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# Document

Number: 

# AA) IV-A-3

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# A-81-2 1

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# trb Unite d Stale s Environmenta l Protectio n Agenc y En v Supp ( Cinci r D (^ —* *— » * P. 2



## IV-A- 3 Researc h an d Developmen t 

# Tes tMetho d Purgeabl e Halocarbon s Metho d 60 1

1

. Scop e an d Applicatio n 1. 1 Thi s metho d cover s th e determi

natio n o f2 9 purgeabl e halocarbons

. Th e followin g parameter s ma yb e determine d b ythi s method : Paramete r Bromodichloromethan e Bromofor m Bromomethan e Carbo n tetrachlorid e Chlorobenzen e Chloroethan e 2-Chloroethylviny l ethe r Chlorofor m Chloromethan e Dibromochloromethan e 1,2-Dichlorobenzen e 1,3-Dichlorobenzen e 1,4-Dichlorobenzen e Dichlorodifluoromethan e 1, 1 -Dichloroethan e 1,2-Dichloroethan e 1,1-Dichloroethen e trans-1,2-Dichloroethen e 1,2-Dichloropropan e cis-1,3-Dichloropropen e trans-1,3-Dichloropropen e Methylen e chlorid e 1,1,2,2-Tetrachloroethan e Tetrachloroethen e 1,1, 1 -Trichloroethan e 1,1,2-Trichloioethan e Trichloroethen e Trichlorofluoromethan e Viny l chlorid e STORE TNo

. 3210 1 3210 4 3441 3 3210 2 3430 1 3431 1 3457 6 3210 6 3441 8 3210 5 3453 6 3456 6 3457 1 3466 8 3449 6 3453 1 3450 1 3454 6 3454 1 3470 4 3469 9 3442 3 3451 6 3447 5 3450 6 345 1 1 3918 0 3448 8 3917 5 CA S No

. 75-27- 4 75-25- 2 74-83- 9 56-23- 5 108-90- 7 7 5-00- 3 100-75- 8 67-66- 3 74-87- 3 124-48- 1 95-50- 1 541-73- 1 106-46- 7 75-71- 8 75-34- 3 107-06- 2 75-35- 4 156-60- 5 78-87- 5 10061-01- 5 10061-02- 6 75-09- 2 79-34- 5 127-18- 4 71-55- 6 79-00- 5 79-01- 6 75-69- 4 75-01- 4

1. 2 Thi s i s a purg e an d tra p ga s chromatographi cmetho d applicabl e t o th e determinatio n o fth e compound s liste d abov e i n municipa l an d industria l discharge s a s provide d unde r4 0 CF R
601-1 July 1982 136.1

. Whe n thi s metho d i s use d t o

analyz e unfamilia rsample s fo ran yo r al l o fth e compound s above , compoun d identificatio n shoul d b e supporte d b ya t leas ton e additiona l qualitativ eP. 3

technique

. Thi s metho d describe s analytica l condition s fo ra secon d ga s chrqmaton.r'aphi ccolum n tha tca n b e use d t o confir m measurement s mad e wit h th e piimar ycolumn

. Metho d 62 4 provide s ga s chromatograph/mas s spedromete r(GC/MS ) condition s appropriat e fo rth e qualitativ e an d quantitativ e confirmatio n o fresult s fo r mos to fth e parameter s liste d above

. 1. 3 Th e metho d detectio n limi t(MDL , define d i n Sectio n 1 2. 1 )H ) fo reac h paramete ri s liste d i n Tabl e 1

. Th e MD L fo ra specifi cwastewate rma ydiffe r fro m thos e listed , dependin g upo n th e natur e o finterference s i n th e sampl e matrix

. 1. 4 An ymodificatio n o fthi s method , beyon d thos e expressl ypermitted , shal l b e considere d a s majo rmodifica

tion s subjec tt o applicatio n an d approva l o falternat e tes tprocedure s unde r4 0 CF R 136. 4 an d 136.5

. 1. 5 Thi s metho d i s restrictedt o us e b yo runde rth e supervisio n o fanalyst s experience d i n th e operatio n o fa purg e an d tra p syste m an d a ga s chromato

grap h an d i n th e interpretatio n o f chromatograms

. Eac h analys tmus t demonstrat e th e abilit yt o generat e acceptabl e result s wit h thi s metho d usin g th e procedur e describe d i n Sectio n 8.2

. 

### 2

. Summar yo fMetho d
2. 1 A n iner tga s i s bubble d throug h a 5-m Lwate rsampl e containe d i n a specially-designe d purgin g chambe ra t ambien ttemperature

. Th e halocarbon s ar e efficientl ytransferre d fro m th e aqueou s phas e t o th e vapo rphase

. Th e vapo ri s swep tthroug h a sorben ttra p wher e th e halocarbon s ar e trapped

. Afte rpurgin g i s completed , th e tra p i s heate d an d backflushe d wit h th e iner t ga s t o desor b th e halocarbon s ont o a ga s chromatographi ccolumn

. Th e ga s chromatograp h i s temperatur e pro gramme d t o separat e th e halocarbon s whic h ar e the n detecte d wit h a halide

specifi cdetector.< 2

- 3 > 2. 2 Th e metho d provide s a n optiona l ga s chromatographi ccolum n tha tma y b e helpfu l i n resolvin g th e compound s o finteres tfro m interference s tha tma y occur

. 

### 3.

. Interference s 3. 1 Impuritie s i n th e purg e ga s an d organi ccompound s out-gassin g fro m th e plumbin g ahea d o fth e tra p accoun t fo rth e majorit yo fcontaminatio n problems

. Th e analytica l syste m mus t b e demonstrate d t o b e fre e fro m contaminatio n unde rth e condition s o f th e analysi s b yrunnin g laborator y reagen tblank s a s describe d i n Sectio n 8.5

. Th e us e o fnon-TF E plasti ctubing , non-TF E threa d sealants , o rflo w controller s wit h rubbe rcomponent s i n th e purgin g devic e shoul d b e avoided

. 3. 2 Sample s ca n b e contaminate d b y diffusio n o fvolatil e organic s (particu

larl yfluorocarbon s an d methylen e chloride ) throug h th e septu m sea l int o th e sampl e durin g shipmen tan d storage

. Afiel d reagen tblan k prepare d fro m reagen twate ran d carrie d throug h th e samplin g an d handlin g protoco l ca n serv e a s a chec k

o n suc h contamination

. 3. 3 Contaminatio n b ycarry-ove rca n occu rwheneve rhig h leve l an d lo w leve l sample s ar e sequentiall yanalyzed

. T o reduc e carry-over , th e purgin g devic e an d sampl e syring e mus tb e rinse d wit h reagen twate rbetwee n sampl e analyses

. Wheneve ra n unusuall yconcentrate d sampl e i s encountered , i tshoul d b e followe d b y a n analysi s o freagen twate rt o chec k fo rcros s contamination

. Fo rsample s containin g larg e amount s o fwater
solubl e materials , suspende d solids , hig h boilin g compound s o rhig h organohalid e levels , i tma yb e neces sar yt o was h ou tth e purgin g devic e wit h a detergen tsolution , rins e i twit h distille d water , an d the n dr yi ti n a 1 0 5 ° C ove n betwee n analyses

. Th e tra p an d othe rpart s o fth e syste m ar e als o subjec tt o contamination ; there

fore , frequen tbakeou tan d purgin g o f th e entir e syste m ma yb e required

. 

### 4

. Safet y 4. 1 Th e toxicit yo rcarcinogenicit yo f eac h reagen tuse d i n thi s metho d ha s no tbee n precisel ydefined ; however , eac h chemica l compoun d shoul d b e treate d a s a potentia l healt h hazard

. Fro m thi s viewpoint , exposur e t o thes e chemical s mus tb e reduce d t o th e lowes tpossibl e leve l b ywhateve r mean s available

. Th e laborator yi s responsibl e fo rmaintainin g a curren t awarenes s fil e o fOSH Aregulation s regardin g th e saf e handlin g o fth e chemical s specifie d i n thi s method

. A referenc e fil e o fmateria l dat a handlin g sheet s shoul d als o b e mad e availabl e t o al l personne l involve d i n th e chemica l analysis

. Additiona l reference s t o laborator ysafet yar e availabl e an d hav e bee n identified! 4 6 1 fo rth e infor

matio n o fth e analyst

. 4. 2 Th e followin g parameter s covere d b ythi s metho d hav e bee n ten
tativel yclfcssifie d a s know n o r suspected , huma n o rmammalia n carcinogens : carbo n tetrachloride , chloroform , 1,4-dichloiobenzene , an d viny l chloride

. Primar ystandard s o f thes e toxi ccompound s shoul d b e prepare d i n a hood

. ANIOSH/MES A approve d toxi cga s respirato rshoul d b e wor n whe n th e analys thandle s hig h concentration s o fthes e toxi c compounds

. 

### 5

. Apparatu s an d Material s 5. 1 Samplin g equipment , fo rdiscret e sampling

. 5.1.1 Via l —25-m Lcapacit yo rlarger , equippe d wit h a scre wca p wit h hol e i n cente r(Pierc e # 1 307 5 o requivalent)

. Detergen twash , rins e ca p wit h ta p an d distille d water , an d dr ya t10 5 ° C befor e use

. 5.1.2 Septu m —Teflon-face d silicon e (Pierc e #1272 2 o requivalent)

. Detergen twash , rins e wit h ta p an d distille d water , an d dr ya t1 0 5 ° C fo r on e hou rbefor e use

. 5. 2 Purg e an d tra p devic e —Th e purg e an d tra p devic e consist s o fthre e separat e piece s o fequipment : th e sampl e purger , trap , an d th e desorber

. Severa l complet e device s ar e no w commerciall yavailable

. 5.2.1 Th e sampl e purge rmus tb e designe d t o accep t5-m Lsample s wit h a wate rcolum n a tleas t3 c m deep

. Th e gaseou s hea d spac e betwee n th e wate rcolum n an d th e tra p mus thav e a tota l volum e o fles s tha n 1 5-mL

. Th e purg e ga s mus tpas s throug h th e wate r colum n a s finel ydivide d bubble s wit h a diamete ro fles s tha n 3 m m a tth e origin

. Th e purg e ga s mus tb e intro

duce d n o mor e tha n 5 m m fro m th e bas e o fth e wate rcolumn

. Th e sampl e purger , illustrate d i n Figur e 1 , meet s thes e desig n criteria

. 5.2.2 Th e tra p mus tb e a tleas t2 5 c m lon g an d hav e a n insid e diamete ro f a tleas t0. 1 0 5 inch

. Th e tra p mus tb e packe d t o contai n th e followin g minimu m length s o fadsorbents : 1. 0 c m o fmethy l silicon e coate d backin g (Sectio n 6.3.3) , 7. 7 c m o f 2,6-diphenylen e oxid e polyme r (Sectio n 6.3.2) , 7. 7 c m o fsilic a gel , 7. 7 g m o fcoconu tcharcoa l (Sectio n 6.3.1)

. I fi ti s no tnecessar yt o analyz e fo rdichlorodifluroromethane , th e char

coa l ca n b e eliminated , an d th e polyme r sectio n lengthene d t o 1 5 cm

. Th e minimu m specification s fo rth e tra p ar e illustrate d i n Figur e 2

. 5.2.3 Th e desorbe rmus tb e capabl e o frapidl yheatin g th e tra p t o 1 8 0 °C

. Th e polyme rsectio n o fth e tra p shoul d
601-2 July 1982P. 4

no tb e heate d highe rtha n 1 8 0 ° C an d th e remainin g section s shoul d no t exceed.22 0 °C

. Th e desorbe rdesign , illustrate d i n Figur e 2 , meet s thes e criteria

. 5.2.4 Th e purg e an d tra p devic e ma y b e assemble d a s a separat e uni to rb e couple d t o a ga s chromatograp h a s illustrate d i n Figure s 3 an d 4

. 5. 3 Ga s chromatograp h —A n analyti

ca l syste m complet e wit h a tempera
tur e programmabl e ga s chromatograp h suitabl e fo ron-colum n injectio n an d al l lequire d accessorie s includin g syringes , analytica l columns, , gases , detector , an d strip-char trecorder

. Adat a syste m i s recommende d fo rmeasurin g pea k areas

. 5.3.1 Colum n 1- 8 f tlon g x0. 1 i n I D stainles s stee l o rglass , packe d wit h 1 % SP- 1 00 0 o n Carbopac k B (60/80

. mesh ) o requivalent

. Thi s colum n wa s use d t o develo p th e metho d perfor

manc e statement s i n Sectio n 1 2

. Guideline s fo rth e us e o falternat e colum n packing s ar e provide d i n Sectio n 10.1

. 5.3.2 Colum n 2- 6 f tlon g x0. 1 i n I D stainles s stee l o rglass , packe d wit h chemicall ybonde d n-octan e o n Porasil

C (100/ 1 20 ) mes h o requivalent

. 5.3.3 Detector—Electrolyti cconduc

tivit yo rmicrocoulometric

. Thes e type s o fdetector s hav e prove n effectiv e i n th e analysi s o fwastewater s fo rth e parameter s liste d i n th e scope

. Th e electrolyti cconductivit ydetecto rwa s use d t o develo p th e metho d perfor

manc e statement s ^n d MD Lliste d i n Table s 1 an d 2

. Guideline s fo rth e us e o falternat e detector s ar e provide d i n Sectio n 10.1

. 5. 4 Syringes—5-m Lglas s hypo

dermi cwit h Luerlo k

ti p (tw o each) , i f applicabl e t o th e purgin g device

. 5. 5 Micr o syringes—2 5 pL , 0.00 6 i n I D needle

. 5. 6 Syring e valv e —2-way , wit h Lue r end s (thre e each)

. 5. 7 Syringe—5-mL , gas-tigh twit h shut-of fvalve

. 5. 8 Bottle— 1 5-mL , scre wcap , wit h Teflo n ca p liner

. 5. 9 Balanc e —Analytical , capabl e o f accuratel yweighin g 0.000 1 g

. 

### 6

. Reagent s 6. 1 Reagen twater

—Reagen twate ri s define d a s a wate ri n whic h a n interferen t i s no tobserve d a tth e MD L o fth e parameter s o finterest

. 6.1.1 Reagen twate rca n b e generate d b ypassin g ta p wate rthroug h a carbo n filte rbe d containin g abou t1 Ib

. o f activate d carbo n (Filtrasorb-30 0 o r equivalen t(Calgo n Corp.))

. 6.1.2 Awate rpurificatio n syste m (Millipor e Super- Q o requivalent ) ma y b e use d t o generat e reagen twater

. 6.1.3 Reagen twate rma yals o b e prepare d b yboilin g wate rfo r1 5 minutes

. Subsequently , whil e maintain

in g th e temperatur e a t9 0 °C , bubbl e a contaminant-fre e iner tga s throug h th e wate rfo ron e hour

. Whil e stil l hot , transfe rth e wate rt o a narro wmout h screw-ca p bottl e an d sea l wit h a Teflon-line d septu m an d cap

. 6. 2 Sodiu m thiosulfate

Granular

. 6. 3 Tra p Material s (ACS )

6.3.1 Coconu tcharcoa l (6/ 1 0 mes h sieve d t o 2 6 mesh) , (Barnab yChaney , CA-580-2 6 lo ttt

M 264 9 o r equivalent)

. 6.3.2 2,6-Diphenylen e oxid e polymer—Tenax , (60/8 0 mesh) , chromatographi cgrad e o requivalent

. 6.3.3 Methy l silicon e packin g —3 % OV- 1 o n 60/8 0 mes h Chromosorb- W o requivalent

. 6.3.4 Silic a gel—35/6 0 mesh , Davison , grade- 1 5 o requivalent

. 6. 4 Methy l Alcoho l —Pesticid e qualit y o requivalent

. 6. 5 Stoc k

standar d solution s —Stoc k standar d solution s ma yb e prepare d fro m pur e standar d material s o r purchase d a s certifie d solutions

. Prepar e stoc k

standar d solution s i n methy l alcoho l usin g assaye d liquid s o r ga s cylinder s a s appropriate

. Becaus e o fth e toxicit yo fsom e o fth e organohalides , primar ydilution s o f thes e material s shoul d b e prepare d i n a hood

. ANIOSH/MES Aapprove d toxi c ga s respirato rshoul d b e use d whe n th e analys thandle s hig h concentration s o f suc h materials

. 6.5.1 Plac e abou t9. 8 m Lo fmethy l alcoho l int o a 1 0-m Lgroun d glas s stoppere d volumetri cfiask

. Allo wth e flas k t o stand , unstoppered , fo rabou t 1 0 minute s o runti l al l alcoho l wette d surface s hav e dried

. Weig h th e fias k t o th e neares t0. 1 mg

. 6.5.2 Ad d th e assaye d referenc e material : 6.5.2.1 Liquids-Usin g a 100-p L syringe , immediatel yad d tw o o rmor e drop s o fassaye d referenc e materia l t o th e flask , the n reweigh

. B e sur e tha t th e drop s fal l directl yint o th e alcoho l withou tcontactin g th e nec k o fth e flask

. 6.5.2.2 Gase s —T o prepar e standard s fo ran yo fth e si xhalocarbon s tha tboi l belo w3 0 ° C (bromomethane , chloro

ethane , chloromethane , dichlorodi

fluoromethane , trichlorofluoromethane , viny l chloride) , fil l a 5-m Lvalve d gas tigh tsyring e wit h th e referenc e standar d t o th e 5.0-m Lmark

. Lowe r th e needl e t o 5 m m abov e th e methy l alcoho l meniscus

. Slowl yintroduc e th e referenc e standar d abov e th e surfac e o fth e liqui d (th e heav yga s wil l rapidl y dissolv e int o th e methy l alcohol)

. 6.5. 3 Reweigh , dilut e t o volume , stopper , the n mi xb yinvertin g th e flas k severa l times

. Calculat e th e concentra
tio n i n microgram s pe rmicrolite rfro m th e ne tgai n i n weight

. Whe n compoun d purit yi s assaye d t o b e 96 % o rgreater , th e weigh tca n b e use d withou tcorrec tio n t o calculat e th e concentratio n o f th e stoc k

standard

. Commerciall ypre pare d stoc k

standard s ca n b e use d a t an yconcentratio n i fthe yar e certifie d b yth e manufacture ro rb ya n indepen

den tsource

. 6.5.4 Transfe rth e stoc k siandar d solutio n int o a Teflon-seale d screw-ca p bottle

. Store , wit h minima l headspace , a t- 1 0 t o - 2 0 ° C an d protec tfro m light

. 6.5.5 Prepar e fres h standard s weekl y fo rth e si xgase s an d 2-chloroethylviny l ether

. Al l othe rstandard s mus tb e replace d afte ron e month , o rsoone ri f compariso n wit h chec k standard s indicat e a problem

. 6. 6 Secondar ydilutio n standards

- Usin g stoc k

standar d solutions , prepar e secondar ydilutio n standard s i n methy l alcoho l tha tcontai n th e compound s o f interest , eithe rsingl yo rmixe d together

. Th e secondar ydilutio n standard s shoul d b e prepare d a tconcentration s suc h tha tth e aqueou s calibratio n standard s prepare d i n Section s 7.3. 1 o r7.4. 1 wil l bracke tth e workin g rang e o fth e analytica l system

. Secondar y dilutio n standard s shoul d b e store d wit h minima l headspac e an d shoul d b e checke d frequentl yfo rsign s o fdegrad

atio n o revaporation , especiall yjus t prio rt o preparin g calibratio n standard s fro m them

. Qualit ycontro l chec k standard s tha tca n b e use d t o determin e th e accurac yo fcalibratio n standard s wil l b e availabl e fro m th e U.S. ' Environmenta l Protectio n Agency , Environmenta l Monitorin g an d Suppor t Laboratory , i n Cincinnati , Ohio

. 601-3 July 1982P. 5



### 7

. Calibratio n 7.1 ' Assembl e a purg e an d tra p devic e tha t meet s th e specification s i n Sectio n 5.2

. Conditio n th e tra p overnigh ta t 1 8 0 ° C b ybackflushin g wit h a n iner t ga s flo wo fa tleas t2 0 mL/min

. Prio rt o use , dail yconditio n trap s 1 0 minute s whil e backflushin g a t1 8 0 °C

. 7. 2 Connec tth e purg e an d tra p devic e t o a ga s chromatograph

. Th e ga s chromatograp h mus tb e operate d usin g temperatur e an d flo wrat e param eter s equivalen tt o thos e i n Tabl e 1

. Calibrat e th e purg e an d trap-ga s chromatographi csyste m usin g eithe r th e externa l standar d techniqu e (Sectio n 7.3 ) o rth e interna l standar d techniqu e (Sectio n 7.4)

. 7. 3 Externa l standar d calibratio n procedure : 7.3.1 Prepar e calibratio n standard s a ta minimu m o fthre e concentratio n level s fo reac h paramete rb ycarefull y addin g 20. 0 p Lo fon e o rmor e second

ar ydilutio n standard s t o 1 00 , 500 , o r 1 00 0 m Lo freagen twater

. A25-p L syring e wit h a 0.00 6 inc h I D needl e shoul d b e use d fo rthi s operation

. On e o fth e externa l standard s shoul d b e a ta concentratio n near , bu tabove , th e metho d detectio n limi t(Se e Tabl e 1 ) an d th e othe rconcentration s shoul d correspon d t o th e expecte d rang e o f concentration s foun d i n rea l sample s o r shoul d defin e th e workin g rang e o fth e detector

. Thes e aqueou s standard s ca n b e store d u p t o 2 4 hours , i fhel d i n seale d vial s wit h zer o headspac e a s describe d i n Sectio n 9.2

. I fno ts o stored , the ymus tb e discarde d afte r on e hour

. 7.3.2 Analyz e eac h calibratio n standar d accordin g t o Sectio n 1 0 , an d tabulat e pea k

heigh to rare a response s versu s th e concentratio n i n th e standard

. Th e result s ca n b e use d t o prepar e a calibratio n curv e fo reac h compound

. Alternatively , i fth e rati o o f respons e t o concentratio n (calibratio n factor ) i s a constan tove rth e workin g rang e (-=10 % relativ e standar d devia

tion , RSD) , linearit ythroug h th e origi n ca n b e assume d an d th e averag e rati o o rcalibratio n facto rca n b e use d i n plac e o fa calibratio n curve

. 7.3.3 Th e workin g calibratio n curv e o rcalibratio n facto rmus tb e verifie d o n eac h workin g da yb yth e measuremen t o fon e o rmor e calibratio n standards

. I f th e respons e fo ran yparamete rvarie s fro m th e predicte d respons e b ymor e tha n ±10% , th e tes tmus tb e repeate d usin g a fres h calibratio n standard

. Alternatively , a ne wcalibratio n curv e o rcalibratio n facto rmus tb e prepare d fo rtha tparameter

. 7. 4 Interna l standar d calibratio n procedure

. T o us e thi s approach , th e analys tmus tselec ton e o rmor e interna l standard s tha tar e simila ri n analytica l behavio rt o th e compound s o finterest

. Th e analys tmus tfurthe rdemonstrat e tha tth e measuremen to fth e interna l standar d i s no taffecte d b ymetho d o r matri xinterferences

. Becaus e o fthes e limitations , n o interna l standar d ca n b e suggeste d tha ti s applicabl e t o al l samples

. Th e compound s recommende d fo rus e a s surrogat e spike s i n Sectio n 8. 7 hav e bee n use d successfull ya s interna l standards , becaus e o fthei r generall yuniqu e retentio n times

. 7.4.1 Prepar e calibratio n standard s a ta minimu m o fthre e concentratio n level s fo reac h paramete ro finteres ta s describe d i n Sectio n 7.3.1

. 7.4.2 Prepar e a spikin g solutio n con tainin g eac h o fth e interna l standard s usin g th e procedure s describe d i n Section s 6. 5 an d 6.6

. I ti s recom mende d tha tth e secondar ydilutio n standar d b e prepare d a ta concentra
tio n o f1 5 pg/m Lo feac h interna l standar d compound

. Th e additio n o f 1 Op Lo fthi s standar d t o 5. 0 m Lo f sampl e o rcalibratio n standar d woul d b e equivalen tt o 3 0 pg/L

. 7.4.3 Analyz e eac h calibratio n stand

ard , accordin g t o Sectio n 10 , addin g 1 0 p Lo finterna l standar d spikin g solu

tio n directl yt o th e syring e (Sectio n 10.4)
. Tabulat e pea k heigh to rare a response s agains tconcentratio n fo r eac h compoun d an d interna l standard , an d calculat e respons e factor s (RF ) fo r eac h compoun d usin g equatio n 1

. Eq

. 1 R F = (A s C is )/(A is C s ) where : A s = Respons e fo rth e paramete rt o b e measured

. A I S = Respons e fo rth e interna l standard

. C i s = Concentratio n o fth e interna l standard

. C s = Concentratio n o fth e paramete rt o b e measured

. I fth e R F valu e ove rth e workin g rang e i s a constan t(«c 1 0 % RSD) , th e R F ca n b e assume d 1 0 b e invarian tar. d th e averag e R F ca n b e use d fo rcalculations

. Alternatively , th e resuh s ca n b e use d t o plo ta calibratio n curv e o frespons e ratios , A s /A i s , vs

. RF

. 7.4.4 Th e workin g calibratio n curv e o rR F mus tb e verifie d o n eac h workin g da yb yth e measuremen to fon e o r mor e calibratio n standards

. I fth e respons e fo ran yparamete rvarie s fro m th e predicte d respons e b ymor e tha n ±1 0-% , th e tes tmus tb e repeate d usin g a fres h calibratio n standard

. Alternatively , a ne wcalibratio n curv e mus tb e prepare d fo rtha tcompound

. 

### 8

. Qualit yContro l
8. 1 Eac h laborator ytha tuse s thi s metho d i s require d t o operat e a forma l qualit ycontro l program

. Th e minimu m requirement s o fthi s progra m consis to f a n initia l demonstratio n o flaborator y capabilit yan d th e analysi s o fspike d sample s a s a continuin g chec k o n performance

. Th e laborator yi s require d t o maintai n performanc e record s t o defin e th e qualit yo fdat a tha ti s generated

. Ongoin g performanc e check s mus tb e compare d wit h estab

lishe d performanc e criteri a t o determin e i fth e result s o fanalyse s ar e withi n accurac yan d precisio n limit s expecte d o fth e method

. 8.1.1 Befor e performin g an y analyses , th e analys tmus tdemonstrat e th e abilit yt o generat e acceptabl e accurac yan d precisio n wit h thi s method

. Thi s abilit yi s establishe d a s describe d i n Sectio n 8.2

. 8.1.2 I n recognitio n o fth e rapi d advance s tha tar e occurrin g i n chroma

tography , th e analys ti s permitte d cer tai n option s t o improv e th e separation s o rlowe rth e cos to fmeasurements

. Eac h tim e suc h modification s ar e mad e t o th e method , th e analys ti s require d t o repea tth e procedur e i n Sectio n 8.2

. 8.1.3 Th e laborator ymus tspik e an d analyz e a minimu m o f1 0 % o fal l sample s t o monito rcontinuin g labora

tor yperformance

. Thi s procedur e i s describe d i n Sectio n 8.4

. 8. 2 T o establis h th e abilit yt o generat e acceptabl e accurac yan d precision , th e analys tmus tperfor m th e followin g operations

. 8.2.1 Selec ta representativ e spik e concentratio n fo reac h compoun d t o b e measured

. Usin g stoc k standards , prepai e a qualit ycontro l chec k sampl e concentrat e i n methy l alcoho l 50 0 time s mor e concentrate d tha n th e selecte d concentrations

. Qualit y contro l chec k

sampl e concentrates , appropriat e fo rus e wit h thi s method , wil l b e availabl e fro m th e U.S

. Environmenta l Protectio n Agency , Environmenta l Monitorin g an d Suppor t Laboratory , Cincinnati , Ohi o 45268

. 8.2.2 Usin g a syringe , ad d 1 0 p Lo f th e chec k

sampl e concentrat e t o eac h o fa minimu m o ffou r5-m Laliquot s o f reagen twater

. Arepresentativ e waste
601-4 July 1982P. 6

wate rma yb e use d i n plac e o fth e reagen t w-jater , bu ton e o rmor e addi

tiona l aliquot s mus tb e analyze d t o determin e backgroun d levels , an d th e spik e leve l mus texcee d twic e th e backgroun d leve l fo rth e tes tt o b e valid

. Analyz e th e aliquot s accordin g t o th e metho d beginnin g i n Sectio n 10

. 8.2.3 Calculat e th e averag e percen t recovery , (R) , an d th e standar d devia

tio n o fth e percen trecover y(s) , fo rth e results

. Wastewate rbackgroun d cor rection s mus tb e mad e befor e R an d s calculation s ar e performed

. 8.2.4 Usin g Table'2 , not e th e averag e recover y(X ) an d standar d deviatio n (p ) expecte d fo reac h metho d parameter

. Compar e thes e t o th e calculate d value s fo rR an d s

. I fs > 2 p o r| X—R | = —2p , revie wpotentia l proble m area s an d repea tth e test

. 8. 3 Th e analys tmus tcalculat e metho d performanc e criteri a an d defin e th e performanc e o fth e laborator yfo r eac h spik e concentratio n an d paramete r bein g measured

. 8.2.5 Th e U.S

. Environmenta l Protectio n Agenc yplan s t o establis h performanc e criteri a fo rR an d s base d upo n th e result s o finterlaborator y testing

. Whe n the ybecom e available , thes e criteri a mus tb e me tbefor e an y sample s ma yb e analyzed

. 8.3.1 Calculat e uppe ran d lowe r contro l limt s fo rmetho d performance : Uppe rContro l Limi t(UCL ) = R + 3 s Lowe rContro l Limi t(LC D = R - 3 s wher e R an d s ar e calculate d a s i n Sectio n 3.2.3

. Th e UC Lan d LC Lca n b e use d t o construc tcontro l charts 17 1 tha tar e usefu l i n observin g trend s i n performance

. Th e contro l limit s abov e mus tb e replace d b ymetho d perfor

manc e criteri a a s the ybecom e availabl e fro m th e U.S

. Environmenta l Protectio n Agency

. 8.3.2 Th e laborator ymus tdevelo p an d maintai n separat e accurac ystate
ment s o flaborator yperformanc e fo r wastewate rsamples

. A n accurac y statemen tfo rth e metho d i s define d a s R ±s

. Th e accurac ystatemen tshoul d b e develope d b yth e analysi s o ffou r aliquot s o fwastewate re s describe d i n Sectio n 8.2.2 , followe d b yth e calcu

latio n o fR an d s

. Alternately , th e analys tma yus e fou rwastewate rdat a point s gathere d throug h th e require

men tfo rcontinuin g qualit ycontro l i n Sectio n 8.4

. Th e accurac ystatement s shoul d b e update d regularly.' 7 ' 8. 4 Th e laborator yi s require d t o collec ta portio n o fthei rsample s i n duplicat e t o monito rspik e recoveries

. Th e frequenc yo fspike d sampl e analysi s mus tb e a tleas t1 0 % o fal l sample s o ron e sampl e pe rmonth , whicheve ri s greater

. On e aliquo to fth e sampl e mus tb e spike d an d analyze d a s describe d i n Sectio n 8.2

. I fth e recover yfo ra particula rparamete r doe s no tfal l withi n th e contro l limit s fo rmetho d performance , th e result s reporte d fo rtha tparamete ri n al l sample s processe d a s par to fth e sam e se tmus tb e qualifie d a s describe d i n Sectio n 11.3

. Th e laborator yshoul d monito rth e frequenc yo fdat a s o qualifie d t o ensur e tha ti tremain s a to r belo w5%

. 8. 5 Eac h day , th e analys tmus t demonstrat e throug h th e analysi s o f reagen twater , tha tinterference s fro m th e analytica l syste m ar e unde rcontrol

. 8. 6 I ti s recommende d tha tth e laborator yadop tadditiona l qualit y assuranc e practice s fo rus e wit h thi s method

. Th e specifi cpractice s tha tar e mos tproductiv e depen d upo n th e need s o fth e laborator yan d th e natur e o fth e samples

. Fiel d duplicate s ma yb e analyze d t o monito rth e precisio n o f th e samplin g technique

. Whe n doub t exist s ove rth e identificatio n o fa pea k o n th e chromatogram , confirmator y technique s suc h a s ga s chromatograph y wit h a dissimila rcolumn , specifi c elemen tdetector , o rmas s spectrom
ete rmus tb e used

. Wheneve rpossible , th e laborator yshoul d perfor m analysi s o fstandar d referenc e material s an d participat e i n relevan tperformanc e evaluatio n studies

. 8. 7 Th e analys tshoul d maintai n constan tsurveillanc e o fbot h th e per formanc e o fth e analytica l syste m an d th e effectivenes s o fth e metho d i n dealin g wit h eac h sampl e matri xb y spikin g eac h sample , standar d an d blan k wit h surrogat e halocarbons

. A combinatio n o fbromochloromethane , 2-bromo-1-chloropropane , an d 1,4-dichlorobutan e i s recommende d t o encompas s th e rang e o fth e tempera
tur e progra m use d i n thi s method

. Fro m stoc k standar d solution s prepare d a s above , ad d a volum e t o giv e 750 0 p g o feac h surrogat e t o 4 5 m Lo freagen t wate rcontaine d i n a 50-m Lvolumetri c flask , mi xan d dilut e t o volum e ( 1 5 ng/pL)

. I fth e interna l standar d calibra

tio n procedui e i s bein g used , th e surrogat e compound s ma yb e adde d directl yt o th e interna l standar d spikin g solutio n (Sectio n 7.4.2)

. Ad d 1 Op Lo f thi s surrogat e spikin g solutio n directl y int o th e 5-m Lsyring e wit h ever ysampl e an d referenc e standar d analyzed

. Prepar e a fres h surrogat e spikin g solutio n o n a weekl ybasis

. 

### 9

. Sampl e Collection , Preservation , an d Handlin g 9. 1 Al l sample s mus tb e ice d o r refrigerate d fro m th e tim e o fcollectio n unti l extraction

. I fth e sampl e contain s fre e o rcombine d chlorine , ad d sodiu m thiosulfat e preservativ e (1 0 mg/4 0 m L i s sufficien tfo ru p t o 5 pp m Clj ) t o th e empt ysampl e bottl e jus tprio rt o shippin g t o th e samplin g site

. USEP A method s 330. 4 an d 330. 5 ma yb e use d fo rmeasuremen to fresidua l chlorine. 18 ' Fiel d tes tkit s ar e availabl e fo rthi s purpose

. 9. 2 Gra b sample s mus tb e collecte d i n glas s container s havin g a tota l volum e o fa tleas t2 5 mL

. Fil l th e sampl e bottl e jus tt o overflowin g i n suc h a manne rtha tn o ai rbubble s pas s throug h th e sampl e a s th e bottl e i s bein g filled

. Sea l th e bottl e s o tha tn o ai rbubble s ar e entrappe d i n it

. I f preservativ e ha s bee n added , shak e vigorousl yfo ron e minute

. Maintai n th e hermeti csea l o n th e sampl e bottl e unti l tim e o fanalysis

. 9. 3 Al l sample s mus tb e analyze d withi n 1 4 day s o fcollection

. 

### 10

. Sampl e Extractio n an d Ga s Chromatograph y 10. 1 Tabl e 1 summarize s th e recommende d operatin g condition s fo r th e ga s chromatograph

. Include d i n thi s Tabl e ar e estimate d retentio n time s an d metho d detectio n limit s tha tca n b e achieve d b ythi s method

. A n exampl e o fth e separation s achieve d b yColum n 1 i s show n i n Figur e 5

. Othe rpacke d columns , chromatographi cconditions , o rdetector s ma yb e use d i fth e requirement s o fSectio n 8. 2 ar e met

. 10. 2 Calibrat e th e syste m dail ya s describe d i n Sectio n 7

. 10. 3 Adjus tth e purg e ga s (nitroge n o rhelium ) flo wrat e t o 4 0 mL/min

. Attac h th e tra p inle tt o th e purgin g device , an d se tth e devic e t o purge

. Ope n th e syring e valv e locate d o n th e purgin g devic e sampl e introductio n needle

. 10. 4 Allo wsampl e t o com e t o ambien ttemperatur e prio rl o introduc

in g i tt o th e syringe

. Remov e th e plunge rfro m a 5-m Lsyring e an d attac h a close d syring e valve

. Ope n th e sampl e bottl e (o rstandard ) an d carefull ypou r th e sampl e int o th e syring e barre l t o jus tshor to foverflowing

. Replac e th e 601-5 July 1982P. 7

syring e plunge ran d compres s th e sample

. Q.pe n th e syring e valv e an d ven tan yresidua l ai rwhil e adjustin g th e 'sampl e volum e t o 5. 0 mL

. Sinc e thi s proces s o ftakin g a n aliquo tdestroy s th e validit yo fth e sampl e fo rfutur e analysis , th e analys tshoul d fil l a secon d syring e a tthi s tim e t o protec t agains tpossibl e los s o fdata

. Ad d 1 0. 0 p Lo fth e surrogat e spikin g solu

tio n (8.7 ) an d 1 0. 0 p Lo fth e interna l standar d spikin g solutio n (Sectio n 7.4.2) , i fapplicable , throug h th e valv e bore , the n clos e th e valve

. 10. 5 Attac h th e syringe-syring e valv e assembl yt o th e syring e valv e o n th e purgin g device

. Ope n th e syring e valve s an d injec tth e sampl e int o th e purgin g chamber

. 10. 6 Clos e bot h valve s an d purg e th e sampl e fo r1 1. 0 ±
. 1 minute s a t ambien ttemperature

. 10. 7 Afte rth e 1 1 -minut e purg e time , attac h th e tra p t o th e chromatograph , adjus tth e devic e t o th e desor b mode , an d begi n t o temperatur e progra m th e ga s chromatograph

. Introduc e th e trappe d material s t o th e G C colum n b y rapidl yheatin g th e tra p t o 1 8 0 ° C whil e backflushin g th e tra p wit h a n iner tga s betwee n 2 0 an d 6 0 mL/mi n fo rfou rminutes

. I frapi d heatin g o fth e tra p canno tb e achieved , th e ga s chromatographi ccolum n mus tb e use d a s a secondar ytra p b ycoolin g i tt o 3 0 ° C (subambien t temperature , i fpoo r pea k geometr yo rrando m retentio n tim e problem s persist ) instea d o fth e initia l progra m temperatur e o f4 5 °C

. 10. 8 Whil e th e tra p i s bein g desorbe d int o th e ga s chromatograph , empt yth e purgin g chambe rusin g th e sampl e in

troductio n syringe

. Was h th e chambe r wit h tw o 5-m Lflushe s o freagen t water

. 10. 9 Afte rdesorbin g th e sampl e fo r fou rminute s reconditio n th e tra p b y returnin g th e purg e an d tra p devic e t o th e purg e mode

. Wai t1 5 second s the n clos e th e syring e valv e o n th e purgin g devic e t o begi n g3 S flo wthroug h th e trap

. Th e tra p temperatur e shoul d b e maintaine d a t1 8 0 °C

. Afte rapproxi

matel yseve n minute s tur n of fth e tra p heate ran d ope n th e syring e valv e t o sto p th e ga s flo wthroug h th e trap

. Whe n coo l th e tra p i s read yfo rth e nex tsample

. 10.1 0 Th e widt h o fth e retentio n tim e windo wuse d t o mak e identifica

tion s shoul d b e base d upo n measure ment s o factua l retentio n tim e variation s o fstandard s ove rth e cours e o fa day

. Thre e time s th e standar d deviatio n o fa retentio n tim e fo ra compoun d ca n b e use d t o calculat e a suggeste d windo w size ; however , th e experienc e o fth e analys tshoul d weig h heavil yi n th e interpretatio n o fchromatograms

. 10.1 1 I fth e respons e fo rth e pea k exceed s th e workin g rang e o fth e system , prepar e a dilutio n o fth e sampl e wit h reagen twate rfro m th e aliquo ti n th e secon d syring e an d reanalyze

. 

### 1 1

. Calculation s 11. 1 Determin e th e concentratio n o f individua l compound s i n th e sample

. 11.1.1 I fth e externa l standar d calibratio n procedur e i s used , calculat e th e concentratio n o fmateria l fro m th e pee k respons e usin g th e calibratio n curv e o rcalibratio n facto rdetermine d i n Sectio n 7.3.2

. 11.1.2 I fth e interna l standar d calibratio n procedur e wa s used , calcu

lat e th e concentratio n i n th e sampl e usin g th e respons e facto r(RF ) deter

mine d i n Sectio n 7.4. 3 an d equatio n 2

. Eq

. 2

. Concentratio n pg/ L= (A s C is )/(A is )(RF ) where : A s = Respons e fo rth e paramete rt o b e measured

. A 1 S = Respons e fo rth e interna l standard

. C s = Concentratio n o fth e interna l standard

. 11. 2 Repor tresult s i n microgram s pe rliter

. Whe n duplicat e an d spike d sample s ar e analyzed , repor tal l dat a obtaine d wit h th e sampl e results

. 11. 3 Fo rsample s processe d a s par t o fa se twher e th e spike d sampl e recover yfall s outsid e o fth e contro l limit s whic h wer e establishe d accordin g t o Sectio n 8.3 , dat a fo rth e affecte d parameter s mus tb e labele d a s suspect

. 

### 12

. Metho d Performanc e 12. 1 Th e metho d detectio n limi t (MDL ) i s define d a s th e minimu m concentratio n o fa substanc e tha tca n b e measure d an d reporte d wit h 99 % confidenc e tha tth e valu e i s abov e zero. 11 ' Th e MD Lconcentration s liste d i n Tabl e 1 wer e obtaine d usin g reagen t water.19 ' Simila rresult s wer e achieve d usin g representativ e wastewaters

. Th e MD Lactuall yachieve d i n a give n analysi s wil l var ydependin g o n instru

men tsensitivit yan d matri xeffects

. 1 2. 2 Thi s metho d i s recommende d fo rus e i n th e concentratio n rang e fro m th e MD Lu p t o 1 00 0 xMDL

. Direc t aqueou s injectio n technique s Shoul d b e use d t o measur e concentratio n level s abov e 100 0 xMDL

. 12. 3 I n a singl e laborator y(Monsant o Research) , usin g reagen twate ran d

•wastewater s spike d a to rnea rback

groun d levels , th e averag e recoverie s presente d i n Tabl e 2 wer e obtained 19 '

. Th e standar d deviatio n o fth e measure men ti n percen trecover yi s als o include d i n Tabl e 2<9'

. 12. 4 Th e U.S

. Environmenta l Protectio n Agenc yi s i n th e proces s o f conductin g a n interlaborator ymetho d stud yt o full ydefin e th e performanc e o fthi s method

.



### Reference s

1

. Se e Appendi xA

. 2

. Bellar , T.A. , an d Lichtenberg , J.J

. Journal American

Water Works Association, 66, 739 , (1974)

. 3

. Bellar , T.A. , an d Lichtenberg , J.J

. "Semi-Automate d Headspac e Analysi s o fDrinkin g Water s an d Industria l Water s fo rPurgeabl e Volatil e Organi c Compounds, " Proceeding s fro m Symposiu m o n Measuremen to f Organi cPollutant s i n Wate ran d Wastewater , America n Societ yfo r Testin g an d Materials , ST P 686 , CE

. Va n Hall , editor , 1978

. 4

. "Carcinogen s —Workin g Wit h Carcinogens, " Departmen to fHealth , Education , an d Welfare , Publi cHealt h Service , Cente rfo rDiseas e Control , Nationa l Institut e fo rOccupationa l

. Safet yan d Health , Publicatio n No

. 77-206 , Aug

. 1977

. 5

. "OSH ASafet yan d Healt h Stand

ards , Genera l Industry, " (2 9 CF R 1910) , Occupationa l Safet yan d Healt h Administration , OSH A2206 , (Revised , January , 1976)

. 6

. "Safet yi n Academi cChemistr y Laboratories, " America n Chemica l Societ yPublication , Committe e o n Chemica l Safety , 3r d Edition , 1 979

. 7

. "Handboo k

fo rAnalytica l Qualit y Contro l i n Wate ran d Wastewate r Laboratories, " EPA-600/4-79-0 1 9 , U.S

. Environmenta l Protectio n Agency , Environmenta l Monitorin g an d Suppor t Laborator y—Cincinnati , Ohi o 45268 , Marc h 1979

. 8

. "Method s 330. 4 (Titrimetric , DPD

FAS ) an d 330. 5 (Spectrophotometric , DPD ) fo rChlorine , Tota l Residual, " Method s fo rChemica l Analysi s o fWate r an d Wastes , EP A600/4-79-020 , U.S

. Environmenta l Protectio n Agency , 601-6 July 1982P. 8



### Environmenta l Monitorin g an d Suppor t Laboratory—Cincinnati , Ohi o 45268 , March'l,9'79

. '9

. "EP AMetho d Validatio n Stud y23 , Metho d 60 1 (Purgeabl e Halocarbons), " Repor tfo rEP AContrac t68-03-285 6 (I n preparation)

. Table 1. Chromatographic Conditions

and Method Detection

Limits

Parameter Chloromethane Bromomethane Dichlorodifluoromethane Vinyl chloride Chloroethane Methylene

chloride Trichlorofluoromethane 1,1 -Dichloroethene 1,1 -Dichloroethane trans-1,2-Dichloroethene Chloroform 1,2-Dichloroethane 1,1,1 -Trichloroethane Carbon tetrachloride Bromodichloromethane 1,2-Dichloropropane trans-1,3-Dichloropropene Trichloroethene Dibromochloromethane 1,1,2-Trichloroethane cis-1,3-Dichloropropene 2-Chloroethylvinyl

ether Bromoform 1, 1,2,2-Tetrachloroethane Tetrachloroethene Chlorobenzene 1,3-Dichloroben/ene 1,2-Dichlorobenzene 1,4-Dichlorobenzene Retention Time
Column 1 1.50 2.17 2.62 2.67 3.33 5.25 7.18 7.93 9.30 10.1 10.7 11.4 12.6 13.0 13.7 14.9 15.2 15.8 16.5 16.5 16.5 18.0 19.2 21.6 21.7 24.2 34.0 34.9 35.4 (mm.) Column 2 5.28 7.05 nd 

### 5.28 8.68 10.1 nd 

### 7.72 12.6 9.38 12.1 15.4 13.1 14.4 14.6 16.6 16.6 13.1 16.6 18.1 18.0 nd 

### 19.2 nd 

### 15.0 18.8 22.4 23.5 22.3 Method

Detection

Limit M/L 

### 0.08 1.18 1.81 0.18 0.52 0.25 nd 

### 0. 13 0.07 0.10 0.05 0.03 0.03 0.12 0.10 0.04 0.34 0.12 0.09 0.02 0.20 0. 13 0.20 0.03 0.03 0.25 0.32 0.15 0.24 nd = not determined Column 1 conditions:

Carbopack

B 60/80 mesh coated with 1 %SP-1000

packed in an 8 ft x0.1 in

ID stainless

steel or glass column with helium carrier gas at 40 mL/min flowrate. Column

temperature

held at 45° C for 3 min. then

programmed at 8 °C/min. to

220 ° and held for 15 min. Column 2 conditions:

Porasil-C

100/120 mesh coated with n-octane

packed in a 6 ft x0.1 in ID stainless

steel or glass column with helium carrier gas at 40 mL/min flow rate. Column

temperature

held at 50°C for 3 min then programmed

at 6°C/min to 170° and held for 4 min. -

601-7 July 1982P. 9

Table 2. Single

Operator

Accuracy

and Precision

' • *



## . ' Parameter Br oinodichlorome

thane Bromoform Bromomethane Carbon tetrachloride Chlorobenzene Chloroethane 2-Chloroethylvinyl

ether Chloioform Chloromethane Dibrornochlcromethane 1,2-Dichlorobenzene. 1,3-Dichlorobenzene' 1,4-Dichlorobenzene Dichlorodifluorome

thane 1, 1-Dich/orcethane 1,2-Dichloroethane 1, 1 -Dichloroethene trans-1,2-Dichloroethene 1,2-Dichloropropane cis-1,3-Dichloropropene trans-1,3-Dichloropropene Methylene

chloride 1,1,2,2-Tetrachloroethane Tetrachloroethene 1, 1,1-Trichloroethane 1, 1,2-Trichloroethane Trichloroethene Trichlorofluoromethane Vinyl chloride Average Percent Recovery 100.9 89.5 105.0 82.5 93.9 91.5 96.3 101.7 91.4 98.3 10.20 91.6 9 7.5 87.8 102.3 9 7.8 101.1 91.0 97.7 86.7 73.5 97.9 91.9 94.1 75.1 91.0 106.1 89.3 101.9 Standard

Deviation 

## % 5.0 9.0 17.3 25.6 8.9 22.4 9.9 20.6 13.4 6.5 2.0 4.3 9.3 18.0 5.5 4.8 21.7 19.3 8.8 6.0 17.2 2.6 15.0 18.1 12.5 25.1 7.4 13.9 11.4 Spike

Range 

### (ug/U 0.43-46.7 1.45-50 3.39-49.2 0.55-50 2.21-50 3.95-50 4.39-133 0.44-50 0.55-23.9 0.75-93.0 4.89-154 2.94-46.7 2.99-51.6 2. 18-43.4 0.44-46.7 0.44-46.7 0.37-50 0.44-98.0 0.29-39.0 0.44-46.7 0.43-50 0. 73-46. 7 0.46-46.7 0.50-35.0 0.37-29.0 0.45-50 0.38-46.7 149 0.82-32.3 Number



## of Analyses 21 20 21 19 20 21 20 20 21 21 21 21 21 21 21 21 19 20 21 21 20 21 21 21 21 21 21 14 21
Optional Foam Trap Matrix

Types 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3 2 3



## ( ^ ^ _Exit

V 4in. O.D. -*
. 14mm O.D. Inlet V 4in. O.D.

V 4in. O.D. exit Sample Inlet 2-way Syringe

valve
^"
—17cm

20 gauge syringe

needle
1 6mm O.D. Rubber

Septum ^10mm O.D. '/, „ in. O.D.

/Stainless

Steel

— - Inlet / « in. O.D.

13X

molecular / ,/Asieve

purge gas filter

Purge gas flow control 1 0mm glass frit medium porosity

601-8 Figur e 1
. Purging device July 1982P.1 0
Packing procedure Construction

Glass 5mm f ^ wool
Activated

7.7cm

yz charcoal

Grade 15 Silica gel 7.7cm

Tenax 7.7cm



### 3%OV-1 Glass wool 1 cm

5mm 7 n i'foot resistance wire wrapped solid (Double layer)

15 cm

Tv 'foo t resistance wire wrapped solid (Single layer) 8cm — Compression fitting nut and ferrules

Thermocouple/ controller sensor
Electronic temperature control end pyrometer Tubing 25 cm. 0.105 in. ID. 0.125 in O.D. stainless steel

Trap inlet

Figur e 2

. Trap

packings

and construction

to include desorb

capability

Carrier gas flow control Pressure regulator

\y^—

fe^dPurge gas flow control \

13X molecular sieve filter Liquid injection

ports Column

oven ~"ir~fc>l— i M i I J u " > C —

Confirmatory

column



# ^ L -Analytical column \ optional

4-port column 6-port selection

valve valve /

Tra P in,et Resistance

wire ^yHeater control

Purging device Note:

All lines between trap and GC should be heated to 80°C
Figur e 3

. Schematic of purge and trap device —purge

mode

601-9 July 1982P.1 1

Carrier gas flow control 

# yl'a Pressure regulator

Purge gas v flow control

v | Liquid injection

ports

r , ^

. '

H

^.Column

oven ^..JWbl!- , n H f l H—^

—Confirmatory column 

# CM '^ j , . n 

# n n 

# ._L> r 

# ° detecto r 

## iQipj^UU 1 t

73 Xmolecular sieve filter Analytical column ional 4-port column selection valve Trap inlet Resistance

wire

! On .Heater

control

Purging de vice Note:

All lines between trap and GC should be heated to 80°C

Figur e 4

. Schematic of purge and trap device —desorb

mode

Column: 1%SP-1000

on Carbopack-8 Program: 45°C-3

minutes. 8°/minute to 220°C Del act or; Hall 700-Aelectrolytic

conductivity

Retention

time, minutes
Figur e 5

. Gas

chromatogram

of purgeable

halocarbons
601-10 July 1982