p. 1


# OAR Box 1124 Prepped by Ollie Stewart



# Document

Number: 

# 60 ) ll-D- 1 Docket Number: 

# A-84-4 4

Printed 4/16/20088:13:21 AM

'

Sheet

60of 70

# IW 

# 'k-M-'M P 

# " Nationa l Cooperativ

e Refiner yAssociatio n 200 0 SOUT H MAI N ST . •P.O . BO X140 4 •McPHERSON . KANSA S 67460 •316/241-234 0 /.•' . 

## Februar y21 , 198 5

Mr . Jac k R . Farme r Director , Emissio n Standard s an d Engineerin g Divisio n U.S . Environmenta l Protectio n Agency , Offic e o f Ai r Qualit y Plannin g an

d Standard s Researc h Triangl e Park , N C 2771 1 Dea r Mr . Farmer : Thi s lette r i s i n respons e t o you r Januar y25 , 198 5 lette r request
ing informatio n o n proces s equipmen t an d associate d emissio n con tro l equipmen t subjec t t o th e "ne wsourc e performanc e standard " a t ou r McPherson , Kansa s refinery . W e understand tha t yo u ar e 'requesting onl yinformatio n tha t i s availabl e withou t doin g addi

tiona l test s o r studies , s o th e followin g response s t o th e ques tion s hav e bee n prepare d wit h tha t i n mind . Th e forma t o f th e answer s belo wwil l b e th e sam e a s tha t o f th e question s a s receive d i n ENCLOSUR E 1 i n a n effor t no t t o repea t th e question s and kee p th e answer s a s brie f a s possible . I . INTRODUCTION N o respons e required . II . FACILIT Y DESCRIPTIO N Fig . I (Dwg . NCRA-F-8278 ) i s a curren t drawin g o f ou r refin

eryfue l ga s syste mtha t shoul d b e sel f explanatory . Swee t Natura l Ga s enter s o n th e middl e righ t hand sid e o f th e draw

ing an d durin g thi s tim e o f th e yea r th e flo wrat e i s approx imatel y8 M M SCF D and i s distribute d a s show n o n th e drawing . Th e flo wo f propane , shown enterin g th e middl e botto mo f th e drawing , i s normall yzer o an d i s use d onl yi f w e ar e unabl e t o ge t natura l gas . Th e refiner yfue l gase s ar e th e Cat , Coke r and Saturate s Spong e Absorbe r gase s and ar e show n en terin g th e drawin g i n th e lowe r lef t hand area . Th e gase s ar e sour , containin g approximatel y2. 8 mol e % o f H-S , an d ar e sen t t o th e Hig h Pressur e Amin e absorbe r wher e al l bu t 5 0 mol e ppmo f th e H_ S i s remove d befor e th e gase s flo wt o th e tw o fue l drum s fo r distributio n t o th e variou s user s throughou t th e refinery . Al l gase s tha t d o no t g o direc t t o a use r ar e blende d i n th e Plan t Fue l Dru m (W-086 ) excep t fo r th e 2. 7 M M SCF D o f ga s fromth e Fue l Dru man d 3. 7 M M SCF D o f Natura l Ga s tha t ar e blende d i n th e lin e goin g t o

Snnnlvlr.a

Refined

Fuels FARMLAN D INDUSTRIES . INC. . KANSA S CITY . MISSOUR I •FARMER S UNIO N CENTRA L EXCHANGE . INC. . ICENEXI . SAIN TPAUL . MINNES0 1P. 3



## Mr . Jac k R . Farme r Februar y21 , 198 5 Pag e 2 th e FP UHeaters . Th e blende d fue l ga s i n th e Fue l Dru mthe n exit s th e dru

ma t severa l location s fo r distributio n t o th e man yuser s throughou t th e plant . Fig . I I (Dwg . D-914-C621 ) i s a proces s flo wdiagramo f ou r Diese l Hydrotreatin g Uni t tha t contain s on e o f ou r NSP S heat

ers . Fig . Il l (Dwg . D-914-N634 ) i s a proces s flo wdiagram o f ou r Cokin g Uni t whic h contain s ou r othe r tw o NSP S heaters . Fig . IV i s a sketc h showin g th e man ystream s enterin g an d leavin g th e Amin e Uni t and wa s th e basi s fo r th e desig n o f th e unit . An overal l sulfu r balanc e i s i n th e uppe r righ t hand corne r o f th e drawin g bu t flo wrate s an d sulfu r concen tration s ar e note d o n eac h stream . Fig . V i s a Proces s Flo wDiagramo f th e Amin e Uni t an d con tain s muc h o f th e same informatio n tha t i s show n o n Fig . IV , however , i f ther e ar e an ydiscrepancie s Fig . V shoul d b e correc t a s i t i s th e officia l design . Als o note d o n Fig . V , i n red , ar e som e typica l operatin g flo wrate s whic h sho w tha t w e ar e operatin g a t abou t 75 % o f design . III . COST S 1 . Ou r Amin e Uni t i s a ne wuni t buil t durin g 198 3 an d 198 4 a t a cos t o f $4.9 8 M M an d pu t onstreamdurin g Jun e o f 1984 . Thi s $4.9 8 M M include s al l material s and labo r u p t o th e tim e th e uni t wa s pu t int o operatio n bu t doe s no t includ e th e initia l chemica l inventory . Abreakdown o f cost s ar e a s follows : a . Purchas e Cos t o f Uni t r 1 . Al l equipmen t and labo r - $4,980,000 . 2 . Initia l chemica l inventory- $25,500 . b . Installatio n Cos t 1 . Include d i n above . 2 . No t available . Annua l Operatin g Cost s 1 . Labo r cost s = $285,000/yea r includin g overhea d

7,12 5 hour s a t $40/hour .P. 4



## Mr . Jac k R . Farme r Februar y21 , 198 5 Pag e 3



## d . 2 . Material s a . No t availabl e - ne wunit . b . Chemical s - 5,00 0 gallon s - $2.85/gallon . 3 . Stea m

- 11,00 0 Lbs/Hr , 5 5 psig , 300°F ,

$3.10/1,00 0 Lbs . 1,50 0 Lbs/Hr , 22 5 psig , 400°F , $4.40/1,00 0 Lbs . 4 . Electricit y= $120,000/Yr . 5 . Wate r - No t available . 6 . N o direc t fue l usage . 7 . Sulfu r - $325,000/Yr . Ke yAccountin g Factor s 1 . Lease d asse t - n o lifetim e established . 2 . Lease d asse t - non e established . 3 . Labo r - $13.50/Hr. , Managemen t - include d i n # 4 below . 4 . $26.50/Hr . IV . REFINER Y COMBUSTIO NDEVICE S 1 . W e hav e 3 6 combustio n sources . 2 . Proces s Heater s Boiler s Compressor s Flare s

a . Size — MM BTU/Hr . Inpu t b . Costs — Capita l Operatin

g MM$/Yr . c . Operation

— Days/Year d . Othe r Fuel s 5 t o 7 0 - - 5 0 t o 15 0 3 t o S 1 t o 3 -
N AN

AN

AN

A 0.1-2. 1 1.5-4. 5 0.1-0. 3 .03-.0 9 35 0 35 0 35 0 35 0 C3 , Slurr

yC3 , Slurr

yNon e Non eP. 5



## Mr . Jac k R . Farme r Februar y21 , 198 5 Pag e 4 3 . NCRAha s thre e ne wproces s heater s tha t ar e subjec t t o

NSPS . The yar e a s follows : Tw o ne wCokin g Heaters , HF-009 Aan

d HF-009B , rate d 6 6 M M BTU/Hr . inpu t eac h tha t wer e complete d i n 1983 . On e ne wDiese l Hydrotreate r Heater , HP-012 , rate d 2 7 M M BTU/Hr . inpu t tha t wa s com plete d i n 1984 . W e complie d wit h th e NSP S b ybuildin g a n Amin e Uni t tha t remove s th e H 2 

## S fromth e fue l ga s and b ycausin g a n Ammoniu mThiosulfat e plan t t o b e built , acros s th e fence , t o tak e th e H 2 

## S w e generate d an d tur n i t int o Ammoniu

mThiosulfat e fertilizer . Th e H- S con ten t o f th e fue l ga s decrease d fromth e forme r 2. 0 Mol e % H~ S t o th e presen t 5 0 Mol e ppmH 2 

## S whic h i s a reduc

tio n o f 99.75% . I woul d sa ytha t th e cos t o f complianc e wa s th e cos t o f th e Amin e Uni t whic h i s state d above . a . N o - buil t ne wAmin e Unit . b . Ye s - ne wAmin e Treater .

4 . 5 . c . d . e . f . I No . No . No . No . don' t kno w None . V . PRIMARY CONTRO L (AMIN E TREATERS ) \ 1 . a . 17. 5 M M SCFD . b . 88 0 Ne t - 97 2 Gros s BTU/SCF . c . 100° F - 15 0 psig . d . 86.8 % H 2 

## S , 12.5 % C0 2 

## , 0.6 % N 2 

## , 0.1 % CH 4 

## , 0.1 % C 2 

## H g 

## , 2 . W e onl yhav e on e Amin e Treater . a . Se e Fig . I V

an d Fig . V

enclosed . b . Designe d an

d buil t b

yFord , Baco n & Davis . c . Jun e 6 , 1984 . d . Desig n - 39. 4 long ton s pe r day , Rang e - 7 t o 39. 4 long ton s pe r day .P. 6



## «. Mr . Jac k R . Farme r Februar y21 , 198 5 Pag e 5

3 . 4 . e . f . g . h . i . j

k . 8,40 0 hour s pe r year . Se e Fig . V . 30,00 0 gallon s o f 20 % MEA , Se e Fig . V . Se e Fig . V . MEA . None . Probabl ynone . Th e uni t wa s onl ybee n onstre a

5 , 6 , 7 . 8 . bee n n o majo r outage s sinc e start-up . Th e bigges t prob

lem s t o dat e hav e bee n freeze-up s goin g through th e firs t winte r an

d some foamin g problem s du e t o imprope r reclaim

e r operation . a . Yes , some - Amin e usag e 13. 5 gallon s pe r day . b . Stil l a proble mbu t continuou s anti-foaminjec

tio n keep s th e foa munde r control . c . Probabl ycausin g th e foaming . d . Ver yminimal . e . None . No . Excellen t fo r 8 months . UO P wil l inspec t ever ytw o year s durin g turnarounds . H_ S concentration s i n swee t ga s fromth e absorbers , H 2 

## S and CO
- loading s i n th e lea n an d ric h amin e streams , amin e strength , an d hea t stabl e salt s i n th e lea n Amine . Lo wH 2 

## S concentration s i n th e outle t swee t ga s hav e neve r bee n 5 proble mt o date . VI . SECONDARY CONTRO L (SULFU R PLANTS , ETC. ) 1 . Th e Aci d Ga s streamexitin g th e amin e treate r i s sol d t o Kerle yIndustrie s wh o operate s a thiosulfat e plan t and mak e Ammoniu

mThiosulfat e Fertilizer . Thi s plan tP. 7



## *> " Mr , Jac k R . Farme r Februar y21 , 198 5 Pag e 6 wa s designe d an d buil t b

yother s durin g 198 3 an d 198 4 and wa s starte d u p Jun e 6 , 1984 . I t i s designe d t o handl e al l o f th e Aci d Ga s w e mak e an d sen d t o them . 2 . Owne d b

yother s and doe s no t us e amin e scrubbing . VII . EMISSIONTESTING 1 . Acop yo f th e EP APS D permi t performanc e tes t i s en close d a s Fig . V I an d consist s o f 1 6 page s tha t shoul d answe r th e question s presented . a . Approximatel y$6,00 0 includin g N O testing . b . No , b

yTota l Sourc e Analysi s Inc . c . None . d . Se e Fig . Il l fo r th e locatio n o f th e sampl e point , whic h i s o n th e fue l ga s lin e t o th e Cokin g Heater s and i s downstreamo f th e Plan t Fue l Drum , wher e some Natura l Ga s i s blende d wit h th e refiner yfue l gas . O n tha t day57 5 MSCF D o f Natura l Ga s wa s blende d wit h 14,79 6 MSCF D o f refineryfue l ga s t o mak e th e blend goin g t o th e Cokin g Heaters . N O testin g wa s als o performe d durin g th e sam e tes t per iod " an d al l thos e result s ar e als o "included i n Fig . VI . Yo u wil l not e tha t on e o f th e Coke r Heater s di d no t mee t th e require d N O concentration s s o modification s ar e currentl ybein g mad e and anothe r tes t ha s bee n schedule d i n th e nea r future . 3 . No . VIII . MONITORING O F EMISSION S AND PROCES S OPERATION 1 . N o respons e required . 2 . None . 3 . W e monito r th e H 2 

## S concentratio n a t th e outle t o f

th e Hig h Pressur e Amin e Absorbe r wit h periodi c gra b sample s fo r ou r own purpose s t o ensur e tha t th e amin e treate r i s operatin g properl yan d t o ensur e tha t w e ar e i n complianc e wit h th e NSPS . W e sampl e onc e pe r wee k wit h a Draege r Tub e unles s operation s ar e change d o r a n upse t occur s an d th e nee d fo r mor e frequen t sample s i s demonstrated . Th e cos t i s ver yminimal , $ 5 t o $1 0 pe r sample , th e accurac yi s plu s o r minu s 10% , an d th e onl yprob

lem s ar e frostin g up o f th e Draege r Tub e whe nP. 8



## Mr . Jac k R . Farme r Februar y21 , 198 5 Pag e 7 runnin g a liqui d propan e o r butan e sample . Thi s

proble mwa s alleviate d byinstallin g a smal l sampl e vaporizer . c . Non e ar e used . 1 . N o respons e required . 2 . N o respons e required . 3 . N o respons e required . 4 . N o respons e required . 5 . N o respons e required . 4 . Monitorin g o f Proces s Parameter s a . None . b . None . 5 . No . 6 . Don' t hav e an

yinstrumen t monitors . IX . GENERA L REFINERY INFORMATION 1 . Th e nomina l siz e o f ou r refiner yi s 70,00 0 BPC D and , excep t fo r Januaryand Februar yo f 1985 , w e hav e bee n operatin g a t th e 70,00 0 BPS D level . Ou r curren t opera tin g schedul e i s t o run continuously , excep t fo r a fou r wee k majo r turnaround o n odd numbere d year s an d a 5 day Crude/Cokin g Uni t turnaround o n eve n numbere d years . Th e quantit yan

d sulfu r conten t o f th e Sou r Crud e tha t w e run ha s th e larges t effec t o n th e aminestreaters . 2 . Th e typica l wt . % sulfu r i n ou r swee t crud e i s 0.4 % wit h a rang e o f 0.35 % t o 0.45% . Th e typica l wt . % sulfu r i n ou r sou r crud e i s 1.8 % wit h a rang e o f 1.4 % t o 3.0% . • Th e highe r th e leve l o f sulfur

- i n th e crud e th e mor e amin e w e mus t circulat e t o maintai n reasonabl e loading s o f H_S i n th e ric h amin e an d this , i n turn , cause s th e hea t load o n th e amin e regenerato r reboiler s t o b e in

crease d t o maintai n goo d strippin g o f th e H 2 

## S fro mth e lea n amine . T o dat e w e se e n o increas e i n th e H 2 

## S con ten t o f the.fue l ga s becaus e o f mor e sulfu r i n tn e crud e oil . 3 . Whe n w e ar e processin g sou r crud e some o f th e distillat e stream s mus t b e desulfurize d t o mee t sulfu r specifica

tion s an

d amin e uni t cost s increas e directl yb yth e amoun t o f sulfu r tha t i s removed .P. 9



## Mr . Jac k R , Farme r Februar y21 , 198 5 Pag e 8 4 . Natura l Ga s i s blende d int o th e refineryfue l ga s sys te mfo r onl yon e reaso n an d tha t bein g t o maintai n pres sur e o n th e fue l dru ms o ther e i s a n adequat e suppl yo f fue l t o maintai n operations . N o blendin g i s don e t o dilut e H 2 

## S concentration s becaus e th e H 2 

## S concentratio n i n th e fue l ga s leaving th e amin e treate r i s wel l belo w th e allowabl e H 2 

## S concentratio n an d ca n b e use d a s fue l directly . X . GENERA L REGULATORY INFORMATION 1 . Ver ylittle , none , minimal . 2 . None . 3 . Negligible , n o routin e repor t i s reguired . XI . CONTACT S FO R FURTHE R INFORMATION Nationa l Cooperativ e Refiner yAssociatio n H.W . Davidson , Proces s Enginee r P.O . Bo x 140 4 McPherson , K S 6746 0 Sincerely , NATIONAL COOPERATIVE REFINERY ASSOCIATIO N

E.C . Ewin g ( Technica l Directo r /al u Attachment s

# Jr P.1 0



## SECTIO NI INTRODUCTIO N

A n EP APS D permi t performanc e tes t wa s conducte d o n Octobe r 1 7 an d 18 , 198 4 a t th e NCR Arefiner yi n McPherson , Kansas . N O performanc e test s fo r HF-009 Aand HF-009 B wer e performe d simul

taneousl yo n Octobe r 17 , 198 4 fro mapproximatel y9:3 0 A.M . t o 1:0 0 P.M . Fue l ga s performanc e test s fo r S O determinatio n wer e performe d Octobe r 17 , 198 4 fromapproximatel y2:0 0 P.M . t o 8:0 0 P.M . N O performanc e test s fo r HP-01 2 wer e performe d Octobe r 18 , 198 4 fro m

approximatel y11:3 0 A.M . t o 2:3 0 P.M . Al l test s wer e performe d i n complianc e wit h EP Astandard s determine d a t th e pretes t meetin g o f Jul y17 , 1984 . Th e followin g peopl e wer e .

- V 

## presen t fo r th e performanc e tests : Joh n Hosma n USEPA , Regio n VI I KC , K S Joh n Gia r USEPA , Regio n VI I KC , K S Car l Vineyar d TSA , Teste r Amherst , Ohi o Bruc e Wood s TSA , Teste r Amherst , Ohi o Ke n Sim s NCRA , Proces s Engr . McPherson , K S NCRA' s operatio n wa s norma l fo r bot h tes t day s with~.n o upset s encountered . Tota l crud e charg e wa s approximatel y70,OCH ) BP D wit h 15,00 0 BP D t o th e ne wcrud e uni t an d 55,00 0 BP D t o th e ol d crud e unit . Tota l reduce d crud e charg e t o HF-009 Aand HF-009 B wa s approximatel y19,00 0 BPD , wit h 4,00 0 BP D fro m th e ne wcrud e uni t an d 15,00 0 BP D fro mth e ol d crud e unit .P.1 1



## INTRODUCTIO N Thi s repor t present s th e result s o f th e NO x Emission s Test s an d th e H2 S Fue l Ga s Compositio n Tes t performe d o n Heater s HF-009A , HF-009 B an d HP-01 2 o f NCRA' s McPhearson , Kansa s Refinery .
Th e purpos e o f th e test s wa s t o determin e th e complianc e o f th e units . Th e result s o f th e test s ca n b e foun d i n Sectio n I I o f thi s report .
Th e emission s testin g wa s performe d b yTota l Sourc e Analysis , Inc. , whos e mai n offic e i s locate d a t 464 0 Telegrap h Rd. , Amherst , Ohi o 44001 .
Th e test s wer e performe d o n Octobe r 1 7 an d 18 , 1984 . Th e testin g wa s performe d i n accordanc e wit h EP Areferenc e method s a s publishe d i n th e Jul y1 , 198 3 Federa l Register , 4 0 CFR , Par t 60 , Appendi x A-"Standard s o f Performanc e fo r Ne w Stationar ySources " an d subsequen t revisions .
Th e testin g equipment , samplin g procedure s an d analytica l procedure s ar e describe d i n Sectio n II I o f thi s report . Th e ra wfiel d data , plan t data , equipmen t calibrations , la b enalysi s report s an d equation s use d i n determinin g fina l result s ar e presente d i n th e Appendix .

### TABL E II . H2 S RESULT S P.1 2 t '+ 

# I

Ru n No . 

## Dat e 1 2

* 5 6 7 prs/dsc f PP M



### 10-17-8 4

10-18-8 4 .011 4 H\

.008 5 \<\$ .009 3 3./

, 3 .005 0 ||. 4 .005 4 jjj^ v



## •Run s 3 an d 4 wer e discarde d du e t o negativ e concentratio n values . 18. 5 13. 8 15. 1 8. 1 8. 8

Th e complet e result s ca n b e foun d o n th e compute r printout s following .Ity*-4 of 4 P.1 3



### Client HYDROGE N SULFID E CONCENTRATIO N 

# /i/aZA <ZSV Projec tNo g?4^~~^5~<- ^ Plan tSit e _ Analysi s Ru n B y _

~ " «oo fb CH 2 

### S = 0.26 3 H^ S (ppm ) = 1.62x10 * (CH 2 

### S )

[VI TN l - VT TN Tsampl e -^/I TN l - VT TN Tblankj VmST D

Samplin g Locatio n Ru n

No . VI T N l VT T N T Vm(STO ) Cone . H 2 S pp m

H 2 S 

# A 

# 1 S'O ooq* ? 

# ^7,' 7 jOJOl /sb^V ^ t 

# r>tM 

# te,6 /Q-i Z 

# -2- Go L-CZDSS- 

# W'tt tO/Vl 

# WK A//A

£CL ,ndi a 

### ( **&*> 

# ,o/oj 

# AS2. 

# /u/A DO<P>£ >?>,& 

# V 

# £L ^ o ,C&\°\ 

# y&.u .oia/ ,<&& tOO°i 3 AS", / /*-/ & 

# A r o ropq^ ? 

# -ygio o/O / 

# A7J7 oog'ci S T
. I 

# JL _X^

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### T ? ^9,< ? 

# .n/oj 

# *HSfl tpo&q jg^ B 

# -£ U ^2^
. -^o ^ *?•<= » /D/g> / 

# /^ L 

# /^b
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# Mt:H-»NNE"

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### ?SA K TIM E N O • > 1 ^ 

### 3 4 

### 5 6 T 

### 9 9 1 3 : i* - 

### 1 2 -M 3 - M 4 1 5 1 6 1 7 lMIN >

1 . 19 7 2.31 8 3.28 9 5 . 15 6 5.74 2 6.57 9 12.99 4 17.09 0 18.09 9 20.42 0 21 '. •! • 3 f 24.45 9 25.27 6 26.46 6 27.64 5 31.20 8 34.64 3 PEA K

NAM E HYDROGE N ETHYLEN E ETHAN E OXYGE N NITROGE N METHAN E C5=.C S + PROPAN E PROPYLEN E IS0-C 4 'Ji — -1 . - 

### 1-BUTEN E I SO-BUTY L T-BUTEN- 2 C-BUTEN- 2 IS0-C 5 N-C 5

= TOTAL S =
CHE M GROUPS : 3UTYLENE S HYDROCARBON S lUNIDE l CITIFIE D RESPONS E MOL-' < 

### 40.45 5 4.52 2 15.39 3 .03 0 2.54 4 32.0 2 3

. 10 3 t .37 6 2.33 4 .41 9

. t T 5



### . 13 2

. 17 0

. 12 9 .39 3 .0 5 7
• Q l I 

### 93.99 9

.52 8 56.9 7 1 0.03 0 S P

GS-VlTj

- .32 3 .34 4

. 16 0 .30 3 .02 5

. 17 7 .03 3 .02 1 .03 0 .30 8

. Od j 

### .00 3 .03 3 .00 3 .00 2 .00 1 .00 0 .51 3

« S 

### .01 0 .46 5 0.00 0 NE T

BT U I 13.84 6 6 7 

### .73 6 249.0 3 4 3 . 03 3 3 . 00 3 2 9 I . 12 3 4.51 1 3 1 .35 3 45.73 7 12.55 0 i 3 . 4 5 r 

### 3.33 1 4. 3 4 9 3.73 3 2.83 3 2.11 0 .43 1 844.57 2 NORMA L I 2
T * * 

### 15 . 156 " 733.72 0 0.03 0 GROS S

BT U 1 3 1 .07 4 7 

### 2.33 9 2" ? 

### 2.27 3 . 3.03 0 3.03 3 323.33 8 4.71 1 3*.62 8 43.86 3 13.63 2 • ; > . 5 IS

### 4.06 7 5.13 1 3.96 3

. 2.93 9 2.23 2 .43 4 334. 3 3 4 IN G SUrV .
16.22 0 833.32 0 0.03 0 ARE A

COUN T 23353 4 1 9 13 6 5 69935 3 8 3 3 8832 0 359 9 1 2 813 6 7363 3 ' 1 1536 9 28J4 1 Zt wZ « ' i 

### 8?l l 1033 6 36? 8 684 1 439 5 77 9 253030 0 6899360* :

.-- • . *•'-« '



### > . 

### DETECTE D PEAKS : 2 0 REJECTE D PEAKS : ERRORS : 0 INSTRUMEN T CONDITIONS : 0 UNIDENTIFIE D PEA K FACTOR S - - RESPONS E MOL-S S = 0 S P GRAVIT Y = 0

NE T BT U = 0 GROS S BT U = 0 GROU P = 9
FILE : T30 9 TITLE : PT=PEAK- 1 CHANNE L NO : 3 PEA K TABLE : PEAK- 1
SAMPLE : DHTHTRFULGA 3 TIME : 13:4 7 METHOD : CARLEAB S DATE : 292:198 4 

# lo-i8-e« {

S 

### EA X N O 1 2 3 4 

### 5 6 7 8 9 1 0 1 1 1 2 1 3 1 4 TIM E

(MIN ) 2.26 3 3.55 5 5 . 18 4 5.74 4 6.35 8 6.49 4 8.39 8 8.62 6 13.02 5 17.2 7 2 20.72 7 22.41 2 3 1 .842 * 35.58 5 PEA K

NAM E C0 2 ETHAN E OXYGE N NITROGE N METHAN E C O C5=.C6 + PROPAN E IS0-C 4 N-C 4 IS0-C 5 N-C 5

= TOTAL S =
CHE M GROUPS : BUTYLENE S HYDROCARBON S UNID I INTIFIE D RESPONS E MOL-S t

. 10 0 5.82 9 .03 8 10.39 3 0 . 00 0 8 1.09 9 0.00 0 .02 7

. 13 3 1.82 3

. 16 4 .31 0 .06 6 .01 8 100.00 0

_— . . 

### 0.00 3 89.44 2 0.00 0 S P

GRAVIT Y .00 2 .0 6 1 .00 0

. 10 1 0 . 00 0 .44 9 0.00 0 .00 0 .00 4 .02 8 .00 3 .00 6 .00 2

. 00 0 .65 6 <0 ; — 

### 0.00 0 .55 3 0.00 0 NE T

BT U 0 . 00 0 94.30 1 0 . 00 0 0.00 0 0 . 00 0 737.27 1 0 . 03 0 0 . 00 0 5.99 6 42.22 5 4.91 5 9.32 3

~ ~ 2.42 3 .68 2 397 . 14 2 NORMA L I
0 . 03 0 897.15 0 0 . 03 0 GROS S

BT U 0.00 0 103.13 3 0.03 0 . 0.00 0 0.03 0 81.8.35 6 X &•. 00 0 

### .03 8 6.26 2 45.89 7 5.32 8 10.10 8 2 .6 2 1 .73 7 993.00 0 ZIN G SUM :

• - • - - 

### 0.03 0 992.92 3 0.00 0 ARE A

COUN T 387 0 25 1 14 2 108 0 34194 6 99 6 230361 O 15V 8 53 6 1024 8 9882 4
• 1044 6 2025 7 445 8 125 5 305030 0 653769 K t *7 \ •


### 1| 1 DETECTE D PEAKS : E-RGRS : 0 J.l :i'Erl T 

### I r

IED 

### 2 8 REJECTE D PEAKS : 1 4

INSTRUMEN T CONDIT I ON: : 0 FnCTOP S - - ?ES ; 

### > 3M3 I iV_- \ = 0 

# ^1 l ME T ST j • i - ^ 

# n S P G9M7 ! T : • = 3

## SECTIONI I PROCES S INFORMATIO NI NSUPPOR T O F FUE L GA S PERFORMANC E TES T FUE L GA S PERFORMANC E REPOR T Date : Start : Finish : 10-17-8 4

2:0 0 P. M 8:0 0 P. M Sou r Gasse s t o Amin e Unit : Ca t Se c Absorbe r Ga s Flo wRate , Unit s Flo wFactor , SCF D Flo wRate , SCF D Ne t Heatin g Value , BTU/SC F Flo wRate , MMBTU/H R Coke r Se c Absorbe r Ga s Flo wRate , Unit s Flo wFactor , SCF D Flo wRate , SCF D Ne t Heatin g Value , BTU/SC F Flo wRat e MMBTU/H R S.R . Se c Absorbe r Ga s Flo wRate , Unit s Flo wFactor , SCF D Flo wRate , SCF D Ne t Heatin g Value , BTU/SC F Flo wRate , MMBTU/H R Diese l Hydrotreate r Separato r Ga s Flo wRate , Unit s Flo wFactor , SCF D Flo wRate , SCF D Ne t Heatin g Value , BTU/SC F Flo wRate , MMBTU/H R Lean-Amin e t o Absorbe r Flo wRate , Unit s Flo wFactor , BP D Flo wRate , BP D Absorbe r Pressure , PSI G Lea n Amin e t o Absorber , ° F Sour.Ga s t o Absorber , ° F Ric h Amin e Level , Pet . Aci d Ga s t o SRU Flo wRate , Unit s Flo wFactor , SCF D Flo wRate , SCF D Ne t Heatin g Value , BTU/SC F Flo wRate , MMBTU/H R Swee t Ga s t o Fue l Flo wRate , Unit s Flo wFactor , SCF D Flo wRate , SCF D Ne t Heatin g Value , BTU/SC F Flo wRate , MMBTU/H R Amin e Concentratio n = 20. 3 Pet . 5.6 3 743,50 0 4,185,90 5 102 5 1 7 8, 8 6. 6 686,00 0 4,527,60 0 110 6 208. 6 5. 5 1,200* , 00 0 6,600,00 0 60 2 165. 6 1. 5 60,00 0 90,00 0 46 9 1, 8 6. 5 60 0 390 0 15 7 10 8 7 7 6 1 6.7 6 94,70 0 640,17 2 50 0 13. 3 6. 6 2,400,00 0 15,840,00 0 82 2 542. 5P.1 6 

### fit?:.



### TESTIN GEQUIPMEN T - EP A METHO D 7 (NOx ) A Scientifi c Glas s an dInstrument s Compan y NO xSample r wa s use da t th e samplin g location(s ) . Th e NO xsamplin g trai n consiste dbasicall y o f a heate d5 foo t effectiv e lengt h borosilicat e glas s probe ; a 2 lite r borosilicete , roun d bottom , shor t nec k boilin g flas k wit ha Pyre x3-way , T-bor e stopcoc k valve ; a mercur y i nglas s thermometer ; a Dwye r U tub e mercur y

manometer ; a Gas t oil-seale dvacuu m pump ; an d variou s interconnectin g hoses , fitting s an dvalves .
Th e U-tub e manomete r wa s use dt o monito r th e interna l pressure s i nth e collectio nflasks .
SAMPLIN GPROCEDURE S - EP A METHO D 7 (NOx ) A NO xsamplin g trai nwa s prepare da t th e samplin g locatian(s ) i nth e followin g manner : 2 5 milliliter s o f absorbin g solutio nwer e adde dt o a collectio nflask . A sufficien t quantit y

o f th e absorbin g solutio nwa s retaine dfo r late r us e i npreparin g th e calibratio nstandards . A 3-wa y stopcoc k valv e wa s inserte dint o th e collectio nflas k an dth e valv e turne dt o th e "purge " position . Glas s woo l wa s place dint o th e inle t en do f th e heate dsampl e probe . Th e prob e wa s tha n place dint o th e flu e an dconnecte dt o th e collectio nflask . Th e prob e heate r wa s turne do nan dth e prob e heated-t o approxifnate y

25 0 degree s Fahrenheit . A U-tub e mercur y manomete r an da vacuu m pum pwer e connecte dt o th e outle t o f th o collectio nflas k wit ha Teflo nte e fitting . Th e stopcoc k valv e an dth e pum pvalv e wer e the nturne dt o th e "evacuate " positions . Th e collectio nflas k wa s evacuate dt o 3 inche s o f mercur y

absolut e pressur e o r less . A s soo na a th e flas k evacuatio nwa s completed , th o pum pvalv e wa s turne dof f an d th e pum pwa s turne doff . A leak—chec k wa s the nperforme do n th e collectio nflas k b y observin g th e manomete r fo r on e minut e t o determin e i f th e pressur e varie dmor e tha n. 4 inc h 

# V

### | : 

### .<X-;-—. 

### Ui-\JX

o f mercury . I f th e pressur e di dno t var y mor e tha nth e allowabl e tolerance , th e leak-chec k wa s considere d XJ acceptable .

Afte r th e NO xsamplin g trai nwa s assembled , th e prob e temperatur e stabilize dan dth e collectio nflas k leak checked , a s previousl y described , th e nitroge noxide s (NOx ) samplin g wa s performed . J M •- ' . 

### tv - A s soo na s th e leak-chec k wa s completed , th e stopcoc k valv e I " an dth e pum pvalv e wer e turne dt o th e "purge " position s an d |L ; 

### th e pum pturne don . Afte r a nadequat e amoun t o f tim e fo r ;\ M purgin g wa s completed , th e pum pvalv e wa s turne dt o th e of f £ positio nan dth e stopcoc k valv e wa s turne dt o th e evacuet e V position . Th e differenc e i nth e mercur y level s i nth e U tub e manomete r wa s the nrecorded . Immediatel y afte r thi s wa s ^ done , th e stopcoc k valv e wa s turne dt o th e sampl e positio n

fo r approximatel y 1 5 second s permittin g th e flu e ga s t o ente r th e flas k unti l th e pressure s i nth e flas k an dth e sampl e "", ' lin o attaine dequalibrium . V • P.1 7

f ' 

# If e

» 

# ' I

i. 

### On e poin t wa s sample da t th e samplin g location(s ) fro m on e samplin g port . A tota l o f "thr'ee' tes 

### ' c 

### run s wer e performed . Eac htes t ru nconsiste do f fou r 15-secon dsamplin g period s
Th e collectio nflas k an d jT " stopcoc k valv e volume , collectio nflas k temperatur e an d

barometri c pressur e we r e recorde do na fiel dtes t for m prior t o eac h15-secon dsamplin g period . Afte r th e completio no f eac h15-secon dsamplin g period , th e followin g procedure s wer e performed : Th e stopcoc k valv e wa s |, : 

### turne dt o th e "purge " positio nan dth e collectio nflas k wan s 

## I f' " 1 r 

### . ' disconnecte dfro m th e samplin g probe , U-tub e manomete r an d £;" . vacuu m pump . Th o samplin g prob e wa s lef t i nth e flu e wit h |p' - th e prob e heate r o nan dread y fo r th e nex t samplin g period , i " Th e flas k wa s the nshake nb y han dfo r a minimu m o f 5 minutes . 

## I4> : 

## • •
I I c • •P.1 8

fK *~ * ll-.'-,


# m:x Th e collectio nflas k wa s transferre dt o a protectiv e

transpor t cas e an dallowe dt o se t fo r a minimu m o f 1 6 hour s t o stabize . A t th e en do f th e 16-hou r stabilizatio nperiod , th e content s o f th e flas k wer e shake nb y han dfo r 2 minutes . Th e flas k wa s the nconnecte dt o a nU-tub e manomete r an dth e pressur e differentia l recorded . Th e flas k temperatur e an d th e barometri c pressurr e wer e als o recorde da t thi s time . Th e content s o f th e flas k wer e transferre dt o a leak-fre e polypropylen e sampl e bottle . Th e flas k wa s rinse dtwic e wit h 5 millilite r quantie s o f deionized , distille dwate r an dth e rinsing s adde dt o th e content s i nth e sam e bottle . Sodiu m hydroxid e (1N ) wa s adde dt o th e sample , dropwise , t o adjus t th e p H betwee nS an d1 2 a s determine db y a p H meter . Th e sampl e bottl e wa s sealed , appropriatel y lable dan dth e flui d leve l marked . Th e bottl e wa s the ntransporte dt o th e laboratory .

lir . 

## IK V &



# rnaj.i /

# ^•< w jfK*.-r-irtKJWT U 

## T^r ; •*'..'VV.). ;

FLU E WAL L

-^• " Vl l 

### PYRE X WOO L PLU G STOPCOC K © PURG E © EVACUAT E © SAMPL E

PROB E

200 0 m l FLAS K 

# rt^ a THERMOMETE R 

# (? \ ^ SHUTOF F VALV E

VACUU M PUM P

MERCURY-FILLE D MANOMETE R 

# m Exhibi t NITROGE N OXID E SAMPLIN G TRAI NP.2 0



## SUMMAR Y O F TES T RESULT S Th e followin g table s presen t th e fina l result s o f th e NO x emission s test s an d th e H2 S test s performe d o n Octobe r 1 7 an d 18 , 1984 a t NCRA' s McPhearson , Kansa s refinery. .

TABL E I . NO x RESULT S



## Ru n No . 1 2 3 AVG . Locatio n

HF-009 A Dat e

10-17-8 4 PP M

11 5 13 0 10 9 11 8 lbs/MMBt u

• • 

### .13 5 .15 5 .12 8

. 13 9



## 1 2 3 AVG . HF-009 B •= • 10-17-8 4 13 2 14 7 13 2 13 7 • .15 5



### ' . \ . 17 5 

### .15 8 .16 3

1 2 3 AVG . . HP-01 2 10-18-8 4 5 5 5 1 6 1 5 6 .06 5

.06 3 .07 3 .06 7P.2 1 

### ^xy^y

>.••'•.'•?•••' ; 

# Sr:

«;-M- / 

### TOTA L SOURC E ANALYSI S NO X TES TRESULT S

K"..-:-j,-rfr. -.. 

# i^T V ^^ : • , *•/ & •-:...- . '.t;-*'-. - '- ' •**'. ' 

### ICRA^".-.

- fT^'^> 5 

### --i ? 

### -"-'
- 

## ICPHEARSON , KANSA S •i-S-ViTSi " 

## 14-05 0 - JF-009 A
• *»*«Jr-«..!-
- ~ - **t^?r*^ ~ .•* . 

## lUN - 

## : NUMBE R i&rir.--r-r • ' . • 

### "LAS KNUMBER /OLUM E O F FLAS K [NITIA L TEMPERATUR E

r 

### INAL' : TEMPERATUR E '•&££•?%. . •

••. 

### INITIA L PRESSUR E .•£X7.
. .-:.'
. .W

. 7 

### "INA L PRESSUR E VOLUM E SAMPLE D MO'xIi'lN" : SAMPL E NO X CONCENTRATIO N PAnfs.-PE R MILLIO N I tX&gAiy.., 

## FACTO R 

# £?•? ' •' • PERCEN T 0 2 OX^EMISSION S ML S OEG . F DEG . F I NH G I NH G OSC C MICR O G LBS/DSC F PP M 0SCF/MM8T U % 

## LBS/MBT U 1- A

2 7 203 4 4 2 6 6 1. 3 27. 7 177 4 34 1 1.2E-0 5 10 0 833 5 3 0.1 2 1- B

1 0 198 5 4 2 6 4 1. 4 27. 7 173 1 37 5 1.4E-0 5

.. _11 7 

## 833 5 3 0.1 4 1- C

2 204 3 4 2 5 8 1. 3 28. 6 187 3 40 6 1.4E-0 5 11 7
_ 833 5 3 0.1 4 1- D

1 2 195 0 4 0 5 6 0. 9 26. 6 168 9 41 3 1.5E-0 5 12 6 833 5 2. 8 0.1 4P.2 2

JatTH0»/l"l^-»irmiMI»ATIOJ 3 © p MT \JSt. erjLFist j CO:»TEM

T o p nna . ©A

O STREAMS S

W * S . Principl e an d eppfica&tfify . a. 1 ^Yirart - ?Ie . Kydrose n sulfid e (HcS ) I s collecte d fro m asourc e i naserie s o f

midge tImpinger s an d absorbe d I

np K3. 0 cadmiu m sulfat e iCdSO. t solutio nt o for m cadmiu m sulfid e (ICdS) . Th e latte rcompoun d I s the nmeasure d iod o we'.rlcslly . A n impinge reonl&inln s hydro* se n peroxid e Is Include d t o remov e SO» a s . a ninlerferin s spiles . Thi s shetho d Is & revisio no f th e Kj S metho d originall y publishe d i n th e FEDERAL RSCISTER . Volum e 39 . No . 47 „ date d Friday . Marc h 8.197<S . 1. 2 JlppIicabiMy . Thi s metho d i s applica bl e fo rthe . determinatio n o f th e hydrogen sulfid e conten tc f

fue l ga s stream s a tpetro leu m refineries . %. Ranye end

sensitivity. Th e SowerSlmlt o f detectio nIs approximatel y 3 ms/m " < 9 ppm) . Th e maximu m o f th e rang e i s "34

0 xng/m " (52 0 ppm) . S . interferences. An y compoun d tha tre duce s Iodin e o roxidize s Iodid e lo nwil l inter fer e L n thi s procedure , provide - I tI s collecte d i nth e cadmiu m sulfat e impingers . Sulfu r dioxid e I nconcentration s o f

u p t o 2.60 0 tns/ m" I s eliminate d b y th e hydroge nperoxid e solution . Thiol s precipitat e wit h hydroge n sulfide . I nth e absenc e of H3 . onl y co-'trace s o f thiol s ar e collected . Whe nmethane - ar d ethane-thlol s a tatota l leve l o f 30 0 ms/m ° ar e presen tI

n additio nt o H.S . th e result s •vtmry tram 2 percen tlo wa ta nK3 . conce'n tratio n o f

40 0 mg/m ' t o 1 4 percen thig h a t a nH. S concentratio no f 10 0 mg/m \Carbo n oxysulfid s &*

» aconcentratio nof

2 0 percen t doe s no tinterfere . Certai ncarbonyl-con talnin g compound s reac twit h iodin e an d produc e recurrin gen d points . However , ac etaldehyd e an d aceton e a tconcentration s o f J an d 3 percent , respectively , d o no l inter fere . Entrains d hydroge nperoxid e produce s a negativ e interferenc e equivalen tt o 100 per cen tof tha to f a nequimola rquantit y o l hy droge nsulfide . Avoi d th e ejectio no f hydro se n peroxid e Int o th e cadmiu m sulfat e im pingers . 4 . Preciyto n en d accuracy. Collaborativ e testin gha s shew n th e wlthln-laborator y co efficien to f

variatio nt o b e 2. 2 percen tan d •ih e overal l coefficien tof variatio nt o b e 5 percent . Th e metho d bia s wa s show nl o b e —4. 6 percen twhe nonl y H, S wa s present . I n " th e presenc e o f

th e Interference s cite d I n sectio n3 . th e bia s wa s positiv e a tlo wH, S concentrations - an d negativ e a thighe rcon centrations . A t23 0 m gH,S/ra \th e leve l o f th e complianc e standard , th e bia s wa s 4-2. 7 percent . Thiol s ha d n o effec to n th e preci sion . H. Apparatus. B. l Samplin g apparatus . 8.1. 1 Samplin gline . Si xt o 7 m m (V « in. ) Teflon ' tublp. 2 t o connec tth e samplin g trai nt o th e samplln ? valve . 8.1. 2 Impingers . Fiv e mldse timpingers . eac h wit h 3 0 m l capacity . Th e Interna l di amete ro f

th e Impinge rti p raustb e 1 m m a. 0.0 5 mm. " Th * Impinge rti p mus tb e poel -

- tlone d 4 t o 6 m m fro m th e botto m o f th e impinger . 8.1. 3 Clas s o rTeflo nconnectln s tubin g

. £orth e Implnaers . 8.1. 4 Ic e bat h container . T o maintai nab sorbin g solutio na talo wtemperature . 8.1. 5 Dryin gtube . Tub e packe d wit h 8 - t o 16-mes h Indleatlng-typ e silic agel . o requiv alent , t o dry th e sa s sampl e Bn d protec tth e mete rtn d pump . If

th e silic aBe

l ha s bee n use d previously , dr y e tl°li'C'(350 ' F > fo r2 hours . Ji'e

weillc age l ma y b e use d a s re ceived . Alternatively , othe rtype s o f des'.c cant j (equlvn)en to rbetter ) ma y b s used , subjec tt o approva l o f

th e Administrator . NOTE.—D o no tus e more tha n3 0 go f aluc o Sel . Silic ase l absorb s gase s suc h a s propan e trom th e fue l sa s stream ; an d us e of exces siv e amount s o f

eillc age l coul d resulti n error s i n th e determinationo f sampl e volume . 3.1. 6 Samplin gvalve . Keedl e valv e o r equivalen tt o odjus tsa s Ho wrate. Stainles s Otee l o rothe rcorrosion-resistan tmaterial . 9.1. 7 Volum e meter . Dr y sa s meter , suffi cientl y accurat e t o measur e th e sampl e volum e withi n2 percent , calibrate d a tth e selecte d flo wrat e c—1. 0 Ut^r/mln ) an d con dition s sctu&ll y encountere d durin gs&mpllns . Th e mete rshal l b e equippe d wit h a temperatur e gaug e Wis J thermomete ro r equivalent ) capabl e of measurin gtempera tur e t o withi n3 ' C «.B * F) . Th e sa s mete r ohoul d hav e o petcock . o requivalent , o nfh e cutle tconnecto rwhic h cu tb e close d durin g th e lea kcheck . Ga s volum e fo ron e revolu tio nof th e mete rmus tno tb e mor e tha n1 0 liters . S. U Flo wmeter . Rotamete ro requiv alent , t o measur e flo wrale s i n th e rang e fro m 0. 5 t o 2 llters/ml n( 1 t o « cfh) . 2.1. 9 Graduate d cylinder . 25 m l size .
. 5.1.1 0 Barometer . Mercury , aneroid , o r othe rbaromete rcapabl e of measurin gat mospheri cpressur e t o withi n2. 5 mm K g (0. 1 in . Hg) . I n man y cases , th e barometri c readin gmay b e obtaine d from anearb y Na tiona l Weathe rServic e station , l n whic h case , th e statio nvalu e (whic h i s th e abso lut e baromttrl cpressure ) shal l b e requeste d an d a nadjustmen tfo relevatio ndifference s betwee nth e weathe rstatio nan d th e sam plin gpoin tshal l b e applie d a tarat e o l minu s 2. 5 mm H g(0. 1 in . Hg ) pe r3 0 m (IC O ft ) elevatio nIncreas e o rvice-vers afo releva - • tio ndecrease . 8.1.1 1 U-tub e manometer..C-3 0 c m wate ; column . Fo rlea kChec

kprocedure . 5.1.1 2 Rubbe rsqueez e bulb . T o pressur- - !z e trai nfo rlea kcheck . 5.1.1 3 Tee . plnchclamp . en d connectin g. tubing . Fc rleakcheck . 5.1.1 4 Pump . Diaphrag m pump , o requiv alent . Inser ts

i emai l surg e tankbetwee nth r pum p an d rat e mete rt o eliminat e th e pulsa tio neffec tof

th e diaphrag m pum p o nth e rotameter . Th e pum p I s use d fo rth e ai r purg e a tth e en d o f

th e sampl e run : tli c pum p i s no tordinaril y use d durin gsam pling , becaus e fue l sa s stream s are usuall y sufficientl y pressurize d t o forc e sampl e ga s throug h th e trai na tth e require d flo wrale . Th e pum p nee d ne tb e Jeak-free unles s l tI s use d fo rsampling . 5.1.1 5 Needl e valv e c

j critica l oil'lce . T o Be tai rpurg e flo wt o I llter/mln . B.l.1 6 Tub e packe d with activ e carbon . T o filte rai rdurin gpurse . 6.1.1 7 Volumetri cflask . On e 1.000 ml . 8.1.1 B Volumetri cpipette . On e 15 ml . 6.1.1 9 Pressure-reductio nregulator . De pendin go nth e samplin gstrea m pressure , a pressure-rtdactio nregulato rma y b e ne?d?( < t o reduc e th e pressur e o f th e ga s strea m en terin gth e Teflo nsampl e lin e t o asaf e level . 8.1.2 0 Col d trap . X

f condense d wale ro r amin e l s presen ti n th e sampl e stream , e corrosion-resistan tcol d trap ehal l b e use d immediatel y afte rth e sampl e tap . Th e tra p ahal l no tb e operate d belo w0 ' C (32 * F ) lo avol d condensatio no f C , o rC . hydrocar bons . 6. 2 Sampl e recovery . 8.2. 1 Sampl e container . Iodin e flask , glass-stoppered : 500m l size . 6.2. 2 Pipette . 5 0 m l volumetri ctype . 8.2. 3 Graduate d cylinders . On e eac h 2 5 an d 25 0 ml . •Mentio nof

trad e name s o l specifi cprod uct s doe s no l constitut e endorsemen tb y th e Environmenta l Protectio nAgency . 8.2. 4 Flasks . 12 5 ml . Erlenmeyer . B.2 £ Was h bottle . 8.2. 3 Volumetri cflasks . Thre e 1.000 lin L 8. 3 Analysis . 8.3. 1 Flask . 500 ml glass-stoppere d lodi n flask . 8.3. 2 Burette . 80 ml . 8.3. 3 Flaak . 12

5 ml . Erlenmeyer . B.3.4 Pipettes , volumetric . On e 25 ml : Iw i eac h 5 0 an d 100 ml . . : 8.3. 5 Volumetri cflasks . On e 1.000 m ' tw o 50 0 m t*

- 8.3. 6 Graduate d cylinder's . One eac h 1 an d 100 ml . 0 . HcogenU. Unles s otherwis e indicated . I fe intende d th» tai rreagent s conform t o t h specification s establishe d b y Ih e Commut e o nAnalytica l Reagent s o f fh e America : Chemica l Society , wher e suc h specificatio n ar e available . Otherwise , us e bes tsvallab ! grade . B. l Sampling . 0X 1 Cadmium sulfat e absorbin gso k tion . Dissolv e 4 1 s of

3CdSO . BH.

O an d 1 m l o f 0. 1 M sulfuri cacid I

naI -lite rvolume ) rl cflas ktha tcontains approximatel y * « Ht c o f deionize d distille d water . Dilut e t volum e with deionize d water . iAitt thoroug l Dy . p H shoul d b e 3-0.1 . Ad d 10 drop s c Dow-Cpmlp. gAntifoam B . Shak e well befo r use . If Antifoam B I

s no l us?'d . lh e alterna t acidifie d iodin e extractio nprocedur e (f-c t tio n7.2.2 ) mus tb e used . 6.1. 2 Hydroge nperoxide . 3 ptrccn' . Dilut e 3 0 percen thydroge npfroxid tt o percen tas needed . Prepare fres h dally . 6.1. 3 Waler . Deionized . distille d t o M U Jor m t o AST M specification s D l 193-7 : Typ e 3 . A l th e nptian o f th e analyst , t h KMnO . tes tfo rnxidizabl e organi cmalt : ma y b e omitte d whe nhig h concentratio n o f organi cmatte rarcno texpecte d l o !• • present e rSampl e recovery . 8.2. 1 Hydrochlori cacid solutio n(HC I 3M . Add 240 ml o

f concentrate d HC

I (M>ec i l cgravity 1.19 ) t o 5C

0 m l of deionized . d

i tille d wale rf

n a1-liicrvolumetri cfl*s' ' Dilut e t o 1 lite rwith deionize d water . M i thoroughly . 0.2. 2 Iodin e solutio n0. 1 K . Dissolv e 2 4 o f potassiu m Iodide (Kl ) I n:< 0 m l of dcloi ized , distille d waler . Ad d 12. 7 ro

f resul

- lime d Iodin e (I. ) t o th e potassiu m lodid t.«. < ltillon . Shak e th e mixtur e unti l th e Iciiiit e ' completel y dissolved . I

f possible , le tlh e K lutlo nalan d overnigh tI n lh e dark. Slow: ! dilut e fo e solutio nt o 1 lite rwit h deloniz ^ distille d water , with swlriinfr . Fille rth e u lu'.lo ni ! J

l I s cloudy . Stor e solutio ni n brcwn-glas s reagen tbottle . 6.2. 3 Standar d Iodine solution . 0.0 1 N . P pett e 109. 0 ml o f

th e 0. 1 N Iodine Kilutl o int o a41lle rvolumetri cflas kand dilut e t volum e with deionized . distille d waler . SU M dardlz e dail y a s I

nsectio n8.1.1 . Th b sol t Uo nmus tb e protecte d from light . Reftgs r fcottles tn d flask s mus l b tkcp l tigh'.l y Mo ; pcred . S. S Analysis . C.3. 1 Sodiu m thlosul/nt e r.olu'.lon, Bta , dar d 0. 1 )« . Dissolv e 24. 8 fto f .sodium thi ' BUlfnt e pentahydrat e (fta,SiO>-5H,0 > ori s 3 o f anhydrou s sodium thiosulfat e (Na& O i n1 lite ro

f deionized , distille d wale rfci ad d 0.0 1 t

ro f cnhydroi u .<odlu

m caihrma ' (Ka,CO. ) an d 0.

< m l o f chloroform (CHCi t o stabilize . Mi xthoroughl y b y shsklns ti b y aeratin gwit h nitroge nlo rnplwoxlniatel 1 5 minute s en d stor e I nu ^lass-stoppcri : reagen tbo'.llc . Standardiz e fcs I n M\-.ll c 0.1.2 . 8.3. 2 Sodiu m thiosulfate . solution , sta : dar d 0.0 1 N . Plpeli e 50. 0 in) o f th e stundai 0. 1 N thiosulfat e solutio nInt o avolumetr flas kan d dilut e t o SO O ml wit h div.l'. h water . 

# III-Appendi x A-4 1

# I

Norr.—A 0.0 1 N phenylatsln e oxid e solu - tio nma y b e prepare d instea d o f 0.0 1 N thio sulftt e (se e sectio n6.3.3) . • . • 6.3. 3 Phenylarsln e oxid e solution , stan dar d 0.0 1 N . Dissolv e 1.8 0 to f phenylarsln e oxid e (C.H.AsD > i n15 0 m l o f 0. 3 N sodiu m hydroxide . Afte rsettling , decan t14 0 m l o f thi s solutio nint o C0

0 m l o f distille d water . Brin gth e solutio nt o p H S- 7 wit h 6N hydro chlori caci d an d dilut e t o 1 liter . Standard U e a s l nsectio n8.1.3 . 6.3. 4 Starc h indicato rsolution . Suspen d ' 1 0 go f solubl e starc h I n 10 0 m l o f deionized . distille d wate ran d ad d I S go f potassiu m hydroxid e (KOH ) pellets . Sti runti l dis solved , dilut e wit h 90 0 m l o f deionize d dis tille d wale ran d le tsland'fo r1 hour , neu traliz e th e alkal i wit h concentrate d hydro chlori cacid , visin ga nindicato rpape rsimila r t o Alk&cid tes l ribbon , the nad d 2 m l of gla t a l aceti caci d a s apreservative . Nore—Tes tstarc h indicato rsolutio nfo r decompositio nby.titrating , wit h 0.0 1 N iodin e solution . 4 m l o f starc h solutio ni n 20 0 m l o f

distille d wate rtha tcontain s 1 E . potassiu m iodide . I f

mor e tha n4 drop s o f

- th e 0.0 1 N Iodin e solutio nar e require d t o obtai nth e blu e color , afres h solutio nmus t t e prepared . 7 . procedure . 7. 1 Sampling . 7.1. 1 Assembl e th e samplin gtrai na s thow n i nfigur e 11-1 , connectin gth e fiv e midg- timpinger * l nseries . Plac e 1 5 m l o f 3 percen thydroge nperoxid e solutio ni n th e fiw timpinger . Leav e th e secon d impinge r empty . Plac e 1 5 m l o

f th e cadmiu m sulfat e absorbin gsolutio nl nth e third , fourth , an d fift h impingers . Plac e th e Impinge rassem bl y i na nic e bat h containe ran d plac e crushe d 1c

e aroun d th e lmplngen . Ad d mor e Ic e durin gth ? run . if

needed . 7.1. 2 Connec tth e rubbe rbul b an d mano mete rt o fir= tImpinger . a s show nl nfigur e 11-1 . Clos e th e petcoc ko nth e dr y ga s mete r cutlet . Pressuriz e th e trai nt o 25-cm wate r pressur e wit h th e bul b an d clos e of f tubin g connecte d t o rubbe rbulb . Th e trai nmus t hol d a25-c m wate rpressur e wit h no tmor e tha na1-c

m dro p l npressur e i na1-minute interval . Stopcoc kgreas e I s acceptabl e fo r sealin ggroun d clas s Joints . . . Nore—Thi s lea kchee kprocedur e l s op tiona l a tth e beginnin go f th e sampl e run . bu ti s mandator y a l th e conclusion . Not e fclso tha tI

f th e pum p I

s use d fo rcampling , i t U recommende d (bu tno trequired ) tha tth e pum p b e lez.k-cheek; d separately , usin ga *«?tho d consisten twit h th e leak-chec kpro cedur e fo rdiaphrag m pump s outline d I n sectio n4.1. 2 o f

referenc e metho d 6 . 4 0 CF R Par t60 . Appen.dlxA . * 7.1. 3 Purg e th e connectin glin e betwee n th e camplin gvalv e an d firs timpinger . b y disconnectin g th e 11n s fro m th e firs tIm pinger . openin gth e samplin g valve , an d al lowin gprocess ga s t o flo wIhroujt b th e lin e fo raminut e o rtwo . Then , clos e th e sam plin g valv e an d reconnec tth e Un e t o th e implr.ye rtrain . Ope nth e petcoc kc n th * dr y pa s mete routlet . Recor d th e initia l dry ga s mete rreading . 7.1. 4 Ope nth e samplin gvalv e an d the n adjus tth e valv e t o obtai naral e o f approxi matel y 1 llter/mln . Maintai naconstan t .(±1 0 percent ) flowrat e durin gth e test . • Recor d th e mete rtemperature . 7.1. 5 Sampl e fo ra tleas t1 0 min . A tth e en d o f th e samplin gtime , clos e th e sam plin gvalv e an d recor d th e fina l volum e an d temperatur e readings . Conduc talea kchec k a s describe d i nSectio n7.1. 2 above . • 7.1. 6 Disconnec tth timpinge rtrai niro m th e samplin gline . Connec tth e charcoa l tub e an d th e pump , a s show nW figur e 11-1 . 

# c P.2 3
urg e th e trai n(a l arat e o f 1 ilter/mln ) wit h clea nambien tai rfpr1 5 minute s t o ensur e tha tal l H. S i s removed from th e hy- ' dxoge nperoxide . Fo rsampl e recovery , ca p th e ope nend s an d remove th e Impinge r trai nt o aclea nare atha tI s awa y from source s o f

heat . Th e are ashoul d b e wel l lighted , bu tno texpose d t o direc tsunlight . 7. 2 Sampl e recovery . 7.2. 1 Discar d th e content s of th e hydro ge nperoxid e Impinger . Carefull y rins e th e content s o f

th e third , fourth , an d fift h im pinger s Int o a500 m

l Iodine flask .



## Cr\ * VALV

l ' l,N I^'" I4»«<CIR S SIUC A Cl l TU3 1


# ted 

# D= ^

HyJ«5* » 

# f«*Jc\ ' == 

# & ==

# n Cr 

# **^ c S u 

## \ 

## So

p« rCA S MI Ttf t

~»u» > (roRAiarvaci i Flgur* lM.'H2$«>mf>lin}1r»in .



# .Ill-Appendi x A- 4 2P.2 4



# C 

# c
Korx—Th * Implnjsr anormall y hav * onlj r & thi n fil m o f

csdmlu m eulfld * remaining ' 'tSiot awate rrlris* . It

Antifoa m D w u no t \-3-A c rU

•Ijn'.flsan tcuantltle * o l yallo w cadmiu m eulttd * remai nI nth * Implnjers , th atlt*m»t * r«ov»r y procedur e dewribe d bslo wmus tb » u»*d , 7.3. 3 PIpst u exactl y D O m l o f 0.0 1 N lodln * solutio nInt o a123 m l £rl»nm»y» r flask . Ad d 1 0 m l of

3 M H Q t o th tsolution . Quantitativel y rlns * th » acldtflsd " lodln * Int o th > ledin * flask . Ciopp» rth * fl»5» Im mediatel y an d ahak * briefly . 7.3. 3 (Alternstv) . Extrac tth » remslnln ? cadmiu m sulfId tfro m th * third , fourth , an d fift h Jmprns»r

» usin gth » tcldlfls d Isdln * so lution . Immadistal y A

f u rpourbij th tacidi fie d lodln * Int o a nIraplnjsr , otoppt rItfend ihak s fo rftfs wmoments , tha ntrarufa rth * liqui d t o th * lodln * fluU. D o no ttrtctsto r an y rlrj » portio nfro m on * Irr.plnje rt o an othar , transls rItdirectl y t o th * lodln * flask . Or.c s th e acidifie d lodln * solutio nh wbee n poure d int o an y glasswar e containin g cadmi u m sulfide , th e containe rmus tb e tightl y stoppere d a tal l time s excep twhe naddin g mor e solution , an d thi s mus tb e don * a s culckl y an d carefull y a s possible . Afte r addin gan y acidifie d iodin e solutio nt o th e iodin e flask , allo wafe wminute s fo rabsorp tio no f th e Hi S befor e addin g an y furthe r rinses . P.epea tth e Iodin e extractio nunti l al l cadmiu m sulfid e l s remove d fro m th e Im pingers . Extrac ttha tpar to f th e connectin g classwar e tha tcontain s visibl e cadmiu m sul fide . Quantitativel y rins e al l o f th tIodin e fro m th e Impinger* . connectors , tn d th e beake r Int o th e Iodin e flaakualn gde!onl:ed , dis tille d water . Stoppe rth s flaakan d shak e briefly . 7.2.3 " Allo wth e Iodin e flas kt o stan d abou t3 0 minute s i n th e dar kfo rabsorptio n o f th e Ht S int o th e iodine , the ncomplet e th e titratio nanalysi s a s l nsectio n7.3 . •Kerr.—Cautlor. l Iodin e evaporate s fro m acidifie d Iodin e solutions . Sample s t o whic h acidifie d Iodin e hav e bee nadde d ma y no tb e stored , bu tmus tb e analyze d i nth e Um e schedul e state d i n sectio n7.2.3 . 7.2. 4 Prepar e ablan kb y tddln j 4 5 m l o f cadmiu m sulfat e absorbin gsolutio nt o e n iodin e fiask . Pipett e exactl y iO ml o f 0.0 1 N iodin e solutio nint o » 125m l Erlenmeye r flask . Ad d 1 0 m l o f

3 M HCl . Follo wth e sam e lntplnge rextractin g an d quantitativ e rinsin gprocedur e carrie d ou ti nsampl e analysis . Stoppe rth e flask , shak e briefly , le tstan d 3 0 minute s I

n th e dark , an d titrat e wit h tb e samples . Koss.—Th e blan kmus tb e handle d b y ex actl y th e sam e procedur e a s tha tuse d fo r th e samples . 7 - . Analysis . Nors.—Titratio n analysi s shoul d b e con ducte d a tth e sample-cleanu p are aI norde r t o preven tlos s o f

Iodin e fro m th e sample . Titratio nshoul d neve rb e mad e In direc t sunlls'nt . 7.3. 1 Usin g0.0 1 N sodiu m thiosulfat e so lutio n(o r0.0 1 N phtnylarsln e oxide , lf ap plicable) , rapidl y titrat e eac h sampl e I na n iodin e fiaskusin ggentl e mixing , unti l solu tio ni s ligh tyellow . Ad d 4 m l o f starc h indi cato rtolutlo nan d continu e titratin gslowl y unti l th e blu * colo rJus tdisappears . Recor d Vr, . th e \olum e o f

sodiu m thiosulfat e solu tio nused , o rV AT. th e volum e of

phenylar sln e oxid e solutio nuse d (ml) . 7.3. 2 "Titrate th e blank s I n th e sam e xazmera s th e eamples . Ru nblank s eac h da y unti l repllcat * vslus s 63ro * withi nO.O S tnl . Aver&a* th * repllest * titratio nvaluo * whic h agr* * withi n0.05 ml . 0 . Calibration end

itanicrdi. 8. 1 etandwdliatlons , B.l. l Btandsrdlz * th * 0.0 1 tf lodln * solu tio ndall y u follows : Plptlt tS s n l o f th > lodln * solutio nInt o ftIS ) m l Erlswr.oys r fluk . Ad d 3 m l e f

I M HC U Tltri*. * rapidl y wit h standar d 0.0 1 N thlcjulfat * solutio no r wit h 0.0 1 N ph*ny!a»ln » oxld * unti l th * to lutlo nI s ll;h tyellow , u>lc ; contl * mixing . Ad d fou rdrop s o f

starc h indlci'.o rsolutio n an d contlnu * tltratln

j slowl y unti l th * blu e colo rJus td!i»pp»m . Recor d V f th * volum * o f thbiulfst * tolutlo nussd . c rV*J . th * volum * o f

phonylwaln * oxld * tolutlo nuis d (ml) , RepsV . unti l ropllci U volus i asr» » withi n0.0 5 ml . AVSMJ * th * rsplleat * tltra tio nvalue * whic h tgre * withi n0.0 1 m l and calculat * th * caae tnormality o f th * lodln * solutio nusin gequatio n0.3 . Repas ttb * standardizatio ndally . 6.1. 3 Standardis e th e 0. 1 Kthlosulfst * solutio na s follow * Oven-dr y potassiu m dl - .chromat e (K.Cr.O. ) a t18 0 t o 200 ' C (38 0 t o 890 " F). Weig h t o th s neares tnllll-rrsm , 3 y of potassiu m dichrcmate . Transfe rth o di chromat e t o aC0

0 m l volumetri cflask , dis solv e i ndeionised , distille d wste ran d dilut e t o exactl y BO

O ml . I na60

0 m l lodln s flask , dissolv e approximatel y 3 go f potassiu m Iodid e (KI ) l n4 5 .ml o f deloniied . distille d water , the nadd 1 0 m l o f 3 M hydrochlori c aci d solution . Pipett e t o m l o f th * dichro mat e solutio nint o thi s mixture . Gentl y swirl th e solutio nonc e and allo wi tt o stan d l nth e dar

kfo r5 minutes . Dilut e th e solu tio nwit h 100 t o 20 0 m l of delor.Ized distille d ' waler . washin gdow nth e side s of th e flas k wit h par tof

th e wster . Titrat e wit h 0. 1 N thiosulfat e unti l th e solutio ni s l.'jh tyellow . Add 4 m l of

starc h indicato ran d continu e ti tratin gslowl y t o acree nen d point . Recor d ' V| . th e volum e o f

thlosuirat e solutio n UJt d (ml) . Repea tunti l replicat e analyst s agre e withi n0.0 5 ml . Calculat e th e normalit y usin gequatio n0.1 . Repea tth e standardiza tio neac h week , o rafte reac h tes tterles , * whicheve rtim e i s shorter . 8.1. 3 Standardiz e th s 0.0 1 N Phenylar sln e oxid e (I

f applicable ) a s follows : ove n dry potaaslu m dichromat e (K.Cr.O, ) a t180 t o 200 " C (36 0 t o 350 * F) . Weig h t o th e near es tmilligram , 2 g o

f th e K.Cr.O, ; transfe r th e dichromat e t o a50 0 m l volumetri cflask , dissolv e i ndelonhed , distille d water , and dilut e t o exactl y 50 0 ml . I na50 0 ml iodin e flask , dissolv e approximatel y 0. 3 co f potas siu m Iodid e (XI ) I n4 5 m l o f deionized . dis tille d water , add 1 0 m

l c f 3 M hydrochlori c acid . Pipett e 5 m l of

th e K,Ci.O , solutio n Int o th e Iodine flask . Gentl y swirl th e con- , tent s o f th e flas konc e and allo wl o stan d I n th e darkfo rC minutes . Dilut e th tsolutio n wit h 10 9 t o 20 0 m l o f deionised . distille d water , washin gdow nth e tide s of th e flas k wit h par tof

th e water . Titrat e -wit h 0.0 1 N phenylarsln e oxid e unti l th s solutio ni s ligh tyellow . Add 4 m l o f starc h Indicato r an d continu e titratin gslowl y t o agree nen d point . Recor d V A. th e volum e o f

phenylar sln e oxid e used (ml) . Repea tunti l replicat e analyse s agre e withi n0.05 ml . Calculat e th e normalit y usin gequatio nS.2 . Repea tth e standardizationeac h weeko rafte reac h tes l series , whicheve rtim e i s shorter . C. 2 Samplin gtrai ncalibration . Calibrat e th e samplin gtrai nccmpone.it s a s follows : 8.2. 1 Dry ga s meter . 8.2.1. 1 Initia l calibration . Th e dr y gai t mete rshal l b e calibrate d befor e it s initia l us e l nth e field . Procee d a s follows : First , as stmbl * th * followin g component s I nsarles : Drylnj tub* , needl e valv* . pump , roUir.tler , tn d dr y gu . miter . Than , le&k-choc kth e tyste m u followi : Plac e avacuu m gsug s (a t lsss t76 0 m m Hj ) a tth o Inlo tt o th o drylny tub * tn d pul l e vscuum of 35 0 mm (1 0 In. l He, plu s o rpinc h of

f th s outle to

f th e flow m*t«.* , an d tha nturnof f lh e pump . Th e vscuu m (hal l romsl n ttabl s fo ra tItu* . 3 0 second) . Carefull y relsas * th s vacuum taug e befor e releasin gth e flo wmotorend . H*»t , eelibra U th * dry S M mete ru tth e •ampltn j flo wret * ipeclflo d by th e method ) t s follows : Connec ta

nappropriatel y site d we ttes tmete r(e.g. , 1 lite rps rrevolution ) t o th * Inle tc f

th * dryingtube . Msk e thre i in dependen tcnllbrstlo nrum , usin gA thu l fiv * revolutions o

f th o dr y su mete rpa

r run . Calculat * th e c&llbrallon factor . y<w; i tes tmete rcalibratio nvolum e divided b y th e dr y ci s mete rvolume , both volume s adjuit c d t o th e sam e reference temperatur e sn d pre»»uro) . fo reac h run , and aversg e th e re sults . I f an y y valu e deviate s b y more tha n1 percen tfro m th e sveraje . th e dry gas mete r l s unacceptabl e fo rus: . Otherwise , us e th e avere? s a s th e cslibratio nfacto rfo reubsrquen ttes truns . 8.2.1. 2 Post-tes tcalibratio ncheck . After eac h fl'-ld Les

tseries , conduc tacalibratio n chec ka s J

naecllo n8.2.1.1 . above , excep tfor th e followin gvariations : (a ) Th e lea kch« V i s no l t o b s conducted , (b ) thre e o rmor e revolution s o f

th e dry sa s mete rma y b t used , an d (3 ) onl y tw o Independen tiu m nee d b e made . I f

th e calibratio nfacto rdot i no tdeviat e b y more tha n5 percen tfro m th e JnltUI calibratio nfacto r(determine d I n sectio n8.2.1.1.) , the nth e dr y ca s mete rvol ume s obtaine d duringlh e les tserie s er e >tceptible . l f

th e calibratio nfacto rdeviate s b y enor s tha n8 percent , recalibrate th e dr y ca s mete ra s In

' sectio n8.2.1.1 , en d fo rth : calculations , us e th e c&llbratlon facto r(Initia l o rrecalibration ) tha tyield s th e lower en s volum e fo reic h tes trun . 8.2. 2 Thermometers . Calibrate apalrj t mercury-ln-slas * thermometers . 8.2. 3 Rotameter . Th e rotamete rr.ecd no t b e calibrated , bu tshoul d b e denne d sn d maintaine d accordin gto th e munufactuitr' * Instruction . 8.2. 4 Barometer . Calibrat e agains taInsrcur y barometer . 0 . Ccleufofionj . Carr

y ou l calculation s retainin gn l leas ton e exl m decimal figurebeyon d tha tof

th e acquired dat aRoun d of f result s onl y afte rth e fln M calculation . P. l Normalit y cf

th e Standar d (-0. 1 K ) Thiosulfat e Solution .

N,»2.033W/V , where : Vr-Weigh tof

K,Cr,0 , used , vV,-Volum e o f

Na£,0 , solutio nused . ml . Kj-Normallty.o f

standard thiosulfat e solu tion , e-eq/llter . 2X39-Conversio nfacto r ( 8 eq . I./nol e K.Cr,0, ) (1.00 0 ml/lllcr)/ - (204. 2 gX.Cr.O,Amo!e ) (1 0 aliquo tfector ) 0. 2 Normalit y of

Standard I'henylarstne . Oxid e Solutio n(Inapplicable) .

H 4 -0.20 3 9 W/V * where : W-Welgh to f

K.Cr.O . used , g

Vi-Vo)um e o

f C.H.A. O used . ml . Nj-Normalit y of

standard phenylarsln e oxid e solution . E»eq/llter . O.5039-Conversio n facto r


# Ill-Appendi x A-4 3< teq . 1,/aiol e K,Cr.O, > (1.00 0 ml/lltert .

(249. 2 g . K,Cr.O,/mole > OO O aliquo t factor ) 

# L
P,3 tion . Normalit y o l Standar d Iodin e Solu N.-N/vVV , where : - . ' - : Ki-Normaltt y o f

standar d Iodin e solution . B-eq/llter . Y,-Volum e o f

standar d Iodin e tolutlo n used . ml . N t -Normallt y o f

standar d (-0.0 1 N ) thio sulfat e solution* , assume d t o b e 0. 1 N» . 8 - eq/llier . ^ , V T -Volum e o f

thiosulfat e solutio nused . a L NOT*.—I f

phenylaxsln e oxid e I s use d tntsa d o f

thiosulfate . replac e N ran d V T I n Equatio n0. 3 wit h N » an d V ^ respecUvel y (se e section s 8.1. 1 an d 8.1.3) . 8. 4 Dr y Ga s Volume . Correc tth e sampl e volum e measure d b y th e dr y es s mete rt o • otandar d condition s (20 * C ) nn d 76 0 m m Hg . V.w.»-V. Y t(T«*/T. ) CP_/P;« » Where : V„w - Volum e a tstandar d condition s o f ga s sampl e throuz h th e dr y ca s meter , stan -

. dar d liters . \*.-Volum e o rga s sampl e throug h th e dr y ea s mete r(mete rconditions) , liters . T«4 - Absolut e temperatur e a tstandar d con ditions . 293 " K . T„-Averaa e dry ea s mete rtempertHure . *K. P w -B»rometrl e pressur e a tth e samplin g site . mmHg . P^-Absolut e pressur e a tstandar d condl - - • . tions . 76 0 mm Hg . . . Y - Dr y ca s mete rcalibratio nfactor . 0. 5 Concentratio no f

H A Calculat e th e concentratio no f

H. S i nth e ca s strea m a t standar d condition s usin gth e followin g equation : C.-KKVnN.-VnN, ) sareple - (V„N,-VnN T ) blankl/V.. ^ wher e (metri cunits) : * ' C M » » Concentratio no f

H 3 a tstandar d con ditions , mg/dscm . K-Co n versio nfactor-17.04x10 ' C34.0 7 c'mol e K£ ) (1.00 0 llters/m* ) <1.00 0 ma/g)/-(1.00 0 ml/liter ) (2H. 3 eq/mole ) Vir-Volum e o f

standar d Iodin e solu tion* * 50. 0 ml . N.-Normalil y of

standar d Iodine solution , C-eq/liter . Vrr-Volum e o f

standar d (-0.0 1 N ) sodiu m thiosulfat e solution . m

L Ki-Normalit y o

f standar d sodiu m thiosul - • fat e solution , c-eq/liter . . Vw.ai-Dr y Ca

s volum e a tstandar d condi tions , liters . NOTX.—I f

phenylarsln e oxid e i ause d In stea d o f thiosulfate . replac e H tan d V nI n Equatio n9. 5 with N A tJi d VM . respectivel y (ss e Section s 7.3. 1 an d 8.1.3) . 

### \ Stability. Th e absorbin gsolutto nI s stabl e fo ra tleas t1 month . Sampl e recover y an d analysi s 6houl d begi nwithi n1 hou ro f samplin gt o minimiz e oxidatio nof th e acidi fie d cadmiu m sulfide . Onc e Iodine ha s bee n adde d t o th e sample , th e rematnde ro f th e analysi s procedur e mus tb e complete d ac - . cordin gl o section s 7.2. 2 throug h 7.3.2 . 11 . Bibliography. 11. 1 Determinatio no f

Hydroge nSulfide , Ammonlaca l Cadmium Chlorid e Method. . AP I Metho d 772-5 L Ir

U Manual o nDisposa l O f Refiner y Wastes , VoL V : Ssmplin gan d Analyst s o f

Wast e Oase s an d Particulat e M titter , America nPetroleu m Institute , Washington , D.0.1954 . 11. 2 Tentativ e Metho d of Determinatio n o f Hydroge nSulfid e an d Mercapta nSulfu r I nNatura l Oaa . Natura l OaaProcessor s As sociation , Tulsa . Okla , NOPA Publicatio n No . 2265-63,1095 . 11. 3 Knoll , J . E. . an d M . R . MldgetL De terminatio no f

Hydroge n Sulfid e i nRefin er y Fue l Oases . Environmenta l Monitorin g Series . Offic e o f

Researc h an d Develop ment . USEPA . Researc h Triangl e Park . N.C . 27711 , EPA 600/4-77-007 . 11. 4 Schelll . O . W „ an d M . C . Sharp . Standardizatio no f

Metho d 1 1 a taPetit* ' )eu m Refinery , Mldweal Researc h Institut e Draf tRepor tfo rUSEPA . Offic e o f Re searc h an d Development . Researc h Trlsnjl e Park . N.C . 27711 . EP

A Contrac tNo . 65-02 - 1033 . Ausus f

1976 . -EP A 600/4-77-033 * (Volum e 1 ) en d EP

A 600/4-77-ODS b (Volum e 3) . (Sees . Ill , 114 , 301(6) , Clea nAi rAc ta s amende d (4 2 U.6.C.7411,7414,760).). )

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