•
FID ignitor I :'\r 'O bead
adjustment knob 1: DELCO beater voltage
DELCO detector
Spring terminal block descnpeons 2: NPO bead curren t 3: FID ignitor current
PlO lamp currenI adjus tment knob
"" 4: FPD ignitor current
The 86 lOC top control panel is divided into four main areas: COLUMN OVEN - The insulated col umn ove n and associated cooling hardware is mounted in the middl e of the top control panel. A direct, on-eolumn injection port is located on the front left face of the column oven. The oven cover is hinged at the rear, and is equipped with an exhaust vent to facilitate evacuation of heat during operation of the high-ou tput, fast cooling fans. DETECTOR AMPLIFIER CONTROLS - All amplifier controls, including gain switches, current controls, and connecto rs, are located on the right side of the top control panel.
LOCAL SETPOn-IT ADJUSTMENTS - All user-selectable setpoint potentio meters are located on the front edge of the top control pane l, immediately above the front pane l "at-a-glance" display. A small blade screwdriver is needed to adjust these trimpots. VALVE OVEN I PURGE-AND-TRAP ACCESSORY - Accessories, such as gas sampling va lves, or the built-in purge -and-tra p system, may be mounted to the left of the column oven. in a heated . insulated valve oven, which pe rmits direct co nnection of enclosed hardware with the column oven. D:\96F.PDOCS\M 10Cll' L EPD
REV. 04-2g..9
231 (of 550 ) 2006(-2016)
232
(
I
Chapter:
lNSTALLATION
Topic:
Column Oven Interior - 86IOC GC Chassis
I
I
I
.-
,~--------------------------
Stainless sled grill separates beating element and ;lIT circulatioa fan from ana lytical column while permitting unrestricted ciKubtioo of heated air in oolwnn oven
Grey column oven cooling fan with fast-cool booster fan
Forced cool air inlct inm column oven located at
right rear of cvea
Iligh-oulpu< elect rical
rn •
bc:ating clement
0
Anal ytical
column
CoIUID.II o ve n air c irccleuoe fan
§ED
Thermostatically cont rolled detector heater block ensures stable detector inlet I assembly temperature
@
t ------
•
Ceramic in:>ul&1of"5 secure heating element in place
Direct oe-column injection port accepts Dxh packed columns and capillary columns (.a wide-bore capillary column adapter is pro vided)
Insulated ow n wall seals with oven lid and permits bigh-tt:mpt.7lltUre operation with minimal heal loss I radiation
TOP VIEW OF 8610C COLUM N OVEN (WITII COLUMN OVEN LID
REMOVED FOR ClARITY)
The product of ten years of gas chromatograph design and manufacturing, the 8610C column oven is an insulated design that permits operation from ambient temperature to 4OO·C, with rapid ra mping to maximum te mperature and rapid cooling to initial oven temperature when operating in temperature-programmed mode . T he high-o utput heating ele ment permits heating at up to 4O· C per minu te, and the assisted cooling fan configura tion permits return to 50 ' C from 25 0 'C in five minutes or less. The oven lid is equipped with an exhaust vent that speeds the evacuation o f hea t from the o ven during cooling. The ov en may also be operated isothermally with e xcellent stability.
The open air circulati on design eliminates gradients throughout the ov en which could affect performa nce. Prepurched openings in both the left and right oven walls permit easy future implementation of accessories and de tector additions. Up to four detectors may be moun ted on the right oven wall for maximum analytical versatility . The outlet from non-destruc tive detectors. such as the PID, are routed within the column oven for convenient series dete ctor operation . Th e column oven may be equipped wi th an op tional second direc t on-column inj ection port for use with a second anal ytical column , and al so may be eq uipped with a heated injection port, with or without
split-splitless capability. D:\96EPDOCS\86 I0CT0P. EPD
232 (of 550 ) 2006(-2016)
233
r- -- - - - - - - - - - - -- - - - - --
f
Chapter:
INSTALLA nON
I
Topic:
Dual Oven 8610C Gas Chromatograph Chassis
,--------------------~J
Dual, independent cooling fans
..•.;:;:::}:;:::::::...
•
Oven ai r circulating fan
Heated detector
L -- ----fl'f-1f • mOUDtmg block
Stainless stee l
wire mesh
Local setpoint
trimpces
lbick insulation between column ovens
Dual independent co-column injection ports
Co lumn oven temperature sens ing probe (thermocouple)
DIAGRA.\i. OF DUAL COLUM1\' OVEN·EQUIPPED 86tOC GC CHASSIS
For cenain special applications, the SRI 8610C gas chromatograph chassis may be fitted with dual, independently-programmable column ovens. Dual column ovens permit a single 8610C gas chromatograph to perform two separate, unre lated analyses simultaneously with independent start times and temperature programs. The immediately apparent advantage to having a GC equipped with two column ovens is the ability, for instance, to perform a direc t on-column injection of a BTEX sample onto a capillary column and flame ionization d etector (FID) using a temperature program,
such as 50'C to 200'C at a temperature ramp of woe per minute, while also performing a gas analysis by direct on-column injection at either an isothermal tempe rature or at a low-level temperature ramp. onto a packed column connected EO a thermal conductivity detector creo) in one col umn oven. By placing one temperature program on channel 1 for the. AD, and a different temperature program on channel 2 for the TeO, two separate column operating conditions may be simultaneously controlled. A more sophisticated method to employ dual column ovens is multidimensional gas
chromatography, Briefly, multidimensional GCs perrmt one sample to be analyzed oormaIly on one column in a main column oven (connected to a dedicated detector), with the ability to "slice" a timed segment of the sample elution and place it onto the second column in the second column oven. to analyze it "under a magnifying glass", of sorts. The first column effluent is direc ted momentarily onto the second col umn and oven, where this "injection" is separated by a much longer, lower temperature column and second detector, providing a well-sepa rated close-up of the time segment slice. D:'.96EPOOCS\D UALQVS1.£P[)
R.EV . OS- I....96
233 (of 550 ) 2006(-2016)
234
,,
,,
INSTALLATION
Chapter.
Detector Mounting Platforms on Column Oven Wall Topic: \ ~---------------------~) FID detector heating block
Insulated colwnn oven lid
DELCO detector beating block and dececror gas supply lines
Column oven lid exhaust vent
GAS FLOW RATES
.................
Ov en lid seals against oven wall
insulation
__...
RElAY FUNCTlottS
•
...._ c...c.aOOVJ)
Detector amp lifier controls and
-..c;I,f(cnlOI)
E
."' . _ <1016(= '000)
F
_
G I-l
...."""--.0( 1 - : \ .. "",:tl_( l ~
~(--,~
o __
•
connections, red p rotective oven cover llbov.n fur clarity of this ilJustnJ..iOQ
B C
.. 0
not
•
0
0 ·"-
0 ..-
.IElTC ....' . .'
•
•• •
Space reserved fee addtimal oeeecr in-ullatioo
All 8610C detector inlets are equipped with detector beating blocks (with ex~ of
ECD and TCD detectors)
RIGHT SID E VIEW OF COLlThtN O VEN WITH DETECTOR MO UNTING
HARDWARE VISIBLE (pID DETECTOR PRESENT)
All 8610C gas chromatographs are equipped \~..i th a thennostatically-controUed heating block
mounted at the base (or inlet) of each detector. This new feature permits the user to pre set the temperature of the detector inlet This is convenient for methods prescribing a specific detector operating temperature, and ensures the tempera ture stability of each detector. Each detector heating bloc k tempe rature may be accessed from the "at-a-glance" display pan el on the front of the GC for view ing on the bright red, digital LED panel mete r. The res pective setpoint potentio meter , located on the top control panel immediately forward of the colu mn oven, is easily adjusted using a small blade screwdriver. The TeD and ECD detectors. d ue to their enclosure in a temperature-controlled detector oven , do not require a he ating block. These two detec tors are mou nted directly to the column oven wall , and the detecto r inlets an d outlets are well-heated by the column oven. The heated detec tor mounting blocks, or platforms, permit easy access to, and mainte nance of the different detectors. The entire FID an d DELCO detector assemblies may be removed for servic e in secon ds. A new PID de tector cell and platform de sign mount horizontally onto a heating block sec ured to the column o ven, an d the sprin g-loa ded PID stage acce pts co mpact 0-1 o r Tracer-type PID lam ps (a 10.2 e V lamp is standard eq uipmen t on SRI PID detectors).
A special electric heating cartridge is used in place of electrical heat ropes used on earli er -r-,
models. The cartridges in use for de tector hea ting bloc ks should provide years of service before requiring maintenance. T he heating cartridge is installe d in a well, d rilled into the top of each cast al uminum heating block, and cartridge serv icing and repl acement is simple to perform . should it become necessary in the future.
o- ,'ItoEPOQc s'.861OC'RTI.EPD 234 (of 550 ) 2006(-2016)
235
ui~k
Sia t
SRI GC Installation Guide
I. Gas In stallation & Connection
,• ':::';"';":,-
1. To connect yourGC to a gas Sll;)ply. we recommend the following; • A 5D foot length of copper tubing • A stainless steel gas line filter • At least 2 sets of stainless steel Swagelok nuts and brass ferrules
-"o'}
"" ';~
SRIGas Line jostaneton Kit
't~~: --
(it is a good idea to keep a few extras on han d)
• A cylinder pressure regulator wi th O-lOOpsi output NO TE: each type of cylinder has a different eGA connection to the
~~~
e
·4. .
regulator (eGA = ~pressed Qas Association). Air is typically e GA 590 or 346. Helium and nitrogen are eGA 580. Hydrogen endargcn-
_ -
me thane are e GA 350. Gas line installationkitsthat include everything yon need areavailable fromSRI: 860o-C590 Air gas line kit (w ith both e GA 590 and 346 inlet fittings) 8600--C580 Helium/nitrogen gao> line kit 86OQ-C35 0 Hydrogenzargcn-metbane gas line kit (the hydrogen CGA is equipped with a nov.' restricror to lim it the escape o f gas in me even t of a leak) "These kits include everythingin the listofrecommendedsuppliesabove, plusa tubingcutter. Each regulatoris supplied with a l/8" Swagelok fitting for easy connection to the copper tubing.
2. Using the appropriate eGA connecrioa asdescribedabove, attachthe regulatorsecurely to the gas cylinder. 3. Secureoae end ofth e I f8~ copper tubi.ng to the reguJator witha Swagelok nut and ferrule. Cut the tubi ng to the desired length before connecting it to the GC . Make sure to leave it long enough to allow you to move your GC around your work area.
l IB" Swageloi<:
'''''9 -
t---l
4. If 'you don't already filter you-gas, install gasline filter(s) in the gas linc(s) whereit:s CC!!.....enientto replace when needed.
.-_.....
.,...",..
""'''-'' .... _ . ~T"
UIIIIII ""'.,-. -..-_-, -.•..." ~ - ~
•
•
_ _OJ
•
.' •
•
~. ~ .
' e'
5.
CoTli1CCt the gas or gases to the inlets on the left-hand side o f th e
GC as labeled. ~VO TE:
the GC shown here is
equ ipped w ith a bu i lt -in air
comp ressor. when using toe internal air compressor instea d of
cylinder air, ajurnper tube is secured to the air inlet and outlet, If you ordered yourGC with en air compressor, it is shipped w ith tie jumper tube in place as shown.
235 (of 550 ) 2006(-2016)
236
Quitk Start GC Installati on Guide ("Gas Installation & Connection- con+.mued)
GAS FLOW RATES CARRiER 1:
CARRIER !:
,_
--
~: .
J '_
?1T PU R~E :
tf!'OROGEN 1 :
H'I'tlR OCEN AiR 1:
z:
"' 0
-_._- -! Fill
6. The press ure that correlates wi th the flow rat e for the col umn, mak e-up gases. and detector s upplies is labeled on the right-ha nd side oftbc GC. For best EPC performance, set the in com ing gas prcssurets) 15-2Opsi higher than the operating pressure listed on
n
the right-hand sideofthe GC. ~-----...,:;:-
9
;
~.
l;:;
'"" - ~
,
i
II. Column Installatio n 1. If you o rdered a colum•n wi th your ere , it is shipped ins talled in the column oven and yo u can skip this sectio n. Otherwise, open the GC lid and the column e ven lid. Accessories
2. Theseinstructionswillcoverthe installation ofa O.53mm capillary column into an on-column injector. The SRI on-column injectoris designed for a 26 gauge syrin ge needle; a 1O~L liq uid injec tion syringe with a 26 gauge needl e is included in the Accessories Kit shipped wi th your GC. A megabore adapter for syr inge injection onto O.53mm capillary columns is included in the Spare Parts Kit affixed to the inside of the GC tid 0 :1 the right- h and rea r
comer.
'",.
_ ......:::--d {
-OR-
d
1{;1
\
-
•
Ac;:essori es Kit conte nts : • 6' Serial or USB cabl e • Tubing cutl:e r • 10uL liquid injection syringe • 1ml gas injecton syringe & needle • 3mllea!<. check syring e
I'
•
I
236 (of 550 ) 2006(-2016)
237
Quitl{ Start rC o ~um n
GC Installation Guide
Installation- continued)
4. Inisert the column end with the graphite ferrule and SwageJok nut about halfwayinto the megaboreadapter and tighten it withthe nut end ferrule.
The rolu mn shou ld extend about ha lfway into the m egal:o-a adapter
5. After inserting the column into the adapter, insert the column and adapter together into the injection port. Tighten the Swagelok nut with a 7116" v.-:elch. You should feel a littl e give from the ferru le, but do notovertighrcnir. You warx it tight
enough to prvent leakage, but do not SII'.ash the ferrule. lreerttae column and ecacte r into the injed.ion port
<
Connectthe columnto the TeD IN tubing
I
6. Slide ano ther l/S" Swagelok nut and graphite ferrule over tae other end of the
•, column. Fora TeD detector, connect the ., nut to the fittinglabeled " TeD LV ' in the column oven.
For an FlO detector, leave about I" of the column protruding through the nut and ferrule. Iase rt the col umn into the FID bulkhead fitting in the column oven wall an d tigh ten the Swagelok nut.
Please see"AnalyticalColumnInstallation" in the IXSTALLATIOX section of your manual for more detailed information oncolumn installation.
ln ee rt th e coru mn pn1 infn the F lO bufkhea:1ft.tng il'1 lhe oolumn oven .....a'!
237 (of 550 ) 2006(-2016)
238
Quitk Start
GC Installat ion Guide
III. Software Installation N01E: There are uaorials in themanual andonlineatwww.srigc.com (click00 the"Download OurDocuments" button) that will acquaint you with the basic functions of the PeakSimple chromatography software included with you: Ge. 1. Connect the ser ial or USB cable to your computer and the GC . The serial port connection is on the left-nand side of the GC, and the USB connection is on the right-hand side.
...
----_ ~
~ ..--
...
2. Locate yoercopy ofthe PeakS imple softw are just inside the front cover ofyour SRI manuaL Insert the CD or floppy disks into your computer's appropriate drive.
'-1'....
'-
J '" 3_ Double click on "My Compurer... then on the apprcpriaredrive to open it. DOL.hIe click on the "setup.exe" icon, and follow the instructions.
.-.--$ --.. .... ..:§
-----_.-. 6. Open the .Edit menu and choos e QveralL In the dialog box that pops up, enter the number of the COM po rt to which you have connected the GC . For USB, enrer t he uaiqueVSB devicenumber that is printed on your Peakximplc disk(s).
I .•,1
1
and on the back of'tse GC. It is a 4- digi: number-that a lways begins \\i lh "S' (5093, 5276. etc. j.
238 (of 550 ) 2006(-2016)
239
Quitk Start
GC Installation Guide
IV. Detector Activ ation O./POR TANT: If you have a pre-configured GC system. pleas: see the manual section for instructions on operating procedures. The manual is organized Li-to sections with labeled tabs. In addition to preccnfigured GCs, there are sections on detectors, injectors, aurosamplers, "a1Ye5.. and more.
,........;----,.......----=-:-=~= The TeO fil ament
A. Te O Detector
current control switch is located to the right of the TCD detector, on the top ~:.t-t:and su rfa ce of the GC
• 1. Your GC pow er should still be ON, and the filaments should still be OFF. The TeD oven is set to 15O"C at the
factory. It is adjustable by turning: thetrirnpctwhile observing the T e D C ELL LOCAL SETPOJl'\" temperature on the LED display. The rrimpots are located on the top edge of the GC fro nt control panel. Allow the Te D to reachdesired operating temperature and stabilize.
,
.
under the red lie.
2. T eO filaments will bedamaged or destroyed ifcurrent
is applied in the absence offlowing carriergas. Therefore, alway s verify that carriergas is exiting. the TCD carrier gas outlet before energizing the Teo filaments. TheTCD carr ier gas outlet tubing is in the column oven, labeled "TeD OtJf." Place the end of the tubing in some liquid; if710 cubbies are exiting L1e rube, there isa flow problem. DO"'lOT tum the Te D current OX ifyou cannot detect carrier gas flow. A filamentprotection circuitprevents filament damageifcarrier gas pressure is ne t detected at the GC, but it canncc pre ven r filamen t damage under all Correct any lack of cerrier gas flow before
circumstances, Te o carrier gas outlet rubi:1S' is in the columnoven, tagged"TCD our
proceeding. ~ j ~
-•_.. -, ,-. I
~
: 'i'II.=
3. With the Te D filaments stillOFF, zero the data
u
..... " )if .
system signalby clicking on the AutoZcro icon on the !eft sideofthe chroma togram. Switch the TeD
•
. ..,- ..
,.". ;
e
.
. ",
; . ' ;'~:: ::: '\.
""
J: . , . , -
current to LOW. The data syste m signal 's deflection s hou ld not be m ore than 5-2CmV for a
i
bran d-new TeD de tector. The re is also a J-nGH current TCD filament setting,but to avoid filament damage, we recommen d yo u ase only the LOW setting until you. are fa.'"!liliar'A"i th yccr GC end TeD detector.
K-
j
..,,,"
,·1;--'-u
'..;? "" G-
?t
A uto Z e ro Button f
·~:l
'.,
239 (of 550 ) 2006(-2016)
240
Quitli. Start
GC Installation Guide
....
B. FlO Detector
.'
I. Set the Fill amplifier gai n switch to HIGH for most applications. Ifpeaks of interest go offthe scale (greater than 5000rnV). set the gain to MEDIUM.
I"'---
. ...-. :, .._- - -
FlO anplffiergain switch
2. Ser the Fro hydrogen flow to 25mUmi'''lute, and the Fll) air to 250mL/minute. The approximate pressures required for this flow through YCl.l:rGC are labeled on the right-hand sideof theGCchassis. In most cases, the pressure will have been set correctly at the factory. Check the hydrogen and air flow settings bypressing the LOCAL SETPOll\'T button while observing the LED display. Tne gas flow settings are adjusted using the rrimpors on the top edge ofthe GC fron t contro l panel.
.
-' .~.'-' - ,-
Tum th e tr im pet wh ile holding down the ~ L O C AL
. I .
S ETP Ol N T ~
"~
c ··
D~
PAAAN:;TERS
• ••••••
•
•
• •
0
•
•
•
•
• • •
• ••••••
button until you read your desired setting in the LED
-
display.
.' .
.. ;
0- -
3. Ignite the F1D by holding the igniter switch up for acouple ofseconds. until you hearasmall pop. The ignitor switch is located on the front panel of yourGC under the "DETECTOR PARAMETERS" beading, with a vertical label reading "FLAME lG~ITE . " Verify that the flame is lit by holding the shiny side of a wrenc h directly in front of the oolJectoroctIet/YID ex..I.,aust ::- vent, Ifwater coadensarion becomes visib le on the w'!CDCh surface, theflame :5
'"
•
c . For all other d stact c rs, and for more inf orm at io n on the TeD and FiD, pl ease see th e corres ponding m anuel sections.
240 (of 550 ) 2006(-2016)
241
QUi~k
Start GC Installation Guide
V. Inject Your Sample NOTE: Ifyou are inj ecting with a Purge & Trap, 1 0-14. or Headspace concentrator; a thermal desorber; en autosampler, or any cfthe heeredon-column injectors(?lV, Spl it/Splirless, etc.), please seeme corresponding manual section for operating procedures.
A. Syringe Inj ectio n
1. Enter a temperature program for the column oven. The temperature program is determined by Lie sampleand the goalsofthe analysis.
--" ,\::...,:
2. For gas samples, fill the ImL gas syringe with O.5- 1mL For liquid samples, fill tire IOflL liquid syringe with lllL removing jhe bubbles before ~.
.
~e..
n-e Avlo zero """""
is on thA left side of l I..:' the chromatog ra m o
'lirrDfi .
3. Click on the A uto Zero button to zero the data system signal. Hit the computer
keyboard spacebar.
4. Piercethe septum in theon-columninjector-wi th the syringe needle. Insert the needl e straight into the on-column injector port; av oid bending tile need le. Depress th e syringe pfuager rc inject the sample, then withdraw the syringe. For the best and
. ,..: .
.---
Syringe injection of O.5mL gas sample into the encolumn injector en 2 Te O eq ui pped Model 310GC
mostconsistent results,usean easilyreproducible injection technique with quick, smoothmovements. B. Valve Inj ection
1. Set the: valve oven temperaturebetween ambient and 175"(: usingthc trimpoton the top edge of the front control panel. Enter a temperature program for -the column oven. 2. Erne:an event program to automatically inject thecontentsof thevalve sample loop. Thevalveis usually in the LOAD position
Ie
..... ..
-_ . ~. , _~_. e
(default), dl......mg whica Relay G is OFF. When reiay G is activated,
the valve is rotated to the L~JEcr position, in which the carrier gas stream sweeps the contents of the sample loop onto the column(s). Set the valve to INJECf (Relay G O1\') 0.1minutes
..
E_
L
.
ve: :I1
G j)~Al
_
LO@ lI NJ£ ~ Tl
into tbe run unless you have specific run parameters that require
~ ~
different tir.:::Jg.
~ ~ ~ ~
....:=.J ....:=....!
c§rnS T~
~
3. Sample is injected into the bulkhead fitting F ""''-4- labeled "SMfPLE N' on the frontofthe valve oven TIle fitting is equipped with a i tS" Swa geloc mrtfor easy connection of sample streams. 4. Press the comp uter keyboard spacebar to initiate the run. The valve will au tomatically rotate to the INJECT position at 0.1minutes (or whetever time you entered in the Events Table).
241 (of 550 ) 2006(-2016)
242
QUi~k
Start GC Installation Guide ....
VI. Print Your Chromatogram
-
-
£I
.
.... p......, d-.
r:. 't
~ ~
1. Choose Ens IEnnt fromthe mainmenu bar. 2. In the Prir.t screen, designate which channelfs) you want printed. Use L1e radiobuttons to pick a single channel,or- select "Multiple:" and click the checkboxes to select the channels you want to print.
!!pO H
••
.~. ~ :~
c-
c s .A
, ...... . . .
~ ,
c:
r 1r ~ r- 5 r: ~
xl
(
3. C lick the checkbox to select "Print header," then
click on the "P ormat.." button to set up the Header. The Header is printed above the chromatogram on the page, and can contain such information as theanalysis date, the sampl e and injection t)'11<=, columnand carrier gas used, client and lab names. and any special commentsabout the analysis L.l.w: you want printed \\-ith thechromatogram Click ..OK" whenfinisbedformarting your header. The Print screen is stillopen.
""'~- - I
- .. . -:: ..
I
- ::.- ....- 1. _ _ f ':, I ~~-l
:-~ ,; j,
4. In the P:i:1t screen, click the checkbox to selec t "'Printchromatogram," then click on the "scrmet.." burton, Choose "Use screen limits" to print the ch romatogram as you see it onscreen. Youcan also choose the chart speed, which determines the number ofinches per minute displayed in the chromatogram timeline. Forexarrplc, if your chromatogram is IOminutes long and you wan t it to occupy 5 inches 00 the paper. choose 05 incbesminure. Click '"O/{"wnen finished,
t
i
.!
j
._ ..• 1i!f """
~c ~ .· ·;
.~ ,_ ,'7!" ~-
..... .. "' . .......
:.loa<."""'W::- ; ,~,~ .. r,..-
j po r . ' ~ M ' '''' - - - ' I'" ,,,_ -'. ~_
C!" ...
...._,.....-.
-.--. ;;.-~
-
:.
. ..... -..,.
"
.,. ..,. ~
-"'. d."""
, ; ~. ,
~_.~
;.......J..,
'-..• :
:5. In the Print screen, d ick the checkbox to select " Print report," then click on the ..Format. .." button to choose the data that will be included in the report at the bottom. such as the component name. retention:i.mie, peak area and heigat. ctc. e lide"ex" when finished
;;" 5-o"'V- ,, ~ 4' < - ~ ~
r
,..,.'0.."......,.. '"'
_ "" ~,,.
6. Now thar you: chromatogram is ready to print, click on dJ.e Prir.t button in the Print screen.
242 (of 550 ) 2006(-2016)
243
GC INJECTORS Model 8640 20-Vial Integrat ed Liquid A utosampler Overview _ _ Protective cover
Tefion™
The SRI Model 8640 20·vial liquid autosampl er is installed on the left-hand sidc of the SRl 86 JDC Gc. The 8640 connects to an
waste l ine
I
additi onal injectcr cn the left side ofthe colwnn oven. This additional injcctormay be on-column, heated, cr split/splitless . It uses a sample tray to hold up to twenty 2mL vials. a sample probe to transferthe samplefrom the vials into thesyringe barreland an injection mechanism to deliverthe sample fium the syringe barrel.through theneedle, into the injcctoTin theGC columnovcnwall. The 8640 uses 60psi ofair or nitrogen 10 actuate its. moving parts. The 8640 functions are assigned relays so that the autosamplcr may be operated automatical1yusing a PeakSimplc event table. The 8640 is shippedwith 100 screw-top vials and septa, replacements for which are available from a variety of suppliers. Extra sample trays and cooled sample traysare available. The cooled sample trays require an externalrefrigeratedJab circu1atoc.
Waste botlle -
•
Pneumatic
Irnes (bundle d six)
. .""'_
8640 with the protecti v e ooverremoved
1 ;--:.
.- -..• ~
.-
_e _
Knu"""
Inject ion piston
. ...._....---.. .
,
-··_ L :.- ~
•
---'.:.- "".
~
Syringe p iston
Add itional vials are available from AIltech Associates , Inc. 15x45mm Clea r Vial Kit: 100 clear vial s with TFE/$ilicone liners A11tech part # 98008 800-255-8324 www.alltechwea.cc m
243 (of 550 ) 2006(-2016)
244
GC INJECTO RS Model 8640 20-Vial Integrated Liquid Autosam pler Theory of Opera tion Liquid sample is sealed into vapor-tight vials which ere inserted into the sample tray. The tray is then inserted intothe Mode18640 assembly and positionedfor thesampling sequence. The 8640 uses 60psi of air or -nitrogento actuate itsmoving parts.
Sampling Probe Sequence The sampling probe, a concentric
=
J
•
Sample fkM'
Pressurizing
gas in ,
~ LJ.' ~ -~
Injection Sequence 1· Load
2 • carrece forward
,.......
.
~ L
/OUI.to
J
Se;:>tum~
Sample Vial
fro m sample p robe
!
•
injection syringe and out the TcfIonN tubing irrto the waste booie. The sampJe probepressurizes the sample vial for a period of time long enough to rinse the previous sample to waste and fill the syringe with sample.
8ar.'lPlem
In
Sample probe piston
needle, is moved down by a piston to pressurize the vial .....i th helium or other gas, causing sample to flow throughthe
,
synnge
- ,;-irr; Probe ,
Gasv~
"...,..!
UII -. : --
I
=
Thcsyringerrecbanisrn begirs the process in the fully retracted position (I). In thisposttion, the sample flows through the barrel of the inject ion syringe, through the needle to the 3 - Inject wastediverter val veand intothe waste bottle. After-approximately O.5mL of ~I: sample is flushed to waste. the syringe barrel is filled wit h sample. The syringe mechanism is then moved forward by a piston. so that the syringe needle penetrates the waste divcrtcr seal. then the GC injection I port septum (2). On ce the injection needle has penetrated theGC injection m port to the full depth, thcsyringe body is pushed forward over the needle. displacingtbcsampleintotheinjection port (3). Once the sample has been injected , the syringe mechanism retracts , withdrawing fro m the GC injectionport.
~~ , .~II T
r
1
""" Waste diver!!!r t't/-~
1/ -"a!M
~ 1:
To ...·.. s~..
- ;: GCinjection port
244 (of 550 ) 2006(-2016)
245
GC INJECTORS Model 8640 20-Via l Int eg rated Liquid Autosampler Genera l Operating Procedures I. Fill each 2mLvial at least75% full with liquidsample. Oosc thevials so that they arcvapor-tight, "",ith the Teflon side ofthc vial septa facing downward into the vial, 2. The sample tray is inserted and removed from the 8640 in one direction only. To rcmovethe sample vial tray,push it away from you, toward the back ofthcGC. until it is free ofthe autosamplcr assembly. Place the filled sample vials in the tray. Reinscrtthc sample tray into the 8640 assembly fromthe front. Pushitgcntly toward the back of the GC until thc whirelines at the tipofthe whitearrow on the samplenay are aligned with the front edge ofthe 8640. The sample tray is then in theready position, with vial numberone in pleccunder the sample probe. The sample tray shown below, right is almost in the ready position(it \\
4. Load or create a column oven temperatureprogram. 5. Load or create an event table. Version 2.74 (and h igher) c fthe PeakSimple software includes an event
table file called··864Oas.cvt" asa general eventtablefor use with the8640 autosampler. When you loadthis event file, the de fault relay descriptions will not match the actual 8640airrosamplerrelaydescriptions. These aurosampler-specific descriptions must be entered by you. the user. The relays assigned to the autosempler are as follows : Relay A - moves the sample probe DO\VN Relay B - moves the sample probe UP. WARNING! Relay C - moves the syringe carriage FORWARD To av oid injury, keep y our hands Relay D - INJECTS the contentsofthesyringe clear of the 8640 du ring operatio n. Relay E - ADVA., CES the tray one position RelayF - PRESSURIZES thesample vial See the event table shov....n at right for 8640 .evt appropriate descript ions. The 8640 relay d escriptions are also labeled on the rightEVENt TlME moNT EVENT f UNCTION hand side oftheGC. Il l) )(l :::.;,ro d i Ll! l>t:&:::.;m S1gl13 ,- OIl 54 r,.." ". H :t,E' O,j',',l-l e.eso 6 . Sct the autosampl er air or nirrogcn tank o I ':") F Oil to 60psL Set the carrier gas to IOmUminur.e 'ilJI P9SSU" orl (pr"ssutr" ho sa -ce , iJr. , OFF F:~ ~ J S~ pressise hoJa'l] sa rilik: trcc e DO',',N (the equivalent psi setting for yourmachine ,j 0350 islabeledon the rightpane]ofthe GC). The 1],, (11) F ':)FF ·vi31 pressure OFF amount of sample used to flush the needle (J.:'5':l e on S::In'~~ coe.. Lf' can be adjusted by varying the pressureof £1. 80)::0 C on S)'llll';~ c3Ti:! <;I;, r Cp": ,::'RD th e gas used to force th e sample from th e '}. S 5 ~ D CiJ 3JI'TIlI'" 'i.rino~ " U..:ECT vial This gas pressure is adjusted w ith the 0)),) C 0.1" S,ll~oit ca-naoe RE:P..:'CT EPC trimpot on th e top edge of the GCs 1,050 .5 a1 ~ " s.-nnce RETLf::N c Co""!'" front control panel, located directly above 1{!1) E on Ti3 1 ao.ece ou the vertical label "VI AL PRESSURE" on the front controlpanel. Usingthe evcnttablc 1.~ Tr3', 2;\'3 ~: ; OFF E ·' FF
"'"
,
,
at right, y o u should count 25 drops duri ng thetimethattbc gas is prc:s.s.nizingthe sample (0.600 minutes ).
t loX,
S 0:-1"
Riii 3'W pr;NlI'.?
n.:-I;j~ SJ ~,,"
or cre LP
7. The injection volume is factory set at I ul., but is adjustable to 0-3!J.L. loosen the 2 hex-head lock nuts. then tum the knurlcdnutwhile observingthe needle in thesyringe burrel to achievethedesired injection volume (please sec the picture on the Changing the Need!e page to locate the locknuts and knurled nut).
245 (of 550 ) 2006(-2016)
246
GC INJECTORS Model 8640 20-Vial Int eg rat ed Liquid Autosampler Ch anging the Needle In the course of normal operati on, th e 8640 samp le injection needle may become be nt or othenvise
damaged and require replacing. Make SUTe the syringe mechanism is fully retracted before starting; this isthedefaultposition to which it should return after assmplc iniectionsequence, Rep lacement needles are available from Cen tral
sample probe
assembly" Waste bottle "
Needle guide w it h
wese d1verte ~valYe and knuried lhumbsaew
Instruments under part num ber 502743. Syri ng e barrel and needle sets are available ucder part ncmber 503 188 . Call C entral Insnumentsat: 225 -261- 1917 Or wr ite to:
P.O. nox 337
Sa mpla size nut (knur1ed ) . , l ock nuts (2) sample out to waste I
Greenwell Springs. LA 70739 USA. 1. To remove thenee dle. loosen the thumbscrew on the top oftbe wastediverterand the thumbscrew on the needle guideclosestto the syringe barrel. Loosenandremove the t\VQ bushingretamers, Carefully lift out the needle. the two TeflonN bushings and the waste diverter valve together; You will have to push the was te divertcrvalve out of'tbe needle guide , and angle the needle ti p out through the s lot in the side ofthe waste diverrer needle guide asyou pull the needle fro m the syri nge barrel.
2 . Slide the waste diverter valve an d the two Tetlon™ bushings offtheold needle and onto thereplacement needle.
3. Placetheneedle inrothe thumbscrew needle guide and the syringe barrel, and carefully angle the needle with the bushings and wasrediverterva lve brtoplace. using the slot
in the.... esc divcrtcr needle guide to getthetip oftheneedle inroalignment with the syringe barrel.
{'"' f-:~~-~~~~~~~~~~
4. Position the two bushings in their cradles, then replace and tightenthe bushing retainers. Tighten the thumbscrews 011 the needle guide and waste divcrtcr.
5. Adjustthesample injection volume by loosening both
loosen and remove these 2 bus tling re>alnel'5, then remove the2 bushings
hex-head lock outs, then turning the knurled thumbscrew to achieve the desired volume. Tighten the lock nuts.
246 (of 550 ) 2006(-2016)
247
Chapter:
INSTALLATION
Topic:
Interfacing The Liquid Autosampling Carousel
.-..-...The SRI liquid autosampler is a multi-position sample injection system that permits the user to conduct unattended sampling, injection and analyses of multiple samples. Because the complete synnge rinse, load and inject sequence is mechanized and automated, the injection technique will be exact and identical from sample to sample, eliminating any variation in injection technique and sample delivery experienced between different operators when performing manual
injections. This consistency will increase sample precision and reproducibility. SRI liquid autosampler connected 10SRi 8610 gas chromatograph
D
o Front control panel of SRI autosampler controller
The autosampler is controlled automatically by PeakSimple software and/or manually at the autosampler control panel shown at left. Through software control, the autosampler is stepped through the sample vial positions until all samples inserted in the carousel have been injected and analyzed (without the need for operator intervention). A simple command in the event table (momentary activation of relay A) causes the autosampler to
insert, flush, draw and inject the needle contents into the injection port. As soon as the needle has been withdrawn from the injection port, the autosampler is stepped to the next vial position to
remain at the ready for the next actuation of relay A.
The sample vial tray may be manually advanced by hand or by pressing the TRAY ADVANCE actuator button. The amount of time (in minutes) that the syringe needle is flushed to clear the preceding sample is selectable using the FLUSH TIME control. The amount of solvent used to flush the syringe may also be varied by adjusting the sample pressurizing gas pressure. The actual volume of flush required will be dictated by the characteristics of the sample being injected. If not overly viscous, a sample flush volume of approximately 100 microliters should be adequate. If sample availability is limited to small volumes, then the flush may need to be reduced to economize on sample consumption. The amount of time that the needle remains in the injection port after the sample has been discharged from the syringe is also selctable using the INJECTION DWELL control. Selectable in seconds. the control permits the user to choose having the needle withdraw immediately upon having deposited its sample, or to maintain the needle in the injection port for an extended period, permitting any sample containing higher boiling or thermally labile components adequate time to exit the syringe and enter the injection port High boiling components require longer needle-injection port dwell times than volatile components. A setting of 1 second signifies that the needle penetrates the septum, injects the sample and is withdrawn immediately, all within the d ura tion of one second. A setting of 4 seconds permits the needle to dwell in the injection port for an additional 3.5 seconds. C: \EP2\DOCS\UQAUTO I .EPD
REV. 02-10-93
247 (of 550 ) 2006(-2016)
248
Chapter.
INSfALLATION
Topic:
Interfacing The Liquid Autosampling Carousel (continued)
Diverter valve adj~
Tetminal bkcl: 1
T ennina1 block 2
~
~ ~o()o
Terminal block 3
00 0 0 00 0 0 00 0 0
/ AirOUl
00
00
AC hne ron!
~~~==~~ Fuse
- -.--J
Pneumatic ports
(<<>10<_
View of rear panel of SRI aW>sampler COftlOIIer unit
2)45
(9
67
)234
1
~~~~~~~~
~
(9
REAR PANEL INTER FACE DETAll.S
56
7
8
~~~~~~~~
Tenninal block: 2
Terminal block 1
COm.r:cnONS NECESSARY AT I
TERMINAL BLOCK 1:
1
,
CONNEcnONS NECESSARY AT
~
Ajwnpcr wiR mu:;f. be COIWl«Ud between terminals 7 aDd 8 of thi"l terminal bJock (inde x enable positioa), Black wire provided.
T enninal block 3
CONNECTIONS
TERMlNAL BLOCK
~
,-
PwpIe wire must be coeeected fum tenninaJ 1 10 RELAY A terminal ttl mtem.oe board. Black wire must be from terminal 2 to D.GND terminal on inl:erface board.
NECESSARY AT
TERMINAL BLOCK 3: Three-wire cottroI cable from autosampler
White bose from aUl~pler
PNEUMATIc HOSE TERMINAL
O@ RJ,d bose from aUlosampier
White hose from auicsampler vial pressurizatioo regulator C:\EP2\DOCS\UQAtn'02. E.PD
O@
- -.L O @ ---+ 0 @ L
Clear hose from autosampler
@O
Black bose from 4U1osaWplcr
@O
Yellow hose from autosampler
@ O~--
@0
+- - -
-'
Blue bose from tray roauco pneumatic pressure regulator
Terminal block is coke-coded to mato:b bose colon
248 (of 550 ) 2006(-2016)
249
Chapter.
INSTALLATION
Topic:
Interfacing The Liquid Autosampling Carousel
The procedure for installation of the autosampling carousel is simple and straight-forward. Pneumatic and electrical connections must be made at the controller unit and at the data system interface board (If in use by the system). Once these connections have been made, the autosampler is inspected for proper docking height with the chromatograph injection port. If the autosampler is intended for use with an early version of the model 8610 chromatograph (low-profile chassis with an injection port 6.5" above the countertop), the carousel will be equipped with three rubber feet that elevate the injection needle axis to exactly 6.S-. Current production models are mounted on a platfonn that elevates the injection needle axis to exactly 10". This corresponds to the injection port height of the current production model 8610 chromatograph. When proper unit height has been verified at the injection port, the autosampler is mated to the chromatograph and operation may begin.
PNEUMATIC CONNEcnONS In addition to connecting the six color-coded hoses from the autosampler control harness to their respective pneumatic terminals 00 the rear of the autosampler controller unit, two gas connections must be made at the lower two pneumatic hose tenninaIs on the bulkhead. The white hose provided must be connected to the autosampler vial pressurization gas supply, using the provided regulator. This regulator shnuld be set to 15 psi. Gas (typically air or nitrogen) is injected into the vial by the outer sleeve of the concentric sampling needle (needle within a needle), forcing sample to flow out of the vial through the center needle and into the injection syringe. The blue hose should be connected to the tray rotation gas supply, set to 60psi with the other regulator provided with the unit This gas enables the tray mechanism to rotate, advance the samples and operate the injection mechanism .
Pneumatic hose terminal
o=mponi
White base must be via a gas
C(l[IDeCted
-~ (proYided), set to lSpsi, to the Illfosampler vial ,...,.,nz.aoo "" "'J'Ply
C:\F:PZ\DOCS\lJQAUTOJ_EPD
@o @ O-+--,,-Color-
"""
@O @O
Blue bose must be comxx:ted via a gas prcssw-e regulalor (also provided), set 10 6Opsi, to
the tray rotation gas supply falso typically aU).
(~air ).
If air is used by both
n:~,
the main air
supply pressure should be regulated to (at least) 75psi in order to mainta.iD a stable gas supply. Terminal block I 12345678
6)
ELECTRICAL CONNECTIONS There are only three connections to be made by the user. A black jumper wire (provided) must be connected between terminals 7 and 8 of terminal block I. The purple and black wires (also provided) must be connected to the interface board terminals labeled RELAY A and D.GND. respectively. These two wires provide the remote activation of the autosampIer advance and sample circuitry (same as INJECf on the controller unit) by the data sys tem or other remote device.
o@ o@ o@ o@
.I
~ ~ ~ ~ ~ ~ l>ll
"'I)'
B lack jumper wire coonected
Terminal block 2
PuIple wire 10 imertace
boud RELAY A l
......
'=
12'''' !~
611
I~l~ ~ ~ ~ ~ ~ JJ
-
.
.
rf
Black WIre to m.te ace boon! D.G ND terminal REV. 03-03·Q3
249 (of 550 ) 2006(-2016)
250
Chapter:
INSTALLATION
Topic:
Connecting The Autosampler To The Chromatograph Injection Port
Injection mechanism (under protective plastic cover)
Autosampler I injection port interface
Standard SRI liS" injection port
(see detail)
Auto6:ampler injector extends from injection mechanism (under cover) at a height of 10"
from the oountertop. equal to the SRI
10'
• 1rp:um=""""Q
L
chromatograph
----J"
•
injection port
;-
height
Front view of SRI model 8610 gas chromatograph
Right side view of SRI liquid autosampling carousel
The SRI liquid autosampler injector mechanism is situated at a height equal to the injection port of the chromatograph. The injection port height of current production units is 10" (25.4cm). Previous models (pre-1992) employed an injector height of 6.5" (16.5c m). A special
fitting is supplied with the autosampler that replaces the
Autosampler configured for early production chroma!ographs with 6S high injection port
N_, gWde
/ I Autosampler
syringe
septum nut normally used to seal the injection port of the chromatograph. This fitting, also containing a septum, c onsists of a liS " to 114" adapter that is connected to the injec tion port, A special cylindrical brass fitting, employed as a needle guide and waste solvent diverter, is inserted into the needle end of the injector mechanism frame and secured by a Needle guide/waste diverter assembly
/
/
<,
/ 1/4" nut
with T etlonFlushcer diverter drain _ _
reducing ferrule
.
• C:\EP2\DOCS\lJQAlJ'TN.EPD
114" to l iS" injection
Standard. injection port using O.S3mm column adapter and fused silica column
DETAil.. OF AurOSAMPLER INJECTION PORT mTERFACE
pori adapter
•
• •••
thumbscrew. From this cylindrical fitting , a 118" metal tube protrudes. This tube, an extension of the needle guide, is secured to the chromatograph's injection port adapter by means of a 1/4" nut with a 1/4" to liS" Teflon
250 (of 550 ) 2006(-2016)
251
Operating and Instruction Manual for Cobra L/S Autosampler
EST Analytical 503 Commercial Drive Fairfield, Ohio 45014 Phone: 513-642-0100 0818 (225) 261-1917 [email protected]
251 (of 550 ) 2006(-2016)
252
Limited Warranty EST Analytical hereby warrants the equipment supplied herewith to be free from defects in material and workmanship at the time of shipment. EST (the manufacturer), agrees to either repair or replace at our sole option, free of parts and labor charges at our factory, any parts of such equipment which under normal conditions of use prove defective within twelve (12) months (one year) from the date of shipment to the end user. EST has the option of inspecting the goods claimed defective at the Buyer’s place of business or having the defective equipment returned to EST, transportation charges prepaid, for inspection. If an item is found defective under warranty, the repaired or replaced item will be returned to the buyer via the same mode of transportation by which it was received. This warranty does not cover equipment or parts of equipment which are modified by the Buyer. The following goods are warranted for the periods set forth only: (a)
Items produced by third party manufacturers shall carry that warranty provided to EST by said third party manufacturers. Such warranty shall be passed by EST, to the Buyer.
(b)
This warranty does not apply to items consumed in the ordinary course of use of the goods, such as, but not limited to septa, vials, caps, syringes and needles.
(c)
This warranty does not cover bent, broken, or plugged needles, glass breakage, or the replacement or repair of parts due to accident, misuse or contamination, or loss or damage to equipment sustained in transit. Claims for damage sustained in transit must be filed with the transit agency. Notice: All instruments should be insured with the shipping carrier prior to shipping, even if the repair is covered under warranty. The insurance must be purchased by the customer, not by EST Analytical.
The foregoing warranty and remedy are exclusive and expressly in lieu of all other warranties, expressed or implied, including but not limited to any warranty of fitness for purpose or any warranty of merchantability.
i 252 (of 550 ) 2006(-2016)
253
Safety Information CAUTION ! The Auto Sampler system will move rapidly to inject the sample into the gas chromatograph. This movement may prove hazardous if untrained personnel are utilizing the system. The system should be operated with all covers and latches secure. The syringe may move at any time. Make certain that all movement paths are clear at all times before powering on the system. Additionally, the syringe or needle may be bent broken very easily if proper setup instructions are not followed EXACTLY. Only trained personnel should attempt to operate the AutoSampler.
The Auto Sampler may operate on 110 VAC to 240 VAC, 50 to 60 Hz, electrical voltage only. This level of voltage may be life threatening if contacted. There are no user serviceable parts located within the housing of the Auto Sampler or power supply. If electrical problems are suspected contact the factory.
Conventions This manual uses the following conventions: Bold
indicates emphasis or a minor heading.
Italics
indicates the current function on the display that is being emphasized. It is usually a display parameter that will be changing as the AutoSampler performs a task.
CAUTION ! messages precede warnings of procedures or practices which, if not followed correctly, could cause serious personal injury or damage to instrumentation.
Symbols as Marked on the Equipment or in the Operators Manual. Protective ground (earth) terminal.
!
ATTENTION
This symbol is indicating special care should be given to this section of the manual.
!
CAUTION
This symbol is indication any incorrect operation could result in an error or damage to the instrument.
!
WARNING
This symbol is indication any incorrect operation could result in personal injurty or damage to the instrument.
ii 253 (of 550 ) 2006(-2016)
254
u
All safety precautions MUST be adheared to when installing and operating the Auto Sampler.
u
Please read this manual throughly before proceeding to install or operate the Auto Sampler.
u
Be certain all personal in the laboratory are trained and are familar with the operation of the Auto Sampler.
u
When replacement parts are ordered, use only EST Analytical parts and part numbers.
iii 254 (of 550 ) 2006(-2016)
255
TABLE OF CONTENTS Warranty .................................................................................................................................. i Safety Information .............................................................................................................................. i 1.0
Introduction ............................................................................................................................ 1 1.1 1.2 1.3
2.0
Product Description .................................................................................................... 1 Key Fertures .............................................................................................................. 1 Specifications ............................................................................................................. 2
Installation .............................................................................................................................. 3 2.1 2.2 2.3 2.4 2.5 2.6
Installation Protocol .................................................................................................... 3 Unpacking the Auto Sampler ...................................................................................... 4 Parts and Materials ..................................................................................................... 4 Power Requirements ................................................................................................... 4 Interfacing to and Analyzer .......................................................................................... 4 Sample Tray Installation .............................................................................................. 5
3.0
Keyboard Definition................................................................................................................ 6
4.0
Syringe Setup ......................................................................................................................... 6 4.1 4.2
5.0
Target Setup............... ............................................................................................................ 8 5.1 5.2 5.3
6.0
Target Setup Protocol ................................................................................................. 8 Motor Positioning Guidelines ..................................................................................... 9 Target Coordinate Setup ............................................................................................. 9
Method Definition ................................................................................................................... 9 6.1 6.2 6.3 6.4
7.0
Syringe Installation ...................................................................................................... 6 Syringe Calibration ..................................................................................................... 7
Method Editing ........................................................................................................... 9 Method Parameters .................................................................................................... 10 Utilizing Standard Solutions ........................................................................................ 14 Suggested Method Parameter Values Utilizing Hexane and Methylene Chloride ............ 15
Operational Keys.................................................................................................................... 15 7.1 7.2 7.3
Hold/Stop Key ........................................................................................................... 15 Prog (Program) Key ................................................................................................... 17 Mode Key ................................................................................................................. 17
iv 255 (of 550 ) 2006(-2016)
256
8.0
Cobra L/S Setup Menus ......................................................................................................... 17 8.1 Configuration Menu .................................................................................................... 17 8.2 Maintenance Menu ..................................................................................................... 18 8.3 Diagnostics Menu ....................................................................................................... 18 8.3.1 Relay Output Testing ....................................................................................... 18 8.3.2 Input Signal Test ............................................................................................. 18 8.3.3 Motor Delay ................................................................................................... 18 8.3.4 Motor Speeds ................................................................................................ 19
9.0
Remote I/O Cable Connections............................................................................................... 20
10.0
Remote Control (RS232 Serial link) ....................................................................................... 20 10.1 Data Format ............................................................................................................... 21 10.2 Command Summary from Host to Cobra .................................................................... 21 10.3 Cobra L/S Command Details ...................................................................................... 22 10.4 Programming System Parameters ................................................................................ 23 10.5 System Errors ............................................................................................................. 24 10.6 Error Codes ............................................................................................................... 24
11.0
Installation of Cables and Mounting Hardware ......................................................................... 24 11.1 Installation of the Cobra L/S to Gow-Mac 600 GC ..................................................... 25 11.2 Installation of the Cobra L/S to HP 5890 GC .............................................................. 26 11.3 Installation of the Cobra L/S to HP 6890 GC .............................................................. 27
Appendix: Syringe Operating Drawings .............................................................................................. 29
Cobra L/S Manual Revision "C", 6/01
v 256 (of 550 ) 2006(-2016)
257
1.0 Introduction 1.1 Product Description The Cobra L/S Auto Sampler combines state-of-the-art component technology with easy-to-use operating features that meet routine as well as research level autosampling requirements. The Cobra L/S is an all-electric, stepper motor driven autosampler providing rugged reliability and pinpoint injection accuracy. The syringe mechanism moves back-and-forth and in-and-out across the sample tray to access sample vials, multiple solvent vials, standards, etc. Variable inject volumes, injection speed, needle dwell times, number of samples per vial, multiple methods per run, solvent flush, air gaping, dual column operation and a host of other autosampling options are all standard and easily programmed on the Cobra L/S's menu driven keypad. The unit uses screw-cap or crimp-top septum vials and easily interfaces with your GC system with all the remote inputs/outputs—ready signal, injection mark, etc.—plus RS 232 for direct communication with an IBM or compatible personal computer. Mounting is easy and allows for quick changes between GC’s if desired. Syringe/injector alignment is via the keypad. The control module mounts on either side of the autosampler for easy access.
1.2 Key Features •
Direct Syringe Injection: Uses 1.5µl - 100µl syringes for minimum sample volume and maximum flexibility.
•
All Electric: No additional cost for gases.
•
Priority Manual Sample feature allows the current analysis to be interrupted for RUSH samples.
•
Variable Sample Fill Rate for viscous samples.
•
Variable Injection Rate to optimize chromatography based on injector type and analytes of interest.
•
Dual Injector Operation allows maximum productivity from GC with dual injectors and columns.
•
Programmable Injector Alignment: No manual adjustments to align injection ports.
•
Variable Dwell Time for hot needle injection techniques.
1
257 (of 550 ) 2006(-2016)
258
•
Post Solvent Rinse user definable with two separate rinse solutions.
•
Internal Standard Injection
•
Two Solvent Rinse capability minimizes cross contamination.
•
Easy To Operate Menu-driven system simplifies method setup and allows for multiple method linking. Up to 10 different methods available.
•
A sample may be run from any position in the sample tray in Manual or Auto mode.
•
Large 120 or 200 position sample tray for overnight operation that lifts off for easy loading.
•
The syringe may be programmed for simple or complex injection sequences through a simple keypad entry system allowing for any type of sample handling with one system.
•
Totally controlled sequences of syringe purging and rinsing allowing improved peak resolution and minimum compound carry over.
•
Fast easy programming from the touch pad keyboard terminal.
•
Easily readable backlit LCD display.
•
Compact size, requires less space than other autosampler systems.
•
Easy hook up and installation.
1.3 Specifications •
Tray Capacity: 120 sample vials — 2 ml, 12 mm x 32 mm vials; 2 Solvent, 1 or 2 Waste, 10 ml vials
•
Sample Size Reproducibility Typically 1% or better.
•
Minimum Sample Size: 1% of Syringe Volume
•
Sample Injections per Vial: 1 to 100; or sample vial capacity.
•
Standard Injection: 1% to 100% of syringe capacity (standard volume plus sample volume cannot exceed the syringe volume.
•
Operating Temperature: 15o to 35oC Storage Temperature: 0o C to 85o C
•
Relative Humidity: 10 to 90%
•
Line Voltage: 100-240 VAC; 50-60 Hz, 115-160 VA 2
258 (of 550 ) 2006(-2016)
259
•
Weight: Auto Sampler Unit - 17 lbs 3 oz..: 7.8 Kilograms
•
Size: Auto Sampler Unit - 25 x 10 x 17 inches : 63.5 cm x 35.5 cm x 43.2 cm
2.0 Installation 2.1 Installation Protocol The complete installation of the Cobra L/S includes the following steps: 1.
Unpack the Auto Sampler and make certain all parts and supplies are available.
2.
Install the mounting bracket to the GC per separate instructions.
3.
Install the Auto Sampler onto the mounting bracket.
4.
Install the cable from the Display/Keypad Terminal box to the rear of the Cobra L/S, see Figure 2.0.
5.
Connect the Remote I/O cable between the Auto Sampler and the GC or data system. See Section 9.0.
6.
Connect the power supply power cord to the rear of the Auto Sampler and then plug the main power cord into a grounded AC power source.
7.
Install the syringe assembly. See Section 4.1.
8.
Perform the Setup and Target Setup procedures (some of these may require removal of the syringe.) Verify the initial mounting bracket alignment to the injection port on the chromatograph. See Section 5.0.
3
259 (of 550 ) 2006(-2016)
260
2.2 Unpacking the Auto Sampler Carefully unpack and inspect the Auto Sampler. Inspect the instrument for possible shipping damage. If damage is discovered, immediately notify the shipping carrier and then EST Analytical. Do not return the instrument without first notifying EST Analytical and obtaining a Return Goods (RG) authorization number. If possible, please store the shipping cartons and all packing material for possible future use.
2.3 Parts and Materials The following parts list is included in the accessory kit. • • • •
Sample Tray Power Cord w/ Power supply Sample Syringe Optional Mount Bracket (This must be purchased seperately)
2.4 Power Requirements
!
• • • • •
I/O Cable (comes with bracket) 4 Solvent / Waste Vials (10 ml) 4 Solvent / Waste Caps with Septa 4 extra Waste/Solvent Septa Operators Manual
ATTENTION
The Auto Sampler is an all electric system with only a maximum of 24 VDC present in the cabinet . No gases or other energy sources are required. The power requirement for the system is an input to the power supply of 100-224 volts and a line frequency of 50 to 60 Hz.. Make certain the electrical voltage is a constant source with no severe drops or spikes in the voltage. If the power source is not certain, install a power conditioner on the electrical line.
2.5 Interfacing to an Analyzer
!
CAUTION
To properly interface the Auto Sampler to the GC, the GC ready (or Analyzer Ready) signal and the remote start signal must be located on the GC and or Data Collection Device. Each GC is different and it may be necessary to refer to the instrument’s manual, or contact a representative for the correct location of the ready and start signals. Connection points on gas chromatographs are unique to each system, therefore, a specially wired cable is required. To insure correct operation of the system follow the wiring schematic supplied with each cable. If a problem exists please consult the factory. The Auto Sampler may also be operated in the Local mode if a GC ready signal is not available. The Local mode allows the Auto Sampler to inject a sample based on a cycle time setting without receiving a ready signal . See Method Parameters Section for more details. The connections will be from the Auto Sampler’s Remote I/O connector (25 Pin D), located on the rear of Cobra L/S, to the chromatograph’s I/O "D" connector or appropriate terminal block connector(s).
4
260 (of 550 ) 2006(-2016)
261
Terminal Cable Connector
Rear of Terminal Box
Power In Receptacle
Power Switch
TERMINAL 24VDC 2.5A
Remote I/O Receptacle
Rear of Cobra L/S
REMOTE I/O
USE APPROVED POWER SUPPLY ONLY
RS-232
COBRA TERMINAL
POWER
REAR VEIW OF COBRA SAMPLER
PC SERIAL PORT ANALYZER/GC AC INPUT 100-240V 1.5A 50-60Hz
Figure 2.0 Figure 2.0 shows the complete installation of cables to the GC and for RS 232 remote control. Be certain all cable connections are made before the power to the Cobra L/S is turned on.
2.6 Sample Tray Installation Unwrap the sample tray and place it onto the sample tray brackets. The tray will only mount in one direction as there are alignment pegs on the holder brackets and corresponding alignment slots in the tray. Once installed, place an empty vial with cap and septa in vial position #1 and the waste / solvent locations to be used. Be certain the waste/solvent tray is located on the correct side of the sample tray for your GC. Note, the waste / solvent tray may be located on either side of the sample tray, see Figures 2.6 & 2.6 a. Tray Mount Pegs Optional Position
Figure 2.6 Figure 2.6a
Support Brackets
5
261 (of 550 ) 2006(-2016)
262
3.0 Keyboard Definition The keyboard provides for a complete entry of all Setup, Method, Configuration, Diagnostics as well as motor operations. The keys perform the following operations. (See Operational Keys, Section 7.0, for a complete description of Key Functions.)
Hold/Stop Key:
Provides both a "Hold" in the current operation and/or a complete abort of the current operation and allows for an exit out of a menu.
CCobra obra L/S L/S /
LIQUID SAMPLER LIQUID/SAMPLER
PROG
MODE
HOLD STOP
ENTER
Robotic Sampling System
Mode Key:
Selects the desired Mode of opera tion: Automatic, Manual or Flush.
Program (Prog) Key: Provides access to: Methods, Configure and Diagnostics menus. Enter Key:
Arrow Keys:
Accepts the numeric value entry and/or menu item selection. It also scrolls to the next data entry item in applicable situations. Allows for selection of all data, the L/R keys allow for increasing or decreasing numerical values and the U/D for scrolling within a menu or parameter.
4.0 Syringe Setup The Cobra L/S will accept most manufacturers syringes however, a SGE 10µl, FN (P/N 506303) is shipped as standard. NOTE: If another syringe brand is used there may be some adjustment required to the lower needle guide. Select the "Configure" menu using the "Prog" key and follow the instructions for "Syringe Setup".
4.1 Syringe Installation
!
CAUTION
1. Loosen the syringe plunger thumbscrew (1) and the two 4-40 socket head screws (4) securing the holder. 2. Insert the syringe needle (10) into the mid needle guide (9) and then down into the lower guide (11). 3. Insert the syringe flange (3) into the notch (4) in the upper section of the syringe holder (8). 6
262 (of 550 ) 2006(-2016)
263
Raise the plunger thumbscrew (1), holding it up, insert the syringe plunger thumbpiece (3) into the Tslot in the plunger retainer. Lower the plunger retainer thumbscrew and tighten securely. Rotate the syringe clamp (6), 90 degrees, to hold the syringe (7) in place. 4. Set the plunger to its zero position by sliding the holder (8) up until it touches the needle, then back it down about 1/64" and tightening the two 4-40 socket head screws (4). 5. Verify that the needle (10) does not extend beyond the lower needle guide (11). Place your finger under the lower needle guide and check. The needle tip should not be felt. If the needle tip can be felt, the needle guide requires adjustment, consult factory.
4.2 Syringe Calibration
1 1. Plunger Thumbscrew in Plunger Retainer 2 2. Syringe Flange 3 Holder 3. Syringe Flange 4. 4-40 Socket 5 Screws 5. Syringe Flange 7 6. Syringe Holder Clamp 7. Syringe 8. Syringe Holder 8 Assembly 9. Center Needle Support 10.Needle 11.Lower Needle Holder Figure 4.1
4 6
9 10 11
The syringe plunger must be properly calibrated to insure injection accuracy. The procedure is performed in the "Cobra Setup" section of the control program. Press the "Prog" key and select the “Cobra Setup” menu, press the Enter key and select the "Configuration" Menu line, press Enter. Now, with the down arrow key select "Vol Calib", press Enter. The "Syringe Setup" screen is now showing. Manually adjust the plunger to zero (if required) by adjusting the holder up, until the syringe plunger touches the bottom of the syringe, then back it down about 1/64", tighten the two 4-40 socket head screws, press the Enter key.
Properly installed syringe.
The next screen adjusts the maximum stroke of the plunger. With the Left/Right arrow keys, move the plunger up, such that the end of the plunger is on the maximum graduation mark of the syringe installed. (Note, record the value show on the line "Volume" for future use). Press the Enter key. Next, using the Left/Right arrow keys, adjust the plunger Figure 4.1a stroke to the maximum position allowed on the syringe barrel. This is generally about 10% above the syringe volume. Press the Enter key. NOTE: If the plunger motor "chatters", the syringe holder is set too high not allowing the plunger sensor to be reached. Loosen the two 4-40 socket head screws and slowly lower the holder until the motor stops chattering. The plunger sensor has now been homed. Look at the plunger to be sure it is at the "0" mark. The plunger has now been set to the maximum graduation (100%) mark on the syringe scale. This will allow the software to properly calculate the sample and rinse volume parameters. 7
263 (of 550 ) 2006(-2016)
264
5.0 Target Setup CAUTION: Severe damage can occur to the Syringe, Sample Vials, and/or Chromatography Instrumentation if incorrect parameters are set. Remove the syringe from the holder. CAUTION: The mounting bracket must be correctly installed before attempting Target Setup.
5.1 Target Setup Protocol The Auto Sampler is designed to inject from up to 220 samples from .8 ml sample vials, however, the 120 position 2 ml vial tray is standard, into most types of GC septum injection ports. Two injection ports may be established anywhere along the travel length of the syringe arm. Target Setup involves completing the following steps. 1. Installing the Mount Bracket and Auto Sampler to the analyzer. 2. Installing the Syringe Holder and Sample Tray with the Waste / Solvent installed on the correct side for you GC inlet configuration. 3. Syringe Installation and Calibration (be certain the syringe is removed before beginning Target Setup). 4. Selecting the Sample Tray Style. 5. Calibrating the sample vial #1 position. Note, never allow the needle to pierce the septum of an empty vial. Always have liquid in the vial. This will help lubricate the needle in the septum. 6. Setting Flush Vertical and Waste Vertical positions. 7. Calibrating the syringe to the injection port(s) location(s). 1
2
3
1. 4-40 x 1" Socket Head Screws 2. Waste/Solvent Block 3. 120 Position Sample Tray 4. Optional Waste/ Solvent Position
4 Vial Position # 1
Figure 5.1 88
264 (of 550 ) 2006(-2016)
265
!
5.2 Motor Positioning Guidelines
ATTENTION
When setting up the Sample Tray and Injection Inlet positions the arrow keys act as a directional input for axis movement (Left / Right arrow keys for Left / Right movement and the Up / Down arrow keys for Front / Rear movement). This movement is achieved when the operator "taps" or pushes a directional arrow key momentarily. If the movement is not "fine" enough, the step rate may be changed from "Continuous" to "Jog", and the number of steps per movement may be changed. To access this menu, from the "Target Coordinate Setup" menu, move the head to a target and then press the "Mode" key. The "Select:" menu comes up, from here, the type of movement, either Jog or Continuous may be set, also the number of steps per movement. Changes are made by pressing the "Mode" key or the arrow keys. The default step rate is factory set at 10. To exit the menu press the Stop key.
5.3 Target Coordinate Setup
!
CAUTION
Press the "Prog" key and select "Cobra Setup." Select the "Configuration" menu line and press Enter. Scroll to the "Sample 1" line and press Enter. Press Enter and the syringe arm will move slightly to the left and out. The arrow keys are now used to move the syringe arm over to the center of vial #1. Press either the Left or Right arrow key to move the arm to the approximate center position of the first row of vials. Using the Up or Down arrow key, toggle to the "For/Back" menu line, use the Left or Right arrows to move the arm to the approximate center of vial #1. Toggle to the "Vertical" menu line and with the Right arrow key, lower the syringe arm to just above the vial cap. Install the syringe and make the final adjustments to the needle position. The needle must be positioned down into the vial to not hit the bottom!. After the setup is complete write down the number coordinates for future use. Press the Enter key and the arm will move to home, toggle to the next menu line "Waste", press Enter. The same X-Y-Z coordinates must now be established for the Waste (1 & 2) and for Rinse (1 & 2) and for the injection Inlets A & B. The procedure for these settings is the same as for Sample #1. The only difference is the inlets will require a finer adjustment than the vials. Once all the coordinates have been established install the syringe and recheck the target locations.
6.0 Method Definition 6.1 Method Editing The Cobra L/S allows 10 methods to be saved into memory. To edit a method, press the "Prog" key, select "Method Edit", enter the method number and press Enter. The next menu will allow entry into the selected Method. Press the Enter key and the parameters will be displayed. The Method parameters will then cycle through with each touch of the Enter key or Up\Down arrow, allowing changes to be made. The method editing may be exited at any time by pressing "Prog" or the Hold\Stop key. If the Enter key has been pressed changes will automatically be saved. If an invalid entry is made, the system will not save the entry. Refer to the following parameter list for values for each parameter. The parameter values are in brackets [xxx]. 9
265 (of 550 ) 2006(-2016)
266
6.2 Method Parameters Parameter
Range
Description
First Vial
[1 to 120]
The first sample vial to be injected.
Last Vial
[1 to 120]
The last sample vial to be injected.
#Inject/Sample
[1-100]
The number of injections to be performed on each individual sample.
#Rinse/Solv #1
[0-20]
After a sample is injected, the syringe will be rinsed this number of times using Solvent #1.
#Rinse/Solv #2
[0-20]
After a sample is injected, the syringe will be rinsed this number of times using Solvent #2.
Rinse Volume %
[0-100%]
The percentage of the total volume of the syringe to be used in rinsing, i.e... a setting of 50% when utilizing a 10 µl syringe would allow 5 µl of rinse solution to be drawn into the syringe for every rinse.
Rinse Fill Rate %
[0-100%]
The plunger stepper motor speed will be adjusted to a speed rating per the input value. Use a lower number if more viscous solvents are being used to avoid air bubbles.
Standard Volume %
[0-100%]
The percentage of the total syringe volume used when adding a standard to a sample, i.e... a setting of 10% (when utilizing a 10µl syringe) would cause 1µl of standard solution to be drawn into the syringe each time a sample was to be injected. If this parameter is used, each sample injection will have standard added to the syringe along with the sample. Note, the standard is always drawn into the syringe first and the sum of the standard volume and sample cannot exceed 100%.
Sample Volume %
[0-100%]
The percentage of the total syringe volume used, i.e... a setting of 10% (when utilizing a 10µl syringe) will inject 1µl of sample solution.
10
266 (of 550 ) 2006(-2016)
267
Sample Rinse
[0-10]
The number of times the syringe is filled with sample and "emptied" to the waste vial. The volume of sample loaded into the syringe will be according to the Sample Volume % Parameter.
Sample Pumps
[0-10]
The syringe will be flushed this number of times with standard/sample solution before the final standard / sample solution is drawn into the syringe prior to injection. The syringe will remain in the sample vial for this process. This helps to purge air bubbles from the syringe before drawing in the final sample to be injected.
Sample Fill Rate %
[0-100%]
The plunger motor fill rate speed will may be controlled with this value. Use 100% for the fastest plunger operation. Use a lower number if more viscous samples are being used to avoid bubble formation.
Sample Inj Rate %
[0-100%]
The plunger injection speed is controlled with this parameter. Use a lower number if more viscous samples are being used to increase reproducibility. Use 100% for the fastest injection speed.
Syringe Offset %
[0-20%]
The syringe offset determines what volume of sample remains in the syringe at the completion of an injection. A value of 10% to 20% may be useful in avoiding volume errors due to bubbles caused by certain sample types. The offset is ignored during the rinse cycle. This parameter MUST be set to if the Pre-Fill air parameter is being used.
PreFill Air %
[0-100%]
The amount of air to be drawn into the syringe before drawing in the standard/sample. This provides a head space of air to help purge the syringe of the entire sample during injection. The value entered is a percentage of the total syringe volume, i.e. a setting of 10% (when utilizing a 10µl syringe) will draw 1µl of air into the syringe. See “Syringe Offset Parameter”. Note, the sum of the standard volume & sample volume & Prefill Air % cannot exceed 100% of the syringe capacity.
11
267 (of 550 ) 2006(-2016)
268
MidFill Air %
[0-100%]
The amount of air to be drawn into the syringe after drawing the sample/standard volume. This air space will be utilized as a buffer between the two different solutions in the syringe. The value entered is a percentage of the total syringe volume i.e. a setting of 10% (when utilizing a 10µl syringe) will draw 1µl of air into the syringe each time a standard solution is drawn into the syringe. This parameter is not used if the Standard Volume is set to “0”.
PostFill Air %
[0-100%]
The amount of air to be drawn into the syringe after the sample is drawn into the syringe. This air volume can reduce “needle burn off” of sample in the injection port. The value entered is a percentage of the total syringe volume, i.e. a setting of 10% (when utilizing a 10µl syringe) will cause 1µl of air to be drawn into the syringe after the sample solution is drawn into the syringe.
Start Delay
[0-999 min.]
This parameter allows the autosampler to begin its sampling sequence at a future time, up to 999 minutes from the start point.
PreInj Delay
[0-600 sec.]
The number of seconds to pause after the syringe needle has entered the sample injection port. In systems where “needle burn” occurs this value can help separate the initial solvent injection from the main sample injection.
PostInj Delay
[0-600 sec.]
The number of seconds to pause (Dwell) after the sample has been injected. This feature allows the sample, time to completely leave the needle, before the needle is withdrawn from the injection port. GC Start and Data Start signals have been activated.
Inject Target
[A, B, A&B, A+B]
There are two injection targets possible, “A” and “B”. The sample will be injected into the assigned target(s). The position of the inlets does not matter, they can be left/right or front/rear. Multiple targets may be selected by entering one of the A, B combination values. The Left/Right arrow keys will scroll through the selections available. 12
268 (of 550 ) 2006(-2016)
269
[A&B]
All volume of standard/sample is drawn into the syringe for both inlet injections. Injection of the sample volume is made into port A and then the syringe goes directly to port B and injects the remaining volume. The injection volume per inlet, is whatever percent was programmed.
[A+B]
The programmed standard/sample volume is drawn into the syringe and injected into port A. Without rinsing, the syringe returns to the standard/sample vial and draws the programmed volume of standard/sample solution, this is then injected into port B.
PostFill Delay
[0-60 sec.]
This parameter allows a pause after the plunger has pulled the programmed sample volume into the syringe barrel. This delay, in seconds, allows viscous samples to completely fill the syringe barrel before the syringe needle is removed from the sample vial.
Operate Mode
[Remote / Internal]
Remote or Local operating modes are selectable by using the Left/Right arrow keys. In the Local mode, the Cobra L/S operates according to the Cycle Time Parameter. In the Remote mode, a GC Ready or Start signal must be received, and the Cycle Timer must be at “0” before the injection can begin.
Cycle Time Minutes
[0-999 min.]
Begins counting time from when the injection is made, (plunger is depressed). The next sample injection process will not start until this amount of time has elapsed. The syringe will however be rinsed, after the injection, according to the number of Rinses programmed. If the duration of post-rinse sequences requires a longer time period than the Cycle time, this parameter is not the determining time between injection cycles. This parameter is only required when running in the Local mode.
Aux. Time Minutes
[0-999 min.]
The auxiliary timer begins marking time when the sampling sequence begins. At the end of the programmed time, the Auxiliary Output switch is pulsed.
13
269 (of 550 ) 2006(-2016)
270
Link to Method
[0-10]
Methods may be linked together allowing the Cobra L\S to run multiple methods in a continuous process. Note: Circular linkage of a single method is allowed providing for continuous sample operations. When the method parameter is set to "0", the Cobra L\S will only run the one selected method.
See Section 6.3.2 for an example of Method Parameter Setup values. The Method example may be used for most sample situations.
6.3 Utilizing Standard Solutions The Cobra L/S allows standard solutions to be automatically added to the sample injection. The syringe will first fill with standard solution and then move to the sample vial and pull up the sample into the syringe. Both sample and standard will then be injected as one “sample”. Standards are loaded into the tray in the far right vial column, vial positions 113 to 120. When a Standard Volume is programmed, the syringe will move to the standard vial position along each row of sample. As an example, all samples processed in vial row #1 will use position # 113 as the standard location. All samples in row # 2 will use position # 114 as the standard location. This pattern is used all the way to row # 8 Standard position # 120. What this means is samples CANNOT be loaded in locations 113 -120, this is reserved for Standards ONLY! This method works well for injection methods into single injectors and in the dual inject mode [A+B] (see Inject Target parameter in Section 6.2). It does not work in the dual inject mode [A&B] because the sample and standard are not sufficiently mixed in the syringe.
Standard Vial Position Row, #'s 113-120.
Figure 6.3
14
270 (of 550 ) 2006(-2016)
271
6.4
Suggested Method Parameter Values Utilizing Hexane and Methylene Chloride
Use the following as an example to setup Method Parameter Values. These values are suggested for solvents such as Hexane and Methylene Chloride. This Method is with a 5µl syringe installed. The sample is 1 µl, with a .25 µl offset injecting into inlet A. The syringe will be rinsed with 5µl of rinse #1 twice and #2 once. Prior to injection, it will dump the rinse twice, into waste, and then flush in the vial 5 times. This should eliminate any bubble problems with any solvent. Method Parameter # Inject/Sample # Rinse/Solvent #1 # Rinse/Solvent #2 Rinse Volume % Rinse Fill Rate % Sample Volume % # Dumps/Inject # Flushes/Inject Sample Fill Rate Sample Inject Rate Syringe Offset Operating Mode
Initial Value 1 2 1 100 10 20 2 5 10 100 5 Remote
7.0 Operational Keys 7.1 Hold/Stop Key The Pause/Stop Key performs two (2) functions: 1. Pause the current Auto Sampler operation at its completion. The sampling continues until a complete sample injection cycle is completed. The method parameters and/or the system parameters may then be edited or a priority Manual Injection may be performed. The system may then resume the AutoRun (where it paused) and complete the method. 2. Abort the current AutoRun or other function. The Syringe contents may be dumped to waste and/ or immediately returned to its “Home” position and the AutoRun may not be resumed from the point it was stopped. NOTE: The EndPause can be turned off at any point before it is actually executed by pressing the Enter Key.
15
271 (of 550 ) 2006(-2016)
272
Cobra L/S C obra L/S LIQUID/SAMPLER / LIQUID SAMPLER
PROG
HOLD STOP
MODE
ENTER
Robotic Sampling System
Cobra L/S Keyboard Overlay
Press Hold/Stop Key - One Time. During any operation of the Auto Sampler the “Hold/Stop” Key may be pressed. Hold the key down until the “End Pause” message appears. For an operation pause, the screen will display the prompt “End Pause”. The Auto Sampler will continue until the current injection cycle is completed. At this point practically any aspect of the Auto Sampler may be updated. Methods may be edited, a Priority Manual Sample may be performed or any of the System parameters may be changed. To resume the AutoRun from the point it was paused, press the “Enter” Key.
Press Hold/Stop Key - Two Times. Pressing the “Hold/Stop” Key the second time will immediately stop the motors. A prompt will appear on the screen to allow the syringe contents to be dumped to the waste vial before returning the syringe to its home position and reset. The method or AutoRun cannot be resumed from the position it was stopped without editing the method and changing the “First Vial Position”. If the syringe contains any solution at this point, press the “Enter” Key to allow it to be dumped into the waste vial before returning the syringe to its home position. CAUTION: Syringe contents will be emptied where the syringe is currently positioned if the "Hold/Stop" key is pressed instead of the “Enter” Key. This could cause hazardous and/or corrosive chemicals to be dispensed into the atmosphere and/or onto the Auto Sampler and Analyzer. 16
272 (of 550 ) 2006(-2016)
273
7.2 Prog (Program) Key The Prog Key is used to access the Cobra L/S Method Edit and Setup menus. The user must select either the Method Edit or Setup screen with the Up/Down arrow keys and press Enter. If Method Edit is selected, enter with the Left/Right keys, a method number from #1-10 and press the Enter Key. The display will change to the method number entered allowing for editing or review. If the Setup menu line is selected, the next screen allows access to the "Configuration, Maintenance, Diagnostics and Motor Speeds" menus. These menus will be discussed in detail in Section 8. To exit the "Prog" key selection press the Hold/Stop key.
7.3 Mode Key The mode key allows the user to begin running samples. Press the "Mode" key and the next screen will display the selection of "Auto Run" or "Manual Run." The user can select either mode with the Up/Down arrow keys. If the Auto Run is desired enter the method number, with the Left/Right arrow keys, then press Enter. This will immediately begin the sampling sequence per the Method selected. If the Manual mode is selected, the next screen allows the user to run a single sample or rinse the syringe. If a sample is to be run the user must enter the Method number and the sample vial number to run. The Left/Right arrow keys are used to enter this data. Press the Enter key and the sequence begins. If Sample Rinse is selected, the next screen allows the user to enter the Method number to run the rinse syringe sequence. Press the Enter key to begin the sequence. NOTE: The Auto Sampler will rinse the syringe according to the parameters in the Method number selected. It is advised that a Method be dedicated to the desired syringe flushing cycle and stored for future use.
8.0 Cobra L/S Setup Menus The Setup Menu allows the user to access the Cobra L/S Configuration, Maintenance, Diagnostics and Motor Speed menus. These menus provide complete setup and diagnostic tools for installation and performance setup. Note: Several of the menus in this section are intended only for a service technician.
8.1 Configuration Menu Configuration menu allows the setup of the sample tray and all needle targets (these were discussed in detail in Sections 4.0 and 5.0).
17
273 (of 550 ) 2006(-2016)
274
8.2 Maintenance Menu Maintenance menu displays the current Firmware revision code and the Plunger count. This is useful in knowing the life cycle of a Teflon tip style syringe plunger. The count can be reset by using the Left/Right arrow keys. To exit the menu press the Hold/Stop key.
8.3 Diagnostics Menu
!
WARNING
CAUTION: Only trained personnel should operate the Cobra L/S whenever the Diagnostics menu is accessed. Damage to the syringe, sample vials and/or chromatography instrument could be severe if untrained personnel attempt to use this menu without a complete understanding of is purpose! This menu will allow the trained operator to move the Front/Back, Vertical, Plunger and Right/Left axis. Additionally, the motor movement parameters may be changed. These are the beginning and ending ramping and the final speed settings. NOTE: If this menu has been accessed, the menu line "Enter To Test", will cause each axis to move until the Stop key is pressed!
8.3.1 Relay Output Testing Additional diagnostic information is available for relay testing. These are the GC/Data, Auxiliary and Spare Output relays and the Input signal data. This information is useful for determining if one of the output relays is not working. Relays maybe wired for normally open or normally closed, the closure is for .5 seconds. The default setting is in the N.O. mode. From the Diagnostics menu, scroll, using the UP/Down arrow keys, to the relay desired for testing, press the enter key. The display will show the selected output, i.e....GC/DATA Start, Enter to test, Stop to exit. To preform the test be certain the I/O cable is properly connected or a VOM meter is set to the correct position to test the output. Follow the instructions on the display.
8.3.2 Input Signal Test This screen allows the GC ready signal to be tested. The normal state should be OFF, once an input signal is received, the OFF will toggle to ON. The screen line "Spare 7" is an indicator showing that the spare (these are signal line inputs for future use) signals are floating "high."
8.3.3 Motor Delay
!
WARNING FOR TRAINED TECHS ONLY!
CAUTION: Only trained service personnel should operate the Cobra L/S whenever this Diagnostics menu is accessed. Damage to the syringe, sample vials and/or chromatography instrument could be severe if untrained personnel attempt to use this menu without a complete understanding of is purpose! This menu is intended for the service technician.
18
274 (of 550 ) 2006(-2016)
275
This menu allows the stepper motor delay time (in milliseconds) to be changed. This time is the duration of pause at the end of one motor movement and the start of the next motor movement. The factory default is 100 ms. The Left/Right arrows will change the value. Press Enter to exit. To test the new time setting you must scroll to one of the motor axis movement menu lines. The best one is probably the Left/Right axis, follow the screen prompts to access moving "all" motors.
8.3.4 Motor Speeds
!
WARNING FOR TRAINED TECHS ONLY!
This screen allows the service technician access to settings for all the motor speeds. This information should be used for reference only. ONLY TRAINED SERVICE TECHNICIANS SHOULD ATTEMPT TO MAKE MOTOR SETTING CHANGES! The Motor speed settings are set and confirmed when the individual axis menu is selected. In the Motor Speeds menu, each axis can be moved for testing, and if necessary, the speed values changed. This allows each of the movement parameters to be altered, ramping for beginning and ending (F; delay between steps for starting rate), (R; delay between steps for final rate), (S; acceleration or ramping speed). Once these settings are entered the Motor Speed menu will allow the user the check the settings. The settings are: Speed...this is the final speed of the motor. Initial Rate (Initrat)...this is the plunger's initial movement speed. Acceleration (Accel)...this is the speed for beginning (accelerate) and ending (decelerate) motor speeds for the balance of the motors.
19
275 (of 550 ) 2006(-2016)
276
9.0 External I/O Connections The Cobra L/S has a 25 pin "D" connector on the rear of the cabinet for External I/O connections, i.e. GC Ready, GC Start, Data Start, etc. The following is a list and pin locations for the signals. Note: The Cobra L/S is supplied with an External I/O cable that will be specific to your GC system however, not all functions shown will be wired in your cable. Be certain the cable you received is correct for your system, see Figure 9.0 for complete cable connections. Pin #
Signal
1. 2. 3. 4. 5. 6. 7. 8. 9. 14. 18. 19. 20. 21. 22. 23. 24. 25.
Signal Ground In 1 Ground In 2 Ground In 3 Ground GC Start N/O GC Start N/C Data Start Com Auxiliary N/O Auxiliary N/C GC Ready Input GC Start Com Data Start N/O Data Start N/C Auxiliary Com Spare Out N/O Spare Out N/C Ground 5 VDC Out
10.0 Remote Control (RS 232 Serial Link) The Cobra L/S can be Remote Controlled through its Serial Interface Link, labeled "RS 232." This may be accomplished in either the "Remote or Local" Mode (this is programmed in the Methods). Commands may be received from either the Host PC or the keypad, however the keypad is LOCKED out with a message on the on the LCD while the PC is programming. The Cobra L/S is started by a signal generated by either the GC Ready signal, the Host PC or the keypad. The Cobra L/S requires a 9 conductor cable to Receive, Transmit and Ground, fed straight through. If you do not have a cable consult the factory. Plug the cable into the 9 position "D" connector on the rear of the Cobra L/S labeled "RS 232" and then into the 9 pin serial connector on the rear of your PC.
20
276 (of 550 ) 2006(-2016)
277
10.1 Data Format The Data Transmission from the host to the Cobra L/S and from the Cobra L/S to the host use the same data format. Communications are RS 232 as follows: 19200 baud, no parity, 8 bits, 1 stop bit and no handshaking.
10.2 Command Summary from Host to Cobra L/S All Commands require 3 bytes, followed by a CR. Shorter commands should be padded with a CR to make them 4 bytes long, total. Q
Get Cobra's attention (Cobra will stop running, and echo ok) and print "PC Host active" on line 4 of the LCD screen. When the PC host releases control, "PC link Idle", will appear on line 4 of the LCD, if the Cobra L/S was idle, otherwise, the run will continue from where it was interrupted, unless an Rn or Gn command had been issued by the host. Note that parameters updated with the MWn command will not take effect until the batch is started the next time.
Attempts to communicate with the Cobra L/S while it is performing a manually initiated rinse will be ignored. After the Cobra L/S has responded to the Q command, the following commands are available: Note...For commands with a method parameter, the examples use method 1. In the Mode After column, remote indicates the PC Host stays in control after the command is executed, and the Cobra keypad is disabled. Local means control has transferred back to the Cobra. Command
Example
Mode After
MWn
77 87 01 13
Remote
SW
83 87 13 13
Remote
Rn V0
82 01 13 13 86 48 13 13
Remote Local
V1
86 49 13 13
Local
MRn SR ST
77 82 01 13 87 82 13 13 87 84 13 13
Remote Remote Local
GO
71 79 13 13
Local
Description Program method parameters (requires parameter string to follow) Program system parameters (requires parameter string to follow) Start running method n Turn off Verbose mode, no status messages will be sent while the Cobra is running Turn on Verbose mode, "PC Host active" LCD message changes to "Linked to host" Request Method parameters for method n Request System parameters Request Current status. One of the following series of two binary bytes, followed by CR will be sent: 1-10, 1-12 0-Running method, sample 0, 101 - Manual mode, 0, 102 - Idle Resume running if a method was interrupted, or return to local control if Cobra was not running. 21
277 (of 550 ) 2006(-2016)
278
GN
71 78 13 13
Local
AB
65 66 13 13
Local
Q
81 13 13 13
Remote
27 13 13 13
Remote
Resume running at beginning of current cycle, after dumping syringe contents to waste, or return to local control. Abort current method, dump syringe and return to local control Echo "ok", useful for synchronizing with Cobra, works to establish communications initially, and does no harm if communications are already working Return cobra to local keypad control, and continue method if one was interrupted (Same effect ad GO)
For both Rn and Gn, the Cobra will transmit "Run Complete" CR when the method is complete. The system will wait for a keypad press, or any character over the serial link, and then return control to the Cobra. A remote program will have to re-send Q to get back to control. All commands should be terminated with a Carriage Return (binary 13). All method #'s (n) should be binary, not ASCII value, i.e. 77 82 49 01 for MR1, except the Rn command, in which the n can be either the ASCII equivalent, or the binary value, i.e. 82 01 13 13 and 82 49 13 13 will both start Run 1. 10.3
Cobra L/S Command Details
To program a method remotely from a host PC: 1) PC sends a Q to get sampler's attention 2) PC waits for ok, indicating Cobra is ready 3) PC sends "MWn" CR, to indicate method is to be programmed. 4) PC waits for ok CR, indicating the Cobra is ready 5) PC sends the following binary string, all word (2 byte) values: Byte#
#Bytes
Content
Allowed Range (PC code must enforce these limits)
0 2 4 6 8 10 12 14 16 18 20
2 2 2 2 2 2 2 2 2 2 2
First Vial Last Vial Num of repeats/sample # of rinse ones # of rinse twos rinse volume Rinse fill rate Standard Volume Sample Volume Num of solvent dumps/inject Num of solv. flushes/inject
1-120 1-120 1-100 0-20 0-20 0-100% 0-100% 0-100% 0-100% 0-10 0-100
22
278 (of 550 ) 2006(-2016)
279
22 24 26 28 30 32 34 36 38 40
2 2 2 2 2 2 2 2 2 2
Sample Fill Rate Sample dispense rate Syringe Offset Prefill Air MidFill Air Postfill Air Start delay (seconds) Pause before sample dispense Pause after sample dispense Target
42 44
2 2
Pause after sample fill Operation mode
46 48
2 2
Cycle time (secs) when Opmode=0 Seconds till auxiliary relay closure
50 52
2 1
Link to method # on method completion CR
0-100% 0-100% 0-20% 0-100% 0-100% 0-100% 0-999 0-600 0-600 0-3 (0-A, 1-B, 2A&B 3-A+B) 0-60 0-1 (0-continuous, 1-GC trigger) 0-999 0-999 (clock starts at cycle start) 0-10 0 for no link
6) Cobra will respond with ok 7) Host sends Rn to start method n. Cobra will respond by starting method. For example, sending R1 (binary 82 49 13 13) starts method 1, whether or not it was just programmed. To start Cobra in Verbose mode, where status reports are sent while running, send the V (86 49 13 13) command first. 10.4
Program System Parameters
1.
PC sends a Q to get sampler's attention
2.
PC waits for ok, indicating Cobra is ready
3.
PC sends "SW" (binary 83 87) to indicate system parameters are be programmed.
4.
PC sends the following binary string:
Byte#
#Bytes
Content
Allowed Range
0 2 4 6 8 10 11
2 2 2 2 2 1 1
Right/Left Final Speed Forward/Back Speed Vertical Final Speed Plunger Final Speed Plunger Initial Rate Plunger Acceleration Normal Acceleration
0-999 0-999 0-999 0-999 0-999 0-255 0-255
23
279 (of 550 ) 2006(-2016)
280
12 13 5.
1 1
Vertical Acceleration Tray Size
0-255 0-3 (only 0 currently supported)
Cobra will respond with ok.
10.5 System Errors Undefined commands will get a response “Undefined command” All parameters must be in their allowed range, Cobra will not edit incoming values. Cobra will wait for an enter key press (ASCII 13) to continue after an error.
10.6 Error codes #1 #2 #3 #4
Undefined command Invalid value Not yet supported Current run must be aborted first
11.0 Cobra L/S Installation of Cables and Mounting Hardware The following section details the Cobra L/S mounting bracket hardware and I/O cable installation. Refer to the drawings for detail.
Terminal Box "D" Connector
Remote I/O "D" Connector
Power In Receptacle
TERMINAL 24VDC 2.5A
Remote Control Serial RS 232 "D" Connector
REMOTE I/O
RS-232
USE APPROVED POWER SUPPLY ONLY
Figure 11.0 Cobra L/S Rear Panel
24
280 (of 550 ) 2006(-2016)
281
11.1 Installation of the Cobra L/S to the Gow-Mac 600 Gas Chromatograph 9 4
2
6 5 7
3
8
1 14
9
10 11
14 13
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14.
12
GC Oven Top 6-32 x 1/2" SH Screw W/ #6 Lockwashers Left Mount Bracket 10-32 x 1/2" SH Screws W/ #10 Lockwashers Bracket Mount Block Cobra L/S 8-32 x 1/2 SH Screws Keypad Terminal 10-32 Square Nuts Right Vertical Mount Block Right Bottom Mount Block M4 x 20mm Screws 8-32 x 1/2 SH Screws W/ #8 Lockwashers 10-32 x 1/2" SH Screws
25
281 (of 550 ) 2006(-2016)
282
11.2 Installation of the Cobra L/S to the HP 5890 Gas Chromatograph 1
12
2
3
20 14
19 16
17 4
18
19 5
15
6
18
7
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20.
Cobra L/S Autosampler Keypad Terminal Box GC Injector Cover GC I/O Cover Left Bracket Support Right Bracket Support Right Bottom Support Side Cover Vent Clamp Right GC Side Panel Side Panel Bracket Support 6-32 x 1/2" SH Screws 8-32 x 1/2" SH Screws 8-32 x 3/8" SH Screws Boss Extension on GC 8-32 x 3/4" SH Screws Keypad Terminal Support Left Tee Slot Block 10-32 x 1/2" SH Screws 10-32 Square Nuts 8-32 x 3/8" Flat Head Screw
13 12 11 8 9 10
26
282 (of 550 ) 2006(-2016)
283
11.3 Installation of the Cobra L/S to the HP 6890 Gas Chromatograph
1 6
5
4 4 3
11 10
2
12 7 13 14
8 9
1. 2.. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19.
Cobra L/S Main Unit Keypad Terminal Box Keypad Terminal Support 10-32 Square Nuts Left Support w/ Brace M 4 x 20 Screws 10-32 x 1/2" SH Screws 8-32 x 3/8" Flat Head Screws 8-32 x 3/8" SH Screws 8-32 Thumbscrews Tee Slot Block 10-32 x 1/2" SH Screws Mount Plate 10-32 x 1/2" SH Screws M 4 x 20 Screws Right Support 8-32 x 1/2 SH Screws Right GC Mount Plate Right Mount Bar
15
16 18
17 19
27
283 (of 550 ) 2006(-2016)
284
Appendix: Syringe Operation Drawings
PreFill Air Syringe Offset
PreFill Air Sample Volume Injected into Inject Port A -or- B
Sample Volume
PostFill Air PostFill Air
Example 1 - Standard Injection Setup
Example 2 - Syringe Offset Used
PreFill Air
PreFill Air Syringe Offset Standard Volume MidFill Air
Injected into Inject Port A -or- B
Syringe Offset Sample Volume PostFill Air Prefill Air Sample Volume
Injected into Inject Port A -or- B
Sample Volume PostFfill Air
Inject Port B Inject Port A
PostFill Air
Example 3 - Using Syringe Offset and Standard Offset
Example 4 - Using Syringe Offset and Inject Mode = A&B
28
284 (of 550 ) 2006(-2016)
285
Use this chart space to log in any method parameters that you must use on a frequent basis.
29
285 (of 550 ) 2006(-2016)
286
r
I
This article, published in the August/September 1992 issue of Environmental Lab, is reprinted here with the expressed permission ofthe author, Richard J. Mealy and Environmental Lab magazine. - SRI Instruments, Inc.
286 (of 550 ) 2006(-2016)
287
,..
~.L.......,act 0 e • ration on • Data Re-e va l uatl ng the calibration process to meet more restrictive
requirements for litigation quality data. By Richard G• .Mealy and Kim D. Johnson
T
tory programs, inc!wJing the 500' ;md series ...( EPA methods. those put>. lishedin SW...,3.l.6.' :.tnd the Conll':ctLabo- i ratory Prcgram.' See Table l fo r :.l I summary of cahbrauon requirements or" I the various regul;uory methodologies. [n eenerct, the 6lX) series of methods offers the least am o unt of guidanc e. and thus islhc most open ro individu:liinter" ,' pretaiion, MeR: recent revuices to the 6CJ(}=
-"-
he ~ibr:uion process represents the: irutiaJ controlling mechanism (or the generation of qual ity cbu. yet there is .1 general lack of guidance: reg:utl.ingspec::ificevalaaucn techniques foe this process. One of the drawbacks of providing such JilIlcguidance is the potentiDl lossof ~ comparability, one of d1e chief data quality objecti yes identified by the EPA. This article !:.'tmUnes critic:l:l aspects of the c::Lljbr:u:ion process, .w:l identifies those features that. if overlooked, can signific.1ll11y impazt the quality of the dat:l generated, lnitially. .1 compariso n of c:1Iibr.1tion precesses, as outlined in the variom regulatory ~ is presented, To provide a more focused scope. discussion is limited 10 the impact on rnethod.s for the analysis of vclaale of! :m.iC$. pesricidelPCBs and semi volatiJc: orprlla. The concepts can be extended lO od1c:r :lna.Iytic:l.l mettlods. It is important to note: thal some of the issues raised here have: been.::t.ddtessed in regu1:J.lory programs Ihllot W~ nOl evaluated speciflCl1lly for [/)is article, The USA TItA..\t1A progr.un in paniculill'"tw i nco~ a requirement that cali m uon dam. be subject to statistical tests for both Zero In(l:rccpt Olnd Lack of Fit. w hich serve to resolve some: of the ;nobIe.:ns :1UOCi:lIed wuh nonline:1r data;ux1 calibration tr sereepc.
COMPARISON OF REGUI.\TORY APPROACHIS TO C.\LlBRAllON There exists a. great deal of diffe rence in the caiibeanon protocols and requsremems of the key regula-
I
I
500 series of methods for analyses con" , ducted under the Safe Drinking Water AC'lISD WAI program introduce several new requirements ttw provide greater I control over the aCCUJOlCV of Ute resultant ca.libr:won. As Table 1- indicates. wide vananon ex ists in ce numbcr of ctlibr:1cion scnda.rds required both within and across the series of regulatory protoco ls. One particul:llly important assumption tim the 500. 600 and SOC()l series :Ll1 siure relates co curve lineanty, In txh of eese melhods. if the percent relative smn&rd deviation (%RSD) of response factors associated with caJ.ibratioo stan-dards is within certain criteria 110 to .35 percenti "tben lin~ d1rough the ori- gin can be assumed" Clearly. there are widely ranging views ~ ng when me inte:t::epl of a caJ.ibr.ltion CW"\'e oeviares signific:lntly!Tom me origin. Inkeeping with the goal to establish data compar.lbilil:y. there is a needto consider the inenrperaticn of a statistical teen- , Rique to provide an objective means of , determining whether :l particular set of
I
d,;ua
essentially has a zero
in~pl
In the event that %RSD criteria emnot: be ccnieved, tbree of me four pr0-
grams allow the user to simply prepare a
calibration "curve" from concentr:1tion vs. instrument response. Vofonunate1y. there an: no requirements for the type of curve .:t.Igorithm flinear regression. poly. nomial fit. etc. ) allowed. Ascleanepcrireriaccnrinue roe volve, this v:uiability between the diffemnregulater protoco ls C:IJl have significant, adverse impacron the comparabilityof data generaed by laboratories. Due to either ~orsite"~ifiepreferences.;ma·
lyncal programs can be base d on methodologies from any of these programs, While e=noftne
p~ tsccnsid e red
I
10 be aeslgned to prod uce quali ly unaty ucaJ euu. the differences between the cali- l
287 (of 550 ) 2006(-2016)
288
bration jX'OtOCOls will ~t in significntly ditf=t d:ua quali ty. (n orderto provide more cc eeot over the pn1ibnuiOD process. eacn element of t1•.; processmusrbeconsideredso that the
mwn number of data pointSn::quim1. As Ulc: minimum number of points required to form a Iineis twa. then a line:lr~ sian (1st order polynomial fit) aetu.ally requires a minimum of three data points to be signifie:tm. Similarly. with each
rnost~eornI:rin:ttion ofelcmcnts
tol' ( e.g... in GOMS). single pointqu::mtitation (muJ.ticomponenl :uWyteS sud1;u PCBs,. <1Od multiple painE C1Iibr.uion "curves. Of these approaches. single point quamitation has the ~ l patential for irw::ruI3C)' because the response
is employed. The basK: "pons- of !he cdibr:uion ~ shown below:
Tablc I: CQmparison o f rerulawry mcdlod rcquiranel\U tot" variowI
M
._-- ...$._".$--_-..... ....- ......
• numberof c:ilibr:uion levels • cdibmriou algoritllm • c:l.b1lntioa Icvds • cl1ibraDon. :.cc:epance aiteria
500
proc=s..
-
8000~
600
,-
,-
£.:0 _ _•
E-. _ _•
.._._c. 'r.;:0CM0
NUMBER OF CALIBRATION
_ _ OF ~C'l't
LEVELS
-
,....,._.... m,_
I' • •
--~
· E..- _
GI
· E--.. _
GI
.~.0000 S _
_CM ' . _.. RIo ",•• 10.-
_RF
of !be c libnJJOlI
-.... -._- ._--""'.- -- - - ..... ._--._--_w_._ --------_.--_.---,._---- ,-- - ,---.
• effca or"~g'" rcwine:s The rcnainder of thisarticle focuses on detailed :wlysis of each of these sececes, In pon;enlar. _ especs """ potentially lead to inaa:urate or biased data:ue discussed. In addition. we identi~ of the mefhods thal: are open to intcrprttatiooorrequirefurdJe:rglridance
cm_
~
~
'0'Jl0 15On
~
Xl'llo iS2S1
• lO'lIol5OW.UoII
.-.-\lSI ••o-'"'IQCJ ."
~ to'llo IlIOl ,lICZ._ • J5"o 1~62:!il
~ 20.5'10 (GC. 'OIORSCl _ _
• 10 ¥'OA
Es.se!:ltiaUy. as the number of calibraDon Ievds incmJses. the rdarive risk. is reduc:ed.asabeaerpialae ofthemalyre·s performana: is otxaincd. The anaIytiC31 ntn.Qme is also an impoctant consideratioDindetc:nniningthenumberoflevels to employ.Foranalyses with a relatively sbon;malysis Iimc. such as the majority of inorpnic parameu:rs. additional Q)j.. br.1tion IC'vdsdo nocrepresem aburdenlO producrioo.1hisisDOttbecase.howeveI'. fa- most organic ana.Iyscs. witb routine:
nm timesol40 to 60 miDurr:s. I...abor.uotics art: engaged in a eeesam sttug&lc between quality :uJd pmducrion. While ~inacasedDWnberofcalibratiODlcvcls
would impnwe !he quality of !he
It
c
"
et::If ...
•
•
CCCY)
,
en-
anaIym to develop a calibra-
Don algtrithm. a wide may ofno nlinear c:l.b0nt00n tedmique options are avail3b1e. these opions. including ~lyoomiaJ fits, exponential;md power'cun'e5. segmerued filS aod even specific manu-
factUm" options. are routinely provided as part of the software bundl ed wi th instrumer1t da.ta Stations. The mosl common approac!"les [0 quamitauon useanaverage response fac-
.,
_.1$'l1o"'_
:111'11<_
_ _ '-D_25"JI.
t.2Cl': 125 oc_ _
from the single samdani analyzed is deemed 10 be representative of the linear· by of the araa.Iyte iJ:s quc:stion.. There :lte two sources of error in single-point quaririwion. Ftm
is designed
~ioo
~--1~5Z& .R!I
~-
CALIBRATION ALGORrIHM WhileIJXlQ laboratories default to the
.... a_
'lIioo'r l~
a2lJ"',: 5CIUCII
.,-
smndan:1 (least squares) method oflincar
~--
-
witb.amiDimumofdalapoina:uebrought light in the next few sections.
to
.~-_.
Tbc use of an average response factor eo normalize differences in
response factors over the calibr:u:i.on range. 'The drawback to dtis approach is if only a single response factor deviau::s signiflcantty from lhe others.. the bias is oormalized by disaiburing an equivalent
degree of bias in me
~ ~on
over the Olhet sWK1a:ds. Nonlineatdai.a~morem:l vanced
st3listical tre:UInent. Typie:tlly. regres..ions cf a higher order. quadratic eqlJOltions or polynomial filS of the data art:: em ployed. The main prtt:lUtlon 3SSOCiated with lhese techni qu~ is the mini-
higher order equation. ODe more dam point is n:quin:d. As witha simple linear ~ the correJalion cocfficicm musz not be: used as a ~ oflinearit)'. The correIaDoo coeiIicienronly provide:s a measun: of how well !be dala pointsfit the equation genc:rmcd. Fmally. as the degree of DOr1Jinc:lrity lccreesee, the curve of a 2nd or 3m order polynomW boa>ma ponbolic lFi..... l, 2) . Thisresults. at the upp:rendoftbccum:. in two solutions for a given daIa point. Unlesslheacmalc:urveiscarefuJ.ly evaluated. the analyst may DOC even be awan: !hat muJ.tiple soIutioos are possible for a
givenrespcnse,Thcconscquenccassoci·
-
ated with this type of situation is that !>ignificantly inaccurate data could be Essenliall y.alinc:lr~onnsults
in lhe cqualionfora5tr.aight1ine. .....hc:reu polynomial fits above me Isr order will result in the equation for :l curve. The
most recent versions of 524.1. 524.2 and S2S. GCIMS methods for the anaI~ of volatile and scmivolatile organics. specifiC1lly ~llow the use of 2ndor 3edorder
288 (of 550 ) 2006(-2016)
289
iIr:;::;::;:;:;;;::::;:;;:;:::::;:;:::;r I
I
! :
"
_ . r.- ~ _
",~U"' I, S>mploo D3u s... J . COnl,","_ 01 L,neo,r
,"""""n ..... :A
i
S ~!
J
from all five d3~ pointsyields acorretaticn coefficient of 0.963. If only the first two :1nd the uppermost d:n:I. points :n used f 10. ~ and :0:». however. the cce-etanoncoefficient is iocreasedrc 0.999. Th.is isa consequenceoftheoenvauon of
~ion ~U3 ri ons
if the response fee«xcatenac:nnot bemet. fi ~ 3 shows the CW"\"d thmare associated with a linearfit as wellas po lyn omi3.1 fitsof orders
1
Zthrough5 for-Sampte DaU1,&t#I .Nole. in p:u11eubr. me signific ull differences in the curve tit: to me d:U.::I in the region
,
!e vel s tandard is signific:JJltl y ~lertr~ . the detection limit. then cccurccy in the , proXilTUry of the deteaion limit is com- :
promised. -ecause linearity of response . bas not ben evaluated in this region. Ultilrotely. the detection limit itself may , come int o qu esti o n. Whiie the m.1joriry . or the regWawry methodsspectfy th:!.cthe low. lev el ~ must be pre~ :ll:l. concentration "near. but above, ce detecti on limit.- methods 524.1 and :5242 allow the to w-le vel standard co ncentra (jon to be :IS muchas tu umes higherthan
#2. the linear regression ca.!eulated
_.
,.. ..... " ...-..
..
i
!
c on r:mge. Methods 524.1 and 5242
require:n1e:lsr. U=e alibr:ttion lewis to encompassafuctorof2OCIlibr:3Iionr.mge (i.e; I 10 :!D. 10 to ZOO). In addi rion. at leas t fout standards are required to cover :I rnnge of a fuctorof50.:md at 1e:lS1fi ve smnd3rds are required fer a range f3CtOr of 100.
....
~oo~
for colibrarion can have a significant im-
pact on the validity of the canbranon equation. Dlibration levels should be ~rablished
based on consi de:rution of: I. the ran~ of the levels. 1. the reporuble detectio n limitand 3. the lmear ram:e of the :llInlytdS). Tlle maJonry ot theregulatory progr.tms revieWed provide littl e gui dance with. ~pect to the romge of ,
~i br:mo"
le vels. A lre ner'lC u:ltemenl is
i provided indi::::lting -thai the le~ls sc·
, ~~
,
~_COE'"
l.00E o
O.OOEo
,,
,,
, ,i , ,
,,
'
the samples. Revisiom to the 500seriesofmethods i represent the tim artempl (odl er rhan the ' CI.P program, where c:Llibrnrion levels are contractuallv defined) to provide r stronger guid:1nC~ reg:ltd.ini the calibra- !
I
The specifi e levels that are selected
J
me consequences that can result from ' est:Iblishing calibrationIevelsbasedsolely i on the expected concentration range of :
·· _bW
H 1OE o
I
Final lv. anatvtes have cereczorspecific; Ii~ ~ges. In order 10 :lCCUr.nd y evaluate noruinQl' regions of the C1Jn'c.1:flere muSt nor be a signifiCU11
identify :1 par:1boJiccurve. This is one or
....
CAUBRAnON LEVELS
the detection limit.'
difference between the uppe rm ost Stand:ud (X) and me tx -nccoceneance level. 1bc conseqUCIll;C of nCl( considerin g this in :tc:ilibr.lr:ion is thzthe usermay fail m
'I<>J
;: . between points 0 nnd E. If !hese higr.e:t'" level curves are used formeSample Data ~ i. .. .mE:... ~L serious inaccuracies would resull.:!t e the upper rangeof the curve-cne recom• mended range for sample qu..:l.lltitation. . Whil e. in specificc:ues.~h of th= , - - 1,-." - r" , St3usti~ manioolat::ions of calibrancn j d..:I..c COIn provide .:l ""hetter fl r" of the -:3libr3rion eq uation to the ctl.t:I.. they can alsc ha ve signir"'ic:mt impact on the qual. ity of the data generated, Essennally. with the number of sutistial pro~s the ccrrelauca coefficient. ~Iy :tvU1l:bIe..:m equaooneen be found The retanve difference between the th.:I.l: will provide:l mathem:l tic:l1 sol ution concentration of the lew-level stand3:d u.e.. ""fit, to any set of data.. Couse- and the repocubledetectionlimit is crmr quenn y. without a complete understandc:Ll IO providingconfidence in the :lCCUing of me :u:tual effect on the r.:IW data, rncy of low-level measurements. Bias is noneof thesesl3IistiC1J tectmiques should mote prcrccncedas the calibrationcurve be used in the genernrion of d:1t3 for approa:hes!he detection limit foca par~ compliance.
I
Ccnseqcenuv. if the low-
t icular~;:U Yle .
ceec uie working linear range of the detecror. Inmeinterestofob[;1.jning accurare resots. il is more importanl rcoertoe the linG]( range 01' me JJUlYle :mdIor instramer u, :md dilutesample: ccnce nrranons thaI exceed this range. A wide calibrauon range. based on only 3 tew calibrurion levels. w!ll nearl y ::Liways result in a cceeecon coefficient ~ dun 0.995. which is frequently used JS ;he sole ~br.Ition evaluation criterion.In me example ofSarnple Data
-4
- -. - , ,
, .. ., . , .,..
-
..
J
-
-
J _ Linew ~ .. ~
.
I
i
- - -2
Regr~ui on
o t
3: 3m order PoJ)'llOmi.oJ Fit 4 -!ttl on:ler PoIynocn>al Ml S= j th (II'On' Pol~al FII ~ : 03'..:1
I lee ted should be based on the C)(pecled
! range of sample results. In some C.:lSeS• . {h I: ··~ )( pected - :o;unp l e conce nrr:tions e.~·
289 (of 550 ) 2006(-2016)
290
--.
! C.u.IllRA110~ ,~ CRfITRIA
-'CCEPT.-\..~ cr
Onceacanbraccnbas been performed,
i
limned me:lSUle oi eonltCl! is oot.1lr.eti.In
crfe- I tmeassuranceor' :lo..T.J:::J1e OuanDO-
addition to ~RSD c ru ena, 'ne C~ pro21'"'..m has cst:l.blished mtnim um resccn se
ucn. The mOsl Stnnge:uCCV accepcance cruena are rcundin Meth od 50'2.:. which recuires me caalvs is or OJ. midpoint suncare 10 yie ld a response wilh:n - "0 per. ; ceuor th;u obtained for the~m1e st:Ind:L'tl :
I ttl~~US(be a serotcruena totietermino:
f:l.C1:Dr .;.., te.,. ,:1
,i dle CUPC is acceptaele lor usc in l::~ n _ ~tl.n~ :In:Li~'t1c:J resuus . This is <>ne o f
~UL~~J ISZSOC::ued ....iUl ccnriuence in lhe ai:nlity to de tect the cnalyre, liow-
I
t'or m05( :lI1cl:-re5. This
--, In addition, this metnod lhel.evwe~inUlc i~========~~~=============l i recuires the:malvsis 01 /; laborarorv iortifi~blank : of the Cl.Ppro" i fL.9U ' : J F ban:hof30 or ; , gra m. the referen ced I' fewer fortified memods have :'01 in t.i;e irntlou calibrauon.
~ pub lished r: g:u I3tOry I methodology. With the J
J
':Xc:epoOfl
I I
~gum ory
only ~Iished JCCept:lI'ICC cmeri.:t if the me:ln response f:u:tor is to be.
usedforquantiution .The
I
.,
:lJlel"l'I:IlJYe.lf 'iRSOcn - ,
."
vrau cn of response
F,.....
II II
~j
."
teri:l l rd::m.ve ~ de·
r:xrors from the clibc::l.· ricn curve l canaoe be achieved, is to sim ply
~~
" ,
0
,
. . c.__
u
10
;!J
,oj .: , c"-:-=-."..,.,~:-:::-:-:-:: 0 I D ;c ~ "", ~
......_
,,-eo-, n ~ OI, ,,,
gene~ :l
~ C__
~ . _,,,,
pkx o( conc=:tcr.ttion vs, response or ~pomc f:JCOt'. This ::.JJows me ge1lCr.U:lon 0'- d.:U:1 without conU'OI of ~ qu:iliry unlil tne :ma.lysls of the rim
~e
..:on ti nu in g calibraaon S Wl~ wbere c
onumg
_ ,,, ,,,,,
,,,,,,,,,",,,_,,," , rlC>ml
ever. r.uher th:l.n in quantit:l.lJon or the JNlyte. As incti~ in Tabie I. even the
criteria:l.SSOC:ued wnn con-
~imaon
venficano n ICc¥)
l t~
sampl~
;l1
a ecoceneaecn of :0
,l lgfL
Fora setcf data that 15 essennen y linear. the , marhemancal basis of a i
Une:J11 egression aaemro ; to ~ lish the IlUdpotnt ~
of tile CW'Ve as the pomr :
I
t whicb. deviateS 1c:l.St from
the linear equation. The elttem o f the deviation then ina=ses:l.I the extremes.. The deviation is 3bsoIute ramer than mauve to co ecen tra uon, ""hie::! erenes the ~t impact:l.t ce [ow er end of the curve. Due to the mag-
i
; ; ;
:
,;
-...
I
rrirude of response associared wi d:!. tl::c higbcsl caibraaon level. the retacve ef... feel is rrunimaL In the esc of sD"Ongly nonli n~ dara, such as that in Sample Dara S<:t .-z. the point aJ: wh:ic:h the curve bccolnC$ nonline::lt f in this case, the: ~ per ctibr.u:ion level) is CCfll:r::u in me m.inimit.:ltion of deviationfrom tbccurvc. 1lri.s effect is ev1c!ent in To3ble .... which TU>lc .:A: Samll'l c Daza Sa I
X
Y
! , I 14OIlOO ssooo
I
Rnpgnv factor
65000
13000
10
1
saeooo
68000
4 5000
indi c;ues that n::larively minimal b;" ~lJ:Ithe upper e~b~on le vei..e ven ~ ns:d~ rin g
uece criten3 for me CCV :md lhc fortilied labor:Uory blanks C3D be met. The correlaaonccefflcient ("r") isthe most co mmonl y used staristiQi measure
RSD .. 1703"-'
-.
is asignific:u'llprobability ttw. the ~
of c;ilibntion =eptnbilliy. One long-
I 365000 I I ~OOOO
CCV is t)'pic:illy equal to the IlUdpo!nt conccne=on of [he ini tial multipoinl ,;:Llibraaon. Wilh line:lorc:::ilibr:1rionltypl.. C:I.IJy the oonn l. tbe aud:pottu: level is :lSsocimrrl witb the tease degree of bias fro m the plot of the c:.3librarion cquarion. ~nscquem.J y. iflbe overall nccoracy of the analysis is less man ZOpetttnt. tDl::m
rcooo
5
50
conce.:1tt':lI1On has lIS gre:ue5( impaa on the continuing c:ili"br.uion ven ficancn (CCV) process. The ccnceecaecn ofthe
suciI. nonline:J1' d:ua. The .-=I:wonship be:we:n bias :llId
sunding anscoac:eptioo is that this ~ ramerer also provides :l mezure of !ine:uity. The corretanon codfiClcrn: is :l me:l.SUfe of the ~goodness of fit" of ;:I
I
mum of 1.00). The maR: the data appe:1C to be r:mdomly dismbulCd. or the ellipse ,
I
appears more as acirele, the: lowertbe "r" value (to a minimwn 0(0). This effect is , Tolbk
X
.:.B: S&mptc 0aQ. Sel
Y
Rrspony
I I '" 50 I 3.650 .00 I 100 6. 800.00 I 10
'00
f'ador
650.000
65000
1.'100.00
70000
9 .000.00
I
I
~
I
I
II
13000
I
I ,
68 000 45000 RSD . 11.J~
,
:;cne:lofdaul poinlS. Basic:J.lly. the COITC_ l:won coefficient c:m be viewed as ;:I
illu:st:r:UCd inFigure4.Conscquc:mIy. even n:sult inahigb: - ("value if the c1ata r.mge issuch that the data c:m be described by a tight d li!"<.
matbemanc:l/proeess~detennines \he Uglltest ellipse: th31 dcnncs
CJ!ibrntionacc:pmncecrite:riashouid ' be Ce$lgned to eva.l\We :he
The more me ellipse ~ b les .:l.slJ'aignt line. the higher ':.'te " (" value (to a maxi-
between the inle'fee";K of th e c;ilibr.Hion
::J. particular t'3Ddom set of daI.a em
~onship
~wwon 3nd ttle r:ponaolcd=onlirnJ.t
~
! I
I ,
290 (of 550 ) 2006(-2016)
291
, I
~ ROLl. TheWIOl in Tables 2.~ and :B . for
Sarnt ne Dat:lScots 1# I ;md#2 show slgnltiT..; lI: J; C.k:~ .'( u ""c::; lor $..lnplc ~ Sa ! ll$J n, IJOIn u n= R ~_ , LSR I~ LSR ,"el;h:n1 1lX.
LSR
X 1
,
,
10 ;0
I
LSR 1IIX l
I
-1.1
0..
I
0.7
~O
I
6.7
I I ., I
13
I
'.9
13
ce rtai nly
~
upper range only mirumallv. While ext! ofthese techniques results in .\ better fit of the d.:1U pcmu 10 the calibration equation. &.ey remain little more th:ll1 ~ manipulaoon le=i1niques. I In the generauon of t:nvironmenw.l WL:l.. ! analysts must be trained to understand mat the use onn ese techniquescan result in misintet'preUtion of lhe &u. I
not an de ment o r the .:.:LIj-
I
bration process. their usc is l":lpidly becorning -o uu ne. Hi¥h -powered calibraucn :1lgorithms:lremcsrcnenused Without understanding the m:1thematical funccons behind them as well ;J.S the
I
Hmuauons to their use and impact on J particular d..:u3 set. For this reason. ui ese tec hniq ues are discussed here.. One of the most routine sortware options .1~Jable is ~ of ."fon:'.ng- the curve through lheorigin. Tbecrencally.a blank should yield no response for a particular 3lla1yte. Due to sign:l.1-to-noisc
-e
Q1I1 neg:1t1Ye bias :1t the low end o f the
cahbranon rr.:lS required b~ most oi me ~gul~ry methods . the low- level sun~ isjust slightly grc[UUl:m the 3CtuaJ
RDL thenthe ROL. would clearly nOI be valid for these c:ilibration sets. One re-
[n:l. regub.lOfy c1inu te l:t1al:1S
co~ider:uions. however. this is r:uely the C.:l.SC. Because many .;naJysts have been :r.tined that .1 curve shou ld ?3SS throu gh the origin. this opuon is selected,
There ;iCC two ways in which curves C:l11 be torr ed through the origin. The first is ::I simple m:nhem:ltic:l1 fonnub designed to result in a slope .:IJld zero..intereepl. The ccer option is a manual one. which
there is a need for more structure :JJld guidance in the ~vallUltion process in order to provide analytical memocs thaI ensure data ccmparabiliry. ::J
iryof d.:n:1 [cmegenernred. Consequently,
quimnent thou should be imposed on C'..1Jibr.lf:ion d.:lt:l. is th.u the 't.- intercept Iexpress ed JS co nce ntra tio n ) should be no gn::Iter than 50 per- Table ..: s..m ~o ,· l/lc _~ in~O:Iu Sct I ~ ....ns cent of the RDL This will mini- l1i1f=n'IiillIl Hjgb!!O) I One rinal conslderoDon ~
ing the evaluation o f calib ra uon data is the bias:lt e:tCh calibrati on leve t thar results fro m obtaining :1 J concemra ucn from the calibraI uon evarcaccn using the 3CtUa.I raw c.:t..libi.loon dala. The son-
I
wareinu.setodJyprovidesgraphic
I
representations of the calibration data. but the plots are typical ly
1
1 66~)
"',.." I ,..
I ( l~) 1
I
17%
10
1
"" II ""
""
f1 '1P)
I
~
I'"'' I "6'>..
5
lJ'io
'30'> '1
,"".. 1I ,.
f4 ':l-)
I
..
I
~
I
' 6'>
7..
62%
'" ,I '"'
SI ':iP
IZ%
I JIS}
fl4~1
,..
RF ." ~II: .._FXIOf' LSR .. ~~ It-SquanJ I 1'f": .. Pol......... ia1 FIt l~d orderl
too small and the resolution 100 poor to be used 10 accuratety evaluare po int-specific bias. Each of [he gener.illy accepted cal lb rarion evaluation mechanisms should be conside red no morethana single data assessment tool. rather than an absol ute indicator ofcali-
bration acceptability. For example, the ccrrelauon coefficient. used freq uently in the inorganic aren a.can prov ide misle;u1ing intonnano n if there is a s ignifj . canl r:u1 ge between Ihe uppermost an d lower calibration levels. EFITCT OF ClJIlVE ~IOOTIDNG'
1206'ilol j
,
ROlTl1NFS
\Vim the :mvent of powerfu l sofrware routinesand instr'.mJenu±u.:l. stations. tte analyst is now provided wilh OJ serres or tools that C:ln be used to ··smoo th'· the tit 01 lily ~ u rve. While Ihcse lcchniques
inc:c.s-- 'j
ingly concerned wnh qualiry :lSSUr.1I1Ce. most doIU1 qwU.iry assessments remain , reacti ve in th::n they rely on qU.:l.licy con. j trOl infonn ation generated .:lurin g the C~ at ::uulysis.. rnther than prior- to the .JIU1ysis or envuu runcnu.l samples. The caibranon process should be vewec as the initiJJ oppommiry 10 assess me qwJ:
RJchanl(l. MeaJy IS me SUiJeMsor of quality assurance at Warzyn. Inc.• a consulting engineenngfirm wirIJ naOona/ :xeser;ce. He bas
I I
I
been mowed in !he er.vrroomental testing incJusrry for 11 }'ears. and hascoordinatedQUaiffyassurance
aetNiDes at t1Iret major laoorar ~ nes for til e cast seven years. Kim D. Johnson 1$ an-3CCOOl'lC ~ WIth ,\fiowe:$t.. an erMronrnent;N~. She was fotmertf me diI'eCr:Jt of J1IiJ!}fJCaJ serviceS at wan,n. frr:. SI'!e haS
ac
morerhSn13years of~in
is based on the repetitive inclusion of (O.Oldata.points unnJ UleCUl'V'C tseveam-
~ and sen-eo in ee role of labotarory rnatJa&ef at c\oo iEbOtalO-
:illy rcreec throu gh the origin.
res over ee past 10;ea:s.
techniques an: oflen used to obcin a becer fit of the data pOInts at either extreme ofthe cali bration range. Typically. the lowendof t:he curve is susceptible 10 poorfit of tr.e calibration equ.mon. 'The most common weighting rouane e mpl oyed to improve the fit is a 11
errvirOnmenrai
CU1""'C -weigi"ring"
X manipuJaaoa of the data. Basic:illy.
each da ta point is weighted by :l.faewr of the Inverse oC the associated conu:nlf"dtion. The ~ult of this weighting, for the ~ntire set of data. is a 91-point cu....·e vs. the original five-point curve_'The results ot tl-.is weighting :l1'esum..-na."ized in Table 3. The fable mdic;ucs tIUl:,J si¥nific:Ullly better ti t is achieved ::lt the low end of lhe cu.;.·e while ::ufecring the midpoint and
REFERENCES l. u.s. EPA. 198&. :-Aetllods fa- (he Detar:nna.lioo of Orpmc Compoullds ill Drinking Wale". fJN 600-4-30039. ~ba. :. U.s. EPA. 198S••~ forlb:: 0rpU: Q emic:Il AIWym ofMIItIll:ipiJ aold Iocbsa-iaJ Wua: _ lcr• .:o CFR?:In 136. Appecdi.t. A. ;uIy. 3. U.s. EPA. 1990. Test Memoas tor EvaJuJrilIg SoIid WaslC. Vol~ IB : ~MWl.iIi..f'hy.I i o;clICllcnuc:ll MellloCo.. SW-&46_1m M... ReY,,1Of1
J. November.
U.s. EPA. 1990. Conuxt ~ ~!l=ll SOW390. StlIeme:'lI of Wort for ~-l:JC .w.J ~ ;es, .\falu-Meci.l. .\1u Jti.("~'tE- :.bIt:I. 4.
5. L"S"'nv...>,tA. 19QO.lJni:ed S13~ A.."1T'~ Ten-it :tnd H~ ~.3ICl"'.ili ;,, ~. Qu.1Il':'. ·~·I :llICC f'ro!=n. USA1'HAMA t'.... M 11 -:'1. = .0. 13"",,",.
I J
"
291 (of 550 ) 2006(-2016)
292
DDD~~ Hayes Separations, Inc. Bandera, Texu 78003
Post OllIe.. Box 1614
Analytical Polymers
POROUS POLYMERS Since the development of porous polymers for use in gas chromatography by Hollis and Hayes in the mid 1960 's, very little has been oone to improve their performanc e. Commercia! polymers suc h as Porapak" iind Onromasorb" have been availab le since th is tim e tor cnromarcqrepmc use. However these comm ercially available polymers have been plagued with proble ms such as batch-to-batch variations, incomplete or inadequate cleanup and shrinkage. These variations and inconsistencies in production and hand ling have led to poor performance and reproducibility.
HayeSep!l analytical polymers and pa cked columns are now available to cnroma rccraphers at a reasonable cost. Ha yes Separations , Inc. takes pride in provid ing the necessary technical assistance to supocrt our users. We gua rantee that our polymers are better tha n any other on the marke t and we are continuing to develop and lest new packing s tor specific separation problems.
-.
HayeSe p~ po lymers are tho roughly cleaned and preconditioned tortwelve hours und er oxygen-free nitrogen before packaging. T hese handling techn iques produce polymers whien are consistently the same , w ith no shrinkage and minimum bleed. Columns packed w ith HayeSep~ requ ire minimum conditioning .
FAX (1l3ll) 796-4655
(1l3ll) 796-4S 12 Muimllm SUrlace
Tap~
Po"",,
Bulk
"'" .-. Density
H;yeStpl! Opnt.llg
PoIymM
T....
mJIVnNTI
A
165 'C
526
Po""'"
Composition"
(1=1ownt 9_highesl)
DVa
7
0.356
(high punty) EGDM (high p unty)
B
e D
190°C
60S
0.330
DVB/PEI
8
e e
442
0.322
DVSlACN
6
795
0.3311
250
0
290
0
DVa (high purity)
N
165'C
405
0.355
OYBIEGOM
9
P
250"C
165
0.420
DV8IStyrene
3
Q
275"C
5B2
0.351
2
R
25O'C
344
0.324
Dva DVBJNV2P
5
S
25O'C
583
0 .334
OVBl4VP
4
T
165'C
250
0.381
EGOM
-
10
'0Vll EGOM PEl
-"
Aa;
Ethyleneglycold~tl'I
NV2P
Pdyetl'lylene'mine
.VP
N-vlnyl-2.pyn:l11idinonll
4-viny\-pyriCl Joe
~~ A Thls polymer sepames permanent gases(h)'drogen. nitrogen, oxygen. anpl . cal'tlon rl'lOf1ClUde. and nibicc;WdeJ8l ambientb:lmpsratutes. It also exh ibits good separation characteristICs for lhe C2 's, hydrog en sulphide and wa ler al higher temperatu res.
~2
,
F..... '
PERMANENT GASES Column: 36' x 1I6w pacIl;ed
PERMANENT GAS STANDARD 500 ppm Column : 25' x l mrn packed wkh Haye$eV' A
witt! HaysSep- A 8MOO """"
Column TelTIt'; 25-
'7IY.!OO "'"'"
Detector : P.E. 900 tc 225 rna
Column Temp: 23"C
M . x 218O"C FIcJot: He 23 ccImin Sample: 25 rt'IicroWtrs Ar
sample;
~
•
He 15 cclmin 20 miCtOliters
plus Hydrogen In
, ,. ....,
,-2.
'-
, """"'"'
1. ~5foI, NIJ'OgIn ~
4, Ar;on 0.5'11>
..""'"""'""
6. Ca1bon Monoxide
So cartIon MonoIliOol 33%
•
,
-
,
•
_..
•
292 (of 550 ) 2006(-2016)
293
HayeSep' a Designed 10 sec e -ete t ee Cl a nd C 2 armoes as wen as trace leve ls of amm on ia and water Ih,s pol ym er el,m,rtalCSm e " eea lorcau 5!Jc wastlt Jl'g 01 mlll enll Jpnor 10 pac k;"9
~'9U I'I! 3
AMINES #1 Column; 5 ' l( liS " SS packed w ith
•
HayeSep- 8 BCVtOO mesh Column Temp : 140" up 10 19O"Cat 16"C1mrn In,eclOr TemP: 150"C Del ecIDr: PE. 900 T-C.
•
•
175m/l Alt, .. 8 180"C Flow: He 30 c:c/m m $ampIe~
Fig u re 4 AM INE S "2 Colu mn : 5' x 1/8" packll'O WIth HayeSeo' a 8CI100 m esh (;Qlu mn 7em~: 140"C up to 1 90~ a t 16"C1mll"l I n~llX Temp: 150"'C oeece- PE. 900 T-C. 175 ma An. x S lSO"C Flow . He 30 cC'min $ample: On-cQjumn injo£!oon
•
•
•
0.2 lhCroliter$ w.~
'"'=.
injection
•
I
I
I. AIr 2. Wate r
'''''--' '---.
•
'So
A. 2. _ 3.Elhytamo...
E!tll'lent ~ ...
\
-'
•
j~
• """"""'""
-.
•
_. ..
•
HeyeSep<" C ThiS polym er is d esig n9d lor polar hyd roca rbons such as hydrogen cya nid e, ammonia.llydltlgen sul phide a nd Willer. HayeSep CS' has similar separation.ch.aracter isrics to Chromosol'tJC 104.
,
A..... _
,
AMMONIAIN HYDROGEN SULPHIDE Colum n : S' .. 1/8 " packed witI'1 Haye5ep8 C 8J(lOO rne$l'l Column Temp: 7O"C Inject>r Temp: 200CC Oeleaor. P E. 900
..
Figure 6
•
TRACE AMMONIA IN WATER
...
Column; 5 ' .. 1/8" SS packed with H.-ye$@p"' C
.''''0'-
COlumn Temp; 115"C Injector Temp: 1~ Det~
rc
P. E. 900 T.C. 225~
225~
An. .. 21SO-C FJow: He JO cclmin
An. x 2 18O'"C
,_.
Fh,1W: He 30 celmi n Sampje : 100 mic rtlliters
Sample: 1 mie:rnlitM
1. A.. 2. CattJOn Oiooooe
,._-
' A~
I . AI.
2. CarbOn Dcaae
4
sec """
w.. r ,-,
.... ,
' hl:e 1: appro:- IS'll> " " - 2: lIDP":- 15'lob
--
I. Iw.
,
5. Un"""",," in
l . C iIIllUn Diuo.tdc
, ................ I.~in
, •
..
.,
.... .....
""""'"
•
,
•
293 (of 550 ) 2006(-2016)
294
H~~ ~ N, P, a. R, S, and T These poIymef'S a~ mte'Chal"lC}eablewith t1'Ie Poapai(!' series Iorseparatioosd kJw'"lOlecUMhalo9_n s. sulptlUfS, wal t' alCO hols. glycols. free fait)' ac ids. esters. keto nes a nd aldehydes.
,
Figu~ 7
8 SOLYENTS Col um n: 8 ' )( 118" SS packed
AMMON IA CoI ;.am; 8 ' ,. 11S" 55 paci
,,
with HayeSe;l* P 6OJllO mesh Co lum n Temp : 800C up to
"""m""
Co'umn Tem p: ec"C
I
18O"C at
In,ectol Temp: 15QGC
•
~
Flow : He 30 cc/min Sam ple: 0.1 microli!e
NH..<)Hwilll on-
'rfeCIiOn
•
I ,
16OClmi!'l l !'lject or Temp; 150· Ma!'lifold Temp: 1800C Defector: 175 rna 2QOOC Flow: He 3C ce:tmin Sample: 0.2 mrc:rolilefS with on
Manifold Temp : 180"C Detector: T.e. 175 rna 2OO"C
column
•,
F'9U~
>gil: malena 's con:aomng
,
,
1. Ail
,_
2. wa.!eI" 4. E!haIIoI
1. A_
S. Acetone
2 . Ammono8 3Mb 3. Water65%
6, CM\ol'OIOOTT
,
;
_... . . J... _
, ,
•
. ..... 10
FIgu~9
....... GAS Column: 10' ,. 118" SS
TRACE WATER ANAlYSIS CoIU1T'1'1 : 9 ' )< VS" N , Paet
packed with
with HaY'l!Sep' R
HayeSep' R
aMOO rnes"
eo-
Col l1ffln Temp : Flaw: He 30 ocImln Sa mpl e: 15 microlite rs
Colum'l Teqlp: 118"C Flow: He 30 CClmin OwIector: varian T.C. writ!
Bend~
,
OIl-Line
Process Analyzer Sample: 10 rnic:rolileB
Ethyl ChbilM
•
•
,
, --
.,...... ."
NT
r
:1 Carbon CbIOe
1. /VI 2 _
12 ppm
a
HyCroqen C~
4
Ethyl~
•
7. p ,opedioo ..
I,
a
MMht'I~
,:
. '
.
294 (of 550 ) 2006(-2016)
295
Fiqut1t 11 HYDR OCARBONS A ND SULPHUR GASES Column- S' )( 11S" pacr.ed wi th Haye5ep ' 0
Flgu~
12
<2', COlumn: 5' )( 118" 55 packed with Haye$ep ' T Column Temp: 32"C Detector; All. )( 216 1BO"C Flow He JO wm,n Sample; 50 microliters
SO/lOO me5h
Column Temp: 900C Flow: He 3C ~l n
,,. '" -..-
-
. ...... 3 ...
c.n:.:w. Doidlt
•
Et~
, a a
7. Hydrogen Su/fJde
Car1x>n:tl S<,lifde
,pB.
•
"
lOP_ n , Propadie...
--
0
Rgute 13
...
lOE1'HANOl. .. ~E
....
Cotumn; 5' )( W' 53 .."..,
.Eth~
;
..J
•
l_v~ .. • ,,
F..... 14 FORMALDEHYDE
Column: 5 ' .. 118- SS paekIId wrttl ~5eP'" T
""'120 '""'"
"_T 1001120 mesh
~mnTem p :1~
Il'JtedOr Temp; 165" Detecto r: P.E. goo T.C. '?S MA
Column Temp: 120-0 lnjeaor Temp: 132GC
DlMdor:
M~han.
Cal'llOn Di<:llritJe;
•S. Etnar>e
~ LA "
!
."
ee. 900 TC.
Alt . .. 32 18O"C Flow; .... 30 cdmin
'225 me. 1!>()4(: Aoor; He 30 cetmin
Sample: Q2 m lCTOlders
.
•
............. •1. e.__
"-
1. Ai
"- "'QWllilIII'PI~ .
.CO
......... 2.
Fal'~
p ,-
.'"
1. _
,
_..
295 (of 550 ) 2006(-2016)
296
~ I NTRO D UCI N G
A UNIQUE NEW PRODUCT
Compari sons of D Formulations
HayeSep@0 This new polymer made Irom high purity d iv inylbe nz e ne is unavailable anywh ere else . It has a high
surface area and higher operating temperaturesman competitive po lymers. Ava ila ble in to ur differe nt porosities with surface area s from 790 to aver BOOm 2/gr am . this range al lows flexibi lity, since in water/ethane separations porosity determines the order of elution.
A_..,.
Bulk
Oitlme'llll'
C. _tv
!m;c, onsl
gram{cc
Surf..:. Area
PotosiTy 'l&
m 2f ll." m
The se D fo rmulat ions exhi bit su per ior separation characteristics for light gases. Significant sepa ration abilities incl ude t he se parat ion of CO and CO: from room
air at ambient temperaturesandthe separation 01 acetylene prio r to other C2's. HayeSep~ 0 is particularly useful in IMe separation an d analysis of water and hydrogen su lphide.
F"tgUte 15 SCOTT MIX 237 Column: ZO' " 1/8 NI packed
Dip
.0317
.3283
69.1
774
o
.0308
.3 311
70. 35
803
.0332
.3334
64 .2
781
FIgUre 16 GAS MIXTURE
H
Col umn : 10' " 118" SS poc ked Wlth Haye5ep" 0
witl'l Ii.,.~ 0
"'"""' ......
>en "", ",.."
Column Temp: 2S'"C InjectorTemp: 100"C
CoIu m n"TemQ: 8O'"C
InJedor Tempe14O"C DeledOr: P E. 900 t c
Oel:eaor; P.E. !KIO tc
,
'I
225_
225 ma l4O'"C Flow: He 30 cd!ni n
Att,
SampIO: V31ce vatw
l< ..
Flow: HE! 30 ccfl'llin Sample. Vak:o v;Ji~ 100 microliter.;
50 mll: fQlllel'$vapor (ambErll) 1. NI1109'"l ibllI;~J 2. ~ygen ~ All d :1 Cilbon 1o\cn::D.!Oe 1'll:l AlI.8 4. - . . 4,S4ii,
S. CaIt>otl 0.:..0. 15"lt
All ,,4 AIt- ,, 4
1
!'MtOge<> (t>oIlan<;e1
c"rQ(><>
2. o.c..oOIll ~ 3. Nllrous Oxoo. 311<0
;
-
.....,.,
L. .
..
Wa\rlf Q.511
!l
~~3'llo
J JL II
296 (of 550 ) 2006(-2016)
297
I Figu~
Figu~
17
Column: '10' x 11ll- SS packed
Column: 20' x 118- Ni packed
with HayeSep# 0
-..tth~ D
10>'120 ...... COlumn Temp: 40"0'2 mn
10M"' ...... 6O"C ISQlhe'"ma! Detector: 3700 varian FlO Range: 10 - n Att. x 16 Flow: He 35 cctm ln
Column
•
""",.amm
'8
C1 • C2's
SCOTT MIX 216 (PrognImmed)
141" 11O"C al24"C1mn Injector Temp: 100 "C
T~:
"
Derec»r. P.E. 900 T.c. 225 rna l4O'"C Flow : He 30 ec/mI n $ampl e: Valoo valve 100 microlile~ (ambiem)
._ .........
•
I . No\fo9I!'\ (balance) 2 eatt>otI tr.6onollode l'llo ~., M . •d 3. Me""" t'llI 4 . c./'tIOIl Oooio
...
7.
e".,.. I""
1. Melha... ,....
...... '" 2. btyIen.
~d
3.
M .x2 ~.,
I~
E~ l'"
J
•
;
","",,'"
Flgurtl 19 C1 • CS PARAFFINS Column: '\0' )Ii 118- SS
--
TRACE UNSATURATES
.
C2. C6
•• • ,
•
HayeSe~ 0 l OOi'1 20 me sh
.
•
pac ked with HayeSe~
0
1001120 nw 5h
•
Column Temp: 120"C ~'D200OC
Column: 10' x 118- SS
Column Temp: 12O"C up 10 200CC at 24'C'min Detector. 3700 Varian FlO Range : ' 0 - 11 Att. x 16 Flow: He 35 ccfmi n
at 2Q"CImin Oeteetor. 3100 Varian FlO Range : 10 - 11 Atl.. lC 16
FJow: He 35cc:lmin Sample: VaJco 'laNe 50 nWen:Jliters
1. AalIylAnll 16 ppm 2. e~ 15 ppm 3. ~ 14.3 ppm
4
~15pprn
~
""", _14.1$ ppm 6. ~ 16 PQ"1l
.
--
•
, ...... """"
1. MtIfW-. a1ll94....
a 4.
!l.
~
•
Q.1019'ICI
e.-- 0-1019"11>
&~~ --""-
,
.
, ,
,
.... .•...
,
•
.
,
...
.. ..
"' '
,
•
..,
•
297 (of 550 ) 2006(-2016)
298
flgu rw21
Figure 22
TRACE ACETALDEHYDE IN AIR 2500 ppm
TEQUILA HEAOSPACE Column: 3' )l 11a· 55 Q3Cked .... i1hHaye ~ D
--
Col......,: 3'
tIB· SS
)l
8D'12O mr.;h Column TItmQ: 100· In,ectOr Temp: 140"C [)elect or: P.E. 900 rc.
"_ 0 100/120mesh
Column Temp; l00"C ~ Temp: 14O"C Defeaor: P.E. 900
225
tc
225
,,
rna 1.q)OC
Flow: H e 30 a :lrrun SamPle: ValcovaNe 100 miCf1)j,tefS
m. l4O"'C
Flow: He 30 ceh'nin Sample: Valco valve
100 InICdlers
"
, l. Ail
' ''''''' ......... ._".. . ,.....
Alt. • ,
2, CarbOn DlOlude Art.x l
,
IW
'2. _
2SOO ""'" !"d .)
- •.
-....
J(
"'"
.
•
_...
F1guN 2. HYDROGEN SULPHIOE Col umn : 10' )l 118~ Ni packed
A.... 23 TRAC:f: ALCOHOLS INWATER Column: 10'
"',, '" "'""
W" pac ked
WIthHayeSepC 0
wi!tt~ D
100'120 ""'" Column Temp : so-c Il'1lectOf Temp: 1oo"C
8D'1OO """"
Column Temp: 7S'"C up 10 15l)9C at 'S"C/mi n FItM : He 33 ca'min
Defector: P.E. 900
rc
225 rna 14O"C
Irfoaor lemp.: 125"'C
FJow: I"Ie 30 cclrnin 5ampl e: Yalco vahoe 50 miCroli1ef3 vapor
DetBCb": P.E. 900 tc
225m. An. J( 1 14Q-C Sample: 3 mi crolit ers
(a mbient)
•
\ •
_..
1 .1W~)
2. e-t>on ~ "AIftlI' 0.~ 3. .,... a;:.ptar ~ 4. HydogefI Sulpt.- ~ 2 Slob
•
.._....•
298 (of 550 ) 2006(-2016)
299
COMPARISON OF ° Do FORMULATIONS F~ure
25
TRACE ETHYLENE OXIDE
Retention Time in Minutes
IN NITROGEN Column: 10' 1\ 1/8 " 55 Pilckec:l witn HayltSeP ® D BOI1oo mesh Co lumn Tem p : 13O"C Injecto r Temp : l00"C Detec1Of: Varian 1400 F.I.C.
AIR
CM.
CO,
CzHz CzH.
CzHIl
H2O
Dip
0.9
1.7
3 .1
5. '
5.8
8 .3
9.0
DO
0.9
1. 7
3 .1
5.8
6.1
8.4
8 .6
An. Hi" Jl 2 14O"C Aow: He JO cclmin Samp'. : 250 m ICrol iters
DB
0.9
1. 6
3.1
6 .1
6 .6
8 .7
8.1
Valoo valve
' This is our stane.ra O. CcMumn: 1O' Jl v e- SS 8 0 1100 me lll
Column Temp: 4 S - C u etec tc r, 175 rna Alt. Ro w: He 30 ecm. n Sample : 50 m ero lit,•• V. lco V.lIv.
Jl
2 150·
.
-
, ,
,
Ftgure 27
Fig ure 26
HYDROCARBONS/SUlFUR GASES Colum n: g' x 118'" HayeSeo p 3 Dip 100/120 mesh COlum n Tem p :
-co-c
"
.
Co lum n Tem p : 25"C Injector Temp: 25" C
Detector: P.E. Sig ma 300 TCD Low current At! x t Flow: He 30 eclmi n Sa mple: 0.5 ex:
Detector : P E. 900 T. C.
300m. Att. x 2 14O"C JO c:etmin, 90 psig
A ow: He Sample: 250 microl iters Valco .........
V,1eo valvo
.....
-.. esc • 31st ,,. " .u .= •• eo'. , n <" '....... ,,•e <'. m ,w_
. ... .' " . ,.
~,
,~
•... .= n. , ~
,~ ,
,'
•
~
~..,....
1.1 '
,.~
NITROG EN IN OXYGE N Column: 30' x 118" SS P.!'eked with HayeSep8' DB
.~ .~
0"
O~
.~ ~
"".,~
"',.""""' '-
---
c.•,.,
,.
N~rogo ~
2
~ · 1>AJ"""
.,
,
,
. ,
299 (of 550 ) 2006(-2016)
300
--
......
Figure 29
Figure 28
AIH
SCOTT MIX 234
Column : 30'
Column; 30' x'1{8' 55 p!eked wi1h 'HayeSep® DB 1001120 mesh Column Temp: 25'C Injector Temp : 2~ Oetec:tor: P.E. 900 T. C. JOO rna 14O"C Row: He 30 CC/min, 90 psig Sample: 250 microlitel'1l Valco wive
.""""
~ ~
~.
__
Oioodde
118" 55 ~cked
"
1001120 mesh Column Tllmp : 25"C
injector Temp: 25"C DetllCtOr. P.E. 900 T. C.
""m.
An. J( 32 140"C Flow; He 30 ecJmin, 90 p$ig Sample: 250 microliters Val"' .....
1. ~fto 2. H!ln:>ll""' ''''
.""""
J(
with HayeSep@ DB
~...
~
All. ,,01 AIL " 32
AIl."a:i All. " a:i AIL
It
08
,. H"""P" 7'" 2. Clx)?on 21' 3. Argon
.
, , , , , , " " " " " y-
0'"'
., , ,
••
Figure 31 ETHYLENE AND SCOTT MIX 216
Figure 30
NITROGEN IN ARGON
-
Column: 30' x 1/8" 55 ~ with HayooSep® 0 1001120 mesh Column Temp; 25"C Injector Temp: 25"C
DeteeIOr. P.E. 900 T. C.
Column : 30' It 1/8" SS packed with HayeSep@ DB 1001120 mesh Column Tllmp: 12O"C Injector Temp: 12C"C Detoctor; P.E. 900 T. C.
,
r'-
300m.
ecc m.
Att. It 1 140"C Row; He 30 ccJmin, go psig Sam~: 250 microlitllfS
Att. J( 1 14O"C Flow: He 30 c:cImin, 90 psig Samplll: 2SO microlitem VaJco .....
verec v alYfl
,
---
.
•
1. ~
, """" ,. • """" •.....-
•
~
1. 2.
7.W_
-..goon 373 _
,t.rgon. _
.
..
-
• •
~
L-
.I : ,• ,, •• ., •, ,,
-
'-
, , , , , •
• • " " " "
300 (of 550 ) 2006(-2016)
301
Figure 32 NITRIC OXIDE IN NITROGEN
Figure 33 HYDROGEN IN HEUU M
Column: 30' • 1/8" 55 I=:acklld ....rttI HayeSe p l3 CB
Colum n: 25' • 1/S" SS pack e d With HaV-s.piSl 0 10Cl/120 mesh Column Tem p: 2~ Injector Te mp: 25"C Detector: P.E. 900 T. C. O. 150 ma It l4O"C R ow: 24 CCJmin N2
100'1 20 mesh
Column Temp: 22"C Inj ect or Temp; 22"C Detector: P,E. 900 T. C. 0, 225 ma l4O"C Row, 30 ceJmin
,
Sam ple : 100 microliteB
Sample: SO microlillil'fS
V _ ......
'-
,
,.-
,
,
•
,,
,'--
•
Figure 34
Figure 3S
IMPURmES IN HYDROGEN
AIR IN ARGON CohJmn: 30' • 118"' SS ~ke
Col umn: 25' x 1/8" SS paekecl with Haye Se p@ DB 1001120 mash Column Temp : 25'"C Irl~ Tem p: 2S"C
with HayeSep@ DB 1001120 ffilil'lih
Column Temp; 22"C Injector Tem p: 22"C e.-aor. P.E. 900 T. C. D. 22S ma 14Q"C Flow: He 30 ccJmin
Deteetor: P.E. !lOO T. C. O.
225m. Row : He 25 or;:Im in Samp le: 250 microlile~
,
Sample : 100 microliters VaIcQ valve
vacc valve
,
, ,
, ,
I'
,,
_..
, , , ,
•
, , ,
•
301 (of 550 ) 2006(-2016)
302
.'-I Fig ure 37
Figure 36
HYDROGEN/AIR
50/50
9' .6% OXYGEN
,~
Column: 25' ~ 118" 55 p ac keo
with HayeSep@ 0
1001120 mesh
I,
Colu mn Tem p; 2S"C Injector Tem p: 25"'C Detector: P.E. 900 T. C. D. aas rna 140"<: Atte nx 8 Flow: He 24 ccsmn
~,
Colu m n: 30' x 118" 58 packed with HayeSep® DB l 00112{l mesh Column Temp: 22"C Injeel or Tem p: 22"C Detector: P.E. 900 T. C. D, 22~ rna
I, ,
, I II,
14O"C
Flow : He 20 ccJmin Sample: 100 emercnters Valco valve
Sample: 50 miCroliters Valco ",alve
.-
1 . ~"
2.
N~ rogen
, e.,,-
~I
•
,
•
, •
- ,.
I I I "
•
~
•
F'lQure 39 IMPURITIES IN NllROGEN TRIFLUQRIDE
Figure 38
99.995% ARGON Column: 30 ' II 1/8" 55 Pi\Cked with HayeSep@ DB
Colum n: 25' x 118" SS paclled with Haye5ep@ DB
,
100' 120 mesh Column Temp: 22"C Injector Temp: 22"C
100/120 me sh Column Temp: 25"'C Inject~ Temp: 25"C
Detector: P.E. 900 T. C. D. Z15 rna 14CrC Flow : He 30 CC/min
Detector: P .E. IlOO T. C . O. .225 rna 14O"C Flow: He 3C CC/min $ample: 100 m iCtOlit&rs
Sample: 250
..
miCfO~ters
VaJco valve Chart Speed: 1 emlmin
Valco val".
.-
1. N" ' - '
'.""'" .....
a.
c.DonT~
• . _ _ TIII_
,
, ,,, e
1
o
J
I
I
l
,
I
,
I
,'-;--
"
302 (of 550 ) 2006(-2016)
303
Figure 40 FAST ANALYSIS
Figure 41
Column: 48"}{ .()C" 10 55 • paekltd wrtl'I HayeoSeP~ 08 1001120 mesh
Coklmn : 3:1' x 1/8" SS packed
Column Temp: 70'C
Column Tlmp: 22"C
99.7-" CARBON MONOXIDE
"'6"}{
.....th HayeSep3 DB 100'120 mesh
,
Injec:1Or r.",p: 7C"C [)etector: P.E. 9CO r . C. C.
Inject or Temp: 22"C
DetK1gr. P.E. 900 T. C. O. 225 ma t4Q"C Row: He 30 OO/min
22S1NI14O'C
Flow ; He 16 ceJmin
$.ampt. : 100 microliters
Sam pl e: 10 microlilers V~val ...
,
,,. ~•
f\I"r<'g en
-
Valoo
..... ..
- _.
,....""Cott>on _
,~
,
,
ea.-- eoo- 1'"
"
na..
,~
• I
~
,,
Figure 42 SCOTT M IX 234
, , ,,
,:,
, "',,""n •
M,r'Ktt• •
•
,
Column: 30' }{ 118- 5 5 packed wit h Hay" Sep' DB 1001120 m u h Column Tem,,: 22 GC J"",eto . Temp: 22·C Oellctor;P.E. 900 T. C. O. 2 25 rna 140 °C
.,.,...., .......... ,•.""'"" ..
Fl o w ; N J 30 ee l.....n
Sample: 100 mU:.o6it e rs Valeo va ive
•
,,
l
, 'l ""'f"....
Jl
,
to
303 (of 550 ) 2006(-2016)
304
POROUS POLYMER MICROPACKED COLUMNS Hay es Sep arations, Inc. has been making porous polymers for ten years . We have occasio nally made micropacked columns for vario us customers as well as sup plied pac kings fa r th is purpose. A few ex amples of t hese are listed on the f ollowing pag es. Of int erest is th e elution ti me of acetylene relative to eth yle ne and ethane. Figu re 43 shows acetylene between ethylene and ethane; Figure 47 sho w s acetylen e beh in d ethyl ene and eth ane; Figure 46 shows acetylene in front of ethylene and et hane; Figur e 48 shows rapid elution of impurities in methane . Ref erences fo r the productio n of po rous polymers are list ed below .
1) Hollis . O.L . Analvt ical Chemist ry 38: 309-316 (1966) . 21 Hollis . O.L. and Hayes, W.V.. J. Gas Chromo4 :235-239 11966}. 3)
Holl is. O.L. and Hay es. W.V., Gas Chrom., A.B . Littlewood , editor, The Inst itu te of Petroleum, Rome , 1966, p. 57-74.
41 U.S . Patent - 3,357,158 December 12,1967. 5} U.S . Paten t · 3.458,976 August 5, 1969. 6l 19 66 IR 100 Award (R& D ma gazine).
Figure 43 SCOTT MIX 216 ' + MAPP GAS
Figure 44 MIX 234
scorr
Colu mn: 10' X 1/1 6" " .0 4 pa cked with Ha yeSep· S 1001120 mash Colum n Te mp: GOoC 3mi" UP to 90°C at 8°Cln'Vn Oetector:P.E. 990 T. C. 0 .22 5 rna Flow : He 14 ee /min Chan seeee : 1 emlmi n S.mplc: 50 n'V crohte rs
Colu m n: 20 ' x 1/ 16 " x .0 4" SS packed with Haye Sep " O 100/1 2 0 mnh Column Temp; 2 5"C DeteCtor: P.E. 900 T. C. O. 225 rna 14 0 · C Att . x 4 Row : , 3. 3 cc/m", He Chart SplIed : 1 cm/mjn Si!IrJlple SIn: 25 rn crolitcrs
.,
,
, , • 1. N1uogen 2 . Me thane J . Carbon Dioxid e 4 . Ethylene
5 . Ae"'tylene 6 . EtlunA 7 . Propyle'" 8 . Propa ne
9 . Propadiene 10.Ml'Ithyac.tyl ene
,• An llnuatlOn
• 2
.. • ,
• 1. Hydr0ll"n 2 . Nitrogen
4% 5% J.Oxy~n 5% 4 _Carbon Monoxide 5'li> 5. McU14".,
5%
6 . Carbon Oio:lCi
5%
LL.i
-----r>f ', O
'
2J
· ~ M,_
.
'
e
304 (of 550 ) 2006(-2016)
305
Figure 46 SCOTT MIX 216 Co(UflV\: 20')( 1/16 ")( .04 " 5 5 packed w,th H. ye 5 epC 0 1001120 m n n Column Temp: 10' Isothermal Oe1e ctor: P.E. 900 1 , C. D.lt 225ma
Ffgure 4 5 MIX 2 16 PROGRAMMED Column: 20 ' ll' 1116" II .04" 5 5 packed with Heye Sep e 0 100:1 20 mesh Col um n Te mp: 25 · C 2mn up 10 1 10 · C .at 8·CllTlln
14O·C Att. )( 4 Flo ... : 13.3 e clmi n He Chil n 5pe8d: 1 em/min Semple Size : 10 microliters
Oe lcetor : P.E". 900 T. C.::>. at 225 rnlI 140· C Att. 1l4 R ow: 13 .33 ec!mrn H"
Cha n Soe ed : 1 cmJmin S e~" Size : 25 ITIICrotile rs
, '"
1. Nitl'ogen 2 . Carbon Monoxide 1 % 3 . M",than e 4 . Carbon Dioxide
'"'"
'" '" '"
5. Ace tyle ne 6 . E1hv'",ne 7. E1"-ne
,•
•
, ,
,I L.--
j• ,,
/~ , , , ,, , ,, , , •• • •U"'"...
,
10 11
,,,,,,
.
•
,, ,, ,, a, •, •,
M i.........
,
•
, ,, ~ T •
48
FAST ANA LYSIS Colum n: 4 8 ' )( 1/ l e " )C .04" 10 55 pa cked WIt h Hay. S. p· DB 100f120 m esh Co lumn Tem p: 70 · C lnj. etor Temp : 70· C Oet""10r: P.E. 900 T. C. O. 225 ma 14 0 ' C Row: H" 16 c clm in Sample: 10 mi" rolilers Va leo va lve
Column : 15 ' " 111 6 " " .0 3"
p. clr.ed with Heye S.p" A 1 201140 me s h Column Te mp: 4 5·C De te eto l :V ICI rnlero T. C. O. 120· C )<
,,, ,,, ,,,
!blllaneel t , Nitrogen 2 . M,tha". 3 . Carbon Dioxide 4 . AcetyieM 5. Eth yle N 6. Ethane
Figure
Figure 47 SCOTT MIX 216
Art .
,
8
Flow : He 8 eclm,n Ch" n Spello : 1 l,;r n/m in S. mple Size: 10 microlite r.
z
,, (bel. ne e) 1. N'tr og efl 2 . Me thanOl 3 . e.tlon Oio.uo.. 4 . Etflyl.nl 5. Et/WM 6.Ace~
'" '" '" '" '"
L
__r ':',' , , I)
1
1
'-f;......'""
3
, 1. Nitregsn 2 . Me1tIane
3 . Carbon Ooo JOd e 4 . El harwl
3 .0%
3.5 %
•
,
2.7% (b,ajance)
j ,
~-"
305 (of 550 ) 2006(-2016)
306
HAY ESEP RT'S RELATIVE TO C2H.
6' X l iS"
S5
Columns
HayeSep 801100 mesh
60 1lC · 30 cc/min . Helium Courtesy: Brien Thompson. Varian
Compound
A
B
C
D
DB
DIP
CF. CH. CO, N,O
.13 .0 9 .54 .62 .63
.10 . 12 .3 2
.08 . 11 .4 7 .59 .45
. 10 . 11 .3 1 .42 .5 1
. 10 . 11 .30 .4 2
1.03 .64 .7 5
.64
. 10 .12 .30 .4 3 .53 .64
F116
C,H,
.44 .49 .6 5
C2 H.
1.29 .8 1 .81
NH,
1.58
F13
1.10
CzH,
1.00
H,O H, S COS . F22
7.06 2.06
1.45
1.00 5.3 1 2.20
3 .02
2. 5 9
3 .10
7.63
3.1' '''
C,H.
4.7 0
C3 HII S O, PO
MA CP F12
5. 90
SF.
IC. 1 • 380 F" 4 NC.
.6 5 .71 .71 .9 0 1.00 1. 14
1.21
.84
.6 8 .70 .90 .8 7 1.00
.52 .62 .68 .70 .6 5 .88 1.00 .95 1.3 5
.6 8 .70 .98 .90 1.00
6.34
1.08 1. 3 6 2.56 3.30
2.58 3.31
1.10 1.39 2.59 3.35
3.75
4.41
4 .0 1
4 .11
4 .10
4 .9 4
4 .4 3
4 .70
4 .73
4 .84
10 .23
8.09
4 .7 0
7.83
5 .02 5.71
5.31 5.80 7 .03 5.89 6.79
3 .67
6.19
3.84 4 .63
17 .92
14 .7 3
16.2 1
6.38 16.74
4.84 3.82 4.8 7 4.96 5.32 6 .47 17 .18
24 .94
16.00
22.93
18.62
19 .10
4 .79
4 .92
5.1 8
3.68 4.90 5.00 5.26 6 .46
27 .35
18.35
21 .46
21.48
22 .11
17.32 19.48 22.88
23 .60
19 .33
21.21
22 .26
22 .66
23.0 1
306 (of 550 ) 2006(-2016)
307
RELATIVE RETENTION TIMES
Ethane = 1.00 Columns 6 ' x 1J8 55 65 °C . He 30 cc/min R
Compound
N
R
5
T
. 19 .2 1 .23
.2 1 .25 .3 3
0.3 0.52 0.59
.3 5 0 .8 5
0 .78
0 .78
1.0 1.0
0.87 1.0
0 .9 2. 1 1 1.0
6 .8 1. 73
4.12 1.87
Q
H ydrogen Air Nitric oxi de
0.2 3 0 .25
. 14 3 .18 6
0 . 17 0.2
.2 1 7
0 .2 1
M ethane Carbon dioxide Nit rous oxi de
0 .30 0 .71 0.80
.256 0 .45 0 .57
0 .50
Ethlyene
0 .83
Acervtene
1.4 1
0.74 0 .74
Ethan e
1.0
1.0
W ater Hydrogen sulph ide H ydrogen cyanide
Car bonyl sulphide Sulphur dioxide
Propylene
0 .19
10. 1
1. 45
2.1
1. 4 0 2 .3 1
19 .3
2.82 12.0 4 .66
0.2 8 0 .5 9
15.6
8.26
2.33
2 .46
3 .0 5
9.78 3 .4 5
17.8
3.20
2.63 3.6 5
19 . 1 2.8 8 28 .8 3.4 19.0 4.91
4 .66
3.67
3.8 8
6.50 9 .5
4.1 2
4 . 39
4 .1 4.7
4 .12
4 .8 4
5.14
11.3
.M eth yl chloride V inyl chloride Ethylene oxide
7 .43 14 .9 17 .7
3.93 6 .0 4
4 .67
4 .92
9.04
6.06
8 .7 8
9.7 9.7
9. 2 17 .3 23.3
Ethy l ch loride Carbo n disulphide
35.0
20.7
4 3.2
Propane Propad iene M eth yla ce tyl en e
12.25 32.4
19 .3
4 .63 7 .55
40 .7
307 (of 550 ) 2006(-2016)
308
2002 SRI Instruments Price uet
All pnces U S dollars
Te l: (310) 214-509 2
www.srigc. com
I I I
IPRODUCT INDEX -,
• LIQUID CHROMA.TOGRAPHS GAS CHROMA.TOGRAPHS
•
I
• DETECTORS AN D STANDALONE DETECTORS • IINJECTORS • LABOR
• MANUAlS • DATA. SYSTEMS • COLUMNS
• ACCESSORIES •
• ITEM
I
PARTS
TRAINING
I I !
DESCRIPTION
o
eaBvca -
~AS~ CALL
R/
0
PRICES SUB.JECT TO C H ANGE WlTHOUT NOnce -
TO C()Nnmt PRICING PRIOR TO R~LEA SJNG A QUO TATION OR ORDER
UQUID CHROMATOGRAPHS 0210-5000
MOD EL 2 10 ISOCRAnC MULTl-UNE UV HPLC S YSTEM
55,995.00
02 10-01 50
$3,995.00
8500-0025
MODEL 220 UPGRADE TO BINARY GRADIENT UPGRADE TO 416 CHANNEL PEAKSlMP!...E DATA SYSTEM UPGRADE TO VARIABLE WAVElENGTH UV DETECTOR
021 0-2050
HP LC INJECTION VALVE WITH REMOTE STAR T
0219-0200
BINARY GRADIENT SYSTEM wJ4.Ch. DATA SYSTEM . MODEL 210
$9 .995_00 I
8500-2000
REFRACTIVE INDEX DETECTOR
$6 ,495.00
867<>0090
LN/C ONOUCTlVIlY DETECTOR BOARD (REPLACEMENn
021D-4000
.-
I
$995.00 $4.595.00
I i
5895.00
I NEW
$495.00
I GAS CHROMATOGRAPHS 0110-0003
110 CHASSIS, 110VAC 60Hz
$ 1,795.00
0110- 1005
110 GASLES S EDUCATI ONAL CGO VIRTUAL OVEN GG, SERIAL
$3,995.00 DISC ON T.
0110-0 350
HYDROG EN GENERATOR MOUN TED ON MODEL 110 CHASSIS
0 110-2203
110 CHASSIS, 220VAC 50Hz
0 110·50 10
110 VIRTUAL OVEN GC CHASSIS. 110VAC 60Hz
$2,49 5.00 DISC ONT .
I I
$1,79 5 .00 $3,9 95.00 DISCO NT ,
0 110·5210
110 VIRTUA L OVEN GC CHASSIS, 220VAC 50Hz
$3,995,00 DISCONT.
0310-ססoo
310 EDUCATIONAL TCO GC, SER IAL CHASSIS ( NO COOLING)
$4,595,00
031ס-סoo3
310 GC MA INFRAME WI EPC , SERI Al CHASSIS
$4,995.00
031 0- 1000
310 EDU CATIONAL TCD GC. SERIA L CHASSIS (WITH COOLING)
$5,295.00
0310-1005
310 GASLESS EDUCA TIONAL CCO GC , SERIAL CHASSIS, NO COO L
03 10-1006
310 GASLESS EDUCATI ONAL
0310-1117
3 10 GASLESS EXPLOSIVES GC. TID
03 10-1 150 0310- 1151
13 10 GASLESS ETHANOL GC
ceo GC, SERIAL CHASSIS WICOOLING
$7.495.00
(CCD), ISOTHERMAL OVEN, SERIAL
310 GASLESS ETHANOL GC (CCO) , PROGRAMMABlE OVEN , SERIAl
031lJ.2203
1310 GC MAINFRAME Wf EPC, 'l2OV50Hz MODEL
861Q.O(X)3
18610C GC MAINFRAME wI EPC
86 1Cl-0004
061 0-0025
$o4,795JXJ $5.495.00 $4,295.00
$4 ,995 .00
$4 ,995.00 I $4,99 5.00
86100 GC MAINFRAME wi DUAL COLUMN OVEN S
:B61OC METHOD 25 GC CCH4JNON-CH4 HC)
I I
$ 7,495.00 . $10.495.00
I
Page 1 PL020 722 .xl s
Prices subject to d1ange
7/22/024 :56 PM
308 (of 550 ) 2006(-2016)
309 All pl"iCIij'i US dollars
2002 SRI Instrum ent s Price
ue
Tel: (310) 214-5092
www srigc com
186 10G BTEX GAS CHROMATO GRAPH . METHOD 5030 COM PLIANT IB6 10G BTEX GAS CHROMATOGRAPH . METHOD 5030J5035 COMP LIANT I 86 10G ENVIRONMENTAL GC (PID- FIDlDELCo-P&T) I 8610C MUD LOGG ING GC (FID-CCD) I B610G MULTIPlE GAS ANA LYZER GC - TCD 8610C MULTIPLE GAS ANALVZER TCD FlO METH I 86 1DC MULTIPLE GAS ANALVZER TCO HID 8610C MULTIPLE GAS'" SU LF UR ANALYZE R 8610G AIR MONITOR ING GC Q.14} 8610C MULTIPlE GAS GC II ITCm 8610C MULTIPlE GAS GC II (TCD-FID-METH) 8610C MUlTIPLE GAS GC II (TCD-HID) 8610C EDUCATIONAL AD GC , SERIAL CHASSIS 18610C EDUCATIONAL TC D GC , SERIAL CHASSIS 186 10C EXPLOSIVES GC (TID) I :86 1OC CFC GA S CHROMATOG RAPH W ITH TC D '86 1OC CFC GAS CHROMATOGRAPH WITH FlO 18610C GC MAINFRAME, 220V 50Hz MODEl 86100 GC MAINFRAME. DUAl OVEN 22 0V MODEl 8610C BTU GASANALVZER GC , TCD I I 8610C BREATH ANALVZER GC S610C BASIC CAPILLARY FlO GC I 8610C SUlFUR GC, FIDlFPD I 86 10C SPME GC I I
8610-0050 8610.0051 8610.0059 861Q.OOOO 861Q.OO70 8610.0071 861Q..OOn 8610-0073 8610.01 1. 8610-0270 86 1G-0271 8610-02n 8610-1005 8610-1 007 8610-1117 8610-1500 8610-1 510 8610.2203 8610-2204 861D-3070 8610-3489 86 10-5400 8610-5670 8610-5700
0 110-2007 86 70-2007 8690-2007
8670-0 150 8670.-0155 8670-1024 8670-1 025 8670-1029 0110-2026
. 'CCD CCD MOUNTEOON MODEL 110 CHASSIS REPlACEMENT CCD DETE CTO R ELEMENT CCO DETE CTOR
•
8690~2026
0110-0020
0110-00 10 0110-1000 011D-4010 0 110-2026
86~01S5
8670-1024 PL020722.X1s
$9.995.00 $ 12,995 .00 $13.495.00 $18,995.00 $20.995.00 $10.995.00 $13,995_00 $14 .495.00 $6.295.00 $8,295.00 $8,99 5.00 $6.995.00 56.995 .00 t $4.995 .00 1 S7.495.OO $9.995.00 'CHANGE $13.995.00 $7,995_00 $ 14,2 50.00 $8 ,995 .00 I
r.,
i FlO-DELCO FlO CERAMIC IGNITOR ElEMENT FlO COLLECTOR ELECTRODE CABLE W In; BNC CO NNECTOR FlO DETECTOR BODY FlO DETECTOR BODY FOR METHANIZER OELCO HEATER I COLLECTO R ASSEMBLY FIC-OELCO MOUNTED ON MODEL 110 CHASSIS FlO-D ELCO DETECTOR ASSEMBLY (Fl O-DELCO
$75.00 $30.00
I I
Page 2 Prices subject to change
! I I
$3 ,790 .00
,FIO-FPIJ MO UNTED ON MODEL 110 CHASSIS FID-PIO MOUNTED ON MODEL 110 CHASSIS FlO-DELCO U OUNTED ON 110 C HASSIS FlO IGNITOR FlO COLlECTOR ELECTRODE (REPL 861OC) FlO COLLECTOR ELECTRODE CABLE (REPL. M 1OC) FlO I NPD DETECTOR BODY
$300.00 $400.00 $300.00 $6,790.00 $4,995.00
$7 ,290.00 $5,495.00
FID • FlO MOU NTEO ON MODEl 110 CHASSIS
8670-0154
$11,495.00
$2.790.00 $75.00 $995.00
ECO DETECTOR
8670-0150
$19 ,490.00 $20,995.00
I
ECD • ECD MOU NTED ON MODEL 110 CHASSIS
8690-0020
I
$17,995 -1)0
$6 ,790,00
,
$7 ,285 .00
I
I
$6.790.00 I $75.00 I
,
$20,00 I S3D.lXl S3lXl.00
7J221024:56 PM
309 (of 550 ) 2006(-2016)
310
1\11
pncee US eenere
2002 SRI Instrument, Price list
Tel: (310) 2 14-5092
www srigc com
.
8670- 1025 868<>-0350 8690-(X)10
FlO DETECTOR BODY FOR METHANIZER EXTERNAl HYDROGEN GENERATOR. 50Ml.IMIN. VERSION FlO DETECTOR HYDROGEN GENERATOR. 8U!LT-IN FlO J NPO CONVERTIBLEDETECTOR FIDJOELCO DETECTOR
B690-0350
8690-1115 8690-2026
8670-0120 8670-1024
B690 .-o35 0
8690-1080 8690-2085
8670-0011 8670-0007 6670-9100 6670-9110 8670-9120 8670-9121 67Q.9122
,
NPO J FlO DETECTOR BODY INPD MOUNTED ON MODEL 110 CHASSIS INPO DETECTOR iNPO CONVERSION KIT FOR FlO FlO I NPO CONVERTIBLE DETECTOR NPQ.OELCO SERIES DETECTOR
01 1 ~ 15
0110-0080 0110-0085 8670-0080 8670-0081 8670-0082 8670-0083 8670-0084 8680-0350 8680-1080 869Q-0080 8690-0085
I
• NPD NPD BEAD (REPlACEMENT ONLY)
869l>OO15 8690-1015 869()..11f5 869Q.2615
8670-1240 8670-1242 8670-1243 8670-1244 867Q.1241S 8670-12416 8670-1247 8670-1248 011fHlO40 011D-4010 0110-2426 8890-004.
,
PtO • PID csu, ASSEMBLY PID l..IoNP 10,6eV wl SEAL. 106-TYPE PlO LAMP 10.2eV wi SEAL 103C-TYPE PlO lAMP SEAL. TEfLONXI, PACK OF 10 ;P1D 45VOC BATIERY (REPl.ACEMEND .PlD HV POWER SUPPlY TRANSFORMER, 8610 A, B MODel PlD HV POVVER SUPPlY CIRCUIT BOARD, 861OG. 310 MODEL PIO DETECTORINlET BULKHEAD FITTING PIO MOUNTED ON MCOEl110 CHASSIS PIO-FIO MOUNTED ON MODEL. 110 CHASSIS Plo- Flo-DElCO MOUNTED ON MODEL 110 CHASSIS iPIO DETECTOR • FPD FPD MOUNTED ON MODEL 110 CHASSIS DFPD MOUNTED ON MODEL 110 CHASSIS PHOTOMULTIPLJER PMl) TUSE FPD DETECTOR BODY SULFUR WAVELENGTIi FILTER PHOSPHORUS WAVELENGTH FILTER NEW FPD DETECTOR BODY WITH BUILT-IN SULFUR FILTER EXTERNAL HYDROGEN GENERATOR, 50ML.IMIN . VERSION IFPD-FID MOUNTED ON MODEL 110 CHASSIS FPD DETECTOR SIMULTANEOUS SIP FPO DETECTOR (DFPD HYDROGEN GENERATOR, BUILT IN FPo- FIO DUAL DETECTOR (DUAL ELECTRONICSl IDFPD-FID DETECTOR (3 AMPUFIERS)
,
I
I
$500.00 $500.00 $500.00 I $5{lOO I $25.00 I $100.00 $125.00 S2OO.00 $5,290.00 $7,285.00 $10,285.00
I
i
,
UPGRADE TCD TO HIGH TEMPERATURE MODEL (HARDWARE ONLY) TCD CELL STAINlESS STEEL, GOWMAC-TYP E Q· RlNG FOR TCD FILAMENT, EACH (MIN. OTY 10) TCD FILAMENT, TUNGSTEN-RHENIUM I TCO FILA MENT, GOLD PlATED, SET OF FOUR AuW 13-300 O-RING, FOR r eo FILAMENT, PACK OF 10
, ,
Pag e 3 Prices subject 10 cha nge
$30000 $300.00 $4,790.00 $2,995.00 $1,295.00 $3,495.00 $5,995.00
53.495.00
TCD • TCD GAIN SWITCH
PL020722.xls
$400.00 INEW $2,295,00 $1 .995.00 $1.795.00 OISCONT. $3.495.00 I $4 ,995 ,00
$5,790.00 . $9,790.00 $995.00 $1 ,000.00 $100.00 $100.00 $495 00 $2,295.00 $6,795.00 $3.995.00 $7.995.00 S1 ,795.00 !DISCONT $4 ,995.00 $8,995.00
$30.00 $1,000.00 $1,000.00 $2_00 $75.00 $600.00
SZO.OO
I i I ! I
7fl.2J024:56 PM
310 (of 550 ) 2006(-2016)
311
1\11 pnccc US
ecnare
2002 SRI Instruments Price list
Tel: (310) 214-5092
www.srig c com 8670-9 127 011 0-0007 8600-0007
8SOO-OOO8 8690 -9007
867o-<1031 0090-0030 011 0-0030
8670-0017
867<>0068 8670-2368
$300.00 I $2.495 _00
$4.290.00
I $6,495.00
5495.00 $895.00
I I
ISYRINGE NEEDLE , REPLACEMENT, FOR lIa UID AUTOSAMPLER .INJECTION PORT COUPLER TO UQUID AUTOSAM PLER CAROU SEL i lIQUIO AUTOSAMPLER CAROUSEl. ,(2 VIAl TRAY 10 STATION PURGE·AND-TRAP AUTOSAMPlER ON-LINE uouio SAMPLER. FO R P&T ON-LINE SYRINGE SAMPLER (NO CAROUSEl) 10 STATION PURGE -AND-TRAP AUTOSAMPlER 220 V
869Q.OO68 869(}.()()53
869Q.OO75 8690-1068 8690-2253
,
DIRECT INJECnON • HEATED SPUT INJECTOR BODY NARROW BORE SPME INJECTOR SLEEVE FOR HID. INJ.) Sl lCOSTEEL LINER FOR SPUT/$PUTLESS INJ ECTOR !SIU CONE SEPTA (PACK OF 25) SEPTUM NUT wi GUIDE FOR 26GA. NEEDLE O.53mm CAPILLARY COLUMN ADAPTER INJECTOR BODY SEPTUM NUT WI GUID E FOR 2OGA. NEEDLE HEATED TRANSFER LINE MOD, wi PLUG SYR INGE 10 ul A DDITIONAL ON-COLUMN INJECTOR, EPC CIRCU IT IHEATED INJECTION PORT UPG RADE SPLI T/ SPLITLE SS INJECTOR UPGRADE, AUT O . VENT GAS PHAS E SPLInER HEATED STATIC HEAD SPACE INJECTOR ADDITI ONAl EPC CONTROL ZONE (NO INJECTOR ADDI TIONAl INJECTION PORT WI THOUT EPC CONTROUCARRIER I HEATED SPUT/SPUTLE SS INJECT OR UPGRA DE W ITH PlY HEATED SPlITiSPU TlESS INJECTOR UPGRADE W ITH PTV, VAlVE
6690~2022
8690-2023 8690-7034 0090-8034
867()'1300
I I
TID TID DETECTOR BEAD TID DETECTOR TID MOUNTED ON MODEL 110 CHASSI S
;20 POSITI ON TRAY, SPARE. FOR 2mL VIALS ICO OLED SAMPlE TRAY
864l).()()2 t
&. TRAP • PURGE BlANK TRAP
86~1305
8670- 13 15 8670- 1320
$ l ,995JXl $1,295.00 52.4 95 00 DISCONT_
$5,290.00 I
• IUAUTOSAJIPLERS a UID AUT OSAMPLER. 20 VIAL RACK
864().()()2Q
$3 .790 .00
$250.00 $3,495.00
DETECTOR, SRI DESIGN HID MOUNTED ON MODEL 110 CHASSIS
011 0-0017
8670-0034 8670-0072 8670-1034 8670-1353 8670-9090 8670-9093 8670-9094 8670-9095 8670-9305 8670-9550 8690-0023 8690-0025 8690-00 34 8690-0035 669C-0045
, ,
I HID
869(}.()()17
864l).()()10
$595 .00
HID • HID DETECTOR BODY
•
I
$495 .00
T CD FILAMEN T PROTECT ION CIRCUIT RETROFID TCD CEl l wi FIlAMENTS, SRI MODEL (EXCHANGE'l TCD MO UNTED ON MODEL 110 CHASSIS T CD DETECTOR SING LE Fll.AMENT TCD DETECTOR TCD DETEC TOR. HIGH TEMPERA TURE (crscc nt. -mcorc. mtc ste . Te O)
8670-9 125
TENAX GR TRAP CAR80SIEVE II TRAP CAR80PACK B TRAP
$75.00
I
$150.00 $7,995.00 $5,995.00 $3.495.00 $5 ,995_00 $6 .195.00
$695 .00 I $150.00 I $20.00 $50.00
$3000
I
I I
$20.00 $250 .00 $30.00 $300.00 $40.00 $1.29 5.00 $795.00 $1.495.00 $795.00
$5,995.00 I $895.00 $495.00 $1 .995 .00 I $3,995 .00 i
I
$20.00 ,
I
$75.00
,
$75.00 S75.OO
Page 4 PL020722.x1s
Pr1ces subject to change
71221024:56 PM
311 (of 550 ) 2006(-2016)
312
All prices US dollars
Tel: (310 ) 214·5092
2002 SRI Instruments Price List
www srigccom 8670-1 324 8670-1330 8670.1335 8670-1350 8670-1450 8670-5050 8670.9556 8680-0052 8680-5050 8690-0051 8690-0052 8690-0053 8690-0054 8690-0055 8690-0064 8690-0075 8690-0086 8690-0097 8690-105 1 6690-1052 8690-2253 8690-5052
~
8670-0062 8670-1501 8670-1502 8670-1590 3690-1087 8690-1088
8670-0060 867D-0061 8670-0062 8670-8000 8690-0062 8690-0063 8690-0064-
POLISHING FILTER. 3" TEFLON TEST TUBE SEALS (1 PAIR) , FOR P&T SPAR GE TEST TUBES (10 PACK) I PURGE & TRAP SPARGING HEAD wi GAS INJ. PORT TRAP HEATER ASSEMBLY WITH T· COUPLE HOT WAND ASSEMBLY REPLACEMT. HEATER ONLY) 1/1 6~ S.S . TUBE FOR P&T SPARGE GAS I VOA VIAL ACCESSORY FOR METHOD 5035, FOR ANY P&T HOT WAND ACCESSORY, ADJUSTABLE , 110V I AUTOMATED PURGE AND TRAP CONC ENTRATOR , METHOD 5030 AUTOMATED PURGE AND TR!\P CONCENTRATOR, METHOD 5030135 10 SAMPL E PUR GE AND TRAP AUTOSAMPLER, w/4 RELAY 80 10 SAMPLE METHOD 5035 PURGE-AND- TRAP SAMPLER 10 SAMPLE HEADSPACE AUTO SAMPLER, w/4 RELAY BO IELECTRIC VALVE ACTUATOR (REPLACEMT . wi TRO) ON-LIN E LIQUID SAMPLER FOR PURGE-AND- TR!\P CRY OCOOL wi ElECTRONICS FOR paT TRAPS TRAP PACKING ACCESSORY METHOD TO- 14 A IR CONCENTRATOR AND VAC PUMP INTERFACE METHOD TD- 14 A IR CONCENTRATOR, AS ABOVE, wffUBE DESORBER 10 STATION PURG E·AND-TRAP AUTOSAMP LER 220V, 4 REL SO UPGRADE PURGE & TRAP TO 503015035 COMPLIANT
THERMAL DESORBERS • VALCO T ROTOR HIGH TEMP.
I I
DESORBER BULKHEAD GAS DELIVERY LINE W ITH CONNECTOR, THERMAL DESORBER 318"GRAPHITE FERRULE FOR TSD (EACH) THERMAL DESORBER SAMPLE TUBE (PK. OF 10) ITHERMAL SOIL DESORBER, MANUAL ACTUATOR I
VALVES • VALCO E ROTOR MID TEMP. VALCO P ROTOR LOW TEMP. VALC O T ROTO R HIGH TEMP . ISAMPLE LOOP SPECIFY VOLUME BETW EEN 0.5mL and 3.0ml) I 4 POR T LIQU ID SAMPLING VALVE, ELECTRIC ACTIJATOR MANUAL GAS SAMPLE VAlVE, 10 PORT ELECT. VALVE ACTUATOR (REPLACEMT. wi TRD) AUTOMATED GAS SAMPLE VALVE, 10 PORT 10 INPUT HEATED STREAM SELECTOR WI TRANSFER LINE BLOCK HEATER wi CARTRIDGE FOR GAS VALVE SOLENOID-CONTROLLED GAS VALVE VACUU M PUMP INTERFACE, DATA SYSTEM CONTROLLED (NO PUMP) CRYOTRAP LOOP, AUTOMATED CONTROL HEATE D I FAST COOLI NG TRAP AND PLUMBING , I THERMOSTATTEO VALVE OVEN UNHEATE D INSULATED VALVE OVEN I
869().0Q65 8690-0066 8690..()()67 8690.Q069 8690-0072 8690-0083 8690-0084 8690-0088 8690-0089
• HEATED INJECT ION PORT CARRIER INLET
$75.00 $15.00 $10.00 $350.00 $250.00
$295.00 $20.00 $2,995.00 $795.00 $5,995.00 $7,495 .00 $6,995.00 $6,995.00 $6,995.00 $595.00 $3,495.00 I $995.00 $150.00 $5,995.00 $6,995.00 $6,195.00 $1,495 .00
$125.00 $35000 $100.00
$5.00 $100.00
$2,995.00 I
$125.00 $125.00 $125.00 $50.00 $1 ,995.00 $995.00 $595.00 $1,995.00 $3,495.00 $495.00 $395.00 $495.00 51 ,495 .00 51 ,495.00 I $795.00 $250.00 I
WJECTORA CCESSOR~S
8670-0025 8690-0075 -
8670-2368 ~670·8000
PL020722.X1S
ON-LINE LIQUI D SAMPLER INJECTION PORT COUPLER TO LIQUID A UTOSAMPL ER CAROUSel SAMPLE LOO P (0.5 to 3.Dcc, SPECIFY) Page 5 Prices subject 10 dlange
I
$100_00 $2.995.00 $150_00 $50.00
71221024:56 PM
312 (of 550 ) 2006(-2016)
313
All
pnces US dolla rs
2002 SR I Instr uments Price List
Tel: (3 10) 214-5092
www srigc com
~(XX)
LABOR
CALL
REFURBISH I TUN E-UP (MIN. CHARGE, DEPENDS O N GC CONFIG.) TRAINING . DAY RATE IN-HOUSE
8tl8O-1500 8tl8O-2OOO 86&l-3OOO
$750.00 $800 .00 I CAlL
'RENTAl
I I I SRI GC MANUAL IPEAKSIMPLE SOFTWARE MANUAl
8600-MANU 6600-S0FT
8600-S500
~EAKSI MPlE •
8600-9000 8600-901 0 8600-9050
I
$1 50.00
I
$1 00.00
PARA WlNDOWS SPANISH UPGRADE MOO . WIN 3.11
$295.00
I I I
DA TA S YSTEM HOS T PCs DATA SY STEM HOST NOTEBOOK PC wi PTR. DATA SYSTEM HO ST DESKTOP PC wi PTR. MULnMEO\A DATA SYSTEM HOST DESKTOP PC WI PlR
$2,995.00 I $2,595.00 $3,495.00
• !AID BUS SYSTEM (WH ILE SUPPUES LAST} 8600-2000 8600-2010
$1,195.00 $59 5.00 $3000 $295.00 $100 .00
:PEAKSIMPlE II DATA SYSTEM FOR MS- OOS
AID BOARD FOR ADDmONAl CHANNEL
~2015
RIBBON CABLE FOR AID BOARD INTERFACE BOARD FOR AID BOARD PEAKSIM PLE DATA SYSTEM MANUAL
8600-2020 8600-SOFT
i
• 8600-1053 8600-1055 8600-1056 8600-1057
8600-1255 8600-2022 8600-4000 8600-4030
860()..4053 8600-4055 860()..4056 8600-4060 8600-4065 8600-4255 8600-4500 8600-5500 8600-5655
8600-S0FT 8670-0232
•
8600-6055 8600-6255
8600-PKC, 86Q().PKC2 86OlJ..PKC3 8600- PKC4
SERIAL DATA SYSTEM IRETROFIT 1 CH. DATA SYSTEM INTO EXISTING GC iPEAKSIMPLE 1-CH. DATA SYSTEM KIT , MODEL 20 3 !S RElAY BOARD FOR MODEL 203 SERIAL INTERFAC E PEAKSIMPlE 1-CH. OATASYST'EM RETROF IT IN EXI STI NG GC PEAK SIMP LE 1-C H. DATA SYSTEM KIT , MDDEl 203, 220VAC 50 Hz SINGLE-GAS EPC Op n ON FOR MODEL 202 UNITS PEAK SIMPLE FOR WlNOOWS SOFTWARE U PGRADE PEAKSIMPLE FOR WlNOOWS SOFTWARE UPDATE RETR OFJT 4 CH. DATA SYSTEM INTO EXISTING GC PEAKSIMPLE 4 CH. SERIAL DATA SYSTEM KIT , 110V MOD.202 SWITCHED AC OUTlET FOR SERIAL DATA SYS TE M 4 RELAY BOARD FOR GC RETROFIT SER iAl INTERFACE, 86 10C 8 RELAY BOARD FOR GC RETROF IT SER IA L INTERFACE , 8610B PEA KSIMPLE 4 CH. SERIAL DATA SYSTEM KIT, 220V MOD.202 PEAKSIMPLE 32-81T UPGRADE FOR 16-81T USER ;PEAKSIMPLE PARA WINDOWS SPANI SH UPGRADE MODULE 1 CH. DATA SYS TEM WI TH 1-121 He SENSO R INSTAlLED I PEA KSIM PLE DATA SYSTEM MANUAL WI TUTO RIAL SERIAL CABLE. RS-232 (08-9 CONN ECTOR S . 6' USB DATA SYSTEM PEAKSIMPLE 6 CH. USB DATA SYSTEM KIT , 110V MOO. 302 PEAK$IMPLE 6 CH. USB DATA SYSTE M KIT, 220V MOD. 302
I
I
$1,395.00 $1,395.00 $ 195.00 $1,395.00 $1,495 .00
$495. 00 I S895.oo IDISCONT . $99.00 DISCO NT.
$2.395.00 52,395.00 $195.00 $175 .00
$250.00 $2.395.00 $99 .00 5295.00 $1.595.00 $100.00 $25 .00 I $2,395.00 f $2,395 .00
,3' x 1/8- 5 .5. PACKED COLUMN
$1£)(100
.6' x 118- S.S . PACKED COLUMN
$150.00
PACKED CO LUMN CTR1 DOU BLE PACKED COLU MN
$150.00 $300.00 !
:r x 1/8'" TEFLON POMPAK a
P_ 6 PL02 0722 .x1s
Prices subject to cha nge
7122J024;56 PM
313 (of 550 ) 2006(-2016)
314
All pricee US dollar$
WNW
srigc com
8600-PKC5 86OO-WBC1 86OO-WBC2 8600 WBC3 8600-WBC4
24 ' x 1/8" 5.5. AT-1 000lCARBOPACK 8 CFC PACKED CO LUMN 15M CAPILLARY COLUMN 15M MXT-S CAP. COLUMN 30M CAPILLARY COLUMN 80M CAPILLARY COLUMN
8600-WBC7 8600 -WB C8 860Q-WSCX
30M MXT-l CAP. COLUMN 30M MXT-S CAP. CO LUMN 30M MXT-WAX CAP. COLUMN
66OD-C346 86OO-C350 860D-C380 8600-C580 8600-C590 867D-1081 867D-1082 867~5000
867D-9305
867D-9554 668D-0052 6680-0350 8680--5050 8690-00 70 8690-0073 8690-0081 8690-0082 ......,.. 8690-0095 6690-03 50 8690-0351 8690-2270 8690-5510 8690-5600
869D-5655
l"ARTS 86OD-MAIN 8670--0011 8670-0017 6670-0025 867D-0031 8670-0034 6670-0060 8670--D061 8670-0062 8670-0068 8670-0072 867D-008O 867D-0081 867D-0082 8670-0083
Tel: (310) 214-5092
2002 SRl lf'ostruments Price list
$495.00 $300.00 $300.00
$50000 $875.00 $500.00 $500 .00 $500.00
GAS LINE INSTAUATION KIT CGA346 GAS LINE INSTALlATION KIT CGA350 IGAS LINE INSTALLATION KIT CGA3BO GAS LINE INSTALLATI ON KIT CGA580 GAS LINE INSTALLATION KIT CGA590 METHANIZER TUBE REPLACEMENT- 6" x 118" METHANlZER TUBE REPLAC EMENT- 2" x 118" - FOR NEVV 6610C GC CIGARETIE LIGHTER POWER SUPPLY. 300W 12VOC HEATED TRANS FER LINE MOO. wi PLUG SRI TUBING CUnER FOR COPPER TUBING METHOD 5035 COMPLIANT VOA VIAL SPARGE ACCESSORY EXTERNAL HYDROGEN GENERATOR, 5OMLIMIN. V ERSION HOT W AND ACCESS ORY, ADJUSTABLE, 110V INTERNAL WHISPER-OUI ET AIR COMPRESSOR, 110V VACUUM PUMP INTERFACE, AUTOMATED METHANIZER ACCESSORY METHANlZER AC CESSORY, IN JET REUSEABLE SHIPPIN G CONTAINER HYDROGEN GENERATOR, BUILT-IN, 25mU min VO LU ME HYDROGE N GENERATOR, BUILT-IN, somtzrnm VOLUM E INTERN AL WHISPER·QUIET AIR COMPRESSOR. DIGI TAL MULTIMETER, GENERA.L PURPOSE H2 1 HC LEAK DETE CTOR, AC POW ERED 'H2 ! He LEAK DETECTOR, BUILT INTO 1 CH . DATA SYSTEM
$39S.00 $395.0 0 $395 .00 $395.00 $395.00 $100.00 $100.00 $495.00
$300.00 I
$10.00 $3,495 .00 $2,295.00 $795.00 $595.00 $495.00 $995,00 I $995 .00 I
$200.00 I $ 1.795.00 $2,795,00 $695.00 $69 .95 $299 .95 $1,595 .00 NEW
nov
I I
GC MAINTENANCE KIT, SPECIFY 110V OR 220V, 861 0C TCD GA IN SW ITCH ·TID DETECTOR BEAD HEATED INJECTION PORT CARRIER INLET HID DETECTOR BODY HEATED SPLIT INJECTOR BODY IVALCO E ROTOR MID TEMP . VALCO P ROTOR LOW TEMP . IVALCO T ROTOR HIGH TEMP . ISYRINGE NEEDLE , REPLACEMENT, FOR LIQU ID AUTOSAMPLER INARROW BORE SPME INJECTO R SLEEVE (FOR HT D. INJ .) PMTTUBE IPMT DETECTOR BODY SULPHUR WAVELENGTH FILTER PHOSPHORUS WAVELENGTH FILTER 667(}.{)l)84 NEW FPO DETEC TOR BODY WITH BUILT-IN SUL FUR FILT ER 8670--0090 UV/CONDUCTIVITY DETECTOR BOARD (REPLAC EMENT) 8670-0 120 NPD BEAD (R EPLACEMENT ONLY) 8670-0 150 FlO IG NITO R I ELCD HEATER 8670-0154 FlO COLLECTOR ElECTRODE REPL. B6l0e Page 7 PL020722.x1s Prices subject to change
I I
I
$495 .00 $30.00 $300.00 $100 .00 $250.00 $695.0 0 I $125.00 I $125.00 $125.00 $75 .00 $150,00 $99500 $1,000.00
$100 .00 $100 .00 5495 .00 5495.00 $300.00 $75.00
$20.00 71221024:56 PM
314 (of 550 ) 2006(-2016)
315
All prices US dollars
2002 SRI Inslruments Price Usl
Tel: (310) 2 14-5092
www srigc com 8670-0155 8670-0232 8670-1 024 8670-1 025 8670-1 034 8670-1081 8670-1082 867 0-1357 867 0-1400 867 0-1401 867 0-1402 867 0-1403
:FID COLLECTOR ELECTRODE CABLE (REPl. 861 0C) :SERIAL CABLE, R8- 232 (08-9 CONNECTO RS , 6' IFID I NPD DETE CTOR BODY Fl O DETECTO R BODY FOR METHANIZER ISILCOSTE EL LINER FOR SPLl T/SPLITLESS INJECTO R .METHANIZER TUBE REPLACEMENT· 6" x 118" METHANIZER IN-JET TUB E REPLACEMENT- 2" x 1/8" PORTER PRE SSURE REG ULATOR wI SENSOR OVE N HEATER I SOCKET SET, 110 OR220V OVE N HEATER ELEMENT FOR 8610A . B, 9300A GC's OVEN HEATER SOCKET FOR 861DA, B, 9300A GC's OVE N HEATE R ELEMENT FOR 8610G GC, 110V
8670-1404
OVE N HEATER ELEMENT FOR 8610C GC , 220V
8670-1590 8670-1814 8670-18 15 867 0-1853 8670-2368 8670-6000 8670-6010 867Q..6021 8670-6022 867~3
8670-6024 8670-6025 8670-6026 8670-6500 8670-6550 8670-6575 8670-6600 8670-9001 8670-9002 8670-9003 8670-9004 8670-9093 8670-9305 8670-9555 8690-0072 8690 0081 8690-0095 8690 -0151 869 0-0152 8690~1070
8690-7000 8690-7100
318" GRAPHITE FERRULE FOR TSD 114" TO 1/8" REDUCING Fini NG, FOR CTR COLUMN , ETC. 1/4" TO 1/8" REDU CING FIn iNG, WITH 1/16" GAS LINE ENTR Y GRAPHITE REDUC ING FERRULE, 118 0.8mm , PACK OF 10 INJ ECTION PORT COUPLER TO LIQUID AUTOSAMPLER CAROU SEL DIG ITA L FLOW CONTROLLE R FLUISTOR (EPC MOD ULE) WIT H CONNECTOR TAN K PRES . REGULATOR wI CGA FiniNG INORGREN GAS PRESSURE REGULATOR INO RGREN PRESSURE REGULATOR wI SENSOR jW An S GAS PRESSURE REGULATOR WAITS PRESSURE REGULATOR wI SENSOR IG AUG E FOR REGU LATOR OVEN CIR CULATING FAN wI SQUIIREL CAGE GREY OVEN COOLING FAN COO LING FAN MUFFIN COLUMN OVEN LID, 86108 GC MAINTENANCE KIT , 8610C 110V GC MAINTENANCE KIT, 8610 C 220V GC MAINTENANCE KIT , 861 0B 110V GC MAINTENAN CE KIT, 861 08 220V 0.53mm CAP ILLARY CO LUMN ADA PTER HEATED TRANSFER LINE, CAPILLARY TIJBING W BING COPPER 118" PER FT. VACUUM PUMP INTERFACE, DATA SYSTEM CONTROLLED NO PUMP) METHANIZER ACCE SSOR Y REUSEABLE SHIPP ING CONTAINER NAFEON MEMBRA NE REPLACEMENT FOR SOML HYDROGEN GEN. NAFEON MEMBRANE REPLACEMENT FOR 25ML HYDROGEN GEN. REPLACEMENT AIR FILTER .O P-AMP CHIP :SCR - TRIAC CIRCUIT BOARD
$30. 00 $25.00 $300. 00 $400 .00 $20.00 $100 .00
I
$100 .00 NEW $325 .00 $50.00 $40.00 $ 10.00 $50.00 $50.00
I I
M
-
$5.00 $25.00 $100.00 $30.00 $150 .00 $350 .00 $150 .00 $250.00 $75.00 $150.00 $100.00 $175.00
I ! I I
$40_00
I ,
I
$100.00 $100.00 $75.00 $100.00 $495.00 I $495 .00 I $395 .00 S395.00 $20.00 I $50 .00 I $1 J)() $495.00 $995 .00 $200 .00 $100.00 $100.00 $100.00 $ 10.00 I $250 .00 I I
.
I KA'N'Nlj
868 0--2000
TRAINING, DAY RATE IN-HOUSE
S800 .00
I
PL020722.x1s
Page S Prices subject to change
7/22/024:56 PM
315 (of 550 ) 2006(-2016)
316
Parker CPI Fittings Chromatographic Fittings Parker CP I fitting s ate rapid ly becoming the standard in l he ctvomat ogr aphic industry. A unlOUe one Piece tenure does awa y with the two piece design of other manufacturer s. This ends assembty contusion and insu res better sealing du ring make-up. Parker CPI components are in ter cha nge able with all Swagelok· components used in Chroma tography . Description 5i:ze Parker No. Cat. No. Price . . BRASS . FITTINGS . ' $13 .00: In s" r-az '<457 11S- {101pkg1 2-BZ 750 " '<458 3116" (1 OIpkgJ 3-SZ 60000 700 NUTS 1/4 " ( 101pkg) 5 50 ' -SZ " css ae6- SZ 60002 9 0<> 10 1 ~ /Si rjen l 6-SZ 1000 6('00" ,·TZ 1/16 " 1.060 1 6.~ ~'' 0 1/8" (10/pl1g) 2-TZ 1.061 10.50 311 6" (10 /pkg) FER RULES 10.00 ' -TZ Only One Requ ired 1/4" (lCVpkg ) 4·TZ 10.00 1'062 aee·TZ 11.00110 '0006 112" IlI:Jnknl 600105 12 00 S·TZ 1116" ~ 1/16 J 1Ih." 14075 H ·l..JBZ 16.0 0 lIB " J 1f8'" x lIS" 2-2-2-JBZ 140 53 11.00 3/1S- x 3/16" x 3/16" 3-3-3-JBZ 60012 1300 1/4" x tl4- x 1/4" 4-4-4-JBZ 140n 11.00 TEES 3/8" x 3/8" x 3/8" 60014 15.00 ~:6~'JBZ 117 x 112" x 1/2" -8-8 -JBZ 600 16 22.00 14063 1/16" .. 1/ ' 6 1,' ·HBZ ' .00 118- x 118'" 2 -2 -HBZ 5.00 '<065 3116'" x 3/16" 3·).HBZ 5.50 600'8 UNIONS 114 " 1l1l'" ~-HSZ reese ' .00 6_50 ae-« 3M' H-HSZ 60020 112" l( 112" 8-8-HBZ 10 50 60022
8
....,
s
T
~
~
REDUCING
:411 iN
~A~~~:"'{
~
E 8:=-
1M 41
!Il:l ~ 10 J_1 ~: 3f'16" to 118" 1/4" 10 1116" 1/4" to ur
UNION
1/." 103116'"
,
3IB" 10 1116"
318" 10 1/4"
111 6" J: 111 6" 1116'" 10 11 6" M 1116" to litl" MPT 118" to 1/8" MPT 118'" 10 1/4· UPT 3t 1l,IO 118" MPT 1t' " 10 118" MPT 318- to 118" MPT 114" to 1/'" MF'T 3/8 " to 1/4- MF'T
MA LE
CONNECTORS
, '0 ve- 10
TUBE END
I t. " FF'T 1/4- 10 1/8" FP T ti4" to " . " FPT 3116" to 118- FF'T 3.18 -10 118" FF'T 3.'8- !0 114" FF'T 1116" 10 118- Tube 1/16- 10 114- 'tcee 118"to 1/4- TUbIl 118" to 3116- TlAJe
C ONNECTOR
3 , 16" kJ " ' " Tube
FEMAL E
CONNECTORS
I
4· 2-H8Z 4 -3 -HBZ 6-1 -HSZ 6-4·....6 2
eooae
1+ F3Z 1-2-FBI 2·2-FBZ 2-4-FBZ 3-2 -FBZ 4·2·FSZ 6·2- FBZ ' ·.-FB2 6·4-FBZ
60036 60638 60039 600<0 6('0" 60044
~:~
,00<8
2~{36Z
1':;-
~.~N~~ PN '
1/ 16-
'"'.
l- FNZ 2-FNZ
,,,.
4· FNZ 6·FNZ 8 ·FN2
3,.'16" 1;4 -
60062 6006<
14073 60066 '0068
~i::
' _50 '00
6'028
14166
-6.60
14167 14174 61030 288 12
5 50 5_00 ' _00 ' _00 3 .75 3.50 4.75 3 ,;~
61034
-
«r
-
61036 610 38
61039 61040 61042
"'"
.. 5::: 550 525
6.50
I
18.00 16 .00 17.00 3100 26 .00 41.00 19.00 20.00 11.00 11.00 12.00 9.00 '4.00
~:g:;
: ~.~
61048
13. 00 18 .00 12.00 15.00 15 .00 19.00 2000 19.00 2400 13.00 15.00 '6 00 16_00 15 .00 2000 1' .00 9 00 10.SO 750
61084 61050 61086 61052 610 54 61056 61058
61059
.:5::
1• .00
01060 61062 'H'6' 1 ~1 69
"61068 066 14151 14152 61010
'<0<7
' .00 2.50
6007'
2_SO 250
60072 600 "
5.50
610n
11.00
5 00
61074 14155
" 60076
'00 250
2 25 300
erct e
60060
4 1~
61078 61080
16 00 17.00 10.00 11.500 6.50 10.00 15.00
'''''
14~~
...
14 055 6001f1
3· FNZ
ae-
~iri=
' 00
--
. -2· TRBZ
1700
::5_50;:
6006'
60056
" '65
25.00 " _00
60058
14 011 600 50 14072 60052 6005 4
' -2·GB2 ' ·'-GBZ 3 -2· GBZ 6 -2 -G BZ 6 ·4·GB2 2 -1·TRSZ 4· 1· 11'162
Price STAINLESS 141575 $25 . 00J5 1.158 3000 61000 28 .00 14159 28.00 23 _OOIS 6100 25 610045 3<00 141605 0
610 18 1.168 61020 61022
' .00 550 5.50 5.25 5.00 6 .00 6.25 5.00
14M2
1/ 16 -
aa-
TOLL FREEORDERING 1-800-255-8324
60030
1"1-Z7H BZ7
."
14 153
,•'"
1A15 6
MPT:Male Pipe Th read
FMTesernare Pipe Thread ':t.
---
1:' "
1/4- {O 118" Tube 114" e ae- Tube as- to 1/4 " T~
aoe-
PLU GS
60026 60028 "067
3·2·TA61 ' ·3 -11'1 62 Z....·TR6 Z 5-4-TRBZ 4-6-ma1 1- N~~ Z·PNB1 3·P N6Z 4.PNBZ
1.'8 -
C A PS
=:
~:~:~~
e-r -aaz
cat No.
~
.' / . . '
.. ; •.•. '::j
". ,~..: ~ .
"
'~"
. , .• .; '•. ,
<" • •• • :. . ;....
AUTECH·· .".
164 316 (of 550 ) 2006(-2016)
317
Ferrules Ferru les
Vespe l/Graphite Ferrules
The ferrules listed here are made from synthetic materials to be used pri marily 101 maklllQ glass-to-mela l and glass·to-glass connections. These ferrules can also be used convemem ly for metal COlumns. Th ey do not lock into place and so can be removed or moved to a offerenl position on the column lor use with different esmnrents. A wide varietyof materials and sizes are awilable. A summary tabl e of the properties of eadllype of ferrule appears below.
The recent devel opme nt of VespeVg raplli le composites giv better results than eittler Q( graphlle alone. T hey do not stlck to gtass or metal, are Q)I'l'Ipletely reusable. and a re less brittle than v esper. The composite is usable at temperatures up to 400 D C. Two types 01composites ate availa ble. The VG l composite is 85% Vespell 15% lYaphite wh ile the VG2 type is 60"4 v escev 40% g raphite. AlfleCh recommends the VG l as lhe best all. purpose ferrule, wh ile m an y 01OUf cu stomers prefer the added lubricity of the VG2lerrule.
vescer
lt
Teflon Ferrules t enon ferrules were the first improvement over O-rings lor coonecting glass col um ns 10 instruments. Being soft, they lonn sea ls even with fing er tig htening. They will conform to the Shape of the co lumn and fin ing upon compression. Their upper tem pe rature limit of 2500C and their cold -flow properties make them unsuitable for high temperatures and IOf temperature prog ramming .
. I
I
iI
Straight Ferrules
I
I
S traight fer rule s are used on glass, metal and 'te non colum ns where th e tub ing size a nd litting size are the same (eg•• l/B~ to 1/S"lit!lng). They are avai lable in all materials in a v ariety of sizes.
Graphite Ferrules
Reducing Ferrules Reducing ferrules are used when you n eed 10 co nnect tubi ng
AUlech 'sgraphite ferru lesare mad e lrom99.95%pure graphite . This means no bleed or decomposition products at hig h
of one size 10 a larger fitt ing ,Freque ntly, g lasscolumns, eSpecially
temcerewres. They are a vailable as either the one-piecedesign or as the fron t ferrules wh iCh must be used with a rnetaJ·bac;f(; ferrule . Uke Teflon, the one-piece graphite is soft and wil l
those o f 4mm 10 . are 6mm 0 0 and 50 req uire 1/4 " 10 6mm redUCing ferrules . A 118" co lumn can be adapted to 1/4" litb ng s o r in,iection ports with a 1/4" 10 lIS- reduci ng ferrule. MOSI capillaty columns connect to 1116" fining s, but the 0 0 01 me capillaries vary from about O.32mm 10 t .emm. For this reason . a wide variety or 111 6" ferru les with ho les tram O.4mm to 1/16'" are off ered.
con tonn to unusual shapes wh en compres sed . With care, they
are reusable but not lor as many limes as the veecer ferrules. T heir upper tempera ture limit is 45OOC.
vespet e Ferrules Vespel was developed lor commercial use in 1962. In 1973 the advantage of v eeee teeves torctvomatographywas realized. In that same year. A illech was tne first to ifltroduce a ful lil'le o f Vespel lerrules lor GC col u mns . These lem.des do not cold flow , are completely reu sable and c an be used at tempera tures up 10 350 "C -t-. They are suitable lor meraJ, Teflon and g lass col umns. At high tempe ratures the y have a tendency to seize on the glass a nd me tal surfaces. T his can be pre vented by appl ying a small amo unt 01Nt!VI:!r·Seez~J 10me back of the ferrules orby using the new Vespe l/g raphite ferr ules.
Zero-series No-Hole Ferrules A1ltech pioneered the use of lhe "Zero-Series Fe rrules." These are avai lable in a variely 01 sizes an d constructio n rnatenar s. T he y can be us ed as IS to seal off a fitting . or you can custom d riB them 10 suit your needs. For cap illary columns 01 unusual sizes, we offe r the Alltech Ferrule Dri lling Rig.
' . STRAIGHT FERRULE 118" Tubing 1/8" Nut
•
REDUCING FERRULE
118"" Tubing
.'
1/4" Nut
! 1/4· to 118" Reducing Fet'rule
Temp Urn"
Matenal -
. .
.
.
.
I enon
25O"C
GrapMlte
4 5Q"C
FERRULEPROPERTlES :' '; ' '' ~
vesoe
35O"C.
vescecc ra r ete VG1
"""'C "",,'C
VesoeifG r a hrte VG2 O- Rings
200 °C
Resealing Properties
Reusability
-
Good Good Exce llent Ex cellent Excelle nt Poor
TOLL FREE ORDERING 1-800-255-8324 .".- .' . , ~. . , . , "
.
.... "'.. "
-
.-..- •...
;I-~
:
Temp
Prog , '
,.'
e xcenent
l::.xcellent
No
Excellen t
Excelle nl
Good Good
Good
Yes Yes Yes
Good Poo r '~
'
SUitab ility fo r Glass
Exc ellent Exc ellent 000-
Ye, Fair
:ftk-.,. - ..., .-.; ....-..:; . ~' . .•.. ..:~ .,1 , ~~
168 317 (of 550 ) 2006(-2016)
318
Ferrules _ ( Teflone Ferrules
I
Graphite Ferrules
. 99.95 0/.• Pure G rap hit,e
• 100% Pure Virgin Teflon • No Fillers • Forms Seals with Finger Tightening • Reusable • Use up to 2S00C
• No Fillers
• Forms Seals with Finger T ightening • Reusable. with care
• Use up 10 450°C
"1-,..., cat. No.
SF-600-T SF-400-T SF·3OG-T SF· 200-T SF-1OQ-r
Size
.9!Y
Price
10 10 10 10 10
$10.50 6.50 6.50 6.50 6.50
10 10
sa.50
13il!·U"il;"'lf1;i'di!;!lj!=-~III!I!~~ 318- Straight Ferrules 1/4- Straight Ferrules 3116" Straght Ferrules
1/8- Straight Ferrules 111 6- Stra!ght Ferru les
@i!·!:li1:U1!t';Ga
j :l;hill! ao1
RF-400J6MM-T 114- to 6mm Fenures RF-400.'3DO-T 1/4-to3l16" Ferru!es RF-4OOI2OO-T 1/4" to 118- Ferrules RF-4OOI1DO-T 1/4"'01116 " Ferrules RF·2OOI1QO.T liS" 1116" Ferrules
7.50 10 7.50 10 7.50 10 7.50 .' ~ "' . - ~ TEFLON No-HOLE FERRULES - --:" ' -. . -. • 1/4- No-Hole Ferrules R F-400~T $8.50 RF-2OOlO-T 118- No.HoIe Ferrules 8 .50 R F-l~T 1 111 6" No -Hole Ferrules I. 8.50
J
'0
I.I.
VespeP Ferrule s
I I L
• High-Temp erature Polyimide • No Fill ers " Forms Seals with Minimal Tig htening • Com pletely Reusable • Use up to 350°C+
•
cat. No.
SF-800- G SF·SOO-G 'SF-4QO-G SF·200-G SF·100-G
...
Size
1/2- S iraight Ferru les
316" Straigh t Ferrules
RF-2OOIO.8-G RF·2OOIO.5-G RF·2OOJO.4-G RF·10011 .l)-G RF-100tC .8-G RF-100!O.5-G RF-100fO.4-G
.. .
.
. . ..
-.
10 10
$24 .00 21.00 21.00 21 .00
I. I. I. I.
1/4 " to 6mm Ferru les 1/4" 10 118- Fe rrule s 114" to lft6" Ferru les 11'8'" to 111S- Ferrul es 118" 10 O.Smm Ferru les 118" to 0.5mm Ferru les
l iS" to O.4mm Ferrules 1116" to 1.0mm 1/16""to O.8mm 1116" to O.5mm 1116"10 O.4mm
Fe rru les Ferrule s Fer rule s Ferrules
1/ 4 " Straight Ferrul es 1/4" -S ho rty· Ferrule s' 118- Straight Ferrules 118- ·S horty· Ferru les' 1/16- Strarotn Ferru le s
I I. I
RF-4001300·V RF-4DO.'2QO-V RF-4OO11 ()().. V
1/4" to 3/16" Ferrules 1/4" to 118" Ferrules
-
10
I. I. 10
10
I.
10 10 10
.
10
11.4- No- Ho le Ferrule s
-
I. I.
I.
$26 .00 26 _00 26.00 26 .00 26. 00
$26.00 26.00
I.
I. I.
.
Price
..
2<00
II..
1118 " No -Hole Fer rul es
21 .00 21 .00 21.00 21.DO 2 1.00 21.00 21 .00 21.00 21 .00 21.00
10
1/4" to 1110 Ferrules R F·200I100-V 1/8-10 1116- Ferrules '0 1116 - to 1.0 m m Ferru les RF-100l1.O-V 111 6'" 10 0 .9mm Fe rrules RF·100/0.9·V RF·100JO.8-V 1/16- 10 O.8m m semne s R F. 10Q,'O.5--V 1/ 16" 10 O. 5mm Ferrul'" 10 R F· l00JO.4.v 1/16- to O.4mm Ferru ~ s . . VESPEL rtO-HOLE FERRULES • . F-400/OoV
$21. 00
I. I. I.
VESPEL REDUCING FERRULES ,' .
R F-4O
2 1.00
I.
Ql y Size VESPEL STRAIGHT FERRULES '
SF-40D-V 15459 S F-2O().V 15458 SF·100· V
Pric e
1/4" Straight Ferru les 1IS" Siraighl Ferrule s 1116"' Stra ioht Ferru le s GRAPHITE REDUCING FERRULES
RF-400I6MM-G RF..woI2DO-G RF-4OQn OO-G RF.2OQf100-G
Cit. No.
Ofy
diMpm jifi E@@;i'j:l;I;III!£f
26.00 26.00
2<.00 26.00
I
26.00 2 6 .00
26 00
." 526 .00
26.00 26.00 RF·100fO· V 1116 · No -H::Jie Fer rule s 10 • "Sbortv" ferrules are ire Applied Science wee ot the sam e sue a s the Pa rker o ne -pie ce metal terrule . ALLTECH" ' . .. . . , . . . _ . ~ • • . ,1 - . TOLL FREE ORDERlNG1-800-255-8324-·:'
=F.2QOfO-V
to
169 318 (of 550 ) 2006(-2016)
319
Ferrules VG2 - VespelfGraphite Ferrules
VG1 • Vespel
Cat. No.
Size
Qly
.. High-Temperature Composite .. 60% Vespel + 40% Graphite .. Forms Seals with Minimal Tightening • Completely Reusable • Use up to 40QoC
Price
Cat. No .
Size Price Qtv VG2 STRAIGHT FERRULES . . 1/4 " Straight Ferrules 10 $29.00 10 15451 1/4" "Shorty" Ferrules' 29.00 SF-200-VG2 1/8" Straighl Ferrules 10 29.00 1545 2 lIB- "Shorty " Ferrules ' 10 29. 00 10 SF-l00"VG2 1116" Straiqht Ferrules 29 00 . VG2 REDUCING FERRULES ' . 400J6MM·VG2 114" to Smm Ferrules 10 $29 .00 1/4- to 3/16~ Ferrules 4OOI3OO-VG2 10 29 .00 400120o-VG2 114" to 1/8" Ferrules 10 29 .00 400/10o-VG2 1/4 " ' 0 1/ 1S" Ferr ules 10 2900 200/1~VG2 118" to 1/16" Ferrules 10 29. 00 10 2OO1O.8-VG2 1/8" to O.Smm Ferru les 29 .0 \ 10 2OOIO.5-VG2 118" to 0.5mm Ferrule s 29.00 2001O.4-VG2 118" 10 OAmm Ferrules 10 29.0 0 100/1.Q..VG2 1/ 1S" to 1.0mm Ferrules 29 .00 10 100/0.9-VG2 111 6" to O.9mm Ferrules 10 29 .00 100 /0.8- VG2 1I 1 6~ to 0.8mm Ferrules 10 29 _00 l 00fO.5-VG2 1116"to O.5 mm Ferrules 10 29.00 10 1/16" 10 0 .4mm Ferrules 1001O.4"VG2 29.00 . - ; VG2 NO-HOLE FERRULES . ' . , -'.
.
VGt STRAIGHT FERRULES . SF-400-VGl 114" Stra ight Ferrules 10 $29.00 15449 10 29 .00 1/4" · Shorty" Ferrule s' SF·~VGl lIS" Straight Ferrules 10 29 .00 15450 tza- "Shorty" Ferrules' 10 29.00 SF·,OO-VGl 10 29.00 1/ 16" Straight Ferrules . VG1 REDUCING FERRULES 400l6MM-VGl 1/4" 10 6mm Ferrules 10 $29.00 400I300-VGl 1/4" to 3/ 16" Ferrules 29 .00 10 4001200- VGl 1/4" to 1/8" Ferrules 10 29 .00 4QO/l000VGl 1/4" 10 1/1 6" Ferrules 10 29 .00 200fl00-VGl 118" to 1116" Ferrules 10 29.00 2nD/D.S-VGt lIB" to O.Bmm Ferr ules 10 29 .00 2001O.5-VG1 liS" to 0. 5m m Ferr ules 29.00 10 200ro.4-VG1 118" 10 O. 4mm Ferrules 10 29.00 100/1.Q-VG1 1/16" to l.Omm Ferrules 10 29.00 1001O.9-VGl 1/16" to u.smm Ferru les 10 29.00 100/0.aNGl 1/ 1 6~ to O.Bmm Ferru les 10 29.00 100J0.5·V G1 1/16" to 0.5mm Ferr ules 10 29.00 l00IO.4-VGl 1116- to OAmm Ferrules 10 29.0 0 " ,. " VG1NQ-HOLEFERRULES , ' ' ., 40010"VG1 1/4 " No-Hole Ferrules 10 $29.00 200lO-VGl 118" No-H ole Ferr ules '0 29.00 100fD-VGl 1/16" No-Hole Ferru les 10 29 .00
." SF-40D-VG2
I
400IO..vG2
114" No·Hole Ferrules
200/Q..VG2 100/Q-VG2
liS" No- Hole Ferrules
10 10 10
1/ 16" No·Hole Ferrules
$29.00 29 .00
29.00
" "Sl1ort y~ ferrules are the Applied Science Iype 01 the same size as the Parker one-piece metal ferrule.
Two -Hole Capillary Ferrules
••
IJ.
A variety 01 Two -Hole ferrules are avai lable which allow the user to conne ct two ca pillaries to the sa me end of a compression fJlting. This arrangem ent can be used for sp litting the effluent of a single capilla ry or packed colu mn in oroer tc use two differe nt detect ors. for sample reco very, or even for splitting the injected sample to two different cap illary or packed columns.
.
- ~- " -- - ---- -
----------"-
- - - - _ . _- - - ~ -
Cross-Section
Cat. No. .
Si ze aty Pri ce Val TWO-HOLE FERRULES .' '''' . ,. 15486 1 1/16" 10 O.5mm Two-Hole Ferrules 10 $3 5.00 1/ 1 6~ to n.amm Two-Hole Ferrules 15481 10 35 ,00 , . "-.•. •~. ' . WG2TWo-HOLEFERRULES <:-; ·· ··,·.. -" :.
Use the OAmm Two-Hole ferrules tor co nnecting 0.25mm 10 fusedsilica tubing and The 0.5mm Twe-Hole ferrulesfor connecting O.32mm 10 tcsec silica tubing . Both VG 1 (85% v esper + 15% graphite) and VG2 (60% Vespel ... 40% g ~ao hite) ale avauabre.
TOll FREE ORDERING 1-80D-255-8324 '
~
--- ------ . _-
I
15488 I 1/ 16" to 0.5mm Two -Hole Ferrules
.
..
. .-
.. .
' '.
.
10 ' $35 _00
ALLTECtI · ·
170 319 (of 550 ) 2006(-2016)
320
) ~ -- - ----- - - I
:
.'1/
FROM DISPLAY
"'
0'
BOARD
~'~F
.1211
noK
,
\)
: ,
LOCALSETPOINT: :
10K
-
U6
5
LM331
i_I
QREENAND REOWlRES OF PHONE
I
,. [I,
.1~ "
,0<, ,r - -CHAS-siS-
-J.--',
I MOUNTED 1 FOOTSWITCH
1 RED: CEHTER
C"-N,!~'::'5~"!'~
...II
€V
I
I "SP ME~
RELAY 'D'
HiJ. ,
@'N""
scaa QSOD 4
TOLOW VOLTAGE TRANSFORMER
/i
"
1,
YEUOWWLREOf PHONe CABLE
TO DISPLAY BO.
I TO I :OISPLAV:
o. 'K
J1
BlACK WIRe OF PHONE CABLE TO DISPLAY BD. " L.£O ~
"ACTUAl"
,, ,, ,
4 ,:
1 I
l.
,,,
•
•
=. ~ -- :i0Y"
~
~.
' ¥1oC
fOHT1l
• •
-t -
..
it
... .1. CII
Vl',"""
M
,
I I I
.......
.I ...
TRIAC DATE
..", CII
~
I
ow
ClII.CUIIOPlIlAU
.~!..~ USl~.12\l 0IIPlll4
OItOUND
,, ,, ,, ,
r
.,
rh C H"'S.'S
T----------- -,•
'"001 ": ~_
fWIII~ "-T~
SPME
l
POWER SUPPLY SECTION .... - - - . . - .
IN JECTOR
BRA SS 'TEE'
{Yfl ~OW)
_
THE:SP JolI! IN.J ECIOA.
Wlt EH THI! ' OO TSWITCH O1 RELAY ' 0' IS AC TlV...Te o
1116"
,,
,,
USf A""'O.lUS'.8I.1:. PULSED VO LTAOE H EAl S
[P
I BOARD I
IPUSHBUTTON)
00
•,, ,
Iha..:;
6000t tM
10K
FRO'" AID BOARD (YELLOVi)
,
0"
SCREW TERMINALS
.,
r"
I
017
:~
1 2
PROTECT CIRCUIT)
"u11~
L.M324 J
-'V- J
........ ~
1
1K
I I
.1.
-J
'''''OHM~
1.8 V REFI!RENCE (WILL NOT TRIP THERMOCOUPLE
07
AJD BOARD R IlMOTI! S''''AT (RS I I
-VVy\o
<,
1O'
o
OUTP UT TO
011
R2
1 WAn
ZeRO .cRO SS 1N~ _
I
INPUT
100 OHM
NON
,
~ oA,..,'_F
INPUT
U'
MOC3010 (3020 FOR 220V)
,
L c,
05
SWITCHED SWITCHED AC HOT AC NEUTRAL
""
•,
• •
1
,.
CA8l E
I (LOCAL AHO TOTAL I I SElPOlNT I 1 I POSHBUnONSI _:
Vollagllo Fftqulnc v
7 01
..
W
JI I-I
SPME CIRCUIT
..
..L ~~
T~ ""';'_.JI
~
I
r
Pag. 1 012
CAUTION , ACHOTM D ...CNf Ul RA l u e HAlAlIDOUS VO ~ lA GU MO Uf PRESENTON
Till S AHO OTHU ClII.CUlT
DOAII OSWIlH.E THE a
c.
POWlRIS QW,
I :
SPME-A SCHEMATIC
"'
320 (of 550 ) 2006(-2016)
321
- -- -.
-- - _. :, III m :,
:I hi : i S~ I
, ii,&, , I
l __
I
~ ..J
...--.:J .• ,7-
dy.
!
i
i
:LiiI : .: J
f~
,.-
•3 e • f3 • c•
""~-
• •s ~
~
• a N N
-
~ N
~
0
~ ~
f-
00 °00
:I:"t1 m:;: S:m
~
-n
,•
•
-------------- "'5c:o n
=<
.,
a! 0
•
», " ::I» m
";.
m
"' ::i!'l~ S.
c •
C')
'" ~
~~ s.
~
J-::E:>:t
zmzm
,. -------------, 'c" :< i!l~ . S • -,-, ------- ""1, -
,,
A'ldolOS teoW)d
,
0
c: ~
0>0>
"'0-1.,,-1
-n -n Z _z_
:J:CD;r-fChQ-f
>c:m:t:"'CI~:::Z::
<~>m:i::tC:;;
ms::-iOmm"t!
C'zOZtD~>
::u =riQ5i!om agog mnC:O::U$o c:-c:- j - f - t - f ::U:::a=i:riPnm ~Ocn-n c:"tJ c:N c: .... -t5::et m =in
.....::I ......
"'O~.,,~
. .. .z ..z
-fC:-lC ~U)cnc.o
• rn '
c: ~ ~
m
o-t -~
"'CIz>z , Zo >mcm
c: 3:~atm ~
"'CI:z:N
..
-
m
Z~Ul~
CI.l-f ::ettA --I
>%
zm 0(1) n
o~~m C-t>m
:i :z:: o~ "'T1
'" •• Z -t
:::m0
m
(/l
-45-12
::t:
-1~
•
~
• 321 (of 550 ) 2006(-2016)
322
'I "JITTER· CIRCUiT: OPT/Ir4IZES
STHEAT·A CIRC UIT BO ARD LAY OU T
TEMPERA TUR E S r ABILI7 Y "-
.
R"
1M
ZERO
POT
:/•
~ " 02 "
UU24
Rn
R5 ~ ' ,W
I
1M
JI TTER OUTPU T TO DETeC TOR HE AT, A ND
CHASSIS FAN CIRCUITS
40.2 K
NV -
•
+6V
1M
•
R10
. lC:
10K
0.1
6
Reo
.
YELLOW
GROUND
., ......c"'_ _
7
..
f], ........
_. .".... --
~.o ••
~~ _0
5
,
,
LM3~1
RED WIRE OF PflONE CAB LE TO DISPLAY BD. " TOTAL SETPOINT" I PUSHB UTTONI
/
•
• •
f
-, COMPARA TOR CIRCUIT: COMPARES THE A CTUAL TEMP ERATURE (PIN 9) TO THE SETPOINT TEM PE RA TURE J 1 (P INIOJ
3
TI' E UIJ14·, INn ilS
._-1--.."..,."..,.--., ",_,
~
I
.".
r+ ,,'~' • QtI .L 1 .L ell . ...! 9~, -'" I •., <' ". ':.':'1" T"'''' "
CIA CUIT OPERATe
USING .I N OH PIll 4 ,UlO ·I!VOHPlH ll,
. ...." c... n
' ",,,c uE()
"M
~ ~,
l... UEI
~,
...rul
oM IBM" ......1
' BlU~ 1
1N S14
0
~GAT EM
U' MOC30JO (220V-M OC304 1)
1" (
SPADE LUG
O'~ N
I ~ IA(: , I IolOU', u n
ON 1MI':'fn IC," , " I... O\'lN MUlU
II" COIU
,
...
.
TO 12
_~~.J )u f1"iVlMJ24 /
OI'9 ~
A0597
. -. ~ _.......,
~ ~,
-.NV'v
R3
0
1M J:1~r~
Ul lK
. ...nc ....o
1 WAn
10
THERMOCOUPLE AMPLIFIER CIR CUIT : DE TERMINES ACTUAL H,MPERATURE OF COL UMN O VE N
Ro
R12
.
'.._ """...'.... • ~
.. • •
COl UIl4N o v e N HE-'TE R CO ll
100 O HM
lM324
POWER SUPPLY SECTION
'''I ' ' 'UC''I'O\'III l •
, .,<
1 2 3
AC O UTP UT TO
sc SWITCH ING
J<
!
HEAT C IRCUi T
TEMPERATURE
TH ERMOCOUPLE
r:
<.' 0'1 '
OVEN
"' ~ AT
CIRCUli
CIRCUIT: SWITCHES A e TO OVE N HEATER TO ACHIE VE DESIRED
PUSli6UTTON S)
AMPLIFIER
S! I
"'
RO
U2
1 V"
1M
DISPLA Y L..-""="-J
THi'RM OCOUPLE INPUT f~ OM COLUMN OVEN
,
10K
I1
,
~
•
J<
SETPOI'iT
.
10K
2
~ 1 rJ.- ~ =~~ ~
,,, ,
,,.- " , ,, DEfEC TOR: ,, ,, CIRCUIT ,: ,, ,, ,
J
1
~~ ,
Rl1
43 Hz
R7
~
TOGETHER P RIOR TO THE COMPARATOR CIRCUI T
-12.V
-6 V
2QK~~
",REEN WIRE OF PHONE CABLE FROM
AND THE se r pa/NT
10K
SE TPOIN T CIR CUIT: US ER ADJUSTS TO SET DESI RED TEMPERATURE OF COLUM N OVEN
COLU MN OVEN LOCAL SETF'OINT: (LOCAL AND TO- A L
SUMMING CIRcum AOD S THE JI JTER
RO
»:
ON THIS BOAR D
Ro
,,
...
<,
"" 1M
OlSPLAY B OARD
+12\1
~: HE AT I
, 1- -,, ,, ~ ,,, ,, ,c --
,
,,
~ I OVEN .
O FFSET
UJ
C3
1M
R14
OVEN HEAT CIRCUIT
R' 'K
J<
~
DISP LA Y BOA RD
-, //
BLACK WIRE OF PHONE CABLE TO DI SPLAY BO. " L EO M
Leo DR' VER CIRCUIT: YELL OW WIRE OF PHONE CABL E TO DISPLAY BO.
PROV/DES VISUAL VERIFICATION OF HEATER FUNcnONS
··AC TUA L~
{PUSHBUTTON)
CAu nO k: ACHOl AHllACC ARE H.UAAOOVS VOlTAG ES AHOARE PRUE/( T 011
nU S .vIOOfHERC'flCUlT lIOAROS
POWEll IS ON.
WHl~ E
filii O,C,
P1001 or 3
STHEAT-A1 -1 SCHEMATIC 'alo; 1 lTiQi~t V. n ate: 05115101
av- R ev. R
u 'FER
322 (of 550 ) 2006(-2016)
323
( STHEAT·A CIRCUrT BOARD LAYOUT
DETECTOR HEAT CIRCUIT
t : lIEAl
••v
NV
ON THIS BOA RD
·.V
R.
1M
R'
a
120 K
-
FOR Te o
J1
.,
\
GREENAH D
DETECTOR HEAT LOCAL SETPOINT: lLOCAL AND TOTAL SETPOlNT PUSHBun ONSI
RED WIRES OF PHONE CABL E FROM DISPLAY BD.
'M 1M
r
J:'
~O_I ,F
RED THERMOCOUPLE INPUT FROM HEATED ZONE
YELLOW GROUND
. 13 {
uv
n A
B
••
•
10K
U' ~
I'-LMl"
TEMPERATURE (PIN 9) TO THE seTPOIWT TEMPERATURE
-If
10K
S '
J
/
10
:a- r" +12V le r-.l .. " 3
1K
JUMPER PROVIDES +12V TO HEU CIRCUIT
r--"
CIRCUI T:
~324
SWlTClIE S A C
UI
A0597
THEUIJU', IN THIS CIRCUlTOPERA.TE US'HO "2V~ PIN 4
AND·1lYO NPlll l!.
,, ,,
:
ro
S WITC HED
INPUT l DLUE)
I BRQW Ht
10 U2
, -/
.,
01
•
1N914
1000HM _ 'WATT ...
,I a
6
5
100 0 ,"M 1 WATT
~
R12
I--
1N40C4
O_1 '~ I '
l M'"
CAUno'l: ACH OTA.ND ACCOWMONAJU! HUUlOQUSVOLTAGES ANt! ARe PRES EN TOH THIS .0.Io1O OTHERCIRCUIT llOAADS.....HIle TIlE ac, POWEll IS011.
II
SCRI
• I--T
Q"" / U 0215 SIII)HI EO/ f OR m EECO AND1HlflMAL
02 ,t,C OUTPUT TO HEATER
Of' S O ~ DEII
"
U2.
Jt •
INP U T
U. MOC 3030 (220Y·MOC3041)
J1
_/ '
,. . _,
AC COMMON
It EATUl S
c~ ~
HEAT
( 1Il-CUlI
AC HOT
DETERM INE S A CTUA L TEMPERATURE OF HEA TED Z ONE
3
OVEN
SWITCHED
AMPliFIER CIR CUI T:
R1
1M
,,, ,
H EA TED ZONE TO A CH/EVE DESIRE D TEMPER ATURE
••
14
~ -/
7
HEAT CIRClJIT
AC SWITCHING
TH ERM OCOUPL E
THERMOCOUPLE AMPLIFIER
,I--- ' • f--'
I I
,
LMJ24
1
, DI!TECTO R::
R"
COMPAR A TOR ClnC UlT: COMP ARES <, THE A CTUAL
(PIN f O}
_
+
&
-,
R1
'OK
U.
CIIASSIS
~
• -x, r
10K
-:-1%' :: 3 LM324
SErpO/NT CIRCUIT; USER ADJUSTS TO SE T DESIRED TEMPE RATUR E OF HEATED ZONE
,,
COOliNG
>io ',, ''''"' <
RIO
US -........ t
+12V
;J-l "'
m
I
10K
DISPLAV BOARD
R,
>, ~I
ADDS THE JITTER A ND THE SerpO'NT TOGETHER PRIOR TO THE COMPARATOR C1RCUjT
OVENCIRCUIT
43Hz
-- , ,,,
.. I- - _ .J
SUMMING CIRCUIT:
J ITIER INPUT FROM
•
t
, 1- - ,, ,, i ,, ••e ,,, <~
,,, ,
,
~ tOYENI
* I
YELLOW \/t,RE OF PflONE CABLE TO DlSPL,t,y BO. " ACTU,t,L" I PUSfiB UTTON)
1 13
W
1K
LMJ24
'0
DISPLAY BOARD
ff
BLACK "'IRE OF PHONE C,t,BLE TO DISPlAY BO. " LED"
/
LEO DRIVER CIRCUI T: PROVIDES VISUAL VERIF ICATION OF HEATER FUNCTIONS
STHEAT·A1-2 SCHEMATIC
Pall _ 2 013
)FUenl me: s lhnt-11·2.lcw
RE
Dale: 121 20'97 110· 0515
8 : R. re ~ 5 ke
t iler
323 (of 550 ) 2006(-2016)
324
STHEAT ·A CIRCUIT BOARD LAYOUT
.
CHASSIS FAN CIRCU IT
~:H EAT I ,_ _ _ J
. ,v
NV
~
SUMMIN G CIRCUm ADDS THE JITTER
JITIER INPUT FROM OVEN CIRCUIT ON THIS B OARD
43Hl
·
5.11>1
13
-=v
/
12
RI
' OOK
'M
UK
R'
02
\
1,
1M
10K
•
:k ..di-
C2~O.' I
0
o , ~
l M' "
III'
•1-'....
10
COMPARATOR CIRCUIT: COMPARES "THfACrUAL TEMPERATURE (PIN 10) TO THE SErpO/NT TEMPERATURE (PIN 9'
.....!. . U2
-10 ' lM324
8
LM3Z4
R3
~.
,
, ,,I DETECl O/! ,, ,, fl E AT C IRCU IT
lO' OHM 1 WATT
28 VA C
RED
WIRE JUMPERS
1 WAIT
r:: of-! 'I=:-,
ClO 10 uF
~
~2 a6004 / ~,
OP TIONAL R ELAY CIRCUI T
ENABLE (SOFTWARE
1
..:=
3
'f-II r- . 12V
5
6
~ 2
A CTlVAT EDI [ SP AC E LUG )
::;..-
~I" R'
r-e-
10
,
7
/'
~
u'
A06'7
10K
1M
. 1
SC R '
THERM OCOU PLE AMPLIFIER CIR CUIT: DETE RM'NES ACTUA L TEMPERATUR£ OF
E-:: 'r
R12
1N4004
THERMOCOUPLE AMPlIFIE~
WIRE
-,
/
(22ov ·MOCJ 0411
4
0
CI RC UIT
WHITE
100 OHM
2 :)
M
OVEN HEAT
26VAC
U. MOC3030
1
1N9104
,,- -"
AC SWITCHI NG CIR CUIT: SWI TCH ES AC TO CHASSIS f AN TO ACIIIEVE DE SIRE D TEMPERATURE
~ ./
"K
LM324
~
"K
R"
U5 ""- 14
TEMPERATURE WITHIN CHASSIS
R7
. ~<
I
"K
i,
CHASSIS I COOLING l , C IFl.C UIT
-4
;:::
011
SfTP O/NT TO COOL
RX
-
TOGETHER P RIOR TO THE COMPARA TOR CIRC UI T
R'
VOL TAGE D/VIDER DETERMiNES FAN ON/OF F
-uv
~ I
AND THE s e r Pa lNT
..
,
, 1- - ,, ,,, ~• ,, " ~ ,, < ,,. -- -
,,
~IOVEN I
OUTPUT TO CHASSIS ' AH
CHAS S IS
Rl
3
c~
O '"~ I
I>--
U2 "
./
2
1
LM324
t12V
L©~ '2 N390~
RELAY
e, 1 'til NO COM
THE 1I02.·,1H THIS CIRCU ITOPERATE USIllGU N O" PI'I. ~ N lI . I N O~ PlN lI
CoUTlON: M:1I0 T .lHO .t.CC(Jt,Ot.IONAAE HAWl00IJ9 VOLTAGES AIOARE PtlESUH ON THII ANOOTHERCIRCUIT BOJ.R lIS WH il E THEG,C, !'OWER IS 00.
I Pall'
3 01 J
I Flhtn. mo: "lloal-11·J.lcw
STHEAT-A 1-3 SCHEMATIC Il IO : 1 212 0~
, 11. : 0
.
II
324 (of 550 ) 2006(-2016)
325
DISPLAya OARO
R. J2
l!:!f
(PU SHBUTT ON I
~
0.1 uF
'2<(' <:
2 £1'10
/
PRESSURE
6e
+i .IV
orrs!J AD JU ST 62K
SEHSOR
• •
.,.
~ R
ua r )--_00-"
r;-i/l.M324
_1.2V
L_
,RI
IK
"...
no
I
i)i)K
'\.
••
3
PHONE JACK TO SENSOR .ALL WIRES)
, ..,..
. ....
J3
R6
...•,.
""" 0 . _ ••
G ~ ","
.
•••
F~ ONA C
DISIRIB UTIO N et:l~RD
,,-
IO"U "
v
'''I
14
I ~ J2
[@
C/, TD C IlASSlS GROU,",O
100K
/
R18
D2
--l "
~ ~ _'" . r;;'t;', " .."Ct. To ,...
--. ... " ,,,.
._. •'IY
,, - i
I
E lEcrRO~ IC PRESSURE CO ~TRO~ClR CU IT
,~
'' ~.
~ - - - - - -- - - - - : ~
, ~
HIGHIOlTMlE
,," -
rowcq,SVPl'\.y CI~C UI T
AN EXTERNAL INPUT (10mVlPSJ) IS NEC ESSARY FO R COMPU 7ER CON TROL OF THE EPC.
DISPLAY BOARD
J2
-;;
l ED DRIVE RCIRCUI T:
IK
P II'OVlOE"1 VISUAl, VE"R'I'lCNION OF
11'491 4
/
I',r
EPC F UM: rlONS
BLACK WIRE CF
.... "
,-
.c.
B l ~ C K WI ~ E
POWER. SUr'PLV S£ Cl~ 8
To...
, l'C . . .
TUBE (page2).
,,"
S,.AN
b"
\ EPCHI.D CIRCUIT BOA RD LAYOUT
THE EP CHI B OA RD PRO VIDES ELECTR ONIC PRESS URE CO N TRO L OF ONE GAS (pnge1) AN D ALSO PR OVIDE S THE HIGH VOLTAGE N EEDED TO POWER EfTHER THE PID L AMP OR THE FPD PHO TO·MUL TlPLlER
LM 3H
1M
.. tlJtJST ~
"'iiii'"
. . .. 1tO
SeT POlN T~
(PUSHB UnON
/
~
1 I NA 1l..
•
~
-T OTAL
1M
RI J .JK P 1 20K
r1
U2
R ED ¥\jIR E OF PHONE CABLE TO DIS PLAY B O.
.,
'
•
O.1uF
'~
"" ".l
_
'
ri l-
~
LM324
I
20 K
LM32.4
CIRCUIT'
\
•
r,
13
" R!SSU.'lE SENSOR CIRCUIT: . / ' f'II'CS!U.'lP.
U2
Col
12
3
62K
/
CO...,P ARA TOR
OETERMIHP.S ACTUAL
+1.2V
1.
U3 ..
C'
29.5M
IHP. COMPARATO/f CIRCUIT
,
R"
12
1M
1M
GREE N WIRE OF PHONE CA B LE FROM DISPLAY 90.
R'
R10
R29
R3I
R12
-,
OESIRED PRESSURE
CIRCUIT ,
lO CA LSETPOlHr
AND f)(TER HAllHf'UT TDGf TII ER PRIOR TO
~ IO.1U~
10K
l'
SErPOIIoiT CIR(; IIl T, UU R ADJUSTS TOSET
ADDS
lOOK
RJO
FOR CARR!FR THIS '5 A GREENiWlII TE WI RE
I_I
"K~__
RJ
-
.....
5U~IoIING
c.. ~ ,!tt ""(KI./lAtol
_ I ....... O'O~ II • • ,
R10
111ir
AlD BOARD 110mV- 1 PSIl
+1ZV
Ul _I" ' "
• ••N . 110
EXT ERNAL INP UT FROM
",Y
". ,. o.
PHONE CAB LE TO DISPLAY 8 1). " LI'"D"
. ~ . . ~
l" '"
·' .IV OIlff'UT
'" "
I l"" " -
"'" ...
.~
." . r .J
..
I oJ I .......
u
l..L')U
Pa ll1t1 ol Z
Fllonamo: opc hl·b .lcw
EPCHI-B SCHEMATIC By:-R. Ft ~,k •
Dale: 12120197
Re.... Delo:4'f7]OI
325 (of 550 ) 2006(-2016)
326
._•••._. -
.
."' .,T,...",.... ,N"
..-.' ..., ~-. 000., ........ "' , -..
DISPLAY BOARD
• , 2V
_
. ...."
.... ......... . ... , .... _ ......
-
('I
~
~
SErPOIN T CIRCUtr.. USER ADJ USTS TO $,£1
-
r
10K
LOCAL SETPOlNT: IPUSHBUnONj +'.2V
~
I
PRESSURE Sf N!lO",
.. _
R4
-TOTA L
SETPOINT{PUSHBUTTON)I
@]"
R
G
"'
1K
J2$ 1K
R2 UK P 1 20K
n,.......
o.
"0 ". n
I r-r.'::-I
lJRU k
/ . BLACKWlIIL! To eH AS! IS
R16
I~
GROUND
/
L ED ORIVElf CIRCUI T; PROVlO£ S \l7SUAl VCR",ICA r lO N OF
(PUSHB UTTO N)
R18
D'
1K
Yr 1N91'
X''' T, ...
,
ElEC'RO~I C
CONTROL CIRCUIT
Hl GHVOtUG E POW eRSUPPLY CIRCUIT
.
,I j!l
1 -<
,r- -
._ •••. .. -.-
~
<11
....T... To ,..
.".
HIGH VOL TAGE N EE DED TO POWER EITHER THE PtD LAMP OR TH E FP D PHOTO-MUL TIPLIER r UBE (pag e2). AN EXTERNAL INPU T ( 10mVIPSI) IS NECESSARY FOR COMPUTER C ONTROL OF THE EPC.
J2
DISPL AY BOAR D
/
ff
BUC K WlRE OF ft1 0N E CABLE TO DISPLAV 80.
.,w ~.
ML ED
M
,.
. ' .' VOUTP vr
."
~.
, ,;
,PRESSURE :~ ------- ----- Ilg
EPC FUNCTIONS
" n ..
v- r-sa
G''''''''
J3
POW ER SJPPLY SECTIO "fS
t"'iiii"1
••
VlM 324
a
l OO K
" ACTUAL
--- -
G
1M
PHON e C ADL E T O CISPLAY BO.
R1
~EG U L.ATO R
/
'~
3
TO
TIP 100
1N91.
R8
PHONE J A CK
a,
Dl
-eucw 'N IRE OF
t
,,
,- ~
ALSO PR OVIDES THE
+ 12 V
M
lKl "RD
rlf-
1M
R17
' 1I0MAC OISl R\lUTlQIol
DISPLAY BD.
p neSSURE SENSOR
~J
•
THE EPCHI BOARD PROVIDE S ELECTRONIC PRESSURE CONTROL OF ONE GAS (pa ge1) AHD
· 1.2V
.-
O.1 11f
1M
I
L......
C4
R14
~
~
P2 >OK ~<
_.....00
I
R9
\
, .....:................_ _.... ,
CABLE TO
R12
CIRCUIT: Of:TERAlINES ACWAl ,,/" PReSSURE
~./
OF PHONE
R15
3
.2K
CIRCUIT
DE$ IREO PRESStJRE <,
GREENWIRE OF PHONE CABLE FROM DISPLAY BD.
EPC
THE COMPARATOR
RED WIRE
I O.1uF
R"
~
TOGETHER PRIOR. TO [
~ .1 . ZV 2 9,&M
I I
EPCHI-B CIRCUIT BOARD LAYO UT
A ND EXTERNA L INPUT
R>1
1lOI<
R30
FOR CARRIER m ,s IS A GREENlWHilE wrRE
rr
.... 'N """"'D ,.,..
' 10 -;
SUM/tIING CIRCUIT, ADDS L OCAL SETPOIHT
A>1 _ ' 00' It CAAl't.. ~ PlI QGIt .... ~ AiD
I~. . . . . .
"' .,.., ~u,," u
.....
R,
Rl
)
)
')
~"
......
'. ' F.Q "'
~
ft n
'ooK
r ,•. J ~.
11
~...
". I V OUTr UT
ti- ,--_...L-' ---= --
PIgl 1 of 2
File na me : epchl .b.te w
EPCHI-B SCHEMATIC 2120111
'ale :412110
BYi R!F.n. ~ e . M..,rjj
326 (of 550 ) 2006(-2016)
327
"JITTER" CIRCUIT: OPTIMIZES / TEMPERATURE
R14 ~ 1M R19
P
•
0 .02 o f
.----i.:-
•
V3 •
/
13
RS< 1M
DISPLA Y BOAR D
a
+12V
U3
R.
2OK~'"
" . ~
I
v
i _ _
~
R1
I
,
R~
,.
1M
RED THER MOCO UPLE INPUT FROM HEA TED ZONE
YEL LOW GROUND
~
RU 1K
I
SErpOINT TEMPERA TURE (PIN f O)
;
.-. ... ,
coou..
.... lfll...
U3
7 SW ITCIi ED
SWITCHED ACHOT INPUT I BLUEI
~LM324
ACC INPUT (BR OWN)
100 0Hr..'I
10
~)
•
•
• .•
01
1 WATT R12
~~R1 .'N~~04r=--±,
1N9104
1 ~~ 0' 02 IS SHORTED
LM324
AC OUT PUT TO HEATER
AND THERMAL
OE$ORHEM HEATERS
DISPLAY BOARD
12
. , 14
R6 ......-N\;
C' U1
I
I'""""""'l
0.1U[
V
_
c.l
en
I'
FOR lH fECO
THE L lll n4 ' 1 1 ~ THIS ~etlTOI'ERA TI!
....'1'.... To, .. _~l ';" ..r;!;, - - -• • •
~
..
USIf(I .UV OMPIN4 AND ·UVO ~ P I N 1\
I
I
/
I
YELLOW WIRE OF PHONE CABL E TO DISPLAY BD. "ACTUAL" IPu SH8 UnONj
LED DR IVER CIRCUIT: PROVIDES VISUAL VERIFi CA TION OF HEATER FUNCTIONS
CAUTlO N ACHOT AND Ace ARE H,ov, I{DOU$
VOU AOU lIlD AAE TH'S AN D
PRESEN T O~
fi J1
~
2 VLM 324
" U
en
1K
I~
3 '6 r-r -,NVv-l-, f' , 1M _ v-I ,. ,
I ""h
• r'
nO: T O:D . . IlIO:~ ""TI ',, '
/
ADS91
1';;;, .. ,J;1<
R11
THERMO COUPLE AMPLIFIER CIRCUIT:
THERMOCOUPLE AMPLIFIER _
I . .... I .L-""'T""
•
OF ALL SIX SOLENOID CIRCUITS AND BOA RD lAY OUT.
CIRCUIT: -,
rV"
fit.i1
•
= . ~ = ...... -. ~~
1
..
LM324
....'....._11_' . "'''..........T,..... I
R10 &
POWER SUPPLY SECTION
.., c,,, ~.uno .IO'"
HEAT CIRCUIT. PAGE 2 DEPICTS THE SCHEMATIC
10K
......
COMPARES " THE ACTUAL TEMPERATURE (PIN 9) TO THE
C2
5
SINGLE HEAT ZONE INTHE G.C. ( Ie TCD 8LOCKj HEATED INJECTOR; ETC.). TH IS PAGE DEP ICTS THE SCHEMATIC OF THE
10K COMPARATOR
•
• • ~:ra; li
10K
R8
(L OCA L AND TOTAL SETPOINT PUSHBUTT ONSI
-
R'
SUMMING CIRCUIT: ADDS THE JITTER AND THE SETPOINT TOGETHER PRIOR TO THE COMPARA TOR CIR CUIT
'v.
3
THE SOLENOID-HEAT BOAR D CONTAINS SIX 120 VAC. OR 220 VAC. SOLENOID CIRCUITS AND ONE SINGLE HEAT CIRCUIT.THE HEAT CIRCUIT PROV IDES TEMPERATUR E CONTROL OF A
HEAT CIRCUIT
10K
SEr pO/NT CIRCUIT: USER ADJUSTS TO SE T DES/RED TEMPERATURE OF HEATED ZONE "-
LOCAL SETPOINT:
,.""
+6V
LM324
~.1_M
R13
-
43 Hl.
V3
LM324
I
14
-
NV .sv
STAB/UTY
12
1M
- -
PIgl1 012
OnER CIIlCUl BOAAllS
WHI,E TliE G.C, ~OWE R IS OH File na me : s olhe at.1 PlIUew
BLACK WIRE OF PHONE CABLE TO DISPLAY "L ED"
80.11
f '
I
SOLHEAT-A SCHEMATIC Datil: 211 ....00· Rev. Dale: 311 5/1
B\f : It
PFEIFER
:R, PFEIFER
327 (of 550 ) 2006(-2016)
328
)
upV ·m
CIRCUlT , 1 IS THe ONLY SO LE NOID CIRCUIT THA T DOES NOT HAVE A NORMAL LY C LOSED INPUT.
SO LENO ID
INPUT FR OM
SWITC H ED ACHOT INPUT (BL UE)
A ID BOARD
.
,
3
Q6oo4
SCR2
'"
'''-''''
'"
~'M
s2
~ wnC": D
S.... Il;ItLD
ACH<.lT II'lPUllllll.l! .
~,
N>IIT IBROl'lINt
100 0HM _
..,' 'M
. •
••
• •
1 WATT
-
~,
"n
ACOUTPU T
OC ~
'"
I
C
';"
I ,
I I
» ;ll
,I
'L
"
,.,
1
~
.
AC
I
IID~OllO
~ ~,
~
......,.,. (IILUPJ
IN""I CUROWNl
. 4
'5
ill S
E TO C
JU MPER
I
•I
IU D
100011 .-
•. "" • ••• ~••T
, W I Tl:tED
• Tn ...
.. .
, ,- '"
~.
'"
10 0 O H M
- ". U Y OPE.. It' PU I
-'-
I't, O
~,C.
'
JU" fE R
, e TO C
10K
t .. n
..
o,
'
I' W "TT
r-+ ~,
ACOU II'U l ~
..
.. ..... ,
,~ .
'"
HOJ\llll
,,,
\
t:l
, 00 OI-
,
JUMPI'R
:
AC OUTPUT
S4
SOLENOID CIRCUIT
......R O
~
.n
--
IOLH IOID I NPUTS
__ ••
SWiTCIIUI
S WITCHED
N"Jl 11lRQWN1
- --
_
"n
S5
."
~, , e roc
_.
''
X "'
_.
8 OLP~"""
-e
- _ _I
QI ON
, w" n
I
~
"' C HOT
lU I M O~:O:ICI ' 0 0 OH M 1 W" TT 1. ,.,I/·MQO;;IH'1~
.....---.
!::
SOl ENOID CIRCUIT
•
~ >
3
ou v
I.... U '~UEI
IG G O HM
011'"
,- - -
,,
,,
I ~--,
SWl TCIlr o
. 3
M' ~
SOLENOI D CIRC UIT
S WlTCftl!D
2
••
.......LYQPr. N ..PlJ1
SO L ; HEAT ,
-r. ,. '~ - ............ . , ~m~J V
'M'
'"
SOL :
~ Ofl M . L1.Y C ~ D
s3
I
,I
~
AC OUTPU T
--" II . _
_on
_.q .."n,
""~ uu
E
=:3 1
"ft !
SOltNO'U
. . .. . ~ _ _
I
I
"
~
ACC
~
SOLENOID CI RCU IT
"n
I
t
ICIRCUll lclRCUrn:IRCUn):; ,RCUlrc IRCUlT CIRCUIT CIRCUIT,
INPUT (BROWN)
L
R22
I
I
.
SOl. I SOL I SOl. I SOl.
ACC
o
I, 1
"n
m"..
SWITCHED
1 WATT
1 WATT
'''''\IlS
SOl HEAT· A CIRCUIT BOARD LAYOUT
100 OH M
100 OHM
IIOl !'fOID
S1
SOLENOID CIRCU IT
~ TC H r:U
AC " OT
ecc
"' Pur Ifl i ,," .
'N.....' 1.-0<'
tO O O HM
t W AT T L
~
I
~ACOllTPUT I ~
I
THIS PAGE DEPI CTS THE SCHEMATICS OF SOLENOID CIRCUITS #1 THRU #6 AND Of THE SINGLE HEAT CIRCUIT.
PII{I.2 01 2
SOLHEAT-A SCHEMATIC
Data: 211&100 Filename: solhll t·a pg 2.tcw Rev. nate - 3H5I01
BV: R.PF EIFER
OR
328 (of 550 ) 2006(-2016)
329
, HYDROGEN GEm.. •TOR STANDALONE · H2·50
~ •
12 VOLT INPUT FROM E Il.TE RNAl CEAPPROVEC POW ER SUPPL'(
/d
..- •
CENTER p o sITIve OUTSIDE GROUND
3SPSI
PQWER JACK
PRESSURE
/
~
II
SWITCH
I
7 A MPS M INUMUM
io !•
~
~
•,
~f VOC~ '"
~
f&
CURRENT LIMITI NG CIRCUIT 6.6 AMPS OUTP UT MA )(IMUM
:ff' " lJ, ~
5 5
(: HASI$
~
1'-./
•
\ lM 33S
I
I
REGULATOR
I
BOTTOM VIEW
~ IIYDROGEN 6 f Nf' Il "T~
P_un 1 01 1
suereme: hydiJon.tew
HYDROGEN GENERATOR HZ-50 SCHE MATIC L...l&1i;,.tltlI09/0Z
Bv:M.WATT S
I!!if.1i"
329 (of 550 ) 2006(-2016)
330
,• ;
L'
•
-=- -In"" ~lli"o jlO•• -;!ii . .... ~
=J I. o
0-
<>-
0
•
0
•
• 0
• • • 0
•
0 0
•
0 0 0
••
'" OlE ~il··""' '' :c~: o. s; "' ,. .... i i~i:1 .. n~
~ i ;: " ~=~ ~:.§ ~:! ~ o·l::°~:S:" ~ ..
.~iiih==li~;~ , :=; ~ p o. " •
" (l
•
•• •• ••
h o .w:.. .
J : ~ i ~:~~ i~! .. ii S ~i:::;:;"~ :;S
•
00
0-
•• •
<>- U •
•
••
•• H • • " •• •; 0• ii •• ! 0
• •• .0
o '
•
~
!•
~
II N ~
0
W
""
C
0
~
~
c0 ~ ~
~ 0 ~ ~
m
~
',•" ~
• ••
-e
•
0
• a ~
~
N Cl
l::!
>8
~:e: c: O
-i0l
lJ>O
:I>
::tl 0
330 (of 550 ) 2006(-2016)
331
Thermocouple Conditioner and Set-Point Controller AD596*/AD597*
.... ANALOG .... OEVICES
I
.-
ADSt6lADW7 FUNCTlONAL u.oat DlAG1lAM
FEAnJAES
u-e..t ot-- with TvP- J lAD5961 Of T'(I» I( 1AD55l71
-..-
~1t
Ic:e I"1:IinI Corn~
-'~ .
T.....pentulW P' OIMH do nll ~ _ 10mVI'C
T""'J*'Iture SM-Poin1 OperWan _ ONIOFF ProgRmm--. SwltdWn, Hyste..... Hlg"
Im ~
D"'--tl. II'lput
PRODliCT D£SCRIPTION
The AD5961ADS91 has . alibntion a<:rnrxy of
The AD59&1AOS91 is. moaol.idlic teIIlP=nue set-poiat CODtnllIc.t whi<:h bas hem opcimizm for 1lX at '*"'aced ~ s=b as tIxM fow:d iD 09Ul eooJ::ld.lfll'tiaric- n. <1r"ri::c' colt jugo;ljc;a...-pc::>UbS ZDCl uaplitic:I a ~ J .... IC lhe:_pje iDplLl to dcrm .. iD-...l ,...,. proporooa.al to I<:mpcn.Mrc. Tbc iDlCroIl ~ is iheD lXXIlpaoxi WIth au estenWIy appI>edllr:t-puUll ooI.lq'C to yjdd a lowimpedalll:e nI'lIdloed 0UIplI.1 "O.l• • Deld-BancI. cc switchin& ~ CIJ!I be ~ srammca Il:Siq I ~=ana.l rcsiswr••o\ItmIaldJ. t1le ADS96' AD'l97 CIU:l. be ~ 1(1 proridI: . 'I'lllace.-pat(lOmVf'C) o;iira;.-lty fmm . ryp: J OJ K ~ siJDaL It CID also be-
ambien l
uxd
IS
a sttDd.a!oDc""tIKl= output
ADS%I~97~ .
indKaIes aa
l!lmDocol1p!e failure aIana lbaI
tbl:l'1DODJUp.. kad "beD opertced ill tbe
TTl. •
llpCD
It
J.tI
KaInC1. « a Iuoou amblcDt
a
ambie:llilanperarure S(abili[)' 2S"C to + lOO"C. If IUP-
~ ~
al1ac:r doe,o.mw 1:hcrmcc
is-nquira:l ,
~)
PRODUCT lDGm.IGKTS I . The ADS96'Aom prtI'ridn C'014 iuaaiDa ....lDP""urim aDd .. hipl piD ~ whidI em be tad u • sa-poiDl computtor . Slagle of t1M' AD5961AOS97 is. hiP quaJil:Y iDmumc:nwiOIl :amplifier lhal a1IoWs t.tle !hemlOCOIlp!e to Oftr most of doe vol t . nlnlf".
2. The iDplu J.
sdf~1 rrrurI.
~4"C
•
tem~ of 6O"C aDd &.II.
rpccifif;atiga of O.lW'C!'C fmm .
,..... fftl TIlr': seDJIIlO" .
TIle AD~~Y7 CIII be ~ witb • ......, supply from +5V 10 +3OV, or dual ~ a.p II) a IDlIII s:pu 01 }6V. T)'J':IDl quieIc:aII: supply = t is 16OIoA wlacli minimizes The
11
""pp1,
n..,
~ _ nquind [or tbcrmoo;oupIe 'cmpeTlllUa dole to 17S"C ( + 100"C to ... S4O"C for AD~9lS). • . Cold iw>ctXm wmpcnatioa is ~ f« :mIbieDt tmlpcI"' In\n!ll ~ &om . 2S'C 10 _ IOO'C. 5. In the ~ modc: , the ADS96IAD597 producao an outpur volup tbat iI:Idi=ta its OWXI tempcnrure.
.
The ~ is ~ in a milbiliry qlU1ifiel1. 'WI: etro;tive 10-piJJ ~ CIU:l. aDd i& trimmed 10 open.tc o-oet &II ambieal lCDl~l'lItun: I"UIIe from ... 2S"C 10 .. lOO"C. ()po::nDoa (Iftr an CZlCl>dod aool*m ~ ~ is posDbk 1rith WdIdy rMuad KI:II:I"aCY. Tbc ~9'6 ril ampIifJ rlw::t llkC:O\lPk sipUs """""""'" du:.....n - 2OO"C 10 ~ 76O"C tlDP"""lWl: nDF 1'"'fCII~ for type J thmDoc:oupIes while the ADS97 em ~~1C - 2OO"C II' + l ZSO"C ryp: K inputs .
'rF;MPERA TURE MEASUREMENT COMPONEN TS VOL J. 8-39
331 (of 550 ) 2006(-2016)
332
UItra-low Bias Current Operational Amplifier Op-so I
APPUCATIONS •
Elitl:*GI .lsrAmpll8w~~
PI! CONN£CT1ONS
• ~andWr'Mld DeIedor"""'PlflBr
• ChemicIIMCl GIl..."..
-,....
-8~ ... '"'
• pH PnlIle 8UIIW AmpIIIer
• FreDlllcklrl • High~YoheI¥i4 • a.geAlilPtiitta
_
•
J
...
s-.u,
~.
8-PIN PlASTIC DIP
GEIlEIIAL DESCRIPTION
...b
.
IV
»r .
...,...
&oPlNSO
cepUonaJly low input <:Un'9fttS overa wide operating temPera-
.....D'-.L
, y. IC"I"'I
''.It.l;
(P-suftIx)
TheOP-80jaalowcostCMOSOperalionaC~affemgex.
~
~
-.)
($-S-)
S1MPLFlED SCIIEIIATIC (
-
...
-.
-H~
~ l.< ~rl '" I
rJr
;;::1
l ,r
'-i,
''1
-.
-
n
(I
II
,I-
,t-
y~
'I-
~
-1r
t-o....
WD
':I,
'"
t;;l,J-1~
JI:::
'1
D
t' '1
~
332 (of 550 ) 2006(-2016)
333
For Immediate Assistance, Contacl Your local SalespellOn
S BURR-BRm IEIEI
:-
INA114
Precision INSTRUMENTATION AMPLIFIER FEATURES
DESCRIPTION
• l.OW OFFSET VOLTAGE: 5Oj.l. V max • LOW DRIFT: O.2~vrc max • lOW INPUTBIAS CURRENT: 2nA max
The I:'i'A1 14 is &..".. cost. ~ purpose iIlSlrJ:Tlell° tJ.tiOn a:nplificr offeri "c excenrlll ~. Its versarile ~ amp design and l lIlll11 size: make il ideal for 11 wide rw.ge of.applications.
• HIGH COMMOH-MODE REJEcnOH: 115d8 mil'l
A sm(le extemLl ~UI[ iCU By gain from 1 to IO.lXJO, lntmaJ inpur proo=aioa COllI withstmd lip 10 =-'Ov wiIbou l damage .
• INPUT OVER-VOlTAGE PROTECT1ON:
""'"
The INA114 is laserllUJUl1Cd forvery Ja w offset V(lltage (5OILv), drift (O.2SIl-YI"C) ...,4 hip common-mode n::jeai
• WIDE SUPPLY RANGE:::2.25 to ±18V
• LOW QUIESCENT CURR ENT: 3mA. max
• ~ PlASTIC AND CERAMIC DIP, SOL-1 6
APPLICATIONS
The i:'JAl 14 b available in g.,pi n plastic and ca'alllic DIPs.. md SOL-16 surUce -mounl padaga.. specified fur Ibl: -lO"C to ...a5~ lemp:nlUn:' n.D!c.
• BRIDGE AUPUAER • niERMOCOUPL,EAMPL.lA ER •
RTD SENS O R AMPLIAER
• MEDICAL INSTRUM ENTATION
..
• DATA ACQUI$mOH
1 TI'3l
v.. (4) ': ~
,-.,
O'-....
~t-~
'" •
.
'.
~
,-
> ,r"/ ... ~
~
j
(i~<
,•
~ ,-
"
1" 1
,. ,
r-<: I
..... ".
~,
L~ I
~~'":-~~
,
""'
r-Cl
G . h~
~
0<1'--- ",\'" "'-(SCE!
_ _ __ . -.._'O .. n_ ~....."
4.74
...,," • ' ...,"MR·"'1 .
~. ~
~
•
T _ Il ~
T. - : : _ PDs.IIQC
• _ _ " " 5,T.... - .
• ro , (5lIIl_ll.. .
'_
_
• T- . I Z ts>:15
_
!"""I ...
t, ~
- . . .. .......w.
IlE:IE31
333 (of 550 ) 2006(-2016)
334
.--.. For Immediate Assistance, Con1ect Your LocalSalesperson
t'.
BURR-BR§@
IE:IE:I
·
INA117
; : 1'
High Common-Mode Voltage DIFFERENCE AMPLIFIER FEATURES
APPLICATIONS
• COMMON-MODE INPUT RANGE: ~DDV (V ~ = ±15V)
• CURRENT MONITOR • BAnERY CEL.L-VOLTAGE MONITOR
• PROTECTED INPUTS: ±5DOV Common-Mode ±5OOV Differential
• GROUND BREAKER • INPUT PROTEcnON • SIGNAL ACQU ISITION IN NOISY ENVIRONMENTS
• UNITY GAIN: 0_02% Gain Error mal( • NONUNEARITY; 0.001% mal(
• FACTORY AUTOMATION
• CMRR: B6dB min
DESCRIPTION The lNA Il1 is a pR'ci,ion uni ty-gain difference amplifier wim very hi;h aJ mJQ01Hn
~
~ ' . T t l
- N-
-' l.' -#/'. . " Ii"
.ln ~ G"Z1'
,- c;:
t-k
~t:J ,. ~ vo i.,
~~.
The INA II? is a vailable in 8-pin plasIic mini-DIP a nd SO -8 surface-mou nt pac~ . specified for !be O"C to +7ifC temperature range. Th e me tal.TO-99 models are available specified for file - 2:l"C lO +85' C and - 55"C U-, -f- i 25°C tempelarure range.
_____,.,. . T"" I~ 1""1l1
4./00
~_
T"" I1I-*il·11t1
;
'll
""_
-~
• T_1ll15T34 1....., _ ,
= ,-
• _ _ _ s._ fAX:ifIl2l" 'S'~
!II\lI:l. •
_IllC1Ol
• _ _ __
SolM'=
IElElI
•
334 (of 550 ) 2006(-2016)
335
DMS-30PC Series Mini, 3 1/2 Digit LED Digital Panel Meters .
INNOVATION ~nd EXCELLENCE
FEATUFIES Very small, ideal for thru{behind the panel or PC board mounting
Full size (O.56") digit height Packaged in a 12-p in plastic DIP. with a color fi lter case (O.9''H x 2.1"Wx O.s"D) Ava ilable In many bright LED colors: red, orange. ambet', yellow, green, blue, and aqua Super bright versions available Low power models available Differential inputs w ith optional ranges of t200 mV, t;2V, and :lOV de Factory ealibrated to within:il eount, no external adjustments necessary Autozero AID converter for long term stability with no adjustments A +SV sup ply is t he only power requ ired ''Display Test" pin available User-selectable decimal point placement Fu lly encapsulated package well suitlltCl for harsh environments Many optional support products to cov'"' virtua lly all possible applications Installation tools lor easy prototyping available: cut-out punch. retaining clip inserter, evaluation bo ard
SOmw
GENERAL DESCRIPTION
)
The DM &-30PC Series is a line of fully ope rational, selfCOfItained and complete 3 1/2 digit voltmeters. The very small , size of eeee di9ita1 vol tmeters has been achieved by integrat. ing the display and convener circuitry inlo one assembly, using the most mOOem microelectronic hybrid packa ging techniques.
The lltSuh is a very sma ll and solid digital voltm eter whic."'l can be handled like a compon ent unlike awkward PC boards or conventional meters housed in plastic boxes.
•
-
~ ....::..J
IN to (-)
AA'
COM\4 TR JMM ED
REFO UT M£FI~
_5V IN
-:i
~
""
" """""""
¥ ,
ro
I
DATA /
"CO
CAIVERS
I
CMA 10 86 dB, high imp edance, diff erential input. o""rvoltage prot ection (to =250V de), and a built-in. high stability. double regu lated reference circuit allows for extreme accuracy (0.05 % . ::t1 digit), repeatability and a very long MTBF, The large (0.56"' 3 1/2 di git LED display is available in a wide variety 01coors including; red. orang e. amber , yellOw, green, and blue to suit every application. The OM&-30PC seree me ters are ava ilabl e in three voltage input ranges : :200 mV (OM$-3 0 PC-o). r2. V de (DMS-3OPC-1). and ~V de (DMS3OPC-2).
Input impedances ara 1,00 0 megoh ms for both the =200 mV and ~V de models and 1 megohm for the ':!:2.0V de model. minimizing circuit load ing. A single +5V de supply (no oth er parts required) makes lhe DMS-30pe Series fUlly operational over a .... ery bro ad temperature range of 0 to +60 &C. The OMS- 30PC Seri es is ideal for high perlorm ance. high renability measurement syste ms where low cost and ease of us e are paramcurrt.
The built·in bezel, )ow power drain. fully encapsulated (plastic) case. and small footprint wlttl large LED disp lay were designed for direct pc board mounting, panel mount application, and mobile/portable instrumentation.
-I.BBB I • •I •, ,, "., I
.
• . "" ""
,
i
DISPLAY TEST
APPLICAnONS Board-lev~1 dlagnostfcs
We;gh scales Automatic test equipment Avionics displays Lablfest equipment Digital th ermometers Harsh environment useage Process monitoring Portable/mobile instruments
Figure 1. OMS-30pe Simplified Block Diagram
335 (of 550 ) 2006(-2016)
336
DMS-30PC
-
MECHANICAL DIMENS IONS
Panel Cutout Dimensions and Optional Bezel Assembly
INCHES (mm)
i
1-1. 8 8 81 Recommended printed d rcuit board finished I'loIe diamet.,. is 0.042 (1.067). ~. 002 (0.051)
Mounting Clip
2 Decimal Ptecea :to.02 (:to.50) 3 Decimal Places :10.010 (2:0.254)
r
! r~ F
ORDER ING INFORMATI ON
DMS-30PC-X-XX INPUT RANGE
o;
ACCESSORIES GainlOH1l81 pot 8ntiometer leit fo r OMS-EB, DMS-ES-ACIOC. and DMS-Ea.DCIOC (see beloW)
RN-OMS
---- I
OMS-3O-CP DIlfS.BZL1
+2OOmV , _>2'1 2 • .zryv
Dl
ADIH>N APPUCAnON BOARDS
vs ..YelIO\IIo'
DMs-EB DMs-EB-HT9
os = Orange AS .. .A.rnl:Jw BS e Blue RS .. Red
DMs-EB·DClDC DMS·Es-.TCJ DM5-EB-TCK DY5-EB-RMS Dl.tS-EB-ACIDC OMS·ED- LP
GS _ Graen
as • AQua
RH • High ln lenslly Red RL _LOIN Powvr Red Gl. • Low Power GIltAI"I
OL "' !.Ow Power Orange
-
-a-... ...
._ ... _ .. _ _ ..
__ "'_"_00__."- _
MlAtipurpose (4-2OmA. gai nfo lt$&l a~l,l$l) Hi gh accuracy temperatu re probe sensing for 200mV models Provides isolated +SV power H ype thermoco uple inputs for ~V models I(.type thermocouple iI'Iputs lor cJ:2.V models For tN . AUS measurements of AC YOltages For AC ~ne-paw8.-ed appIica\:ion$ FlX 4-2OmA Ioop-powvfl"J appIblklos
.. _ ..
-
" --
DATn . Inc . INTERNATIONAl:
_""" US.A. e ~ ._ OA~
Panel cutout puncn
OMS-30 Bezel Assembly DM s-30 Bezel Assembly wth NEMA 4. gaske(
__" " " " _
... ""- _ _ ..
..
_
-.-_.p_ao.._ _
, J
II CABOT 8OOLEVAAD. MANSFI ELD, MA Cl2048· ' 1 ~ TEL (50S) 33i-SOOO ' FAX(SCS) 3JH3S6 DATEl (UNITED KINGDOM) SUll19StoKa TiM. (2S6} 88D-444 • DA TEL (FRANCE) T'" II I 346(l.D IOl DATa (GElW»I't') TlIl (!l9l SU 33oW . OATa (JAPAN!Toi¥! Tel (3J 3779- 11131 • 0aIlI Tel t5l 354-~
"'" 336 (of 550 ) 2006(-2016)
337
, - - - - - - - - -- - - - - - - -- - - - - - - - - -, :0:
-:I
tf1 lVat ional Sem i c o n d u c t o r
~
~
-"'
LM124/LM224/LM324/LM2902 Low Power Quad Operational Amplifiers
r-
W N
General Description
Advantages
~ eonmts of fOI6 alO&Q8l lOelFt. ~ ga'I. - . . . . . . ~ ~ OP8' ldOl >al ~
• ~ r-.:l ror ~ SUClI*eS • Four ~ compwo...100 OP '"'" n a -.gllt
The LM 124
-..t'dI _ _ dIIsogred specdicdy 10 ~ tunI • ...,. l)OW« supply _ a wide f8l9lI of YObgas.. Qlen!1ion from
-*' ~ ~ is aJao pcaIlbIe and ll'le lOw Il"l"llI' IIIQ"'" lUT...: dr-.
os . ......... . . '1 of
lho;I ~
porr.lIW ~ ~.
oc
AclPIieaIlCln .,.. indldI tlIOC'C* and U _
of 1h8
~ ~ ;;arl CQtM;M' lIOioal 00 ~ ~ WI'QI now
can c. _ _ ~ ........... 'lIid in sinJilI'I powIII' Iqlply sys-
*'-- For~!heUl l l!.o& smeso;:an be dmclly~. ~
lIll'"
_--'
an 01 lhe ~ + 5V paww Sl.QlI1 vdtaqe wtIieh is
lJIIAd in digIIaI
and _ ~ ~ e*'lrOPllCl WIlr>OIIl ~::r. adcibonaJ :t 15V ~
" " '-
veer lito
'. . incI UGn 9fC'UIld and lhu ouqM 'oOOl\il9ll can also ~ to grgund, - . thouo;I'l opem.d f,,;m only • 9ngIe lll*'OW SlJpply voltage • The unity p" aou frllqUency IS t~llx.
-"'"
90"
~
• ~..;m .. Ion'n$ of Iogc • ~ dra'I ....llItH tot t:cMry qMfUOl'I
Features • 1~ ~ Wi I """ _ _ 1ur unlty' 9P1
• t..9'" DC ~ U*'" • 'NidI> ~ (1II'IlIy ~l
100 <:9
, U",
(1emp8JaIIn ~)
• WidiI _
"""" . . . ,
~Io ~
or dial "-ClIlliM
lheinput~'I'I'Iitago'I
~
toG NO
~ ~~
Unique Characteristics • 1n
• V..,
IIUIlllIY
bw
: 1511 to = 16V
or.... (700
cumNII
~ofWllQPly ~
~)---es:senI>aI) ....
.......................
• low InpA ~ Cl.'fS'It
~ otlNt YOll8gol
,.-
• Low
and otlsel
2 "''' 5 nA
~I
• ~ ~ IIOIt8ge 1a/lg8 indudes grotn:I • Ditterenoal Input voIU;. I'lfI9G ~ to 1M power sup-
• no. input bias CJ"W1'8nl is also t~
_
--
• AIoWs onoetry """"ll' ,.... GNO ....,
•
'00
• l.Mge 0UlPUI ~ awing
v-: -
0 '0' 10
1 .5V
Conneetfon Diagram • ,..... ,_ r
.-no"
. ..
_
.,-.
.....
~
,. _ r , .....,
~.
.,.
•
..
m
"
"
LM1241
...
_. .. ,-
"
.,
•
-
" "
...
" " " "
.._.. TLI>II9~ :l2
Ol"lter Number Ul1~"AE/&a3 or U11Zo&El8a3 s.. HS PIIeM;e NumDer E20A
==<. --,,=__.-.
--,.
Top VIew Onl... Hul"lltlo« LM12~ Ul12......... LMt24J/U3" , LM12'A.l/ta3" , LIInaJ, LIIV.,y, LM32&J, Ul324M. LM3z...... LM2902M. L.M324H.1.M324AN or LIiII2t02H
~
-,-
s..NSP~""""'J14A.N1""'orN1"'"
--~---~_ . _ . ~
'1.JII' 2U
_
1* _
• •..... 14 _ I * _
0nMt' ~ LM1 2U.W/883 or LM12o&W/183
' 0/1'0D6
s.. ~ ~ ~ W1"1l
. OI " MS
1-213
337 (of 550 ) 2006(-2016)
...
338
fJ1 Na,t.ional S em ico nductor
LF155/LF156/LF157 Series Monolithic JFET Input Operational Amplifiers General Description
n- _
",
r.. J FET ' " or-"""'" ~
the fint lTtOl
...-cn..", I'ligrt~ JFEfs,,"_
filqlo ~
..,.. ~ - ' ....-..:l bipolar b • ..-oo. (8:I -FEf1"I TIChnaIogyl. ThMe lIITOI:IlifierI toeture low input biIIII Uld otIMI CIIIIVflt5IIow offMl VOltagI and oflsel VOlUI~ c*'ifl, ~ wrlh ot1set Adjust wfliCll does not degrao;Ie drift Of commonmoae rajlIc:Iion. The dllVic8ll are also cleIign8d lor I'IigI'I sIlIw raw, wide bandwldln. extremaly f1IIIl Mt1lng tim.. low vo~ • and CIJlTWlt noiH a"Id • low 111 noiM comer.
• Ho;,tI ilpuI itTiCJBdIl108
Advantages
• u- inDUI CItI.- ~ 'lel'np. cHI:
....
ClIIlllbiIiIy
-
10 12n
• Low inllul: .... ~ • ttogn ClClfTnIDn..rnO f'1III'C1Ign mio
.... . . """" .
• Extremely
._ ....
P!'eei:slon '-ljl 3P"d n.ur-ICQ • .... DIll. and..vo ea-tln
• Low
• Looat·tt••oe ~
fII' .. LI"57 _
Connection Diagrams
slew
--
I I4gIl i '.......... bulMrtt
• ~ low l"ICIi8a, low (WI ~
,,"" ... ...
Uncommon Features
0.0 1%
I
,m'
3 ~vrc 0.0 1 pAI$ii
. ~oc ~ ...
• F_
Applications
01; _ •
",.. ,,..
• Low Input biu 00lrrWlt • Low Input 0ffMt e-.nt
• L..o. 'qlu!l or'-t volllq.
• Repillce aqI8l . . . . ~ ancr I!lOCUIt FET 09 .... • RUQO«I .FET e ....,., bIow-<:d frM NItdng ~ ~ MOSFET ..... dIJooicelI • El
Common Features (LF1 SSA, LF1SM, LF 15 7A)
irlU
Lf155A LFl5IA LF151A
unn.
1,5 ·
1.5
j.IlI
".
..
w,.. " "'"'
ra
ra
(A v .. 5)
of
, as 20
~ ,
nVl~
1\.'>1_"
(T op VIews)
•
-- , - ,..
e
,
-.,
-- _
J
• • __
r1,.JMI_"
On:tw ~ LF'HAH. LF 155H. l.J"156H, L.F2S5H, LF2seH, LF257H, Ln55AH, LF3SlAK. U'357AH, LF3580H, LF35SH , ur35&H, LF357H. LMtS5AHII83, LM155Hf883, Ul1S8AH/8U, LMf56H/883, LM157AH/S83 Of' LM157HI883'
"
SHNS~.NumberH08C
~
Order Numbw LF355M, L.F3MM, 1.J'35711, LF355BM, L.F3568M, LF35S8N , LF356BH , LF3!i78N, LF35SN, LF356N or LF357N
s.. NS P.~ NumboorM08A or NOSE
338 (of 550 ) 2006(-2016)
339
SiiiSjm
SCC100GS/SZ75400 Special 0 to 100 psig Pressure Sensors for SRI
Preliminary 1/15196
General Description The SCC series sensors offer an extremely low cost sensor element with a temperature stable ou1put v.!len driven with a constant current source. These integrated circuit sensors were designedfor extremely cost sensitive applications where precise accuracy over a wide temperature range is not required. This part features a protective parylene coating over the sensor element. However, this device type is intended for used 'Nith non-corrosive, non-ionic 'HOrking fluids such as air, dry gases, and the like. The SZ75400 special for SRI is different than the standard SCC100GS in that it has a special long tube attached for pressure connection. All else is per the standard specifications for the SCC1DOGS product. Contact your local SenSym representative or the SenSym factory for additional details.
Features • Low Cost • Internal Temperature Compensation • Small Size • Gage Pressure • Reliable Semiconductor Technology
Closed Circuit v.
- 0 ,,1
Applications • Special Sensors for SRI
Revision History Revision 0 1
Date 1-15-96 1D-4-96
.~
Description Original Specification Chanoe to Closed Bridae
Drawing Approvals SenSym, Inc.:
Printed NamelTitie
Signature
Date
SRI:
Printed Narne/Fitle
Signature
Date
339 (of 550 ) 2006(-2016)
340
SenSym
SCC100GS/SZ75400 Special for SRI Pressure Sensor Characteristics Environmental Specifications Temperature Ranges: Compensated Operating Storage Humidity: 0 to 1OO%RH
O°C to +5O"C -400C to +85°C -55OC to + 125°C
Maximum Ratings Supply Current I. = 1.5mA lead Temperature (Solderi ng 2 - 4 sec)
25O"C
Pressure Ranoe Soecifications SenSym PART NO. SCC100GS/SZ75400
PRESSURE RAN GE 0-100 PSIG
SRI PART NO.
Performance Characteristics Characteristic Ze ronres sure offse!.1@:T.=25OC\ Full sca le sean {" l inearity. hysteresis & reoeatabilitv Temo. effect on soan ''l Terne . effect on offset ''l l ono term stabilitv of offset soan '" Re sponse time (10% to 90%~ Innut resistance] @). 25°Cl Outout imoedance
PROOF PRESSURE (7) 150 PSIG
(1)
{J J
min -30 .0 85 -D.5 -1.5
tvoical -10.0 155 0.1 0.25
-
45
1.5 90
0.1 0.1
-
4.0 4.0
5.0 5.0
max +20 .0 225
0.5
6.5 6.5
units mV mV %FSO %FSO uvrc %FSO ms k k
Specification Notes: Note 1: Reference Conditions {unless otherwise noted):Supply current. Is-1 .0 rnA;Ta::25"C. Note 2: Span is the algebraic difference between the output vonece at full scale pressure and the output at zero pressure. Spa n is ranometnc to the supply voltage. Note 3: Unearity is based on best fit straight line. Hysteresis is the maximum output difference at any point within the operating pressure range for increasi ng and decreaSing pressure. Note 4 : Maximum error band of the offset yottage and the error of the band of the spa n over the compensated tem pe rature range, relative to tne 2S-c reading . Typical tem peratu re coefficients for span and resistance are -2200 ppm/"C respectively. Temperature effects on offset and span are gua ranteed by design. These parameters are not 100% tested in production. Note 5: Long term stability over a one year pertcd . No te 6: R esponse time for 0 psi to full scale span pressure step cnanqe Note 7: If maximum pressure is exceeded, even momentarily, the package may leak or burst. or the pressu re sensing d ie may fracture.
Rev 011796
340 (of 550 ) 2006(-2016)
341
SenSvm
SCC100GS/SZ75400 Special for SRI Electrical Connections Pin 1 2 3 4 5 6 7
8
Function Vsupply+ NIC NIC N/C N/C -VOU! Ground +Vout
vO'
o
4
o NJC
Pin Out (Bottom View)
Physical Dimensions (In inches) 0 .12
Di4J ~ 0 .63
It 0. 3 2 DiaW---.I
0.25
0.5
Approximate Weight: 1 gram
SenSym reseoes the 0Qtrt 10 mike ~ to ¥'f prnduds tww.... So>rISyrn.x- noll n_m. fn1 iablllty.~~ 01 the ~,* .'l'.' or use 01 'iJITi prodac:t or creut desa'tIed /'IererI. necltoef Ooes II ~ anysceoee i,ndet its palen!ngt'Its nor the ng1l 01 OChers.
SenSym 1804 McCarthy Bou levard Milpitas, CA 95035
Tel : (4081954-1100 Fax: (408) 954-9458 Internet: [email protected]
341 (of 550 ) 2006(-2016)
342
&-PIN DIP ZERO-CROSS OPTOISOLATORS TRIAC DRIVER OUTPUT
-.
(2501400 VOLT PEAK)
seMICONDUCTOR"
MOC3G31M
MOC3032M
MOC3G331/
MOC3041M
DESCRlP"TlON
M0C3042M
.~.~
ThJ YOC303XM .-.d MOC304XM 04WiC8S conIisI: d • NGMa Ir*lncI eniUing dodo cpIicaIy fXlI4)led 10 • mclII'lOlilhic lIiIitol deCecW pIlI'b'mil'lg 1M fln:Ian of a ZBrO vobge crossing tu-
f t t'icdrtver. They aN dBsigned 'br use with 8 tr1IC In tile inIerfBa!l atIc9k: ~. II:) ....ipn8n1 ~ from "5 VAC lines. auctl 85 ~ CRTs. said·SlBt8 relays. DIuIlriaI COflt'tlII, prinMn.. moIol's. eaenoIcIs and c::onsuner ~. ek:.
.~
FEATURES
,
,
• ~ IogOe eofGoI of 115 w.c power voltage c:rossing • dv1dl: (If 2000V.\iS typlcaI. 1000VIf.Ls ~ • VDE ~ (Fie" 94766) -ordeMg option v (e.g., MOC3043VM)
•zeo
-- d':;' ~~ ---~
~
• So/el~ ClOnttoIs .. S*afic oownr !IIMIctleII • Temp8dIure oontrd:!
• L.ig1lIng eonIrols • At:; 'II\CllCl' dr"'"
• E.M. cont&ctn • &lid . . . fIIiaY'
.ACmol«~
......
.....
T""
N.
~to+150
T_
V..
N. N. N. N.
P,
N.
~
N.
V.
N.
'0
N.
ABSOLUTE MAXIMUM RATINGS (TA = 25'C unless
.......
-_...
hnIIne..,. TOTAL DEVICE
SD'age T~ttn
LMd 5cIder TIfl'Ip8l'8tlnl
J~T~RaoIge
. . . . &Igt~P*1ICdlgt.fiIHr.t_1b*lJ local o.ric:e Pow. Disslpralion@25-C
.......
DeRle above 25-C
--
ConnIaua Farw.d OJnwnI
TobIf ~ D1ttllpiilb. 25'"C AtrtIienI.
DenD IIbcw 2S'"C
DETECTOR
0lJ..S1lD 0ulpuI T«mhaI VoIt8ge ,... ~ aq. CIoIwcC (pw" 100Ja, UO PJ*J
-
"......
".
APPUCATIONS
T,*, ~ DiIa/plIb:M\ 0
MOC3043M
~C ~~
0-.- above 25'C
T"" T,
V_
0""
'.
1. IIot8IfOn surge vcIage. VISO- it an inSlIrMldeW::e ciefec:tjc; breakdown
otherwise noted)
...,"'
...
~to +1OD
'C 'C 'C 'C
7see 250
'""'*I
2114
mwrr;
mW
...
60
,
V
"'"
'20
mWrc
U1
250
MOC3041MI2M'JM
COO 1
mng. For IhlIIest, Pins
.....
250 for lOMe
MOC30311U2U1'3M
N. N. N.
1=
..
V A
,
mw
1.76
mWrC
land 2.,., cornnmn.lfld Pins 4,
Sand 6 .... ccmmon.
.-. .2Dt1 FItnltlId t
DIIIIZM
.....
' . J .... OajiOl.a n
tOF.
••
!'dU,
'_
342 (of 550 ) 2006(-2016)
343
6-PIN DIP ZEROeCROSS OPTOISOLATORS TRIAC DRIVER OUTPUT
FAIRCHIL.C SE M ICONOU C TOR"
1IfOC3031M
(250/400 VOLT PEAK)
MOC3032M
MOC3033M
MOC3041M
1IOC3042M
1IOC30431ol
B.ECTRICAL CHARACI ERIS1ICS CT. -:m: ' - _ _ _
....,...,.
INDMDUAl. COMPONENT CHARACTERISTICS
--DC _ EJIlTTER
DETECTOR PIIi. . .o
Tnl CoIWAIeM
........
......
IF" 30 rnA
V,
AI
\9-t1rIl:b
"*y.... ~ ,.O ... 1]
,,-:c:.a.¥:I'9JElwI-.c.
~ ·UDrMpesk,.1F .. 0
QkIIR*ocl~doa.
'" • D _ _ i , IIDt8 3}
TRANSFER CHARACTERlSncs
LED TlIQoIt Cunwtt
ttIIibI c.-. EDIt DirdoI
.......
-
'000
"""'"
MlJQ(lJ...,;)CJGC'lU
...
"OCtUiiMXJOC!M
AI
....... ......
T,.
.""'''''-''ID.-'''
....
AI AI
MIn
UnIb
,.s
V
'00
...""
•
V Vila
...
.....
,. 15
...
""""""'" V..
... '00
U
(TA" 2%5"'C UNea CIIWWiM ~
Condition.
1,"' UT1oUT.Z" __ 1IIlIdI . . . . . . . . . . . . . . .
LMbge" Inl'llliled StatII
-
'''~
"'1Fr.
AI AI AI
....
--_.,."", "" T"
..,
(fA " 2S"C UNus.tA\elwiI:I ~
T"'~
ZERO CROSSING CHARACTERlSncS ~
'-. V",
. ,.",
,.25
AI
VIIl-&V
""""'"
IOn
,.",
•
mA
...
-... ........ '"
V
1. r.t . . . m..c be appIed.ttwt dvA:I Nfif\1. 2. AI ~ _ ~ 10 ~. an'" YUle leW ..... OfflqUllll to ma In- ~. N«JlII,41C11d opeml'Q ""lies be lwNn rn..x 1fT (15 "'" b WlC3031M .. M0C304tW.10 mAb MOC3032M & UOC3042M, IS rnA llor MOC3033h1& JrIOC3C)I 3M)..t IIbso/utIo rn-.l,: (60 mA). 3. ThiI• .-ac ~ s.. R9'- 8u 1eiII.uL CemT ~ dWdS • • bdon~"~thrri*w(s) onr-
••
iill
mt _
.... 343 (of 550 ) 2006(-2016)
344
"r------ - -- - -- - - - - - - - -- --,
~~ :!~~
~
LM35/LM35A1LM35C/LM35CA/LM35D 3 Precision Centigrade Temperature Sensors
*~
General Description
n..lM3!5
~
~ :I
~ ~ ~
lI.n ~ ~ ~ YOItagIII is ~ plopor1iol_'" lI1lI CeIw. ~) ~.. ThlII.M3:i 1hw lIN an ~D¥W ~ MmpMU.nI iHtlKIIl!l CIIIbratId In· I(eMn, _ tlw .... is not f~ to tubtraCll large c0nstant VCJItage from III 0Ulput to obtain OOI'MtIliIrrt grade acaIinlJ. ThlI LM3S 00.. ~ reQUire MPf extemaI edbrallon or 1rIrnr'*'II to pr~ typIellI aeeurade$ ot % y.-e
c..,.
at mom lempoQh.-a and :t%OC.,....tull - 55to .... , 50"0 1IIIfTlI*IlU'e ~ L.ow COJ1 lS eeeee by b1m"*'ll and
caIlbmIon at 1M waf. ~ 'The lM3$',1cNr oo.4PUC 1~ - . Iin_ OIIIPUI. and preciM W1enInt ~ibmIon ..... ~ to r..tout or c:onWDI ~ ~.-y . • UMd 'fIo'ith ~ ~ SI4IPfi8S. or wi1I1 plut ...-:l ........ auppleLMIl:_q60,....tromb~ •• _ ...,.Iow"'~ 18ss .... 0. 1-C In SIll • . n.. UGS II ..-d 10 opefM _ • - 5.5" to + tSO"C ~ ..... M * Ihot LW35C iII ..-d lor . - ill!' to +110'0 rwoge ( - 10' 'III'ItI ~ --=Jl. 1M t.M35. . . . ill
'*' _
-
--
...-.tlle ~ In heImeCIc T04Irwlstl11or ~ ~ ... LM35C is al90 lMIiIabIu In the plastIo 10-82
w-
.
Features
• C8litJiated ~ In • Celsius lCenllgracloJj • LinNr + 10.0 mV/"C lICIIlu flIcwr • O.5"C IICC&ftCY g.Jll1IlIl ~ (Ill .... 25"CI • Al¢Mlforful - 55" to +l!iO"C ranwe • Su/tabItl tor l8f1'ICtIl appicalionlo • La- CDlIt dull to _ _ ...... ~ • ~ trom .. 1o:JD ¥'Ob ~ .... eo "" ~ chin
•...,......,_.IQ, •
lI.llll"C in 1IIilI.,
• ....... _ ily onl!r :l: Y..C ryp;e.r • LQW ~ 0UIPUl 0.1 n tor 1 1M Il;-.d
ConnKtion Diagrams TCHO
..
.... c:..~.
....
M~
"e-Io
--
pOo
I'tOUI'IlI!: 1. s-le Cei ,tlgi ... T-.-...... ser- ( + 2"C to + 1SO"C)
~_+1~ _"
+1'l11'C
- +~III'V IIl " ~
_ _ MO _
..
-se-c
."
344 (of 550 ) 2006(-2016)
345
BURR -BROW N '!:
INA128 INA129
1
E3 E31
Preci sion, Low Power INSTRUMENTATION AMPLIFIERS DESCRIPTION
FEATURES
The IKA 128 anI.! J'l'.: A129 are low power, general
• l OW OFFSET VOLTAG E: 50pV max • l OW DRIFT: O.~VI'C
purpose instrumentation amplifiers cffcrir.g exce llent ;;.C'C'.uacy. TM-rr ven.a.tile j -op amp dc:sis:n and smilJ size make them il:eaJ :Or a w ee renge of:!pp1ication~.
max
• l OW INP UT BtAS CURR ENT: 5nA m a.x • HIGH CUR: 12OC9 mIn
~;-f~ck inl'"..t circuitry provides ....-oe Ca::1dwiCth ever: at hii6 gam (2O
• IN PUTS PROTECTED TO =4aV
.... s:::gle exrercat resistor sets
• WIDE SUPPL Y RAN GE: =2.25 to =18V • LO W QUIES::::::NT CURR=NT; 100J.1A
• S-PIN PLASTIC OfP, 50-8
The P.\AI Zllil :-:AI 29 is laser trimmed for very lew offseevoltage (SO)lV). d.-i tt (O.SL:-V!"C) and high cernmoo-mode rej ec tion (l 20dB at G ;:: 100). I: operates with power supplies as low a ~ ~-15V. a.'l<.l quiescent cum::nt is only 700~-\-l&al fo~ battery operated sys tems. Interaal ia;lu:. pretecnoa can witbstand up rc ±40\" w-itbxn damage.
A PPLICATIONS • BR IDGE AMP LIFIER • TH ERMOCOUPLE AM P LI ~ I ER • RTD SENSOR AM ?LI FIER
• MEDICAL IN STRUM ENTATION
Tbe
. DA TA A CQUlsmoN
"
J " c--'- CjC~" "'''~ ~. N. I
v
~
,
P:';~ 'o~
L ,
:
~~
8
c .
~AI 1 8.'IKA129
~leOl"1'.....
~~
.
•
- I
,,~
~\¥--'
~
tV¢-:
'- - ~
I IV
.....---.-VV'--r
; •
_ ,a
'"
,
""~
~
2!
,
11"A~ 2'. :"'-1 211
0-21,-"".",.,,~~
-
is available ia 8-pm
DIP. a;,d S0-8 surface-meum ?,!c~,ge$ . specified fo:the -J.WC :o - SS "C" !e:r!pera':tt"e reese. The IKAHIl is a.sc ava ilable in C:ual cor.fi guratiolt.. the !:" AZ!28.
I
•
v,
, ,
,j.J . Q
I'
c v_ t'Cr."~...
"""",, _
_
•
:;~ ~ · I'i:: Go' : \.I.O:. T ~. ~ ~.
_
••,, --.r;cl. : _. ~ T__ ;,z .. ~
1':lnIO.=_ ~lNQeII".;;Q " ~. ~$l(. =-- !.3R ~ 0ll?
,:
_
- . . ."
•
Ul: . {3ZlI: . " ·~"I "
"
:" Iili':-"" "r..- V Mi>2-' '' '
_.
~.loa~ ·:Il:
,
345 (of 550 ) 2006(-2016)
346
I~
I
hI
,m lilli
.; \1 i !
mi·, u: · ] is ! u
©
~
c
i
~ i· - - ,. ~
N '
..~~ ·1-II
" II
, .~
~ ~
~ f[ ~ , ! N~
=
•
jm I
I:
• "" """ "" "" "" "" "" ,
I
w
,; z
•
, ,
"", , I
•
"~
t
•• • ••• ••• ••• •" •" " , ••• •• •""
\ \ I , \ \ I I \ \ \ I \ \ I I \ , I \ \ \\ 1 ~ \ 'I I - - - \ \11
..' ,", '",'
•
n
~
o
•
• o
~
~
~
~~~f.I' ·: ······ 111
,
s
"
,, !:!
-0
': '0 '
", ", ", ",, "", '" ", ", ", ", ",
s•
•uz
g
w
;
Oe
• ... .
~II
. ~ ut!'
5!t:z ~~ su s~~~ ,, ,, -c
0
. •"• C'"" 8-'S'
iI
.• '. lIE:'~~9
,!
•• ...... _...
•
• 0
z
346 (of 550 ) 2006(-2016)
347
Zt91l:
.. ............. . .. "..... ••• •
•• I!
~
!!l ,
a ~.l .
,•
I
iii
'II 1,_
ill
trt
!d
III
@
0'" a, ! 158 i!!~i •~.t! I-! ... ··i
:: 6 1II-
:::~'
,I
.!. ~E
' J.
'1' .1
I
~ •
oIoi: g••
•
~
• '''" i·' .. .:.. .. . ...
••~~
••• !I,I • [;! i
~ "..·
~ n
I I
• •
I,u
~
,.... , ,,• ,•• , ,•• ,-'
~
a' , .
..1. . 1. .1 "
•
•
I .•
i\.:.~_
i~
,
~.l..
I-
=
'~!. "1
~~_
!.I . ....
N
E w ~
· ~
N
W
•~ E ~
~·u A • I
.~ ~ ' ; •I I'":1I! ~~ ~ i ·1·II· ~'"~ 1111
,
•
.i ~gQ
.-'"
~
U
~~!
0
Ii,
;;
I
•
•
...... ....• ..... ,
•, , •
h
\ \
•
"
\
I
\
•
•••
,
..
I
,
•
•
,
1 • I • \ , \
I
•
...
' \ \ 1 :. \ \~ ~
\, \, ~I ~•
\ \~ ~
.: •: II:
: : :
~\~:::' .' • , I • • -~
'"" '" ", '" '" '"'" ''"" '"
'" '" '" '"
,• o
.. .
~I I
•
347 (of 550 ) 2006(-2016)
348
I,
••
I
I
e .,
-"
..I
I
•
no
:. d.l. t,;" ~
•
'" " ""
•
~~ 1,1. 'I II :I • •
III
:!'
:f i l I • ...
•
!
-- -
CD
---
- -
u
a.
f
-. .-.-
~
!:
W
"i! U
H
•
z .
.-=-e = ·-=-earn •
;~
8~
a=::J
•
0
• •
iii'"
L-':-- .ono.
z-
0
::0
0<>0. _
. []
~
-.
" "
.'
@O~~ 0
-
~s..
- =-
•.• ••..•..•
~
••• •" ••"§~ •• O.
J
l§ II"l
=i o• :8
... •
~
II
-~ ..... ....
·i• , ••
-. ••• ~
~" "3 •
-..- .-••• ••.. i=3 -~
~-
riO
o§ .~
.,
00
w.
-- -
~r
~
e
~§
. ~.
i1.L e es
ri
~
z
348 (of 550 ) 2006(-2016)
349
.
!
.
- I ..
, P
r.:t
~
. .~
... ~
...
I
o ~ ~
~.
,
~
" ~~
,~,
~
:= c_ ~ N
,
~
0~
e
~ I
'"" ....
.. N
II' "i d ",,1 Il,!'l
~;'I ,~~ ~
g LiJ ~
r
h'"' ," II !i:1 .11'1'1 "r 'I,'j I
e!
Oil
I;:d: ..uh *to
..... ..
•i
349 (of 550 ) 2006(-2016)
350
- .x.r-....-
~
:>-4
..
--
;.0 _..... •...
..---... .......
, e... .......
CA555~. LM555
HARRIS SEMICONDUCTOR
nners for TIming o..lays and Oscillator Applications in Commercial, Industrial and Mifrtary Equipment
""'
FOIJtJJtes
.-.• •
DeSCTiptiOtr
......
~end~Opef1IIIon AdJuslabl. DufJ Cyde
Tll4 CAS55 andCA555C Itf8 hiohI1 stable 1i'Nr:s b use., predston Iimn;.md 0GC:illat0( appbtlon$. N 00...... .,.. monolithic trl~~ ciR:uU ar& ~ af produci"og IIQCI,Ir.tto limt tlWJ)'$ Icc p&f1Ol.1S ranging fn:m miclOs.......llds Ifv'ou(tt t\OtIt$. Thew dIMc:es oro eeo UISlll'fd ill' utabI9 ......riIb ,Or tIfl8n1lioA and DIn mairUi'I an acec.nlafr contmIOO tree t\I'V1i1g ff9QUlllflCY and ct.rty C)'dt Vth ~ bIIO tIdomBI rlJ&istmand one capecioI.
• 0utpLft c"......· at Soutdng ot SI... "p.;S1 VI'10 200mA .. Ovtput CapeIlIe 01 om1ni 'rn, D ... NormaUy ON MdOFF 0utPtJb;
_"""--
• HIgh TeIi,4*'1II:ure Se.blity •••••••
.Applications endUC14SS
~ .;lrwlts of Ihe CA555 arod CMS!iC ITW)' be u ~ ty 1tMI ia......g edge 01 the wawlIIorm AlQnal. and !he 0Uf$M 0( these ciralilS can SOoted 01 lWIk qJ 10 a 2'CIOmA CUrnml Of
• Prect8lon 11rnlng
• ~l'ltielTIftngl • l1me o.t.r Gwa••~'~"'Qnn
ci'twrnt~ _
n.-; tr.>O' are
Orrferlng lnfortTJstJon PAATNO.
nMP.RAI«lE
PACKAGE
~
~lu.129C
CoUIi65M
-sec 1l:l.t2!5'"C
SOOC
• eesccTQ.5 Mila! can e ad E'l&slle DIP
~
-ss-<: 1o . 'f25"C
CADM5T CA0555CE
-55"C10...12S"C
CaOSS5CU
O"'C 1lI.o.7f1'C
C a O!5 E6C''06
O"'C.,~
~5:5CT
O"C10 +7'tI"'C l7"Cm +"1O"'C 10 .1O"C
~
I.Jot!Il5dCN
~ to .7f!"C
n len
lid PIa$tic 0;>
i'ldvwy 'WM i--.
sass
*~
electrioal
<:huacwr~
8 F'
•
8
o-c
d lNd: ~ b'
padalggs wIh :similar tftrmi'W . ~ e.g. Mld~, J.lCl555 and IotC14S5.,. ~)'. The CAS:i5 lypg cilt:ui~.are IntoodcKt br appPeatlQns r&(JJItlnQ premium ~ I perbnn6flOe,. Thlr CAS5SC ~ chwit$ Ilf1l
SD K:
"
T'O-S MllW Call
•8
Il~
• DttlotM T~ ana ""'
NORTIiERN CALIFORNIA
d SQIC'
""'" [liP on>
(400) .'2-5522
370 TOUKJNS CT. I GILROY, CA 95D20 I FAX: (4U8)842·7315
Functional Disgrsm
.,-
.... ,
"""""', """" ,
11a
IOU)
""'"""'-__,"', W OE
ltl-5 ~ ~ \!lift Formod
.
z..-
~ CA555C, J.M5iSl$C (IIEW.
""'YEW,
..... .....--
,.
CAN)
,
i
1
Filtl Nu~
834.2 ._ ~~
r
T
350 (of 550 ) 2006(-2016)
351
P,,11Ef. ~ 'Bf?iJJ/r1 FIEL. 1~:fiSF.1~ ·
•
l",~ . T~
..
'"""~
-
-"
< ,
.
.
.
---
.~slow
irKlication • Pus/l.!Cl .Jl!Sel
''" Approximate Si.z,
• Ouicl< e(>M eeT Of sctew ,,,,",",,,IS
~OpenIti~
Volt3ge
TripT.-n" . t
200% of f\BIlng .
lnlemlpt Capacity
•
• 8U!lon ee eees ,'" visible trip
-
ThO'",.
"""""'"
"""""
""-
• Compacl~ • Variety01tme delay "plions • Toggle ad... tion
NEWDESfGN
I
,.'
W9 Magr>etic • Variety01 tn1£! delay options
• Togglol ad """'oo
• OplOonal BU'
for manual onI\>ff aM ",,;~ • Dpcoonal s",,sWltcn
% @@
'i\l@@
IQrmanw l(Jtl/O~
-~
..""
s witch a""; lable • Desogr>e<:l lo rneel IEC aM 'JDf
'etlU"erner'lS.
%@ c
.M· •.83' .1.54 ' 11
.66' .1.38' x l .3S· d (13.7 " 15.9 " 39.():j) (168 .34 9 .349d) 35 oz (lOg) 1.5 oz. (4JgJ
•
a
,
'i\l@ a
• ,
'i\l@
•
•
c
•
•
,
• •
c
.7S" x 2Y x Z. l"C1
.15"" 2D"" 1£4 "d (19.1 "50 S . 42. 1dl
2 oz. (57g)
.69" .1.Jl1" .1.6' 11 (17.5'34.9 . 40 .6d) 2 oz. r.;Tg)
2.5 oz. (11g)
(19,1 • 53,5.53 0<:1) 2.5 oz. (71g)
,IW . 1,89" " l . n "d (24.9 . 48. 43.8d) 1,2 oz. (:l5gJ
(17.5 " 34 .9 " 406<1)
.69". 1.36" " 1.6"d
1
,
10,2
1
1
1 Illrwgh 4
1 tllr""9h 4
SeriesTrip
Series Trip
Series Trip, both pojes
Series Trip
seeee Trip
S6-ies Trip wi or S... \CI1. S/1unrTrip. ReloyTrip, Dual Coil Ser>es Trip. Dual CoilS/1un:T
$Me$ Top.. lor wlo Au. , Swi'C1• S/'
• s.-n.-< Trip. one pole:
025-20 Arnp$
1·35 Mlps
...fO .......,
pole
5·:;>0 Amps
O..5-SO Amps
sovcc
50VDC
"""""
sovoc 250VAC
2SOVAC
250VAC
Q.2S-ZA McQeis _ 4.5 1028Sec. 3- 1SA t.IOdeIrI _
t -4A MOdelS_
32'IDC
10 103OS.,.;.
1010 45 See. 5-35A Models -
221015 Sec.
se co see.
'.OOOA 0 32VDC
2.(OOA,. e SOVDC I,OOOA e 2fn1AC
• eooc
1,000A It SOVOC 2.000A e 25(J11AC
.250' (5,35) Quick CoMec:l (00 not soldefj
.2!>D'(6.35)
.250' (6.35)
Quic~ Connec~
OJiI;:k Co n"""l.
Snaps " to SJ8" (15.9)
7116 '-26 Thread ea
panel cutout lrem
Busni"!). 15132"- 32 Th rea ded 8uSM inQ
the front
0.5-SOAmps
,,"OC
eooc
02 5-50 Amps
55"'"
551roC 277VAC 48lNA{; 3I:l-Wye
~s.:l2
Sc", ...
rt e sesec,
JOms 10 150 Sec .
JOms 10 150 See.
~uponlrip
Oepeodong upon tIl p
s-35A Mod
.,.".". spe<:il>&CI.
CU'W ~.
o.5·25A MoOels 2.(XXIA C 50VDC l,QOOAO 250YAC 30-50,1, Mode!s_ 1.000", I) 50VDC or25OVAC
025--2OA ~s ·
2.000A @65VDC 5.0(XlA@277VM;
g.5-<" Model:.11 to 30 Sec. 5·35" Models f; to 22 S
0,S-.4A MQdeob -
C.5'2 SA MOdels -
2.000A05OVOC SOIIOC
'S·32 Screw
'6·32 Screw
Sn a;:>$ inlo
318'-24 ThrN d lld
15fS2"- 32 Threaded
575. U S"
B....I1Ing
......,
zs
as
SOO"
(222 .
O.25·SOAmps
U N ""
4NNN:. 3
or 2:LJVAC
QpU on ~
W6.
'. -
·
• Optional lighted roc, e", • Models with au><.
'.,)XIA 0
OptKms "
.
· --
1.000A0 25CNAC 30-5OA Models -
'''''''"''
' W31 .
·
• Rocker accuator in • Pus/'II~"" actuation • Toggle Iduation /Q< m¥lual ()(\IoIf nrious room for man..al on/oft • Co.",e"i.,,!. snap-
s..~C h 0f11y. Me
Current RoIIi~
. W2;3i . .
Th_
"""""
'i\l @ GJ @ '" 'i\l @ • e c a e
No. 01 Poles Circtlit Func:Don
W33' .
.
• LabOr·S3I4tlg snap- indicll!lQfl in ITIOO'ltil1g • pusn·to-rese1 • Button e~tends lOr vi~lrip
and Wei ght (per pole)
W58
"""'"
cartridge fuse and
.
•
-'
.'
W2B
,~,.,
"
, .
.....
•
_. I(-. - -
NEW DES IGN
NEW
~~.5)
pane l cu:ou t
2,00QA 0 65\IDC 5,00ClA 271VM; or 480VAC 39-Wye
e
,,"",.
48QVAC 30--Wye
2h5OA~s _
2.QOOA 0 65\IDC 2.5OOA 0 277V1J:.
.2SO· (6.35) Ouid< ConCll"Ct, ' 10-32 SCrew
, 6-S2 Tapp.!<.! Hole-s, M3Tapped 1'1 01-:;. S,",PS ;"10 00...... Cl/lOJl l,om me fronl
~ 1 0·32
SuJd
' 6· 32 Ta pped
Holc~,
M3 Tapped HOIe~
.-
from 1M
rz
"
"
"
oz
SpecifiCEliollS8,' dlor agency recogrutJomi do nor necessarily apply /0 all moaeIs wilhin 8 partiwl81series. When rooI tipie rolinr;s are lisled. no indMduaJ l3lirlg may be exceeded by rile combinaricr> of oIllers.
351 (of 550 ) 2006(-2016)
352
9jI National
.-"
-.
;c.I Semiconductor LM138A1LM138, LM338A1LM338
5·Amp Adjustable Regulators General Description The L\lI38
01 adjus:abla 3-:8m\Il\IlI po$ilMl IIOltaQ.
.-gulated a. Ion; u :M
mauntJm
,"cui 10 outPtJt dill..........
i.,-- do not SI'1OI'IoQrCtIil outPUl p.nc1 n..p.an....-.s "'_ l... , ~ ' _~ 'Il
~
dell
.... rd ~ oN'! 2 ......en 10 ..c ll'le 0VlPJIl ItOIlage.. C¥tIU c;rcwt dBsogn IlIU ..-.IlIld in ~ to.
l( -*-b ani ~ '" • S1UlCaI'C Sl1NI TQ.3 ~ ",",-lIlOSa ... I. T i1 U C3SA '5 n'~ 'tlr - otO"C S; TJ S
W"'.daI
~_
........
:lie e'- """"t lirTIlt craRy allan
eo 0& ora_
' ..... .,. Iu~"iII_d lI'le
0_ .
iIll!~P'lG~
_~.dy. "" ~1OrS "'8 ~ . . . - IN
e_
is
sowat«l "" TJI eMl 01 eeeee :0 '1!"tlI'(l\I8 lI'a/'lSMt'Tt f'Mp;lftSe. ...... byIlUS"'Q ;". oJC,"unenI C... _ ':he ~s "Pel_ felMC'''9 ~ • ..., ' . . . .tors 01 (Iit(:r_ dMigns. lI\e LM13e ;,"5t'al ,"=,'; a g ll, I " OO"e' 01 severalllUl'ldred >'011$can b..
e-c-c !: ;J
s; - 1Z!>"C.
Features G...,amlHd 7/J, ~M e,, ~1 <;.\11'''''1 • G....,.."leed 5A 01.1"",,, C~H.nl • Ad~!lIbIe Ol./lllYl dow'" 10 1.2'1 •
• Guarattteeo ltlO.......1'O g "'II'Ol'
• C~rrent ~llnIl constl~t ",,'M ' ~~,a l\.l'. • lOll ,," e1ec::nc.1j ~n ,n l" e""'''' , ,,.~
• 0vttJul: ~ •
sno<1..::rl;lJ1l DtCIt'C".ecI
G........_
1-" C'I11I:"" " OM ,,_ . ,'.... 1'lOI
"""""
• GuwarR&ed mu.
o.c, o-.n :....
(tM 1S8 A.
..
,~ tlOIl (t.... , ~~".
LM33eA)
.........,
I GuIrvtt_
.nc:r_
pie . -...:ton .
tel
m.m
+ ' 2!'C. 1.Ild thllM3Ja .. ra ted
CII-
~ C\oITeI"Ile fr!)lft II'le f8lJo.'I.Itottot snort ~ el l''''• . ~l$ .. I
nol e~e-;to(l.
a
lr ¥1'5rS ;or ~ ~
,. 1/ftICl..- ~&ll t... el :he LW1:Jl111111i11''' ~
rent
~
mu.
'13 ~
·aa o
·~llCIri
{lM 13aA.
Applications •
~w::K" ~_ i U!l:l . i S
• eor.tam CYrTenl rll9U"" crs • 8an"Y cnlVQ....,
Front Vl_
o
Order N_ _ LM33&ATI LM 33IT S_ HS PKO<~ Mum_ T03B
3onom VIew Ora ...
~
'.:J 13aAK STEEUUI13f1KSTEEU LM3: . .. ... STEEUUI33Iolll STE EL s... "s p~ Hum_ K02A
1-1 09
.,-
352 (of 550 ) 2006(-2016)
............................ ... , ......, ......." ............
353 i,,,,- -1
,..,• I '"
t' ~'
; .'
I,
I"IV , '~-'
,.' . \
. I I , '
'f',.'; ·" !'
Ci: 'I
Plastic Medium-Power Complementary Silicon Transistors .• . doslgned for geMral-purp09a 9mplillar and (ow....~ed switching a~licahon,.
,;; -!t$:. ':.1· ,r
I, ,•
-~ -~
,'. s , • ", J r.~ ,.'i' ;j "-
"
,
,.:~ I . - ~-
, :·c -,I
(:t! ~;,, ' /
;,:
f ~
,'f~f~\' ~ :~
."',:.
!j'~j
;, ,J.: ,! (' } ':. :' -'. ,' . ~ 4" :1.' :
f j, I' t:t~"
.Mil ' ~1
:-;,=."'.-,'~1
;;;;;;;;::;::-;:= ;::::= -:: .
.o.oIRBipol ar Power 1,,,,,. ,. ,\11' "''''''..... '"'.. ,.
T IP 10 1* T IP102*
HlijIl DC Cumlnl Galn-
liFE · 2500 [TYP)@ Ie " ...OAd: ConllClQr-Emill e. Soatamg VollagfI_ @I 30 mAde VCEO (IYI ) " eo vee (Minl - TIP1 00 . npl06
PNP
.. 60Vdc (Min] - TIPl 01 , TIP106
. t OO Vdo (Mill) - TIP102, TIP107 l ow CollAclOf-Emltler Sall)raU on Vollage-
T IP1 0 S TI P106* TIP1 07*
IJCE{SIlIJ .. 2.0 vee (Max) @ Ie ~ 3.0 AD;;
. 2.5 Vdc (Max)@ le . 8.0 A40 MonolithicConalruc:tion with 8ulll-l n Bu..-Emll... Shu..., Roliiston l Q-22OAB CompactPackage
_ _-
... .......
' MAXIMUM RATINGS
:~.'. ~:
I . .•. "
NPN
TIP100
RIUn"
Symb ol
~0...e ~1 1JoII10I
TIP1111 , nei ee
TlPt02, TIPI07
""
" ••'".0 "
' 00 ' 00
VCEO
CoINlot-81.. VoIago
Vco V' Ie
Ernrt.-e... VolllQll CoIINlor C~mml
TIP1ClO, Tlpl11S
CoroII'IUOus
P. ..
•
Bt.MI CUlT' ''' ToIIl P _ () ..1paII00Il 0 TC. ss - o D.rm..tIow 2S·C
E
Po
""","".lur, Rlrv-
BAMPERE COMPLEMENTARY SIUCON POWER TRANSISTORS 80-80 - 100 VOLTS IOWAnS
Ado Ado
w_ wr o
eo 0."
lJnctI~ Ind~ lo»d EnetlIV (11
DARLINGTON
Vdo Vdo Vdo
i.c
Po
TOItl PcrIoer () "ipaton@ TA.2$ ·C 0.,,"' 11110'" 2S'C Op.lld"" Ind Slo"gl J~nction
Unll
00
mJ
"
W. .
O.o Ul
TJ, Ttltl
.-
lIiEflNAI. CHARACTERISTICS CflerlCttftttlc It",",,, ""Il.'lte, Jundloo10CIM
~ 65 1o .
....,.se
R.., R
TIl'lIm" RlIlIltra, J\Q;Ilon D Alt'b t. nl II ) 1 1 A, L . on mH, P.RF. • 10 Hz, VCC----;-20V, Rll€. 100n
o-
WI' C '0
150
I,,,
U..
'eM ' eM
62.5
CASE 221...-<15 TI)..2:K1AB
T" Te
U
IO
't,v I = &<>.'> e
<,
g
;L z: C<><-
"-
~ u ~
. I"
~ := C ", /7 , TO
o
•
~~ " ~
• ••
<, T.
10
.. .
<, I'-.. <, <,
M
,m
.~
T, T(NPEAATURErca
..
,-
Flgll r. 1. Power DeraUng
" .I.~ "....... .,. _llfol. '""""",,"""" <:II01:M ... ..... ~,. "'~ _ ilL" 7
MoIoIoia Bipolar Power " ..nsis\ol' Oevic:ll Data
oYo,,'l.-l~ •.
....,
353 (of 550 ) 2006(-2016)
,
II
354
•
., Glow Discharge Photoionization Detection Lamp (PID) - Modell 08 From the "Pioneers
c.= •
= ,... .. =• ,=.. ~
of PIDT/·,,,
Scientific Services Co. , Inc. P. o . Box 31 7. Rocky Hi ll, NJ 08553
108-10.0/10.6 The most popular of our line of PID lamps is the Modell 08-1 0.0/1 0.6. This model is used in all PID detectors employing glow discharge lamps w ith the exception of the HNU type' . This M odell 08 utilizes a small and efficient envelope (see Dimensional Drawing below). The VUV energy is emitted in spectral lines at 10.0 eV to 10.6 eV. (. For H NU style i nstl'U~.
Photo graph of Modf"l l 08
..--,
SH'
ou r origina l P1D lamp Madel l 0J)
Dimens iona l Drawi ng
i
I
I
ee ,=.. ...
-' I • '1;.7;2
,
,
.
~'-
-
,~
Dime nsions in inc hes
~
Only $ e'''"I,I1.. SeN" " a il e ... a th ,... monlt> wa ...,nty. p
354 (of 550 ) 2006(-2016)
355
METAL PACKAGE PHOTOMULTIPLIER TU BE
HAMAMATSU
R7400 U SERIES compact size (1 6m m diam eter, 12mm seated length), Fast Time response (rise t ime 0.78ns) r - - - - - - -- - - - - - - - - - -
The R7400U se ries is a subminiatu re photomultiplie r tube with a 16mm diame ter and 12mm sealed length. A precision engi nee red 8-sta ge electron muttouer (composed of metal channel dynodes) is inco rpo rated in the TO-a packa ge to produc e a no ise free gain of 700 ,000 times (A7400 U). Its imp roved meta l channel dynode desig n increases photoelectron collections efficiency b y 30% than the previous type. The R7400U series also featu res excellent response time wit h a rise time ot 0.7805. Various types of the R7400U seri es
( 'I Jj ,
;'
. ~:"" ;;,-'
are available with different spectral response and gain ranqes, including those selec ted specifically fo r photo n co unllng applicatio ns. Hamamatsu also provides a hem ispherical lens i nput option 10 the se ries (R7401 and H7402) , effectivel y dou btin g tho active area.
left A7«JOU
AI~ l:
A74()l/R74Q2
FEATURES • Wo rld's smallest photomultiplier tubes assembl ed in a TO-8 meta l package (1f7th c' the Hamamatsu R547). Th e necessary components are buill into a TO -a p acka ge wh ile retaining fun photornultipfee tube perf ormance to create a new gen era tion of photosenscrs. • Inc rease d photoelectron co llection efficiency. The improved metal-ch ann el dynode delivers pho toe lectron collection emceocy 30% higher than torme - types R5600U. • Photon coun ting types : A7 400P serie s. The A7400 P series is specially selected on account of low no ise and high gain fo r use in photon co unting ap cncenon s. • Hem's pnericallens window type s: A7401 (bialk ali), R7402 (multialk ali). Th e hem isph erical lens window doubles the effective input area to 12m m in diameter.
SER IES UV to Visible Ra nge
So lar B lind S tandard
- , - -_.
~ ul ~t i on .c:?~
UV to Near fA Aang e
R~7~'~O::OU::/~R~7~ 40~O~U~.::03l = R~74~O~O~U,':.O~6'-,_~ R7~'~O~O~U~-{)::'":/R:7C4?_O_ U ._ 02l_R_ 74~O U'~
R74QOU -09
For Photon Co:..J:1ting '- - ' .. W :lh Lens
R7400P-C1!R7400P-(J 4
R74QOP/R 7400 P-03JR7400P-06
- -R7401"(Vi"S]b"reRa:nge'j'
·..:=-+......,Rc7c4~02;;';;IV"ic'i~b"'le to Near IR"Range )
._. :!~_~ Yes
Yes
G EN ERAL
Dynod e
-_.._.. . Wei{;h:
:
Strocte re
R7"OOUiP Series R 74C1 fc:l 74::2
SP.'"""!l
R740 11R7402
.
..
_-
VOLTA GE DISTRIBUTION RATIO I arecccocs K 0 ,1 j 0 )"2 ~3 Oy4 i
Ratio
1
App:r,x. 5.3
,
--- -
-
8
--,. .
F; 7~ U'P
Un it rnm?
Me:e.1CI".annel
...
Num ce- of Stage
Ambia:ll.'remce-a w e
!
Desc ripti onIValue 8
Parameter fl.tlfll mum e necnve Area
p''":Jx. ~3
5
to +50 _- .8;) .
-
----
·C
-3D 10 ...50
Cy5
Dy6
g
--
0y8
Dy?
P
0.5
t
:-S ~hl~~; ;; ie'c-a; ~;~hh' ~; 1 ,e;u~;e;';; ~l~ 'MCle9~la:I~~; ava, : abiiit~-;I; '~~;;$- ;~'c;~;e-d:~ ;~',; ~,~o: ,or"l ",a : e~La; m ay'~~,~ PI~·;;e· ~ ;;~ ..;: ,",'",h---"C, S_d.U o:"e. . ' --- -.. __ -- - - - - - - - - - - _. _- _ __ - -- --- -- .. -l "t<"''' .11 10~ :um, ~ hc
,c' bl""110
b'; ,; ,' MAMATS lJ 's
" h . ,,~ .. w"~ ow'
o.:,
no" "" . 1\ 0 0,,11'":
c tc ce ·, I'~o~e "'0 ;'ar le C ~ (;
·,~ ~ :s
H"",,,~ ,,,
~ "Y
0:
~c
'r.50 oC'.. ,ti l'ly
:"0 ci'ce'"
~".c.'
,~ ~ .~ ~", .
1(;' po • • ,t·lc ,n"ee W'4cie ,
1>,..., h.. ,~,n Ie 1993 Ham""'''l'u
Q' c ·T i.", ~~ ,
~hc:onI C!
SP H , ~ , c" l\on, ~,/'
h K
355 (of 550 ) 2006(-2016)
356
SCHEMATIC INDEX (page 1). cmCUIT BOARD R E v SCHEMATIC MODEL 8610-C LAYOUT
C
MODEL 310 LAYOUT
B
AC DISTRIBUTION BD. 86101310 CIA
AC WlRlNG Al\'D TYPICAL LAYOUT
USED IN MODELS: 8610 310 110
2021203
OF 861G-C GAS CHROMATOGRAPH
IZJ
0
AC WIRING M l> TYJ'ICAL LAYOur O F 3 10GAS CHR OM ATOGRAPH
0
IZJ
0 0
DISTRlBUI'ES 110/210AC VOLTAGE
IZJ
IZJ
IZJ
IZJ IZJ
IZJ
0 0 0 0 0 0
0
IZJ IZJ
0 0 0 0 0 0 0 0 0 0 0
IZJ
IiiJ
AND%8 VAC TIIROUGHOllT 1HE G.C. EPC, TK\tPERATIJRE & DETECTOR PAR AMETDt SETPOll'iT CIRCUITS
8610 DISPLAY BD. (pagel)
G
TER, AIR COMP ~ DISPLAY DRIVER
8610 DISPLAY BD. (page 3)
G
FID IGNITOR, VALVE ACTIJATO R RELAYs, SPLIT VENT SOLEr;OID
IZJ
0 0 0
EPC.TEMPERATVRE & DETECTOR
0
IZJ
0 0 0 0
IZJ
8610 DISPLAY BD. (page 1)
.~
cmCUIT DESCRIPTION
G
ALAR.\{. CARRIER
m
310 DISPLAY BD. (page I)
C
PARAMETER SETPOI/'.' cmCL1TS
310 DISPLAY BD. (page 2)
C
AIR COMP., DISPLAY DJUVtR
310 DISPLAY BD. (page J)
C
FID I GNITOR, VAL VE ACTt'ATOR RELAYs, SPLIT VENT SOLE. OID
110 DISPLAY BD. (page 1)
B
EPC;n:M P ERATtJRE & DETECTOR PARA.lI,fETER SEfPOINT CIR CUITS
110 DISPLAY BO. (page 2)
B
AIR COMP., DISPLAY DRIVER
ALARM, CARRTER FILTER,
x
FIX> IGNITOR,
EPCBOARD
D
PRESSURE CONTROL
IZJ
0 IZJ
OVEN BOARD (page 1)
E
POWER SL"PPLY. JITTER cmcurr, CHASSIS COOLINGFA. ClRCl..iIT
IiiJ
IZJ
0
0
OVEN BOARD (pllge 2)
E
COLUM:'f OVE."i HEAT ING AND COOLING CIRctnTS
IiiJ
IZJ
E
IiiJ
IiiJ
0 IiiJ
0
TnU'ERATURE CONTROL OF HEATED ZONES . C IR CUIT I.
0
IlEAT BOARD (page 2)
E
TEMPERATI,"RE COl\TRO L OF HEATED ZO~S. CIRCLTIS:Z &. 3.
181
181
181
0
PURGE & TRAP BD. (page 1)
C
TRAP J HEATING CIR CUIT, TRAP COOLl:'fG
IiiJ
C
TRAP 2 HEATING CIRCUIT, SPARG E GAS SOLE"'iOID
IiiJ
0 0
0
PURGE & TRAP BD. (page 2)
0 0
HlVOLT BOARD
B
IDGH VOLTAGE POWER SUPPL Y FOR FPD ANDPID DETECTORS
IZJ
181
181
AMP BOARD (page 1)
D
AMPLIFIER BOARD POWER stl'PLIES
IiiJ
181
181
AMP BOARD (page 2)
D
TCD PROTECT CIRCUIT. POWER SL'PPL Y & A.\ U'LIFI ER
IiiJ
IiiJ
181
AMP BOARD (pllge J)
D
ECD ClRCLlTRY & AMPLIFIER
IiiJ
IiiJ
IZJ
AMP BOARD (page 4)
D
DELCD POWER suPPLY
IiiJ
181
IZJ
AMP BOARD (page S)
D
FID & DELCD A.\1PLIFlERS
IiiJ
181
AMP BOARD (page 6)
D
PID & FPD MU'LlFIERS
IZJ
IZJ IiiJ
IiiJ
AMP BOARD (page 7)
D
OYfIONAL Z!'J(O eors AriD ATIErWATOKS FO R DIITECTOR AJ\.U'LlFIERS
~
~
~
ACCESSORY RELAY BD.
A
AID L'ITERYAC E BOARD FOR AUfO-SAMPLERS
IiiJ
IZJ
SPME BOARD (page 1)
A
SL"iGLE PHASE MlCRo-EXTRACTION CO:'n'ROL C IRCUIT
181
181
SPME BOARD (page 2)
A
TEMP£RATURl: COrrrROL OF HEATED ZONES. CIRCUITS Z &]
181
181
0 0 0
HEAT BOARD (pllge 1)
ELECTRO~C
GAS
,\!
0 0 0 0 0
0 0 0 0 0 0 0
356 (of 550 ) 2006(-2016)
357
SCHEMATIC INDEX Ull!ge 21 CIRCUIT BOARD SCHEMATIC
R E V
5IlJDENT REAT BD. (page 1)
A
STUDENT REAT RD. (page 2)
A
STUDENT HE AT BD. (page J)
A
EPC-HIVOLT BD. (page 1)
A
EPC-WYOLT BD. (page 2) ~ODEL 2021203
AID BOARDS
SERIAL DATA SYSTl'.:M COMPONENT DATA SHEETS
CIRCUIT DESCRIPTION PO\\'ER Sl.'PPLY, JI1TER CIRCUIT,
8610 31 0
110
ZD2nOJ
D
181
D
D
181 181
D 0
D 0
f'RESSlIRE CONTROL
D D 181
181
181
D
A
WGD VOLTAGEPO''''ER SUPPLY FOR fPD A.'iDPID DEI'ECTORS
181
181
181
NJA
LAYOUT OF MODEL 20Ul03 SDUAL DATA ACQUlSmO."I1 BOARDS WJTHL~ THE G.C
181
181
0
D 0
AIDBOARD TROUBLE-SHOOTI."OG. TESIlNCA..'m MAL''TAffiANCE
181
181
AD597. OP'.Ml. L......1I... ltiAU7.DlGrrAL DISPLAY. LM114. PRESSt"RE SEI\'SOR, ACIUATOR, ID'PS
181
181
0 181
181
D
D
D
D
D D D D
0 0 0
D 0 0
0 D 0
D
D
D
D
D
D
D
D 0 D 0
0 0 0
0 0 0
D 0 0
0
D
D
D D 0
D 0 D
D 0 D
D D 0
D D
D
D
D
D
D D 0 D
D
0 0 D D
D
D 0 0 D D
D D
D D
D 0
D D
NJA NJA
COLlJMNOVEN HEAn~ CIRCVIT
TEMPERAnJRE CONTROL OF IttATID ZO:''E. COOLlNGFAN cuecurr OPTIONAL RELAY CIRCUIT
~IS
t: LI:Cl'RONIC GAl'!
-,
USED IN MODEL.
0 D D
181
-
357 (of 550 ) 2006(-2016)
358
U!o....' . .."· ... 'II!!!!
"""y,,,... -7 Iml -".. 10
'''"
.u
OM .
.
YI.'_'
"..w.... -,
, ro
DISPLAY
. 'Il l'" ; ~u ou -7 TO: : : 'r.t'0 ...~~ ~u ~ .'lA''' I ! ! : .'t, •••• ------'"""""'"'''"'''''''''¥j'...... J ~ 'OMlICWlO
DISPLAY BOA RD
,j ,
.. OOCII.... .
H ;:1.23;SIWJ111 =fJ• •
,OU-:;I="I OVI. ....1. -----~"I1:J1oO
I
.
Jl","O.
ctlJDo: __• '\ --g lOOlTll Cl'OIII
.,~.
I
•••
i
OVEN CIRC ULATIO N FAN M OTO R
- :II
~ r-
~=-=-::
'ODll~'O""
Ae
""....~'"
\11""
.z: -==~.J ..., ....1I LOCCI
-
-.........
HEAT lOARl)S , 0 0 U f CT"".
.,ov,nfY l"= =il <,
=a:r _
¥
/'
o
o~~. @
II
_, ~ 10 D\II~ IDARD, ~"""'''·''''Rl!1
I:
i! ...C lIO...1I ...... IC ~
-
~
O
T>IE CHAit .. '"" ,, OillATn CHI
DC .ROII Tile "010"'10.
. . \/Ql To "'" ... , I ~ 1HE ."".. , ''''' ''1 11100'10
"" "'T""
.""ot
Mil
I II"....... E IIRlDOE 't 1$ " '£0.
FP O
' .0..
• ~QlIlAIORI
o .....••
AMP
o
flO
o
0
::
; ' C TOflI
AMP
! •.
I
A
. ,_.
.-
I
'~ " "" TlC
A
POD
"
AM P
P L I F I
-I
'. II l lii II
.·. . 0, • • i,
0 ••
""""'- '-
I0 0•
I •••
··
• • •
~ ~
A
DELCO
AMP
I
R
0
E
I
SUS BOARD S ARE THE f PC, HEAT, OV E ~, PU RG e & TRAP AND HIVOL T B OARDS. THEse BOARDS CON TRO L THE GAS PRE SSURES, DETECTOR PARAMETERS AND TEMPERATURE OF HEATED ZONES W ITHIN THE GAS CHROMATOG RAPH. THE CONFIGURATION OF THESE BO AROS DEPENDS ON THE OPTIO NS ORDERE D.
'--
..
~
0 0
,
;0
.WlTC M
,I .
CHAS SIS CIRCUL A TION FAN
..... I'i ,
lOO"lll
0 "-
_________1
~
,
_no
c..u.IM'
..... toiti'
.....~1 ...,
' ....0.
_.-
/'
l!:=} .o~~ ~. r,.-. ::::~",,~· <=~ IlJ~U.T--tt-l---+~~~J ..u,.... 4t ~~. .
F£ GOJlATORlI
\
II...... eOl<"~c,IO'" 1:[v:,li;::~:'~~1
o
AIR CO MPRESSOR OPTION
',. . rn = . I
'
0 11.......
'\Y
"I
I
.o~
-, :t...
M'."'!_
_.
l' "'''"<_ 1. ~ _ I ""
BU S BOARDS
_ AC"' ~
'011 --..
H I """'"""
.,.......~
. '" ...., I
_ _l it
......"...
~ .. .
~"'''D,
.~=~. r~ ~ _.u I;1I?r' 'I 'I ' iI
•
'm
-_..
<' _ .• • •
._ . :
.. lU"" -
I ":~
OP r oo ~
,c
"me"
~
, - - - J'O AC .... ' , OClIlIW. ACCI
- " 0 "...c''''''' o III,,",c TOOVEN OOAR O
~
MAlC'tL.SSI8
OROUND 9TUD
- -
~
...... ~ o ...,... lMU II'A<: 1 CU Ll "'OM OQ"' . VII-II Tll NllIIO.....e
"0"
.on "
-
- -
~ -"
- ........i-..................
AC POWER LIT
--'!'-n-n-n-fj;- -- --- ---
'III I
I, ,
,
ACWIR'
AC DI STRIBUTION BOARD
A.ND TYPICAL LAYQUTOF TH E SRI 8610·C GAS CHROMATOq
,
_.
H R.~:: ·:::~;.'::. R
358 (of 550 ) 2006(-2016)
359 ~ IODlSPLAYBOARD
...
Wi
r .._-I
COMPRESSOR OPTION
-1
II~
r-:
I
~=: W .
~
•
.j!1
C1"ClILAtlo",
"-.:"~
I
l
' 0 .....0 0IIII
-_ .... ---_..-..._-"" .........=<;:1;
-
~ ~=
-_. ~
•
--
'r1
~
• -"'J
~-~
-~ N\1II' ''-'' , _ COW\IT1.Il
~
FANMOTOA
••
.oc.
I
I : .: n
OVEN CIRCULAnON
~
~i
· "I I:· :. illh ·. :
/
-
_.-"
I - •
~
~
--=8= ~
I ~I
/
Ii
~
.. --- -
...,,
--
·-1.234
._-
'-'---;1'AIR
,
_..
DISPlAY
_ _ _ _ _ _T. _ _ .......' _
. . . . _ . - . - _ . .1 ....
_~
_ _. _
".--_._-~- -
r-
BUS BOARDS - -
\ AJO
OOAAD
.... "
.
ffiil
I-
••
m
AC POWEI INPUT 'ARD--·......lI .. QO.NI_
~=
i
MAlNCHASSIS
OROUNDSTUD
rh ) 359 (of 550 ) 2006(-2016)
360
8610 AC DISTRIBUTION BOARD
............ INPUT FROM X·FORMER AND INTERLOCK SWITCH NOTe: F7 114A fUSE)
II
usee FOR TilE DELCO Bl\IOOI!
~
......,., ........... 28\/',\C.2
•
2IVAC1t2 ....
CTG~DIfII2
OTONon ....
~ n V ACjj2
UVAC'I2 . . . ::l4V81AS .... 24VBIAS .... 28""Of1 ...
=.••• .
;;:;;r 'lIA
'MA
,~
24V BIAS
t:::
2'\1 BIAS 2lVAC.1
28VAO.,1 ...
..
ACHOT
ACHOT ... ACC
. "
••
,.
~ e-I
n
,.
"
28VAC /111
...
ACC
1;t;i:1~ < ug:u0 • • ~<
m
MAIN CHASSIS GROUND STUD
;; U
-....
...0 '
0 u:J: U
lOti;::.:; U
~
~
0(
<,
U;l:t!
i
-e~u
0(
~~<
.
;;tnni ~
::>
~:J:tl i:~o(
"
-15
;t;~
~nj
~
~ ~~
~
~utl
~.<
~
~x~
OUTPUT TO AMP BOARD
;1:;.6 O u
0(
ux
<~u
~ ~
'"
USED IN THE MODEL 8610 GAS CHROVIATOGRAPH
./
SEPA RATE GROUND WIRES
310 AC DISTRIBUTION BOARD IIl",,-''''II.
INPUT FROM X·FORMER AND INTERLOCK SWITCH .
...... "
• •
II..
t---.- 28VM: 12 •
28V",0'2 ~ CTONOIZ_ nVAC.2 __ 24YBlAS -4
CTQHDU
~215VACI2
0iffiT
~ ,. , ,• • -
NOTE:U (14A.FUSE) 1$ USED FOR TKe DELCO
•• ••
., ..,. e-I
BRIDGE
"
••
•
24" BIAS 24 V BlAS
::I"VElIA!
...
28\/'''C'1 -4 ACHOT -4
ACHOl ACC
.
Ace
rh
.
u:r~
,,1--1o
~.
"
i~.G
o<
~
MAIN CHASSIS GROUNO STUO
-4
n vAC" - .
~ 21VAC., 28VAC fll1
<,
0 '
~
0
~:ro
-
..... - 1"'u "'o u u u:r
>~~ «~ o(~u ~ 0(
OUTPUT TO AMP BOARD
-4
USED IN THE MODEL310 GAS CHROMATOGRAPH
ea REV. ./
SEPARATE OROUNG WIRES
Plge1of1
861G • 1G • B
Fllenlm.: ACDIST·ea,tcw
AC DISTRIBUTION SCHEMATIC Dat t '
! /!Ml
REV, Oall: &1131.
8 :R.Fnl' B : M.
( ( 360 (of 550 ) 2006(-2016)
361
Rl lSEE CHART}
R1 (SEE CHARTI
ELECTRONIC PR ESSURE CONTROL
CHART
PUSHBUTTON CIRCUITS. SEVEN POSSIBLE CIRCUITS.
+UIJ P1
~<
.,
+UV
ALSO SEE CPC BOARD SCHEMATICS.
>OK
~
>OK
, PHONEJACI( TO EPC BOARD
PHQNE JACI( TO AMP BOARD
J2
J1
AIR' AIR 2
TOTAL 9ETPOINT PUSHBUTTON
I
ACTUAL PUSHBUTTON
SIONAL + TO DISPLAY BUFFER AMP SEE PAGEl
-
B
LED ISEE CHART )
"1 \:lI!E CHART)
~
CARRIER 1 ONLVTO TCD PROTECT SEE AMP BOARD SCHEMATIC
R' (SEE CHART)
.,2V
~
' WITCH
Jl R
....-;!'.=:-_
TOTAL SETPOINT PUSHBUTTON
,
ACTUAL
PUSHBU~
•
.~ -';> LED (8EE CHART)
I l~; I} , ~-'H;
._... ._~
DISTII'8 UflON
0 11. TRAN SFORIIIEII. IlOAA~
...-.m.' 1
--.-.-".. • "
~
LED (SEE CHART )
POWEAS UPPLY 5l!C TtON FROM ~C
-
.~
~
• Y"
,
\
".L
.. ..T
• ---:L. ':.':
Tt '~
~
TEMP. ACTUAL TO ALARM CIRCUIT SEE PAGEl
2.2M 220K 220K 220K
,. ,.
WI G ReE N ORI!I!N GR EI!N ORI! IIN GRI!I!N GREBN G RII!.I!N G Re E N
B EAD VOLTS R!!AC TOR TI!MP
120 YE I.L OW 60 .4K YII LLO W TCD PROT . CT 4UK Rllo VII'IIT. OV I!N P"OT. :l90K ft .D Fl.AM1i 10 NIT. ' OO o h mYE L l.OW PlD CURReNT 40.:lK YI!I.1.0W HID C U .. RIINT 4.02K YELLOW PMT VOI.TS 20K y eLLOW ece C U" RI! NT " .02K YI!LLOW "7.7K O""NO I! .ee.7K ORANO. 10 0K O ft A NQII 10 0 K O _ N G Ii .. e3K ORANG . 220K ORANGR SlL3K O_NGB eO.4K ORANGl! "".7K ORANG E;; 48.1K ORANOB 40 .2K ORANG. 40.2K ORANOI! 40 .2K ORA NGE 40.2K ORANGE 40 :2K ORANGl!! 40 .2K O R A NOS 7l1K ORANG. 1I0.4K ORANGE 44 .2K ORANGe 100K ORAHGS 40.2K ORANGl!!
DISPLA Y BOARD PUSHBUTTON CIRCUITS
.. u •
Ii......
~ ..
'T'':.':
7
J
SIGNAL + TO DISPLAY BUFFER AMP SEEPAGE:l
..",......
.. . *..,. ....... ••• H~I~-11~:.rI~_.
L' '''-
!.::'
I
TOTALB~ PUSHBUTTON
SIGNAL + TO DISPLAY BUFFER AMP SEE PAGE:l
ACTUAL PUSHBun ON
J2
I
\
•
LOCAL SU PQINT PUSHBUTTON
V
I
./
PHONE JACK TO ItlVOLT BOARD
>OK
~.....
PlO OR FPD LOCAL SETPOINT SPDT ON/OFF PUSHBUTTON
HEA TED ZONE PUSHBUTTON CJRC UITS. FIFTEEN POSSIBLE CIRCUITS. ALSO SEE HEA T, PURGe &. TRAP AND OVEN SOARD SCHEMA17CS.
.,
..2V P1
S70R_58
V;
LEO ISEe CHART)
PID ANO FPO PUSHSVTTON CIRCUITS. ALS O SEE HIVOLr eOAROSCHEMATICS.
>OK
"OK
HYDROGE N 1 HYDROO l!.N2
\
\ R
VJ
'>OK
CAFlRI&R' CARRII!I'II 2 PURGI!
VIAl. PRIl SSURe
LOCAL seTPOINT PUSHBUTTON
~
R1 VALUE
.11"
r
____I
P'g. 1 or Ii
Flktn.me: dltpl.y·k1 .tcw
8610DISPLAY·K SCHEMATIC
",Jill;,l ¥Ii]; w )
361 (of 550 ) 2006(-2016)
362
,
~....-_
+12V
CARRIER FlLTER BAKE·QUT SWITCH (MOMENTARY)
01
.30
AIR COMPRESSOR ACCIRCUITS
' WAn
100 OHM
10
.L ei ~~)
R1 02
~, ... uF
100K
8
.+1.2VLM'"
19K
r
'7
12
Rt & cs PRODUCE A FIVEMINUTE TIME CONSTANT. CARRIE R Fl. TER BAKES FOR FIVE
U'
~
\"
MNUTES.
OVEN MAX
AND TEMP. ACTUAL
FROM HEATED lONE PUSH· BUTTON CIRCUITS
'EE
PAGE 1
I I I I
)-i I I I
I I SIGNAL . f ROM ALL PUSH. BUTTONS
.. r:: • • ~ . " ..
'/
6 I
.1
55
seRt ~
h
D12
-e-
Q6oo 4
/.-1' r'\
A IR COMPRESSOR
I'f
- -=
TO C ARRIER FIllER +
I:
TO A IR COMPR ESSOR +
r=-
=
ON 1OFF SWITCH
1N4004
CARRIER FI LTER l EO
-
...
,
TO CARRIER FilTER . FRO M AC HO T BU S BLOCK IUNSWITC HED) FRO M AC NEUTRAl. BUS BLO CK (UNSWITCHE O)
TO AI R COMPRESSOR •
ALARM OUTPUT TO INTERLOCK SWITCH
ACHOT U NSW ITC HED
U GHT8 WHEN
h
07
1K
L M324
AND POWER RELA Y.
FILTER IS ON
TH IS CIRCU IT SWITCHES
+u v <,
+UV
R1
. _. ..
110K
lOOK
1K
Off AC POWER TO THE
THERE ARE EIGHT ~U1 "" TO VERIFY TH E THERMOCOUPLE RANGE OF FIFTEEN HEAT lONE CIRCUITS. 1N91 4 3,12 1,14
U1
..~:~ ,c
2.1'
I OI Q. C
&,10
U1 E,'
I
L.M3 24
10K
1N91'
~
,.
". \
L M3 24
" ~,
I' 20K l ERO P OT
~
1M
U2 •
+511
, ,,\ '
- '/ 2
~l'I
.
SIO,(GND ) 810. +
Lf3 58
~ • • D •
c,,_ ""ooo
~ ""'" R
Il......y
013 OISPLAY
_
." -;;; rw : - 1.234°°° "J
-;
-= -=-
, /
r: f-r
SIG.IN
DISPLAY
TOGG LE SWITCH
DISPLAY BUFFER AND ZERO OFFSET
1" 'ERt.OCM .Wl1....
LE Dl-IOHTS WHEN THERMOCOUPLE GOE S LOW
ACT UAL ..:::.
c.:..; .,. O"O~
"
1K
ALARM r=1
=.J
02'
LMJ2.4 OVEN
+12V
.n CtO _
SCR2 QGOO'
~.
.10
~.
.n
I I
MOC3030 (220V.MOC30411
,
L
./
, I'.. , U' ,
." ,1-;'
,a ~ •h 1
BUS BOARDS IF THERE IS A THER MOCOUPLE CIRCU IT FAILURE. SEE AC BLOCK SCHEMAT IC .
100 OHM 1 WATT
U'
...;.
CIRCUIT
D1.()4
+"-7••
100 OHM 1 W ATT
ALARM
'I
LM 324
&EE PAGE 1
,1
/
rnOCJOJO (22OV.MOCJ041)
+UV
R2
U'
1 WAn
~
100 OHM 1 WATT
1N40 04
+ t2 V
100K
AC HOT UNSWITCHEO
CARRIERFIt.TER AND
100OHM
I
Pl gl2 o'5
FI1.nama: dl spll y·k2 .tcw
DISPLAY-K SCHEMATIC atl: 0 / 28/
ete:
.'
1
"
362 (of 550 ) 2006(-2016)
363
FlO IGNITOR ADJ USJ1I ENT POTP11S TYPICALLY SET TO -400.
BLACK 10 VAC INPUT FROM TRANSfORMER
__ ae . - ae
H -I £ 000 uF (+) .., +
n~
251/
L..!!..J
35 AMP BRIDGE
FlO IGNITOR A SSEMBL Y ON UPR/G HT M~TA L B RACK ET ON THE LEFT SlOE OF THE CHASS 'S CIRCUL A nON PAN
H
•.i!l
-evoc CHASSIS CIRCULATlON
FID IGNITOR NORMALLY CLOSED MOMENTARY ON SWITCH
FAN
RED
eecn n ea
MAK VOLTAGE. (_fOOO) -......-..
--J r-,.
_
SO
LM338
VIEW OlIT~ ADJ
100 OHM 112 WAn
-
J1
• 12 W C INPUT
SEW Dll'lT VOLTAGE
....
IGNITORlNPDBEAO ' OH"IAT ROOM TEMP.
PLUGS INTO PUSH TERMINALS NEXT TO DETECTOR ASSEMBLY
N .
.n"
.,
20K
:; /
r
0 LOCAL SETPOINT PUSHBunON
,
0 L
TEMP. ACTUAL TO ALARM CIRCUIT SEE PAGE:Z
SIGMAL+ TO DISPLAY BUFFER AMP SEe PAGE 2
<,
flO IGNITOR ON DISPlAY BOARD
.,
ADJUSTMENT
<,
TO IDENTICAL CIRCUIT
t.
AS ABOVE
\"
J1
/
,
YELLOW LEO ~ INSTALLED BACKWAROS FOR NEGATIVE FIOIGNlTOR VOLTA GE
PaT Pf IS TYPICALLY SET TO-300.
OVEN MAX PUSHBUTTON CIRCUIT
SIGNAL + TO DISPLAY 5UFFERAMP BEE PAOE2
PUSHBUTTOti CIRCUITS
TtOlNPD B!'AD
R1 IS!!!. CHART)
\
...-
ACiUAL PUSHBunON ,
IGNITOR INPUT FROM ~CHASSI S SET TO-400. TRANSf ORMER . - ae (+) .., +
" I
100 ' OHM
TOTAL SETPOINT PUSH5UTTON
V
, FID
1K
P1
I:J' 1K ...-
PHONE JACK FROM no IGNITOR ASSEMBLY
HARD-WIRED TO BRIDGE
rl7 '<,
•
V
"1.I-
U
\
D ...- - .
G
ecrroe
FID IGNITOR CIRCUIT
WHEN MOMEHTARY SWITCH IS FLIPPED UP, I GNITOR IS AT
TID/NPD VOLTS CIRCUIT
620 OHM
:J' 500.,OHM
\
TOTAL BETPOINT PUSHBUnON ACTUAL PUSHBUTTON
PHONE JAC K FROM NPD IGNITOR ASSEMBLY
I
<,
T1OINPO VOLTS PUSHBUTTO ,V CIRCUITS ON DISPLAY BOARD
8
YEI.LOW LED INSTALLED BACKWARDS FOR l'lEOATIVE TIOIMPD VOLTAGE
SIGNAL. TO DISPLAY BUFFER AMP SEE PAGEl
/..
'> \,
r
I PIge30te Fllenam.: dlsp lay_kU cw
DISPLAY-K SCHEMAT.IC ' . ·12120 , Ill:
"
. ens e
•
363 (of 550 ) 2006(-2016)
364
)
! SOLENOID CIRCUIT FOR ACT/VATION OF 'SPARGE', 'SPLIT VENr. 'CRYO TRAP'
AC HOT
AC COMMON
TO LIGHT THE VALVE OR VACUUM PUMP LED(S) ONLY, THIS SECTION OF ANY OF THE THREE SOLENOID CIRCUITS /S USED.
UNSWITC HEO UNSWITCHEOI
CK T,11 1
THERE ARE TttREE
100 OHM 1 WATT "':20Y.M OC 3 04 1~
MOC3030
ttln ... ... u
SO L ENOIDI INP UT FR OM
'10
.
'
.!~!?
- ,- R" m
R14
i'r ....ra ,-
~U-~
.,
r,- - -."
IDENTICAL SOLENOID CIRCUITS TO Bl!'LECT fROM. SOL ENOID CK T• • 1 SO LENOIO CIl,T. U SOL!! NOIO CIl,T• • !
l.
'
I
r-e:',
,...
L e-!s
_
~
u.
Q'
"10
SEEAC
~
R13
---
TO
JUMPER PINS 1 & 2 OF THE MOC. 00 NOT INSTALL THE CHIP OR THE SOCKET•
MOe PAOS
.,2V ~1-- --r-
~
SOLENOID
10K
100 OHM
~D'.
VALVE 2, VACUUM PUMP: YELLOW LED (INSTALL ED BACKWARDS)
JUMPeR
10K
TO Lf. O
BLOCK 8CHEM.
r- -,
2 N3 10 3
,
Il
~
-ft;
VAl VE ' 2 011 • VACUUM PUMP
SOLENOI D CIRCUIT FOR A CITVArlON O F 'SPARGE ~ 'SPLITVENr, 'CRYO TRAP'
\SOlENOID ell.'
.121
.,,, SOLENOib
'""" .., !'R OM
.~~ .... " ..
AC HOT
100 OHM MQC 3 UO __ __ _• . , W ATT · ~201l.MO.. ~ ~~ .~
.
'
• 1I t1
- ,.
R" SCIU oa0 04
I ::..
~OlENOIDCKT·t31
"0
~
t'"""..,0
T ::.:
I
-
AC HOT UfIIl WlTCHf D
RL.Yt
R1e
10K 2NJ903
II
O.
VAL~ :
eee sc
SOLENOID CIRCIJIT FOR A CTIVATI ON OF 'SPAR GE', 'SPL IT VENT', 'CRYO TRAP'
~"" FIl.OM
'\ _
BLOCK ' CH ~"".
-uv
RELAY CIRCUITFDR ACT/VATION OF 'VALVE l'
TO
~
SOL£ NOlO
AC COIolMON
UNSWlTCIlEO UN S'NITCIIEO
VI!LLOW LED
(INST......LED aACKWARDS,
'1:
AC COMMON lm !ll'llfCHED
100 OHM 100 0HN
1 WATT
' W ATT
.""'~
"''''
TO SOLEN OID
see AC
(I t OCI\ Sctl EM.
DISPLAY-K SCHEMATIC
PI g&4of5
FU,na me: dl.pl.~.tc:w
0,
"
. 42l2DJi~
;1611IlOi
t re,
: R. Fenllkt
ytpus
364 (of 550 ) 2006(-2016)
365
'.
VIRTUAL OVEN PROTECT
R1lSEE CH..... . ' +12V
"
'OK G LOCAL SE1POINT PUSHBUTTON
R
TOTAL. SETPOINT PUSHBUTTON
ACTUAL
PU~TT.2.!:!..
PHONE- JAC K
TO OVEN BOARD
•
7
SIGNAl... r O DIS PLAY
BUFfER AMP see PAGE 2
""
CIRCUlT S EE
LED (SEE CHART)
R1 (SEECHART)
•
TEMP. ACTUA.L TO ALA RM PAG E
z
MULTIGAS 2 TCO PROTECT
+uv PI
20K L.OCAL S!TPOINT PUSHBUTTON SIGNAL·
rODISPlAY TOTAL SETPOINT
PUSHBUTTON
BUFFER AMP SEE PA GE 2 ~ lClllIJ:£tt
PHONE JACK TO EPC BOARD
"
8
-
ACTUAL PUSHSUTION
'''"
..... . .K FROM CARRIER 1 10
~ LED (SEE CHARTI
DISPLA Y BOARD PUSHB UTTON CI RCUITS Tctl f R01ECT SEE N/.~ BOARD SCHEMATI C
"K "K FROMCARRlERt TO TeO PROlECT SEe.A.MP
BOARD SC ~ EMA TIC
P' lll 5 of 6
8610 D1SPLAY-K SCHEMATIC
..
Dale: 10118102
B
: M. W.~
a 0;
365 (of 550 ) 2006(-2016)
366
R1l SEECHART)
R1 (SEE CHARn
EUCTRONtC PRE SSURe CONTROL PUSmwTTONCiRCUtTS. FOUR POSSI8L~ CIRCUI TS. ALSO SEE: £PC SOARD SCHEMATICS.
t1 2V
OELCO ANO I!CDPUSHBUrroN CIRCUITS. ALSO SEE AMP BCMRO SCHEMATICS.
VALUE \,&Q 220K GREEN 2201< GREEN 1M GREEN
LOCAL SETPOlNT
AUXR..IARY
220K
GREEN
PUSHBUTTON .........: TOTALSEtPOlNT
TeoPROTECT FlO IGNITOR P1DCURRHlT FPC VOLTS EeD CURREtU
453K 100 40.21< 20K U2K
RED YELLOW YELLOW YElLOW
P1 20K
o
L ~
PUSHBUTTOH .........: TOTAl.SETPO INT
""""'R
J2
!
PU~ BunON
-1
L
ACTU AL PUSHBU TTON
-
B
-
~
-
/ SIGNAL + rODISPLAY 81.f'FER MdP see PAGE 2
I\Y /R
PHONE JAC K TO AMP BOARD
J1
2
SOARD SCHEMATIC
P1
S;; ~~ •
J1
........~....
'7
y
'PHONE JACK 'TO HIVOLTBOARD J2
HEA1EDINJ.1
z
0
IU K
ORANOE
DELCO BLOCK .(0.2K
ORANGE
FlO BLOCK
"0.2K
PIDBLOCK ECOBI.OCK
15K 44.2K
TeDBlOCK COL OVEN1 CHAt.S1S
---: ....-
\
1201<
.40.2K
383K
ORANGE
ORANGE
ORANGE
ORANGE ORANGE GREEN
---,
PUSH'unO' ~
J1
R y
SIGNAL.
- ' TODISPLA, BUFFER AMP SEE PAGE 2
PHONE JACK TOHEAT AND OVEN BOARDS
TOTALSETPOINT PUSHBUTTON ./
L _PU~U~ -1 ACTUAl
B
~
2
LED (SEE CHART)
\
.-r--::::::e:./~=--+-~
I
B
~
BUfFER AMP SEEPADE 2
LOCAL SETPOINT
" r:
./ TOTALSETPOJMT pUSHBUno, ./ ........._ _ ACTUAL PUSHBUTTON
R
DELeD REACT• 10.4K YELLOW
20K
PIC OR FPD LOCAL SFTPOI NT SPGTDNIOFF PUSHBun"" SWITCH
ACTUAL P!JSHBUTTON
YELLOW
SIGNAL+ rODISPLAY
Hl!ATED lONE PUSHBUITON CIRCUITS. FIVt! POSSIBLE ClRC4Jlrs. ALSO SEE Hl!ATANDOVEN SOARD SCHElIAnc s .
R1 (SEE CHART)
+1 211
c
»:
L Ee (SEE CHART)
+12V
20K
PU SHBUTTON
~
PID A ND FPD PUSHBUTTON CIRCUI TS. ALSO SEE!HIVOL r BO.ARO SCHEMA TICS.
"
/:
B
CAR RIER 1 ONLY TO TOOPROTECTSEEAMP
L Ee (SEE CI-lART) R1lSEE CHARTI
LO
Ji
\ ' y- -"1r--:!:....-: :.! :-- - -'
PHONE J ,t,CK TO f PC BOARD
~
*
lOCALSETPOIHT
J1
P1
~ B1 CARRIER 1 HYDROGEN 1 AIR 1
+t2V
P1 201<
CHART
L ED (SEE CI-lART)
2
_' SIGNAL.
TODISPLAY BlJFFER AMP SEEPAGE 2
DISPLA Y BOARD PUSHBUTTON CIRCUITS
TENP. ACTUAL TO ALARM CIRCUIT SEE PAGE 2
_1IV
1""11 n
PO'N£R S UPPLY I£CTlON
=q1 _
-
=
WI
f llOM AMP BOARD
Q
..~ lil
~ .,. 10 "
iIl.-..aq
.,.. . ..
CllOUCl
(DIll" .m
r~
="
I
(J .........
=
H I"
~.
... 1<1
=
I
- . .,
TN ~um"'. D~ TIQ
1
- . ..
UIIN(Hl2VDN PIU
= ...
.
_......."
ANDDROUND ON/'INIt.
Page1of3
310 DISPLAY..C SCHEMATIC
,...--_...JL...';:;"';"':..j-_.=.=:.:=r;.:':":":'::"'--1 IFliename : 310dll play-c1.tcw
c ate: 12flO19r
I
By: R. F'nll
366 (of 550 ) 2006(-2016)
367
so ~.....
" IV
BAKE-ouT SWITCH
.\lV
'"
"'lOOK
100 OHM 1 WATT
•
R'
•+1.2V i1.Mm
~
+1.7\1'
"'
10
~ 1000 \IF
lOOK
R'
14
-' 113
BAKES FORFIV!! MINUTES.
LM324
.,
07
'K
-
-
.,lV
ZONE PUSH·
>-
R' ' 10K
BUTTON CIR.CUITS
'EE
PAGE 1
PUSH·
_.
u:-=~
Ul
OEE
PAGE1
ALARM OUTPUT TO INTERLOCK SWITCH AND POWER ReLA Y.
ACHor
FlLTER' S ON
ALARM CIRCUIT
TH IS C IRCUIT SWIT CH ES
c 2,13
~324
u ... c 5,10
R.
U,
IK
e.s
. , 7,'
./ LM324
I
I
..
01.04
·1
.'\ 1
10K
•
LM324
~./
I
6
10M
+t 2V
OVEN
POT
~
ACTUAL
I
C10
~
A~"
L::!J" //
lK
(a ND)
2
510.+
., N
lF358
DlSPLAY BUFFER ANO ZERO OFFSET
• • •
•
L ED LIGHTS 'MiEN THERMOCOUPLE a OES LOW
,p "
.~ ~
0"
_
' I (LAY
_.
DISPLAY
_
..=.
" ". :.01.234 ••
-ev : : 810••
-
.. nnoa<. fWli CIl
10K
. '• 1 r-;/ of 0.01
IS A THERMOCOUPLE
CIRCUIT FAILURE. see AC BLOCKSCHEMATIC.
~,
L"'314
U2
"18
scaa
OtSOO4/
R22
7
ZERO
C. 3 .u
\M
0"
MOC30JO
RIO
1N914
•, ~ • 1-1
122OY-MOC)040)
2
BU S BO ARDS IF THERE
100 OHM 1 WATT
U'
.... ' "" ,j;: ~
a
u'
,
aurroas /
TO AIR COMPRESSOR.
L.::.
UNSWlTCHED
100 OHM 1 WATT
R19 SIGNAL+ FROMALL
TO AIR COMPRESSOR +
OFF AC POWEFI. TO THE
THERMOCOUPLE RANGI! OF SIXTEEN tlEAT ZONE CIRCUITS. 1N9'4 ,,12~ t ,t 4
07
!"EATED
AIRCOMPRESSOR ON/OFf SWITCH
CARRIER fILTER LED LlGHTSWIEN
R
lOOK
FROM AC NfUTRA.L BUS BLOCK (UNSWITCHED)
tt .2V <,
TtlEREARE EIGHT ''U1'I TOVERIFY THE
TEMP. A CTUAL FROM
FROM AC HOT BUS BLOCK (UNSWlTCHEDl
_ /-" I:
1N4004
-~ v,
R'
U3
nME CONSTANT, CARRIER FILTER
so
~ 012
SOR1
Q6001tJ
InOV-MOC304GI
12
A AVEMINUTE
,
r.: :: , • 2 , , • ...,
TOCARRIER FILTER·
-r=
1 WATT
U2
MOC3IJ30
R1 & CI PRODUCE
10K
TO CARRIER FII..TER +
, 1'\ f..::.
100 OH M
.lCS ~./
R'
~
ACCIRCUfTS
,.....
IMOMENTARY I
UNSWlTCHED
AJR COMPRESSOR
CARRIER FILTER
.
ACHor
CAkRtER FlL fER AND
•
r=
c::.
,
/
',-f-;
SIG.1N
DISPLAY TOGGLE SW ITCH
c
I
Pa\l.2 Q'3
IFlieneme: 31Odllpl.y<2. tcw
310DISPLAY·C SCHEMATIC Olte: 12/20/97 I By : R. Fenlke
367 (of 550 ) 2006(-2016)
368
-
.......J ae
10VAC INPUT FROM TRANSFORMER
ae
• .J ~
FID IGN/TOR ASSfMBLY ONVPRIGHTM!!TAL BRACKET ON THe LEFT SIDt! OF TH/! CHASSIS CJRCULATIONFAN
"" 10000 uF :: CAPACITOR
+~
+
25 AMP BRIDGE RECTIFIER
FlOIGNITOR ADJUS'f1fEH T POT P1JS TYPICALLY
/
- f r-.
0
100OHM 1 WATT
o
tAAX \IU1.TAGE. (-1000,
AD IGNITOROR NPO VOLTS PUSHBUTTON CIRCUITS ONDISPLAYBOARD
1K FoRFIDIGNlTOR 500 OHM FORNPO
4-
"VOC \ J INPUT
....-.. l]\ R
PHONE JACK FROM FlOlQNITOR ASSEMBLY
HARQ.WIRED TO BRlOOE
,.
r.'-J
B
......... SETPOINT VOLTAGE
IO ~ I TO lUN F O
I CHMAT
Il.OOMTEMP,
PLUGSINTO PUSHTERMINALS NEXT TO DETECTORASSEMBLY
-
1\ B
DEo\O
.,
I
-
'00
OHM.
/.
R
v
/
.,
JI
OUT~
-,
\
SET TO -4t)O.
WHEN MOMENTARY SWITCH IS Fl.IPPED UP, IGNITOR/SAT
LM338 BOTTOM VIOW
AOJ
FlO IGNITOR NORMALLY ClOSED MOMENTARY ON SWITCH (EU MINATE FORNPO)
TOTAL SE'TPOIHT PUSHBunoN
SIGNAL. TODISPLAY BUFFER AMP see PAGE 2
I
---
ACTUAL PUSHBUTTON
~
YEUOW LEO INSTALLED BACKWARDS FORNEGATIVE FlOIGNITOR CR NPC VOLTAGE
~
FlO IGNITOR OR NPOVOLTS CIRCUIT .
AC HOT AC NEUTRAL SWITCHED SWITCHED
SOLENOID CIRCUIT FOR AcnVAT/ON
\
OF 'SPUT VENr 100 OHM 1 WATT +12V
R13 SOLENOID INPUT
R1S
/;
10K
\! 2N3903
FROM
AI D
BOARC
MOC30:sG
l22OV.MOC304C)
~
,• , •• ~ 1-1 a
U.
100 OHM 1 WATT
Rt4 SCR' 06004/
Lrt.!. il TO SOLENOID SEEAC
"
BLOCK SCHEM.
I
P.ge:ll
on
IFlIenllm. : 310dl .pl.~~Uc",
310 D1SPLAY·C SCHEMATIC Dale: 12120191
I
By: R. Fens ke
i 368 (of 550 ) 2006(-2016)
369
.,
R1IS!! CHART'
.
.,2V
EL ECTRONIC P/fl!SSVRl! C
.
Rl (SEE CHART)
.,2V
.,
20K
20K
LOCAl.SETl'OlNT PUSHBUTTON
"
\
.»:
Jl
Jl
TOTAL SETPOINT PUSHBUTION
R
I
y
SIGNAL .. rODlSPLAY BUFFER AMP SEE PAGE 2
PHONE JACK TO EPCBOARO J2
"
0
.~
~
PHONE JACK TO AMP BOARD J1
,,2V
.,
t,
20K
.l
.,'"
PHONE JACK
.....-: ACTUAL
\"
PUSHBUTTON
• .....
~
LED(SEECHART)
-
fR()IAllP I ~AAO
--
. .,.
... (if
_
~-
r7
220K
AIR 1
'M
GREEN
FIDIGNITOR 100 PID CURREIfT 40.2K FPDVOLTS 20K ECDCURRENT 4.02K DElCOREACT. BOAK FlOBlOCK DacDBlOCK PlDBLOCK ECOBLOCK TCDBLOCK
...'K 40.2K
"K
44.2K
120K
YELLOW
'ELLOW
YelLOW YelLOW YELLOW
ORANGE ORANGE ORANGE ORANGE ORANGE:
h ZONE PUSHBUTTON ClRCVfr. Al.SO SEB HEA T SOARD SCHalA TJCS.
./ l.OCAL. SETPOINT PUSHBUTTON ./
\ R
,
SIG~Lt
TODISPLAY BUFFERAMP SEE PAGE 2
TOTAL SETrolNT pUSHBunON
.,...
~
•
T••
tl
SIGNAl. + TO DISPLAY BUFFER AMP SEEPAOE2
.-/
0
• ,c", '"(.. .." T~,.. ....
\
PHONE JACK TO HEAT BOARD
,
POWI';. SU""lv netlO..
~ --
H~ T~D
J1
TOTAL. SETPOINT PU5HBUnON
0
=.-
v"
LOCALS... .NT
J1
TO Hrvo;: BOARD
ACTUAl PUSHBUTION
SIGNAL.. TODISPLAY BUFFER AMP SEEPAOE2
o
SPOT OHIOFF PlISHBUnON SWITCH . /"
'
I
HYDROGEN 1
P1
/ -
.......
TOTAL SETf'OlNT PUSHBUTIOH
I&Q
GREEN
20K
.....-:
R
\
./
R1 (SEE CHART)
57 ORS8
PI. OR,PO
0
lOCAL SElPOINT PUSHaUTTOH
R1 VALUE
LEO(SEECHART)
pt D AND F~ PUSHBUTTON CIRCUITS. AL SO SEE HI VOLT BOARD SCHEMATICS. ,~
.....-:
2
1\
LEO{SEE CHARn R1l SeE CHART)
CHART ~
./
•
'1
DELeD AND ECOPUSHBUTTON ClRCVITS, AL SO SEE AMP BOARD SCHEIlfAncS.
*..,. -.-
~.
••
"
L.ED (SEE CHARTI
Tl1( UU N ', OM
,
"01'
I W DOP£IIATE UlIMG' l2VON PIN , ,t.H O ~ OIJ N D ON PIM 11,
DISPLAY BOARD PUSHBUTTON CIRCUITS
I
PaOli 1 012
IFli llname: 110dll pla)'-b1.lcw
110DISPLAY-B SCHEMATIC Oat. : 12120197
I
By: R. Fenak.
369 (of 550 ) 2006(-2016)
370
FlO IGNITOR OR NPD VOLTS PUSHBUTTON ClRC lJlTS ON D/SPLA. Y BOARD
flO IGNITOR ASSEMBLY ON UPRIGHT METAL 8RA CKETON THE LEFT
10VAC INPUT FROM TRANSFORMER
--lac·
.J
J..
SfDE OF THECHASSIS
10000 uF ~+ CAPACITOR
~ac +
/
2!5 AMP BRJOOE RECTIFIER
r1
LM33B
BOTTOM VIEW
~ \
1 WAn
.t
-~
------
J 12.VDC
\
SIGNAL + TO DISPLAY BUFFER AMP
I
SEEPAGE2
ACTUAL PUSHBUTTON
HARD-WlRED
.........." INPUT
100
OHM
/";
+-(r -4100 OHM
/
CJRCULA noN FA N
TOBRIOOE
~.
rtt
t•
<, SETPOINT VOLTAGE
IONITOflINPO BEAO
1 0HlllAT ROO "'! TIIIIP,
PLUGS INTO PUSH TERMINAlS NEXT TO OETECTOR ASSEMBLY
50
--
1-/--,"
20.
BLOCK (UNS~TCHEDI
..,.
~
L.LoJ
AIR COMPRES.'OR ... ,.~ ON I OFF SWIT....,.
DISPLAY DRIVER CIRCUIT
FROM AC HOT BUS BLOCK (UNSWITC HEDJ FROM AC NEUTRAL. BUS
-
TO AIRCOMPRESSOR +
R19
------"
+n v
POT
lk
DISPLAY
3 ,1 .n
1M
~
R18
ZEllO
c;
TO AIR COMPRESSOR .
I
FID IGNITOR OR NPD VOLTS CIRCUIT
toM
r PI~2Df2 IFllename: 110dlspllly-b2.lcw!
Date: 12f20/97
I
8y ; R. Fenlklll
( 370 (of 550 ) 2006(-2016)
371
_
DISPLAY BOARD
-
+12V
0,
C2
I
;
-=- _.
PRE SSURE SENSOR
~II" :
cIRcum
+ 1.2V
[%1J frSZ\~ ' I
82.
03 P2
20. ~<
I
b
+1.:ZV
ZERO O FF SE;T
PRESSUR; SENSOR
\
.8
,
,.
1["1 : '- v·
62K
..
"
i~ fq:?L JVV'\o 100K
1.. '
•
,
,,,. .....
<><: 1
- . -..
IOU<:
FR~AC
~STRIDU T10N
""""
-"I
C4
0.1 uF:
r-:,~ U2
n
,t -
•
12
THE EPC BOARD
lM 324 "H" ....CEL""
+12 V
., AD ' I
PHON&:.lA CK TO R EOULATO R
0"
,.
,.~ R(I
1Nti4
\
.
~
o
I
J3 . 'IU ~
017
YEllOW WIRE OF PHOIllE CABLE TO DISPLAY BO. "ACTUAL" jPUSHBUnON
- _.• fL r-1!.:: d"'~;'':' -1J1f:lr--oIr;,:;---'.~,~"'" ... .. ~ -, -n.. Df.t
• ••
, ." .
"1 '- -~-
. --
•
t
~
r"I'I\oM
~.
·111
AN EJ< TERNAL INPUT (10mV/PSIIIS NECESSARYFOR COMP,JTER CONTROL OF THE EPC. THERE ARE TWO IDEN TI CAL CIRCUITS
ON THIS BOARD. /"
z
BlJICK \'jIRE t O CHA5SIS
l M324
0" 100.
"""''' 0"
/
,.
LED DRI VER CIRCIJj r: PROVIDES IIlSUA L
DISPLAY BOARD
J2
D' vr 1N914
/
"'£RtfICATION OF EPC R/NC1l 0 NS
'f
BLACK WI RE OF PHONE CAB LE
TO OISPlM BO. '"l EO"
on"
~ ,
ell"'"
PROVIDES ELECIRONIC PRESSURE CONTROL OF GASES WITHIN THE GAS CHROMATOGRAPH
1M
J'$ ,.
v
:~ I -c
~ '13 • • 14
1001<
,.
I
1 1'1:4
EP:CIRCUIT' 2
07
POWER SUP PLY SECTlOHS
"'0'
R'
8 I
V
,
R2 3.3K P1 201<
" 00II 00
I
100.
,.l.,1D Vun24
U3 •
PHONE J ACK TO SENSOR (ALL IMRESI
ITl ..... ..... ..... = .""-
/
• /', ---tt
7
"
CIRCUIT BOARD LAYOUT I EPC-G , ,I ",e , EP: CIRCUIT' 1 -- - - - -- -- - - - l: ~jl!!
CJRCUIT
R13
8
o
o
f7"VCM 324 - --~,
SUMMING CIRCUIT: ADOS L OCAL SErPa/N T AND EXT EIm Al lNPlfT TO GE THER PRIOR 10 I THE COMP ARATOR
..
\l...!:;
u'l: >----'
- 1.2V
C M ~' e ~ PROOR. BOIdl~ " I
M>
-A
5
AD JUS T
"
CfTER MINfS ACTUAL / ' PRE SSURE \
3
__ ,
I~
0"
~ 10K
I' 14 U31 ') • ---t /' I ; I 13"- LM324 •I
LOCAL SETPOINT: IPUSHBunO NI
wou
100K
,n n "-.
D"".".....IIT" WI""
fVV"w
Mil ' II M"
R111
II"
. ~
LTlOH
. "zvou T ~ uT
"
U•
.. .. ON
." ., :tV OUTPU t
~
rPII g1l10f l
EPC-G SCHEMATIC Ollte : 1 2 12C /~7
'Bv: R. ffnskll
R...... Dil le:,
371 (of 550 ) 2006(-2016)
372
TH E OVE N BOARD PROVIDES CON TROL OF
CHASS IS COOLING
OVEN HEATING AND COOLING AND CONTROLS THE INTERNAL TEMERATURE OF THE G.C. CHASSIS. THIS PAGE DEPICTS THE POWER SUPPLY CIRCUIT, JITTER CIRC UIT AND THE CHASSIS COOL ING CIRCUIT. see PAGE TWO FOR OVEN HEATIN G AND COOL ING CIRCUITS.
FAN CIRCUIT
QVEN-F CIRCUIT BOARD LAYOUT O". N·... " c:e
I
JHURlN PUT
~ ii
IlOn o ll Of CHASSIS FAN CIRCUIT,
/
VOLTA Ge OfV/DEFt
C OM,I'AR FS
+12V
5.1M
28 VOLTS tIC
18 VOLTS AC
FROlll POWER $ UPPl V SECTION
FROlll POWER SUPPLY SECTION
TEJifPER AruR.
TEMPER A W RE
Wlt n E WIRE
REO WII'tE
U.
MOC3030 06
R28
U4 +
Rl
.-1/
3.3K
100 OHM 1 WATT
10
THERMOCOUPLE
r--
f-I_
L-.:r-~
4 !:I
7
.....
_-
~
I......
2 3
6 5
1 WATT
~ ~
BR2
R21
1..I
4 r-'1
SeRl 08004
C7
fi
RED
ac + ~ L ;~ 1_ ac • h r rw
10 2411 CfiASS IS
fAN
L.=.
BRIDGE
10 uF
blAC K
RECTIFIER
~
Tn ,pCRA TURE
ACTUAl. OF- CHASSIS
R25
1M
OPTIONAL SOLENOID CIRCUIT - - - - ,
•..., ~ ••"
.~
"""
.., -,
.. . . . . - -,
__~
u..
,
......
,
._§. .;
~
9. . . M=___ L--.I
WIIIt_
_
II""""'l
...._ ." a.(al!Jll
. rl ... ... "
.
~=
..... 1" · 1
a' """O
~:::: -
II
r
~.. .
. . ..
12
..l C6
U4
O.1UF~
I 13
,
,-
;~ ~ I'IO~~':"') ',~~'~
'~':,'~
_
:
~ , .... , s t- .-.
CIRCWT:
DErERMl liU
AD597
...._ _•
CO "
~
I
,
AMPUf.IER
r--
u.
USESTHISCtRCUlT ""
1-- -
1-
9
• ' - - '12.
VACUUMPUMP OPTION
~
1
SIiIJ"-SENSING
2
Ii
1N914
(220V-MOC3041j
ruCRMO COIJPtf
3
1
: :;,2 I ~
100 OHM
LM324
AMPLlFIER[:f, 1 10
s : s:l
T
-,
l OOK
8
~
I
..... I
CIRCUIT: S~TC/jES Ae TO HEATEDZONE TO ACHlEV!' DESIRED
/
....---------------+-----'-f~_'
CIRCUITS
THtll'ERATURE (PIN I ) TO THE SC""INT ,_TO)
1
~ ..
r- ~ I
ec SWITCHING
ne ",crtllt!.
OCTERMINC:S FAN QNIOFF s e rPO ' loll 10 COOL rl' .I4P1'"RATURE IN CHASS IS
COO' ," .
,
CIRCUIT,
R36
'
IS " I COMPARATOR
l MIS PAGEj
AfII)
I
1Ii ~ t
SHOWM Ot
~;I~G
-I
-
!lQ
IFRQM U1 PUU
I
~
L - - _,
.lin EAC1ACII T
Fb
a0
I
".,.-
OO,.... ,Q
.'}-' . LM324 THE lM32,r . lN THS
11.,,;:;;,,1
POWER SUPPLYSECTlON
e
.... I eRiJl c e +
r "'J
JITTER CIRCUIT M
• •
-~~-
~c -
+II.
I co ;r':. ..
. , I •., ... "'II
"r-:-:!" ... I Yrr';,' ~ ..:.:- :.:.. .," I
T
::.-!... -r-
~ C" T tl ..
""""" . . .....
V C1 COI "
-IH
/'Am'''-_ ,
/IN
~~ , , _. ....... JrAkJI'I'
.. .... ny .r-t
....
1M
I
'~ ' ~ .... .
'"
UJ •
_
_
.~
"1't5: I'RE~ E NTc,>tllllS ~ NDOlIiEII:
AND ·1ZV ~"'" ' 1
POWER ISOll
w
'a ~~~~It·, ILOBE~D~::m""
• ....m
l,Mm ..
'M
I
ClIl,CUIT I O.-\r:tOS WIl LE Tl£ G.C
0 VE N~ F
/
SE ' ".",..,- """"...,
I
CAl/l al: 4CfIOT .l.HD ,t,CC(l"' ~ .. ME llo\V.RDOUS VOt.T-'GI: S ~ t.I (]
U:~Il::2C:~~4
PIg.1of2
File n am e; ove n-l pg1 .tcw
SCHEMATIC ale: 12/2«/97
Roy. Dalril: 311)9101
Pi"U.,
B : R en e B : R.
372 (of 550 ) 2006(-2016)
373
... ._
l U'PERA T U R E P ROO R ~ . _
" TOTA L $ETPOINT" TRIMM ER POT
R33 10 K .......
__. _
.,
R'
10K
10K
~VV_
9P A DE lUG
'IF.Dl'MlIT! WIRE FROM T'l1E AID 8 0A RD
~
+12V
P1
if
20K
'M
~
[lI SPLAY BO ARD
SETpo rNT CIRCUi T, USER ADJUSTS ro
.,
.19
10 K ~ 12
."
GRUII AMI)
REOI'i1R!! Of P ~ Nf.
An DS All ,NPUTS TOGEr'HER
12
,.
14
..L
'M 1M
C4
COMI'A RAT OR
~ ~:
12
THE.&CTlJAl
lM'"
I
RJ5
,.
r ITHERMOCOUPLe l
110... 004
INPUTr RO'll COLU"'N OVEN
R
-
T/ fER MOCOr,JPtE AM PU F rf:H CIRCUIT: D!! TERMW f: S ACTUA L TH I Pf:R A ruRE OF C()(WNOVEH ' 'f'j;l lOW WIlt !
y~ Ul
D't
,
CONTROlS THE /
""
J ITTER
INPUT
HlOK
C " ~ T ON :
Rl2
D.
Mov", rED AS O VE
ME HllZARDOUS """ YA'1U .\NO.o."'E ONTHISAND
1.1K
LI! TIlEOC. l M; IIlIS0N.
1N9 14
n VOLTS N:. S UPPLY SE CTION
2&VOLTS Il.C FROM POWER SUPPLY SECTION
WHITE WIRE
~ E DW I I\ £
f lilOM POW ~fII
CIRCUIT OI'ERATE USlIIG . 12'11 0 11
~I"
4
AhD ·t2 VD NPIN11.
R13
~
,.
R14
10"1 04
';
{0.200VdclJ--..-J
V\
I
Be
_
100 OHM 1 WATT
,
.,,"'.''-'I . _n
D~
"'--------'P'l lI D
~h · I
I
Rl1
~
1M I WITCI<£O AC 1I0 T l'lI'UT l DLUE)
I.1
.......... _LACK
SWITCI
AO'
INPUT IB ROWNI
100 OHM 1 WATT
1
. 16
"
SCR1 Q 800.
, a
"'. no.,..
+ 14:~ I • ,.,
----"
~"
..
-
....... ~ ..... (.)
~
I M ~ O'l'/foI I
.....,
GREY BLOM:R 30 SECOND O ELAY
1N91.
" ..." • • 0 ....._
C5 10uF
I3R1
Be l HE L.. n~-.1Il nes
'00'
U,
",0
I,*,Ul 18 L.Ut.'l
'12
UTI_l l Y _TlDOII
I
~c c
:CUlT 80~"'DS
100 OHM 1 WATT
_IQtf ~
.o.C IOOl
t220V-MOC3041 )
c-;r
e
"
MOC30JO 100 OHM (220V-MO C3041) 1 WATT
ACHOTAND
+1Z V
THE G HAY B LO INER
.21 t UV
0'
.....
MlJFFIN FAN
HEATER C O IL $ W1 fCIil'D
U' "'MOC3010
Dl
I
'----=::.
COOL 2erRell",
,
10.7 Vdc) 1)4 (0.2 Vac) t R20 l 100K LMJ24
1N4004
U' ADS97
.~,
I1'LlIl l
I~~ .
LM1 24
LMJ24
"" AC OU TPUT TO COLUMN OVEN
.o.c 100'
,"0
10
~
STATUS
I 1 WATT
l MJ 24
"J-e l UAl" IPUBHBUTTONI
R9
.....:"'"'t...
e
411-
t Wl l ~I I'~
1 WATT
100 O HM
t
"LED"
\
r-
TEW~R AnJRE ("'N~J
Pl ION[ CAIIU . TO DISPLAY ftD
O ND. I
N4004
AC SWlrCWNG CIRCUIT , S WITCHES A C TO OVEN HE A TER TO A CI/Il;Vf QESIRED
TOAPCRATURE
'J2
TEMPER A TURE (PI H II TO THE
SETPOINT
OIsP!."" DO.
It
I
PHONE CABLE TO DISPLAY BO.
100 OHM
•
CIRCUI T: COAIPARES
C,'llL EFftOM
LOC ALSETPOINT; lPV$1l8UTTONI
REOM REOF
I
- BLACKWIRE OF
P~ONE CABLE
10 DlSflLAT BD
t12V R18
m~
~
Jl
~324IPHO~ACK\ " TOTAL SETPOI r4T" I
lM324 SUIoIIofIPlI) CJRCUlT:
T[ lolP£ RA JlJRE
PR OVlOf S VIS UAL ... VERj FICA HON 01' ~ OVEN HEA TER FUN CTtONS
10K
z
""" "" "
." u :o DR IVER CIRCl/I'T, '"
~. ~
10'
SET OVEN
40.2K
J'
D'
U'
R3 5.1M
. t2 V
1I0AII.0
R.
R30
.13
fIISPLAY
OVEN HEATING AND COOLING CIRCUIT
.1?;11
u
1L.=: AC OUTPUT TO
'COO' ''''
GRAVBLOWf R (OV E N a LQW[ RI
1.... Uf F.N FIlN
I
IP. glt l of l
File namo: o..... n.{ p gZ ,tCVf
O"IO i 121 __ rev, DlIte:
By : R. By : R.
373 (of 550 ) 2006(-2016)
374
OVEN-' CIRCUIT BOARD LAYOUT
CHASSIS COOLING
T HE DUAL OVEN BOARD #2 PROVIDES CONTROL OF QVEN HEATING ANDCOOLlNG .THIS PAGE DEPI CTS THE POWER SUPPLY CIRCUIT AND J ITTER CIRCUIT.
·~..
FAN CIRCUIT
OV II...
(NOT USED) __
l': ~ :
HEA TING AND COOLING CIRC UITS.
OPTIONAl SOLE' OIOCIRCUIT
;,T
,I,
; :
• ;
V
~
r;.,
b
-~...
~I
_ ......
rJ,
l"
I
I
I '"
I
COOLING
:
j
CIRCUITS
I
' :..c t- -
,
ANO
,
=
" '''''''
!O'...
.~
:I~~ o
.... ,...." -'r 7 :: :: , "0"'"
.'
':01
,~ ~
~Ol
,=" .w """""- I" ;r"1h ~
O." n "
ARI HWROOU S vot.T AGESIJ+O ARE PRESENT 011 THIS A~ D OTH ER
/\NO .12V ON"'M11
POMOIl.IS ON.
JITTER CC"IR~ CU~IT~
POWER SUPPLY SECTION
r-
... ...,
I
CAU1l0lt ACHOT A14D ...cC
T " II LJUl" ~ Tl1IS CIfl.ClJITOPERA TE
U SING ' l 'N ON PIH ~
- - .... .
_ _ """'i•.• IUIII • ,''''''" _
l
I e : "" I - I Ji:
III ~~
. . . ,--,
'---;;;===;-- - - -'-I "_ ..,0.."..",.._ _
t
OVEN HEATING
' .''''"' ,,"
.
, "" \J It"_OOOC_'I ..oc. .. ,.."". '''' O~ '' . ..." ......."
I
DUALOVEN CONFIGURATIONREQUIRES THEUSE OF ASTANDARD OVEN PCB FOR OVEN 11AND ASECOND OVEN PCB \\ITHOUTTHE CHASSIS COOLING FAN CIRCUITFOROVEN #1. IFNECESSARY, ASTANDARD OVEN BOARD MAYBE USED FOR OVEN 11,PROVIDED THATTHE CHASSIS COOLING CIRCUITISLEFT UN·USED. OVEN.fIl lS THE SCHEMATIC DIAGRAM FOR THE OVEN BOARD 'MTHOUT THE CHASSIS COOLING CIRCUIT; AS USED FOR THESECOND OVEN IN ADUAL OVEN CONFIGURATION.
VACUUM PUMPOPTION USESTHIS CIRCUIT "-
•"........."" '_ ,,",,00'" ,..... ......-_.
I
~ e
see PAGE TWOFOR OVEN
1- -
L___ ] i -
.. 1. ,101 - T'
,~~J.
;:;r
1. ...
TI."
" ,.
...
••,.
= ·'1'
1
.-
9p ,""
, I ..
O.
--:;;;;;:.:;;;;;:-=:::::;;;' ·...'IF" ·OfICI.01· ."V"] IOU /
NV
.=~...
~ " A."''''
U1 :r
••
u,
I .. """
'"
CI ~CU IT IIOAI«:lS WHILETHe G,C.
1M
_~
I "'.."0=,:::,,,,=' /
1~,,1 ...-~i;:!;.,,·, I-P'-"-'o1-2-l I
Fllll111.me' I/"al ovon.' ,:i--;;"1,tew
DUAL QVEN-F #2 SCHEMATIC
bIWI
2/01
B . R, B;
oiler
374 (of 550 ) 2006(-2016)
375
..._
TEU PIl RAT UR ~PROGIlIAM ".
R33 10K
~
"40£ LUG
" TO TAl. SE TPOINT"
!l........-....AA A _
v v......---,
0'
.,
10K
10K
REo.WotlTE WIRE FRO" THE N0 80AIilD
DISPLA Y BO/l.RD
+12V
RI
<'0.2K
I I
n~ IMMER
~
+12V
if' 20K
P1
.30
13
J lnER INPUT
5.1M
10K
U,
10K
~LM324
lEi/PERA lVRE
SUMMI.YOCIRc um /l OO! AU. INPUTS TOOETII ER
,-
I'
.24 ,
CIlEEIOAII D ~eDWIRES
r
OF PHONE CABLE FROM
LOCAL SETPQlNT:
COMPARATOR CIRCUIT, COM PA RES THE ACTUAL TEMPERATUR E (PIN eJ TO THE SE TPOINT Tl':MPI"R ATlIRE
DISPLAYB D,
IPUSHIIUTTONI
(f>lN5J
0 ..
08J,IN4004
09 1 1N4004
"'ove~""I I I"""X INPUT FROtli COLU" "
~
0 y
~
,
a 1 0 .7 V~c)
.,,,,
.21
U4
(0.2 V,c)
+
R20 '
3 100K
JITTER INPUT
R'
""24
RU
. 2Z
100K
9 .1K
Ace A~ H.uAAOOUS VOLTM1U oUlDAlIll! P RE S~ TON l otrs AND
ON, IICftCULT9OARO$ _ \.! TH!QC PO'fI!II 15 ON.
, I
I +12V
AD591
(PUSHBUTTON)
U3
013
21VOLTSAC FROIII powm SUPPLY SECTION _
TE WlRE
lot l9
CIR(tJ1T 0i"ERAT!. USlN-:;. I:NOH PIN' MO·I2VONPIN 11.
H ~AlE R C O I L
...'~
,~~
0 11
-•
o.
..-
•
_ ,
"GATE"
•
·
1'""°,"".'(
=
j
0 12
:)-2- lO"T ,
LM324
1M
V\
a ~E Y BLOWl'R
,O Sf: CONO Df'LAY
SWITCHED AC HOl INPUT
SWITCIt EO
{BLUEI
InHOWNI
.CO
INPUT
LM324
R"
2K
_ ... . . _ ,.. _.If
21 ~OLTS AC FROMPOWER
SIJ Ppl Y SECTlON RED WIRE
t< "11 .1-"~
.,:-1
RED
.m
_ . '•• 010
OOl 0
"" IIDI . . "'. C111C. U.IlO• • OJI,
"" 'J<. ~
TH E UU2~ ' . 1H
'"
AC OUTPUT TO COLUMN O\' ~ N
I IBI.U ~I
MO C3030 (220V·MOC3041)
C'.L
rr
UUFFIN FAN -, MOUNTED ABO VE THE GRA Y 8L OWER
100 OHM 1 WATT
STATUS
.Wl , GllfO . w ITOMfll .~ o ~o I+
ua
,
•
COOl-I ClRC tn T, CONTROLS THE '/
-
1N914 •
"WUT I"CU' I
\
~
t OO K
~ ~,
~~
TO DISPLAY S O, " ACTUAL"
U2 ~ 8
Jf/
1
C2
MOC3030 100 OHM (2 20V.MOC3041J 1 WATT
Ci\UTIQtI 1\010T "'NO
_
O"'~
Ul
05 1N9t4 U7
r
...J§t
SWlrcllE O
100 OHM tWATT
l M324
' YELLOW WlRE OF PHONECABLE
10
~.~
i==
.RD
I
-..
CIRCUIT , SWlTeIlES AC TO OVl" H HEA TER TO A CHIE VE' DESIR~O TEMPER A TURE
I
+12V
~
HU T
-@
Joe SWITCHING
· TOT4l. SETPCtn"
J1
THERMDCotIf'LE A MPU"ER CIRCU'" D £TCRMINr:S ACfUAl TEMPEc RU U" I' OF COI..UMN OVr!N
~
PHONE c...el.£ TO OISPU. YBO.
PHONE J ACK 1
J1
2OK~~+_
RED WIREOF
*
c;1iLM3204
OVEN
{EOORl vtRClRCUlT, 1 1( PROVIDES VISUAL '" I I BLACKWlR! OF VERI f'I CATf O/li OF ~ PHONE CABU OYEN HEA l f.R TO DISPL AY BO. FUN CTIONS "LED"
Jl
2
!I 0lllt D
J'
017
10K
01
U2
019
SE. TPQWT CI'ICUIT, lISER AOJtJSTS TO S ET DVl:N
OISPLAY
OVEN HEATING AND COOL ING CIRCUIT
.a
1M
14
03
POT
·U V
100 OHM tWATT
t OO O HM 1 WATT .
~ SCR1 Q6 004
..;.
Ae OIJTPUT TO
·CooL' ·
GRAY OLOWElt t1LOWHl)
(OV ~ N
DUAL OVEN-F #2 SCHEMATIC 'li te: U I20197 '8 Ie :- 3109101
Bv: R. f en si..
: R:'PI.lt e,
375 (of 550 ) 2006(-2016)
376
) ~JITTER"
,.
R15
~
R14 ~1 M
P
/
•
u,
•
0.02 uF
CIRCUIT: OP T/MIZES TEMPERA TURE STABILITY
. 6V
NV /
14
~'.
I
R'
u,
""
J1
2OK<:<
I.
\'
,r
HEATZO)!E LOCAL SETPOINT: (LOCALAND TOTAL SETPOIN T PUSH8unONSi
,
SErpO/NT CIRCUI T: USER ADJUSTS TO SE T DESfRED TEMPERATURE OF HEATED ZONE ""R7 ,
SETPOfNT TEMPERATURE
{PIN10j
U1·5 ekl. 3 U1.5 c kl. 2.
I
RED
~ l ~
RIl ~-
..
...ooo_ .
.~~""''''''''''''' MMI
............. 'I~ :::: rJ, .v.. ,~
,-~
00""..
~
•
.,U.,"-.:J.,
SWITCHED
(BLU !!:1
ACC INPUT (BR. OWN)
'If,1!......, ~ 200 ohm
~8
R3
01
"
,
1M
U2 ..
•
UIO
OPTIONAL
1N4004-
S CR1 Q6 004
_1
~ ,
R33 :::..~
EN....BLI! Ir"~"~ 10K IHEATZON I! II Ol'lLY)
NO
2
"
LM32'
YEllOW WI RE OF PllONE CAB LE TO DISPLAY eo. ~A C T U A LN
""
-
......... .In
THELMU4'11N nll' CI" CUlTOl'WT'!
USlNG.UVDNPlN. AN'O·1 tv ON "'" ' 1.
"
Ii'
lK J1
(PUSHBUTTONI
'"
L
-
r::1:
._.
LM3 2. 4
)l'~~+-\
POWER SUP PLY SECTION
it.h'
0"
~
100 OHM 'WATT
1N'1.
HEATED ZONE
oc,~~
..10'
'00 OHM 1 WATT
. .,
1D
THERMOCOUPLE
THERMOCOUPLE AMP L1 FlE R 2 .. 15 15 lHA114
Ul
YElLOW GROUND
SWITCHED ACHOT INPUT
ACHIEVE DESIRED
AMPLIFIER CIRCUIT: DETERMINES ACTUAL TEM PERATURE OF
/
THERMOCOUPLE INPUT FROM HEATED ZON E
HEATED ZONE TO
LM324
CrRCU/T: -, COMPARES -, THE ACTUAL TEMPERATURE (PIN 9) TO THE
"'VJ;:--- V
~
CIRCUIT: SWITC HES AC TO
7
10K
10K COMPA RA TOR
r
Ulll
AC SWITCHING
R10
1
TEMPERATURE
-;;::;::::-::::::,.,t2. ", '1M CAB LE FROM DISPLAY BD.
FOR HEAT CIRCUITS #2 AND #3.
R.
1M
GREI:NAND RED WIRES OF PHO)!!:
CIRCUIT #1. SEE THE NEXT PAGE RI1
I
10K
a _
TEMPERATURE CONTROL CIRC UITS. THIS PAGE DEPICTS THE SCHEMATIC OF HEAT
TOG ETHER PRIOR TO THE COMPARATOR CIRC UIT
R'
1.
.UV
~
ADDS THE JITTER
AND THE SETPOINT
LMJ2:4
Rn
THE HEAT BOARD PROVIDES TEMPERATURE CONTROL OF HEATED ZONES IN THE G.C. (Ie Te O BLOCK: HEATED INJ ECTOR; ETC .). EAC H HEAT BOARD CONTAINS UP TO THREE
SUMMfNG CIR CUIT:
-6V
43 Hz
DISPLAYBOA.RD
_
HEAT CIRCUIT #1
C_UTION: ~OT AND ACe Ntl1'lAlAADOUS VOLT..DU IJIDAAI! P1lEUNT(lI(TH:S AND O'nlEll; CIRCUITI OMDS 'MIl L! TIl! G.C. 'OWIlI. lSON,
/
BLACK WIRE OF PHOH E CABLE TO DISPLAY 00 '1 1
LED DRfVER CfRCUIT: PROVIDES VISUAL VERIFICATION O~ HEATER FUNCTIONS
I
_
" L.EO
N
I
I
••
'
I
I
Page 1 or 2 fll. n.m.: hlt-g pg1.tcw
376 (of 550 ) 2006(-2016)
377
, :
POWE R SUPPLY
:
____ _ _ _ _ _ _ _ L _
-- --- ---- -- ---
-- ,, L
_
- - ,
....!::
0(5"
~ g;.
I
,
u
L- r - - - - - - ttUT-G
,
PCIII~ 1R:Cln
, ~, ~
'---t'
, i
!
!l •
, ;
• I• ,
~ I• ..> •
.. _il; i ~
2~i ~ , 1'"""5:'" '. - 'I ..., ~-
, 1 I ~~
-"
i~
1
,""-,
!
i
, ,•
;;
I.~ ,"~
~:a~
::i 't ,, :~ ~ .. u => ~~
..
II' , .. lctil::
i1 "S
r"' ,'l 377 (of 550 ) 2006(-2016)
378
,.
R14 RU
fROM DI SPLAY BOARD -\o12V
~
U3 •
:' 02 "
9
11 3
Rn DESO RBTl ON SETPOINT : 200 DEG. C, TYP.
NV
"
/
R5 1M ROJ
1M ' BAKE': FROM AID BOAAO REtAY ·B', ACDS &0 OEQ. TO TRAP SETPOINTB
,,
1@
ZOK
\
1M
C,
RZ GREEN WIRE OF PHONE CAB LE
L OCAL. SETPO INT
5
Rl
LM324
COI.lPARA TOR CIRCUIT: CO",PARES THE ACTUAl.. TEMPERATURE (pIN .) TO THE
100 O HM 1 WATT
tC .
-,
'61POW'
LM'"
Tf lfPERA nJRE (PlN'O)
RlO
TH ERMOCOUPL E
R"
200K
R Y
Jl
l- f-J ..:: If
ONe
PI ZOK
_
1 2
10
It
_
3
8
_
45
1
~v.: 13 LMJ24 16
U,
1N91 4
DI!TfRMINES ACTVAI. TEM"ERA TURE OF TRAPS
+12V R1
1M C1
"
t
,{1
TO TOTAL SETPOINT ON DISPLAY BOARD (AOSORBTION SE TPOINT: 30 OEG, C, TYP.)
Ul
R2ti 1K
A D551 7
.2 ~ 1N914
~
C21
Jl
O.1!,1F
1.
"9
..--'
I2
LM".
1M
10
rEI 19
' 1 U+ '/
YELLOW WIRE O F PHONE CABLE TO DISPLAY BD , " ACTUA L" (PUSHBUTTON)
uF
~-
I ,,"''' D
.... "", (1o.. ""l
.Wll "'I D... ..·'..... lkUQ
••
POWER SUPf>LY SECTIO N
= -I:= t. - -. ~. COD!
,J;""""V
::.:,'t
_ I l l H UO_
l
(
-~
I . ...
_I
..... .
""'
J. n
~-
~:IO IV ,~-
~ r'"'
. . ~U .. ~ .II
T +-T"' ' ' ..;r T.,,,, 011 .1.
011
.
,"
'I T_ D' OUoI
TH& UUJ4.. IN tHIS ClRctJlT OP ~AA T£ USIt«ltl ZV ON I'UI' AN O·12V ONPIN \t ,
BOAR O' WH I~IT HI G.C, ~ II ON .
·'10
i
BLACK WIRE OF Pti ONE CABL.E TO DISPLAY BD , " LED" +O.12VDC
R~2
100 1<
I O~
R23
(220V-M OC3040)
::: ,, ,
V
II LM324 L....- ... 7 R24
HEATO
UZO . 6
100 O HM 1 WATT TRAP COO LING FAN CIRCUIT
I
100 OHM 1 WATT
Q
R25
5
SCR2 Q8004/
Pag. 1 ol 2
I Filenamo : p & t-d pg1 .tt w
TO ...12V
TRAP
~
-
ac +
e -J .....,
ff
\
211/ CT 2 ~V
~
CllUTIOI<' ACIIO I AIIO ACH'U 1IVLAAE HAZAADOOS \'O~ TAGES ANDARli.PRiSEH TOH THISANOO1HER CIRCUIT
"9
DISPLAY BOARD
1m ,
lK
..1 +5V AS TRA P
U' MOClOlO 1
'~D''''O ....' 1UI1ITIO
+12V
R2t
3
R.
• "v
_.
,.~~'" om= "
/
, ...-J
+'\.. 14
rHERtAOCOUPLE
A."""R~
_
TO J1
U2
•
WIRE OF PHONE CAB LE
ne 4 Ii
SC R1
0<.04/
A.C O UTPUT TO T RA P1 A ND SPAR GE FILTER HEATERS
LM J 24
+12V
R10
12
U2 +
!,IF
1M
\
16K
~ e.~ ["7
_. U3
LM 32:4
5
J:.
~
e
10K
-! r<
j::; • r-, r
10K
R10
1
, 5
R6
J1
RT
."
1
Rl1
SW ITCH ED AC NEUTRAL IN PUT (BR OW N)
100 OHr~ 1WATI
MOC3030 j22 0V-MOC3040)
I
~,
SWITCHED A.C HOT I NPUT (B LUE)
U4
SUMMING CIRCUIT: ADOS TIlE JITT ER .....,0 THe SETP OIH T TOGETHER PRIOH TO TilE COMPARA TOR CJRCUIT
10K 2
U,
RELAY' F' IT' l l INPUT , ftOM AlD BOAR O TOACTlVAU. HIGHrt OW 5ETPOINT
2N3903
\J.w
·OV
R'
100K
AC SWITCHING CIRCUIT: SIWTCI1ES AC TO TRAP HEAreR TO ACfflEVE DESIRED TEMPERATURE
TRAP #1 CIRCUIT OF PURGE & TRAP BOARD
' OV
LM 324
R" ~ \!y 16K
+12V
48.1K
.
U' . / '
L M324
43 Hz
STABil ITY
12
/
Rl
/
10
,M
P
\
• JI m R • CIRc um OPTIM' ZES TEMPERATURE
3N24 8 ..r
ac -
~
P & T-D SCHEMATIC ~
.
'
Rev. Delo : 12/ ' 210 2
•
( 378 (of 550 ) 2006(-2016)
379
0"
P
,.
/
,M
014
"JITTER " CIRCUIT, o n/MIl ES TfMPFRAruRE S TAOIl lTY
10
" .OZ,F
U'kC Ii
LM324
on
"~
U ' I _
DESORBTION SETP01NT: 200 DEG. C. TYP.
.,
~
.~
/ 48,1K
~
1m
\
•_
R'
GREEN WIRE Of PHONE CABLE
LOCAL SETPOINT
0. 0"
R32
-, . U3 . "
AIO nOARO
t
,
U'
uuF ,
OF PURGE 8. TRAP BOARD
TEMPERA TURf
U4 MOC3030 (220V·MOC3040)
I
-.~ U,
10K
5
0J1
ZOOK
WIRE OF PHONE CA BL E
R
CIRCUIT, COMPA RES 7HEACTUAl TH~"t;HA TUI>E (P/H " TO flj E " SSTPOINT TEMPERATURE fl'INt Ol
.rLMJ Z4
Y
Jl
P,
GN
I.~
l.t
_
rr--
1 :2 3 4 S
10 ll
/
~
~
LM 324
10
.,
100 OHM 1 WATT
U'
,
TO
01
.'\ .
0
"
U'
1M
10K
~
t
U1
R16 1K
A0 597
0.1u F
J1
J
+12V 100 OHM 1 WA TT
.l ~
U2
r,-V
1
SPARGE GAS CONTROL
' 28 "K
@ '\..!::
2N3U J
U,
-
a
R' l ,
..
~.ouI'
•
-l -
0' 0 SCR3
1m
II
BLACK WIRE O f PHONE CA BLE TO DISPLAY BD, MLED"
Rf LAY CIRCUITS FOR ACnVATJON RLV1 OF VA LVE 1 - - , .1
IC)
I
10~ 'J\~
2N)K 3
I~
fi'
OIlANGI!!
...
IlRO ~N
I!
To vlU.n~ 1 ""l\IATOOI
Ill...' .",.
""0_
100 OHM MOC30 30 (220V-M OC30.0j 1 WATT
,, ,0
,K
'LM' "
SWITCHED SWITCHED ACHOT AC NEUTRAL INPUT (BLUE) INPUT (BROWN)
027
.6
DISPLAY BOARD
Jl
YELLOW WIRE OF PHONE CABL E TO DISPLAY BD. MACTUAL" (PUSHBUTTON]
01
30 DEG, C. TYP.l
14
TEMPE~A ruRE O"
SE T POI~ r:
'SPARGE' : fROM AJD BOARD RELAY 'E' , A.CTIVATES SPA RGE GAS SOLENOIO
."
r;~324
1N914
TRAPS
CT TO TOTAL SE1POINT ON DISPLAY BOARD (AOSORBT ION
r+e 4 >I
SC R,
0 6 004
~~~::;~f:g~~,
B t - - +12V R1 7 B
020
~
tHERIlfOCOUPU!
AMPLIFIE'~
co1-
~
COMPARATOR
10K
THERMOCOUPLE
OED
1CO OHM 1WATI
AC OUTPUT 1 0 T RAP2
L M324 +12V
SWITCHED AC NEUTRAL INPUT (B ROWN)
0
LM324
01
, ,, •a 4
j:
10K
0 10
1
SWITCHED AC HOT INPUT (BLU Ej
A CHIE V~ D~slR£D
SUMMING CIRClJIT: ADOS THE JITTeR AHD THE S~POtNT TOGETHER PH'OR TO THE COMPARATOR C/R CVlT
10K
•
INPUTFROtll TOACTIVAT & K1GHI\.OW SETPOlNT
AC S Wi rcHINO Clfl CUlT, SWITCHES AC to TRAP m!At ER TO
TRAP #2 CIRCU IT
R11
REl..AY 'C' 1,",21
10K
"'c. 1M
0'
'M
100K
TRAP SEfPOINTS
.7
j.w
"V
LM)24
2N3903
J1
"K
/
14
'1 4K" ; FROMAID BOARD RELAY '8 '. ADOS10 OEG, TO
FReM DISPLAY BOARD +UV
NV
./
n
,.
.,V
43Hz
L. _
CO"1 0""'/ 1--1 '--
AC OUTPUT TO SPAROEOAS SOLENOID
_, ..,~
P & T-D I
PillIZof 2
FII IIJllme: p & H I pg2,te w
SCHEMATIC Dale: 12/20/9 7 ev, ate:
: R. Fe nll l ' M.
W~ tl!l
379 (of 550 ) 2006(-2016)
380
THE HIGH VOLTAGE SECTION CONTAINS THE CIRCUITS THA T SUPPL Y POWER TO THE PID
DISPLAY BO ARD (DETECTOR PARAMETERS) +12V 40.2K FOR PIO
.,
ZO.
FOR FPO 4.0211. FOR HID
20'
-
SETPOIHrCIHC/Jl f,
ON/OFF SWITCH
GREEN AND RED WIRES OF PHONE CABLE FROM DISPLAY BO,
LOCAL SETPOINT: (LOCAL AND TOTAL SETPOINT PUSHBUn ON S)
.,
pjD OR VOL TAGE 1'0 " FPD
-,
10
,. J,
U1
C~~i •
'r,.
1
.J
•
LM324
-,
•• "
., ,.
+ EMCO U SB HIGH VOl-TAGE POWER
S
• ~
SUP PLY
~
.10
:e,
.
z> °lil . ~
w
o
•-=-
., On ~
~>
fr:"! _ 0
•U
•o
R9
v
HID ADD: 4700pF
+12VDC . 1
(REG ULATE D)
+12 VOC . 1 FOR HID, PIO, FPO
.
-"U1 . " • 12
POWER SUPPLY SOURCE:
IJ:: , 2~
••
lM324
'O HM S WATT
/
.,
f EEDBACK TO CHFffREH TlA~
. IoIPUI'IER
:Li::
TRANSISTORS Qf & Ql PROVIDE THE REQUIRED INI'UTVOLrA GE TO THE Hi GH VOLTAGE POWER SUPPLY
2 N ~066 I ~
DN SDl.DER SIDE
RI1
,
3
-,
1K
.J , C'~O.01
10K FOR HID 1K FOR 1'10
U'
YELLOW
WIRE'
LM324
,F
O.OFO~D
~
so ·
- F'"O~~
-
,.
," ,. ..J,.
1500 VOC MAX.. OUTPUT
+
. 12
)( 1000 PI~~ E R E! H TlA ~ AMPUFtS": COMPARES tHI! ACtUAL CURRI!Nr DR VOLTAGE (PIN 13) TO THI! !~TI' OINT CURREH rOR VOLtA GE (PINIO)
Pf;~::DAC~~:~!~DS:~iD,
Hit."
0
t
(10 uf) PID·FPD
~Fl .U D
C2
LAM P, THE FPD PHOTD-MULTIPLIER TUBE AND THE HID ELECTRODE.
rtt .......
/
TO PIDLA MP OR PMT
22M FOR HIO 100K FOR PIO, FPC
FPD VIVID I!
~o~
-,
10M
•
_.Y;
FPD 7
J' I R1
U1 6
J1
JUMP .' FOR \ FPD ...,
100K
. MP
*
JUMP I FOR I PIO/HID \
RI7
DY l a o
.18 ·700 VDe
/
PIO, HID CHASSIS GROUND
'K
LM)2.4
OF PHONE CABLE TO DISPLAY BD. -ACTUAL-
OISPLAY BOARD
ff
BLACK WIRE OF PHONE CABLE TO DISPLAY BD. -LEO"
POW ER SU PPLY SECTION
"" ".
_rl . .~
0""• • •
M"
I I ""
f ROli AC OlSTRl8UTICIl
","'"
V
0.0''"" "i ~
.
T~,.,
_.
" , \lOCO!
0 . . .. 0
,m
I Cl ~, .l" T,;o"' '''' T•.,•• ~L >4 . Ie · I V-¥~· -u, . ~" ~ liT:'"' ~., ".. ;:r:.. .."' .,. ~'.o ~ ,..
-- •::t0_ ~ • rrt _...
••
.leu
. . ,.,
' 11\IOC "
._u _., ."....
lUI)AMPLIFIER FORPIDOR FPC1$: lM324 FOR HID: l F347
IIOTE: THERE CAMBEUP TO TWO DETECTORCIRCUITSPERBOARD. ,ANV CQMBINAnOMOFPI C, HID & FPC)
THEUU24 AIID THE
LFJ41 IN THIS CIRctllTOPERATE USING '1 2VON PIN" GNPON ~N &,ANO . 12VOH PIN lI
I
I P, ge 1 of 1 Flle n. mll: hIYOII-t .l cw
HIVOLT-C SCHEMATIC
..
. Ie: 1 / :
,
B : R. F.nske
380 (of 550 ) 2006(-2016)
381
POWER SUPPLY SECTION OF AMP BOARD VR'
POWER SUPPLY #2
"
" "
II YAC'l ' I.OA1'lN'HIIIO\IIl D
C"
.R'
21VAC FRDMAC OlSTRIBUTIOK GRO UND BOARDOR TRANSFORMER 28 VAC PINS8,7&8
POWER 5U PPl. y tl21S A +12 V AND -12 V SUPPL Y BIASED 24 VOl. T5 ABOVE GROUND POTENTIAL. BY VR3 OF THE B IAS POWER SUPPL Y. THIS $UPPI. Y /S USED BY THE FID, PID, DELCO AN D FPD DETE CTOR AMPLIFIERS.
+12 '11 C11
1000 UF ,$V
ac + ac
cn
C12 1000 uF
J5V
BRIDGE RECTIFIER BR80150
\2
R EG.
"7an
C14
10 uP
0.1 uF
OOV
.n: V
REO.
VIU
BIAS POWER SUP P LY VR'
m
DR' FRDMAC DISTRIBUTION BOARD DR TRANSFORMER PINS 1 &2
REO.
ac +
.,....
24VAC
470uF SOV
nc
THE BIA S POWER SUPPL Y MAINTAINS A 24 VOLT DC
24 VOLT
C14
BIA S
0.1 uF
POTENTIAL DETWEEN GROUND #1 AND GROUND #2.
V OLT A GE
BRIDGE RECTIFIER BR80 &D
VR.
POWER SUPPLY #1
Jau
'R'
28VAC FROMAC DISTRIBUTION GRO UND BOARD OR TRANSFORMER 21VAC PINS:S, 4 & &
"
CI7
- ra v C1B
1000 uF
ac +
"V
nc
"
REO.
GROUND
C19 1000 uF
"V
B RIDGE
RECTIFIER BReOSD
C21
C" 10 uF
1911
oov
0.1 uP
·12 V
~
rowe» SUPPL Y #1 IS THE PRIMARY POWER SOURCE FORAl.L FUNCnON5 OF THE AMP BOARD AND AL SO PROVIDES +12 VAND -12 V TO THE AID BOARD. ONl. Y THE TCD CIRCUIT REQUIRES AN ADDITIONAL AC VOLTAGE INPUT. SEEPAGE 2,
VR'
D
.-- .... '~O"""
loI'NlyllOOO _~
CHASSIS
28 \lAC fl
GROUND
GROUND
• • • .
AMPLifiER BOARD LAYOUT
llyn (f IU" " , lOy n . .ChO_ ..y ....
, u·,"n- : .11 5. . ... n C_
' CO
•••
S ECTION
••
' 0 .... . 0 ......
..
,_ O '~O
_
TCO
SECTION
OI'""
,,-
...OUI AC
'...,.."". . ..
DELCO SECl ION
DELCO
AMP
em
AMP
FlO AMP
FPO AMP Page 1 ot 1 Fllenen1e: Amp-e1 .1ew
AMP-E SCHEMATIC
D~ to: 1212019 7 I BY: R. Pen t k. ev. 0 "10:9127/02 I Ely: M. Will'
'I 381 (of 550 ) 2006(-2016)
382
\ 1I0 TE: MODa 3\G STUDENT Teo G,C., ~1I0 MODEl. 110 STANDALONE
TCD SECTION OF AMPLIFIER BOARD
DETECTORS DO NOTHAVEAA IJD 10 AII0. THUE Moons REQUIRE ZlIlO POllAND Anl' NUATORS TO
BRB05D
1BVAC INPUT FROM
TRANSFORMER PINS 15 &. 16
Ie l!
+. 700 uF, 35 II ac + I-' r; h; CA.P ACITOR ac BRIDGE RECTIFIER
''',00<,
+12V
f ROM DISP LAY
""'"
I""
+12V
PROtE CT " LOCAL
>OK
~ lOCAl,. I ETI'OlNT
10 ",V_ 1 P5I
,
,
a
en
-
\t
IK
,.
~'''R'~
PHONICAaLI FROt.llllSJ'LA'l" 80"'11.0. TC: O ' ROuC t "10 1Al.ISE1POINT' {COURIEIl PRESSURE "'CTU"'L . IlOMOIIPLAY BO"'RD. 10"'v _ I PSII
BOARD
ON AMP B D.
.-
7.15 OHM
10 OHM
O"IH
LOW QA'H
HIGH
BK
I~ B""
I~
GREEN
I ~ ~ !I-
G
R
=
LM338 REOULA TOR
BLUE
1\ NOT E: FOR MULT1G AS 2 ONLY REPLACE RESISTOR ATRJ' WITH A JUMPE:.R
tK
Ie
BLK
•-
WHT
SIGNAL OUT TO
AID BOARD
I-
TO
1mYELLOW WIREOF PHOHe CAIll-E TO DISPLAY BO. t CO ' Ro n e T "ACTUAL" {VOLTAG E TO OROUN OOH REO flLAMENT I
'0
O','l,A'l" 80"'11.0
J1
ZERO
HEAT BOAR D
lK
""
•
B OTTOM VIEW
OED
~ J1
\
I
2N390J
1 o.1 11F ~2
0"
TERMINAL
-
f-J \
~
R3G
R31
~ot "f
•
LOW
....
Off
SW ITCH
~ .--U'v
I .1-
HIOH TCDG AIN
IUPOINT"
SCREW
HEAT
II
RELAYl
reo
453K
fROM
~
8 0"'10
RI
CHASSIS MOUNTED TCD CELL
RELAY OPENS IF CARR IER PR ESSURE IS LE SS THAN SETPOI NT
QUEM w11l!
10ARO
H O,. D ~PLAT
ADJU ST T HE OfTECTl)It OI,lT PUTS TO f lllllt OfiSIREO LEVEL SEE THE "l.l!RO POTSAND ATTEI
BLAC K
"
BLACK WillE Of PHONECA8 Le TODISPLAY BD. "' CD ' ROTECT I.EO·
Pago 2 017
I
Fl lonil me: Am p-0 2.t cw
AMP-E SCHEMATIC .... , e nseue0 ev. a ;
Ii;
382 (of 550 ) 2006(-2016)
383
ECD CU RRENT SECTION OF AMP BOARD
ANODE ONC
Q~U: N
\'; ''1. 0 ' PHON!
fltOM DISPLAV
0<,""
+UV
DISPLAY
10 A1I.0.
01
."
...nv
"LOCAL
2
Dn ' OIIll "
20K
~
.~
ECOCUR.!IEIlT LOCALSUPOINl
R10
,.
0"
REO ANO
DISPLAY BOARll ECO
CU MfNT
.,.
-tctc,
5£TPOlN1"
V
' OOOM
·12V
2
r;-
U10
V•
opeo
UB)
-,
+12V
2K
OPSO
R21
If 11
·12V
,2 U'•7 ..J l~: :
.,2V
'oo K
0" rJ-C1O
~
""
-;-
Rtl
. 12V
10aK 'f'El LOW WUI,U TO
U~B
Rtl
ECC CE LL
2
t1 2V
-.......
C HAS SiS
MOUNTE D
+12V
~ ~F
loF356
CUf\RE ~T
• .02 K
\..
~~F
CAlM ' ROM
1U K
", e
.--
' .I K 1...
Ctl
0 115
l'"'
~O'"'
·12V LM331
"V
<~
' V-uln
R23 100K
WAVEFORM AT CAT HODE
~~
'~ONE CABLl!
T
0"
TODISPLAY DOA,I\O"l l tr,
80ARD
"
. NC
rBLACK Wl R.l OP
10
CATHODE
-12 V
J1
"ACTUAl,."
DISPLAY
r
·12V
0\
J1
'M
+1ZV 3
"
1Ntl4
.11
lK
LF356~ f--
. :,t?
• U7 •"\"'-1•12V
RIZ
,
R"
r;-
NOll: MODEL 110 IlUOENT TCo
D.C.' AND MODEL 110 ITAHDAJ.ON I
10K
0" \K
r
DUECTORS 00 NOT tlAVlIJt AID BOARD. ' fl~ U MODIiLI 'U QUlll:1
ZERO POTS ~ o ATT E N U"'TO Il~ TO
'M
LF356
SIGNA L
OUT TO AID BOA RD
c131 -
WHT
""'~
. 12V
'7
AMp·E SCHEMATIC
I PIgEl3017
AD~U $T T H!
OI!TEC TOIlOUTPUTII TO T11EIR DI51REDLliVSL.. U S TKI · ZEROPOTI ANDAnE.HUATORSPAGe INTHIS leCTION.
OLK
0.. 1M 0"
+12V
2
f-
I
Filename: Amp -e3.tc w
~
".
. ons ,
0: II
e:
••
383 (of 550 ) 2006(-2016)
384
DCLCD BRIDGE ASSEMBLY ON U PR IG HT METAL BRACKET ON THI: RlGHr SIDE OF THE CHASSIS CIRCVLATJONFAH (OUTPUTOF 25 AMP BRJDGe POWERS THE 12 VMINI·FAN ON FRONT OF G. C. RED UD)
DE LCO P OWER S ECTiO N O F AMP BOARD
THiS CiRCUITRY COIlTROLS THE TEMPERATU RE OF THE DELCO REACTOR. SEE PAGE5 FOR THE DELCO ELECTROM ETER SCHEMATiC. THE DELCO REACTOR is LOCATED 011 THE RIGHT SIDE OF THE COLUMII OVEIl.
-
t12V
RED,WHITE & YELLOW WIRES TO T-COUPLE AMP & ELECTROMETER
-;::
-,
. - ac . ~ ~ 10000uF . - ac + h., + CAPACITOR
10VAC INPUT FROM TRANSFORMER fROM DISPLAY BOARD
DELCOREACTOR HEATERWIRES PLUO INTO PUSH TERMINALS NEXT TO DETECTOR ASUMSLY
Jt
R40
20K
.J,. 1~~" ~ 80V
t LOCALSETPOINT: (LOCALAND TOTAL $ETPOIHT PUSHBUnONS I
GREENAND REDWIRES OFPHONE CABLE
rr
8
R"
.-
...
8
10K
~
R"
LM'..
8
1M
THERMOCOUPLE AMPLfFIER CIRCUIT: DETE.RMINES ACTUAL TEMPERA TURE OF DELCO REACTOR
.
100HM LM324
,.
R48
R..
10K
L 1 10....1 '
~ c"1- _ .. ,24 •i7 f-"'V ,I-' • I--'
,,, ""9
7
U, •
\ 't
YEL.lOW ANDWHITE THERMOCOUPLE IHPUTWIRES YEL.lOW FROM DELCO REACTOR. 1WHITE (THEREO WIRE IS THE SIGNAl OUTOP THE DELCO CELL, SEE PAGE Ii FOR DELCO ELECTROMETER CIRCUIT.)
(
V •
U,
SPADI!
GRAY/BLUE
10
1M
I
r
rEMITTER
'-...I
"-
' O.4K
2N30 ~~
BASEr
1OHN ATROOMTEMP.
I
BOTTOM VIEW COLL. C )
25 AMP BRIDGE RECTIFIER
SETPO/NTCIRCUIT: USER ADJUSTS TO SET DESIRED TEMPERATURE OF DELCO REACTOR
DELCO REACTOR
U' AD597 THERMO COUPLE AMPLIFIER
R" 1M
"
U3 •
13
" LM324
SI"ADE
rE iii GRAYNELLOW
Q~
2N3~
-,
)
R<7
lK
LED DRIVERCIRCUIT: PROVIDES VISUAL VERIFiCA TION OF DELCO REACTOR HEATING
-,
COMPARATOR CIRCUIT: COMPARES THE ACTUAL TEMPERATURE (PIN 6) TO THE SETPOINT TEM PERATURE (PINS)
J'
*
r;::;,
r:
L9 J' BLACK WIRE OF PHONE CABL E TO O1SPLAY BD. " LEON
YELLOWWIREOF PHONE CABLE TO DISPLAY BD. "ACTUAL" j PUSHBUn OH)
I
I
TO DISPLAY BOARD
A MP-E SCHEMATIC
PAge,"017
FlI~n ..m~: Amp~4. tcw
,
,
;1.: a v.
ft 0;
ona 0
••
( 384 (of 550 ) 2006(-2016)
385
r:.lj
C~ R3
TO PIIOV IDI A l OWG.llN 'OR Ttl ' MUOLOGGER AN ADOlTIOtW. 100 ...... 0 lualSTOR II CONNECTED III PAl\AU.El tACROSSI 113.
2000 pP 100M
HIGH ~ FILTERED 10 0M 1000 pF
---'?
.,
c,
FOR UTAAINPUT PROTECTION R' MAYee CHANGEO TOA 1UX RES ISTOR
c:r .~ R1
\ SIGNAL INPUT FROM COLLECTOR
BNe
07
GAIN SWITCH 100 pF 2000M
1
•
U,
HIGH
r-rBLK
'~ "
....z 6 r-v 121
..-- "'4
3 C1 0 1uP
•
R3
1M
C~R2~ r1_~t.O uF 100K c r: R1
06
~
10K
4e ilK C, . 1.1 uF
0'
G RO UN D ED)
c~r~t.0.1 uF
r=1
CI O ,1 ~ F
o.
1 .1 lHA117P (PINS 1,5,8 ALSO
a
SIGNAL INPUT FROM DELCD COLLECTOR (RED WIRE)
4
~~ : ,01 u F
+1~ 2
• 7 8
Ul '/'4
SCREW TERMINAL
1 0M
t'
O.l u'
~12)
C7 UII'
:I .1~~'~ r-vl2 l L F3 ~8
,
SIGNA:" OUT TO AlO BOARD
_,M
~~
;S.;-t ~
3 OP 80
,
'" 7
U, , )
.1'1~'~ r-v lZl
lK
1101£: 1I0J"~ n o STUDENT TCD a .c .• AHO WOOE\. 110 S TAN O A ~ OHl! OETECTOIlS DONOT HAVE" N.....O BO"RD. T~ESE MODELS REQUIRE URO PQTS "NO AnEN U"T ORS TO .l.DJun T~E DETECTOR OUTPUll TOTIiEIR DESIREDLEVEL.sn. n u ' U RO PQ,SANO ATTiNU ATO F\S · PAGE , N THIS SECT ION•
THIS CIRCUITRY AMPLIFIES THE SIGNAL FROM THE COLLECTOR PR IOR TO OIGlTIZATI ON BY THE AiD BOARD,
+~ C. O .l ~'
06
10K
FlO, NPD, HID, TID ELECTROMETER SECTION OF AMP BOARD
M EO
,
1M
-
WHT
~
~
DEL CO ELECTROMETER SECTI ON OF AMP BOA RD
MEO
LOW
GAlH
" OTI , 1I0 0 E ~ 310 $T UOI!N T TCD D.C.• ANO lolOCEL 110 STAND A.LO ~ f OIT ECTO,\ S 00 NOT Ii"V E AH NO BO" Ro . THeSE NODELS REQUlltf ZERO POTS AND "Tn:li UATORS TO " oJU$T THe DETECTOR OUTPUTS TO THEIR DESIRED LEVEL. SEe m e · ZIiRO ' CTS ANo,\n ENUA10RS' P AGE IN n us SECTI O ~ ,
THIS CIRCUITRY AMPLI FIES THE SIGNAL FROM THE DELCO COLLECTOR PRIOR TO DIG ITIZATION BY THE AiD BOARD.
SWITCH SI HIGH
r-rBLK +1 :Z~ C4 0.1uJ'
3 ,'<{.~ U' --;- ·4
·1 2V'1
IC '
INA11 7P (PINS 1,5,8 ALSO GROUNDED)
O.
;M
-
SIGHAL OUT
10 AJO SOARD
WHT
4tilK Ci l i'1 11F
OS , ~ 1M
I
~
I
-
P' II, I oI 7
Fl1onam, : Amp·ClS,lew
AMp ·E SCHEMATIC n • 12 I B 'R I lE't:~ : ~:Z7 10'l
385 (of 550 ) 2006(-2016)
386
C3 .3
2000 pF
MED
100M
.,
C,
PID ELECTROMETER SECTION OF AMP BOARD
NOT£: MOCI£L ~ \ Q n UDENT reo D,C.• "'100 !,lOOlt 1\0 Il ,," OALONE
THIS CIRCUITRY AMPLIFIES THE SIGNAL FROM THE PID COLLECTOR PRIOR TD DIGITIZATION BY THE AiD BOARD ,
DEU CTOAI DONOT HAVE AN1JD 1l00RD. T ~ lIl I NOO£LS REQUIR E lEIlD PQn AND AYUNUATOR$ TO ACJ Un TIiI o n l cro ll OUTP UTS TO THEIR tI I IIlI OU VIL. SEe THE "URO POU AHD AnEN UATOfl$ " PAGEli'l TIoI1S lECTIOH.
0.01 uF LOW
10M
.,
C,
.
270 pF
1000M
HIGH
SIGNAL INPUT
eNe
+12\1 U
.6
FROMPID COLLECt OR
2
10K .7
Ul •
'K
3
7
t-vUI
•
C7 O.l uf
·12V' t2
oeec
,
. 12V III
U2
~Ill
2
lK
,
~1UF
e3
2000 pF
.3
100M
••
WH7
4&lIK
e.
"
,.
0.1 uF
~
MED FPD ELECTROMETER SECTION OF AMP BOARD
HIGH FILTERED 1000 p F
THIS CIRCU ITRY AMPLIFIES THE SIGNAL
270 pF 1COCM
...OJUST TlII! OI Tl CTQR OUTPUTS 1 0THIIR O
DIGITIZATION BY THE AiD BOARD ,
"
Non: MOOE~ ~,o STUDENT Te O G.C . AND"'ODEl 1\0 STANDA LON E C£TECTOIlS DO HOTHAVE AN '-10 BOAII O. 'IlIl!!! MODELl REQ\JlRI! ZERO POll ANOAn EliUAtO RS TO
FROM THE FPD CO LLECTOR PRIOR TO HIGH
+12V IZ
••
2
10K
U1
,
5 lGHAl OUT TO ND OOARD
·12V " GROUNOE O)
C'
.7
lOS
INA1t7 ? (PINS 1 ,$,8 ALS O
., eNe
C. O.1uF
~
3
,
C2
SIQNAL INPUT f ROMf PD COLLECTOR
e LK
CI O.l yF
eLK
CI O,I
~11)
.12V_1
3 • 7
U'
C7 O.1u F
3 ·12V ' 2 OP8G
r-vt
21
,
2
C4 O.l uf
~
• is ¢1UP
·12V lfl:1 lNA117P (PINS 1,5,8 ALSO
GROUNDED)
SIGN AL OUT TO AiD DOARD
'4
WH7
4t19K
C6 . 6
1M
0 .1 uP
~ P'lI' 8 olT
Fll.n. mo: Arnp·Cl6.tcw
AMP-E SCHEMATIC Oa\ o· 1 ~ 12 0J97 Rev. ale:
,
B :R.Fen$o
386 (of 550 ) 2006(-2016)
387
BLACK
FlO, PID, DELCO, FPD, NPD, HID, TID POT AND ATIENUATOR
TCD POT AND ATIENUATOR
ELIMINATE R ~ 11M) AND ClI (O.1uF); CHANGE R4 FROM 49iK TO 1Kj ADD l OOKFROM WIPER Of 2CKPOT
CHASSIS MOUNTED TCDCElL FROM
SCREW TERMINAL ON AMP BD.
.IEAT
'l .f
• •
BK
"
GREEN B
- 'K R• '0' ~
; t;
I~:;f R
\.
BLUE
'"'"
TO HEA'
0
6W
BOARD
Jt
*
"'0
ZERO POT ASSEMBLY
INA.117P (PINS 1,!!,B ALSO GROUNOED)
,
.
"-
TeO: ZK POT
"-
SIGNAL t
WHT/ A TT E NUAT O It
L100K
B
ECD POT AND ATTENUATOR
W:\"EO
"'''STo"
VALU ES IN OHMS
t 2~
U'
+U V
;'Vb ~~ ''I: 0 0'6 IJ"0
.'-'
~VLF356
.,
3
r 014
'K
.)"
,
'JzoUnV
B
I Plgl701l I
ALL OTHERS: 20K POT
•0
0
•
"
BLK /
"
\.
SIGNAL "
SIGNAL t
WHT/ ATT ENUATOR
·12V
RW 20K 2EOO POT
5.1(
,~
100K
r-r--:
+12V
a
012
ELIMINATE R15 (1M) AND C13 (O.1uF); CHANOE R14 FROM 1M TO 1K ; ADO 1M FROM WIPER OF 20K POT
.,.
ou
ATTENUATOR ASSEMB LY
1M
I'
20K POT
WHT/
~~
\..,.
\
t?
·12V ZERO
SIGNAL t
.
1K
-1;S.~ tv
YELLOWWIRE OP PKONE CA.BLE TO D1 SI'L#,Y ac. TCO PROTKT "ACTUAL" IIlOI.TAGETO GROU ND ON REO FlLAJ,lENTj
BlK
BLK RED
SIGNAL-
e LK /
,
,
o•
04
C$ O.1I1F
-
SIGNAL·
BLK/
An EN UA T OR
L
OHM
2
"B
'-" '~ ua . /
WZERO
....-o",-.,ro ,.
WHY
3 t12y".~ C4 O,IIlF
-
DOARD
-
FH,nama: Arnp..z.tew
AMP-E POTS & ATTENUATORS t ' 212 01 ..v 011 :9/271
~
) 387 (of 550 ) 2006(-2016)
388
ACCESSORY RELAY BOARD (14 RELAYS) WITH EXTERNAL CONNECTOR
TO
TO
TO
LAWSON BOARD
LAWSON BOARD
LAWSON BOARD
/'
+12V
+12V
R4
+12V
R2
R3 RELAY 4 10K
10K
RELAY 3
<
04
10K
1~
03
2N3903
2N 3903
. ,2VFROM AMP BOARD
lUF
RELAY 2 01
I--'
N
2N 3903
, \
2N3903
\7 I
NO Ici INC
.-
I
NIC
NO C
NO ICI INC OPTlo .....t
'AOelUQ ~OI'l
OPTlO.. AI. ,PADE l UGFOR
SPA[)( llJO 1"011
' AnOH O'"
F.t.!:Tnll nR
FASTON 0 111
•
1 211 10
NC
NO C
r-
RELAY 1 10K
~~
02
4
+12V
R1
:
(?\-:,
le,
TO LAWSON BOARD
OPTlON"1.
SOl-DE", CONNEC11ON
9
•
BOLDEFl CONNEC1 10N
7
6
6
4
SOLDER CON NECT ION
3 2
1
. P.g11 ofZ
GROUND
'Ill. :
(
( 388 (of 550 ) 2006(-2016)
389
DUAL REMOTE START PULSE STRETCHER
..12V
+12V
,
r-
RS
"12V
.. 12V
U,
U2
R1
55S TIMER
S5S
R10
1M
R'
10M
,
1M
10K
C4
2N3903
R6 10K
l "'O "' ~ N T "' RY
,.
START CIRC UIT . 1 GROUNDlHQ OF TNE INPUT
PRO DUC ES '" ~ S~CON O NEGA TIIi E GO ING PUl 81
ON T~ ~ OUTPUT WHICH TRIGGERS TNI! LA W SON OOAR O REMOTE STA RT FUNCTION,)
Ii ~'"' , C'
lUF ~ "'. " '~ ' ~
RlZ
TIME R
ONO
R' 'OK
i: ~ ~'"' ~ +12V
10M
0 13
; ~ ..LC1
10K
~l:F~
R14
Rl1 10K
2N3903
______ 1 _
"L "'~ ' ''' STA RT CIR CUIT' 2 C...OIolENTARY GROONDINGOF THE IHPUT " RODUCES '" J S£COND NEO",TIVE GOINO Pl/lIl! ON TIlE OU TPUT WH ICH TRlGGERS Till!
10K
'7
'N
o;;;;V
LAWSON BOARD R E ~ O T I! STAII T FUIoICTlGloI,1
Pig' 2 Df 2
RELAY-C SCHEMATIC -ot ll :
389 (of 550 ) 2006(-2016)
390
Chapter: Troubleshooting Topic:
Leak Checking your GC
There are 3 wa ys to c hec k for gas leaks in a GC. The 1st method of leak checking is called " 'o okin g fo r bubb les" or "snooping the fittings", Snoop® is a specific brand of leak check solution. but SRI suggests a mixture of isopropyl alcohol ( IPA la nd water. The alcohoi reduces the surface tension of the water so it flows into the cracks between the tUbing and the fitting. otherwise water ale ne would be fine. Don't use soapy water beca use if the leak check solution gets inside the GC tubing or fittings, it will contam inate th e system.
- c, • A Jow cost disposable medical syringe is perfect for plac - :; ing a drop of lee k check solut ion at tn e joi nt where the ~ tube ano tne frtting meet - A 3mlleak check syri nge is provided with evert SRI GC ~.
Apply gas pressure to the syste m then place a droplet or two of leak check solution on the tube connections. If tiny little bubbles are visible then the fitting is leaking.
, u.
Using the liquid leak check solution can be difficult however when there are many fitting s to test or when some of the fittings are hot, ( this wi ll rap idly boil off the leak check solution ) making it impossible to tell if there are bubbles from a leak or bubbles from the water boiling awa y,
Liqu id leak checking is the least effective way to chec k for gas leaks in a GC system.
- -0"-"'" """ - ......... . M2Il263.p ub
Ie ••
page 1 of 4
390 (of 550 ) 2006(-2016)
391
Chapter: Troubl eshooting Topic:
Leak Checking your GC . .. .
... .
'=::-.:.:: .~
The second method of leak checking is to use a leak d etector. Leak Detec tors are made by several different man ufactu rers, but in most cases they con sist of a vacuum pump and a thermistor detector which mea sures th e th erma l cond uctiv ity of the gas that is sucked up through the hand held probe. When heli um or hydrogen flows through the thermisto r, the thermal conductivity is a little greater than the therma l conductivity of air. so there is a res ponse on the mete r of the Leak Dete ctor.
Commercial leak detectors are avalab!e from sev· eral different manufacturers. Prices range from about $600 to $2 000 . '.
,
- ---
e
Ap ply gas pressure to the system then sniff around all th e fillings with the Leak Detector. Th e display on the Leak Detecto r ind icates a leak.
Unlike the liquid leak check solu-
tion, the leak Detector ca n be used on hot fitting s. but is difficult to use if there is any airflow around the fittin gs ( such as in a GC oven with the fan runn ing ).
Some leaks may be too sm all to detect, and some fitti ngs may be in-accessible. Be careful with the probe around live electrical circuits or heaters
page 2 of4
391 (of 550 ) 2006(-2016)
392
Chapter: Tro ubleshooting Leak Check ing your GC
Topic:
The third meth od of leak checking is call the " pressure drop" test. The pneumatic system is plugged at the end of the ga s flow path . Th is may be the outlet of the de te ctor or the end of the column . Plug the pneumatic system off a the end of the gas flow path. You have to knowwhere the gas exits to the atmosphere
Use a swagelok fitting or a
swagelo k nut with a GC septum to make a gas tight seal. If the plug lea ks, the te st will not work.
The system is then pressurized using the E PC ( electronic pres-
sure regulalor ) built-in to the SRI GC . The EPC is then turned dawn ( or off ). Because the end of the · gas flow path is plugged , the gas is trapped ( under press ure ) in the pneumatic system . If there is a
leak , the gas pressure will drop. If the entire system is leak free, the pressure will remain for many minutes before it slowiy drops. The
Use a swageJok cap or pug frtting, or use a GC septum in a swage!OK nut to make a leak-tight seal
rate at wh ich the press ure drops is indicative of the magnitude of the
leak
-----
. - ~- -
Monitor the system pressure to see if it /' drops fast. slowly or not at all ..
•
••
•
9'
• • • • •e •.
•e •,.. •e, ., · , ,, "• "" •• ,•, ,, •. • • • o
o
.\1.a.."'l263.pub
------1
--
,~, ,~~. ~"'
<........ -
•• . . - . - -
~-~-
\
.
I;I
t
ELECTRON iC GAS PRESSURE CONTROLS
r ...: ~;-
•• .- ••
\\ •..-.... ~ .
9
':",=_... .
1\'
', t "''="J'' \' u
l
t\
e
e
~
r
~
:
•
V
.
-:-
u
.-
~
•
-
'0'
-
~
.o.
•
.o.
"~
;
C • i .....
; "
I~
; (: ~~
.
Pressurize the system using the EPC, then tum oown the EPC pressure
page 3 of 4
392 (of 550 ) 2006(-2016)
393
Chapter: Troubleshooting Topic:
Leak Checking your GC
If the pressure does not drop at all, or drops very slow ly, then th e entire system is leak-tight. In some way s, this is th e bes t way to check for leaks, because one test verifies th at eve ry connection in the syste m is hold ing pressure . With a complex gas system . or one where some of the fittings are in-accessible cr hot it may be d ifficult to use the leak check liquid or meter. Also, the pressure drop test ca n detect leaks that are too sm all for the other methods to see.
If the press ure does drop quickly, th ere is a lea k in the system. To locate the source of the leak, move the plug from the end of the pneumatic system to the next fitting upstream and repeat the test. If the system now ho lds pressure, th en the leak must be somewh ere between the location of the previcus plug and the current plug .
I Injector I
~
I
@)
Detector
Column
~
0
-- -
Directi on of gas flow
P lug the pneumatic system off at th e end of the
gas flow path. You have to know where the gas exits to the atmosphere
I
Injector
Direction of 93S flow Move the plug to the next fitting upstre am in th e pneurnatic system and repeat the pressure drop
test
I I nJ~/~ C005 By moving the plug location step by step upstream, eventually it will be obvious where the leak must be.
----_
Co ILmO
Direction of gas flow
Detector
..
A gain move the plug to th e next point upstream and rApt'! at tile test. When the svstem does hold pressure, you have passed the lea k location
\ fan263.piJD
page .j. of4
393 (of 550 ) 2006(-2016)
394
(
Chapter:
INJECTORS AND GAS VALVES
l
Topic:
Electric Valve Actuator Maintenance
~----------------------------------~) If the gas chromatograph in use is equipped with an electrically actuated multiport gas sampling
valve and, after discussing the trouble experienced with the technical support staff at 8Rl Instruments, a valve actuator replacement is deemed necessary,
•
•
•• •
then a replacement valve actuator may be pu rchased
(or ordered under warranty) and the replacement may be performed in the field by the user.
By following the steps outlined below, the user may effect the replacement of the actuator in
a relatively short period of time without much difficulty.
SRi gas chromatogram equipped with electrically actuated gas sampling valve
STEP I: Remove power from the unit and allow it to cool to ambient temperature. Disconnect the power cord from the AC supply (waIl outlet). Unplug the 5-wire modular plug on the cable that exits the base of the actuator housing. STEP 2: Remove the two brass thumbscrews securing the valve oven cover. Then remove the valv e ove n cover. Remove the top insulating blanket directly beneath the val ve o ven cover. STEP 3: Note tha t there are four holes in the insulating blanket at the base of the valve stem. These holes permit access to four Remote control wand Phillips-head screws that secure the valve oven to the stand-offs mou nted on the valve actua tor through the bracket Remove the four screws (a magnetic de vice may be needed to retrieve the (secured by two screws through the insulation). brass thum bscrews) STEP 4: Using a 9/64" Allen wrench, loosen the set screw on the side of the collar securing the valve stem shaft. ~ This will re leas e the valve assembly. Then lift the valve Tbermosraned • @ • oven slightly away from the actuator assembly in order to valve oven insert the Allen wrench into the two set screws present in assembly the top surface of the collar ring. These screws go through the bracket must be removed . Stand-offs and -~;n:::olii"=::IlT valve stem collar • STEP 5: Remove the four hexagonal stand-off posts mounted thro ugh the bracket into the valve actuator assembly. This will free the valve actuator asse mbly from the bracket Electric valve actuator and permit replacement Remove defective actuator assembly assembly (used and substitute with replacement valve actuator. Reassemble with multiport in the reverse order , from step 5 lO step 1. sampling valves) STEP 6: Verify proper valve operation after reinstallation. Verify that the valve position matches the position indicated on the remote control wand . Li sten to the valve when rotating to hear for actuator jamming or other unusual noises . VJEW OF VALVE OVEN AND
Valveoven~
'~:l
_+-_
If any difficul ties are encountered during or after the valve
ACTUATOR ASSEMBLIES AS SEE N FROM FRONT OF UNIT
actuator replacement process , contact SRI Instruments technical support for assi stance at (3 10) 214-5092. If an actuator is suspected to be defective, cons ult with SRI before attempting removal. The problem may be located elsewhere in the system and diagnosis may be possible over the telepho ne. D:\EPIDOCS\VLVACTRI .EPD
394 (of 550 ) 2006(-2016)
395
EPC Calibration: I. With the gas o ff connect a 0 - 30 ps i gauge to the union on the output of the EPe. (Inside the instrument. the EPe's are on the left) 2. Adjust the EPe SET POINT on the top of the front panel to 20 psi. Verify the SET POINT is at 20 psi with the pushbutto ns. 3. With the supply gas o ff. Zero the disp lay [ 0 a selling of ·0.0 using th e OFFSET PO T adjustment on the EPC- board sho wn be low . 4. With a supply pressure of 30 psi turn on the supply gas . 5. Adj ust the SPA:'Il POT on the EPC board to make the gauge pressure equal to the SET POINT pressure. 6. Repea l steps 3-5. until the ZERO is -0.0 and the gauge and disp lay both read 20 psi.
/
OFFSET
~-..I . ~ SPAN
395 (of 550 ) 2006(-2016)
396
CHAPTER: Topic:
:\I AIYfENANCE Installa tion of the optional Air Compressor in SRI 8610C GC
Pans List: TOGGLE SWITC H FLAT WASHER LOCKNUT 6" COPPER CONNECTING TUBING 1116" to 1/8" SS BULKHEAD FITTING AIR COMPRESSOR with extended leads and extended output tubing
Quantity I 4 4 I I
I. Tum off all gas supplies to the GC and removeA C power plug from o utlet. 2. Remove the BOTTOM CO VER of the GC by removing the 6 retaining screws. 3. Mount the AIR COMPRESSO R to the existing stud s (see accompan ing diagram) with supplied WASHERS an d 6/3T LOCK NUTS. Secure all wires and make sure no wires are contacting the AIR COMPRESSOR AIR COMPRESSOR \\, 11 become hot when ope rating. 4. Remove the hole plug from the GC front pan el hole marked as internal air compressor on/o ff switch. 5. Install and sec ure the TOGGLE SWITCH through the CIRCU IT BOARD with wires facing towards the bottom o f the GC. 6. Solder the 2 wires from the TOGG LE SWITC H to the 2 bottom connector hole s on the CIRCUIT BO ARD to the left of the TOGGLE SWITCH. 7. Remove the hole p lug from the GC from panel hole marked as ER COMPo, . OUT
8, Mount the STAINLESS STEEL BU LKHEAD FITTING in the opening marked as AIR COMPo on the left side of GC.
OUT 9. Connect the extended gas tu bing from the AIR COMPRESSOR to AIR CO:vl P. marked on the left si de panel of the GC . Ro ute the tubing OUT away from e lectrica l components. 10. Connect the 2 wires from the AIR COMPRESSOR (0 first 2 posi tions of the blue terminal block, which is nex t to connector holes for the TOGGLE SWlTClI wires on the CIRCUIT BOARD. 11. Disconnect the FLU ISTOR A S S E ~1BLY (B in diagram) by loosening nut C in diagram wi th a 7/1 6" wr en ch and a 7116" wrench on po int D to prevent the Tefitting from coating.
C:\\VJNWORD'DOC\A.IR .DO C/rl
REV .06·18 -97
396 (of 550 ) 2006(-2016)
397
CHAPTER:
Topic:
:\'IADITENA..'ICE
Installation of the optional Air Compressor in SR18610C GC
Warning! Excess torque or stress on FLUISTOR ASSEMBLY can damage the delicate del-ice. 12. Disconnect FLUISTOR ASSEMB LY by loosening nut A with a 7/ 16" wrench. 13. Remove the STAIJ'>,'LESS STEEL BULKHEAD FIT"fr.'G from the oc, 14. Remove the frit if present. inside the STAI:\'L.ESS STEEL BUlKHEAD FII lING by
inserting a 1/16" diameter rod into the BULKHEAD FITTING andcarefullytap the end of the rod on a desk. Without removing the frit, air supply pressure can be reduced from
approximately 12 psi to 7 psi, which may result in low FID sensitivity. 15. Re-install the STAINLESS STEEL BULKHEAD FITTING and FLUISTOR ASSEMBLY.
I
16 . Connect AIR COMPo and AIR OUT
#11
BULKHEADS. which are marked on th e left side panel of the GC, with supplied 6'" COPPER COI\"NECIDG TUBING. 17. Re-secure the BOTTOM COVER of the GC . Toggle Switch
Terminal Block
Ai: Comp:essor
6" Copper COMectir.g
A
Tubing
Fan AJr
Compo
Out
Ftuistcr Assembly
Transform=r
C:\WINWQ RD\DOOAIR.OOClrl
REV.06-18-97
397 (of 550 ) 2006(-2016)
398
ELECTRONICS Replaci ng the OP-Amp Chip In You r SRI GC Testing the OP80 or LF356 Amplifier Chip(sj The parts kit in the plasti c tackl e box under the red lid ofycur SRI GC contain s a sp are 0 P80 o r LF3 56 amplifier chip. Additional OP-Amp chips are availabl eunder SRI part number 8690-1000. FID, NPD, HID, T ID. PID, FPO . and DELCO detectors use the O P- Am p chip. The OP-A m p c hip amplifies the ana log detector signal. You shoul d rep lace a detecto r's OP·Amp chip when you're not getti ng the sign al response that is otherwise consistentlyobservedfrom your detector.whenthe detector signal is pegged up (5000mV) or
down (0), or when the detector bas failed the Wet Finger test.
..
If your detector signal ispegged up or down, try the following:
liB
1. Tum OFF the GC power (fo r at least 10 sec ond s) . 2. Shut down th e PeakSimp le software progra m.
The OP80 Amp Chip
3. Re-launch PeakSimple. 4 . Tum the GC po wer O N.
5. Withoutzeroing the data system signal, observe the milliVoltreading. Ifit is still pegged at 5000mV, rep lace the OP-Amp c hip. Sometim es the signal \\;11be pegged at or near O, but sooOm V is much more common with a faulty OP-Am p cmp, Wet Finger Test: 1. Make a "V' sign with the first 2 fingers ofyour hand 2. Moisten those fingers (lick them ).
3. Place one finger on the co llector e lectrod e, and s imultaneous ly place the other on bare m e tal. Iike the colwnn o ven lid. Make your con tact brief, and observe the millivo ltreading. 4. The data sy stem signa l shou ld jum p from OtoSOOOmV (max volta ge), an d come back down when you remo ve your fingers. If your contact does not produce a similarly significant change in the millivolt reading, then you should replace theOP-Amp chip.
Ifyou have dummy loads or the means to create them at your disp osal. you m ay use the method outlined in the tab le bel ow 10 test the O P-A mp c hip(s). !fthe readings are not within the ta rget range. you should
replace theOr -Amp chip(s). DETECTOR GAIN TEST DETECTOR/51
DUMMY LOAD
TARGET GAlN (S) READINGS
F D / NPD /H D / TD
16000MOtm resesor ccrrecec kl cereer of SNe jlIck and QI"OU1d
HIGH (+2DOOmV). MED (100mV). HI FLT (+2000mV)
PO
16000MOtm resistor romeCIed 10 cersee of BNC jack ClOd gfOU'ld
HIGH (+10 00 mV l, MED fl 0 0 mV ), LOW (l OmVI
16000Motrn resislor correc ted 10 cer.ter of BNC
HIGH (+100l)mV). MEO (100mV). HI FLT (+1000mv l
FPC DELCO
jack~nd 9l'Ot.I'ld
,.",..--
l OCMOtm re Sistor comecled 10 red & wtllIl Wl n!
HIGH ( +1400 mV) , MED (14 0mV) . LOW (l 4mV)
398 (of 550 ) 2006(-2016)
399
ELE CTRONICS Replacing the OP-Amp Chip in Your SRI GC Replacing the OP -Am p Chip
I. TwnOFFand unplugthe GC. 2. Remove the 6 screws hold ing the bottom panel o n the GC
chassis. Support thepancl whileyou gently rock the GC onto its back, then lower the panel to your working surface to access the chassis interior. 3. Locat e the Amp board in side the GC chassis on
.. The amp boa rd is the long board on the right hand si de of the GC chassi s mtenor
the right ha nd sid e. Remove the protective steelplate by loosening the two thum bscre ws that secure it to me aluminu m stand-offs, an d set it as ide.
4 . There are four possib le places on the A mp board for the OP-Amp chip, depending on the detector to which it is assigned. From the top (or front, with the CiC in normaloperatingposition). the Amp board sections read FPD. FlO , PID , and DELCO . Ifpresent , the [\;PD w ill be a t the FID position. as would a TID if present. However, because the circuits arc identica l, this isjust a general guide. The Amp bo ard will be populated according to the detec tors installed on the GC. X ote thai each circui t has a pair of chips, almost identical in appearance, installed side by side; the OP-Amp chip is the one on the left.
5. Use a small flat bladescrewdriveror simil ar too l to pry the O PAmp ch ip out of its socket and off the Amp bo ard . (A poc ke t knife nail file was used in the picture).
OP8D Amp Chip
Marker.
6. Noteth e serni-circular depressionon one end of the OP-.-\."llP chip ; this is 2. marker for proper orientation of the chip, and it corresponds with a s imi lar mar k on the socket. The e nd of the chip bearing the marker faces the top of the amp board. so
you will install it with that end facing away from you. Care fully position the chip over the socket so that each of tbe eight pins occupies aholeand press it Into place. 7. Test the new OP-Amp ch ip with the metho ds described 0 ::1 the previous page.
399 (of 550 ) 2006(-2016)
400
GC ACCESSORIES H2 ·SO Sta nd-Alone Hy drogen Gene rator Overview Your SRI H;! ~5Q Stand-AloneHydrogen Generator consistsof agenerator-cell mountedon a metalchassis. Thegenerator- cell is attached. to the chassis with twoscrews for easydisasscmbly-c-justunscrew them, unplug the power cord. and the entire cell comes off On the metal chass is is a pressure gauge. an interior pressure switch. a dessicant bottle. and a toggle valve shut-off for isolat ing the generator cell. The dcssicant bottle contains Indicating Molesieve dessicant beads which tum from blucto gray when they absorb water. Water vapor that is released from the generator cell wi th thehydrogen is remove d by the dessicaa t before reac hing the GC column. thus dryingthe hydrogen gas. The ~ -50 cansupply cnoughgas fora detector or two as wei ) as the GC carriergas, Daring operation. there is about 40mL of hydrogen gas stored in the dessicant, 'which is en ough to operate a split inj ecto r for-short pe riods, in additio n 10the dctcctcrt s) and carri er. The toggle val ve shut -off facilitates checking for leaks and allows th e ~-5 0 to reac h operating pressure more quickly, while the interior pressure switch maintains the operating pressure. As a safety measure, a pressure release valveprotects the generatorcell from pressureo....erload. An externalpowersupply/transformerthat is provided
enables the H2-SO to operate on various voltages around the world. You mayuse any approved POWCT supply
rated lOO-240YAC with l2VDC, 7amp output. Conveniently, the H2-50 produces 50mU min at 35psi (241316Pa., 2.4bar) using distilled water from the grocery store.
The SRI H,-50
-Dessicanl bottle_
-_.....
- 20ml Syringe --~ Pressure
gauge
Approv ed external power supply
Cool ing fan
400 (of 550 ) 2006(-2016)
401
GC ACCESSORIES H, -50 Stand-Alone Hydrog en Generator
Theory of Operation The SRIH,-50HydrogenGencrarcr separates ~'atcr intohydrogen and. oxygen using a ProtonExchange Membrane (pEM). The warcron theoxygen side of the PEM is disassociated into 0 2and hydrogenprotons. The hydrogen proton is transported through the PEM to the hydrogen side. where it recombines with an electron to make
f\.then bubbles up through the water reservoir. The H 250 Generator Cell
, -::, ;:::--=-~~,, .i- Vcttage -,... /
m-
,
- Fili I H2 gas out
Powerplug ~ (connects to ~50 chas sis)
Water rese rvoirProton Excr.ange Membrane
-
r
,,_.
_
- T77,L.?----
(PE M)
Oxygen & water ou tlets
Ope rational Diagra m of t he H 250 Generator Cell
Ii I
,,
®
I
Wate r reservoir !
®
@ ~
/\
@ Proton Excnange Membrane
Hydrogen side
(PEM)
Oxyg en side
!
H + e-= H2
1-
, H
H Te-=H
H
0, V
2
"" I/o 0 , I
H,
H+e-=H2
~o
1\
H
H
0,
H
!
I
V
401 (of 550 ) 2006(-2016)
402
H2·50
GC ACCESSORIES Stand·Alone Hydrogen Generator
General Operating Procedure Use the H,-50 on a Oat, level surface, awa y fromopen flame and any other ignition SOW'CCS. including sparlc: sources. 1. Remove the nut with the septum from the Fill I H2 Out port onthe top of the generator cell. 2. Use the 20mL syringe mounted on the right-hand side ofthe ~-50 chas sis to inject clean di sti lled water intothe waterreservoir. Although clean tap water will work in a pinch,use distilled water whenever possible. Fill only to thetop fill line ; do notovefill. Replacctbemn and septum on tbefill port and hand tighten until the nut contactsthe black o-ring 00 the fitting.
3. MakeSW'C the dessicantbcttle contains dry beads. Dry dessicant beads are blue in color, they tum grey when wet. See below forinstructions on recharging and rcplacingthe dessicant beads. 4. Connect the
~ -50's
"H2 OUT" fitting to the GC's hydrogen gas inlet. Output from the Hl -50
"HYDROGEN OUT' fittiDg is connected to the GC with 1/8" or 1116" 0 .0. tubing. Make sure thered and black power cord is pl ugged into the H.,-50 chassis, and co nnect the ex ternal power suppl y c ord to the generatorand a wall outlet. Makesure yoU havethe correct input cord forthevoltage youare using. Properly used, th e transformer is not a spark source and poses no ign ition threats.
5. Close the JL shut-offvalve. Always build up pressure initially with the toggle valve shut; it will take 5-1 5 " minutes, 6. TheH 2 g as pressur e is preset t o 3Spsi (241316Pa, 2Abar). Once this pressure is attained, the interior pressureswtrch will shut o ff the CWTCDt to thegenerator: Thc water in the generator cell reservoir should stop
bobbling 7. Wait IOm inutcs to make su re th at 3 5psi (24 1316Pa, 2Ahar) pres sure is maintained Ifprcssure is not being maintained. there is probably a leak.. Chec k: the d.essicant bottle; it shoul d be s oug against the o-ring. Make sure the FiJll ~ Outport nu t and septum are intact and snug. Check th e bottom ofthe wat er reservoir aroundthePEM formoistureto ensuregeneratorcell integrity; if you findany seepage,tighteneach of theeight
screwsthat bold the ceil layerstogether. 8. Ifyou fiad DO indication ofa leak after 10 minutes ofstabilization at 3Spsi (24 13 16Pa, 2Ahar), open the
toggle valve to let the ~ gas flow into the GC. 9. Whenthe water in the gcreraror cell water reservoir reaches the bottom fill line, it is time to re fill it. 10. Case the toggle valve . II . Unscrcw the Fill I ~ Outportnut and septum anduse the syringe to refill th e c ell to th e top fill line. 12. Replace thenut and septum, and tighten unti l snug.
13. Sinceyou have thecell pressure vented, it is a good idea to check. the des.sicant for any grey coloringto see ifthe beads need recharging. Ifthcy do, follow the instructions on the next page (Gen eral Operating Procedure continued).
402 (of 550 ) 2006(-2016)
403
GC ACC ESSORIES H "50 Stand-Alone Hydrogen Generator z
General Operating Procedure continued
Recharging and Replacing the Dessicant Beads Periodic recharging ofthc dcssicant beads will be necessary as they absorb water during operation and tum grey. The bluecolorof the dry beads comes from cobalt chloride.. Takecarenotto bakeout the dessicant beads withany food item. 1. Bcforcyou loosen the dessicant bottle on the ~ -5 0 chassis, vent the hydrogen pressure in the generator cell by unscrewing the nut capping the fill port on the top of the cell. Itwill hiss audibly until it isreleased.
2. Dry thedessicant beads by pouring them onto a paper plate and cooking them in a microwaveoven for 23 minutes. Or, pour them onto a glass or metal pan and bake them in the GC oven at 250"('. Do not microwave or baketbeplasticdessicantbottle. The dessicant beads canberecharged over and over again; they lastindefinitely. Sbould you need them, dry dcssicant beads are available in kilogram quantities from Alltech ( I-800-AL LTECH; part # 055 53).
3. Let the beads cool especiallyafter microwaving them. Refill the dessicant bottle withthe dry, blue beads. 4. Rcplacethe bottle 00 the 1 ~-50chassi s and hand tighten it. Tbcrc is an o-ring that engages with the bottle top ; tighten thebottIeuntil itis snugagainst the o-ring,
S. The dry dcssicantcontains some air which will purge out during the first fewminutesof operation. You may notice yourretention timeschange temporarily sincethecarriergasmayintially be amixture ofbydrogcnand air for a fewminutesafterdessicanrreplacement, The FlO flame may alsobe hard to lighruntil pure hydrogen
comesthrough. You can speed up this equilibrationprocess by buildingup pressure in thegenerator cellthen venringwitb the toggle valve 2-3 times before reconnec ting the H2-50 to the GC . Keep in mind that the
internal pressure switch will cut the curr ent when the cell reaches 35psi (24l3 J6Pa, 2.4bar), so you don't need to build up too much pressure before venting it Experiment to learn what works best foryour partieular GCsysrem.
403 (of 550 ) 2006(-2016)
404
GC ACCESSORIES H,-50 Stand-Alone Hydrogen Generator
Maintenance an d Troublesh oo ting
If the water in the ~-50 water-reservoir looks cloudy, itneeds to be rep laced:
1. Remove thenut with the septum from the Fill / H2 0 l.1t porton the top of the generator cell, 3. Turnthe generator over and pour the water out Whenthe water is almost all out, shake the generator to help it dra in. 4. Usc the syringe to refill the water-reservoir with clean, distilled water through the FilI /~ Out port.
5. Replacethe nut and septum on the Fili i ~ Out port.
SRI ~-
I
I Red & black powe r cord
-
Powe~ piug
See the fo llo wing page for PEM replacement
For service. call 310·214·5092.
404 (of 550 ) 2006(-2016)
405
GC ACC ESSORIES H,-50 Sland-Alon e Hydrogen Generator
Maintenance and Troubleshooting continued lfthc Prot on Exchange Membrane (pa f) changes color. it most likely n eeds to berep laced.. New ~-50 PEMs are available from SRI under part # 869Q..()15 1.
I. Put the replacement PEM in clean distilled water to soak wh ile you take apartthc generator cell. 2. R emove the generator cell from the H~-50 chas sis by unplugging the red and black power cord from the
cha...."is. and unscrewing thetwo screws that hold the clamping plateagainst the cell. 3. Loosen the eight screws that hold the water reservoir lr1 creme nlal!y with a philips head sc rewdriver. Loosen each screw in loosen the increments; firston e, then theone opposite. and so on in a screws in this star-like pattern. As you progress, be mindfulof thespring in the waterreservoir,don't loosenthe screwstoo suddenly, or it may pop open the reservoir, presenting safety and damage risks, Yoocan feelthepressu:rc ofthe spring relax as you loosen the screws sufficiently; hold the top of the Hand le the generator cell firm ly with one hand while loosening the screws with the other.
1 -'
8·
.~ . ..
3
<:r, -
.;~ :~
4. Once the screws are removed, carefully take the water
reservoir offthebottom ofthecellandremovetheoldPE.\t
.,•
Beverycereful handling and moving the graphitecoil,as it can easily come apart 5. Takethc new PEMoutof itsbath and positionit centrally within the ring of screws. Place the water-reservoirback on the bottom, over the PEM; the rEM should protrude slightly on all sides oftbewatcrreservcir; 6. Oncethe PEM is properlypositioned, tighten thescrews in increments until the water reservoir is snug against the ' -
-. Positio n the PEM
centrallywithin the o rcre or
screws
---'
bottom ofthe generatorcell. 7. Put the generator cel l back on the chassis an d secure it with the plate and two M-JC'\\oS. Plug the red and black power cord into the chassis.
8. Plug the l-l-50 intoa wall outlet and pressurizethe generator cell to 3Opsi. Check: the bottom ofthe water reservoirarouod the PEM formoisture. ifyou see any seepase. tighten each ofthe eight screws a little more.
405 (of 550 ) 2006(-2016)
406
H
2-50
GC ACCESSORIES Stand-Alone Hydrogen Generator
WARNING!
Warnings and Safety Precautions: The ~ -50 generateshydrogen,which is an extremelyflammable gas. Undernormal operation, the safety features of the H 2-50 protect the operator. However, operators must usc common sense and take basic precautions. Hydrogen burns with a flame that is invisisble to the naked eye. Do not use theH 2-50 near any
flames, sparks, or sources thereof including labovens. heaterelements, bunsen burners, torches, etc. When venting thehydrogen from the generatorcell, NEVERopenthe Hz-50togglevalve nearan ignitionsource! Hydrogen is Don-toxic, but it can cause asphyxiation in confincdspaces by displacing oxygen. Usethc~ 50 in a ventilated room with an ambient temperature of 5-4O"C (40-1OO"F). Ifthe GC power is interrupted or cut off during hydrogen generation, flip the toggle valve to isolate the generator cell, then disconnect the external power sourcefrom the ~ -50 and the ""1111 outlet. This is a good general response in any situation of uncertain risk; ifyou' re not sure what' s happening, isolate the cell and pull thepower plug. That way. you can
take the time to diagnoseany problemswithout H2 accumulation. Familiariz.e yourselfwith the safe operation ofthe GC and other equipmentto which you intend to connect the Hz-50. The ~ -50 is designed to be safe under the following EnvironmentalConditions: •
indooruse;
•
altitude up to 2000 meters;
• •
temperature 5"C-4O"C; maximumrelative humidity 80'%for temperatures up to 31"C. decreasing linearly to 50'%relative humidity at 4O"C;
•
POLLUTION DEGREE = 2 in accordance with lEe 664.
WARNING!
406 (of 550 ) 2006(-2016)
407
Changing the PEM membrane on the SRI hydroge n ge nerator
The SRI Hydrogen generator is most common ly found as the stand-alone H2-50 version shown to the right.
A sma ller 25ml/min version may also be foun d built-in to some SR I B6l0C GCs.
'.
407 (of 550 ) 2006(-2016)
408
Changing the PEM membrane on the SR I hydrogen generator 1) The Proton Exchange Membra ne ( PEM ) used in the SRI hydrogen generator may need replacing periodically. If the generator does not make hydrogen at all, or only very little, if the membrane looks very dark or dirty, or if the generator gets hot and steamy, it may be time to replace the PEM.
2) Remove the H2 generator cell from the GC or stand-alone chassis, then gently wiggie off the black wire connector on the top of the cel l.
3) Loosen the eight screws which clamp the top of the cell to the bottom. Initially, ju st loosen each scre w a little bit and loosen them evenly tc avoid putting too much stress on any one screw. The water in the cell will leak out when you do this, so it may be a good idea to do this over a sink.
page 2
408 (of 550 ) 2006(-2016)
409
Changing the PI=M membrane on the SRI hydrogen generator to ) 8e sure that the aluminum stand-offs on the bottom of the cell don't rotate as you remove the screws. Hold each sta nd-off with a small wrench if you have to.
5) With the eight screws removed , the top of the cell will pop up due to the spring inside which pushes the graphite rope electrode against the PEM. Carefully lay the top of the cell aside.
6) Peei the old PEM off the bottom. Check the platinum screen for bits of old
PEM material. If the platinum screen seems rough or has sharp edges, use your fingers to smoo th it down
:Vfar'224,pub
409 (of 550 ) 2006(-2016)
410
Changing the PEM membrane on the SRI hydrogen generator 7) Examine the old PEM for clues as to why it may have failed,
8) The new PEM is available from SRI under part# 8690-015 1 for the 50ml/min H2 gen and 8690-0152 for the 25m l/mln model. The new PEM is crystal clear and comes in a plastic bag. It is easy to think the bag is empty because the PEM is clear.
"
9) Sea k the new PEM In clean water prior to installation, The PEM is extremely hydroscopic ( absorbs water ) and will expand slightly as it is soaked. Soak the PEM for a minute or two.
Man224.pub
pagea
410 (of 550 ) 2006(-2016)
411
Changing the PEM membrane on the SR I hydrogen generator
10) Place the new PEM in the center of the cell. It should fit snugly inside the circle of eight aluminumstand-offs.
11) The graphrte electrode is constructed of a coil of graphite rope. In most cases it will stay together, especially if you handle it gently.
12)
Sometimes the coil will
come undone, so you may
"
have to rewind it and ooax it into position within the recess of the plastic disk. Do this in such a way that the coil of graphite lays flat.
\1ll1l224.pub
page S
411 (of 550 ) 2006(-2016)
412
Changing the PEM membrane on the SRI hydrogen generator 13) To keep the graphite coil from coming apart as you reassemb le the cell, place a thin
ruler or strip of cardboard over the coil while positioning the cell top on the bottom. Once the top is in place, slide the strip out.
14) Replace 4 of the 8 screws, but just engage the screw threads one turn. Examine the cell from the sides and bottom to ensure the graphite coii is centered. If not, remove the screws and nudge the coil into the center of the cell.
15) Replace and tighten the eight screws. Tighten gradually and in a alternate pattern to avoid over-stressing the plastic. Finally, re-connect the black wire to the connector on the top, fill with clean water and re-attach to the GC or stand-al one chassis.
Ma:1224.pul::
pegc 6
412 (of 550 ) 2006(-2016)
413
Chapter: Hydrogen Generator Topi c:
Using the Extended Run H2 Generator kit
The SR I Extended Run !tit for the H2-50 Hydrogen Generator consists of a moorneo Hydrogen generator cell and electronics, a peristaltic pum p, and a large dessfcant cham ber. The extended run cell comes equipped with a water level sensor which tu rns the pelistaltic pump on and off automatically to maintain a constant water lev el inside the ce ll. A one gallon tonre of grocery store qua lity distilled water is sumcient for two months o r more of operation. The large dessicant chamber holds abOut two pounds of ind icating mole sieve dessicant. Th is quantity of oessicant is also enough for two month continuous operation at 40mllmin or lo nger if the H2 flow requ iremen t is lower. In the photo to the right , you can see the bott om third of the chamber has turned gre y after one
Pe ristaltic pump
mo nth of use.
The pe ristaltic pump re-ctreulates the distilled water from the bottl e past th e oxygen side of th e PEM ( proton exchange membrane ) . Beetro-osmotic drag pulls th e water through the membrane to the hydrogen side. VVhen tile wa ter level nses to th e tip of the wa ter lev el sensor, the peristaftlc pump shuts off. Excess wa ter is retu rned to the disttDed water bottle.
By pumping the water across the oxyge n side of the PEM instead of directly into th e waler reservoir we ca n avoid pump ing against the 30 psi of H2 pre ssure in the water reservo ir, which is hard on any pum p and prone to lea ks. The oxygen side of the m embrane is at ambient pressure , so a simple peristaltic pump ca n be expected to work rel iably and fo r a long tim e. A disposable 5 micron 25mm syri nge filter is used to prevent d og ging of the passageways inside the HZ ge nerator trcm dUSl: and small fibers which seem to find their way into th e water res ervoir despite all precautions. This filter should be changed w heneve r the dessicartt is re-gene rated. Al most any breno of syrin ge filter is OK to use , but we supply a MJlli pore MiIl ex~ LS part# SLLS025NS.
5 micron Fitter
1/8 ' I.D. 1/4- 0 .0 PVC inlet tubing
Silicone outl et Tu bing baekto water bottle
1116 ' 1.0.
118- 0 .0 Silico ne Outlet tUbing
rnan266.pub
413 (of 550 ) 2006(-2016)
414
Chapter: Hydrogen Generator Topic:
Using the Extended Run H2 Generator kit
A one gallon bottle of grocery store distilled wat er makes a good water reservoir. Cut hol es in the top and feed the 1 /4~ tygon and 118- silj.. cone tube s all the way to the bOttom . Put the cap back. on to keep dust and fibers out of the wat er. Most pump problems resu lt from clothIIlg nbers dogging the internal water passages of the H2 cell.
-c.
The desstcenr chamber has a pressure gaUge, pressure r elief valve ( 45~i ) and two quick connect fittings. Th e bra ss quick connect is the inlet and the silver quick co nnect is the outle t.
Press ure relief valve
When ctlanglng the uessicant. or if you want to bypass the dessicant chamber, the inlet and outlet frttings sim ply plug tog ether. The dessicant chamber stays pressurized when you unplug tne con nections. Th is is im portant becaus e this allows you to re-ge nerate th e dessscant, pre-purge the air out and leave the unit pre-pressuri zed wit h hydrogen. ready t o be reInstalled with minim um system down-time.
The inlet and outlet quiCk connect fittings m ate to-
gether
ma n266.pub
414 (of 550 ) 2006(-2016)
415
Chapter: Hydrogen Generator Topic:
Using the Extended Run H2 Generator kit
Many customers opt to purchase a sparedessicant ch amber so that when they arrive on-site to perform th e monthly or periodic maintenan ce , th ey have a pre-charged dessicant
cham ber which they can swap right into tne system. This avoi ds the down-time which wo uld otherwi se result from fhe time it takes to pu rge air out of th e Chamber after re-gen erating
th e deseicant bea ds. Since th e H2-50 makes a maximum of 50
O-;.......
O-ring
sea l
.,. .-.ii;
t:·" - ";.. ~
; \", , '
,' i
;0;'
~
~ ~~ ~.~!.\ J" 1
cav.e- Ii . j e . e ~_~
rnVrni nut e, this can take hou rs .
It makes more sense 10 swap dessrcam chambers in th e fi eld and re-gene rate the old chamber back in the Jab.
., -
The desslcant chamber has eight wing-nuts whiCh secure the top, compressing a ru bber a-ri ng which seals in the pre ss ure.
-- -
To chang e or re-qenerate the dess icant beads. release the pressure in the desslcant ch amber by pushing the button on the top of the silver outl et q uic k connect fitting . Verify ( usi ng the pressssure gauge) that the pressure has bled down to ambient before removing the nuts.
l oosen each of the eig ht wi ng-nuts a littl e at a tune
l oosen the wing-nuts evenly. l oosen each winq-nut a litt le bit at a time be fore removing any single win g - nut . This protects th e plastic top from un-necessary stress.
man166.pub
415 (of 550 ) 2006(-2016)
416
Chapter: Hydrogen Generator Topic:
Using the Extended Run H2 Generator kit
Remove the top of the desstcant chamber by
)
lifting straight up . The brass inlet quick con-
ned: fitting has a tube wh ich extends all the way to the bottom of the cessicant chamber. Inspect the outlet at the bottom of the tube to make sure it is not plugged Of blocked . (There is a metal flit i n the t ube to prevent blockage from dus1 )_
Pour the dessicant beads into a glass bow!. Don't use a plastic or metal bOwL Microwave the beads for 5-- 10 minut es unt il th e blue color
returns. 00 NOT USE A MICROWAVE WHICH IS A L SO USED FOR FOOD.
The beads wi ll be very hot wh en yo u remov e them from the microwave oven , so allow them to cool , then pour them back into the dessi-
cant cnamter. DO NOT PUT TH E DESS ICA N T CHAMBER INTO TH E MICROWAVE OVEN. Re-assemble the desstcant cham be r and th en purge the chamber with dean hydrogen from a cylincler. Verity t nat the Cllamber holds pressure by watching the pressure gaug e afte r , - - - - -- - -;-;,...L:: pressurizing th e chamber to 30 psi.
Pu rge the air out af the chamber US-
ing d ean lab hydrogen
Don't forget to change the fi tter.
rr.an26G.pub
416 (of 550 ) 2006(-2016)
417
Model 302 Six Channel USB PeakS im ple Data System The Mode l 302 may be used withanybrand or model ofGC or HPLC offeringan analog detector output signal ranging from -5V to +5V. It includes three independent programmablecontrols (OV to +5Y analog outpu t) for temperature & pressure or HPLC gradient formation. The Model302 has six channels. whic h can be randomlyassigned to one offourtime beses, which allows independent startand stop times for fourseparate instruments. Fcur rcmore start inputs compatible with 2·",rire switch closures (typically output by GCsand HPLCsas a remote stan signal)arealsoincluded for your usc. Two pulse stretchersare providedto accommodate intstrumcnts with remote start signals shorter than one sccond(such as Hewlett PackardGCs). Thecomputerto which ) 'OU connecttheModel 302 must support USB (it musthaveat leastone t.:SB port-e-rev2.0 or higher-s-end use WindowsN 98. 98SE. ME. 2000. XP or newer).
With your purchaseof thcModeI302, you shouldrcccivc the following: items: I - Model 302 Data System box (front and rear views shown below) 2 - USB cable for connection to your computer's U SB port 3 - Manuat (either the PeakSimple Chromatography Data Systems or the SRI general productmanual) 4 - PeakSimple for windows'" software(inside the manual cover)
G akSim O le a:r~""~
ill1
'fl ,_
i'
£;!!""""='" '
The M odel 302 comes in a sturdy alurninumbox ccessricgoftcp aod bo
thumbscrews for easy inrerior eccess. The brass thumbscrews are on the left· and right-hand panels of the Mode l 302 box .
Front Vi ew
PeakSimple ChromatographyData System Sj~
Chann el USB Po rt
PCM'ER Ind icator LED
Rear View Ooe nins for analog sign a! cable(s ) and remote start device connections ..., .......-
oe
-_ . ,, ~
~
......._W = .. Dt"" ~
r.~
Breaker
POWER switch
• USB ccnnecor
Power cord
417 (of 550 ) 2006(-2016)
418
Model 302 Six Channe l USB PeakSim pl e Data Sys tem 1. Open th e Mo del 302 Verifythat theM(rle1 302 ispoweredOFFand unplugged, Rcmove thethumbscrews on both sides of the Model 302 box and slide the top cover up and of[ It is connected to the bottom of the box by a groun d w ire , so just set it next to the
bottom hal fofth e box . H gh vaIlage
alum inum / safely cover
Power Supply board
rI
;'I --Fdil -' I.
..., _ dI ' ------=30_
The Modcl302 box contai ns two circuit boards. The board on the right-hand s ide is the AID board. The board on the le fthard side uOOerthe removablehigh voltage aluminum safetycove-is the PowerSupply board. Hyou need to remove tbe high
vo lt age al umin um sa Cct)" cove r, ALWAYSunp]ug th e Mnd cl .'\02 fro m
\
,I
,
t he wall power outlet first (you do not
need to rem ove it for the wir in g connections described here).
2. Connect the Ana log Signal Cab le(s) NOTE" The analog output from some GCs and LCs can have a rangc ofup to 10vo lts OC. The Model 302 can tolerate this voltage in~ butsignalsabove 6 volts will generate unwanted noise an dsigrals above 5 volts wil l be " c lipped" (the tops of thc waveforms will be cut off). Use the 1voltoinput rypically avai lable on the back ofyour instrument 2- L Ro ute the analog signal cab les from your instrument through the 0fX-'1l hole in the back ofthe Model 302. ..... ' 2-2. Strip 114" of insulation from the "signa l-s" and "signal-" wires of your instrument's signal cables. 2-3. Remove any j umpers placed in the
T
Ch anne ls l -s scre w t ermin als at thc factory. Insert the "signal-vwire intotheAID board SCTC'\\' term inal marked .. I +" and secure the
conne ction with a small flat -b lade screwdriver; 2-4. Insert the "signal-t' wire into the AID board screw terminal marked "1 -" and
securethe connection. 2-5, Repeat the connection ofsignalcables
for channels 2. 3. 4. 5. and 6. Any unused Channels 1-6 a nd GO (grou nd) screw terminals
channels MUST have both inputsjumpercd to ground,
418 (of 550 ) 2006(-2016)
419
Model 302 Six Channel USB PeakSimp le Data System
~
.3'_
...
The remote start wires for the first two ins truments are inserted into the se screw terminal s on the Power Supply board.
e©i ,,'fi'. .-'"
~ .;c.'. " ___
e.
e0 3
46.
3. Connect the Remote Start Cables (OPTIONA L) The Model 302 remote start capability allows you to start the damsystem by means ofa switch closure. Four separare rem otc startcircuits permittheusc-to individually start TIMEBASE I, 2,3, and 4 of the data system. In some applicati ons. the chromatograph being used with the Modcl302 may offer a remote start signal output or switch closureoutput that permits starting an integrator or other device when the STARTbutton is pressed on th e chromatograph 's on -board control panel. Typically. this signal can be used to start the Model 302. TTh.ffiASES 1 and2 arc equipped with pulse stretchers. 3-1. Route the remote start cable from your insrumcrmhrough the open hole in the back of the Model 302. 3-2. Strip 1/4" ofinsulation from the "+" and "-" v.ires ofyour remotcstart cablc(s). 3-3 . Insert the "+" wi re into the Power Supply board sc rew terminal marked "# 1 !N'" and secure the connection. 3-4 . Insert the ••~.. wire into the Power Supply board screw terminal marked "# 1 a" and secure the connection. 3-5. For a second instrument, insertthe "+" w'ire into the "#2 Do... terminal, and the"-" ",'ire intothe ";';'2 G" terminal
The screw termi nals fOT the third and
fourth instruments' remote starts arc on the AID board, The bankofscrew tcnninalsis labeled "DIGITAL IN'" under "1 2 3 4," Connect the "+" wires for thethird andfourth instruments to screw t erminals 3 and 4. respectively. Connect both "-·' \ v-ires lathe "GD" screw terminal next to the "4- screw terminal (on the right-bend side). ]I.-O TE: TIMBASES 3 and 4 require a remote start signal ttarpcrsise longerforthan one second. Check your instruments '
specifications(forexample, Hewlett Packard GCs produce a H~I)' shortremote start pulse, so you should connect one of these to TIMERASE t or 2, which arc equipped with pulse stretchers).
419 (of 550 ) 2006(-2016)
420
Model 302 Six Channel USB Peak Simple Dat a System 4. Connect the Externa l Event R elay Wi res (OPTIONAL) The Mode1302 has eight0-5 volt TIL level outputs that are wired to a bank of mechanical relays with screw terminals for easy connection to any device which may be operated from a contact closure (normally open ~O] and normally closed [NC] contactclosures). Theserelays may betumcd OlvandOFF individually and automatically through a PeakSimple timed event table. Manual control is also available via the computer keyboard. Conned your devices 10 the A-H Relay screw term inals -4',"",",_
4-1. Route the external event wires from your instrument through the open hole in the back oft he modc1302. 4---2. Strip 114" ofinsulation off of each wire.
4-3. Select which dev ice should be connected to each event ("A" through " H"), then insert th e wire into the appropriate scrcwtcrmi nal on the Power Supply b oard, and secure the connection. Make and keep a lis t ofea ch device you connect and the Relay it is conn ected to for your re ference (you will need this information to activate the devices automatically with an event tab le or manually with tbcmousc).
5. Re place the cover on the Model 302 and secure it with the thumbscrews. 6. Connect the USB Cab le to Your Computer The Model 302 is equipped with a USB co nnector. A US B cable (p rovid ed) connects the Model 302 to your window s1M computer's USB / r port. This plug and play interface permits th e Model 302 to be loaded onto and operated from a desktop or laptop co m puter that su pports USB (rev. 2.0 or higher). 6-1 . Secure oneendofthc USB cable to an availabl e USB port on your PC.
~..
6-2. Securetneomerenc iome usa connector on the back ofth e Model
302.
USB port
.'
-
i
•
I I
J ....
~
420 (of 550 ) 2006(-2016)
421
Model 302 Six Channel USB PeakSimple Data System 7. Connect Power to the Model 302 Th e M odel 302 is provided with a power cord which
plugs into a standard 110(or220) volt outlet. Plug the Model 302 intothewall outlet TumONthepowerswitch and verify tbat the POWER LEDon thefront ofthe Model
The power LEO is lit when the Model 302 is connected to a power source & switched ON.
302 is lit.
8. Ins tall Pea kSimple Chromatography Software 8 ~ 1. Locate your copy ofPeakSimplc, which is shipped inside the front cover ofyour manual. Insert the CD orfloppy disk(s) intoyourcomputer's appropriate drive.
...... ......,. ..'"~
""""'''''''-''''''''''''~-'
'.
""'_. . . _ . . !_.->;
P'p ': ! E<, g ...
_ ..;. <
~
_
.:::J
0.0
' - I~ .~
3.
8-2. Open the appropriatedrive through MyComputer, then doubl e cl ick on "Setup.axe" and follow the instructions . By defau lt, th e
setup program places the PeakSirnple application directory on the hard drive: c:\peak2000. If you put the application directory elsewhere, take note ofthe path as you may have to enter it in a
dialog box duringtheUSB driver installation procedure.
" ".....
.
,0•.•,
::r
" .,...~ I,.'1 ., -
9. Install the USB Drive rs There are three important files saved to the PeakSimple app licati on
dircctoryat the conclusion ofthesoftware installation:ll_USB.inf, LL_USB.sys, and LL_USB2K.sys. These files arc required for Windows to recognize the AiD board connectedto the computer's USB port. 9-1. Double-click on the MyComputericon on your desktop, then on Co nl rol Panel, then on Add New Hardware, which should open the Add New Hardware Wizard. 9-2. Click the Next button twice, until you get to the screen that gives you a choice between letting wmdoc,-s find thenew hardware, or selectingft yourselffrom a list. Clicktheradio button to cho ose the hardware from a list and click the Nextbutton.
f ffiJ
i Mv
L~om p"u~
,
j
13"",:1,: ... _ ~t:
....
_ "
;n
.kl
~""
~
"._~
... r_ _
. ... :;;;.:;;!",t_ _
1. ,~
. - -- --.......,
,... ~ .. ".~ ...
'~_
.::.:J ..
;:.;
e..
-> ..iJ ~
-... ....::."
"-
--
.'~'.." 34~
-~~_
1 Control or: := "=" ~- _ . ' ;;.;;' ""§h5iWY" . .,,",,'
.-
4-*' III
58.
:
'~, ~= """, ~e _"" '~ ' ''''''''''''''
-.-.-.... ...,.""" ......... "'''''.,..~ _ "' _ ''''''· ~ _ '" l . ..
421 (of 550 ) 2006(-2016)
422
Model 302 Six Chan nel USB PeakSimple Data Syste m
_.. . . .> - -_.. ~...._-... ..:._-,. ....
~
k'?~ F-~'
~- ""'"
[ .~,
~
..........~
V
~t,~~ .....,.' "',,,,,,,,
. . ....... :s';';;"""""""'!'_
~~
~
.-
.-
,
-
.
-~-
J
.......
9 3. Scrolldown the hardware list, c1ick on
-V
Universal Serial Bus
~
" ....
_-_... .
_~
-~
.
,.. " " ~ e : -
~r
.... .
~~ , ~ . ---::
I
the Have Disk button.
,..C ::h ..
from the PeakSimplc directory ("Copy manufacturer's files from: c:\peak2000j.
-_-_.;,;;",,,,,,,..,,,,,,,,,,,,,,,,,,,:::::=::::-!t
i tt:
_
. ... _
"""".......
.. , , . . _
__
""'-
_
~
...
~ , - _ ."' _-._
I"
:d
9-5. When you click
J
t iOiM'dft!ift * ~
L -
___ _ .oJ
drivers arc for Lawson
c"'"
Labs. Cl ick Next on
__ .._3 1
_._-
.. C! ,.. - .--_..........."
~
Windows \\; 11 finish - t-.
.oJ
OK again, the Wizard will confirm that the
following screen, and _ ,
-_
I
" c.,.,;.,iJ ~~ 1
;,3 ~'
[ ~.::
this sc reen a nd the
,~
.
.-
~ I ",'
j
e ,..-n
,_rtf
you click OK. the wizard will verify that you want to co py files
_ .. ._-
. u- C~:'- -I
- ; i;.i- " ' " ' " ~
:9
~
\ Ib i . ,
Lti>I ~
9-4. Click Browse and navigate to the PcakSimplc application directory, or type in the path ("c:\peak2000" or the nam e you have chosen). TheWlZattlshouldlinUtbcLL USB.inffile. Wben
f'!!§t
:bo~ _
~ ..:-.
'-':",=- " ~. e- ,,_ ...
controllers, then click Next. Fro m th e following screen click
........._ _ ._
... ....... . _ _ ..._ _ _
o.;, _ _ _
~
1(P
!~ ._.. _ _ . _ --
I r..:~ r- ~ '"' :",,;-.
,~.
installing the software fOT t h e Model 302.
J
Click Finish.
9-6. Restart your computer (you MUST resta rt your comp uter before the drivers will work). Openthe Control Panelagain. then System. then click on the Device Manager tab. lfthe USB drivers have been successfullyinstal led. theUnivetEal serialBus co-rroners section will Jist " Lawson Labs, Inc. USB Data Acquisition
H
""""",",
I
-,
I
,I
I
"
..... I I" " ~ 'J
-r--.
422 (of 550 ) 2006(-2016)
423
Model 302 Six Channel USB PeakSimple Data System 10. Launch PeakSimple 10- 1. Do ub le-click on the PeakS imple icon to launch the p rogram. Verify that co mmunication has been estab lished bet...veenyour competer and the Mcx:l.el 302. An errormessage wi ll appearif communication is IlOtestablished. This is normal untilyou complete the following step.
10-2. Each SRI USB data system has a unique -l-digit USB device number beginning with "5" (503 l , 5032 , ctc.).
ThisLD. number is printedon the back of your Mo del 302, and on your
IDE M "_ lOt _ r... t"'
)ii I.! ~
.
:'£:wc .-.,! . ...... ~-~~
',."-
r~
~
PcakSimplc disk. Open the PcakS imple Edit menu an d choose Overall. Enter your Modcl 302 LD . number in the box
Iabeled rccm port I USB oevce number." Click OK, and Peakximplcwill attempt to "wake-up'tthe dera system. Click the
Save All ~ icon so you don't bavre to
~~ _
f-f'-""
/,--
re~ the USB d~;~ nwn~.
-
... lQ..oI P - ...... _
~_ .e-cl ~....
- - .._
r
~
-..
..
~
,"-
Doo'. d
.a.s; .-d~ """'=
~ _ ..........
cc
iC ; =-
I
c......r
Enter lhe 4-dlQil USB cevce number here ._
••
•
" E'J
10-3. For the remote start option: Open the Ed1t menu and choose Channels. Click on the Details button tor channel I. Verify that Remote start is enabled (the box should be checked). Repeat th is step for channels 2-6 ifnecessary
10-4. For inforrnation nbout using Event tables, man ual Relay activation, ctc., seethe "'PeakSimple Tutorialsand the"PeakSimpie Sofiv.me" sections in tbemanuel (and online at www.srigc.com-cclick on the "Download
Our Documents" button on the homepage).
423 (of 550 ) 2006(-2016)
424
Mo del 302 Six Channel USB PeakSlmple Data Sys tem 11. Sta rting an Analysi s 10-1. Theuppcrright comer ofthc PeakSimple chromatogram \\-iadow contains real-time information pertinent to youranalysis in progress. Thestatus oftherun(SfA.' ID BY, R'IDolis displayed in capital letters uextto the millivolt(mV) reading, underneaththe amountoftime into therun
-,
-, fk
_ I t:' E4 l
r_
~
•
~
O l
!
•••
•
t .- '
e.
...
-'31:P1O''---- - - - - - - - - - - - - - - - - - - - ' ~
~
~o
11-2. Hit your computer keyboard spacebar to begin the run. and the data is plotted cnscrccn in the chromatogram windowv,
.,
•
• • • .-
Press Ihe spa ceba r to beg in the run
'\ Press the End key to step merun
11-3. Hit the End key on your computer keyboard to stop the run.
Te chnica l Support: Ifyou have questions ceproblems , call SRI tor free technical support at 3 10-2 14-5092, gam- 5pm California
time.
424 (of 550 ) 2006(-2016)
425
Chapter:
MODEL 202 DATA SYSTEM HARDWARE
Topic:
Model 202 Hardware Orientation
The SRI Mode l 202 PeakSirnple Chromatography Data System is a four channel, analog to digital converter, controlled by our powerful PeakSimple Software. The Model 202 may be used with any brand or model of HPLC or gas chromatograph offering an analog detector output signal. The Model 202 also feat ures two independent, programmable controls which can be used for temperature and pressure ramping or HPl C gradient formation. There are also two Remote Start inputs that are compatible with two-wire switch closure signals typically output by GCs and LCs as a remote start signal . Eight TTL outputs (0 to 5 volts) for computer control of external events come standard with the Model 202. If TTL outputs are not adequate for your application, the Model 202 also contains relay circu its offering normally open (NO) and norma lly ciosed (NC) switch closures . Electronic Pressure Control (EPC) and a switched AC power output may be
ordered as an option for the Model 202 .
•
POWER
SRI a....... fOIIr
MOOEL202 s.r1oIl Part
PeakSimple Chromatography Data System (front view)
Opening for an analog signal cable RS232 serial port and remote device connections connector
\ SRI Instruments, Inc;:. • 11008 P:ilradin "oad Las VqJas. NIl 891 19
{70213l1.,2210 {FAX) 3&1-96 90
/
Optional switched AC power ouput Optional Electronic Pressure Control
o --
o
/
/
• -_ -. .....
-~
(rear view) The Model 202 comes w ith a built-in serial interface for connection to your desktop or laptop computer's COM Port, (See the "PeakSimple For Windows" section in this manual for minimum system requirements.) You should have received the following with your Model 202 purcha se: (1) Model 202 PeakSimple Chromatography Data System Box (1) Serial Data Interface Cable for connection to your computer's COM Port (1) PeakSimple For Wi ndows software package (1) PeakSimpIe Chromatog raphy Data System Manual
425 (of 550 ) 2006(-2016)
426
Chapte r: MODEL 202 DATA SYSTEM HARDWARE Topic:
Model 202 Installation Connections
To connect the Mode l 202 to your ccmputer it will be necessary to access ccn nection terminals inside the Modei 202 Box. Verify that NO POWER is applied to the unit before performing the following procedure!! Remove the thumbscrews on either side of the Modei 202 Box and carefully slide up the top ccver and set it aside. Figure 1, (below), depicts the layout of the Model 202 circuit boards and all wiring connections. To connect your system to the Model 202 Data System; please complete Steps 1 Through 7 as shown below and described on the following pages.
STEP 5
I
STEP 6
STEP 4
I
I SRI MODEL 202 CHROMATOGRAPHY DATA SYSTEM WIRING DIAGRAM
-...., - ..
.. •
-
.--
STEP 1
LAWSON 202 BOARD
"OTE: FOWEll: nus UI'IIT ON BEFORE BOOTINO P~IMPLE SOFTw ARE
._. rH~r-'-1""!'
IITL ,
•
., , ..=•
II
•
•
"
.I ...
•• • ••
,II
RELAY (serpsJ
•
•• • ••
BOARD
f- ~ _
__... _.._...__ . _.......
. ..
STEP 3
...
_-" ........... -...·..·.11.·
~
.. "
II
-.J \
OPTIONAL ELECTRONIC
:
RESSURE CONTROL(E.P.C.) BOARD
STEP 7 -
Install PeakSimple Fo r Windows software.
I FIGURE 1 I 202~.tcw
011211198
426 (of 550 ) 2006(-2016)
427
Chapter. MODEL 202 DATA SYSTEM HARDWARE Topic:
STEP 1:
Model 202 Installation Connections
Connecting the analog signal cab le(s): NOTE : The analog output from some GCs or LCs can have a ran ge of up to 10 volts dc. Although the Model 202 will allow high voltage inputs such as this; be advised that signals above 6 volts will generate unwanted noise and signals above 5 volts will be "clipped". (The tops of the waveforms will be cut off.) Route the analog signal cables from your instrument thro ugh the open hole in the back of the Model 202. Strip 1/4" of insulation off of the 'signal +' and 's ignal ~' wires of your signal cables. Insert 'signal +' into the Lawson 202 board screw termina l marke d 'CH 1 sig +' an d secure the connection usinga small screwdriver. Insert 'signal -' into the Lawson 202 board screw terminal marked 'CH1 sig -' and secure the connection using a small screwdriver. Repeat the connection of signal cables for channels 2, 3 and 4. Any unused channels MUST have both inputs jumpered to ground.
STEP 2:
(OPTIONAL) Connecting the remote start cable(s): NOTE : The Model 202 offers remote starting capability as a standard feature. Two separate remote start circuits permit the user to start the
MAIN and A LTERNATE Trigger Groups of the data system by means of a switch closure , such as a footswitdl. In some ap plication s, the chromatog raph be ing used with the Model 202 may offer a remote
start signa l output or switch closure output that perm its starting an inte grator or other device when the START button is pressed on the
chromatograph's on-board control panel. Typically, this signal can be used to start the Model 202. Route the remote start cable from your instrument throu gh the ope n hole in the back of the Model 202. Strip 1/4" of insulation off of the '+' and '-' wires of your remote start cable. Insert '+' into the RELAY (serps) board screw terminal marked '#1 IN' and secure the connection using a small screwdriver.
Insert' -' into the RELAY (serps) board screw terminal marked '#1 G' and secu re the connection using a small screwdriver.
NOTE: Be sure to check the "Remote Start" box in the Pea kSimple For Wi ndows EDIT - CHANNELS - DETAILS scree n for the appropriate cha nnels. Refer to the "PeakSimple For Windows" section of this manual.
STEP 3:
(OPTIONAL) Connecting the external event relay wires: The Mode l 202 features eight 0-5 volt TTL Level outputs that ma y be turned on and off individua lly and automatically by means of a timed e ven t table. Manual contro l is also available via the keyboard. These outputs may be used to control external events or devices. If TTL level
outputs are not adequate for your application, the Model 202 is also equipped with eight relay circuits offering normally open (NO) and normal ly closed (NC) con tact closure s.
427 (of 550 ) 2006(-2016)
428
Chapter: MODEL 202 DATA SYSTEM HARDWARE Topic:
STEP 3:
Model 202 Installation Connections
(Continued) Route the external event wires from your instrument through the open hole in the back of the Model 202. Strip 114" of insulation off of each wire. Select which device should be connected to events 'A' through 'H' and insert the wire into the appropriate
screw terminal and secure the connedion using a small screwdriver. Refer to the "PeakSimple For Windows" section 01 this manua l for setting up event tables, keyboard activation, etc.
STEP 4:
Connecting the Serial Data Interface cable to your computer:: The Model 202 is equipped with a RS-232 serial port. A DB-9 type serial cable (provi ded) connects the Model 202 to your personal computer throug h the PC's COM port. This simple interface permits the data system software to be loaded onto, and operated from, either a desktop or noteboo k PC for portability in field operations . Secure one end of the Serial Data Interface cable to an available COM port on the Back of your PC. Secure the other end to the 06-9 connector on the ba ck of the Model 202. (Refer again to Figure 1 tor location of the Serial Data port.)
STEP 5:
(OPTIONAL) Connecting to the switched AC output: Connections for the switched AC output are pre-wired at the factory. All you need to do is plug your device into Ihe cord provided ; activate relay 'A' using PeakSimple software and the oullet will be powered. (1 AMP maximum) NOTE: The switched AC output must be specifically requested at the time you order the Mode l 202.
STEP 6:
Connecting power to the Model 202: Slide the top cover back onto the Model 202. Secure the coverwith the two thumbscrews. Model 202 units are equipped with a power cord which plugs into a standard 110 (or 220) volt outlet Plug the Model 202 into the outlet and verily thaI the POWER indicater on the front of the Model 202 is lit.
STEP 7:
Installation of PeakSimple Software: Refer to the "PeakSimple For Windows" section of this manual for details on proper installation and operation.
428 (of 550 ) 2006(-2016)
429
•"•
a
> L
,<
:to~J:
l$ z
~ ;u
",:i : ,.., rn 1Il1l:)o z J: eg .. ;:o ;!l; ~ ~;ri
"••
~ ~ 8 fil[P
~ ~ ~g ~ S iizz::U
~
.. ", ~ 2'"
: ..
zn
", m " -< C:
~i:l 2 ili=l ~q ~
g :i!
i
~g:c:
mo -
"
•
n , •
" <
•"
0
<
z
oz 0
~
0
c~
<
It Z n O::\l
0
•<•
.
~ ,. I'll... Cll s8 S :l' ''' o '''
"•"
... m ..
.
", <::)0
~
_::t:r21
n " ~. zo < . 0
.
<
8 ;• S •
·. " ~!.
0
z
, ••=
0
" h
~
0
c
~
-- -• - "" a~ 0
,
•
••
"z ~,+,.!1 f:
x.> I
0 ~
O
I
, ~
n
'"
"
~
<
0
~I
~ ."c rng: ...
00"' '"''_
~ ~
~IO
< <
•
....... -
~ -P-j...L
i5~ !il~
•
"<
<
-
I
1
i
0 .. ;: 0
, I.
i
-w
i : ~ m
,...,.i:
•
I
-• """
~:n ,
o g
•","•
~
s ""
•0_ >
I ~
i
-• "
~ N
m ~ C
·
•
I
~
~
~8 ~~ o
.
I•
~
~
I
~ I
n
•0
-• <
)o O!!. ::::f" i
i
w
•
~
~
a
"<• I
~
I
~
n ~
•
~
"
• • · ~C/l o "
I
Io C/l
~:::tm
s"
•
m;l!
D:l tIl
:5:"C » Ch -I _c>'
ao
%
1
•o •
• 429 (of 550 ) 2006(-2016)
430
OPTIONAL AC OUTPUT CIRCUIT #1
OPTIONAL AC OUTPUT CIRCUIT #2 AC HOT IN
Ae HOT IN
U3
U3
R28
R26
R"
100 OHM 1 WATT
sc
r.:
1 2
• 5
3
4 t-+l1 WATT
~
UOC3041
CONTROL FROM LAWSON BD. RELAY 'A'
100DHM TRlAC
Q'OO4
ACOUT# 1
1000HM
R27
1 WATT
1000HM
TRIAC Q6004
1 WA.TT
Ae CONTROL FROM LAWSON BO.
AC
J.r U
cur In
RELAY'B'
Pilillt 2 of Z Filoollm9: "'IK.... pg2 .tl:w
SERPS·G SCHEMATIC nate :
121'201~1
I
By: R. Fenske
2tffi03 - ev: M Watts
430 (of 550 ) 2006(-2016)
431
quickSlorl
Model 203 Sing le Channel PeakSimple Data System J
The Madel 203 may be used with any brand or model of GC or HPLC offeri ng an analog detector output signal ranging from 0-5V. It includes tV¥"O independent, programmable controls (0-5V analog output) for temperature & pressure or HPLC gradient formation. A remote stan input compatible with z-wi re switch closure s
-I
(typically outputbyGCsand HPLCs asa remote stan signal) isalsoincluded for your optional use. Ope n the Model 203 Verify that the ~fodel 203 is not plugged into a wallsocket and is therefore powered OFF (no power switch). Remove thethumbscrews on both sides ofthe :\lode1203 box and slide the top cover-up and off It is connectedtotbe bottomofthe box by the ground "ire, sojust set it next to the bottomhalfofthe box. There is a wiring diagram of the Model 203 circuit boards and all wiring connections on the inside ofthe lOP cover. Use this wi ring diagram (shownbelow) to complete steps 1-5 as described on
thefollowingpages.
/ STEP 2 /
(optional)
STEP 5
••
I.Lf
t I
o.
I
i'
'! '-W-
G . - ---,
!O
<
. '
i;;~~~
• ' - -, 1
~ ~
r!jlii' fl
US!. I~~~o ~;~~~ ••
'Ljs
,.-
Q
- :\ -
0
I
o
°• •
~.Y
~
'" z
0 N 0
w c>
,. 0
i!;
W,·F
ST EP 3 (optional)
-~§l§
h.~,
-~W'.".
-
0 -
:fo ~
431 (of 550 ) 2006(-2016)
432
Quick Ilarl
M o d el 2 03 Single Chan nel PeakSim ple Data System
STEP 1: Con nect th e Ana log Signal Cable 1-1. Route the analog signal cablefrom your instrument throughtheopen hole in the hack of the Model 203. 1 ~2. Strip 114" of insulation from the "signal-s" and "signal-t'wires ofyour instrument's signal cable.
.......
.
"".,.....", '" -. v..,.. w ..·"
.-. -.,.. ;,wp,.
-'''''''' '''''
.
- - "-' (~ . ~~ - /
.., .....
:: ~
Route wires through this hole
1-3 . Insert "signal -s" into th e Lawson 203 board terminal marked "signal-s" and secure the connection with a small flat-blade screwdriver.
SCTn\'
1-4, Insert "s lgnal-" into the La\\"SOn 203 board screw terminal marked "si gnal-" an d secure the connection.
STEP 2: (OPTIONA L) Connect the Remote Start Cable The Model 203 remote start capabil ity allows you to start the darn system by means ofa switch closure. In some applications, the chromatograph being used with the Mode1 203 may offer a remote start signa l output or switch closure output th at permits starting an
integrator or other device when the START button is pressed on the chromatograph' s on-board control panel. Typica lly. this signal can be used to start the Model 203. 2-1. Route theremote start cable from your instrument through the open hole in th e back of'the M odel 203 . 2-2. Strip1/4" of insuIation from the "+" ard -vwires of your remote start cable. 2-3. Insertthe - +" wi re into L;'::203RLY board SCfC'\.\." terminalmarked - IN" and secure the connection.
,
H3
i
Connect th e "+" a nd "-" wires of your lnsaumenrs remote start cable to the IN and GND termm a's here.
2-4. In sert the "-" wire into the 203RLY board screw
terminalmarked "GND" and secure the connect ion.
•
-.
Replace the Model 203 cover and secure it with the th umbsc rew s.
432 (of 550 ) 2006(-2016)
433
Quick SI811
Model 203 Single Cha n ne l PeakSimple Data System
STEP 3: Connect the Se rial Cable to Your Compute r The ylodel 203 is equipped with a RS-232 serial pon . A DB-9 type serial cable (provided) connectsthe Model 203 to your Windows P' computer through the PC's COM port. This simple interrace permits the Madel 203 to be operated from a desktop or laptop computer. -I 3-1 . Secure one end of the serial cable to an available COM port on your P'C. 3-2. Secure the other end to the RS-232 serial port on the back oftbe Madel 203.
DC powerinput
Serial cable (0 8- 9 type)
STEP 4: Connect Power to the ModeJ 203 Model 203 units areprovided with a 15V DC power supply which plugs into a standard wall volt outlet. Plug the power supply output plug into the back of tbe Model 203 and plug the power supp ly into the wall outlet. Verify that the POWER LED on the front ofthe Model 2OJ is lit. 15V DC power sUpply
433 (of 550 ) 2006(-2016)
434
M o d el 203 Single Channel PeakSimple Data System
QuiCk llorl
STEP 5: Install Pea kS imple Chromato graphy Softwa re
5- 1. Locate your copy ofthe PeakSimple software, which is shipped insidethe frontcoverofyourSRlmanual. Insert theCDor floppy disk(s) into your computer's appropriate drive.
---_:.:n",,-.....,,
p .. .!idi
..-_,
5-2. Open the appropriate drive through My Comp ute r, th en double click on "Setac.exe"and follow the instructions.
_
.,,._..•, .." mO. ""~'"
5-3. Double-clickonthePcakSimplc icon to launch the program. Verify that communication has been established between your computer and the Model 203. An error message wi ll appear if communication is not established. 'tt y . .1
.,
... _.-.........
-'
'J
"-'k' 0. '
., ,
•
._--
_I
1'" _ _
:;;;.
~ ,.., ~
I"';';'
"'r-
"'-
r ~ '-~i>_
.l."' ••
'_"'.··"'H , ,..., .. /OO •. ==:J ~
"..--- ~...,,,-
~,
L~==============---~ ..:..
2ooc=l: ~ ~
f c.4:rz: Ji"1'iiii"" -.
"' .:.>--
~~
5-5. For the remote start option: Open the Editmenu and choose Cha nnels . Click on the Details button [or channel 1. Verify that Rp.mote star! is enabled (tilt box should be checked). :.r~ _ ."" JO r3 ;~q
......
"'"
=-- .-=- F" H ":s ,.. .)7-7"1:.
434 (of 550 ) 2006(-2016)
435
quick Slorl
Model 203 Single Channel Pea kS imple Data System
STEP 6: Starting an Analys is
6-1 . The upper right comer ofthe PeakSimple chromatogram window contains real-time information pertinent to youranalysisin progress. The status ofthe run(RUN, STANDBY) is displayed in capitallettersnext to the millivoltfmV) reading, underneath theamourrtoftimeinto the run.
f1Io ilil
v_
! ! _ 1IdI>
. .. iii s. '."
I"
L1 NO:Lc
~~
O ~~" :R : ~ ;/UNl .. ~ ..ooc
liON u~_
J
4
~
, ~g l§Z!1f4 : ,~-
j
0-'1 "
_ ., .. 11
.
~
I I
k
\
-u.xo'-- - - - - - - - - - - - - -- - - - - - -'
6-2. Hit yOW' computer keyboard spacebarto begin the run.. and the data isplotted onscreen in the chromatogram window.
6-3. Hitthe End key on yOU! computer keyboard to stop the run.
More on PeakSimple: This Quick Startguide presents a verybrief'Introduction to PeakSimple. There arc nn orials In the manual and
online at v..ww.srigc.com (click on the "Download OlIT Documents'; button) that will acquaint you with Pcekfiimple's basic functions. Ifyou have questions or problems., call SRI Ior free technical support &I 310-2 14-5092. Sam - SpmCalifornia time.
435 (of 550 ) 2006(-2016)
436
Chapter:
MODEL 203 DATA SYST EM HARDWARE
Topic:
Model 203 Hardware Orientat ion
The SR I Mod el 20 3 PeakSimple Chroatography Data System is a Single channel, ana log to dig ita l converter, controlled by our powerfu l PeakSimple Software. T he Model 203 may be used with any bra nd or model of HPLC or gas chromatog raph offering an ana log detector output signal. Th e Mode l 203 also features two independent, programmable controls 'Which can be used for temperature and press ure ramping or HPLC grad ient formation. There is also a Remote Start input that is compatible with two-wire switch clo sure signals typically output by GCs and LCs as a remote start sig nal. Eight TTL outputs (0 to 5 vo lts) fo r computer control of externa l ev ents come standard with the Modei 203. lf TTL outputs are not adequate l or your app lication, the Modei 203 ca n also be ordered with optional relay circuits offering normally op e n (N O) and normally clos ed (N e ) switch closures. POWER
• SRI
MODEL 203 PeakSimple
Chromatography Data System
Single C hannel Serial Port (Irent view) DC Powe r Input
15 vee
+
o -::>- -
Opening f or an analog s ignal cable and remote device connections
SRI Instruments, Inc. 67008 Paradise Road Las Vegas, NV 89119
(702 ) 361·2210
RS232 serial port connector
SERIAl. NUMBER
e ol_ I ~D £lATE
I
(FAX) 36 1·9690
I
(rear view) Th e Mod e l 203 comes with a bu ilt-in serial interface for connection to your de sktop or lapt op compute r's COM Port. (See the "PeakSimple For Windows " section in thi s manu al for minimum sys tem requirements.)
You should have received the l oliowing with your Mod el 203 purchase: (1) (1) (1) (1) (1)
Mode l 20 3 PeakSimple Chromatography Data System Box Serial Data Interface Cable lor connection to your computer's COM Port 15 Volt de Wall Tran sformer PeakSimple For Win dows software package PeakSimple Chromatography Data System Manual
436 (of 550 ) 2006(-2016)
437
Chapter: MODEL 20 3 DATA SYSTEM HARDWARE Topic:
Model 203 Installation Connections
To connect the Model 203 to your computer it will be necessary to access connection termin als inside the Model 203 Box. Verify that NO POWER is applied to the unit before performing the following procedure!! Remove the thumb screws on either side of the Model 203 Box and carefull y slide up the top cover and set it as ide. Figure 1. (below), depicts the layout of the Model 203 circuit boards and all wiring connections. To connect your system to the Model 203 Data System; please complete Steps 1 Through 6 as shown below and described on the following pages. S RI MO DEL 203 WIR ING DIAGRAM
STEP 4
1
~ -cc
STEP 2 /
•
....,•
·· , ·· , .. ··, ·, ·· , ·,
~
~
V
H
0 0 --
•
'"
f- ~
-
o
•
"
f-
~
•
0
•
l:S8l r.I3T C'OtO ~ !~
-~ ~
•••
~ ~
f- ~ ••
• f'0-
c
!?
•
0
f-
~
' I--
'0-
0
0
Ol
~ ~. >ef. ~
nay
eoHTACT Q,O.UlIU
n:: opno~a:..
~
o
I '"
I
.]~§~
44
' -
•
l1:
.,
<: i\
.:
STEP 3
Inst all I STEP 6 - PeakS imple For Win dows I software.
, FIGURE 1
I 437 (of 550 ) 2006(-2016)
438
Chapter: MODEL 203 DATA SYSTE M HARDWARE
Topic:
STEP 1:
Model 2 03 Installation Connections
Connecting the analog signal cab le: NOTE: The ana log outp ut from some GCs or Lcs can have a range of up to 10 volts dc. A lthough the Model 203 will allow high voltage inputs such as th is; be advised that signa ls above 6 volts will gene rate unwant ed noise and signa ls
above 5 volts will be "cli pped". (The tops of the waveforms will be cut off.) Route the analog signal cable from your instrument through the open hole in the back of the Model 203. Slop 1/4" of in sul ation off of the 'signal +' and 'signal-' wires of your signal cab le. Insert 'signal +' into the Lawson 203 board screw terminal marked 'sig +' and secure the connection USing a small screwdriver. Insert 'signal .: into the Lawson 203 board screw terminal marked 'sig -' and secure the connection using a small screwdriver.
STEP 2:
(OPTIONA L ) Connecting the remote start cable: NOTE: The Model 203 offers a remo te starting capability as a sta ndard feature. This permits the user to start the data system by means of a switch closure, such as a footswitch. In some applications, the chromatograph being used with the Model 203 may offer a remote start signal output or switch closure output that permits starting an integrator or other device when the 8TART button is pressed on the chromatograph's on-board control pane l. Typically, this sig nal can be used to start the Model 203.
Route the remote start cable from your instrument through the open hole in the back of the Mod el 2 03. Strip 1/4" of insulation off of the '+ ' and '-' wires of your remote start cab le. Insert '+' into the 203RLY board screw termin al marked 'IN' and secure the connection using a small screwdriver. Insert' -' into the 203RLY board screw term inal marked 'GND' and secure the connection using a small screwdriver. NOTE: Be sure to check the "Remote Start" box in the PealcS imple For W indows ED IT - CHANNELS - DETAILS screen for channel 1. Reter to the "PeakSimple For Windows" section of this manual.
STEP 3:
(OPTIONA L) Connecti ng t he external event relay wires: Th e Model 203 fe atures eight 0-5 volt TTL Level outputs that may be turn ed on and off individually and auto matically by means of a timed event tab le. M anu al control is a lso availab le via the keyboard. T hese outputs ma y be used to control external events or devices. If TTL level outputs are not adequate for your application, the Mo del 203 can be fitted with eight relay Circuits offering norma lly open (NO) and normally closed (NC) contact closures. NOTE: Re lay contact closures must be specifically requested at the time you orde r the Model 203.
438 (of 550 ) 2006(-2016)
439
Chapter: MODEL 203 DATA SYSTEM HARDWARE Topic:
STEP 3:
Mod el 203 Installation Connections
(Conti n u ed) Route the external event wir es from your instrument through the ope n hole in the back of the Mod el 203. Strip 1/4" of insulation off of each wire. Select wh ich device should be conn ected to events 'A' through 'H' and insert the wire into the appropria te screw terminal and secure the connection using a small screwdriver. Refer to the PeakSimple Software section of this man ual for sett ing up event tables, keyboard activation, etc.
STEP 4:
Connecting the Serial Data Interface cable to your computer: The Model 203 is equipped with a RS-232 serial port. A 08-9 type serial cable (provided) connects the Model 203 to your persona l computer through the PC's COM port. This simple interface permits the data system software to be loaded onto, and operated from, either a desktop or notebook PC for portability in fie ld operat ions. Secure one end of the Seria l Data Interface cable to an available COM port on the Back of your PC. Secure the other end to the DB~9 connecto r on the back of the Model 203. (Refer again to Figure 1 for location of the Seria l Data port.)
STEP 5:
Connecting power to the Mod el 203: Slide the top cover back onto the Model 203. Secure the cover with the two thumbscrews. The Model 203 req uires a minimum input of 14.8 V de to operate. 110 volt un its are provided with a 15 V de transformer which plugs into a standard 110 volt out let. To avoid damaging the unit; plug the transformer output plug into the back of the Model 203 first and THEN p lug the ma in transformer into the wall outlet. Verify that the POWER LED on the front of the Model 203 is lit.
STEP 6:
Installation of PeakSimple Software: Refer to the "PeakSimple For W indows" section of this manual for details on proper installation and operation.
203-.. S.lcw 01120/1.8
439 (of 550 ) 2006(-2016)
440
••
POWER SUPPLY "~"u ~ I lKl
GIfJ
15 · 2.0\ Vdt ' N ~ U T FRO"" WALLTRANSFORMER
to
to
DO~fm
LAWSOIf DOARO
UW S O ~
•
A
.t ,,'
' ll V
i I t_ _ •
,.
A
~e
l OCO'"
i .
'
e
1 .,,,,
,..
•• ALSO SUP PL!I!S 112 V AND GROUND
1 00 0u~
TO TIlE 203 NO flOARD
rc
'0
~WSO N
LAWSON
t"W50N
0 0 "110
8(JA RO
c
o
E
F
Re LAY
'"
" '"
~
" ~ N JMl I
Nt
R ~ L AY ~
••
~
~
1N3803
!l O CN e
0
n
._---,
,
I MOMENTARY GROUNniN G OF THE INPUT PROOUCES A 2 SECOND Nl; GATIIIE GOING PULSE ON THE OUTPUT Wille tl TRIGGERS rue 203 NO HOARD REMOTE S1ART FUNCTION,)
en
.n\,
1·"",
b "
~~
It~""y 7 _
10K
, •
" l H3lHl l
No e ll C
E
F
"
-, OPT IONAL RELAY CIRCUITS: USED WHEN A CONTACT CLOS URE IS NEEDE::D fOR ACTIVATION OF EXTERNAL DEVICES.
R" 10K
7
r"
r: : ~ en
+1ZV
n24
,..l
O1"F~
L:~LAY ~ ___
G
. uv 10M
~
I ON'}'
'10 CIf(;:
Rl1
T IMER
' 1211
NOC llt
u, '55
T
eW:
1
REMOTE START CIRC UIT
n
. 12V
f
1M
c
HUMID
lIo e lle
--'-'- -
+12V
R22
~
'i/
eUl
1." we ON
'11'"
~l~
2HUOJ
NO CIIC
•" '._,-
'"
LAY/SOt! OOA~O
"~
II. LAYI
, ~
ro
'0
,
· n ...
.1 2V
.,
~O C
I i
ro t
. I!V
2tuWGI
»c c
,.
1812 '-..-
DOM O
RElAY I
<0,
1 1
CI ~
D O~I\O
-t av
"'
~
8PAUU l~ ~
LAWSOII
~
Il&LMl
'
0 11
~.,",
Q1~ _
2N~)
1K
ON
-
cur
"' ..... "
I Pa ge 1 of 1 •
I
F lhlll~ rn o :
203rly.tcw
i
n ate: 1 ,, ~ v. b"I ~:
\ 440 (of 550 ) 2006(-2016)
441
Chapter:
INS TALLATION
Topic:
Serial Data System Hardware Orienta tion
All SR18610B and 86 lOC gas chromatographs are equ ipped with a built-in four-channel se rial data acquisition system. This system permits the acquisition of up to four analog signals in addition to providing control over the chromatograph's temperature, carrier gas pressure (if equipped with
electronic pressure control, also referred
to
as EPC), and event functions. :--10 additional interface
board is need ed , as is necessary when using the singl e-cha nnel expansion bus data acquisition boards in use with pre·I 995 SRI 8600 series gas chromatographs. All terminal connections previously found on the interface board are present on the serial interface board. Eight software-controlled relays provide external event control. The serial data acquisition system may be retrofit into early 8600 series gas chromatographs oa request Consult with SRJ sal es or technical sUPJXJrt for details. Th e SRI serial data acquisition syste m may be configured as an independent device. e xternal [0 the chro matograph. permitting the use o f a compact notebook or palmtop PC as the data system (via a serial port cable). L, this config uration (shown below), the serial interface is contained within a power supply-equipped protective case and may be used with any bran d or model of HPLC or gas chromatograph offering an analog detector output signal (0 - 5.0V). Both MS-OOS and Window!'> versions of PeakSimple software is provided with the serial interface unit and SRI GCs.
_eow. SR - _ . . .
PeakSimple Chromatography Data System
IIotOIIH20t
SRI Model 202 Serial data a<;qUisitioa unit in stand-akme case with llOVAC
Opening for analog signal cables, rem ote device connections 1M 1 1 "' ~ MF«nl
puwe1"
RS·232 serial
Optional switched AC power oerler
port connector
controlled by event control A
80111
38112 OEl..A MO Sl.lfD. 'roFlflA1'lC.l;, CAS05ail
El. IiCn OfllC
1:310)211'-5092
e Ol
1'Ql( 214-!;0!'l!
supply
PREasUR E
Main power switch
ow'Vf!:!!I @
'N@! Detail of rear panel of model 202 Serial data acqwsition unit
Every serial unit. whether installed in a SRI gas chromatugraph. or built into a stand-a lone external unit (sho wn above), is equipped with an RS -2 32 serial port. A DB-9 type serial cable (provided) connects the se rial data system to the PC through the PC's COM port. This simple interface permits the data system software to be loaded onto, and operated from either a desktop or notebook PC for portability in field operations. Connections to and from the GC or LC are routed through the opening provided on the rear of the serial data system unit, If the serial data system unit is equipped wi th an optional swi tched AC outlet, an external AC-powered device may be controlled by plugging it into the AC receptacle provided. The power to this receptacle is controlled by relay A. If the serial data system is equipped with the EPC option. two bulkhead connections will be found O P. the rear panel. Carrier gas is connected to EPC IN . and the pressure-controlled output is connected from EPC OUT to the GC injector carrier gas inlet Th e programmable EPC option is controlled by the data system.
441 (of 550 ) 2006(-2016)
442
Chapter:
INSTALLATION
Topic:
Serial Data System Hardware Orientation (continued)
...
o o
i
R~lay H
:;
,
u w
Rclay G Relay F
I.!l
o
o
Ou t-
o o0
0
Groo nd
0
" ' " '''''
:; :;
ribbon c.abk to RS- 23 2 connector
- -
S
g
-
I 11-12VOC OIl Grcen d
®
"t Rd., RelaYAB
&
1 9~l d
Roo stnpe on IDC
+ 12VDC lnrlIl
~
0
0 " •
", ".
{I
Slglllll GrOl..'tlJ Te"1' _ Prcgnom 2 TelT;'_ Program I Sig:Joll Ground
0
hlP~1
I
Relay E Relay 0 Relay C
<:I
DDD
I
Remote S"'rt 2 Re<':'XJl.e SlMl 1
1
.'
•
ru'• ,
0 0 0 0
-.
CHANN EL :.1
®
+ GD -
SRI Serial port data acquis ition system board terminals
0
0
Remot e start inputs (2)
.. '0
'0
Power supply area.
,
I
0
§J
_ _ _ _ _ _ _ _ _ .0 '0
0 Serial port data acquis ition hoa rd
I
Power supply terminals
.... / •• .•• ....•• ...••. .... •• ~
Signal interface T erminal Strip I
Externa l events Terminal Strip 2
0 1111! I I I j II]] I:::::;:::~
I!(I ll I f 11 1110
'0 '0 '0
'0 '0
So ftwa re-controlled relays A • H ----<
0
FROl\T OF PROTECTIVE CASE
0
'0
'0
0 1
0 n []
0 0
~
EPe circuit board (optional)
Location of SRi seria l port data acquisition boa rd inside stand-alone power supply case D,'.9fEPDOC ISFJW AT A1.E PD
0
0
iii
O[j~...
~ 0
The SRI serial data acquisition sys tem board, illustrated at left, may be installed directly into the chasssis of most SRI gas chromatographs, either at time of manufacture, or as a retrofit. This board permits the gas chromatograph to communicate bi-directionally with the data system via a standard RS-232 serial port , in addition to acquiring analog signal data from up to four detec tors simultaneously. The SRI model 202 serial data acquisition board replaces the earlier expansion bus-type data acquisition card supplied with early 8600 serie s gas chromatographs, and is included as standard equipment built into every full-featured SRl 8610B an d 8610C oc. The serial data acquisition hardware supports the external event relay convention implemented in early PeakSimple II software. Eight TT L level outputs on the serial data interface board are connected to eight relays found on the edge of the power supply circuit board. These softwarecontrolled relays permit automated or man ual control of external events and devices. Also found on the powe r supply circuit board are two separate remote start inputs, for the data sys tem main and alternate
control groups . Four analog signal inputs are available on serial interface board's terminal strip 2. All unused inputs must be connected to signal ground do not leave inputs "floating". RF,V O.12J -'I(,
442 (of 550 ) 2006(-2016)
443
C hapter:
INSTA LL ATIO N
Topic:
Serial Data System Hardware Orie ntation (continued)
,
,
<±J ·Eo Alrernate group _ _ . (J) M am group " "
'"•
Remote start input terminal strip
'0 ." ~ 'Eo ,,•
~" PO\\'c r supply
termma' Is
<. ."" 1"0 '0
+5
5. --::: + 12 •• / " " Grou
I~
.'0." ,• j'" u
Powe r su pply area
_0 :;
- Eo
_¢I
PROTE CflVE
Each e xternal even! relay offers three switch terminals: 1 common 1 normally open 1 normally cl osed
u
g
- G I~· -e ~
." u
COVER
- 0 :; .G ... _€I ~
_0
~ ~
- ¢ ...Q
Software-conrrolled. . / _0.9 g -e ~ relays A -H '0 - o:D g
-
-IS> C
. Eo
. . -------------0 ~
0'
Ex terna l events terminal strip
• ." u
ae 2
<±J
,
The SRl serial data sys tem's user-accessible connection terminals are located inside the stand-alone power supply case to the right of the covered power supply + l~ V
Relay signal from serial interface board / data system
--1
Terminal screw description Normally closed Common Normally open
0
0
°1 »> -~v'\l (II 1 - -
,0 (])
0-
--........
Relay screw terminal D.W6EPDOC\SERD.'\ TA3.EPD
All user-required connections available on the serial data acquisition system unit are located inside the unit's case , To access these connections. the two screws holding the cover plate of the serial unit in place. along with the cover plate, must be removed and set aside. With the front of the serial unit facing you, the power supply's metal protective cover is visible to the left interior of the chassis. The user-accessible screw terminal strip is exposed on the right edge of the power supply section . T he serial data system offers two independent timebases and control groups, for the control of two separate GCs or LCs, It also offers two remote stan inputs that are compatible with two-wire switch closure signals typically output by GCs and Le s as a remote start signal. To connect a remote start signal. locate inputs 1 (main group) and 2 (alternate group). Connect one wire to the G terminal (ground), and the second wire to the IN' terminal for the desired control group. The remote start capability should then be activated in the appropriate channel's PeakSimple Details screen. The serial data system is also equipped with eight electromechanical relays that are controlled by the PeakSimple data system, T he relays may be turned on and off individually and automatically by means of a timed event table, and manually by direct keyboard control. When a relay event is activated, the serial data system inter face board outputs a signal which is sent to the re lay dri ver circuitry in the power supply section . Each re lay offer s three connections for control versatility normally open, common, and nor mally closed. The diagram at le ft ill ustrates each relay' s knife switch-type operation.
Schematic diagram REV, Q.l-20-%
443 (of 550 ) 2006(-2016)
444
,
i
Cha p ter :
PEAKSlMPLE SERl"U. DATA SYSTEM INSTAL LA TION
Topic:
Serial Data System Diagnostic Procedure
,
I
i
,~ . --------------------------------~/
DC power inp'..It terminals from AC power suppiy
o
o
DO
1 , -----, SRI SERIAL PORT DATA ACQUISmON INTERFACE (LAWSON Model 202)
'----~l
r I -- - ,
!
!
All ueused cb:ume1 mputs should Temperature program be connected to circuit gecccd output.~ 1 and 2 are vie. wire jumpers as shown be low 100000ed here OD Tenniaal Strip 1. Ramp signal from data system is
meesured with Signal interface Terminal Strip 1
refereace to ground
{
Th~2
has
all
outpu1 ribbon cable IDC-I}7% plug that: must
be oriented
1!S
indicated above
I secced switch closure bcrweee Remote Start I or 2 and grouru' terminals is needed to start l'UL
and fi.rmJy seated on this 2O-pin
header.
~
0000000000
<:>
1rI. lll l l l l lh ~611A
Two yellow wires connect to ground and Relay A terminals for switched AC ou:let control
Be O!:F G H1R Z
SIgnal mterlace
TerminaJ strip 2
Test Procedure For The Serial Pert Interface Board 1. Verify that the software's DETAll.S screen shows the Lawson 202 selected as the AID board type (lower right corner of screen). Verify that the proper COM port number is entered in the PORT ADDRESS box (center left of screen). Do this for- each channel in use. Unused channel inputs should be jumpered to ground (as shown above left). 2. Check that the serial cab le is plugged into both the computer's appropriate COM port and the serial port interface's serial connector. Make sure that the RS-232 ribbon cable is properly connected to the 2G-pin header on the circuit board (see plug orientation above).
3. With the software running, connect a 1.5 VDC battery across the channel 1 + and - inputs. A signal of 1500 mV should be displayed on the screen. Connecting the detector should show a signal. 4. With a DC voltmeter, measure the voltage between TPI and ground on terminal strip 1. The reading should reflect l OmV per degree of default oven temperature, as entered in the DETAll..S screen (50°C = 500mV). This voltage should track a ramping temperature program (if loaded). 5. Plug a lamp or other load into the switched AC outlet on the GC or interface case. Toggling relay A should energize the load. The terminals A and ground should toggle between 0 VOC and 5 VOC. 6. By momentarily jumping terminals RS I and ground of terminal strip 2 with the REMOTE box clicked on in the DETAILS screen, the data system sho uld switch to R~'"NING from STANDBY. The system should not restart after the END key is pressed. If all tests are passed, system is OK. D:\EP2D:lCSlSEiUNsr4.EPD
REV. ()!(..15-94-
444 (of 550 ) 2006(-2016)
445
,~ -------------------------~" ~~
iI
Chapter:
MAINTENANCE
T opic:
Testing The Signal Input of The Serial Data System
\_---------------------------~ Th e SRI serial port data system is equipped with four channels of precision da ta acq uisition. In fact, the signal inputs available on the serial port data acquisition interface offer the precision of a digital voltmeter. Any 0 to 5VDC detector signal may be connected to anyone of the channel inputs. and the millivolt reading will be displayed on-screen. This reading should matc h the readings of any pr ecision meter connected to the same input. No special calibration of detector signal inputs is required.
If it does becomes necessary to verify the precision of the serially-interfaced signal inputs, the following procedure will permit easy confirmation. In order to confirm the precision of the signal inputs , temporary electrical connections are made at the serial port interface' s terminal strips. First, connect a wire from the temperature ramp output on the serial port interface labelled "TP l ", to the + (positive) terminal of an unused channel input. Then connect another wire from the ground terminal to the - (negative) terminal of the same channel input, as illustrated in the diagram below.
o +E)
B ,
o
0 0
o
{ Serial port data system interface board (Lawson 202)
D;m 7= ews
tS!
~ L.lLWl.lll.l..U "." " 0' 1 2 :3' q..L 1 2--L + 1+- + - +- __ Tll' "'7
""''' ' ' '
Relay outp uts
\
Remote start inputs
I
[jjjj]jjjjjJj
-,}~A B C 0 E F G H SI$2 is)
Make thes e connections to test the accura cy of the serially-interfaced data acquisition system Connect one wire from T P I to Ch. I ...;. terminal. Connect the ground te rminal to 0
0
the Ch. 1 - terminal Remember to disc onnect these temporary wires before returning the serial port interface back to se rvice
Whether the serial port interface board is built into the GC. or is installed in its own stand-alone case, these connections will permit the temperature program signal output by chan nel 1 to be fed back into the data acqu isition circuitry for channell . The temperature program signal o utputs l OmV for each degree. Whe n the two test jumper s are in place, an arti ficial signal is generated by loading the AREATEST. TEM file, included with the PeakSimple software, onto channell. When this temperature file has been loaded into the channel 1 temperature programming window, starti ng a run will send a ramped temperature program signal from TPI into the channel l + input. This signal is plotted, and the user will see that the on-screen readings matc h those of a reliable digital voltmeter, dO\NTl to the third decimal place .
D -\ Q ~EPlX)cS\SIGTfsro F.PO
445 (of 550 ) 2006(-2016)
446
{,-- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -
i
!
Chapter:
PEAKSIMPLE SERL'cL DATA SYSTEM L'ISTALLATION
Topi c:
Serial Da ta System Remote Start Operation
,
- -- - - - - - - -- - - - - - - - - - - - - - - ,I
,~ .
The SRl serial port data system offers a remote starting capability as a standard feature. This pe rmits the user to start the data system (and SRI gas chromatograph, if attached) by means of a switch closure, such as a footswirch. In some applications. such as when a different brand of gas chro matogra ph is being used with the serial data system, the chromatograph offers a remote start signal output. (or switch closure output) that permits starting an integrator or other de vice when the START button is pressed on the chromatograph's on-board control panel, Typically, this signal can be used to start the serial data system.
e
DO o
rr:
,...-,
~D fIl" -'
o
o
IUT'" -
~ 7<'f----'
A switch closare between termi:::l.a1 S1 me! GROlTh."D remote ly starts the clwmeis assigntld to the MA.ll'" comrol poa;:l_
A switch closure between terminal 52 and GROU}l.;'D remotely start!. the cbaaeels ass:i;ood to the ALr.::.RNATE COJ:nl'OJ grou;'J.
~
ill o A s=pIe ~ or pcshbunoc
_ ---'lI'---' Serial
JX)!t
---.
3-
- " 1--' - '
__
_. ._.. _. ;j
_
.
_
I
e
data system bncrface board (Lawson 202)
-~
-+
II
.... .
I - "- ~~ '"
.........
-.
_
~
...
_
0
-~-
_ _
0 0
. ...
~ '-. - -:=I --_.. --.:::: 3I '-~---. 0--
.. a - -._..
~_
C
...
_ .__.... _
..... _
_. ~
.[ j
,
1
·
)
[ -
)
. ..
ca _ _ _ _
C'a:DeQed as s:town in the diap-am. at left may be used. to provide the S'NiIcb "losu."'e required by the serial data sy501t,''tlJ
Once the hardware has been configured for operation, the PeakSimple program must be i..istructed to seek 2 remote start signal for the appropriate control group. This is selected from the
CO,,-rnOLS • CHANNELS - DETAILS screen for each channel in use. The REMOTE box located in the lower central portion of the screen should he "X'ed 011. As shown at left, the screen indicates th: selectica of the remote start feature for the MAIN = 1 group. The factory defaulted MAIN group channels are Ch, I and Ch. 2. By default. Ch .3 and Ch, 4 are set to the ALTER." iATE control group.
446 (of 550 ) 2006(-2016)
447
TO
13102: ...5097
·15W World Wide 1- Two Wire Universal Input
•r
-
P . 03
.
PSA-15W Low Profile Adaptor Series
.-.
: • Two Wire Operation
• <250~ Leakage
: • Zero Minimum Loads . •surn t'' Height
- ISO 9001 Quality System .. Extended Design Lite
~:J:*+r:i
.. Networking .. Notebooks
.. Periph erals and Terminals .. Portable Instruments
~"."'m"'l7Ji" 'D.tt·W, i • UL1 950 !E127643) ' • GSA 22.2 234 {LR56927-162j
.
• TUV leG950. EN6D950 !S96535S3j • Japan 91 -55156
~ Dimensions: ..Length: 11 Qmm (4.33in) • Width: ssmm (2.56in)
.. Height 25.4mm (1.Dln) • Weight: 200gm (Soz)
l·m!· lil~':i$ j,Si i[.m_ DC Ovtput 1 Voltage "/
Moael
PSA-15W·050 (pr I PSA-1 5W·120 IPr, .
,~\U l;em~ , ~~" ,ot
t 1) M".~~'eO' ~I
t.cac Mi l'l.
I
5V I OA 12V I OA
I I
"u
i
i
2.5A I 1.25A I
Ripp le (1)
I
~eglJla:ion
pop
I
line
5DmV
I
..2%
120mV
I
+1 %
~
I
Load
I
j
I :5% I
i
1.5%
I
cc C ~lP;>;
r;:J I I~J~ ~y lJ,S"'9 a 1 Z....I;~ .1'WlS(e~ ~,( 1,,,,,-'l,.d wl l ~ a l 0""0 ,~ ~Jei!o' ~"d ~ 0,1"'le {e'l"'"~ ;" :»;,all!'
TOT>=ll..
P.03
447 (of 550 ) 2006(-2016)
13102145CS7
TO
448
P . D?
i
ISO9001 • BABT Fac ility Approvals ,, I
........................ .............. .... ................ ................................ .
PSA-15W Low Profile Adaptor Series , '
[''':''It·;4tmet AC Input Voltag e
ACInrush Current (Cold , foil Load) 20A max (120VAC) 40A max (240VAC) AC Surge Immunity lEG 10~H-5 ; IEC801-5, Level 3
leakage Current Dielecuic Withstand (Hipol) 12msec.120VAC
DiD
-25 to .. 75:>::: MTBF
"
(fulllo' d. 240VAC. 25'C) Emissions FCCClass 8 I EN 500B1-1 : EN:55022 B Immunity I I EN 50082.1:IECiB01 .2 Levdl3 IEC,B01·3 Level Z IEC;801-4 LeV~i 2
less than 250.uA
zcmsec. 240VAC Overcurrent Protection
Storag eTemperature
100,000 nrs. mibimum
0 4Arms (120VAG) O.2Arms (24 0VAC)
Hol;-up Time (Full Load)
i
,!
0 to 50'C
AC Input Freq:lency 47 to 63Hz AC Input tnrrent (full Load)
300CVAC, 1 rnrn., l OmA
.
Operation Temperatu re
90 :0254 VAC
,, .,
.
15W World Wide - Two Wi re Universal input , .
AC Mating Co nnedor 1 Core. IECEN 60~20/G7 (2 wire! , DC Output Connect or : 2.1mm (10); 5 5f m (00) Coaxial Center Pos~!ive ...tancaro I
'
Short ::::ircutt, Auto Restart
ENTERPRISECO., lTD. 15. lane 530, Chung Cheng N. Rd. i Sanehung City, Taj~ej : Taiwal'l24103. R.O.C. Phone: B86-Z-98&-2126
Dimension Diag ra m
Un it : mm (inch)
I
886-2-980·5255 Fi!.X: S86-2-981-7085 : 885·2..g83-3222 J
PHIHONG USA :
Western O/tice:
i 374 S. 1i.i1pit2s B~.~ . j M~Pl!as. CA S5035
j Phone: .t'08·94S-7SS8 : Fax: 4Ce·S4&S0S3 Email: l/SasaleS@;::Ili.'1Cngus:il.CQm I r.:e m~:
,
h::P:tAw......_ phil:l~ g ~-sa _::or.:
. £zstem Office: : 3005 s-coeeae ~:I
Phone: (510) 865-9311 Fax; (610) 656-5920
448 (of 550 ) 2006(-2016)
449
The Re-Integ rate O pt io n Th e Re-integrate option is used to fu lly re-integra te a baseline in PeakSimple. W he:1 chang es are made to a baseline often a partial integration will occu r, selecting Re-i ntegrate w ill pe rfo rm a full integration on the baseline. The Re-integrate opt ion can be selected by clicking on Edit in the PeakSimpl e menu bar and then Re-integrate from the list of options .
I
The View-Res ults Wi nd ow Th e Results window displays the resu lts of the ch romatogram runs performed in PeakSimpie . T he Resu lts window is opened up by clicking on View in the PeakSlmp Je menu bar and then sele cting Res ults from the list of options. T he Chann el opt ion serellbar specifies wh ich of the fo ur chan nels the res ults data should be displayed fo r. When the Reco gnized pea ks o nl y checkbox is selected on ly the results for named peaks w ill be displayed . The Undetected compo n ents a lso checkbox display s the results for the undetected components as we ll as the detected co mponents in the chromato gram run when the option is selected .
Qwndl
FS
Ct-.aTldl Ch.Yn:rJ Ch.:n-leI ~ :.,ir,:!OOI:l
Fl O =-1 1 F12 =-6
Re.'rem
Ern""
, . _..:.0-
Updat e The Update button in the Results window updates the DOE link between the Results data and the DOE host prog ram (typically Exce l). Save
p "",...
... ~ ':rf '
::i ."''' --' ' ~ l'''-'''< M ,j. - "..
:I "'".' c.....,
Selecting the Sa ve button in the results w ind ow open s up the Sa ve results f ile window . In the Save resul ts file window the results file is saved w ith a .res extension. The file is an ASCII file an d not the raw chrom atogram data .
::1' _
;! ,"" .::o"
~
~=
:::!!~ 15"":'-;:
a ~~
~ . ~..,
- ;0::".
-"' _bl _Ot'
.
~ .-ac:o.. . .""" "" ",
Integration As a co nve nience the integrati on butto n in the res ults wmdow ope r s up the same lnteqratic n window that can be accessed in the Ch ann els window . For more information on the Integ ration .......indow cons ult the Cha nnels-Integra tion po rtion of th is manual.
"
r Po.oo, ~ --l -»~~ - !:i_ ""''' ~ 1 ,
f u;:: ls; oo .li: ,. .-: i:"""
~ ~_""' f~;; XI ~
I" 1" 2
I" J
~."~""', ro :xr. ' _'~l l :n;;
'r
•
L_
I
- - I'
!' ""
r ,
r
Il~_ ~ ~
s~ .......t .ox
PeakNTdx-13.pub
449 (of 550 ) 2006(-2016)
450
The Vi ew -Results Window (cont.)
;' W . ij J2&
.I
Fo rmat Se iecting the Format butto n in the Res ults window open s up the Edit fo rmat window. The Ed it form at window allows the user to specify the ir.for mation that is to be incl uded in the Results tab le. The A va i lable optio ns box in the Edit format window d isp lays all the ava ilable opt ions that can be included in the results but that aren't selected . A n optio n is added to the Selec ted option s box by high lighting the item in the Available box and click ing on the righ t facing arrow butto n. To dese lect an option from the Selected box high light the item and click on the left fac ing arrow button . The Dec. pl aces dialogu e box spe cifies how many decima l places a highlighted unit will disp lay in the Results ta ble.
-
I·"
.-
~" --£j}
9}
i •
If.::::-
r-
-
*:
2J
-.-.. '. '
r .......• _
_
t ",_ ~ · r
.11: :
,.....
]m
' ''~ - '
C lose
mo... ::;;:',.;.
.,
[..-
- -
......... .1 ... . _ .. 1. ]
·=--....... 1
<- -.to.. r'
j
~
I
~ ,,' =:....II
- 5 'i
j ::r ~.li<.:
r....,
The Clo se button exits t he Results window and returns the user to the main screen.
/oJ_
.s !
EI W\tlI: 0.51G .1:&::3. :;';2
r. [UTro:i
r i..:rr
Calibrate
r .:: ::.-r r: ~ :11:.1:"
T he Calibrate butto n recalibrate s a recognized peak in the Results table. Highlighting a pea k nam e and selecrlnq th e Calibrate button op en s up the Recalibration Leve l window. T he window specifies which peak level sho uld be cali brated . Fo llowing the Re calibration level windo w IS the Calibration win dow which is discussed at further length in the Calibrati on section of th is d ocument.
~ ."';
r
~
I
r- ,:jCX'
CO
- ria".•
-
S;U ,rem .= .,..
;
= ,= ;." k"""
: ~ I"'"
t ~';·
< "'-""
... .,.." .
~ "',] !Y<>
!li'"
jO , r. i'F.f='~ ;s. ~'%l i .... Ib :, it "
.. ,..
"'- IU _ ~' "
i.rn< ~
. .
•• •
~
.
'
,-""
-~.'
, ~ I'f l
Pclm
~
,
=, - ·· 1
I . U.
-"::=-1
.: ,. CoI_ "
.... - ,......."."X-"
---
--"-to ..... ~ ,~ 1 ........
".
,
, ~
-.
""''' ' --
,
~
I,
",
.
lJiiO:ll'C
I
r' ".
I
I .r ... ..
0..;.,
,-" ""
--,..
1
Ca li brate All The Calibrate all button recalibrates at! the recogn ized peaks at once. T he Cali bra te aUbutton calibrates at! peaks with existing calibration curves on a pa rticular calibration revel. If named peaks a re in the res ults table without calibration curves an error message; (NOT ENOUGH DATA POIN TS ) w ill be displayed . The ca librat ion will
~
cr: c=;
r
,-,. ! ,I
-...- I ~
_
. . .....
::o . ~
. 0
:-
,
PeakNTcoe-r 01 pub
450 (of 550 ) 2006(-2016)
451
The Vi ew -Results Window (cont.) Copy The Copy button in the results window copies the results report to th e Clipboard. Once the repo rt is cop ied it can be pasted into ot her program s i.e , Exce l. Copy Resu lts L o g
T he Copy results log button copi es the .Iog f ile for the re sults to the Clipboard . T his log file can :>8 pasted into any W indows program . A certain numbe r of lines in the res ults log w ill always be copied , by defaul t the number is 20 . If more th an 20 lines are needed for an ap plication the user m ust modify the pea kwi n.ini file located in the VVindows folde r. The default entry in the file is ( SpareLines=2 0 ), delete th e nu mber 20 and insert the number of lines that are needed (up to a maximum of 100).
Clear Results l og Clicking on the Clear results log burton e rases the results log tHe .
Show Resu lts log
---
.._" ....._ ......,._.. . ..._ ,-'''' ..,..... - .... _.. :::~ ~ ~ -
" ..... ~. _ :
....•....,...
.
u. ~
""
.
'. ~ .-
,-
",-
T he Show results log button when selected op ens up Wind ows Notepad to view th e resu lts log. Add to Results Log
To add the current report to the resu lts log click the Add to results log button. The rep ort can autom attcany be added to the results leg at the en d of each chromatog ram run by checking t he Add to res ults log checkbo x in the Postrun w in dow .
.•.
PeakNTdcc-15.pub
451 (of 550 ) 2006(-2016)
452
Th e View-Relay/Pum p Wind ow
;QiC'tltlttftt,
l
, ~ Sil." ~N l fJN/O~
The Relay/p ump window manually controls the actions of the re lays in PeakSimple . Th e Re lay/ pump window is opened up by ope nin g th e View me nu and then se lecting Re lay/pump win dow from the list of options.
• B
~ iEl
T.'''''BAYHm '''.T
I C TRAP;:2HEAT
Sele ctinglDeselect ing a Relay To mam.:ally activate a rel ay cl ick on the letter next to the re lay label to make the button dark. To dea ctivate a relay select the specified lettered button to turn it black. Press ing the co ntrol button and the letter corre spo nd ing to the re lay together also selects/deselec ts the relay.
xl
iD
'IrA"W- Si"A'\ER
-
SPA.=l G;:: GAS C'~IJFf
~
TRAP:!:1"'EAT
:; I VALVE!;1 lOAOJlNJECT~'
H 'J.:..LVE::2LOtJ).INJ; CT
~r,petd:
1'"'"3""'" II
" 1 ,: -
.'
>.:._ ;y ' .
P um p Spe ed When an SRI H PLC pump is co nnected to th e data system the pump speed can be con trolled in the Relay /pu mp window. To change the pump speed click on the arrow icons to increase or decrease the pump speed . The pump speed ca n also be entered by highlightin g the value in the box and typing in the new numb er.
y ~~ - (tt~ :> ~ 2:!:...J ~~ ~
~~
Describing a Relay To labe l a re lay in the Relay/pump wi ndow right click on the m ain scree n and se lect Eve nts from the list of options. Once the Events window is opene d up click ing on the Des cri be bu tton opens up the Event description wind ow. To ente r a relay description click on the specified re lay's d ialogue box and ty pe in the information . T he descript ion of the relays has no effe ct on the relay function and will not affe ct hardwa re.
e.
I ~ "'U T VENT or;IO"F
;: I T~ "-" !lo'J- £ 5r; ~ ,a , l i ~.Af'~ ~ [ ..I . Q;
f.-Q«,'\;.L 5t-..;.~E
g j5~ARG~ se D~ !O~
e IriO<>_:>::: hEAl .tH"'" .\f" ~l .~ , 1U. £C7 !::!: f;'.<..J.'~ r ~2 LC.:.D.tlJ;::T
-" PeakNTdoc-1 6 pUb
452 (of 550 ) 2006(-2016)
453
Th e View-A utosampler Win dow T he Autcsarr.p ler wi ndow aHows a list of control files to be run automatically. Control f iles are the ma ster files which specify all parameters including tempe rature pro gramming, component. and event files. T h ese control file s run tasks in PeakSimple. To open up the Autosa mpler window click on the View m enu in the me nu bar and then select Autosam pl er f rom the ava ilable opti ons.
S la rt/Slo p Th e Start button when pressed be gins the op eration of the a utosarnpler queue or rep rocess ing queue . A queue must be created or loaded before th e co n tro l files can run. On ce the autosamp Jer is in op erat io n the Start button changes into the Stop butto n. The Stop bu tton ceases the autasamp ler operations that w ere p rev iously runnin g.
Batch Reprocess in g M od e To se lect Batch reprocessing mode cl ick on the check bo x to the options left . Whi le using the Batch reproc ess ing m ode the user loads a list of previously stored chromatog ram file s in th e list box to t he left and the n se lect s a c ont rol fi le which w ill reprocess the data fil es. When the operation beg ins PeakSi mple will load each data file in th e list into cha nnel 1, perform the specified functions. and then increment to th e next da ta fife in the list. T he S tart at dialogue box sp ecifies whlch control fife number to beg in operation at first. If no nu mber is e ntered the autosamp ler will begin at the first control fi le. The Sto p at d ialogue box specifies th e last cont rol file to be run befo re operati ons of the autosa mp fer c ease. If no num ber is ente red in the dia log ue box the autosampler will end after the last control fi le in the list is ru n. Th e Delay " x" m inutes radio button when se lected sp ecifies ho w' many minutes PeakS im ple w ill w ait be fore running the next control file in the list box . The W ait fo r rem ot e s t art radio button when se lected instructs the autos amplor to wait fo r a remote start sign al before advancing to the next control fil e. T he Resta rt at end checkbox restarts the que ue after ge ttin g to the end of the control fi les in the list box. In the " x " t imes :he user ente rs the number of tim es the control fi les in the list b ox s ho uld be cyc led if the Rcs tert ar And checkbox is selected . If the value 0 is selected the queue wi ll be cycled con tin uou sly. C lose T he Clo se butto n clos es the Autosa rnpler win dow when it is selected .
Dose
PeakNTdcc -17.pub
453 (of 550 ) 2006(-2016)
454
The View-A utosampler Window (co nt.) Add...
Add
Seiect the Add button to add a control file to the queue. Selecting the button ope ns up the Select contro l file window where the file can be loaded into the Jist box. Each control file in the queue must have a diffe rent name even tho ugh almo st identical actions are pe rformed .
Add Multip le/ Bat ch Reprocessing
ledd 1JJ.Jt~ __
T he Add m ultiple button allows the use r to load multiple data files into the Jist box . Click on the button 10 open up the Select control file window and the n click on a con trol file name to open up the Se lect data filenames win dow. Se lect as many da ta f iles as needed by pres sing the sh ift button and clicki ng with the mouse curs or and then click on OK to load them into the queue . The Add multiple button is on ly us eful fo r use with the Batc h rep rocessing mode . D elete
F.. r ......
E_
ll!t
~"'""'
=c
~'" SOol.Y!' !:U l>'f' 6(;· .C>P
..
.....: '
,"' ~
jf ....~ ...·.DTI j
r
eo "l;,,;s~
~ I> ~
<:12 o. R . 1 iJ"R
~
:lO:u
::J r&.=
<-
..
I "'" '1
.
.oJ
~
J
:=I "-- I
j
Delete
After h ig hlighting a co ntrol fi le in the list box to the left select the Delete button to remove that co ntrol file f rom the queue . Load Select the Loa d button to open up a previous ly saved que ue file. Click ing o n the Load button opens up the Load autos ampler queue window w here the qu eue file ca n be selected and loaded .
S a ve
se ve...
Selecting the Save butto n open s up the Save autosarnp te r qu eue w indow . Sav e th e que ue in the fil e box by na ming the file and selectin g save . It is recommended that at! files be saved to the PeakSim ple directory.
I
~
=1
Clear The Clear button erase s the entire qu eue. Pea<'NTdoc- 18.put
454 (of 550 ) 2006(-2016)
455
Th e View-Autos ampler Window (cont.)
Eoc..
Ed it
After highlighting a control file select the Ed it button to modify that con trol file. Selecting the Edit button loads the contro l file on the Peak Simp le main screen. To make any changes click on the ma in sc reen, do all modification s, and th en select Save all from the PeakSimple file menu .
I
Ed it A ll
Etit aJ ..
To edit all the con trol files in the queue at once click on the Edit all butt on to open up the Au tosamp ler q ueue spre ads heet. Many of the comm on ly adj usted contr ol file paramete rs a re displayed in the spread sh eet enabling the use r to in put ch an ges to the queue. Not all c ontrol file paramete rs ca n be modifie d using Edit all (only t he pa ram eters that are se lected in Form at) and so mu st be done individ ually with th e Edit function .
A utosamp le r Queue Win dow
""",....>eo..- ' ..... _ ''... <'0
Clo se
...,::-", _ _ .. - '.'"
_ceo .... ,...
The Clos e button exits the window after promptJng the user to sav e the sp readsheet.
.,''''...', ,...... . .
_ ~c""!
~"'"
'
... ,
__
.. .
•
. .
Ca nc e l The Can cel button exits th e spreadsheet w indow without prompting the user to save. Add
I ACL i
Selecting the Add button opens up the Select control fi le w indow where an ex isting control file can be ad ded to the q ueue . A d d Copies After highligh ting a control file in the spreadsheet se lect the Ad d co pies button to add cop ies of the file to the list. Once the Add cop ies w indow pops up input th e numbe r of copies to be made in the dia log ue box and spe cify wh ether the file names should be incremented. The Add co pies button is usefu l for creati ng a queue from scratch with a sing le control file .
~ .~-,' ·" dS7~··
1:7
~I
~
tncrerr:er:I ±.fa I~enarr.e tsr each copy
OK
C ~I
I
I
Pe<:lk NTd:)C-19.pub
455 (of 550 ) 2006(-2016)
456
Autosampler Queue Window (co nt .) Delete The Delete button de letes a highlighted control file off the list. If no file is high lighted then the last file will be deleted from the queue .
t-f~··
Fill
The Fill button fills a spreadsheet col um n, row, or cell with selected text. Once the desired cells ar e hig hlighted clicking the Fill bunon opens up the Fill autosam pler options box . Input the text to fill in the informati on fiel d and spec ify whether the text should be incremented fo r each
row. Update Co ntrol Files
I .!.!pd~e conuol fil~s:
j
Iext to I~III
I
Caned I ~~
OK
J
Selectin g the Update control files bu tton sa ves all changes to the control files in the list.
Pri nt
p"~
1
The Print button prints the queue spreadsheet. Fo rm at
I formal.. I
To ch ange the format of the q ueue spreadsheet and open up the Edit format window select th e Format button. In the Edit for mat wind ow a fo rmat type can be added by selecting it in the Avail able wind ow and then hitting the right facing arrow button . To remo ve a form at type f rom being disp lay ed in the spreadsheet highlight the format type in the Selected box and click on the left facing arrow.
Load Now
2!J
~.-
::-
!V~ '"
IoU ,-
~ ,-
'"'"'
--
(,.... v CI>'OCIicf> 0'- . t;oco;; lo-"e ~.
'"'~
........ ~
(po.,.,
,_"C] ~
~ ,It
~
1.""" r.. 1""0'';'' 0 100 , ~< J~_
r'I :='1. . . .,.r :
"" r, rJ
0
"'"'I
I
After highlighting a control file select the Load now button to lead that control fi le to the main Peak Simple screen. Click on the sc ree n and ma ke any changes to the centro l file and then select Save all to save the Ch anges.
Pea1<.NTdOC-20.pUb
456 (of 550 ) 2006(-2016)
457
The View -Chan nel " X" Options T o view' a spe cified chromatcgra m ch an ne l c pen the View menu in the PeakSim ple menuba r a nd select a channe l to be viewed ; either 1,2, 3, or 4 . Keyboard shortcu ts can alsc be used to alternate viewing between chromato gram channels. Hitting F9 displays chan nel 1. F 10 displays channel 2. F11 displays channe l 3, and F12 d isplays channel 4. Furthe rmore the numerical icons in the PeakS un pte too lbar can be used to tog gle between chrom atogram ch annels .
.. ,.• -•
.
~"
-
~
~' " F ""
Unzoom To unzoorn from a close up view of a chromatogram select the Unzoarn tool from the View menu o r hit F5. PeakSimp Ie w ill ZOO:11 out to the f irst level with the soriginal d isplay units of the chromatogram when the Unzoom too l is used. The Unzo arn button in the PeakSimple toolbar ca n also be used to unzoom a chromato gra m or F6 on the keyboard .
"
"-'"
~
'--- -- t . y o . ~ .
,.,. • • •
Refresh The Refresh tool in the View menu re· draws th e chromatogram screen to fix any glitches or resolve an error. Pressing Enter o n the keyboard also refreshes the screen.
I ,...
,
~
:
..
1
, ~
j
The Help Menu
,""
Abo u t Pea kNT
T o view pr oqrarn information about PeakSimp le click on the About PeakNT opti on in the Help menu. The PeakNT window will pop up and display the information.
S ho w Too ltips
I,':: :l version 2.74[MSI
Del 32001 lei C~I' 'J1t 199' -2WJAWl ;, ;;>,he' i">gton
The Show tooltips option in the Help menu toggles the PeakS imp le tooltips off or on. W he n Show too mos ;~ checked a he lpful tex t tip wi ll appear whe n the mouse cursor IS held over a too ! or button in PeakSimpIe. The tooltips provi de relevant inform ation to the operatio n and use of the PeakSimp le da ta system. P'?akNTo cc -z t .pco
457 (of 550 ) 2006(-2016)
458
The Acquisiti on Menu The Acqu isition menu contai ns the comm ands to run a chromatogram run whe n hardwa re is connected to the PeakS imp le data system . All Acquisitio n menu comm ands have correspo nding keyboard hotkeys for con venience. '. -
Ru n
.
/~ No aclNechi)l'YlC1s ingrc~p
The Run command beg ins a ch romatogra m run on the main trigger group when hardware is conn ected to the data system. The error message ~ N o active channe ls in I ~~ ~I qrc up" appe ars ~vhen no hardware is available to make a t __ ()K: chromatograph run. The spacebar ca n a lso be us ed to start a run.
Ii
Sto p The Stop command is used to end a chromatogram run once it has been started . Using the Stop command ends the chromatogram run withcut running any of the Postrun operatio ns. The End butto n can also stop a chroma tog ram run. St op+Pos tru n The Stop+Postrun command e nds a chromatogram run and executes the operations specified in the Post run scree n. Holding the Con tro l button and pressing End on the keyboard is the same as the Stop....Postrun co mm and. A lt
The Att m enu in the Acquisition menu controls the acquisition commands for the alternate trigger group . Th e + button be gins the alternat e trigger chrom atogram run, the - button stops the alterna te triqqer run, and t he I button on the keyboa rd stops the run a nd begins the Postrun operations fo r the altern ate trigger gro up .
Re-initia lize The Re-initia fize comma nd reestablishes the co nnection between the hardware and the PeakSimple data system. A connec tion be tween hardware and the data system has to exist for re-in itializa tion to occur.
?eakNTdoc-22 .pub
458 (of 550 ) 2006(-2016)
459
Loopback Test: For Data Validation
-
A loopback test may be performed if you are required to validate the precision of the G.C. or Data System's analog to digital conversion. This test requires the user to install a jumper wire on the AID board inside the G.C. or Data System. Description of Test: A jumper wire is installed on the AID board between 'temperature program one', (TP1) , and 'channel one signal input', (Sig. 1+). A data file is then loaded into channel four. When the 'Ioopback' mode is selected in PeakSimple, the data on channel four is
routed out TP1 to the channel one signal input. When a chromatogram run is started, channel one will begin to reproduce the data loaded into channel four. After the run has completed, area counts from a specific data peak may be collected and the run repeated
several times. After at least three runs, the user may then calculate the average area coun ts and the percent relative standard deviation,(%RSD) and thus the precision of the AID converter. Less than 0.5% RSD is typical for the SRI Model 202 and 203 AiD boards . Setting Up The Hardware: With the G .C . unplugged, remove the six screws securing the bottom cover. Flip the G.C. on its back and locate the AiD board on the right-hand side. Remove any wires from
TP1' and 'SIG 1+' and add an insulated 22 AWG wire between TP1 and SIG 1. Refer to the diagram below for jumper placement.
Most systems will FOUR CHANNEL LAWSON 202 BOARD
contain the Four
Channel 202 Board . Also, verify that SIG 1is grounded. Add
~
DoO,TA~
c - . ...... (tv....Tl OW
. , .
•
''''-':1IClN'O
=.: ...... c..........
another jumper if
1·· ········· · 1 ** A. CO. ' CM .... ....
needed . Some systems will contain the Single
Channel 203 Board . Also, verify that SIG 1is grounded. Add another jumper if needed.
ADDAJUIiPERfROIITI'"! TO $lG 1. AND Vl'RIl'Y SG '.IS GROUNDED
SINGLE CHANNEL LAWSON 203 BOARD ~
DoO,'AI"OlI1" ' _ ~ "- TO
,-----,-' You could also run the
TP1 wire to SIG 1+ through a reiay for automatic hardware se tup.
]······· ·1
AOO ... JU-WPER fROII TP1 TO SIG,. AND ~EIlIN SIG 1.1S GROUNDED
459 (of 550 ) 2006(-2016)
460
Loopback Test: (continued)
Selting Up The Software: Re-attach the bottom cover and plug the G.G. back in. Tum the G.G. power on and start PeakSimple. Verify that the computer is communicating properly with the G.G.. In the EDIT·OVERALL screen, check the LOOPBACK box. Set the START TIME to 0 minutes and the END TIME to 10 minutes. Also verify that the SHOW RETENTION WINDOWS box is checked . In the EDIT-CHANNELS screen, check the ACTIVE, DISPLAY and INTEGRATE boxes for channel l . And check the DISPLAY and INTEGRATE
I!! ~aIcSiorf>Oo for WrdQws ~
1"' , ~
~
..sM!~
l:I'il' _
~ Le:~.! ...... =t~~o~ : U!' ,
.. i_. _ _. .._ =.
"~
'''~='~'::'r~''-'n~~j.J1I' . , Il' _
_
.. _ ......
:~
__
~ .:J I;;gllr;::::" _
.,;_,if~
o;.;;,;"
..,;·_L
"
. .......... .-.;~~j ; "
, I ' .~
:. ::.:.:.::-,~
.. ,_:",,: ,:::-,..
_ ..... ~ . ". ", ..
':::~.,"::,~":.:: ..
,, :-
l. " '~ I ::.
.... ,..._ _m__..'-::
';'1" 1x l
boxes for channel 4.
In the EDIT-CHANNEL 1DETAILS screen, set the END TIME to 10 min. Set the SAMPLE RATE to 1. Set the DEFAULT DISPLAY LIMITS 10 256 MAX and -25.6 MIN. Set the TRIGGER GROUP to MAIN. Glick OK to close the DETAILS screen. Then repeat for CHANNEL 4-DETAILS. In the EDIT-CHANNEL 1INTEGRATION screen, set the AREA REJECT to 100. Set the PEAK DETECTION SENSITIVITY to 'PEAK=95%, BASELlNE= 60%'. Set the SPIKE CHANNEL=NONE. STANDARD WElGHT=l . SAMPLE WEIGHT=1. and make sure the TANGENT DETECTION BOX is UNCHECKED. Glick OK to close the INTEGRATION screen . Then repeat for CHANNEL 4--INTEGRATION.
•
.
1--------1
'..
.u.
460 (of 550 ) 2006(-2016)
461
Loopback Test: (continued) Software Setup: (continued) In the EDIT-CHANNEL 1· COMPONENTS·LOAD screen, highlight the 602.cpt sample compo nents file and ciick OPEN. Click OK again to close the COMPONENTS screen . Then repeat for CHANNEL 4-COMPONENTS.
~
3 ~ '" "'!!I L.
-
In the FILE-oPEN screen. select CHANNEL 4 at the bottom of the window and then highlight the 602.chr sample chromatogram fi le and select OPEN. Th e 602.chr sample chromatogram that is now disp layed on chann el four represents the da ta that will be fed back through the AID converter.
!!! P"
,kSlnlpl8 for - ...-..
. .'
..
.--
Load c:hro..atogl'iIJI'l file
I.ooi.';" " :,j<:::l_
Starting the Run: Au to-zero channel 1 by clicking the 'Z' button. Depress the SPACEBAR and the chromatogram will start running. The data on CHANNEL 1 should appear to be an exact replica of the data that was fed into CHANNEL 4.
IE': f3:-
~_
"-
...
...
-----
..
,.
'''':''': ....h1!I..!U
T'I"I
,
dB
6:f!'iw",-
.........c:.,'jWdV
.....
f!Ih'l'~ (H0 1 ~: ~..:...q " 1 .. .
,- ~
..
,!-.:,.;,;...::::::... ...:..-....,.;.;.:-:: .. ... - -- --'---":::
:3
-.,--..
~..
Collecting the Data:
. ..
fl!~ .. ~':*'..X..." . ~.~ ...~ " " ..._ , ., ............
CEJ
:' :-:r - -I
•••••••••
.~.L~:l!l.l)) "0 ·< '4?';.;;;:;.,t"' U ~~~,;~ ~~_~m H1 ~-;;-~-; ~t~
• • •
:
•
--:
-
1....
After the run has completed, make note of the area cou nts of one of the pea ks by left-cl icking on one of the peaks. Toluene, for example. may have an area cou nt of 931. Repeat the run three or more times; for each run, record the area counts of the same pea k. Once the data ha s been co llected from at least three runs; an average area w unt can be calcu lated as well as the percent relative standa rd deviation.
461 (of 550 ) 2006(-2016)
462
Loopback Test: (continued) Calculate the Standard Deviation: Using the data collected, calculate the average area counts for Toluene. Typically this value is around 950. Then calculate the %RSD which is usually less than 0.5%. You may notice that there is a sma ll magn itude of error between the CHANNEL 1 and CHANNEL 4 area counts. This is due to the DIA converter and not the NO converter. Since the loopback test measures the PRECISION of the NO converter and not its ACCURACY, this minor discrepancy is insignificant
Save Your Loopback Test as a CONTROL FILE:
If you wish to run this test again or if you continue with the next step and modify the Peakwin.ini fiie, you will need to save the loopback parameters as a CONTROL FILE. In the FILE·SAVE CONTROL FILE screen, type in loopback.con and click OK.
e ,,-~ I;-. _ ~
-.
....-
......_
'S,M .,;,,:;,:.:......
~,
--
-....
•
-- ............
.
.. CEJ
--
:...._ j:MM<... :"""..
C ' _AV.' ~ .3 , ~
n+ l • __ •
: :!J.J.:i -.---
: ~~
.liE ::I :£1 .i:t1 fi'ifr
tu _
~g='-
. , .-
_..'"..... -...-.-
r~
."
'""~ "~'\. rUIoO ,
..-
~~tt::ri i~b i:tki ; i<~~\£ , ,c"ik-.s"_ ~l -
-
. -
Modifying the Peakwin.ini File, (optional)
ff desired, any inaccuracy of the D/A converter can be adjusted by attenuating the LOOPBACK OUTPUT to match the input signal. This adjustment can be made by entering the line "LoopbackFactor=X" in the [Lawson] section of the PEAKWIN.lNI file located in the WINDOWS directory. The default val ue of 'X' is 0.098. NOTE: Changes to the Peakwin.ini file will not be recognized unless the PeakSimple application is restarted. After you have obtained the average area count for Toluene on CHANNEL 1, exit PeakSimple by pressing 'Q', then 'Y'.
To calculate the new value for IX', first detennine the average area counts of a specific peak for CHANNEL 1 and a lso determine the area count of the corresponding peak on CHANNEL 4. Next, divide the CHANNEL 4 area count by the CHANNEL 1 area count. Multiply this rat io by 0.098. Substitute th is new value for 'X'. For example, using 602 .chr as the chromatogram file , the to luene area count for CHANNEL 4 is 953. If the average area count of tol uene on CHANNEL 1 is 931 then the ratio would be 953/931 = 1.0236. Multiply 1.0236 x 0.098. the answer is 0.1003129. Round th is new value for 'X' to 0.1003.
462 (of 550 ) 2006(-2016)
463
Loopback Test: (continued) Modifying the Peakwin.ini File. (continued) Find the PEAKWIN.lNI file in the WINDOWS sub-diredory. Double-click to open it. Scroll down until you find the [Lawson] section. Place the cursor at the last line of the [Lawson) section and type "LoopbackFactor=X" , and then press ENTER. X is the value you calculated earlier. For example "LoopbackFactor=O.1003".
[Statistics] R2lnciudlilZIllI'"O;O
II
Q=exc ludp 1:include cha nges r-sq statistic ,-,-.
[Lawson] Debug-.,
DH- ~i tes la wsonXX.er r on fa ilure serial data 5trea ~ to disk-large files
debug· 1 f or
1-write 1 = single-channel hi gh speed data ~ d e enabled Hz. O-calculated internally for best re solution IJz no auerag ing 2 sets internal AID filter cutoff - 1100 nz sees . o-ealculated internally 8-no 1-yes cal1brab dur ing sign-on sequence OD-FF i n hexadeciaal sets TTL logic state
DebugRead-O
SingleChannel-lJ SalllpIl!'Aatl!'- 0
Auerage-1 Filter-2
Inter-tln-a CaUbrate-1 ReiaySenslil-IU' BaudRate-1 ]i.-out-SUIU' HaxCount"'1
1=960'1
1-u: ng
2 =2'-011 3=1200 " =600 5 =3 0 0
' ~:
[ U
B
l,
rr: H:
jf
E:
llri ll i s ees before autolllilitie restart. II for neuer t: Any Ualue sets te .p prog to . 11 degree r es ol ut i on g ~ no edge trigge r 1- positiue edge 2- neg. edge ~ Sets AID board gain Sets l i ne freq for Hodel 203 board only 0=(1 -20) Se ts running auerage f or 203 board n=0 .1 Se t t o 1 to assune Hodel 213 connected
Edge Tri gger-2 Gain-1
linefrequency-6ft Localthllerage-Jt lODpbaC~Factor-U.098
(PH
TopMargin- 000
II
aof dots to leaue as page Rargin
Press ALT-F then S to save the file. Press ALT-F then X to exit. Restart PeakSimple and load the loopback.con control file you saved earlie r. Run the ioopback test again. The accuracy of the DIA converter should be impro ved. (Channel 1 toluene area counts should clo sely match the channel 4 toluene area counts). End of Test:
Tum off G.C. power and re-connect the original AiD board wiring. The loopback test is completed .
463 (of 550 ) 2006(-2016)
464
Chapter: Pea kSimple Topic:
Using the Win dows Scheduler program to trigger PeakSimple's Autosampler queue
Th e V\'indCJINS Tas!<: Scheduler program is supplied with the Windows coeratinq system. It is founc under Progra"slAceessorieslSystem Tool s. The Schedu ler you to trigger a PeaKSimple Autosampl er Queue or a specific control fi le at a scheduled time and date, or on a regu iar repeating basis using t!1e computer's
auows
Po
[ ct:
'l_
r~
l id
.o,go...,.,f
~
.. _. _-
~ - - - -.
~ ~~
.i..I
.:..:., r_
,:,.-.,
'~-?J-l
, Scheduled T.asks
system clock ( timezcate ).
When yoo d ick on t he Acd Scheduled Task iron in the SChedu:er program. a VllZS.rd will guide you through the process. When you get to the scree n where you specify which program to start . enter the fol!o'Ning line mcx1ified for your part icular situation:
........ . """'- -
: -""-*,. .,...; ",,,~.
,,,, _
I>,o -..... ~ _
.-
c:\peak2000\peak2000.exe -atest.que
• • ,j
C:\peak2000 is the folder cr directory where the PeakSimple softwa re has been installed. If you have installed PeakSimpie in a different folde r. substi1:ute th e name of your PeakSimpie fold er.
~
~=""IIlo. ..:..rSo'~
. :. r "",_
..:..rA.'U'--
:..::...JAI :AJ:'OOO
~ ""/;!{j 'Mi'
e
=;: -l'
1
-'~
.:.J "" ~ '_
,,-.. . :. - _. ..:..J_
'..J l1Q;o ~
i..:.J l'J::
test.que is the name of the Autosamp'er queue fil e which you m ust have prevlousry created in Peak Simp le. Note that the -a m ust precede the name of the .que tile. wben you create the .cue file in PeakSim;Ae you can save the que uno e- a."'lY ne-re yo:.:. want. 7he -e is a wlnocws prograrr.m ing con·ve ntion and must precede the r.arne of the que iiie you warrt to
,,-
~ l1 ~
..Jl l(b",;:> ~H10
peak2000.exe is the name of the actual PeakSim ple sortware program. If you have instafJed PeakSimple under a different name ( tat er versioris of Peak.$im~e may in fact have a affer· ant nam e) use t he na me of tne PeakS;m ple program as it exist s on your computer.
- ~ C! c ·
". ,,-
: ~ s! (F t
,, ~
.:.J .:.J
~ .,."". ,, ~
.;»
o<...
,j,,"' """"'t:t _ 13I
..J"
_ I'
..J ~ .. -I "'~
,,-
~ ..:.;-
r'.
......, _
.'
5 i-7· ~ 1~1 § '§01 ""~ "~
lu.
. -,
run.
....
CO<* ..... ..,.,.. _ . . ~ . . I0 _ ~ - -
...... ;0;0 _
When the Scheduler starts Peai
"""
" d<>..,,~ _ d,,"
-
~
=-:"',.. ~ ~ ~ ~~
specifie d Que ue wm begin . M. tr. e e nd of the
~
.......
. ...
-
--- - -~ ~
:"' - -
,-' --- ".. <
queu e, PeakS im ple will wait for the delay time specified in the queue. and then Pear
'l\iJ1 cicee eutcmeccety.
.=i=== man264.puo
464 (of 550 ) 2006(-2016)
465
GPC Fro m PeakSimple Data Acquisition
Introduction The following is an outline of how PeakSimple data acquisition softwareJhardware can be used to acquire and analyze (in conjunction with an appropriat e spreadsheet) gel permeation chromatography data. At this time. two different version of PeakSi mple software were required
for successful analysis. Version 2.08 was used to collect the data and obtain result tables for narrow polymer standard chromatograms, while version 2.09 was used to obtai n the peak. slice information for broad unknown po lymers. That is, using 2.09, th e volt age difference between
the detector output and the subsequently drawn baseline was obtained for each data point and saved as an ASCII file. which was then imported into Excel for in-depth GPC analysis. Ultimately, it would be preferred to use only one version of PcakSimple. However, 2.09 (the latest version) was not stable while acq uiring data.
Th e program would cras h after
approximately 5 minutes. Furthermore, the time display in the upper right hand cornet did not appear to work and retention windows wer e not visible on the screen although a compo nent file was active. Thus, 2.09 was used only for obtai ning slice information with non -acti ve channels. To illustrate how PeakSimple can be used for GPC analysis, I have included 3 narrow polystyr ene standard chromatograms (4 standards per chromatogram) and polymer chromatograms
two
broad unknown
Chro matograms were obtained usin g a Waters 510 pump (U6K
injector), an ethyl acet ate mobil e phase (1 mlJrnin), a series ofUltrastyrogel$ co lumns (Waters 106,104 and 500 A) and Waters 24 ]0 refractive index detector. All po lymers were pre-dissolved in ethyl acetate and chromatograms were collected at I Hz. Polystyrene stan da rd concentrations were 0.1 % w /w or less (50 IlL injection volume) whil e bro ad unknown polymers were approximately 1 % w/w (75 J.lL injection volume).
Also included are co mponent files,
containing the standard identities and expected retention windows, a n event file for integration, and tw o ASCII data files containing slice information for the broad unknown po lyme rs, and an Excel file with in-depth GPC analysis.
465 (of 550 ) 2006(-2016)
466
Obtaining a Calibration Cu rve Polydisperse polymers in solutio n are fractionated acco rding to size or hydrodynamic volume duri ng GPC. which is also known as size exclus ion chromatography. Molecular weight is related to the hydrodyna mic volume. In GPC a dilu te polymer solution is injected into a solvent stream which then flows through a series of columns packed with porous gel beads . Smaller molecules pass through and around the beads while larger molecul es are excluded from all but the largest por es. Thus fractionation occurs wi th the largest molecules eluting first. The
molecular weight of an eluting polymer molecule varies exponentially with eluting volume, the latter of which is proportional to time under constant flo w rat e condi tions. To obtain molecular weight data and convert the GPC chromatogram into a molecular weight distribu tion, the relation between molecu lar weight and elution time is obtained from a series of polymer standards of known molecular weight. The calibration curve is thu s obtai ned from a ptot of the logarithm of molecular weight versus time. Given that GPC is a comparison of hydrodynam ic volumes, unknown molecular weight determinations will be relative to the calibration standards. For a good introductory refere nce to polymer science, see R. J. Young and P. A. Lovell, Introduction to Polymers. Using PeakSimple 2.08, the result table for each of the three polystyrene standard chromatograms was co pied using DDE into Exce l. The natural logarithm of molecular weight versus time was plott ed and a best fit analytical approximation to the curve was obtained from a third order polyno mial,
P(l~ ) .
This is the calibration curve relating molecular weight to elution
time.
Obtaining Molecular Weight Averages The most common and convenient way to charact erize a distribution of molecular weights making up a polymer sample is using molecu lar weight averages such as, number average molecular weight (A-f,,), and weight average molecular weight (M .. ), as shown in the following figure for a typical polymer chromatogram. .U " is defi ned as a sum of prod ucts of the molecular weight of'cach fraction multiplied by its mole fraction. That is: M .. = "LX/V! I where X is the j
mole fraction of molecules of molecular weight mass M
j •
The weight average molar mass is
466 (of 550 ) 2006(-2016)
467
defined as a sum of the products of the molecular weight of each fracti on multiplied by its weight fraction.
WI '
That is: M" = L w,M, . Additiona lly, it can be shown that the number
average molecular weight, in terms of weight fraction. is equal to: M " = ratio M
"IM ~
lfl:(W,. I.\( ).
The
is known as the polydispersity or pclydispersity index (PD I). The POI is often
used as a measure of the breadth of the molecu lar weight distribution.
P olymers that are
monodisperse (i.e. all chains have the same molecular weight) would have a PDI of 1.
•
t
I
!In
A typical polydisperse polymer molecular weight distribution showing the approximate locations ofM " andM .. .
Using PeakSimple 2 .09, polym ers 1'000604 and 1'000606 were integrated (using the GPC event file) and the results saved in ASCII files. The ASCII files were imported into Excel and the corresponding sa mple times were added as a third column of data starting at time equal to zero. Only slice and time data corresponding to the major peak of interest were retained (columns A,B and 1,K respectivel y). For each time slice. a corresponding molecu lar we ight,
M i ' was calculated using the analytical equ ation fitted to the calibration curve (columns C and L. respectively). Note that extrapolation of a few minutes outside of the last standard (MW = 1.000.000) is usually not a problem. Furthermore, the refractive index response of the detector is proporti onal to the w eight concentration of eluting polymer. independent of molecular weight. Thus, the weight fraction,
Wi .
of polymer in any slice is equal to the detecto r vo ltage response or
height (baseline subtracted) divided by the sum of detector voltage responses for each polymer
467 (of 550 ) 2006(-2016)
468
elution slice ( i.e.
WI
= heigh t I / r. height •• columns D and M respectively) . lltf ., was obtained by
multiplying w. and M , and summing the appropriate columns (see bonom of columns E and 1\1)
1/ M ~ was obtained by dividing each w, by M and summing the appropriate columns (see j
bottom of columns F and 0). Thus. the molecular weight averages for the two polymers were obtained and are summarized in the fo llowing table. Polymer Molecular " 'eight Averages
I
POOO604
POOO606
M.
143,000
299,000
Ai.
69,500
99,300
POI
2 06
3.01
Obtaining Normaliud Molecular \Veight Distributions
As mentioned th e pol ydispersity index (PDI) is often used as a measure of the breadth of the molar mass distribution. However it is a often a poor substitu te when compared to a graphical representation of the complete molecular weight distribution curve, especiall y when comparing polymer distributions. To a first appro ximation, the raw chromatogram (a graph of detector response, 1 (1. ). ver sus elution time, t.) is a graphical representation of the distribution. However, the chromatogram height is injection concentration dependent, making comparisons difficult, and I . is often non-linear with In(M ) , as evidenced by a third order calibrati on curve.
A normalized mo lecular we ight distribution fu nction is given by w(M ) = -dw/dln(M ) . Conversio n of 1 (1. ) versus I. to a normal ized molecular weight distribution plot {i.e. w(Af) versus M or In(M) ), is obtained by considering that the weight fracti on, dw, of polymer which elutes between I. and Ie + dt. is given by: dw = !(/.)dt./
l /(f. )dt. where the
integral in the
denominator is simply the area under the chromatogram. Thus, an analyt ical approxi mation of
dw at the 1tJJ. slice is
Wi '
the weight fraction of polymer
468 (of 550 ) 2006(-2016)
469
A normalized analytical approximation to the distribution functio n, w(Al, ) , is thus obtained from: w(M,) = - Wtl d In(M,) .
Given that M decreases as t ~ increases, the same weight
fraction, dw, of polymer that exists between t , to
t~
+ dz, also exists between In(M) - d 1n(M) .
d ln(M f ) wa s obtained by evaluating the first derivative of the analyti cal equ ation fitted to the calibration curve,
frequency -
dtJ .
dP(I~ )/dt.
and multiplying by the time interval {i.e. the I Hz sampling
(W(M;)1) 1/2 was evaluated point by point (columns Hand Q) and plotted
agai nst molecular weight to give a normalized distribut ion that is injection concentration and calibration curve independent, as seen in the Excel file.
469 (of 550 ) 2006(-2016)
470
Ii'. ~
,
~i f:
,
•
• l
U~U
~
Ul!h
I
~
•
~~UI
;;~ , ~" ! •
~
•
•• Nme !
~
•'"
.... -m
§ ~
I•
Q Z :%%
...............
usu i• J Hu . ... . • ~
= •
•
.... '!!: '!iii ~
1
i
lD~fcq
,, ~
-.• " ~
••
~~
¥ 5• • N"'l~oa'"
3 3
a
3 3
0
••
• ~ •
f •
~
~
i
I niD
5
'"
"
n---...
I• i
i
i-
~
={]
H •• 1 ~1
t l~ .' g· ~
..---- ,>
i,
!hlpru 1
•
• J i \ •
•
r •
t
I
J
•-
B89g0 0-»:-, rg g g Q g 0
~
•I0
•
~
!
•
!
i
I
~
0
C
•
,r
Ii
•
•
•
u i,
~
"t·•
•••
~
V ~ ~~
!
U
~
; ' o •
·
~
•
f
~ "'I • f01 ,0 f~ .1 .... r,' ~'l.-
.." %::
.
H .. .
~
~~
·
:t~ -~
iii-
i~
. 0'
i .l
~
"-
470 (of 550 ) 2006(-2016)
471
Mar 25 S S
•• Z
SOl:l246 9 78S
11: l Oa
,i :il '1 '" 'j '.
Analog Signal Ou1Put Cables
I
_I~
i
The fOUowin! figure and cebte »1'10.... cabin avail&hk to conneC\ ..n Hf' 5890 A..... AL~; q~ ( III chllnnel (variab le' PC signall, + 1 Vor + I mV marimum) 10 e recorder. integrator• .ar: l(~, 1)
converter
eM a oomputc:uy"em. U. second outpul channel IS i1'1slalle.j. a seccnc Clibl ;1 Z 1 ; 1"~., :1
fequirt(J .
",-,
[so
I ,
i
~ .... SI¥i.
Ii
.- ,'0" l\OW)
I). .
CotCVlCl
! * /1 ,;;;l
QYI)lj.1ilI11O
(l5ellO-Mr60
A... II.ll1e
An.""
-..o'~
~5
,i ,
.,!, I
I'
~sc.~OOQO :
S!«n.1O,"put C. Mu
(] It
-!
:~
I
471 (of 550 ) 2006(-2016)
472
The EDIT-CHANNELS-COMPONENTS·DETAILS Screen (continued) Internal Standard Peak PeakSimple allows any peak to be referenced to any other peak for internal stan-
dard calculations. Typically all analyle peaks will be referenced against a single internal Standard Peak (Benzene [peak #2] in the example shown below). To reference other peaks to Benzene, the number 2 must be entered in the Component Details screen dialog box labeled Internal Standard Peak for each analyle peak. Notice that the Results scree n, (View -Results) . will reflect the new value for all the peaks' internal resutts.
:,. . ...._" _ ...... ~- ..::..._·I~~...,...:;-· ,.. :
:-:-~ ~€"i~ ~ pe.oot ~dJ' , ~ '€:At.:.-=·:.::~~t~
..":,.
...._-.
.._
, •.110""".....
, - ._
~
..,.... .
-
~. --
- '"' . -',
!:
- ,iiiN--.-.--,-,...l't.. _
si' -"'-
., . ~ _ liJ uw
., ::;.-
II Z-J'l
"'-:- IOI I''''~ "::-'=-O::
~
OlIl"
L :::=;:F=:io" . -, ,ccc
,-
. -- -
-=;.;"
e
,.... ...1,,ll.1n, 111 _ __
" ·
,Ui~ _ :=--,,
-
-:±=-t~_ --',,",: -:= .
, e.-o::.J,.;C. _
- ,-.
Reference Peak
A Reference Peak is used to shift the retention windows of other peaks. In the examp le be low, ethylbenzene eluted prior to its retention window so therefore it was not integrated. By entering a value of 4 in t he Reference Peak box, ethylben zene's retention windows are referen ced to chloro be nzene. [peak #41. Ethylbenzene's retention window is then shifted by a percentage equ ivalent to chlorobe nzene's distance from the middle of its retention window. T his sh ift in the ethylbenzene retention window allows ethy lbenzene to be integra ted . .;.!UI", • ,-, .
..... ... l:thyl oen7 fln .. integ r3tad
472 (of 550 ) 2006(-2016)
473
The EDIT-CHANNELSCOMPONENTS Screen (continued)
:~~;£k1~i~:~;f1i~ii!7 l;;£~~:JT :t' J:;~t~f¥~;r~
The Change Button
•
,
~nt
..; -
J •
1_ I:Hoo '
.. .
.::;. : ~";l..:-; ~ y e-fJd' L.w
<1.000
,
1 n(J(l
.'N '.-
DCUlI'08Xa.L f'1NU .0lII.
-~~ ~~
4"
..::-::. ::;
-.,:
Click on an existing co mpo nen t to select it. Click on the Change butto n to cha nge the parameters of the component.
The Remove Button Click on th e Remove button to rem ove the co mpo nent fro m th e component table. ; ,:] 6iJI_etl'
The Load Button
;
~6J2.(# ~Q ........ cp!
Click on the Load button to load an existing com po nent file , designated with the .CPT file extension.
The Save Button Click on the Save butt on to save a new component file, or to update an existi ng one. Remember to always use the .CPT extens ion when naming the compo nent file. The saved file name appears at the top of the components window indi cating the file in use.
The Clear Button Clickin g on the Clear button deletes all component data from the compo nent window. Th e component file name is also removed .
The Print Button Clicking on the Print button se nds the file data and the co mpone nt table information to the printer.
473 (of 550 ) 2006(-2016)
474
The EDIT-CHANNELS-COMPONENTS Screen (co ntinued) The Calibrate Button
Afte r creat ing a com ponent table, each component in the table will need to be calibrated . This allows PeakSimple for Windows to not only identify each analyte peak, but also to quantify each peak using a calibration curve. Th e calibration curve is calculated from user-ge nerated results obtai ned at several different concentrations that span the expected range to be encou ntered in actual samples. Inject a standard con taining a known concentration of the component you wish to calibrate. Use a concentration higher than what you would expect to encounter in your analyses. A nother few samples should be run at lower levels. using prec ise dilutions of yo ur sta ndard. Make note of the area counts or peak height at each concentration or use the sho rtcut method described in the next section.
The Ca libration Window
In t h e Edit-ChannelsComponents screen, highlight the component to be calibrated and select Calibrate. If this is the first time calibrati ng a component. an error message will appear which says "Not enough data points", This is simply a warning to inform you that PeakSimple currently does not have enough data points fo r the ca libration method in use. On ce enough data is entered for the calib ration CU N e , this message will no longer appear. Click OK to bypass the error message and continue to the calibration window . Th e Calibration window will open and allow you to enter the raw data that you previou sty obta ined. In the example shown, data is ente red into the table in the upper left comer of the calibration screen, beg inning with the lowest concentration and ending with the highest concentration . If you wish to enter th e data in descending order, check the Show fis t in descending order box . W hen ente ring data into the tab le, first enter the concentration injected, then the area count or pea k height obtained.
~~~~~~J~F1~4'
.'
1
S_
St =
1
•
1_
._
a ... '
~
l"""'-'
1_ "
2.....
... 0 ,= _ -- ,5 ._,
ll!o1 ~:I'5Il 5.155
...
a
Enor
:,. ....- '~ :_.....r. ,,---
~ ;. ; ._ -;.if. -~
..-
..
,-
.-
-
:
._
":
~· 1
,. ·
-
• OFt
- ~~:;f.'
~ -- -
",:o::::';<'''':.~ __~-
474 (of 550 ) 2006(-2016)
475
The Calibrate Button (continued) As data is entered for each concentration, a data point will be added to the calibration curve displayed in the lower section of the window. You may use as many as seven con centration levels for your cali bration curve . In the fictiti ous exa mple to the right. a Benzene standard was injected in concentrations of 10 ppm, 50 pp m, and 100 ppm. The area cou nts from the FlO detecto r we re 100, 500 and 900, respectively. Notice the three corresponding data points on the newly ereated calibration curve . W hen calibration for each component has been com pleted, click on the Save button to save and name the component's calibration file. Then click on the Close button to close the calibra tion window. In our example, a unique file named BenzFID.cal was crea ted. The BenzFID.cal file name will now a ppear in the Components window next to Benzene.
-.
..
WARNING:
Do not use the same calibration curve file name for two different channels or detectors since each detector requires its own calibration curve. tie BenzFID.cal; BenzPID.cal; etc)
Calibra tion is required for each compone nt you expect to be present in your sample, and fo r each detector you will be using in your analysis. Once cali bration curves have been completed , and calibration files saved , every component in t he component ta ble should show an associated calibration file. Pea kSimp le will now be able to quantify each comp onent when actua l samples are injected.
,"'ill", F: ;,
".
~~~~~:i ~~=:-;'~~" : ' ~5~" .~
I
.•
l J
,, ~
SOl
II
. _
r_ 1_ Dr
•_
OJ
r_
1
.0...
. ~
_
._~O_
....
1_
.
1._
2.~
2._
J...:J.~
:I 1M
5.J'U .,_
.....
S-_
"-_
-
.IUI:_.CAL IOUIt.IlE.t:A&. CH.OAOFCAL
..UN"'" .. CAL c..u ~
.......otI..CAl-
~
475 (of 550 ) 2006(-2016)
476
Calibration Screen Shortcuts As an added convenience, PeakSimple for Windows offers shortcuts to commonly used screens. These shortcuts may be acce ssed by pointing to the desired channel and clicking once on the right mouse button . The following pages describe the shortcuts availabl e to set up calibration ta bles and calibrate components. After a known standard has been run and the peaks have been identified. a new compo nent table may be constructed by simply positioning the mouse pointer over a peak and click ing once on the right mouse button , ("rig ht-clicking-). The shortcut me nu will appear. Select Add componentfrom the menu . A retention window will be drawn horizontall y across the peak . Right-click agai n over the peak and select Edit component The Component Details screen will open al lowing the pea k to be named and numbered. The exam ple below shows Benzene as peak #2. The com ponent has been named F-benzene to avoid confusion with a benzene peak from anothe r detector such as a PID . Note: It is im porta nt that you choose the component name carefully since the calibration file name is derived from the first eight letters of the component name. The F-benzene calibration file would be named F·benzen.cal.
-,
,\
}
I1\ ,Ii
\, i,
Righ t-click over the pea k agai n and select Ca librate. If no calibration curve exists fo r the peak , a window will open asking if you wou ld like to use a calibration file. PeakSimple offers a template calibration file aptly named TEMP LATE. CAL. Click yes to use the defaull TEMPLATE calibration me or select your own by clicking Browse. This example uses the template cal ibration file. Another window will open asking you to select the Recalibralion Level. Selecll00 for 100 ppm standards, 50 for 50 ppm, etc.
Nt
~ - - -
,
..-
ifl.l -
476 (of 550 ) 2006(-2016)
477
Calibrat io n Screen Shortcuts (continued) Click OK to accept the Reca lfbralion Level. The Calibration screen will open and a flashing asterisk (*) will appear along the existing calibration curve depicting the new data point. Notice that the calibration curve has been named F-benzen.CAL. If the new ca li a brat ion data po int is acceptable, clic k Accept New to update the calibration curve data. In the example to the right, the updated F-benzen.CAL calibration table reflects the new area count of 939.627 at the concentration level of 100 ppm . (The prev ious calibration data of 900 area counts at 100 ppm is shown in the Previous #1 colum n which is 'grayed out'). Notice also that the third data point (100 ppm) in the calibration curve has been shifted up slighijy to incorporate the new data, (939.627 area counts). At this point, if the new cali bration curve data is deemed to be acceptable, click on Close to automatically save the new cali brati o n fi le , an d c lose the Cal ibration window.
._-
-;.j _1'
ffiO'
"'" ...
-
.'."
M IM
'...., ,"'" ow" ,m ' "Yo nMii =5:l_ . *+-l'rt ~--s= .... ...;'~~ . __ ~·i
',",
Calibrate All PeakSimple offers a time-saving feature for recal ibrating all peaks with ju st one mo use click . After a calibration curve has been created for each compon ent , click on View· Results to bring up the results window. Select Calibrate All and choose an appropriate Recalibration Level, then cl i c k OK . Pe ak S imp le w ill automat icall y reca libr ate a ll compon ents at the selected level and save ea ch component' s updated calibration file.
477 (of 550 ) 2006(-2016)
478
Calibration Screen - Use and Statistics Radia l Buttons To improve the calibratio n accuracy, chroma tographers ma y prefer to average the areas of 1, 2 or 3 replicate injections . T he Use radio button allows the user to select how many injections are used in the calculation of calibration factors, (CF). Ca librat ion Factors are used to construct the calibration curve using the formu la: CF = area count divided by the amount injected. The example to the right shows the calibration data at the 100 ppm concentration level, (circled), with the Use button set to the defa ult setting of Current Area / Height Only. This setting uses only the latest calibration data to calculate the calibration fa ctor for the #3 data point. (CF = 939.627 / 100 = 9.396)
This next example shows how the calibration curve is changed when the Use button is set to 1 Previous Areas Also. Th is setti ng averages the last two areas to derive the average ca libration factor. Notice that the calibration fact or is now 9 _198 when the two area co unts are average d together. (939.627 + 900.000 / 2 = 919.814 average area counts. The CF is calculated as: CF =9 19.814 / l Oa = 9.198 ) Setting Use to 2 Previous Areas Also will average the last th ree areas to derive the ca libration factor. The Calibration Sta tistics screen shows calibration curve details such as the Average Slope of the Curve, the Y Intercept, the L.inearity of the curve, the Number of (calibration) Levels, the Standard Deviation and Relative Standard Deviation of Calibration Factors, the R2 and the Formula used which is based on th e Method selected .
478 (of 550 ) 2006(-2016)
479
Calibration Window- Methods The Method button opens the Recalibration Type window which allows the selection of one of six formulas used to draw the calibration curve . The algorithms are described below and corresponding calibration statistics are shown. In the fo llo w ing : X is the sum of the ext ernal mea sures over the catibrallon ev-
••
Y is the su m of the corresponding a reas at those ca libl'3 ttOtl
~~.
n is the number of ecwe ca libration levels Sewr.al ol hM $UrTl$ are used , tor mstarce: X2 is the sum of the sq uares of ee e~emal measures Y4 is tM su m o f the (are a to t he 4th power) XY is the sum of l he (e xte m a l rneils ure • area) X2 Y is the sum of (e lda m al measure sq uared • area ) Vpt: is the sum of the (area f extern al measure) et c.
S ing le line through origin ; T he resulting ca lib rat ion curve is define d as
where: x is
The restJting fador is ltlefef()le the ave rag e of the ca librati on fa ct ors at th e calibration levels. Note: any exp!icit caJibl'at tOll ever po.'Il iIl:r-:O IS ignored (and n is red uced by 1). There rTM.ISt be at least one calibration Iewl, not incIud,ng any ~l at PO. Single line: The resulting c anbranon cu rve IS
eenoer as
y"Ax+B where x is external measure y is area
ex ·
A=( (XY· nl YI I I 0 B"'( (X . Y2) · (XV . XI ) 1 D D=( (X2 • n) -
eX•X»
No,"" ThIS IS a least sq uares fit algo rthm O\Ier the ca libration 1eYeIs. A painl a t (0 .0) is 8 1$(1 assumed (by incrementmg n) unless the re IS a 're .ady a valUe at x=O. or It IStabsticsJR21nciudeZero 1$ set to 0 in the P EAKWIN .INI file . There m ust be at least 2 cajbrii tiOn lev!'l's_ EPA ni les allo w tn e use of S ing le line Fit provided thai the sta ndard devia tio n of calibr ation f.actors is <20% Mu lt ipl e line segments: There IS no ftt 8u lling formu la he re , Just inteorpolat ron betwee n
the levels. and the origin_There must be at least one cahbl'atiofl ~
479 (of 550 ) 2006(-2016)
480
Calibration Window- Methods (continued) Parabolic:
The resuling ca libration curve is d efined as
y:Ax2+B whenl : x externa l mellSure y is area
es
A =( (XlY ' ru - (y ' Xl ) >/ 0 8=( (y ' X4) - {XlY ' Xl» 1 0 0=( (X4 ' nJ- (Xl ' 1
xa
Note s: T hIS is a teaSl SQua res fit algori th m over the calibrat ion levels. A pont at (Om IS also assumed (by Incr ementing nJ Urlless there is aJrudy a value at x=O. or if (Stat$ticsJR2lncludeZero IS set to 0 In the PEAKWININI file There must be at Iea~ 2C
"the
Quadratic through origin: The resu lting calibration CUlYe is defined as
-~ x is eoe mar meas ure y is area A"( (XY ' X3j - (X2Y ' X2) I 0 B=( (XV ' X4) - (X2Y ' X3» I D D=( (X3 ' X3 ) . ex4 • X2)
Notes: This is a 'east squ a res fit algor ithm ove r the cal ibfa lion leve ls The re m ust be al east z calibration 1e"", ls.
QuadrMic: Th e res utirlg call1fation curve is defined as
rAJa t-Bx+C
where : II: is external measure
y is Neill
A=( (XYOX· rXlt(XTX2-X"X3) (X2Y"X2-XY*X3j"(X-X-X2 "n) I 0
8=-( (XY"X2-rx3)"{X2"X3-X'X 4) (X2Y·X3-xrx4)"(X2·X2·X~X3» )
c-r (XY"Xl.Y'X3)*(X3"X3-X2"X4) _
IE
(X2'r'"X3 - X"X"'l"(X2"X2 -X·X3) )IF
0=( lX3"X -X2"X2) "(X2"X2-X"X3) (X4"X2 ·X3"X3)"(X"X-X2" nj ) E"'( (X2"X2·X "X3)"(X2"X~X"X"') (X3"XJ-X2 "X4)"(X"X2-X J - n) ) f=( CX")(2 -X3"n)"(X3-X3-X2 "X"' ) (X2'"XJ ·X"X4 )"(X2 "X2-X "X J )
Noles : Th iS is a least squ ares fit algorithm Olle r !he CilI,bration levels. A point at (O,C) IS also assumed (b y increm enllng n) unless there is alre~ a value at r-O . o r If [StatisticsjR2loc1udeZero is set toO Ki me PEAKWlN.INI file There must be atle~ 2 cabbret o n leve ls (J if th e ong in is not assumed ).
480 (of 550 ) 2006(-2016)
481
The Calibration Window (continued)
: : - _ "~_
[J
The Accept New Button If the new calibration data is acceptable. Click Accept New to update the calibration curve data.
The Close Button Automatically saves the new calibration file and closes the Calibration wind ow.
The Load Button =! F-t--o:en CAl.
Click on the Load bullon to load an existing calibration file, designated with t he .CAL file exten sion.
:J F..,..."CAL
::l T~ C"
i!!l Toluer>ol-~
~ Fdlenz.CAl.
~F """"CAL ~ " ~ cal
"'-«
~ S _e8
The Save Button Click o n the Save button to save a new calibration file, or to update an ex-
isting one. Remembe r to always use the .CAL extension when naming the calibration file . The saved file name appears at the top of the calibration ~()«tt <;.il
wi ndow indicating the fife in us e.
~ F '-'-"CAL ~ F-d"bo. [Al
~8 t!"1lA. c'"
=
.:1 aorneooecal
The Clear Button Clicking on the Clear button deletes all ca libration da ta from the ca libration window. The calibration file name is a lso rem oved .
F"odbcnz,CAL
::J F-IokJenoo.
~ B """nDcal
-
:J loiilCdtcal
~ ChOob e..l
.:!!l £ ~ e.tI
:!ic........ur
-· ~ £~ CAl
~ sm-t UJl
-
~
...
~_~~~#Bf}H'--
c s;.., _ ~ I Caoil>'.-.. -r D'IL1 .. .. ~
~
,-
¥ ~.~ : t
J ~ . ..:" ~ L
~ -- -,..,.,. - ~
The Print Button Click ing on the Print button sends the file data and th e ca librati on curve informa tion to the printer.
481 (of 550 ) 2006(-2016)
482
The Edit -Chan nels-Po st ru n Win d ow The Postrun Screen is used to determ ine all the actions that are to be don e in PeakSimp Je after a chr omatogram run . Cl icking on the Postrun box for channel 1 in the Channel con tro ls window will open up t he Chan ne l 1 post-ru n actions window.
Pew",
I
Save file as "X" T he Save file as checkbox , w he n se le cted. automatica lly saves a chromatogram fil e to disk after a run is comp leted . T he file will be saved under the fi le name and path entered in the information field to the right of the ch eckbox. Aut o-increment
When selected , th e A uto-increment checkbox will incrementa lly add a nume rical d igit to the entered filename after e ach run . For ex ample, a chrom atogram run saved as RUN .CHR wou ld be saved as RUN1.CHR afte r the second run and RUN2 .CH R after the t hird run .
.. po
,.
~~31 !m...."HFi
.~
_
r s.....e~$ r Qll.. H;J 'ed:l~ r f!;r1lfWJt; r: Upd.,te.QDE fri< ElIe~~
P'
""-'lo«re:nent
JOi 1.LOi,;
I
r: Fi" ,4ll=:/!('r: @oo
(;)~I
F"
r r
Smoottdut
r::
c.:~ ~ib~
f;~ilibIdle al1eYet
~""'tl$ [f" ltc.e.lW
"
r ""'" I
The Save res u lts checkbox whe n se lected will save the data in the resu lts sc reen to disk after a chromatogram run (Note: This is not the revr data but instead is the A SCII results). The Add to res u lts lo g " X" checkbox adds t he res ults of a run to the resu lts log specified in the information field to Its right. It will be saved under the same filename as the raw da ta but wah th e extension .RES. for exam ple 602.RES . The Pri nt results checkbox will print whatever is specified to be print ed in the Print format wind ow, th is m ight inclu de the chromatogram and its results data . The Upd ate DOE link checkbox when selected will au tom atically update the Dynamic Data Exchange link once the run is completed. Ex ec ut e "X" The Exec ute info rmation field op e ns an y executable fi le ( .exe . .bat , .bas ) afte r the chrorr.atogram run is co mp lete d. Note : Be sure to include the full filename and path for the executable file . Central is returned to PeakS im ple whe n the called app lica tion doses. Restart ru n after " X"
Tho Restart run afte r "X" checkbox and inform ation field restarts a chromatogram run after an inputted de lay tim e . T he delay time is inputted in m inutes and can be repeated as many time s as is e nter ed into the times to tal inform ation field . Note: If 0 is entered into the times total information fi eld then the run will be restarted an infinite number of times.
Peeserlcoc-t.cub
482 (of 550 ) 2006(-2016)
483
Th e Ed it-Chan nels-Postru n W indow (c o nt inu ed) Recalibrate at level " X"
~. s;-..;;,.. ~I ~ [n=l ~ kJ'>i-:a~ r" 5~ je$ ;J:f r ~d:llo reM:l ~ 1 C.~I.LC:i
r: Etftr~",b r The Recalibrate at level ' X" checkbox and info rmation field receubratcs all identified peaks at the end of a run at a given leve l from 1 to 7. This feature is normally imp lemented as part of an autosamp ler que ue. Detailed instructions are given in the A utosamp ler queue documentation section.
;,~e:
I
-
....
UpWteQDErk c
-.....,., ~"",.,..., -
r: R~"' llUn-~'t~ I :;Q oo Jl'II"IUte: [O ~r.:a: r R ~"''' al le-veI: [I" I"
-"II,
IC r~1
~ rnooih IJS:
Ir
Co~ d..t.. to r:h~, IT::"
1
.1
0'
I
"""' I
Smooth first
The Smooth fi rst chec kbox runs the sm oothing algorithm as it was last app lied to the chrom atogram before the fin al integration is done , If the box is left unchecked no smoothing will be done to the chrom atogram run .
Copy data to channel "X" The Copy data to cha nnel ~X " che ckbox and information fie ld inputs the chromatogram run into Whatever channel is selected in the information field. Only the values 1 to 4 can be inputted into the information field as there are four chromatogram channels in Pe akSimple.
Peak NTdx -2.pub
483 (of 550 ) 2006(-2016)
484
The Edit-Ove ra ll Win dow
.,
The Overall controls window is used to define and cont rol many of the option s in PeakSim pIe . Clicking on Edit in th e PeakS imple menu bar a nd then Overa ll from the drop down menu w ill open up the Overall contro ls window.
fileuci£
~iew ~Cl;JU;." itio rl
HeO·1
W -Coanne.:.
,
-
I
-- I
Mcnual inte~ ation
~c le}s "';l"l'~
J
Unkn own pea ks are lab e led " X"
S t,;btractl~dd
The Unk nown peaks are la beled intorrnation field, when fill ed out , labels all un known pe aks the value that is in the inform ation field. If t he word Peak was entered into th e information field then all unknown peaks wo uld be labeled Peak.
The Show retenti on w indows checkbox is checked by defau lt and thus rete ntio n windows ar e visible in Peak Simple; unchecking the Show rete ntion windows checkb ox remove s the rete ntion windows from sight. The COM Port I USB d ev ice nu m ber " X" informatio n field specifies the COM port or USB device number that is to be use d for the connection between Peak Simple and hardware. The COM port number is typ ically 1 or 2 while the USB device number is typ ically betw een 5000 a nd 999 9.
channels...
imoothirm-..
-
,
~''''''""""",,., • .aooId j J'
:- ~ .O!l ~
!
-
r
~~B.r
'-'.-:Da
:- ~-
.... """""I1!'- f .(jJi
~~ _
~ De; . .. :;l~""O";-
i.. . 11_
..........- ·-
I .
.......'.
~"'l;;'~
M
~to l
,
. \0<"4
•I $I.ot.p:ocr€t
"'~ D~ d~ 'IIIb<~
DoI
....,.l r $.o• • _ ............ ~
i=' E_ ..... . r401,...
r ....-.1>:¢00< r s_~
f
01:.
I
..
~
-.A5:::._.VV1_ """'...., ItT" ~ e-a !
Label peaks onscreen by
The Label peaks onsc reen by options box enables a pea k to be labe led by as man y as fo ur options. The Number checkbox labe ls all peaks with their peak number. The Name che ckbox labels all peaks with their f ull name. The A bbreviated name checkbox labe ls all pe aks with a sho rter. four ch aracte r abbre viated nam e while the Retentio n time checkbox labe ls peaks with their retention times. The Draw lab el vertically checkbox specifies w hethe r peaks should be labeled hor izontally or vertically on the chromatogram screen . When th e box is checked the peaks labels will be drawn vertically whe n it is deselected they w ill be drawn horizontally.
n
i OiU 2633 i
Gradient setti n gs Gradient sett ings are only use d when PeakSunp te is controlling an SRI HPLC Pump . T he Min and Max voltage settings are used tc calibrate the Pump.
484 (of 550 ) 2006(-2016)
485
The Ed it-Overall W ind ow (continued) Default display period Th e defau lt display period options box is used to define the d efault d is play limits for a PeakS imp le chromatogram . The Start information fie ld is used to specify th e default beg inning limits while the End field is used to specify the end to the default disp lay lim its. The start and end display limits can also be adjus ted by the left and right arrow s below the chromatogra m in the main display window.
Postrun file ove rwrite prote ction
-£ 1 11",->",,>b_ W>oIo<
,,'!, r N-.""
r;ou f", / ~sa ~ ,
.
oovct~. r:
1' 1:'
I'
s,.... I~_~ f'ld~ ' ........... _
I
_ ~c_
I:'fI.-_
- o.o...t ¢1l' "",",,-
-!
I:' C,_ lot .. """",,,,,,
~ P",,,,,"I,p- ~ .. ,,,..._
I
....~~ ol~ at ... ...,...,.., .. ~
t.+o.d.UlIo .,..~! f'
E''''' ,....,.
r ~..._boobd. rs_ ~
Postrun file overwrite pro tect ion pro tects a saved file from be ing w ritten over w hen the auto increme nt featu re is se lected in the Postrun window. Instead of wri ting over a used filename an auto-incremented run will sele ct the next unused number in the sequence to save the file to d isk. For example, if fil e TEST02.CHR already exists on disk PeakS imple will save the file as TEST0 3.CHR.
t
;; !~ -....~ f ~ -" "' '''-''~-
W@
-~ r
S~,. b " t.olh "';C ..,".DiA _
~ .... _
I
01: '
tt
I
, -,
~
..._
c..:.
c....-':::'''''~--'''=c....
-"'
Amounts bel ow an MOL of " X" will be reported as "yn Peaks with a value be low a specified Minim um Detection Level or MO L w ill be reported as whatever is spec ified in th e secon d info rmation field, typically N/D or not detect ed . The number thaI is below the MDL will not be repo rted, only the entry in the second information field will be seen.
Default d ata file path Typ ically a ll PeakS imp! e files are sav ed to the PeakS imp le directory but by entering a full direct ory path into the Default data file path information field anothe r directory can be selected to save files to . Note: It is recommended that users sa ve all PeakSimple files to the PeakSimp ie directory. Jf necessary export files to a different directory a fter sa ving th em to the PeakSimple directory. Reset relays at end of run The Reset re lays at e nd of run check box when selected turn s off all re lays (A -H) at the end of a chro rnatoq rarn run . If the box is let:: unse!ected the relays will not be shut off afte r a chrom atogram run . Hardware lo op back and Software loopback are used for syste m valid ation and w ilt be disc ussed in further det ail in the Loopb ack test section. Peak.NTdoc-4 pUb
485 (of 550 ) 2006(-2016)
486
The Edit-Overall Wi ndow (continued ) Save fi les in both .A Se and .CHR formats T he Save files in both .ASC and .CHR formats chec kbo x when selected saves file s in the ASC format (ASCII ) and the .CHR format (chromatogram). If the checkbox is not se lected files will be saved only in the .CHR format.
pm ' ;;;; \\
-"~--~] ~jUX""""
Automatically save data every " X" m inutes
0.- 'o:>oi~"" ~ f .. ~ _
_
&-~ _ "' M~ ol~ ",",",,' __ :"' 00 ~ D cJ ~Jol. ji ..
The Automaticall y save data every "X" minutes che ckbox a nd information field when seJected saves the data during a chromatogram run at intervals specified by the information in the inform ation fie ld. This feature is useful fo r run s whe re power outa ges are frequent and data ca nnot be lost.
r;; f7
j::"
_ J r
E......... .. ""' 01 _
r s,........ 1:>:co»:l.
i_
Iio, .. _
.. SC ...·.j Gl~_"""
.....,...",...... _ _
r~__
(lI;
.
~ " ruoo
c..c.
PeakNTdoc- 5pt.;b
486 (of 550 ) 2006(-2016)
487
The Edit-Colors Win dow The Colors window determines the co lor schemes th at are to be used throu ghout PeakSimp!e. Open the Co lors wind ow by selecting Ed it from the PeakSimp le menu bar and then Colors from the list of options.
ManL~1 intel1~\i-;;'"L.i
Selecting the Bac k g ro un d butten with the mouse cursor opens up the Background co lor window. The back ground color ca n be cho sen from a set of 48 colors by selecting a color and then affi rming the choice by clicking o n the OK butto n.
v
StbtractJBdd C~r\."l!!s. ..
E5i " . ,J
..!.I
r-'. 1i~,.z;j ~.J
: d-.-.,......... l-a·
' __
z,."
_
g
,
I I I
.l!u~ 1l~ 1r ~_".,
I 1 I
~.
The co lor of the labels contro ls the color of the wor ds that be long to the peaks. Th e color of the label s is changed by sel ecting the Labels button to open up the Labels color w indow . In the Labels color window select a color and then pres s on the OK butto n to make the change to the labels co lor .
The color of the ze ro axis is chos en by clicking on the Z ero axis button and then se lecting a co lor from the Zero axis color w indow . Clicking on the OK button closes the window a nd makes t he change to the co lor of the ze ro ax is. Don't set the Zero axis co lor to the same color as the Gra ph backgro und because they wo n't be distinguishable fro m each othe r.
j
9l'1J.;
~moo tt1ing. ..
Th e Grap h backgrou nd windo w is ope ned up by selecting the G rap h backg ro und button in the Colors wi ncow. The g raph background color is changed by se· lacting a color and then clicking on the OK button to make the color change .
T he peak color is the co lor of the circle at the top of each identified peak and is determined by the Peak color window which is ope ned up by selecting the Peak button in the Calor w ind ow . Select the desired pea k colo r and then click on the OK bu tton to clo se the window an d affinn the change .
~<:1JeYi
·
I
I
t_
r- ''c' ' ''''''''-r '']! 0.-,. r
.e._ cob>'
r-r r l:" r ... r rs: . r r u; C " "'1lI
. ._._--
. O;: "II. WC • •
.
_ • • 11 • • •
_ IliJ 111011 III r
_r ~
fl:oa
r r rrrr rr r r r rrrrr !
0 1(
I
UtaII
I
t ..v
T he ba se line is the line tha t run s along the bottom of the peaks and its color is changed by sele cting the Base line butto n and then choosing a color from the Base line co lor window. T he change is ma de once the OK button is selecte d and th e Window is clo sed .
The data line is the signal line that makes up the peaks in PeakS imple and its co lor is defined by se le cting the Data lin e button in the Co lors wind ow an d th en se lecting a co lo: from th e Data line colors window . Once the des ired color is se lected ap ply th e col or cha nge by clicking on the OK button to close the window. PeakNTd x...{).pub
487 (of 550 ) 2006(-2016)
488
The Ed it-Colors Window (continued) The overlay line is a data line from a chromatoqrarn that has been overlaid on top of an existing chromatogram and its color is chan ged by se lectin g the Overl ay line button in the Colo rs w indow and then selecting a color with the mouse cursor in the Overlay line colors window. The color changes a re m ade once the OK button is se lected and the WIndow closes .
L. -=i~.~ ·
":1 I l,.ot:..... I
f
I
E...-,.
I
Il_
! I
""'-'<."
,-~::FJ :
1 01:
1
~
-
I
Printed line th ickness
--
I
.1:_';.... ko>o .
Reten tion windows are the ho rizontal bars that appear onscree n and the ir color can be changed by clicking on the Retention windows bu tton in the Colors window and then selecting the des ire d color in the Rete ntion windows colo rs window. To apply the color chan ges click on the OK butto n to close the w ind ow .
The thickness of the Data line and the Overlay line whe n a chromatogram is printed is dete rmined by the Data line information field and the Overlay line information field. T he thickness of the Data line is determined by the numerica l value in the Da ta line information fie ld, l a r~ ger numerical values wil l resu lt in thicker lines. The thickness of the Overlay line is a lso determined by the numerical value in its informatio n f ield. Larger numbers in the information field will result in a thicker over lay line.
I
to.....··
~~ .
~ .... col:n.
r:: rr llir. rr
I
!!! r
r
[iii !:lO Iii I:iI
I u u liiil3.Q • • . iii • • • • • •
•••••••• r . r
. 8 Ji1," C
.
--t:r
rr r r r r r r rr rrrr r r
I 1" 1 '-' 1 ' '' 1 [>~e.->:.,.., 01"."
Pe::!kN l doc-i .puo
488 (of 550 ) 2006(-2016)
489
Man ual Integ rat io n The manua l integration to ols are used to manually draw in th e baseline in a PeakSimple chromatogram. The manua l integration toolbar is opened up by se lect ing Edit from the PeakSimpJe menu bar and then cl icking on t he Manual integration option. The manual integration toolbar appears to the f ight of the Pea kS imple toolbar in the upper right ha nd co rner of the scree n. Off Integrat io n Too l
I.el
The None integra tion tool adds the area of one peak to the ar ea of an adja ce nt pea k. Once the None integration tool is se lected click on a va lley between two peaks wit h the mouse curs or to change the base line .
Drop Integ ration Too l
Unl
The Dro p integra tion tool drops the baseline between two peaks stra ig ht d own onto an existing baseline. T he Dro p integ ratio n tool is used by selecting the Drop tool in the ma nua l integration toolbar and the n clicking on a va lle y between two peaks to change the baseline.
Based Int egrati on To o l
S thractlMd ~ _
;imoothir'l!l... -
~
The Off integ ration tool or the mouse cursor is used to end a manua l integration mode once it has been se lected . W hen the mouse cursor icon is selected no more chan ges to the baseline of a ch romatog ram can be performed until another manual integrat ion tool is selected.
None Integrati on Too l
q,.,re, .. .Q v er.!lll... QJlors...
ItAr
The Based integrat ion too l ra ises the baseline to a va Jle y between two specified peaks. To change the base line se lect the Based tool a nd click on a peak with the mo use cursor to raise the baseline up to the va lley.
.... ----
ese , .,
.,.
.
-~
~6iV ; ...
-,
I
•
,
,
--
, -
""
:=-.~.
..
,,, ,~,
, , ,
,.,
.',,-...-
- ,.
.-",
.. ,
' ~_l
..
.~
,
i
•
, ..
"
.,. "".~. ,
1
,
J
-
,
~' .~ ,.~ . '
..5
-,
.- , .. .. -
s
,
.
~
?
-,
..
" . . ..... " ...
,
-
,,
. ,
, ,'
,
.. - -- -- -
.'
",
,
,
I '-':"I
-
..
':::'!. ' .M• • , .- ' ... , .-. " ",r. .......... '" ". ,. : ..... iihZ: , i ~
~
,
I
~
i.
.-1.
~ ~
,
,
..<01
•
/,
'.
--- -
,
'.
,
" ./
,
..
,
- ..
PeakNTdoc-8.pub
489 (of 550 ) 2006(-2016)
490
Ma nu al Integrat ion (cont in ued)
. ..
Lead Skim In teg ratio n T ool
The lead skim integ ration too l skims a peak 's area off of the leading edge of an adjace nt pea k. To skim a peak off of the leadi ng edge of ano the r peak select the Lead skim to ol from the manual integration toolbar and then click on the vall ey between the two specified peaks with the mo use cursor.
\
j' ,
L._._.;.,. _ _ -
. ' . #9" . . •
- ...
Tra il Skim Inte gration Too l
i
,.
~
-
?
~
, ~-",_• •. ~ ~. " "
J • • ' . " " .. "".'.•' " '-" ''". ~"" <,
..
The Trail skim integration too l skims a peak's area off of the trailing edge of another, adjacent peak. To skim a peak off of the trailing edge of another peak select the Tra il skim too l and click on a valley between two peaks with the mo use cursor to make the change .
lead Horizonta l Inte g ra tion Tool ~
-.
-
~ ", U • .~ ." ·
The Lead horizontal integration tool draws the baseline horizontally for the leading peak wh ile the trailing peak's baseline stretches from the horizontal line to the next valley. The Lead horizontal tool is selected in the manual integration toolbar and once a valley is selected the cha nge to the baseline is made. Trail Horizo nta l Inte g ration Tool
-- I
-- =- . , . ' ~ ':-''' ''' ''''. '' ~.' ~""
I
---..-._----_
- -_._- ---
11h.1
The Trail horizontal integration tool draws the baseline horizontally fo r the trailing peak while the leading peak's ba se line str etches from the horizontal line to the previous valley in the chromatogram . The Trail horizontal tool is used by selecting the Trail horizon tal tool in the man ual inte gration toolbar and then clicking on a valley with the mouse cursor to make the change.
•."-';!
i
'-
._--
!
:- _
-
----~--
-Peaksrrocc-a pub
490 (of 550 ) 2006(-2016)
491
Manual Integration (continued) Inh ibit Integration Tool The Inhibit integration tool ends a baseline afte r a valley the reb y stop ping the pea k's area from being co unted along with th e rest of the chromato gram. To use the Inh ibit tool select the tool in the manual integration toolbar and then click on the valle y between two peaks to end the baseli ne .
Rubber Band Integration Tool
_ __ - ..J
3
'
1)).\1
Th e Rubber band integration too l is used to manually draw the baseline in a chromatog ram . The Rub ber band tool is selected in the man ual integ ration to olba r and is clicked and dragged on the chromatogram to draw in the baseline .
Undo Integration Too l
'-,
- , - -- --
\ f _.-'
- ..--.-.. -""'-
- - ', -
- -~ -
, ,
Th e Undo integration tool rem ove s all chan ges do ne to the ba se line of a chromatogram w ith the manual integration too ls. To use the Undo tool d ick on the tool in th e manual integration toolbar and all cha nges will be undo ne .
Note: Changes made to a chromatogram with the Reverse and Zero integration tools cannot be undone with the Undo tool. Revers e Integrati o n Tool
.
,! ,
!.j:ii LBJl
The Reverse integration too! inverts a selected peak or a sel ected g roup of pe aks in a chrc matogram. A peak is inverted by selecting th e Reverse tool in the manual integration toolba r and then clicking and dragging the m ouse curso r over the peak.
I
! -.
-- -- .
,. ,
--
Ze ro Integrati on To o l T he Zero inte gration tool sets the val ue of the data line at ze ro starting at a se lected point. T o zero the data line at a given poin t select the Zero tool from the manual inte gration toolbar and click on the data line with the mouse curs or. P,eakNTcc :::· 10 pub
491 (of 550 ) 2006(-2016)
492
The Ed it-Valle ys Only Optio n Th e V alleys only optio n is ava ilable on ly wh en the M anual int egration tootbar is open in Peak Simple . T h e V all eys only op tion can be se lected by opening up the Manual in tegratio n toolb ar in th e Edit menu and the n selecting the Vall eys only option immediately bel ow Manua l integration in the drop down men u. W hen the Va lleys o nly option is selected all changes made to the base lin e of a chro matogram will snap on ly to the va lleys of the chromatogram . W hen the Va lleys only option is turned off change s ma de to the baseline of a chromatogram wi ll go to w herever the mouse curs or was clicked.
The Ed it-S ubtract/Add Cha nnels Menu The SubtracUAdd channels menu rem oves or adds the analog data signal from/to one cha nnel in PeakSimole from/to an other ch annel. T he SubtracUAdd ch ann els menu is op en ed by selecting the Ed it menu and then by cricki ng on Subtract/Add chan ne l in the drop down menu.
B.. _."'=Ot ""'- - -~ew
:D
~ CQti ~:tioo
Channels...
Q ..ertll .. £OIOI i ...
, -Subtiactl~dd char.....e ls.. S-rnool...... I1..•
j
Eile IJ.j_~ Yew a cQUWtioo D Cb.Ylnels...
r
Q,,·er!l.. ~obs. .. M~
N el)"alion
Y'i:r e}'.;.~/
S ubtracting a Ch an n el
To subtract one channel from another channel click on the Subtrac t radi o button w ith the mouse cursor and select the ch a nnel that is to be taken awa y in the firs t dia logue b ox . In the sec ond dia logue box select the chan ne l t ha t is to h ave the first selection taken away from . Click on OK with th e m ouse cursor to effect the ch anges.
~I hom.
'0
C~ !In"
d r.-::l
I . ...:J
A dding a Cha n ne l
To add one cha nnel to a nother cha nne l select the Ad d radio button in th e Su btract/A dd channels m enu . Select the ch an ne l tha t is to be added by selecting a num ber in the fi rst d ia logu e box and then choose the ch annel that it is to be added to by selecting a number in the second dialogu e box. A ll changes are made once the OK button is sele cted .
Peakrv tdcc-t t.o ub
492 (of 550 ) 2006(-2016)
493
The Edit-S moot hing Wi nd ow The Data smoothing w indow determi nes a ll the smoothing options that are to be perfo rmed on a data line . The Data smoothing window is opened up by se lecti ng Ed it from the PeakSim ple menu ba r and then selecting Smoothing from the Jist of options.
~ieo.'J !cqui s~ IFeD I-'.cil: .. -q,.....;,;_.
Q.lfer.:!!.. ·Co lo!t ... M~i 1"ll ~dliorl
... Y;lII~!I~ ~nly
The Source c hannel dialog ue box sp ecifies which channel the data line that is to be smoothed is in. The Des t ination channe l is the ch an nel that the smoothed data line from the source channel will be disp layed in.
Meth od The method of smoothing is determined by the smoo thin g algorithm se le cted in the Met hod box. The Moving A ve rag e a lgorithm se ts each samp le to the average of the sample s around it ind uding itself. The nu mber of sa mples tak en in to account depends on the Filter w idth. Th e O lym pi c algorithm is simi lar to the Moving Average but the highest and lowest values in th e set of sam ples are discarded before the average is ta ken. Th e Savits k y-Golay algor ithm is sim ilar to the Moving Average but each of the sam ples is we ighted according to a set of we ighting factors . Inc reasing the number in th e Orde r dialogue box gives more we ight to the centra! samples w hen using the Sa vitsky-Golay method .
t:e~p
B e·integrale
ch=me!:-jn3 Qe:stinationchennet f23 ~wrce
,-r.MetJ1<>j- -~
~
- --
-,
Mcrvirt:;l AV8'I.!ge
r r
O IJ.'m~c
Sa.. .itzky.(iOOy
Order.
r
F~ler ~idth: ~ [teretionc: 6.ppl,Y
I-
11"
Close
Filter Width
The Filter width dialogue box con tro ls the num ber of samp les that are to be taken into account w hen using the Moving Averag e smooth ing method. A filter width of 2 means tha t 2+1-t-2 samp les are tak en w hile a filte r width of 5 means that 5+1+5 sam ples are taken. Ite rations
The Iterations dialogue bo x con trols the number of times a sm oothing meth od is to be appnec to a chromatogram peak. Eve ry iteration smoo thes the data line more than tre previo us iteration eventually making the data line flat.
PeCi.l<.NTco::;·12,put:
493 (of 550 ) 2006(-2016)
494
,!
.IE ~
I
•
~!
I
6
•
February 1, 1999 1) PeakS imple for Windows software and Chromatography Data System ( PeakSimple) is written, manufactured and maintained by SRI Instruments, lnc, a Nevada Corporation. --....
2)
PeakS imple for Windows software has been under continuous development
since 1994. Periodic testing of the software is perfonned by SRI employees. 3) PeakSimple software is designed to be se~-va l idating to enable quick verificat ion by customers that PeakSimple is functioning consistently, reliably and ac-
cording to specifications under actual operating conditions. 4)
Self-validation is perfonned by configuring PeakSimple into the "Loopback
mode- ( see loopback instructions in manual). In this mode, an actual user gener-
ated chromatogram which is loaded into channel 4 is re-played ( like a tape recorder) through the TP2 output channel, and then re-acquired and processed
through anyone of the remaining input channels . This is done 7 or more times to insure that data is being processed consistently and reliably. The results from multiple loopback analyses are used to calculate the percent relative standard deviation ( precis ion ) of each peak in the chromatogram. Chromatographic data is highly variable, and the precision obtained is dependent on many factors including the peak shape, signal to noise ralio, interferences, co-€Iuting peaks, data acquistion rate and customer selected integration parameters. For this reason, self-validation is more valid than factory validation, since self-validation takes into account the exact chromatographic conditions and user specified parameters in effect for the particular application whereas factory validation can not.
man15l.pub
494 (of 550 ) 2006(-2016)
495
Getting Started In this section, we will cover the basic information needed to set up proper commu n ication wit h your G.C. or Data System hardware. The Windows v ersion of PeakSimp le requires the use of the serial port interface tha t is built into most 8610-C and Model 310 gas ch romat ographs. This data acquisition and interface unit permits you to acquire up to fo ur separate ch annel s of data simultaneously w ithout the need for additional ha rdware or acquisition boards .
~PnkSl ...pl. f.. WI.do-
BOo f "
y, ~
_le ! x !
".,
~lMrlio ~
1DONG BTIX Ch . 1 electo r
c.
20'.00'
Yl'9 561l2 .d u
Ol~ ~
Boo
~ ±J
-
,...
l .C
aluen ltrylbennne
"'
IOfobcnzen
.
-ZUll O
~ I ". 1 ' .080
p-Didl lorob
r
..!..!!l!..I
I
' .OD~
The earlier IBM PC-compa tible ISA expansion bus data acquisiti on cards (AD100 and AD1 10) us ed by PeakSimple 1/ and PeakSimple III data systems are not supporfed by PeakSimp le for Windows . However, all chromatograms acquired using DOS-based PeakSimple 1/ and PeakSimpl e 1/1 continue to be compatible with th is W indows version and may be imported as native fil es.
Identifying Your COM Port Before attemptin g to establish communication between your G.C. and the seria l data syste m interface, be sure to check that all the necessary electrical connections have been made, including the connection of any optiona l rem ote start cab les. Select an unused serial port on your PC and identify the COM port number assigned to it. It is important that this port NOT SHARE AN INTERRUPT with any other device used in your computer. Typical PCs are equipped with two COM (or serial) ports. COM 1 is typically used by the mouse or some other pointing device. COM 2 may be open (unused) or shared with another device, such as a fax modem, scanner or other periphera l. Determine which COM port you will use and rem ove any other device that may be in co ntention with that specific COM port number. Refe r to your PC's hardware manual fo r instructio ns on changing COM port address es and device drivers. Mos t COM ports are provided with D8-9 conne ctors (ni ne p ins configured in twa rows 5 pins over 4 pi ns - within a D-shaped plug or chassis connector). If your PC has a 08-25 serial port (25-p in connector), you will require a OB-25 to DB-9 adapter.
l,.fo o oo oo ooo oo o~
''-'\ooooooooooocl'DB-9 Serial Port Connector
08-25 Serial Port Connector
495 (of 550 ) 2006(-2016)
496
Establishing Communicat ion The cab le provided with your G.G. or data system has a male 08-9 plug on one end and a female 08-9 connector on the other end . Plug one end of this cable into yo ur available computer COM port and plug the other end into the G.C, or Data System DB-9 conne ctor and tighten the retai ning screws. Plug your G .C. or Data System into an approved GFCI protected outlet and turn the power switch to the 'ON' position. Start Pea kSimple by double-clicking on the PeakSimple icon ( or by clicking 'Start', 'Programs', 'PeakSimple' in Windows 95 ). Whe n PeakSimple loads, it will automaticall y attempt communication with your G.C. or Data System using COM 1 as the default COM port. If the serial port interface does no t respond, you will see the following error messages appear on the screen: "Can't wake- check power and cable" foll owed by the message "Acquisition system is not funct ioning".
PeakS imp le for Windows Acquisition
sy~tm
is not lunclwning
'5
_._ --- .___ _-- -----0._- .::::==:
..._ - . t-o lD _ _"'" I!OIO
t!~,. r
These messages indicate that your computer cannot communicate with your G.e. or Data System through the default COM port, COM 1. You will need to set up the correct COM port in PeakSimple. To do this, click on the EDIT pull-down menu and select OVERALL. Change the PORT NUMBER to the COM port into which you chose to plug your interface cab le. Click O.K•. If at anytime you wish to force PeakSimpJe to reinitialize communication, click on the ACQUISITION pull-dawn menu and select RE-INITIALIZE. If the COM port information is correct and communication errors still appear when the computer attempts to activate the serial port interface . check the serial port connections at both en ds of the interface cable for loose connections. Also , visually check the serial cable for nicks or cuts.
..
. ..• 0 ...
~,
_
..... _ _ 1
--~ ~=
0 _ _ ._"_
-11'5'"""
...1I'ii"""
0 ........... _
0 __ -
0_
.. _ _
1--- ---, _ ....._....-.... _.~ r .............-1 • r ._ _ •
_
l!! PeakSimpia for Windows
A·li""n tlelp
t.~ Edil y.RUN' 512.000
-ZS6.00 0 '-----------~-'
.!..W.ill 0.000
~ 1.00ll
It is important to understand that in order fo r PeakS imple to communicate w ith your G.C. or Data System, at least ONE channe l must be ACTIVE. To determine which channels are active, click or) the EDIT pull-down menu and select CHANNELS. A channe l is active if the box next to ACTIVE is marked with a checkmark. The EDITCHANNELS menu is described in gr eater detail in the EDIT section in this manual.
496 (of 550 ) 2006(-2016)
497
Chapter: PeakSimple Topic:
Installation of USB drivers for use with Model 302 USB data system On t his com p uter the CD is in the
Install PeakSimple softwa re from the installation CD or from a down load from SRI's website http ://www.srigc.com. T he download is a zip file which must be un-zipped using PKZip or WinZip. From the Wind ows RUN comm and click on setup.exe in either the CD drive or the directory where the download was saved.
..
~-
At the conclusion of the PeakSimpIe software installation. there will be 3 important files saved to the applicatio n directory. The application directory could be c:\Peak2000 or it could have another name which you specified during the installation. The 3 import files are named LL_U SB.inf, LL-U SB.sys and LL_USB2K.sys. These tiles are required to make Windows recognize the AID board connected to the USB port of the computer.
E:\ drive
,
'
1 !~
., OK
.e.~ - _.
Ca"'Cel
..._ -- ......- ...... ~
...
--_.""'.
"",Z Ii'J " ="' ::::"'!!O'~l~·~ .::_ _..._.M .....__
Click on the W indows My Computer icon and then Control Panel and then on Add New Hardware.
Click on the NEXT button several times until you get to the screen which allows you to select hardware from a list. Scroll down the list until you can Glic.k. on Unlvcl ::>dl acrid l 6u ~ controllers
\12l1262.pub
r Y" iR_ (e ~ WCfll
toseect the har£tw~aiSiJ
~ S,.,tern """=
.r:~
Tece tb>e
eont:oIefs
,~ U~ Serial Bt4 caIKEI -" \tI) MModem El'lUl'Jel'dto'
Pagel
497 (of 550 ) 2006(-2016)
498
Chapter: PeakSimple Installation of USB drivers for use with Model 302 USB data system
Topic:
From the followin g screen clic k on the button Have Disk
-
Browse to the Pea kSimple application directory ( Peak2000 or other name you have chosen ). The Installation Wizard shou ld be able to find the LL_USB.inf file.
I~ ·
tlt C:"i
'T" -.:.
:;;;jI'tOkW
I
-.
.0.1 0",,-_
.:J
I ....J C':
•
When you click OK, the W izard will ver ify that you wa nt to copy fiies from the PeakSimpie directory.
x
f "
Imelt the mcniactl.l'er':t ~ Osk no the drive selected. d'"d then click OK.
I:__ A OK
ConreI
--
I, !
_ --_ ---'._---.. _-".,.
... . ...
...
~
...
... ;m.\1a:l262 .pub
Page :!
498 (of 550 ) 2006(-2016)
499
Chapter: PeakSimple Topic:
Installation of USB drivers for use with Model 302 USB data system ? !~
You must RESTART the COMPUTER before the ' drivers will work.
;-
:M:S73SI(3)X PO Audo O~ :lOS Mode",PU-4C'1 EII"IlktgCi.:m:"pal JO}Stick
V.'d'flil. Duvn: f"' .....rn::.. Modem
1~-~.; ::~~~':::B~ro"""O'
Once the computer has restarted right click on My Computer and ;examine the System/De vice .-i-"!'~ 'Manager Scree n. If the USB 1drivers have been successfully ;installed, the Unive rsal Serial Bus Controllers sectio n will list lawson Labs Mode l 301 version 04.
ATEN USB In Se1~ l:a>1e
~wsonl~ M 00eI 301
VetSio!1()11 NEC USB O;len Hoot Ccm~olCl I l)o.l
NtC USSO~ H~Conkobef[E 1H
SiS 7001 PO tQUS~ Cpen HO$l. Cort:ob JS6 Roct Hoi>
USB RoctH
USB R«t K..e
R.......
I (;.-<0 1
You can now launch PeakSimpie. Each USB data system has a unique USB device numbe r which must be entered into the Edit' Overall window in PeakSimple. The USB de-
Enter the US B device 1. 0. number in Pea kSim ple's EdiVOverail screen.
r~~~~~~~~~~~f---~-~4
vice 1.0. is listed on the back of each GC or stand-alone data system and will be a 4 digit number start ing with 5 ( 5031,5032 . etc. ) Once you enter the number PeakSimple will attempt to wake up the data system . Don't forget to click the SaveAIi icon so you don't have to reenter the USB device 1.0 . again.
~1
p<>al<'ion'i\:,.,.".b\t -
- g,~ .~ -- -
Mrr~ £\'1
- Noot>...
~ f\.
· D-'<::
_·
"If
NllOfle
" ~ name
~_ ;;_R_.... _·~_.... _· _
-
~ 0I'_ 1abe~
~ ~!i!- ~ p-:udol ~Otbolnl.lOl~ :QO
... be ~ed eo.
, - - - - --
M
MIll:;l.[OJ
Seaeh _ . ne b, jl lD Dtanal plloc:es-:
Sue t!W :.y
~'
!
I
- GF ....., ~
-
,
I'
13
~
Dec:nil ~ ~
;;:0--
--
I I'
q
~fan262.jJ ub
Page 3
499 (of 550 ) 2006(-2016)
500
Chapter: PeakSimple Topic:
Ope ration of serial port Models 203 and 202 on computers with USB ports only
So me Windom co mputers sol d afte r 2001 may not have serial ports. Th ey will have USB ports. To operate a serial port N O board from a computer with only USB po rts. an adapter is required . SR I has tested the lOG EAR www. ioqear.co m Model GU C232A and found it to be comp atible with Pea kSimple software.
Fo llow the installation directions which come with the logear product, then examine the My Computer/P roperties\Device Manager screen and click an the Ports icon. The serial port may be assigned to Com 5 which is only supported by vers ion 2.83 and later PeakSimpie . Do wnl oad t he lat est PeakSimp le version fro m SRI's website http://www.srige.com if neces ~
,
.;
"-~bJ~
- V- ~ ~~ ....
3li€2J • d:J IX fjl}/oj " ~ l)IEk _ i ~ ~ .ld6P'''''
~
<3
Fkl~ ~
cmro..~
0: -3 Herd (jli: conlttole" "- .~ ~o.,.""" .jj ~
; ,.. i;;J 'l
/. e
1olG"li""
li~~=~~,
~ -;l ~ o"' ~ itm~ l l EO' Pnntef ""'" llPT1] ,.,.J USB tD S..... F'l>1 1O'JMJ,"
--.:J
I- ...
~- ,- ~
..
." .. -~-_ . .. _~ _..
-.. '- "'= - --'---"= c rick on the Ports icon to see wh~t comport was assig ned to the USB adapter
:\1Ul:!6 1.pub
500 (of 550 ) 2006(-2016)
501
Operation of Menu Bar PullDown Menus All PeakSimp Ie for Windows features may be accessed from puJldown menus. When you click on a menu bar item, a pull-down group menu will open to permit navigation to specific group features . These pulldown menus may also be opened by pressing the key and the letter key corresponding to the underlined Jetter in the menu bar item name. For example, to open the EDIT menu press and the letter "E" (This is not case sensitive).
fAO- _$TAN() BY
:.! 1
The FILE Pull-Down Menu The FILE-NEW feature will clear the display of all active channels in the Main timebase without starting a new chromatographic run. To open a previously saved chromatogram file , select FILE-CPEN. A LOAD CHROMATOGRAM FILE screen will appear which will allow you to select any file from any directory
(folder) on your system . Choose the channel (1-4) in which you wish to display your saved chromatogram and than click OPEN .
FILE SAVE The FILE·SAVE feature saves the displayed chromatograms of all active channels. The name given to the file(s) is the same name that is displayed in the Data Boxes below the menu bar and will be given the default. CHR extension. This file name is editable by the user by changing informalion in Ihe EDIT-CHANNELSPOSTRUN pull-down menu . See the EDIT section for more information.
F ,I ~ ", ~ I ~
a.
F1<1f;(l2
under tl' o p .........
...
,""l. '
501 (of 550 ) 2006(-2016)
502
The FILE-SAVE-AS Pull-Down Menu To save a newl y created chro matogram file . select FILE-SAVE AS . A SAVE CHROMATOGRAM FILE scree n will appe ar which will allow you to save the file in any directory (folder) on your system. Type a name up to eight characters into the File Name box and choos e wh ich channel (1-4) you wish to save and than click SAVE. The file will be saved as a binary file by default. with a .CHR extension. You may also select to save the file in ASCII format with a .ASe extension .
The FILE-SAVE-ALL Pull-Down Menu The FllE-SAVE-ALL feature will automatica Uy save your chromatogram as a .CHR file; your temperature program as a •TEM file; yo ur com ponent table as a .CPT file; your event tab le as a .EVT file and then save s them all under a control file (.CON file). DEFAUlT.CON will be used if no other name for the control file is specified using the SAVE-CONTROl FILE fealure. All print information is also saved when you save a control file.
The FILE-PRINT Pull-Down Menu Numerous fields are available for print information. When you access the FILE-PRINT pull-down menu you will notice that any combination of one to four chan nels can be printed out on a single sheet of paper simply by marking the circle next to the channel number. Print informatio n concerni ng the header, chromatogram and report can be easily ed ited .
502 (of 550 ) 2006(-2016)
503
The FILE-PRINT Pull-Down Menu (CHANNEL 1) When you access the FILEPRINT pull-down menu you will notice that you can select to print any combination of multiple channels by clicking on the circle next to the word multiple. You may also choose to print individual channels by clicking on the circle next to the desired cha nnel. Click on Channel 1 to edit the Channel 1 information in the Print Header, Print Chromatogram and Print Report For-
mat fields. Rather than enter unique information for all four channels , you may wish to che ck the Use channel 1 fo rmat for all channels box.
PRINT HEADER FORMAT Clicking on the Print Header FORMAT button will allow you to customize the appearance of your printed chromatogram header. Input your Laboratory name, Analysis method,
Sample type, Column, etc and check the box next to each field.
Analysis date prints the date in your PC's BIOS.
Print out Temperature Programs, Events and Components file names by checking the ir boxes: or clic k on List to print the comp lete Temperature Program, Event Table or Compo-
nent List. Copy from: selects which channel will provide the List informa-
tion. Check the Comments box and click on Comments ... to enter custom ized information about your analysis. You can cha nge the Font, style and size of your printed text by click ing on the Font box. Select a size that will
provide readable text while still leaving room for your chromatogram and re-
port.
503 (of 550 ) 2006(-2016)
504
PRINT CHROMATOGRAM FORMAT You can also edit the chrom atogram print parameters whe n you access the FILE·PRINT pull-down menu. Check the Print Chromatogram box and select Fonnat. The Chromatogram format screen allows editing of the chromatogram Start time and Stop time and the Min and Max mill ivolt lev-
els. The Chart speed setting will determine the size of the chromatogram section of your printout. A sett ing of 1.0 inches/minute for a 5 m inute chromatogram will produce a 5 inch chromatogram print. You may need to experiment with this setting to fit your header, chromatogram and report information all on one printed page. W hen the Use screen limits box is Checked only the displayed section of a chromatogram will be printed. The Draw retention windows box allows for retenti on windows to be printed as well. The Labels section of the scree n lets you select what useful information will be printed along the borders of the chromatogram , and above the peaks. Clicking on Left margin , for example, will bring up the Edit format screen which wi ll allow you to select from a list of measurements which will automatically be calculated and printed in the left marg in of your chromatogram . T o cho ose RSD. for example, click on RSD from the left column and then click on the right arrows (»). RSD will now appea r in the selected column on the fight. ClicK OK to Close the window. Edit On peaks and Right margin in the same manner.
..... Pl'13.pub
504 (of 550 ) 2006(-2016)
505
PRINT REPORT FORMAT
..
A report may be pri nted along with your chromatogram to summarize component retention time , area co unts
or other data. Clicking on the View pull-down menu and selecting Results will show a preview of your report.
-~- -.
'i:!lI""-=E__. TJi- ;-;;~
..,
~~'jc'" "~ :i:.:rl-:E£'
-,,,.,,~±;_.,,.~
" ".-~'= "'''.-'l ;
_
Click on the Print Report box and select Fonna!. The Report Format screen will appear wh ich will allow you to select from a list of meas ure ments which will automatica lly be ca lculated and printed on the bottom of your ch romatogram. To choose AREA, for example, click on AREA from the left column and then click on the right arrows (»). AREA will now appear in the Selected column on the right. Clicking on the box ne xt to Recognized peaks only will place a check mark in the box and only those peaks which integrate properly with in nam ed retention windows will be printed in the report. Checking the Peaks on printed chromatogram only box will
allow the report to show only those peaks defined by the Chromatogram format- Start time and Stop time, This feature allows you to set up your report to ignore all peak s that appear outs ide your window o f interest Checking the Undetected components also box will report information about all named peaks even if no peak is present within the retention window . Checking New page for report will print all report information on a separate page. Click OK to close the Report format window. You may print out as man y Chromatogram Copies as you need by entering a number in the Copies box and selecting Print P,,-·p&H pu!>
505 (of 550 ) 2006(-2016)
506
The FILE-PRINT CHANNEL Pull-Down Menu After all Print parameters have been set up, the easiest way to print out a chromatogram is to use the FilePrint Channel quick keys . Hold down the Ctrl (control) key and then press F9 (function #9) to instantly print the Channel 1 chromatogram. Press Ctrl F1D to print Channel 2, Ctrl F11 for Channel 3 or Ctrl F12 for Channel 4. Of course you may also sele ct these commands from the pull-d own menu.
The FILE-PRINTER Pull-Down Menu
SETUP
Selecting Printer setup from the FILE pun-down menu will allow you to enter the Prin ter Properties screen
for your specific printer. This screen is similar to W indows Printer Properties screen that is access ible from the W indows Control Panel. Typi cally, us ing your printer default sett ings with portrait orientation will produce a visually appealing printout.
The FILE-OPEN CONTROL FILE Pull-Down Menu PeakSimple for Windows uses Control Files, identified with the .CON extension, to save the operating settings of specific methods. To load a Control File, drop down the FILE menu and select OPEN CONTROL FILE . A window will open which will allow you to use standard W indows navigating tools to select from a list of .CON files, located on the Drive or Directory of your choice . Click on the desired File Name and then click O.K.
~~E~=~
- .!'l loftoO _
.~ :!! o
.!!I ""-
506 (of 550 ) 2006(-2016)
507
Th e FILE-SAVE CONTROL FILE Pull-Down Menu Once you have set up all of the user-definable parameters within PeakSimple for Windows that meet the requirements of you r system andlor your specific analytica l method, it is wise to save these settings for future use . PeakSimple uses control files, identified with a .CON extension, to save the operating settings of specific methods, this includes the event table, temperature program, component table , print information, calibration tab le , etc.
..
>- -
.-!"!'-
'ii~;~~ffi,~~ '~~1
e.
~ ' ,", . O _ .
.;:~. •m;~~~~t"
...
~~~~~l.~~ ,"'. ~
-
,.
,
e
OM
~,-
- -
"- ,~~:-,-,-,-
....- , . ':: ~:~ :
-
...."
-
e e
-
..
e
----:.....
-
-
.0
';;;:;'•.= --':..;...,., ..!
.±I3
E• ,',1'1' ' , ''''''~' ''''''',;,. -.
A control file is like a photocopy of your operating settings that you can reload for use at any time. When using co ntrol files , you only need to set analysis parameters once and then
save them using a descriptive filename, followed by the .CON extension, (for example. BTEX.CON ). To save the co ntrol file , drop down the File
!l Oeld.Cl1I ~ VW1 tm !l V~ctIIl
- ~ VIdlJ.cm
menu and select Save control fi le. Enter the name for you r file in the File name box and cli ck O.K.. If you want these current settings to be loaded by default ea ch time you start Pea kSimpIe, name the control file Oefaultcon.
FILE-ALT NEW The FILE-ALT NEW feat ure will clear the display of all active cha nne ls in the Alternate timebase without starting a new chromatographic run .
FILE-EXIT Exits PeakSimple for W indows. Click Yes to save any changes made to your cont ro l file parameters.
Pw-w16 .....
507 (of 550 ) 2006(-2016)
508
The EDIT-CHANNELS PullDown Menu The EDIT pull-down menu allows you to modify most of the operating parameters for your specific appliselecting EDIT-CHANNELS cation. will bring up a screen which will enable you to select which of the four channels are active, displayed and inte grated. Each channels' operating parameters such as Details, Tempera-
ture, Events, Integration, Components and Postrun infonnation can be easily modified.
The EDIT-CHAN NELS -DETAILS Screen Clicking on the Details box for Channel 1 will bring up a screen where you can ente r a Description of your analysis. End Time displays the length of the chromatographic run in minutes. By default, the End Time is determined by the length of the temperature
program but you may modify this field to end the chromatographic run at any time .
The Sample Rate should be set to a rate sufficient to ensure that 20 data samples are collected for each peak. For example: A Sample Rate of 1 Hz wil l allow the collection of 20 data points from a peak 20 seconds wide from base to base . And a Sample Rate of 10Hz will allow the collection of 20 data points from a peak 2 seconds wide from base to base. The analog to digita l converter is limited in its ability to sample high rates when many channels are active. T he limits are : 50 Hz wit h one channel active, 10Hz with two channels active and 5 Hz with three or four channels active. The Default Display Limits can be adj usted to view data above and below the 0 mV base line. A minus (-) setting for minimum wi ll display negative go ing peaks. The ratio of min./max. display limits is maintained when you click on the Display minus and plus buttons in the main data acquisition screen. The Remote Start feature allows the user to start a chromatographic run using an external signal such as a footswitch. Check the box to enable Remote Start. (There must be an internal connectio n made to the AIO board in order for th is option to work .)
508 (of 550 ) 2006(-2016)
509
The EDIT-CHANNELS-DETAILS Screen (continued) Trigger Group The Trigger Group selection assigns the channel to the Main or Alt trigger group. The picture at right shows the Channel 1 Details screen with the Main Trigger Group selected . Any Channel with the Main trigger group selected will start runni ng when the SPACEBAR is pressed and end when the END key is pressed . Any Channel with the Alt trigger group selected will start runn ing when the + (plus) key is pressed and end when the - (minus) key is pressed. W hen acquiring four detector signal inputs from one gas chromatog raph; verify that all four channels' Trigger Group is set to Main. This ensures that all four channels are acquiring data synchronously by using the same timebase. If two channels of data are coming from an SRI gas chromatograph, and you also wish to acqu ire two cha nnels from an external input device such as an
HPLC, then select the Alttrigger group for channels 3 and 4. This allows for asynchronous data collection.
Subtract Baseline In Channel "X" Checking Channel1's box for Subtract Baseline In Channel "X", where "X" is 1,2,3 or 4, will cause the chromatogram in Channel 1 to subtract the baseline stored in Channel "X" , while running in real-time. Load the baseline to be subtracted into an inactive channel to ens ure that the data is not deleted by the start of a new run on that channel. (Uncheck the active box, see Edit-Channels). Baseline subtraction can also be perfonmed using PeakSimple's Edit-Subtract/Add Channels feature, however, this is not a real-time function, but a post-run function, done at the end of the chromatographic run.
Overlay Data In Channel "X" Checking Channell's box for Overlay Data In Channel " X" , whe re " X" is 1,2,3 or 4, will overlay the data stored on Channel " X" onto Channel 1 using contras ting colors. The channel selected for over1ay can be either an active or inacti ve channel. Whe n the overlay channel is active then the overlay will be seen in real-time .
Relative Retention Shifts Are Based At " X" Minutes Relative Retention Shifts Are Based At " X" Minutes. Enter into this box the time, in minutes, that the sample is actually injected onto the co lumn . This is done to ensure that relative retention times are correctly calculated . See th e EDIT-CHANNELCOMPONENTS section of this manual for more details.
509 (of 550 ) 2006(-2016)
510
The EDIT-CHANNELS-DETAilS Screen (continued) Unretained Solute Time If resol ution has bee n selected to be printed in the chromatogra m report. then a Unretained Solute Time value needs to be entered to ensure correct resolution cal cula tion s. Enter the number of minutes an Unretained Solute takes to pass through the column. This va lue is used in the determination of pea k reso lutio n statistics.
Control By The AID Board that is built Into the SRI gas chromatograph includes two digital-toanalog co nverters or DACs. DAC1 is primarily used to control the column oven # 1 temperature ramp by introducing 10mV I °C to the oven heating circuit and is programmable by editing the Channel 1-Temperature contro l window. DAC 2 is primari ly used to control the co lumn oven #2 temperature ramp . Carrier gas E.P.C. pressure is al so programmable by editing the Channel 2-Temperature/Pressurc control wind ow . The OAC s may be used to control Pressure by following the procedure described below and the n select ing Pressure in the Control By window of the Edit-Channels. Details screen. To avoid startup difficulties , the Carrier E.P.C. is shipped disabled . To enable the use of the DACs to set up a Pressure Program , only a single wire 1············ 1 need s to be moved inside the G.C.. ~ ._--
•
,
,
•
__ --_,,-
;lit
I········.··· .. ,
stripe on the AID Board. This is the
.
.,j. ... ..'.. .....
i'iliIJl
$INGlE CHANNEL
IIIOll!1. 203 A'O II(I.U D
-
...
~
--_..... ---_ _
Unplug the G.G. and remove the six screws wh ich secure the bottom cover. Tilt the G.C . onto its back and rem ove the bottom co ve r. The AiD Board is green in col or and is mounted on the right-ha nd side of the G.G. chassis. Locate the Green wire with a White
...."'_.-.... ......
!········ I
.
Carrier Program wire. Nonnally this wire is con nected to a ground (GO) screw term inal. Unscrew the Carrier Program wire and co nnect it to the temperature/pressure #2 (TP2) scre w te rminal also on the AlD Hoard . Re-attach the botto m cover, con nect power and re-establish commu nication betwee n the G.C, and the computer. Select Pressure in the Control By window of the Edit-Channels-Channel 2·Detalls screen . A pressure program ramp set up in Channel 2 will now control the Carrier Gas E.P.C.
pressure by introducing 10mV for every P.S.!.. Tum the Carrier 1 Local Setpoint to zero. This is necessary since the Local setpoint is added to the progra mmed E.P.C . input in determining the Carrier 1 total setpoint.
510 (of 550 ) 2006(-2016)
511
The EDIT-CHANNELS-DETAI LS Screen (continued) Selling Up Grad ients for Chromatography
n -II..... .
£1
Liquid
Data System users may wish to use the AID Board DACs for setting up an HPLC solvent gradient. PeakSim pie for Wi ndows allows the user to control the flow of two pumps , provided they operate from a zero to five volt (05V) ramp input. To operate the pumps , several interna l connections must be made between the HPLC and the Data System. Unplug the Data System and remo ve the two screws which secure the top cover. Route the Pump A and Pump B control wires from the HPLC to the Data System and connect the Pump A control wire to TP 1 and the Pump B control wire to TP2. Re-attach the top cover, connect power and re-establish communication between the Data System and the computer. Set up the Gradient ramp on channol one (TP1 ) to control th e flow
of Pump A into the system (1OmV I '!o) and the Gradient ramp on channel two (TP2) to control the flow of Pump B. Modifying the Gradient ramp program on Channel 1 to rise from 10% to 90% will automatically create a Gradient ramp program on Channel 2 that decreases proportiona tely from 90% to 10%.
e-,
FOUR CHANN EL MODEL 202 AID BOARD
. , , . ""'"..."'"
-""""'~_Tl"""1o
I ••• •• •••
•••
+ - + - • • • •
" I
A WlIlE.- IP1 WU COIC THf. FI..OW
OF....- •.• _
fJIOL
_ ",~ lM.J. _
r--- I············I . .·.. II ,I ,I:
~ b · · ~· · · ~ ·
SINGLE CHANNEL MODEL 203 AID BOARD
1;·,..... 1 -1--
._.._...,...::."""....... lIT.
_
_ nrJNU-'u••
~
• ,
t.
•
A_~
TP2IM Ll CONTltOl
_
r-r-
li1i
I" •••••• , •
I •
• •
• •
~
J
T,.. flOW 01' 'UI . Z,
Gradient Limits Zero and Span may be scaled in the Edit-Overall screen to account for an y offsets. PeakSimple allows for a vott~ !J e o ffset
and scaling factor in these fields to calibrate the voltage output to match th e
pump's requirements.
511 (of 550 ) 2006(-2016)
512
The EDIT-CHAN NELSINTEGRATION Screen PeakSimple fo r Windows allows you to defJne specific integration parameters necessary for the proper ana lys is of
your sample data, such as peak and baseline sensitivity and area reje ct. Any of the Integ ration parameters described below may be modified either before or after data collection.
Pressing the ENTER key will update the report and the results of the chromatogram currently being displayed.
Peak Detection Sensitivity The Peak sensitivity setting determines how PeakSimple detects the beginning and end of a peak. A high Peak number requi res only a small sl ope change to initi ate the start or end of a peak . A low Peak number req uires a very large slope change to
initiate the start or end of a peak. SOl Vl:N
~n ~
..n..
fr·'·'
It"····
SOI.VE"I
Notice thai wilen
Notice that whe n Peak =
-~-
95. Be nzene is , Integrated .
J\
,
-
Peak = 25, Be nzene is riot
-,
~
.. ..
Integ rated .
) \,
The Baseline sensitivity setting determines how PeakSimple attaches the baseline to the data line. The larger the Baseline number; the more likely PeakSimple will draw the baseline to a valley between two peaks. The sma ller the Baseline number; the more likely PeakSimple will drop a vertical line from a valley to a horizontally constructed baseline be low the peak. . ToIu"".
~JlJ
C I
roi..u
""nL.m. /
T. I....
n.
~r" -"'-' V/ I
Baseline = 60 Baseline attached 10 valley of pe aks .
IS aropped to tho> h,,~ ...lrn..
/
~~I
Baseline = 10 A verti ca l line
, L
1\
)
i ~
-'-"- ' - -
Pw.ptl l pub
512 (of 550 ) 2006(-2016)
513
The EDIT-CHAN NELSINTEGRATION Screen (continued) Area Reject If a chromatogram contai ns peaks whose area counts fall below the threshold defined by the Area Reject for that channel, the peak will be igno red and no integration will occur. If the peak area is of interest , you can lower the Area Reject va lue until the peak in question is integrated . Integrated peaks are marked with a circle at the top of the peak.
~~~
The de fault Standard
Weight of 1000 and
Standard Weight PeakSimple for Windows determines the internal or external standard res ults by the ratio of the STANDARD divided by the SAMPLE .
the de fault Samp le Weig ht of 1 000 results in an 'nlernal standa rd of 10.000 lor
I
r~ :1 fl<.~. .~ ' .U l 1C'.Sf'J
The Standard Weight setting may be changed to adjust the channel's quantification, affecting internal or exte rnal peak results by the factor entered . For insta nce: A setting of 2.000 will double the weight of the sta ndard thereby doubling the internal or external standard results. (Increased to 20 .000 in the exampl e shown.)
Sample Weight
, .......
I ; ·,,~:;:~~ ....,.;:t~ .t . -_. ~ -.: ' ~ -
SOLV£lIT
A Standard Wepgnt of 2 .000 Ooubles the II'Il etmll sta noard res ults.
I'Wil:rl ~7f'nr ~ ,,:,
The Sample Weight setting may also be changed to adjust the channel 's quantifica tion, affecti ng internal or external peak results by the factor entered . For instance: A setting of 2 .000 will double the weight of the samp le thereby halVing the Interna l or external standard results. (Decreased to 5.000 in the example shown.)
/\-
\,
""
\ /\\
, .• • ,
14Z~" ZIUlOClll . ' .'
.
t
i-p'.,
_ • •• _
-_.~-
' ::c:~ ·~ ·;; ".j-~I·:;t •
. ".
'~ ."%;11.
SOlVENT A ~ Weig ht
..
of 2.000 halves the ,"Iemal standa rd ~
\\
AU ....•
\
f~
iiirJ' 1' ~..~~: l ,N ) 1 47. 5 49 5.00ll~ [;7~' ~~~;;::'~': ~i~l~ UIWL ' ••~" ~ , !:,~ ' ~"
513 (of 550 ) 2006(-2016)
514
The EDIT-CHANNELSINTEGRATION Screen (continued) Spike Channel Another feature of PeakSimp le for Windows allows you to display the results of a m atrix Spike Channel sub traction. Th e exam ple shown below demonstrates the peak area counts of a unspiked cha nnel being subtracted from the area counts of a spiked channel.
Before Spike Channel Subtraction ~=~".'.=._
4Utr
LT.COJF~"S"f ' Sf.
S LVENT
enzeneu· ~ !J
A I
.,;...
'
'
"
_ _ L
Notice th at the area cou nts for Benzene are 939 on the spiked channe l, and 242 area counts on the unspiked channel.
After Spike Channel Subtraction -
~
..-
- --
". -
.- E=;;?'..e"1:':-' "1:'::-:""' - ':::
,
.... """
un, w•
.,-"
~
~.
,~
..
- ioN "
'iN
,
~____ __
--
'l.n i
m .•
~~maf
After se lecting channel 2 as the Spike Channel, the area counts for channel 2 are subtracted f rom channel 1 to equal 697 . (939 - 242 = 697) . The difference of 697 indicates the area counts of the amount of sample spiked into channel 1.
514 (of 550 ) 2006(-2016)
515
The EDIT-CHANNELSTEMPERATURE Screen PeakSim ple for Windows fe atures temperature-proqramrranq of the G .C 's column oven(s). Access the EditChanne l 't-Tempereture screen to specify the temperature paramete rs to be used during the analytical run . The temperature program is capab le of executing an unlimited number of temperature ram p and hold periods during the analysis as well as maintaining a single tem pera ture througho ut the run for isothermal operation.
The Temperature Segment Details Screen The Add Button Click on the Add button from a blank
Channel 1 temperature control window to create a new tem perature program fo r Column oven # 1. (Use the Edit-Channel 2Temperature screen for controlling column oven 1t2). Type in the required data in the fo llowing fields; In itial temperature . the Hold period in minutes, the Ramp rate in °C I min , and the final Temperature, or the duration of the Ramp. The length of the run is automatically calculated by provided PeakSimple based the information in these fie ldon s, and is also displayed In the EditChannels..oetails End TIme field . Additional ramp segments may be added by clicking the Add button again.
,~=~~~~~!!:======~ I~
In isotherma l operation. the Initial and the final temperature are the same , so a Ramp rate of 0.000 is ""tered . The Hold peri od determines the length of the analytical run.
515 (of 550 ) 2006(-2016)
516
The EDIT-CHANNELSTEMPERATURE Screen (continued) The Change Button Click on an existing temp erature program seg me nt to se lect it. Click on
the Change button to change the parameters of the segment.
The Remove Button Click on the Remove button to remove the seg ment fro m th e curre nt program .
c.,;J.:tj"" ,· ..,;
;;--- - - ; c--,
The Load Button
,-~~"
••
,~
__
•.•
~
3@l ~mJ$J;1: .. _.•• .• , ~~
; .!l lOO'¥"in lem
:!J ChZt"'"
- ,:J £~~
Click on the Load butto n to load an existing temperature control file, designated with the .TEM file extension.
.!lGp _
, L
The Save Button Click on the Save button to save a new temperature co nt rol file. or to update an existing o ne .
Remember to
use the .TEM extension when naming the temperature con trol file. The saved file name appears at the top of the temperature control window indicating the file in use .
.:l l~
:l "" ~
: :J ~"'"""....
. .!!l lip _
The Clear Button Click ing on the Clear button deletes all temperat ure data from the temperature control window. The temperature program name is also removed .
The Print Button Clicking on the Print button sends the file data and tempe rature program profile to tne printer.
516 (of 550 ) 2006(-2016)
517
The EDIT-CHANNELSCOMPONENTS Screen PeakSimple for Windows can identify and quantify sample components through the use of a component table . The component table ena bles PeakSimple to recognize each pea k by its reten tion time and compa re the area counts against the ca libration curve to produce actual co ncentration data. The user can edit the component table for each channel by accessing the Edit-Channels-Components screen. When a component table is loaded , the table will show each component by its peak numb er, peak name, the start time for the retention window, the stop time for the retention window, and the associated ca libration file name. Different com ponent tab les may be used for each active chan nel and any compon ent tab le can be saved as a component file for future use. Component files are designated with a .CPT extension. The component file-nam e app ears at the top of the Components screen .
0:: -
COMPONENT DETAILS Select Add to add a new component to a blank or existing component table. The Component Details screen will ope n allowing the user to inpu t specific peak para meters. As a minimum, enter the Peak Number, Peak Name, Start time and End time . Other optional parameters are the Expected peak time, the concentration Units to be reported, any Internal Standard or Reference peak information, peaks measured by Area or Height, hand ling of Multiple Peaks, the MUltiplication Factor and Alarm parameters.
.~::~1~ ~:'~~~~ £:~ ~'r"":... .
0_00
::' ,Led:: 0 _00 :,
~
0_00
:'
;iG·~~4~~~~~~ ..
Pw-p~6 . pub
517 (of 550 ) 2006(-2016)
518
The EDIT-CHANNELSCOMPONENTS·DETAILS Screen (continued) Peak Number, Peak Name, Start and End A blan k Component Details screen is opened by se lecting the Add button. Enter a unique Peak Number for each component, typically starting with 1 and incrementing for eac h add itional peak. T hen enter a unique Peak Name for each component. Start and End defi ne the beginning and ending of the retention wi ndows, which is used to identify the peak . The width of the retention window should be set wide enough so that small fluctuations in the peak's retention time will still allow for proper integration.
~1~:~~±ct":f!:1,~ ~±~j!t;0~:~' ~ -
:~~,~~~1tT\:j~~
:, ~~~gNi;;L£:~~~:~ '-~..;..;;
~t~~~~i£ , ~~~;
Internal Standard and Units Intern al Standard calculations are used to correct for injection size variations, or to compe nsate for changes in detector sensitivity. An internal sta ndard pe ak is added to the sample prior to injection at a known co ncentration. The internal standard peak is calculated j ust like any other peak using a ca libration curve, typically a single point calibration. The known concentration of the internal standard peak is entered into the Internal Standand dialog box of the Component Details screen , In the example shown below , Benzene has been chosen as the internal standa rd peak. The known conce ntration of Benzene is ente red as 100. and ppm is entered in the Un its dialog box. Wh en a chromatogram is integrated and a report is produced, the externa l calculation yields a result which is the peak area x cal ibration factor (slope of the calibration curve) = external standard result. The internal standard calculation yields a result wh ich is the external result times the ratio of the known concentration of the internal standard peak divided by the external result for the internal standard peak. As shown in the example to the right, note that while the externa l result for Benzene yields 104.95, the intemal result yields exactly 100 (the known conce ntration) as a result of the calculation 104,95 x 100/104,95 In the same way, the internal resutt for every analyte peak which is referenced to Benzene is ca lculated as external result x 100/104.95 = internal standard result.
.,
518 (of 550 ) 2006(-2016)
519
SRI Instruments
PeakSimple 2000 Chromatography Integration Software
Basic Tutorial "l".- _ _
. ,.
....r,,;Ill' ..,
- , Ill ~_
• ,
• , • •
· >!, to'" ~~
.
-,
,
I
,
.• ~
;
Installing PeakS imp le 2000 from floppy disk or CD-Rom
Installing PeakS imple 2000 from software download
A
A. Start the Windows oper ating system and use a n online browser 10 access www.sng c.co m .
l
I
I
Start the W indows oper at ing system in use on
your computer. (Windows 95, 98, ME, 2(00)
B. Insert the PeakS :mple 2000 dis( or CD into your floppy disk drive .
C. Go 10the Start me nu in the bo ttom left hand corner of lhe windows screen and se lect Run from the set cf icons.
I ,0
B. From the menu on the left hand side of the screen select Down load our Software and then down load Peaks.mere 2000 from t he fOllowi ng pa g e. C.
save lhe file to a tempcrery fo lder and then double click en !I: from My Com p uter 10 a llow the program to see-ex tract.
From the run menu. type X:\setup (where X is the letter of your compu ters disk drive) . D. Once all the f iles have be en extrac te d successfully dc ubte-cucc the insta ll fi le a nd press the Continue E. New click on the Continue button with your butto n w!ler. pro mpted. mou se Cl.XSOf" or press lhe enter key 0:"1 your keyboard 10 beg in insta llation. E. Fol low e e c nscreen insuuctons to com plete th e in. staUation of Peak Sim ;>le. To complete installation follow the onscreen instru ctions pro vided by the installat io n wiza rd.
i
IF
SRI Instru ments 20720 Earl Street Torrance. CA 90503 U.S.A Telephone: (310) 214·5092 Fax: (310) 214-5097 [email protected]
519 (of 550 ) 2006(-2016)
520
Launchin g PeakSimple 2000 1. Clic k on the wi ndows Sta rt button in the bottom left-hand comer of th e screen. Se lect Prog rams and then PeakS im ple from the list of program grou ps on the scr een and then click on PeakS imple.
-. --
~ --
--
2. Th is wi ll la unch PeakSimple and initi alize the data acquisiti on system.
M
~ - -
. ~ ~
<-
_
-
~
._--
e
•i
.. -.-
.-_....
I~
1""-.::'7:: '",
~_
5
4. Most of the commands and optio ns in PeakSimple are equipped with tool tips that will automatically pop up to disp lay useful information whe n the mouse cursor is hel d over a command. To tum off the too l tips desele ct the tool tips option in the Help menu.
---_ '.' . _
< .
, ."
' ...
, ~, ,", .
. ..
Open ing a PeakSimple Data File .
, ·h
~
,, _ _
-
_
,,~-,-. _
..._
~
.
-,
_
_
,
...
. _'. ~
, _
.
, . ,'
. . ,~
~
.
-
~~
1. To open a Pea kSimple data fil e or chromatogram, beg in by selecting File in the PeakSimple men u bar and then choose Open .• . from the set of options.
,
~
..... 0.1 ... ~" :'JT
::J
:.:;:; m::;;::
J:"' -. , .'
,
~ "t;". _
_.
-
.2. The Load Chroma togram File wind ow is now open. The PeakS imple software indudes a nu mber of sample chromatogram data files that can be o pe ned, displayed , and manipulated. One file, 602.CH R, will be used throughout the rest of the tutorial. Sele ct file 60 2.CHR from the PeakSimple directory, choose Channel 1 as a destina tion channel, and then select Op en to loa d the file .
. J'", _
. _.. _.".,.., .. """"""." """'
. " -'
L "
~
.••
1
,
_. . •
;0._
""",,, r -
o .
.-T'-'
.. , ••
., • ,
-----"",;
- .--
j
,
-
I
520 (of 550 ) 2006(-2016)
521
Adjusting Display Limits 1. To adjust the display limits of a chromatogram click on either the T magnifyi ng glass icon or the - magnifying glass icon to the left of the chromatogram. This 'Nil! increase or decrea se the limits by a factor of two each time you click on the icons. 2. After opening chromatog ram 602.CHR, practice making the display limits smaller bu t the peaks larger by clicking the + mag nifying glass icon.
-
3. Practice making the display limits larger but the peaks smaller by clicking on the - magn ifying glass con.
. ....
~
- - -~
Zooming 1. To zoom in on a specific pa rt of a Peak Simpl e chromatogram , click and hold the left mouse button and drag it over the desired area.
~
i
2. After opening chromatogram 602.CH R hold the left mouse button and drag it over the base of the toluene peak. let go of the mouse button and there will be a larger view of the area that was selected. 3. To return to the original display limits of the chromatogram and unzoorn the area selected press F6 or select the unzoom icon located in the PeakSirnple tootbar at the top of the screen.
.. '"
.
521 (of 550 ) 2006(-2016)
522
Dragging Retention Windows
_..
: .- -
1. To drag a retention window bar place the mouse cursor on the bar until a double sided arrow pops up. Click on Ihe left mouse button and hold and then drag the retention window bar to its desired place. 2. After open ing the chromatogram 602.CHR zoom in on the benzene pea k and the smaller peak to its left. Locate the benzene retenti on window bar and dra g it over to the sm alle r unnamed peak to the left of the benzene. Because this is a sma ll peak it is not imme diate ly recognized .
3. Right cl ick on the chromatogram over the unnamed peak and select Integ ration from the
t- -
resulting menu . 4 . From the integration window locate the Area Reject d ialogue box, erase th e 100.0 in the box, and add the number 10.0 to the dia logue box, Click OK and the integ ration window will
• "
---
-
~T
•
exil 5. Press the Enter or Return key on your keyboard and the sma ller peak wi ll now be recognized as Benzene.
-
--
""... -". r
r,
"' r , I~' ~
-.
r,
.. .;
"-~~ Ol
I
Co.-,...
-
I
--~--
......... ,. -
522 (of 550 ) 2006(-2016)
523
Manual Integration
-
1. To man ually adjust the integration baseline and peak separation in a chromatogram use the manual integration toolber provided by Pea kSimp le. To open up th e manual inte gration toolbar select Ed it in the PeakSimple menu bar and then click on the Manual Integration op tion . The manual integra tion too lbar will now appear to the left of the chromato-
gra ph . 2. The manual integ ration toolbar con tains nine types of manual integration options. Four of th e most commonly used options are None integration, Drop integrat ion , Based integration, and Ru bber Ba nd integ ratio n. 3. T o make a baselin e ignore a peak use the None integration tool. After ope ning chromatogram 602 .CHR and the m anua l integrat io n toolba r, zo om in on the baseline of the solvent peak and the smalle r unrecognized peak immediately to its right. Click on the No ne integra tion tool in the manual integration toolbar with the mouse cursor and then click on the valley between the two peaks where they me et the baseline . The area of the small peak is now added to the solvent peak.
4 . To undo the changes made to a chromatngram at any time simply dick on th e Undo integrati on tool in the manual integration tool ba r. After selecting this tool all integration changes made to the chromatogram will be undone.
• --".
-~----
[3 01
5. O ick on the Undo tool with you r mouse cursor and select the Drop integ ration tool to en-able the dropping of the ba sel ine below the between th e two peaks. After selecting the Drop tool d ick where the va lley of the peaks meet the baseline with the cursor. The baseline shou ld now be dropped below the base of th e peaks and a line should extend from it to the baseline.
523 (of 550 ) 2006(-2016)
524
6. After the ma nual integration between the two peaks is dropped use the Based integration to ol to ra ise the baseli ne to the valley between the peaks. Once the Based integration tool is selected . d ick on the valley between the solvent peak and the sma ller peak to its righ t with the mo use cursor. Th e baseline will now extend up to meet the valley of the two peaks.
7. O nce again click on the Un do tool in the manua l integ ra tion toolbar to remove all changes done to the chromatogram. select the Rubber Band integration tool to manually draw a baseline. Once the Rubber Band too l is serected take the mouse c ursor and click on a part of the baseline. Wh ile holding down the left mo use button ex tend the line to ano ther part of th e baseline further to the right of the sta rting point and let go of the mouse button. Th e base line will now be drawn according to the line tha t was d rawn using the Rubber Band inte gration tool.
J
Calibrat ion 1. To tum th e raw area of a peak into a realworfd number the peak first needs to be calibrated. To cal ibrate the Tolu ene peak in chromatogram 602.CHR, open up the file and then right click usi ng the mouse on the Tol uen e peak. After right clic king on Toluene select Cal ibrate Toluene from the resulting menu.
-
2. Fro m the Recalibration level window click on the third level radio button 3 (100.000) and then se lect O K with your mouse curso r. "'GO. ::i.I:t.
as.;)
Ti>·
'f'. :
.. ;<.~
..
ii!:~
rIi.t.:.~~
;- l l'4w.l - ... } ;7l'J(I;>r.
t...
rr-
o:
I :,..,,,
I
524 (of 550 ) 2006(-2016)
525
3. Afte r selecting OK from the Recalibration level menu the Calibra tio n menu for T oluene will pop up . Check to make sure the flashing asterisk on the calibration curve is on Jevel 3 and then d ick on the Accept New button to the right of the window.
------
4. Once the new data is accepted, click on the Method button immediately be low the Accept New button. The Recalibrat ion type window will now open allowing the user to select a meth od of calibration. By default the calibration type is set at Muttiple Line Seg ments . lect the Quadratic (Ax2+Bx+C) radio bulton and then click on OK with th e mouse cursor.
, ....,.,- .,.....
se-
~....,..,_
-..'M
-.,~~":I r ,
5. After changing th e me thod of calibration click on Statistics in the upper right hand comer of the Calibration level window. The Calibration statistics window will pop up revealing the statistics for the calibration of Toluene. Glick OK with the mouse cursor to close the Calibration statis tics window and then se lect Close from the Calibration window to fin ish calibratin g Toluene.
-.,,,,'
~- .
- ,_., ~
-"' ~""
",. w
...
(,"" ..._.,-: , ~
~
Overlay 1. To com pare two or more chromatograms overlay th em usi ng PeakSimple. To overtay two chroma tograms first open chromatogram 602.CHR and then click on th e 2 button in the PeakS imple toolba r. A second chromatogram channe l is now open in the PeakSi mple window. 2. Once the second cha nnel is open select File from the PeakSimple menu bar and then d ick on Open. The Load dlromatogram file window wi ll ope n up displaying a list of files to load. Select chromatog ram FID602.CHR to load and then select the 2 cha nnel radio button to loa d the chromatogram in the second channel.
££Ct , __ .
525 (of 550 ) 2006(-2016)
526
3. Once FID602.CHR is open in the second channel right dick using the mouse on the chromatogram in the first channel and select Channel Details from the list of options.
4. After the Channel 1 details window appea rs . on the screen locate the Overlay data in channel check box and select it. Look to the dialogue box to the right of the Overlay data in ch annel check box and insert th e number 2 in place of the 1. Click on OK with the mou se cursor to exit the Cha nnel 1 details window. 5. The chromatogram FID602.CH R is now in place overlaid on top of ch romatogram 602 .CHR in channel 1. Chromatogram 602 .CHR is in blue while FID602.CHR is in red .
--- -.. - ..-.
·. -
r
.,.---
'-
o
·
-
.
_
--.
",
-~.
_:C::='::~~~r~ ,.~ ~
.-..
~
J
.. ..
.
~
,
~ .-
Printing a Chromatogram 1. T o print a chrom atogram first open chromatogram 602.CHR. Once th e ch romatogram is open select File from the PeakSimp le men u bar and then select Print from the drop-down menu .
2. The Print window will open and will allow the user to custom ize the printing of a chro mato gram. Click on the Fonnat button for the Print header to open up the Header format window. Add or delete any in formation in the window by click ing on the fie lds and inserting the desired information. Click on the OK butto n when all the desired info rmation is inpu tte d to dose the INindow.
. _.- . .
1..:r
.
~
,= -.~--
··., •
._ -
' 0-
,~
"
-
-'
~
,
~ - - --
526 (of 550 ) 2006(-2016)
527
...
,
~
"
,-
0
--
..-
....
6. select Print in the Prin t window to prin t the chromatogram or d ic k on O K in the Print window to exit the window.
'~
...:=..-J 0-
--.. ,-" .-.• .
~
~
C
,
-.
~
-' I t_
~,
.....F"7 "'l't
.-
'.' - '
4. In the Print window locate the Pri nt report
5. Once the Report format window is op en click on External in the Available dial og ue menu (on the left) and then click wi th the mouse cursor on the right facing arro w button to add External to the selected dialogue box (on the right). After Externa l is added to the Selected dialogue box d ick on Units with the mou se cursor and dick on the right fa cing arrow button to add Units to the Selected dialogue box . Click on OK with the mo use cursor to exit out of the Report format window. ! ~)
~ · F,
...r::- """
~~
...,.. ....... check box and click on the Format button to its right
,
·lcw.....i-:u' ,.,.., _
3. In the Print window click on the Format button for Print chromatogram to open up the Chromatogram format window. Locate the Chart speed dialog ue box and insert th e number of inches each minute on the chromatogram wi ll take up when printed (for a nine m inute run try 0.50 inches per minute). After the Chart speed is entered click on OK to exit the win dow.
f
,,
-''-='-"I'1 ...• "• - - -- r-, , ~-
- ~ .
•
.
~ -" --" -
-E:!
-==...
--- -. ,-iii !~ · -11 It- -. _._- • '-_._-- - • -_.
-
•
- -
-- ,. .
·
-'-
~ -
Exporting to Exce l 1. In the PeakSimple too lbar dick on the Resuits window button 10 open up the Results window. Once the Results w ind ow is open click on the Co py button to copy the results data to the Windows clipboard.
2. Make sure Microsoft Excel is loaded on the computer. If Excel is not loaded you can copy results data and chrom atog ra ms to Microsoft W ord or PowerPoint. Open up Microsoft Exce l by dicking with the mouse cursor on the Start button in the bottom left of the W indows screen and then Programs and the n Microsoft Excel in the Windows Program m en u.
--
527 (of 550 ) 2006(-2016)
528
6. Once Excel is opened select Edit from the Exeel menu bar and then Paste from the drop down menu. The results data is now placed into the columns and rows of Excel. Using the mouse cursor, select a box to the right of the results data in the Excel spreadsheet. Go back into the PeakSimple tor W indows NT program and hit Close to exit the Results window.
...... .'
---.,.. -•.. ... . .
------= ..
!~
'
~
7. Right click with the mouse cursor anywhere on chromatogram 602.CHR and select Copy picture from the resulting menu. Go back into Excel and select Edit from the Excel menu bar and then Paste from the drop down menu. The PeakSimpJe chromatogram will now be displayed next to its results data in the rows and columns of Miaosoft Excel.
..•
This concludes the PeakSimple 2000 Basic Tutorial An Advanced Tutoria l can be obtained by going to: www.srigc.com online If you have questions or would like to place an order call: (3 10) 2 14-5092
528 (of 550 ) 2006(-2016)
529
I
PeakSimple 2000 Chromatography Integration Software
I, i
Advanced Tutorial ,... - _ to-,.. :::: .,,1;;1 1:1 .
-
;
,,
~
...
I
..
",. .., ..
~
, ~
"
.
4 - - -.
-.
-
---
-
~
..
~
- "'= ~'. ' .
.
-- .
- .
= , ,-
_ . ----
--
.
"
') ..
..
..
•. , '-l
Install ing PeakSimple 2000 from floppy disk arCO-Rom
Instal ling PeakSimp le 2000 from software download
A
A
S tart the WlJ1Claws operating system in u se on
your comput er, (lNindows 95. 98, ME, 2000) B.
i
Insert the PeakSimpie 2000 diSk or CD inlO your dis k dnve.
c . Go to the Start menu ln the boltom left hand corner of the windows screen a:1dselect Ru n from the sel of rcoos.
Star1 the W indows opera ting system a nd use an on line browser to a ccess www.srigc.com.
B. From the me nu on t he left hand stc e of the scree n sAlact Download our Software and then dow nload PeakSim ple 2000 from the f ollowi ng page. C. sa ve e-e file to a ternpeary fOlder an d the n do uble click on it from My Ca"npu le r 10 allow th e program 10 I self-e xtract. i
D. From the run me nu , type X :\&etup (wh ere X is th e letter of your co m puter;> disk drive) . D. Once au u-e files have been extracted su ccessfully doubie-click t'le ins tal l file and press the Con tin ue E. Now d ick on !he Continue button with your button when pro mpted, mouse cursor or press the enter ke y o n your keyboard 10 begin in st allation . E. follow tne c nsnreen instructions 10comple te th e instcu auon of PeakS1lT:ple. F. To romplele installation follow the coscreen insu ccucoe curing the ir..3!e lic.Uon ~ .
SRI Instruments 20720 Eart Street Torrance, CA 90503 U.S.A Telephone: (3 10) 214-5092 Fax: (310) 214-5097 [email protected] g c.com
529 (of 550 ) 2006(-2016)
530
Manual Integration 1. To manually integ rate the Pea kS imple baseline in a chromatogra m use the manual integration tools found in the manua l integration toolbar. To open the manual integration toolbar first have chromatogram 602.CHR loaded and then select Edit from the PeakSimple m en u bar. From the drop down menu select Manual in te g rati o n with the mou se cursor. The manual integration tooroar will now be disp layed to t he right of the Pea kSimple toolbar in the lett most pa rt of the scree n.
'.
.r I
2. Use the None integration too l to add the area of the smaller peak to the area of the Solvent peak. First, zo om in on the so lvent peak. the sm all er pea k to its right, and the ir baselines. Once the chromatogram is zoome d in select th e None integration tool from the manual integration loolbar. W ith the Non e integration tool selected click once, using the left mouse button, on the valley betwee n the solvent peak and the smaller pea k.
3. Use the Dro p integration tool to drop the ba seline from the va lley of the two pe ak s to an existing baseline. To drop the baseline sele ct the Drop integ ration too l from the manual integration too lbar. Using the mouse cursor, c lick on the valley between the solven t peak and the s m aller peak to drop the baseline.
4. The Based integration too l ra ises the baseline to the valley between two specified peaks. With the baseline dropped. click on the Ba s ed integration too l button and then click on the va lley between the solvent peak and the sm aller pe ak to its rig ht to raise the baseline to th e valley.
....:::::.
1M
?"
..
b ,
,.;:.-- "~
530 (of 550 ) 2006(-2016)
531
5. T he Lead skim integration tool allows a peak's area to be skimmed off of the leading edge of another peak. To use the Lead skim tool first unzoom off of the solvent peak and the other s ma ller pea k and then zoom in on the Chlerobenzene peak, the Ethylbenzene peak, and th e baseline. After the chrom atog ram is zoomed click on the Lead skim integration to ol button and then c lick on the valley between the two peaks with the mouse cursor.
-- J
6. The Trail skim integration tool is similar to the Lead skim too l except a peak's a rea is now ski mmed off of the trailing edge of a nothe r peak. Select the Trail s kim tool button fro m th e manual integration too tbar and then click o n the va lley between the Chlorobenze ne an d Ethylben zene peaks with the m ouse cursor to see the Ethylbe nzene peak skimmed off of the Chlorobenzene pea k.
7, The Lead horizo ntal tool constructs the ba seline horizontally fo r the leading peak wh ile the trailing peak's baseline stretches from the horizontal line to the next valley. Unzoom off of the Chlorobenz ene and Ethylbenze ne pea ks and instead zoom in on the Solvent peak, the smaller peak to its right. and th e baseline. Click on the Lead horizontal integra tion tool in the manual integration too fbar and then click, using the left mouse button , on the valley between the solvent peak and the other sma ller peak.
r-'.:--
,
8. The Tra il nonzonta l integration tool drops the ba seline horizo ntally for the trailing peak w hile the lead peak's basel ine stretches from the horizonta l line to the previous valley in th e chromatogram . After selecting the Trail h o ri zontal tool in the manual integration toolbar c lick with the mouse cursor on the va lley between the two zoome d in peaks.
-
531 (of 550 ) 2006(-2016)
532
9. The Inh ibit tool ends the baseline afte r a valley effectively inhibiting a pea k's area from be-lng counted with the rest of the chromatogram. To use the Inhibit integration tool select the Inhibit tool button from the manual integration too lbar and dick on the va lley of the Solvent peak and the smaller peak to its right.
C'~ : i"
" .. ....
=
I
10. The Rubber Band tool is used to manually draw the basel ine in a chromatogram. To use the Rubber Band tool first scro ll the X-axis
scrollbar all the way to the left to 0.000. Select the Rubber Band tool from the manual integration toolbar and draw a line from the valley between the Solvent peak and the small peak to its left to the vall ey between the smaller peak to the right of the So lvent peak a nd the peak to its right
11. To undo a change made to the baseline of a
--
chromatogram with the manual integ rati on tools use the Undo button fou nd in the manual integration toolbar. To undo the changes made to the basel ine us ing the Rubber band tool click on the Undo button with you r mouse cursor. Al l changes made to the baseline wi ll now be undone.
.- .
'- ~ .
~,, ;
.
<, - .
,
,
.;:c, .. ... .
"~k
.
-
.
. -
.
._
~
12 . The Reverse tool allows the inverting of a peak in a ch romatogram. Note: To reverse the on'entation of the X-axis in real time go to the Events table. First unzoom off of the Solvent peak and the smaller pea k to its right and then select the Reverse tool from the manual integration toolbar and click and hold the left mouse button whi le the area of the chromatogra m you wa nt to reverse is dra gged over with a black box. Let go of the mouse button when the desired area is se lected to reverse the orientation .
.. ..
-- .-
-
-'
..
532 (of 550 ) 2006(-2016)
533
13. The Zero tool is used to set the value of the data line at a selected point and farrowing in the chromatogram to zero. First undo the changes done to the chromatogram by the Reverse tool by reopening 602.CHR in the Pea kSimple men u bar. Note: Changes made to a chrom atogram by the Reverse tool and the Zero tool cannot be undone with the Undo tool. Once the file is reopened dick on the Zero tool and click anywhere on the baseline between the Ethyfbenzene peak and the two pea ks to its right with lhe mouse cursor to set the data line at zero.
...
~
......
,
--
.-
Creating Component Tables 1. To create a component table from scratch open up a second channel in the PeakSimple window by clicking on the Disp lay Channel 2 button in the PeakSimple too lbar. Once the second channel is open click on File and the n Open to get to the Load chromatog ram file window. Se lect file FID602.CHR from the list of files and select the Channel 2 rad io button to open the file in channel 2. Click OK with the mouse cursor to load the file.
• . .~ ~ , '
2. In channel 2 locate the second tall peak from the left and right dick on it with the mouse cursor. From the resulting menu select Add component to add a retention window bar to th e peak. Once again right dick on the peak and select Edit compo nent fro m the men u to open up the Component details window.
i
....... -
-
....
-
--
533 (of 550 ) 2006(-2016)
534
3. O nce the Component details wind ow is open locate the Peak number dialogue box and add th e number 1. Immediately underneath the Peak nu mber box is the Pea k name dialog ue box. In the Peak name dialogue box input benzene to name it. l ocate the Units box and put ppm to make the units parts per million . Locate the In case of multiple pea ks options box and se lect the radio button for Show la rgest peak o n ly. Click on OK with the mouse cursor to dose the window. 4. Go to Edit in the PeakSimple menu bar and th en Channels from the resulting menu. The C hannel controls win dow is now open. Locate the Channel 2 options box and the Integrate checkbox. Check the Integrate checkbox a nd the n dick on OK with the mo use curso r to dose the window. The peak in the second channel s hould now identify itself as benzene.
5. Locate the large peak to the right of the benzene peak in the second channel. Right click an d then se lect Add component to add a rete ntian w indow bar to the pea k. Right click again and go to Edit componen t to open up the Component deta ils window. Ch ange the Peak num be r to 2 . the Pea k name to toluene . th e Units to ppm, and the In case of multiple pe aks options box to Show la rgest pea k only. Click on O K with the mouse curso r to exit the window .
_ _ _r
-
...... ~~ -
.---
....-
, ..,...M _
_ '
... ,....
- ....
--
-
__
'-
"'"...---
,-_--._ -
.
. -=--.::::::-..=.......:=... ~. =. -
..
-- - ..... ....,." .,0. ......... __ M" r-..... ..._ ,.. .. _ .' . ~_., _ _ ' r-~
~
. .
--- '~ - ~:
:z. _ ..:' --.-.-:= --- - - . -'- --- -.. :.;.:-::;:"-'-.=.
!"*
..=:...J
,
. ... . .
-,.~
,
.
.-
...'"-
-
------,
-
.
...
- ,."
-
-
.
0
.
-,,-
---: ..,-
•
'._.- ......'--
- ~-_ _ -'-'-'
~k-
. ~-
....-
~ - ~_ .
. . .......... .....
..-
r '..- - ·
534 (of 550 ) 2006(-2016)
535
7. Right click anywhere on the se cond channel and se lect Components from the list of op tions. Once the Ch annel 2 components window is o pen make sure all the data is correct and then d ick on Save to sa ve the Compone nt data to disk. Name the file Cta ble and the n cl ick on OK to close the window. An un limited number of component windows may be ad ded to the component table.
1 --r-- -
- ---.-
'.
• '.<
~ . ~ -:=...
~
....=:.- .....:::::- ~ ~!
Tem perature Programming 1. To modify the temperatu re prog ramming in -',
PeakSimple firs t open ch romatogram 602.CHR an d then right clic k anywhere on the chromatogram. From the drop dO'M1 menu select Temperat ure to open up the Temperature co ntrol wind ow.
2. In the Temperature con trol window d ick using the mouse cursor on the set of numbe rs in the box an d select Change from the group of buttons be low. The Temperature segment details window will op en allowing the modification of the temperature program ming. Locate the Hold for dialogue box an d insert a 2 in the box . C lick on OK to clo se the window and go ba ck in to the Temperature co ntrol window.
...
.'
..
-
-- --_. -=
-:.::....- -=-- - -- ----
Jt
;.,"'J: l:>:"~ !Jrti ~ IIU-e- ~:J'::1:C j:>
~, .....
J(
r;";
:~'j H. J;) en l
535 (of 550 ) 2006(-2016)
536
3. Select the Add button from the Temperature control window to open up the Tem perature segment details window once aga in. Leave the Initial tempe rature at 200 and insert a 1 in the Hold fo r dialogue box. Change the Then ramp at dialogue box to 5 and the Untilternpera ture is box to 250. Click on OK to dose the window and to see the new temperature data added to the temperature box. Click on OK to close the window.
-
-.'
.. ~
1>,t ,J: ;.,..,..,. .......,
"Cld. IQl:J ~- (u T'->,:tre:'1!4
fS
"" =
~~ ...n
t VO' ,,,,.-..,,,~ l-..r ~.l ;)((
ce:
...l :
iI:' 1("
" I
I
I
c~
-_. .. ,-. - - -_. .
--
,~-~
.. - ----'"
-.-
--£:.......:
Events Table 1. To modify up the Events table in PeakSim ple open up chromatogram 602.CHR and zoom in on the benzene peak , the sm aller peak to its rig ht, and the baseline. Right click anywhe re on the chromatogram and select Event s fro m the drop down menu. Doing this will open up the Eve nts window where specific events can be added to the chromatogram. 2. Click using the mouse cursor on th e Add button to view the Event deta ils window. A fist of event types a re available with the ir radio bu ttons to eithe r selec t or des elect the event. Note: The event types to the left of the window are reet- ttme and thus wi/I only affect the chromatogram when AID hardware is connected. The event types to the right are concerned only with integra tion and their changes will be immediately evident after returning to the main screen and selecting Rei ntegrate from th e Edit menu bar.
. ~ . ;-'~I;
/
-- .
....::..:...J
..
--'~
-
..
...... -
"'" ~ -
..
- -::¥c--
, ,
,
-
';,,-
-.
-.-
- ...- -_. --- --. ..'_.. ... "--... ..-- _. C-·· ----.• .
"
•
-'=-
,_.O· ..
•
~
-"-l
,~"
•
Iff' .......
.
- ........ _ <.. ,...
~ :-:::... ~ .
- ~.~
..,.,-.-.,. _
• ~-", .-.
.
-.- .
•
._,~ ,.
._
' - ' "':-
.-
..-
~ "'
.. ~j
-
.~ -
_
:;;; a
I
536 (of 550 ) 2006(-2016)
537
3. In the Event deta ils window locate an d select th e relay G radio button wit h the mouse cursor and then loca te the Event time dialogue box and enter .1 in the box. Click on OK to exit the window. Note: The relay might be used 10 ac-
tuate a valve wh en hardware is connected. The event type wi ll now be added to the Even ts ta ble. Sele ct the Add button and now locate and select the Zero event type radio button . Leave the Eve nt time box at 0 .000 and once aga in click on OK to exit the window and add the event to th e Even ts tab le. Note: The
Zero event auto-zeros the detector signal at the beginning ot tne ron. Click on the Add button again an d se lect the Integration-Based im m ed iate rad io button in the Even t details window and input 1.86 in the Event tim e dialogue box. S elect OK to exit the window.
,
4. There are now three ev ents in the Events table. Cli ck on OK to exit the Events window and then hit the Enter button on the keyb oard to rei ntegrate the baseline accord ing to the events in the Events table. Not ice that the baseline is connected to the data line at 1.86 min utes.
-
-~
,
Overlay and Subtract 1. To overlay one PeakSim ple chromatogram on top of another chromatogram open up a second channel in the main screen and load chromatogram 602.CHR in the first cha nnel and ch romatogram FID602.CHR in the second channe l. Right click anywhere in the firs t channel and se lect Channel details from the drop down menu.
,--
~""""
8M t
_""" 'ft""",".""",.-,:,.-......
!
2. In the Ch annel 1 details window locate the Overlay data in cha nne l ch ec kbox an d check it and then input a 2 in th e dia logue box 10 the right. T he chromatogram in cha nnel 2 is now ov erl aid on top of the chromatogram in channel 1. The overlay appears in a different color.
-.
.-
."-
-
..
537 (of 550 ) 2006(-2016)
538
3. Right click anywhere on the first channel and sel ect Over lay adj ustment from the drop down menu. In the Overlay adjustment window locate the Facto r scrol l box in the X box. Experiment scrolling the X factor up or down to shift the ov erlaid chromatogram to its right or left. Locate the Factor scroll box in the Y box and experiment saolling the Y factor up or down to move the overla id chromatogram up or down. Click on the Close button to close the window. 4. To su btra ct a chromatogram in one channel from another cnannel, right click using the mouse cursor on channel 1 and select Chane n el de ta ils. From the Channel 1 details window dese lec t the Overlay data in channel checkbox and then click on the O K button to exit the window. 5. Go to the Ed it menu ba r and select Subtractl Add channels from the drop down menu. In the Subtract/add channels wi ndow make sure the Subtract radio button is selected and that channel 2 is being taken from channel 1. Click on the O K button to make the changes take effect and have ch annel 2 subtracted from channel 1. The normal way to use this feature is to subtract a drifting baseline from a cnromatogram.
Res ul ts L o g 1. Open chromatogram 602 .CHR in the PeakSimple main screen and then select the Resu its button from the PeakSimple toolbar. In the Results win dow click on the Clear resu lts log button at the bottom of the window. aick on Yes from the resulting window to clear the resu lts.
,
x
, ,y
, _.
;-.:
-
~ ::O:: ~7.
- --_.
•
l:ox -:i ~:;J
S ~.·~
r r.";"
.-
1=""''';-I
.. -
" • "i-~ ) ..
r= ~
,
;.:...."
r.~
. --.-....- -.. - '.-- -,
.
.
:. '_- --"" '.'.-..- -_ .- .- - - . --- -;--- ,
-
~
~
.• j ..t:::t=-. .
r- !«
J
..,,"-.-.
,
•
'-
.. ..., •
~i
••~
,
-
,
,
,
~"""''' la:=J
"-
Y.
"""
..., 17";]
~ ~ : rI
."
,.
. *.,~
'"
~
I
.
-
}
-
•
, a
~
... ,..-
- ' O';;'
-
-
~.
~
-..., I ' J ~ S i
, -r
2. locate the Add to r esults log button and click on it three times to add the results on the screen to the Results log three times. Click on the Show results log button to view the resuus log in the W indows Note pad . D dt the W indows Notepad prog ram by selecting File from the menu bar and the n Exit
538 (of 550 ) 2006(-2016)
539
3. In th e Results window loca te the Copy results lo g button at the bottom of the window and cl ick on it with the mouse cursor (don't confuse the Copy button with the Copy results log button ). Open up Microsoft Excel (or if Excel is no t loaded Microsoft Word or PowerPoint) and select Ed it from the menu bar and then Paste to copy the results log to Excel.
4. Go back into PeakSimp le and close the Results window by selecting the Clo se button. Right click using the mouse cursor on the chromatogram and select Postrun from the drop down menu to open the Post-run actions window. From the window locate the Add to results log checkbox and add a check to the box. By selecting the Add to resul ts log checkbox all results from data analysis will auto-matically be added to the results log after the run is done. Click on OK to exit the window. In this way a summary of many analyses can be automatically created and then exported from PeakSimple,
."..." .'". "
.=--"
"
"
. ., •
•
.
...............
U
.... ."
..
-
~
•
~ . ---
.
"
. .
"' •_,J::e& ..,::::. "
--._.... --, - '---
I,
r,.~._ _ _ <> r ~x
.-
c-
.
~
"
....
- .-.P
-
r <... - ..
r
nO" , "",,-'
This concludes the PeakSimple 2000 Advanced Tutorial Further documentation can be obtained by going to: www.srigc.com online If you have questions or would like to place an order call: (310) 214-5092
539 (of 550 ) 2006(-2016)
540
ATTENTION! AVOID THESE COMMON ERRORS 1. In general, SRI Instruments does not recommend using nitrogen as a carrier gas. If
nitrogen carrier must be used with a TCD , the current must be set to LOW. High current TCD operation with nitrogen carrier will destroy the filaments. Using nitrogen as carrier gas in capillary columns will drastically reduce the separating ability of the column. Use of helium carrier is suggested wherever possible. NEVER TURN ON THE TCD FILAMENT CURRENT BEFORE CARRIER AND REFERENCE GAS FLOWS EXIST THROUGH THE DETECTOR AND HAVE BEEN VERIFIED. THE TCD FILAMENTS WILL BE DESTROYED IF ENERGIZED WITHOUT THESE FLOWS! The 8610C gas chromatograph, in programmable and educational models, is equipped with a filament protection cutout circuit. This circuit will de-energize the filaments if the column carrier gas head pressure falls below a preset value (factory set to 3psi). This will prevent the filaments from incandescing if the carrier gas is interrup ted to the detector by a removed septum nut, disconnected column, or empty carrier gas cylinder . It will not prevent filaments from damage if nitrogen carrier gas is used in conj unction with high filament current, which is prohibited and will void the warranty of the TCD detector. NEVER OPERATE THE TCD ON HIGH CURRENT WHEN USING NITROGEN CARRIER. 2. The SRI educational TCD-equipped gas chromatograph is equipped with a manua l pressure regulator in lieu of a flow controller for carrier gas flow. The full-featured 8610C GC is equipped with programmable electronic pressure control (EPC) of carrier gas flow . Therefore , hydrogen carrier gas should not b Lused with either GC configuration. If a leak, column breakage, or other failure occurs, hydrog en gas could
~
be released in dangerous concentrations, creating the potential for a fire or exp losio n to occur. Helium carrier offers an almost identical Van Deemter curve and performance to
hydrogen carrier gas, and is the recommended substitute carrie r gas. 3. When se lecting a port address fo r the serial data acquisition interface built into your 86IOC gas chromatograph, you must verify that you are not using a COM port on the data system host PC that is being shared with a mouse. Some PCs offer a DB-9 serial port labeled COMI, and have a DIN-plug type mouse with a separate, small, round plug and port. Thi s may also be on the COMI address. Consult your PC manual for information. If you are connecting to COM 2, and your PC is equipped with an internal mndem, change the modern' s COM port address from COM2 to COM3 or COM4 to avoid conflicts. Failure to do so will prevent the PC-based data system from communicating with the GC via the serial port. If you have any doubts regarding the configuration of your PC' s COM ports, use the MS-DOS MSD.EXE utility to inspect your hardware se ttings.
4. If you have an NPD detector, do not use hydrogen as a carrie r. The detector bead will overheat if the hydrogen flow is above 5 nil/m in. Also, do not forget to install the NPD restrictor and resistor supplied, if your NPD also performs as a convertible FID detector. Do not tum the bead voltage above 4 volts or the detector bead will bum up. The voltage can be monitored with the digital display on the front of the unit. The
display reads out in l /l OOths of a volt - 4 volts will be displayed as 400 units on the digital display. D; ~96EPDOCS\ATT'Om. EPD
REV . 07_:3 _96
540 (of 550 ) 2006(-2016)
541
[~ -------] WARRANTY: WARRANTY AND WARNINGS SRI will r<:pair
or replace any cereceve plIrtS
within two
y~~rs from the da ft of
ConSllmmablc iu:m s such .... I~mps , hea ters. septa . NPD beads, ECD detecto r cell , DELCO heaters. FPD photomultiplier tube s. trapS, filters . TeD filamentli. co lumns. syringes. t tc. lie exclud.,,;l. Rcpl.cementor repair $!IaU be the pun;hlse r's o nly remedy,.ad in no case .elow. So agent, ""preselttllnve, distnbuwr or emplo)'« of S RI has autho..-y to am eDdw s wunnIy in any ""'y. In 1tI" event tIl at any term or provisio n of this warnnly U jUbjcct 10 u lid clai m ofu nenfo rceab1.lny , $UdllUIn or plV' ;sWO WJI be nano...i y etlllwual., the: ~ pmvlllOlU shall eeveeeiess SUM"e, g n.nti nc SRI Ite I ~ po$loible protectIOD l!len uillable under b ....
WARNINGS AND HAZARDS:
Pu rch:L~er
is awareof and aa:cpu comp k:te rC$poltSibilil! for
opcraaon a t the equipmo:ntknowing tha t: 1) F lammab le gases suc b as hydrogen an d aI,oDlmdhalle are n-quind for operation of 101Tle deu,clO"'. anJ adaqu.at.:: pn:'ilutions must be t.>ken hy the user 10 inSl.l.I1 .safe and 1m-free Cas line rubior with flow snUbbers, 'Illick WUloff valves.
"m.
4) RadioaCl;i..e maJeriti is presenl insid e the £C D deeeer. u u die IISCT" respoll$ibility10comply Wllll all regulalio n~ aM s:afery precalltions . and 10dispose of tile detector in IIle nlanller p~ribed by regulaIol)' aZ"ocits. ECD d=rsan: trailSferred ~y from V&Ic:o lDe..HO'Jston T exas . 1(1 the ll'\Ir::baser, aDd all lto;:c-nses. d«ai.l~ of operation. " 'Imrly, disposal, etc . are solely lIle responsibilily of Vako and the purdluer. $) Toxic. haurdous. or poi..,oous sol wC'
ro.- "'!"" ratiotl nf the ELC D det=r. Other dde:torS lIIa~ re__ or form roxic compound s. req uiring Open.llODunde r it fulllCbolId or Woe of a Respi rato r. Sta.odan:ls or sam ples required to calib~ me GC may be to5.io. Ilu .a.rdo u$. o r lUmruble, 6) Eye dama ging ultra -yio l" r Ha: ht is " mil"'; by the P1D lI.mp. Eye pfOte(;tio n sho llid be worn at itl] emes when opcrati n, tit" GC. 1) BuLh 'lu a.litive and Quallutiwe r", ulas from GC ID.!.a System ere subject to many sources of error. Th e magnitude of the erro r is variable , and must be ' tati ,rically evalu n ed and co ntro lled by the ope rlltor . Respon<.i bility fo r Ihe X Cllr3.C}' of the results obtai ned is solely the open tor's. SRI m.akes no c1ulIl5 regarding the acc uracy, bias, Dr precisio n of tile n:sults. 8) All SRI eq uip ment is imcnded for ope ration by trained laboratory person nel only . 11 i:; the I"'rchll$er' , responlabllny to IIm'l acccss SO thitl only qua lified laboralnry ,echnlClans ma y O~rate tile equ ,pm..nlanJ 10 ensure IIlal they are prov ided with all neccesary uiety 1lPpuat1i5. ll'lUUilI:. and proc ed ures I\) minimiz.. inj u!)' andlordamlge in die eve nt of itn KClde nl o r malfunction (fonce.a ble o r DOlI) 9} Enol'Sand:or "bup " IDly llXi$1 in illtegntion 5Ofi'ware.
OPERATING TIllS EQUIPMENT SHALL CONSTIIUfE ACCEPTANCE OF ALL TERMS AND PROVISIONS ABOVE.
PLEASE READ! !! OOOI. EPD
541 (of 550 ) 2006(-2016)
542
THE~MnRONMENTALTECHNOLOGYVE~CATION PROG~1
ET~
om1
a EPA I '.... [ ... _
.... ""' ... .. ... .""'''''
Joint Verification Statement TECIINOLOGY TYPE: APPLICATION:
GAS CIIROMATOGRAPHY MEASUREMENT OF EXPLOSIVES IN CONTA.'flNATED
son.
TECHNOLOGY NAME:
:Model 8610C Gas Chromatograpbffhermionlc Io nizat ion Dete ctio n
CO MPANY:
SRI Instrum ents
ADDRESS:
20720 Earl Street To rrance, CA 90503
WEBSITE: EMAIL:
www.srig e.ccm hagold smil h @ea rthlink.net
PHONE: FAX:
(310) 114-5092 (310) 214-S097
The U.S. Environmental Protection Agene y (EPA) has created the Environmental Technology Veri fication Program (ElY) to facilitate the deployment of innovative or improved environmental tec hnologie s through performance verification and dissemination of information. The goal of the ETV Program is to further environmental protection by substantially accelerating the acceptance and use of improved and cost-effective technologies. ETV seeks to achieve this goal by pro vi ding high quality, peer-reviewe d data on technology performance to those involved in the design , distribution, financing, permitting, purchase. and use of environmental techno logies. ETV works in partnership with recognized standards and testing organizations. stakeholder groups consisting of regu lators. buyers. and vendor organizations, with the full participation of ind ivi dual technology developers. The program evaluates the performance of innovative technologies by developing test plans that are responsive to the needs of stakeholders. conducting field or labora tory tests (as appropriate), collecting and analyzing data, and preparing peer-revie wed reports. AU evalua tions are conducted in accordance with rigorous quality assurance protocols to ensure that data of Icnown and adequate quality are generated and that the res ults are defensible.
EPA_VS-$CM-48
Augl:lSl 200 1
542 (of 550 ) 2006(-2016)
543
he Depamnent o f Defense (DoD) has a similar verificatio n program kn own as th e Env ironmental Security
echnolcgy Certification Program (E STCP). T he purpose of ES TCP is to demonstrate and validate the most re mising innovative technologies that target Dolr ' s most urgent environmental needs and are projected to ay back the inve stm ent within 5 years through cost sa vings and improved efficien cies. ES TCP emonsrrattons are typi cally conducted under operation al field conditions at Do D facili ties. The ~emonstrations are intended to gen erate supporting cost and performance da ta for acceptance or validation of ~c technology . T he goal is to transition mature environmental sci enc e and techn ology proj ects through the ~emonstrationl validation ph ase, enabling promising techn ologies to receive regulatory and end user cceprance in order to be fie ld tested and commercia lized more rap idly . frhe Oak Ridge National Laboratory (ORNL ) is o ne of the verification organizations operating under the Site haractcrization and Monitoring T echnologies (SCMT) program. SCMT. wh ich is admin istered by EPA 's ~ational Expo sure Res earch Lab oratory , is one of 12 technology areas under ETV. In this verification test, OR-'lL e valuated the perfo rmance of exp losives detection technologies. Th is veri fic ation statement provides summary of the test results for SRI Instruments ' Model 86lOC gas chrom atograph with thermionic onizat ion detection (GClTID ). This verification was conducted jointly with DoD's ES Tep.
VERIFI CAT IO N TEST DESCRIPTION his verification test was designe d to evalua te technologies that detect and measure exp lo sives in soil. The est was conducted at ORN L in Oak Ridge, T ennessee, from August 2 1 through 3D, 2000. Sp iked samp les of f';no\\."D concentration were used to ass ess the accuracy of the technology. En vironmental ly contaminated soil funp les, collected from DoD sites in Californi a, Louis iana. Iowa, an d T ennessee and ranging in oncentrat ion fro m 0 to approxim ate ly 90,000 mgfkg, were used to assess several performan ce haracteristics. Th e primary constituents in the samples were 2,4, 6-tri n itrolo lucn e (TNT); iso meric initrotoluene (DNT), including both 2,4-dinitroto luene and 2.6-dini trotoluen e; hexahyd ro- I ,3,5-trinitro1,3,5-triazi ne (RDX); and octahydro- I ,3,5,7-tetranitro- l,3 .5,7-tetrazocine (HMX). The results o f the soil analyses conducted under field conditions by the GCJTID were compared wi th res ults from refere nce aboratory analyses o f homogenous rep licate samp les analyzed us ing EPA SW-846 M ethod 8330. Details of he verification, including a data summary and d iscussion of res ults. may be foun d in the report entitled
Environmental Technology Verification Report: Explosives Detection Tcch nology-SRJ Instruments, GCITlD. EPA/6OOIR-OlI065.
DESCRI PTIO N he SRJ Model 86 10C gas chromatograph (GC) is a transportable instrument that can provide on-si te analysis of soi ls for explos ives. Co upl ing this transporta ble gas chro matogr aph wi th a the rmionic ionization elector (T ID) all ows for the determination of explosives in soil matrices foll owin g simple sample reparati on procedures. Samples are extracted in acetone, dilut ed, an d injected d ire ctl y onto the GC column within a heate d inje ction port. The high temperature of the injectio n port instantaneousl y vap orizes the solvent extract an d exp losives, all owing them to tra vel as a vapo r through the GC co lumn in the presence of the nitrogen carrier gas. Th e stationary phase of the GC column and th e programmabl e o ven temperature eparate the compo nents present in sample extracts based on their rel ative affi nities and vapo r pressures. !uPon el ution fro m the column's end, compounds containing nitro groups are ionized on the surface of the ith~nnionie bead, an d the increased conductivity of atmosphere within the h eated de tector is measured with a pollec tor electrod e. In this verification test, the instrument was verifi ed for its ab ility to detect and q uantify ,4-dinitrotoluene (2.4-DNT), RDX , and TNT . Analytical nm times were typically less than 7 mi n and eporting limits were typ ically 0. 5 mg/kg. ' E C H ~ O LOGY
EPA.Vs.scM48
543 (of 550 ) 2006(-2016)
544
liVERIFICATION OF PERFORMANCE lIne following performance characteristics of SRI' s GOTID were obse rv ed.
!{Precision: The mean relati ve standard deviations (RSDs) for 2,4-DNT, RDX , and Th'T were 15%. 14% and 3% , respective ly, indicating that the determinations of all analytes were prec ise.
~CCJlrdC}': Accuracy was a ssessed using the perfonnance evaluatio n (PE) soil sampl es. which were spiked to ~minal
TNT and RDX concentrations 0[0, 10.50, 100.250, and SOO mglkg each by an independent aboratory. The mean percent recoveries for RDX and TNT were 9 ] % and 97% , respectively, indicating that Jthe ana lyse s were unbiased. 'aJs~ posirive/fulse negatiYe results: Of the 20 blank soils, SRI reported TNT in five samples (25% false positives). No false positives were reported for 2,4-DNT and RDX. False positive and false negative resu lts Iwere also estimated by comparing the GClfID resu lt to the referen ce laboratory result for the environmental ~d spiked samples (e.g., whether SRI rep orted a result as a nondcte ct that the reference laboratory reponed ~ a detection, and vice versa). For the se so ils, 3% of the 2,4- DNT resul ts and 7% of the TNT resu lts were tePorted as false posi tives relative to the reference laboratory results, but none ofthe RDX resul ts were eported as false positives. Similarly, a small percentage of the results were reponed as nondetec ts by SRI i.e ., false negatives) when the laboratory reported a detection (2% for RDX ,4% for TNT, none for 2,4joNT ).
Irompld~nns: The GClTID generated results for all 108 soil samples for a completeness of I ~Io.
Icomp a rability: A one-to-one samp le compa rison of the GC!fID results and the reference labo ratory resu lts !was performed for all samples (spiked and environmental) that were reported a s detects. The correlation Foe'fficient (r) for thc comparison of the entire soil data set for TNT (excluding one suspec t measurement for ~e reference laboratory) was 0.95 (slope (m) =- 1.32). When comparability was assess ed for specific FDCen1r31ioDran ges, the r value d id not change dramatically for TNT, ranging from 0.8910 0.93 depending ~n the concentrations selected. RDX correlation coe fficient with the reference laboratory for all soil results sligh tly lower than TNT (r = 0.85, m = 0.91). The GClfID's results for RDX correlated better with the teference laboratory for concentrations <:500 mg/kg (r = 0.96, m = 0.83) than for samples where Fncentrations were >500 mglkg (r a 0.49, m = 0.56). For the limited number of data points where both the tefermce Laboratory and SRI reported results for 2,4-DNT (n = 14), the correlation was 0.44 (m - 0.33) .
twas
I{'ample Throughput: Throughput was approximately three samples per hour. This rate was accomplished by operators and included sample preparation and analysis.
~o
as#! of User No particular level of educational training is required for the operator, but knowledge of ~hromalographic techn iques and experience in field instrument dep loymen ts would be advantageous .
EPA-V s.scM-48
Augw; t 2001
544 (of 550 ) 2006(-2016)
545
ChromLab
J~.(J.~_~-- -. J'-I
A Chromatography Tec h nology and Development Compan y
Customized O n-site GC S u pPOrt an d Trainin g; Senrices ChromLab w ill train of your personnel in the efficien t se tup. operation and routine calibra tion o f yo ur GC equipmen t We wiJI assist in th e tr ansfer o f new GC methods to your la boratory site. We will also op timize yo ur GC d ata handli ng methods and develop stan dard o perating proced u res for you r personnel to use after the tra ining is
com plete. Trai ning is available in the following areas: • • • • •
Bas ic GC Capillary Column GC Headspace GC Thennal Desorption GC GC Data Handling.
These support and tra ining services will greatly reduce yo ur GC d owntime and overall operatio nal costs to give your org anization real long term saving. You r personnel will ga in a solid understanding of their GC sys tem and the confidence to perform routine calibration, mainten ance and troubleshooting .
Providing Expert Tech nical Leadership Burton S . Todd, is the Technical Direc tor of ChromLab w ith over 30 years of hand son expertise in providi ng application su pport and training in Ge, HS /GC, GCjMS and GC data handling. He has worke d with hundreds of companies, large and sma ll
assisting in the specification and setup of GC and data handling instrumentation. He has p rovided success fu l so lu tions to solve difficult analyti cal challenges and helped to build the confidence and skills of labo ratory personnel through cus tomized training tailored to meet their needs.
For M ore Informa tion
For more informa tion on these an d other GC support and training services please con tact ChromLab at 610-644-2260 or Fax yo ur inquires and questi ons to Burto n Tod d. We w ill be g lad to assist you in develop ing a su pport program to help meet laboratory's goals. your
Phone : (610) 644 -2260
FAX: 1610) 644·2478
The Chromatography Laboratory Resource
545 (of 550 ) 2006(-2016)
546
eraU Eval£olatiQn: Th e ov erall perfonnance of the OCrI'm fOT fue ana\)''!.\!> ofl,4-DN1,RDX,and TNT as characterized a s p recise and unbiased. As with any technology selec tion, the user mu st determi ne iftliis echnology is appropri ate for the application and the project' s data quality obj ectives. For more informa tion n this and other verified technologi es, visi t the ETV web site at http J/www.epa. gov/etv.
./
~,~ . / / , . 12/ >/ /(j W. Frank Harri s, Ph.D.
Direct or National Exposure Research Laboratory Offi ce ofResearch and Development
. .. j)
"Fi .
J~~;t~arqllSeehth.D.
Assoc iate Laboratory Directo r Biological and Env ironmental Sciences Oak Ridge National Laboratory
-
director
Environmental Security T ec hno logy Certification Program Department of De fense
NonCE: EPA and ESTCP verifieztion s arc based on c:vaIuations ofkchr.oJogy perfomaowcc under speafie, predetermin ed cri teri a and appropriale quality assurance procedures. EPA. ESTeP, and OR1\'L mak e no expressed or implied warranties as to the peforrnance of the technology and do not certify that a technology will always operate as verified. The en d user is sol ely responsible for c omplying with an y and all applicable federal , Strite, and local requirements. Men tion o f eomrnen::iaJ product names does nol impl y endonemeDt or recommendation.
EPA.vs.SCM~ g
The aceoompanytn 8 """ ice iI;::Jn iDu:p1 pan o r lh is vmtlean
A ,,&1l:iI 200 1
546 (of 550 ) 2006(-2016)
547
I A Chromatog ra phy Techno log y and Deve lopment Co mpany 12 verno n Lane
Malvern, PA 19355-2933 (61 0) 644-2260
GC & GC Data Handling Application Support and Training Services Applica tion S u p port and Training Services
ChromLab provides a full range of supp ort, train ing and method devel opm ent services for ch romatography and data h andling instrumenta tion, including: •
Complete installation and setup services forGC instrumen ta tion and sample introduction systems including Headspace and Therma l Desorption.
• • •
On-site training in GC and GC Da ta Han dling for laborat ory personnel. Development of effective operator manuals and in-house trai ning program s. Method develop ment for Ge, HS/GC, capillary GC and fast GC analysis.
Benefits Pro vided to GC C u s tom ers ChromLab g ives your co m p a ny the benefi ts of on-site chrom atograp hy expertise.
lVe provide a pplicatio n support and training services for yo ur GC instrumentation tailored to meet the needs of yo u r laboratory when yo u need them a nd on a costeffective basis. • • • •
Reduced setup a nd traini ng costs with on-si te training for yo ur p ersonnel. O n-site GC and GC data handling method setup and calibration for quick impl ementation of cost saving QC/QA chromatogra phy methods. Custo mized Headspa ce G C, Therm al Desorption meth od s to so lve difficult sam p le analys is cha lJenges. Setup and training in regulatory compliance method s - EPA, OSHA, ASTM
ChromLab provides its s u pport services to the fol lowing ind ustries:
• •
Petroleum, Chemica l, Energy, Environmental Flexible Packaging, Con v e r ting, Paper a nd Flooring Products, Inks and COdlings
•
Pharm aceuti cal, Food a nd Beverage
Phone: (610) 644-2260
FAX: (6 10) 644-2478
The Chromatography Laboratory Resource
547 (of 550 ) 2006(-2016)
548 DEPARTMENT OF THE TREASURY tJt.;rTED STA TES CU STOMS SERVI CE
FOI'1"l ~ Ot4B~. 1515000'3
OECLARAnON FOR FREE ENTRY OF RETURNED AMERICAN PRODUCTS 190 CFR 10.' lC.5 '0 6, 10 66 1 0. 6 1 1 ~ 4 1 . 1 23 4.1 43 23 14S ,3S 3 EN1RYN O " DArE
"'''''"''';;;;;'''''"'''
''''"'"======'''''
1_'_''_'_'
~
_
OTY A,ND 5 1ATE IY lolANtJFAC'llJRE
I
g "lARK S, N~ B ERS, A,N[llJE'SCRIP11QN C6' ARTlC lES AE'T'UFINED
_lI'. .
• ,,_ walu!! d ~ a l'Xie IS S10.000 Of more and !he aftide& ar. no! .......""001 that you
t .....
S
,,,,r;. marlo.ed ....:1'1 ee na "", and aoaress of U.S. ~r8l' . Pf~ aro-adl 1XlPoe5
Y'JUf <:1010'" lot
$ 1afIj$
gI any ~ or OfP\er
as ....menclltl Goxl!;. AenJfned ,
11. I oedare lhal lhe intormato~ gry«lll!)O\ffl1$ true and com'!d to Itl& I)eSl of my I
" ,1l1Ou1
'$ SOGNATURE O' AUl">tORlZ1OoG
ClJsra.os OF"11Cl:'",---- - - - - - - - - - - - - - - - - - - - - - - - - -- - - - - - - -- - - - - - ---
ow.,..
NOTE: " me Of ulb ma~e cons'g nu i:s a eo~ra ton . lh1storm muSl toe signed by lhe Ilresiaenl. w:e Ilfll~MI. MlCI'1l!llry. or lr OlalOU. et' of !he COrporlllion. or ey any employee of t~ e corporatIOn whO ~olds a ~wer 01attorT'ey and a cenifical
or ~ .
NobCQ ' 8quirQ(j ~ P_rworlr. R8du<:toon Ad of 1980 ; Th
Siil emenl ' lIqUlrlll:! tl1 5 CFR 1320 2 1:
The est omalEld awrage bo.Jrdrtr'l assccated "'"'" this col!aetiOr'l of inIorm aLon 1$ 6 fT>Orote1: Il8'" responeerl or .<;OlXWdI\lleIlel" deolIncf;ng on ndrndual Con"rnenls co r'\CXlt'l'lfl'l the ac:curaet oIll'11$l;lunMn ntlma:e and SU9Qe$:iOnS 'or ~I"ll tra=; bo..on.»tt s."'Cdtl blI djrlldtd III U,S , CusIorns Service. p~ Uanagernel"l Bt rdl, Washington. OC202Z9. arcrtflll 0I'tce oIM.i1Magl1mentn Budraet p~ ~ P'O!9CI(151s.0G43 ). W~ DC 20503 , •
~
---.........
Customs Form 33 11 (031390) 548 (of 550 ) 2006(-2016)
549
_.
Chapter:
PREFACE
Topic:
RETURNS OF EQUIPMENT FROM OlJrSIDE U.S.A
In the event an item of SRI equipment needs to be returned to the factory from outside the U.S. A., please make a copy of the U. S. Customs form 3311 provided on the facing or reverse page, and include the filled out form with the shipping documents. This form will allow the equipment back into the U. S. without any customs duties, and will speed up customs clearance delay.
Before returning any goods, please obtain a RMA number ( return material anthorization ) from SRI. At the time the RMA is issued, you will be advised on preferred methods of shipment and shipping companies. SRI will normally request pre-paid FEDX delivery. To obtain an RMA contact: SRI Instruments Technical Support
20720 Earl St. Torrance CA 90503 U.S.A.
310-214-5092 fax 5097
\ep\docs\HOOI. epd Rev. 12·31-1997
549 (of 550 ) 2006(-2016)
550
UNITS OF PRESSURE EQUIVALENce (eQUAL TO 1 PSI) 1 psi
- 2.036 in. Hg (inches of mercury) - 27.68 in.
w.e.
~nches
of water column)
_ 51.715 mmHg or torr - 0.068947 bar _ 0.06804 atm (atmospheres)
- 6.8947 kilopascals or KPa _ 0.0703 kg/em' - 2.307 It H,o
REV. 04-J2J.M
550 (of 550 ) 2006(-2016)
