P. 1



# OAR Box 

# 1338 Prepped by Ollie Stewart



# Document

Number: 

# 52 ) F

. R Februar

y13 , 199 1 Docket Number: 

# A-89-1 1

Printed 6/17/20081:48:08PM

Sheet 52 of 105P. 2



### " * 5$%8 > Federa

l Register/

Vol.'56 , No.J 30v/-Wediesday;'Feb'ruary t 13 , )1991J /



### Rule s arid;Regulation s delayed , timel y notic e wil l b e publishe d i n th e Federa l Register
. ADDRESSES : Copie s o f

th e stat e submitta l fo r

thi s actio n ar e availabl e fo r publi c inspectio n durin g norma l busines s hour s at : th e Environmenta l Protectio n Agency , Regio n VII , Ai r Branch , 72 6 Minnesot aAvenue , Kansa s City , Kansa s 66101 ; Publi c Informatio n Referenc e Unit , Environmenta l Protectio n Agency * 40 1 M Stree t SW. , Washington , D C 20460 ; Environmenta l Protectio n Division , Iow aDepartmen t o f Natura l Resources , Wallac e Stat e Offic e Building , 90 0 Eas t

Grand , De s Moines , Iow a50319
. FO R FURTHE R INFORMATIO N CONTACT : Wayn e Kaise r

a t (913 ) 551-760 3 (FT S 276-7603)
. SUPPLEMENTAR

Y INFORMATION: O n Octobe r 17,1988 , EP A revise dth e preventio n o f

significan t

deterioratio n (PSD ) regulation s a t

4 0 CF R52.2 1 (se e 5 3 FR40656 ) fo r

nitroge n oxides
. Thes e regulation s establis hth e maximu m increas e i n ambien t

nitroge n dioxid e concentration s allowe di n a n are aabov e th e baselin e concentration ; thes e maximu mallowabl e increase s ar e calle dincrements
. Th e intende deffec t o f thes e regulation s i s t o requir e al l applicant s fo r

majo r ne w stationar y source s an dmajo r

modification s emittin g nitroge n oxide s t o accoun t fo r and , i f necessary , restric t

emission s s o a s no t t o caus e o r

contribut e t o exceedance s o f

th e increment
. O n Novembe r

20,1990 , th e IDN R submitte da n amendmen t t o chapte r 22.4(455B) , "Specia l Requirement s fo r Majo r Stationar y Source s Locate di n Area s Designate dAttainmen t o r Unclassifie d(PSD), " whic hincorporate s b y referenc e th e revision s t o 4 0 CF Rpar t 52.21 , effectiv e Octobe r 17,1988
. Th e stat e rul e wa s effectiv e Novembe r 21

- 1990
. Th e stat e als o provide da demonstratio n tha t

i t meet s th e . condition s fo r

approva l o f

adoptio n o f th e NO 2 incremen t

progra ma s detaile d i n th e EP A guidanc e memorandu mo n th e subjec t

date dAugus t

17,1990
. Th e abov e memorandu mdescribe d specifi c condition s fo r

EP A approva l o f astate' s adoptio n o f

th e NO xincremen t rule
. Thos e condition s pertaine dt o regulator y language ; incremen t consumptio n analysis , incremen t consumptio n fo r

th e transitio n period , an dlega l authority
. EP A ha s evaluate d th e state' s submitta l i n accordanc e wit h th e Augus t

17,1990 , guidanc e an dfind s tha t th e stat e submitta l i s acceptable
. EP A i s publishin g thi s actio n withou t prio r proposa l becaus e th e Agenc y view s thi s a s anoncontroversia l amendmen t

an danticipate s n o advers e comments
. Thi s actio n wil l b e effectiv e Apri l 15,1991 , unless , withi n 3 0 day s o f it s publication , notic e i s receive dtha t advers e o r

critica l comment s wil l b e submitted
. If suc hnotic e i s received , thi s actio n wil l b e withdraw n befor e th e effectiv e dat e b y publishin g tw o subsequen t notices
. On e notic e wil l withdra w th e fina l actio n an danothe r wil l begi n a ne w rulemakin g b y announcin g a proposa l o f

th e actio n an destablishin g a commen t period
. If

n o suc hcomment s ar e received , th e publi c i s advise dtha t thi s actio n wil l b e effectiv e Apri l 15 , 1991
. EP A Action : EP A i s takin g fina l actio n t o approv e arevisio n t o Iow arul e 567

- 22.4(455B ) which , adopt s b y referenc e th e PS D NO xrequirement s of 4 0 CF R52.2 1 a t 5 3 FR4065 6 (Octobe r

17,1988)
. Nothin g i n thi s actio n shoul db e construe da s permittin g o r allowin g o r establishin g apreceden t fo r an y futur e reques t fo r revisio n t o an y SIP
. Eac h reques t fo r revisio n t o th e SI Pshal l b e considere dseparatel y i n ligh t o f specifi c technical , economic , an denvironmenta l factor s an di n relatio n t o relevan t statutor y an dregulator y requirements
. Unde r 5 U.S.C : 605(b) , I certif y tha t thi s SI Previsio n wil l no t

hav e asignifican t economi c impac t

o n asubstantia l numbe r o f smal l entitie s (Se e 4 6 FR 8709)
. Thi s actio n ha s bee n classifie da s a Tabl e 3 actio n b y th e Regiona l Administrato r

unde r th e procedure s publishe di n th e Federa l Registe r o n Januar y 19,198 9 (5 4 FR2214-2225)
. O n Januar y 6,1989 , th e Offic e o f Managemen t

an dBudge t

waive dTable s 2 an d3 SI Prevision s (5 4 FR2222 ) fro m ' th e requirement s o f

Sectio n 3 o f Executiv e Orde r

1229 1 unti l Apri l 1991
. Unde r sectio n 307(b)(1 ) o f

th e Act , petition s fo r

judicia l revie w o f

thi s actio n mus t

b e file di n th e U.S
. Cour t o f Appeal s fo r

th e appropriat e circui t b y Apri l 15,1991
. Thi s actio n ma y no t b e . challenge dlate r

i n proceeding s t o enforc e it s requirements
. (Se e sectio n 307(b)(2). ) Th e Agenc y ha s reviewe dthi s reques t fo r revisio n o f

th e federall y approve d SI Pfo r conformanc e wit hth e provision s o f th e 199 0 Amendment s enacte do n Novembe r

15,1990
. Th e Agenc y ha s determine dtha t

thi s actio n conform s wit hthos e requirement s irrespectiv e o f th e fac t tha t th e adoptio n o f

th e revisio n b y th e stat e precede dth e dat e o f enactment
. Lis t o f Subject s i n 4 0 CF RPar t 5 2 Ai r pollutio n control , Incorporatio n b y reference , Intergovernmenta l relations , Nitroge n dioxide , Particulat e matter , Sulfu r oxides
. Dated : January 28,1991
. Morri s Kay , Regional Administrator. 4 0 CF Rpar t

52 , subpar t

Q , i s amende d a s follows : PAR T52—[AMENDED ) 1
. Th e authorit y citatio n fo r par t 5 2 continue s t o rea da s follows : Authority : 42 U.S.C
. 7401-7642
. 2
. Sectio n 52.82 0 i s amende db y addin g paragrap h(c)(53 ) t o rea da s follows : § 52.820 Identificatio n o f plan . **** * .'(c) * * *

, (53 ) Revise dchapte r 22 , rul e 22.4(455B) , submitte do n Novembe r 8 , 1990 , incorporate s b y referenc e revise d EP A PS D rule s pertainin g t o NO x increments , (i ) Incorporatio n b y referenc e (A ) Amendmen t

t o chapte r

22 , "Controllin g Pollution, " Iow a Administrativ e Code , subrul e 22.4 , adopte db y th e Environmenta l Protectio n Commissio n o n Octobe r 17 , 1990 , effectiv e Novembe r 21,1990
. (ii ) Additiona l materia l (A ) Lette r

fro mth e stat e date d Novembe r

8,1990 , pertainin g t o NO „ rule s an danalysi s whic hcertifie s th e materia l wa s adopte db y th e stat e o n Octobe r 17,1990
. [F RDoc
. 91-345 1 File d2-12-91 ; 8:4 5 am] BILLING . COD E 6560-50- M 4 0 CF R Part 6 0 [AD-FRL-3867-1 ] >/ Standard s o f Performanc e fo r Ne w Stationar y Sources ; Additio n o f Method s fo r Measuremen t o f Polychlorinate d Dibenzo-p-Dioxins , Polychlorinate d Dibenzofurans , an d Hydroge n Chlorid e Emission s Fro m Stationar y Source s AGENCY: Environmenta l Protectio n Agenc y (EPA)
. ACTION : Fina l rule
. SUMMARY

: Th e purpos e o f

thi s actio n i s t o ad dMetho d23 , "Determinatio n t o Polychlorinate dDibenzo-p-Dioxin s (PCDD's ) an dPolychlorinate d Dibenzofuran s (PCDF's ) fromStationar y Sources, " an dMetho d26 , "Determinatio n o f

Hydroge n Chlorid e Emission s fromStationar y Sources " t o appendi x A o f

4 0 CF Rpar t

60
. Thes e method s ar e bein g promulgate dt o determin e complianc e wit hsubpart s C a an dE ao f

par t 60
.P. 4



### Federa l Registe r

/ Vol
. 56,! • No
. '3 0 7 Wednesday , Februar y 13.
. 199 1 / Rule s an dRegulatipn s 575 9 DATES : Effective Date: February 13 , 1991
. Judicial Review: Under

sectio n 307(b)(1 ) o

f th e Clean Ai r

Act , judicia l revie w o f th e action s take n b y thi s notic e i s availabl e onl y b y th e filing o f a petitio n fo

r revie w i n th e U.S
. Cour

t o f Appeal s fo

r th e Distric t

o f Columbi a Circui t withi n 60 day s o

f today' s publicatio n o

f thi s rule
. Unde r

sectio n 307(b)(2) o

f th e Clean Ai r

Act , th e requirement s tha t

ar e th e subjec t

o f today' s notic e may no t

b e challenge d late r i n civi l o r

criminal proceeding s brough t b y EP A t o enforc e thes e • requirements
. ADDRESSES : Background

Information Document. Th e Backgroun dInformatio n Document fo r th e promulgate dtes t method s may b e obtaine dfro mGary McAliste r or Roge r Shigehara , MD-19 , U.S
. EPA , Researc hTriangl e Park
. Nort h Carolin a27711 , telephon e numbe r (919) 541-1062
. Pleas e refer

t o "Summar

y o f Comment s an dResponse s fo r Method s 2 3 an d26. " Docket Docke t Number A-89-11 , containin g materia l relevan t t o thi s rulemaking , i s availabl e fo r publi c inspectio n an dcopyin g betwee n 8:3 0 a.m . an d3:3 0 p.m . Monday throug h Friday , at EPA' s Ai r

Docke t Section , roo mM-1500,1s t

Floor , Watersid e Mall , 401 M Stree t

SW. , Washington , DC 20460
. A reasonabl e fee may b e charge d fo r copying
. FO RFURTHE RINFORMATIO N CONTACT : 

### Gary McAliste r

or Roger Shigehara , Emissio n Measuremen t

Branc h(MD-19) , Technica l Support

Division , U.S
. Environmenta l Protectio n Agency , ResearchTriangl e Park , Nort hCarolin a 27711 , telephon e numbe r

(919) 541-1062
. SUPPLEMENTAR Y INFORMATION : 

### I
. Th e Rulemakin g Unde r Subpart s C aan dEa , th e EP A i s regulatin g emission s fro

mmunicipal wast e combustor s (MWC's ) includin g settin g emissio n limit s fo

r polychlorinate ddibenzo-p-dioxin s (PCDD's) , polychlorinate d dibenzofuran s (PCDF's) , an d hydrochlori c aci d(HCl)
. Ther e ar e presentl y n o method s publishe din 40 CF Rpar t 60 , appendi x A , t o measur e an y o f thes e pollutants
. Thi s actio n woul dpromulgat e on e metho dt o measur e th e PCDD' s an dPCDF' s an d anothe r metho dt o measur e th e HCl
. Summary of

Reference Methods Metho d2 3 i s use dt o measur e th e emissio n of

PCDD' s an dPCDF' s from MWC's
. A sampl e i s withdraw n isokineticall y fro

mth e stac k

throug ha probe , afilter , an datra p packe dwitha soli dadsorbent
. Th e PCDD' s an d PCDF' s ar e collecte din th e probe , o n th e filter , an do n th e soli dadsorbent
. Th e PCDD' s an dPCDF' s ar e extracte dfro m th e particulat e matte r

an dth e adsorben t withaho t organi c solvent
. Th e extracte dPCDD' s an dPCDF' s ar e separate db y capillary ga s chromatography , an dthen , eac hisomer i s identifie dan dmeasure dwithmas s spectrometry (GC/MS)
. Th e tota l PCDD' s an dPCDF' s ar e th e sumo f th e individua l isomers
. Toxicity factor s ar e no t use din th e calculation
. Metho d2 6 i s use dt o measur e th e emissio n o

f HC l fro mMWC's
. A sampl e i s withdraw n at

aconstan t

rat e fro mth e stac k throug haprob e an dimpinger s fille dwithadilut e acid
. Th e HC l i s collecte di n th e implinger solution
. Th e chlorid e io n i s separate db y io n chromatograph y an dmeasure db y a conductivity detector
. Background In 1983 , th e America n Society o f Mechanica l Engineer s (ASME ) recognize dtha t

th e testin g fo

r PCDD' s an dPCDF' s neede dt o b e standardized
. In February o

f 1984 , th e ASM

Econvene d acommitte e of

governmen t representatives , testin g consultants , equipmen t

manufacturers, an d

. incinerato r

operator s t o writ e a standar dtes t

procedur e fo

r PCDD' s an d PCDFs
. Thi s wa s eventuall y distribute d a s adraf t ASM Eprotoco l in Decembe r o f 1984
. Th e procedur e tha t w e ar e promulgatin g wa s derive dfro mthi s draf t ASM Eprotocol
. Ther e ar e some change s i n th e quality assuranc e (QA) requirement s an dth e solvent s use dto recove r th e sampl e i n th e promulgate d method
. Becaus e more labele d compound s ar e available , th e metho d wil l requir e additiona l labele dinterna l standard s an dsurrogat e compound s whic hwil l provid e bette r representatio n o f th e entir e rang e o

f PCDD' s an d PCDF's
. Th e filter

an dsoli dadsorben t ar e extracte di n th e laborator y with toluen e t o assur e ahig hPCD D an d PCDFrecovery efficiency
. Additionall y th e propose dsampl e recovery solvent s use dfo r rinsin g th e sampl e trai n glasswar e i n th e fiel dwoul db e aceton e followe db y methylen e chlorid e witha fina l quality assuranc e rinse usin g toluene
. However , th e result s fromth e toluen e rins e ar e no t

use di n calculatin g th e tota l PCD

D an dPCD

Femissions
. EP A wil l continu e t o revie w th e toluen e fiel drins e quality assuranc e results an d continu e t o evaluat e th e desirability o f replacin g methylen e chlorid e with toluen e fo r fieldrinsin g sampl e glassware
. II
. Publi c Participatio n Th e opportunity t o hol dapubli c hearin g a t 1 0 a.m . o n February 7,199 0 wa s presented , bu t

n o on e requeste da hearing
. Th e publi c comment perio dwa s fromDecembe r

20,198 9 t o Marc h5 , 1990
. III
. Significant

Comment s an dChange s t o th e Propose dRulemakin g Thirtee n comment

letter s wer e receive do n th e propose dtes t methods
. Thes e comment s hav e bee n carefull y considere dand , wher e deeme d appropriat e b y th e Administrator , change s hav e bee n mad e i n th e propose dtes t

methods
. A detaile d discussio n o

f thes e comment s i s containe di n th e backgroun ddocumen t entitled , "Summar

y o f Comment s an d Response s fo

r Method s 2 3 an d26 " whic hi s referre dt o in th e ADDRESSE S sectio n o f thi s preamble
. Severa l commenter s thought that , ther e wer e no t

enoug hstac k

samplin g organization s tha t

wer e experience d withMetho d2 3 t o avoi dmajor delay s in securin g samplin g an danalysi s contractors
. Man y o

f thes e commenter s als o thought

tha t ther e woul dno t

b e a n adequat e suppl y o

f calibratio n standard s an daudi t

samples
. W e believ e tha t

th e numbe r

o f test s require d immediatel y after

promulgatio n o

f th e regulatio n wil l no t

excee dth e capabilitie s o

f th e availabl e samplin g an danalytica l laboratorie s an dtha t ther e wil l b e a n adequat e suppl y o f labele dstandard s an daudi t samples
. Th e ful l effect o f th e testin g requirement s fo

r th e ne w an dexistin g source s wil l no t

b e felt fo r abou t five years . W e believ e tha t

thi s i s adequat e tim e t o allo w fo

r th e necessar y expansio n o

f testin g capabilities
. Som e commenter s requeste d alternativ e procedure s or method s t o Metho d23
. Whil e tester s alway s hav e th e optio n o

f requestin g alternativ e methods , request s shoul db e submitte d after th e metho dbecome s final
. Any reques t shoul db e in writin g an dshoul d b e accompanie db y an y supportin g data
. Man y commenter s thought tha t th e ga s chromatograph y column s specifie d in Metho d2 3 wer e no t

th e mos t appropriat e choice
. Th e colum n requirement s in th e metho dhav e bee n revise dt o allo w th e teste r t o us e an y colum n syste mprovide dtha t

th e teste r ca n demonstrat e throug hcalibratio n an d perfonnanc e check s tha t

th e column s provid e th e necessar y isome r separation
. On e commente r

thought tha t Metho d 2 6 shoul db e modifie dt o allo w isokineti c samplin g s o tha t it coul db eP. 5

5760 , , Federa l Registe r / Vol
. 56 , .No
. 30
. / , Wedngs-day , .-February * 13, , 199 ^ / Rule3 * ftjidj Regulation s applie dt o source s wher e hydrochlori c aci daerosol s ar e present
. W e agre e tha t isokineti c sampling ; ma y b e importan t a t source s othe r

tha n MWC's
. W e hav e compare dMetho d2 6 an da n isokineti c samplin g trai n an dfoun dtha t the y generall y giv e simila r

result s a t

stac k concentration s abov e 2 0 PPM
. A t lowe r concentration s th e isokineti c samplin g trai n seem s t o hav e anegativ e bias
. W e ar e continuin g t o investigat e thi s problem , an dma y b e abl e t o approv e a n alternativ e metho dusin g isokineti c samplin g fo r

futur e use . Anothe r commente r

wante dEP A t o develo p aQ A audi t

sampl e fo r

Metho d 26
. A n audi t

sampl e i s bein g develope d an dwil l b e availabl e fo r validatin g th e result s o f

complianc e tests
. IV
. Administrativ e Th e docke t

i s a n organize dan d complet e fil e o f

al l th e informatio n submitte dt o o r

otherwis e considere db y EP A i n th e developmen t o f this ; rulemaking
. Th e principa l purposes , o f th e docke t

are : (1 ) T o allo w intereste d partie s t o identif

y an dlocat e document s s o tha t the y ca n effectivel y participat e i n th e rulemakin g proces s an d(2 ) t o serv e a s th e recordi n cas e o f judicia l revie w (excep t

fo r interagenc y revie w materials ) (sectio n 307(d)(7)(A))
. Unde r Executiv e Orde r

12291 , EP A mus t judg e whethe r

aregulatio n i s "major " and , therefore , subjec t t o th e requiremen t

o f aregulator y impac t analysis
. Th e Agenc y ha s determine d tha t thi s rulemakin g woul dno t resul t i n an y o f

th e advers e economi c effect s se t fort hi n Sectio n 1 o f

th e Orde r

a s ground s fo r

findin g a"majo r

rule; " Th e Agenc y has , therefore , conclude dtha t thi s regulatio n i s no t

a"majo r

rule " unde r Executiv e Orde r

12291
. Th e Regulator y Flexibilit y Ac t (RFA ) o f 198 0 require s th e identificatio n o f
. potentiall y advers e impact s o f Federa l regulation s upo n smal l busines s entities
. Th e Ac t specificall y require s th e completio n o f

a n RF A analysi s i n thos e .instance s wher e smal l busines s impact s ar e possible
. Becaus e thi s rulemaking , impose s n o advers e economi c impacts , a n analysi s ha s no t

bee n conducted
. Pursuan t t o th e provision s o f

5 U.S.C
. 605(b) , I hereb y certif

y tha t thi s promulgate drul e wil l no t hav e a n economi c impac t

o n smal l entitie s becaus e n o additiona l cost s wil l b e incurre dfromthi s action
. Thi s rul e doe s no t

contai n an y informatio n collectio n requirement s currentl y approve db y OM B revie w unde r th e Paperwor k

Reductio n Ac t

o f 1980 , 4 4 U.S.C
. 350 1 et

seq. Lis to f Subject s i n 4 0 CFRPart6 0 Ai r pollutio n control , Municipa l wast e combustors , Polychlorinate ddibenzo-p

dioxins , Polychlorinate ddibenzofurans , Hydroge n chloride
. Dated : January 11,1991
. F
. Henry Habicht , Acting Administrator. Titl e 40 , par t

6 0 o f th e Cod e o f

Federa l Regulation s i s amende da s follows : PAR T 60—[AMENDED ] 1
. Th e authorit y citatio n fo r par t 6 0 continue s t o rea da s follows : Authority : 42 U.S.C
. 7401 , 7411,7414 , 7416
. an d7601
. 2
. B y addin g i n numerica l orde r Method s 2 3 an d2 6 t o appendi x A a s follows : Appendi x A—Referenc e Method s Metho d23—Determinatio n o f Polychlorinate d Dibenzo-p-Dioxin s an dPolychlorinate d Dibenzofuran s FromStationary Source s 1. Applicability, and

Principle 1. 1 Applicability
. Thi s metho di s applicabl e t o th e determinatio n o f polychlorinate ddibenzo-p-dioxin s (PCDD's ) an dpolychlorinate ddibenzofuran s (PCDF's ) fro mstationar y sources . 1.2 Principle
. A sampl e i s withdraw n fro m th e ga s strea misokineticall y an dcollected'i n th e sampl e probe , o n aglas s fiber filter , an d o n apacke dcolum

n o f adsorben t

material
. Th e sampl e canno t

b e separate dinto a particl e vapo r

fraction.The PCDD' s an d PCDF' s ar e extracte dfro

mthe
. sample , separate db y highresolutio n ga s chromatography , an dmeasure db y high resolutio n mas s spectrometry
. 2. Apparatus 2. 1 Sampling
. A schemati c o f th e samplin g trai n use di n thi s method , i s show n in Figur e 23-1
. Sealin g grease s ma

y no t b e use di n assemblin g th e train
. Th e trai n i s identical , to that describe din sectio n 2. 1 o f Metho d5 of

' thi s appendix * wit

hth e following additions : BILLING. COD E 6560-50-1 2

### tv*w — 

## " " T' "••• ^


# t
Ga s Flow ^ Stac k Wal l

\ Heate d Glas s Line r 

## \

s -s"Typ e ^ Pito tTub e Temperatur e Senso r Condense r Temperatur e

Senso r Temperatur e Senso r

Incline d Manomete r Recirculatio n

Pum p
Empt y Dr y Ga s Mete r Empty

Coars e

r

### Calibrate d Ga s - 1 Orific e
_ 

# Exi t V *

?

Incline d ^ i Manomete r Silic a Ge l

Vacuu m Gaug e 

# 1

Vacuu m Pum p 

# Figur e 23. 1 Samplin g trai n *

BILLING COD E 6560-5I M CD D . CDC D C O rr C D 1 - 

## < O C n 

## 2 p C O 

### o

CD , C L a , C D C O D . 0 ) 

### •n CD ' CT ' 

### S". . 

### < 3

C O co 

### s e C D 1 C O 

### ». - 3 D u CD- - 0 0 c o 3 .



### cn V I O S

### 576 2 Federa

l Registe r/

Vol
. 56 , No
. 3 0 /

Wednesday , Februar y 13 , 1991 ' / Rule s and-Regulation s P. 7 

# 77 H

2.1. 1 Nozzle
. Th e nozzl e shal l b e mad e o f nickel , nickel-plate dstainles s steel , quartz , o r borosilicat e glass
. 2.1. 2 Sampl e Transfe r

Lines
. Th e sampl e transfe r lines , i f needed , shal l b e hea t

traced , heav y walle dTF

E(% in
. OD withVf

e in
. wall ) withconnectin g fitting s tha t ar e capabl e o

f forming leak-free , vacuum-tight connection s withou t usin g sealin g greases . Th e lin e shal l b e a s short

a s possibl e an dmus t

b e maintaine da t

12 0 ° C 2.1. 1 Filte r

Support
. Teflo n o r

Teflon

coate dwire
. 2.1. 2 Condenser
. Glass , coi l typ e with compatibl e fittings
. A schemati c diagrami s show n i n Figur

e 23-2
. 2.1. 3 Wate r

Bath
. Thermostaticall y controlle dt o maintai n th e ga s temperatur e exitin g th e condense r

at <2 0 ° C (6 8 °F)
. 2.1. 4 Adsorben t

Module
. Glas s containe r t o hol dth e soli dadsorbent
. A shemati c diagrami s show n in Figur e 23-2
. Othe r physica l configuration s o

f the : resi n trap / condense r

assembl y ar e acceptable
. Th e connectin g fitting s shal l for mleak-free , vacuu mtight

seals
. N o sealan t grease s shal l b e use din th e sampling ; train
. A coars e glas s frit i s include dt o retain

- th e adsorbent
. 2. 2 Sampl e Recovery
. 2.2. 1 Fittin g Caps
. Groun dglass , Teflon tape , o r aluminumfoi

l (Sectio n 2.2.6

) to cap of f the
. sampl e exposedsection s o f th e train
. 2.2. 2 Was hBottles
. Teflon , 500-ml
. 2.2. 3 Probe-Liner

Probe-Nozzle , an dFilter

Holde r Brushes
. Inert

bristl e brushe s wit

h precleane dstainles s stee l o r Teflo n handles
. Th e prob e brus hshal l hav e extension s o f stainles s stee l o r

Teflon , at leas t a s lon g S s th e probe.
. The:brushe s shal l b e properl y size dan dshape dt o brus hou t th e nozzle , prob e liner , an dtransfe r

line , i f used
. BILLIN G COD E 6560-50- MW* -» ' I i p ,m II.. . i » | fi ^, < •*ir—^^^^F - T " ••» ' W "C H w-cm W •• . ••-f- j

. ; Condense r Sorben t Tra p Flu e Ga s Flo w*

$20/1 6
Wate r Jacke t Coolin g Coi l Glas s Woo l Plu g Wate r Jacke t XA D - 2 Glas s Sintere d Dis k D . 

# ? £2 . W 

# 4 . OD •• » r\ *— > o r - c n P> 

# \z p t o o 

# f C D C O a. 

# I

Figur e 23.2

. Condense ran d adsorben t tra p

BILUN Q COD E 6560-SO- C c r
0 3 *• »
C O

» 

### c 

## 5 " BO O S 3 Ct , W 

## ,2 O Q . C 0 9 E X 

## §

C dP. 9


### 576 4 Federa

l Registe r/

Vol
. 56 , No
. 3 0 /

Wednesday , February 13 , 199 1 / Rule s an dRegulation s
2.2. 4 Filte rStorag e Container . Seale d filterholder , wide-mout h ambe rglas s ja rwit h Teflon-line d cap , o rglas s petr i dish . 2.2. 5 Balance . Tripl e beam . 2.2. 8 Aluminu m Foil . Heav y duty , hexane rinsed . 2.2. 7 Meta l Storag e Container . Ai rtigh t containe rt o stor e silic agel . 2.2. 8 Graduate d Cylinder . Glass , 250-m l wit h 2-ml graduation . 2.2. 9 Glas s Sampl e Storag e Container . Ambe rglas s bottl e fo rsampl e glasswar e washes , 500 - o r1000-ml , wit h lea kfre e Teflon-line d caps . 2. 3 Analysis . 2.3. 1 Sampl e Container . 125 - an d 250-m l flin tglas s bottle s wit h Teflon-line d caps . 2.3. 2 Tes tTube . Glass . 2.3. 3 Soxhle tExtractio n Apparatus . Capabl e o f

holdin g 4 3 x 12 3 m

m extractio n thimbles . 2.3. 4 Extractio n Thimble . Glass , precleane d cellulosic , o rglas s fiber . 2.3. 5 Pasteu rPipettes . Fo rpreparin g liqui d chromatographi ccolumns . 2.3. 6 Reacti-viais . Ambe rglass , 2-ml , silanize d prio rt o use . 2.3. 7 Rotar y Evaporator . Buchi/Brinkma n RF-12 1 o requivalent . 2.3. 8 Nitroge n Evaporativ e Concentrator . N-Eva p Analytica l Evaporato rMode l II I o r equivalent . 2.3. 9 Separator y Funnels . Glass , 2-liter . 2.3.1 0 Ga s Chromatograph . Consistin g o f th e followin g components : 2.3.10. 1 Oven . Capabl e o f maintainin g th e separatio n colum n a tth e prope roperatin g temperatur e ±° C an d performin g programme d increase s i n temperatur e a t rate s o f a tleas t4 0 °C/min . 2.3.10. 2 Temperatur e Gauge . T o monito r colum n oven , detector , an d exhaus t temperature s ±1 °C . 2.3.10. 3 Flo w System . Ga s meterin g syste m t o measur e sample , fuel , combustio n gas , an d carrie rga s flows . 2.3.10. 4 Capillar y Columns . A fuse d silic a column , 6 0 X 0.2 5 m

m insid e diamete r(ID) , coate d wit h DB- 5 an d afuse d silic acolumn , 3 0 m X 0.2 5 m

m I D coate d wit h DB-225 . Othe rcolum n system s ma y b e use d provide d tha tth e use ri s abl e t o demonstrat e usin g calibratio n an d performanc e check s tha tth e colum n syste m i s abl e t o mee tth e specification s o f

sectio n 6.1.2.2 . 2.3.11 . Mas s Spectrometer . Capabl e o f routin e operatio n a taresolutio n o f 1:1000 0 wit h astabilit y o f

±5 ppm . 2.3.1 2 Dat aSystem . Compatibl e wit h th e mas s spectromete ran d capabl e o f monitorin g a tleas tfive group s o f

2 5 ions . 2.3.1 3 Analytica l Balance . T o measur e withi n 0. 1 mg . 3. Reagents 3. 1 Sampling . 3.1. 1 Filters . Glas s fiber filters, withou t organi cbinder , exhibitin g a tleas t99.9 5 percen tefficienc y (<0.0 5 percen t penetration ) o n 0.3-micro n diocty l phthalat e smok e particles . Th e filterefficienc y tes t shal l b e conducte d i n accordanc e wit h AST M Standar d Metho d D 2986-7 1 (Reapprove d 1978 ) (incorporate d b y reference—se e * 60.17) . 3.1.1. 1 Precleaning . Al l filter s shal l b e cleane d befor e thei rinitia l use . Plac e aglas s extractio n thimbl e an d 1 g o f silic age l an d a plu g o f glas s woo l int o aSoxhle tapparatus , charg e th e apparatu s wit h toluene , an d reflu x fo raminimu m o f

3 hours . Remov e th e toluen e an d discar d it , bu tretai n th e silic agel . Plac e n o mor e tha n 5 0 filter s i n th e thimbl e ont o th e silic age l be d an d to p wit h th e cleane d glas s wool . Charg e th e Soxhle twit h toluen e an d reflu x fo r1 8 hours . Afte rextraction , allo w th e Soxhle tt o cool , remov e th e filters, an d 

### dry the munde r

aclea nN

2

### stream
. Stor e th e filters i n aglas s petr i dis h seale d wit h Teflo n tape . 3.1. 2 Adsorben tResin . Amberlit e XAD- 2 resin . Thoroughl y cleane d befor e initia l use . 3.1.2. 1 Cleanin g Procedure . Thi s procedur e ma y b e carrie d ou ti n agian t Soxhle textractor . A n all-glas s filte rthimbl e containin g a n extra-cours e friti s use d fo r extractio n o f

XAD-2 . Th e friti s recesse d 10 - 1 5 m m abov e acrenelate d ring a tth e botto m o f th e thimbl e t o facilitat e drainage . Th e resi n mus tb e carefull y retaine d i n th e extracto r cu p wit h aglas s woo l plu g an d astainles s stee l rin g becaus e itfloat s o n methylen e chloride . Thi s proces s involve s sequentia l extractio n i n th e followin g order . Solven t Wate r

Wate r Methano l Methylen e Chlorid e Procedur e
i n a beaker , rinse once wit h water , an d discard . Fil l wit h wate r a secon d time , le

t stan d overnight , an d discard . Extrac t wit h wate r fo r 8 hours .

3.1.2. 2 Drying . 3.1.2.2. 1 Dryin g Column . Pyre x pipe , 10. 2 c m ID b y 0. 6 m long , wit h suitabl e retainers . 3.1.2.2. 2 Procedure . Th e adsorben tmus t b e drie d wit h clea n iner tgas . Liqui d nitroge n from astandar d commercia l liqui d nitroge n cylinde rha s prove n t o b e areliabl e sourc e o f larg e volume s o f

ga s fre e from organi c contaminants . Connec tth e liqui d nitroge n cylinde rt o th e colum n b y alengt h o f cleane d coppe rtubing , 0.9 5 c m ID , coile d t o pas s throug h ahea tsource . A convenien thea t sourc e i s awater-bat h heate d fro m astea m line . Th e final nitroge n temperatur e shoul d onl y b e war m t o th e touc h an d no tove r4 0 °C . Continu e flowin g nitroge n throug h th e adsorben tunti l al l th e residua l solven ti s removed . Th e flo w rat e shoul d b e sufficien t t o gentl y agitat e th e particle s bu tno ts o excessiv e a s th e caus e th e particle s t o fracture . 3.1.2. 3 Qualit y Contro l Check. Th e adsorben tmus tb e checke d fo rresidua l toluene . 3.1.2.3. 1 Extraction . Weig h 1. 0 g sampl e o f drie d resi n int o asmal l vial , ad d 3 ml o f toluene , ca p th e vial , an d shak e i twell . 3.1.2.3. 2 Analysis . Injec ta2 fil sampl e o f th e extrac tint o aga s chromatograp h operate d unde rth e followin g conditions : Column : 6 f

tX V s i n stainles s stee l containin g 1 0 percen tOV-10 1 o n 100/12 0 Supelcoport . Carrie rGas : Heliu m a tarat e o f 3 0 ml/min . Detector : Flam e ionizatio n detecto r

operate d a tasensitivit y o f 4 X 10

—" A / mV . Injectio n PortTemperature : 25 0 °C . Detecto rTemperature : 30 5 °C . Ove n Temperature : 3 0 ° C fo r4 min ; programme d t o ris e a t4 0 °C/mi n unti l i t reache s 25 0 °C ; return t o 3 0 ° C afte r1 7 minutes . Compar e th e result s o f

th e analysi s t o th e result s from th e referenc e solution . Prepar e th e referenc e solutio n b y injectio n 2. 5 /i l o f methylen e chlorid e int o 10 0 ml o f toluene . Thi s correspond s t o 10 0 jtg o f methylen e chlorid e pe rg o f

adsorbent . Th e maximu m acceptabl e concentratio n i s 100 0 fig/ g o f adsorbent . I

f th e adsorben texceed s thi s level , dryin g mus tb e continue d unti l th e exces s methylen e chlorid e i s removed . 3.1.2. 4 Storage . Th e adsorben tmus tb e use d withi n 4 week s o f cleaning . Afte r cleaning , i tma y b e store d i n awid e mouth ambe rglas s containe rwit h aTeflon-line d ca p o rplace d i n on e o f

th e glas s adsorben t module s tightl y seale d wit h glas s stoppers . I f precleane d adsorben ti s purchase d i n seale d containers , i tmus tb e use d withi n 4 week s afte rth e sea l i s broken . 3.1. 3 Glas s Wool . Cleane d b y sequentia l immersio n i n thre e aliquot s o f methylen e chloride , drie d i n a11 0 ° C oven , an d store d i n amethylen e chloride-washe d glas s jarwit h a Teflon-line d scre w cap . 3.1. 4 Water . Deionize d distille d an d store d i n amethylen e chloride-rinse d glas s containe rwit h aTeflon-line d scre w cap . 3.1. 5 Silic aGel . Indicatin g type , 6 t o 1 6 mesh . I f previousl y used , dr

y a t17 5 ° C (35 0 °F) fo rtw o hours . Ne w silic age l ma y b e use d a s received . Alternatel y othe rtype s o f desiccant s (equivalen to rbetter ) ma y b e used , subjec tt o th e approva l o f th e Administrator . 3.1. 6 Chromi cAci d Cleanin g Solution . Dissolv e 2 0 g o f

sodiu m dichromat e i n 1 5 m l o f water , an d the n carefull y ad d 40 0 m l o f concentrate d sulfuri cacid . 3. 2 Sampl e Recovery . 3.2. 2 Acetone . Pesticid e quality . 3.2. 2 Methylen e Chloride . Pesticid e qualtity . 3.2. 3 Toluene . Pesticid e quality . 3. 3 Analysis . 3.3. 1 Potassiu m Hydroxide . AC S grade , 2 - percen t(weight/volume ) i n water . 3.3. 2 Sodiu m Sulfate . Granulated , reagen t grade . Purif

y prio rt o us e b y rinsin g wit h methylen e chlorid e an d ove n drying . Stor e th e cleane d materia l i n aglas s containe rwit h aTeflon-line d scre w cap . 3.3. 3 Sulfuri cAcid . Reagen tgrade . 3.3. 4 Sodiu m Hydroxide . 1. 0 N . Weig h 4 0 g o f sodiu m hydroxid e int o a1-lite rvolumetri c flask . Dilut e t o 1 lite rwit h water . 3.3. 5 Hexane . Pesticid e grade . 3.3. 6 Methylen e Chloride . Pesticid e grade . 3.3. 7 Benzene . Pesticid e Grade . 3.3. 8 Ethy l Acetate . 3.3. 9 Methanol . Pesticid e Grade . 3.3.1 0 Toluene . Pesticid e Grade . 3.3.1 1 Nonane . Pesticid e Grade . 3.3.1 2 Cyclohexane . Pesticid e Grade . 3.3.1 3 Basi cAlumina . Activit y grad e 1 , 100-20 0 mesh . Prio rt o use , activat e th e alumin ab y heatin g fo r1 6 hour s a t13 0 ° CP.1 0



### Federa l Registe r

/'Vol
. 56 , No
. 3 0 /Wednesday , Februar y 13 , 199 1 / : Rule s an dRegulation s 576 5 befor e use . Store i n adesiccator
. Pre

activate dalumin ama

y b e purchase dfro

ma supplier an dma y b e use da s received
. 3.3.1 4 Silic aGel
. Bio-Sil A 100-200 mesh
. Prior to use , activat e th e silic agel b y heatin g fo r at leas t 3 0 minute s a t

180 °C
. Afte

r cooling , rins e th e silic agel sequentiall y wit h methano l an dmethylen e chloride
. Hea t th e rinse dsilic agel at

5 0 °C fo r 1 0 minutes , the n increas e th e temperatur e graduall y t o 180 ° C over 2 5 minute s an dmaintai n i t at thi s temperatur e fo

r 9 0 minutes
. Cool at

roo m temperatur e an dstor e i n aglas s containe r wit haTeflon-line dscre w cap . 3.3.1 5 Silic aGe l Impregnate dwit h
. Sulfuri c Acid
. Combin e 10 0 g o f silic agel wit

h 4 4 g o f concentrate dsulfuri c aci din ascre w cappe dglas s bottl e an dagitat e thoroughly
. Dispers e th e solid s wit

hastirrin g ro dunti l a unifor mmixture i s obtained
. Store th e mixture i n aglas 3 containe r wit haTeflon

line dscre w cap . 3.3.1 8 Silic aGel Impregnate dwit h SodiumHydroxide
. Combin e 3 9 g o f 1 N , sodiumhydroxid e wit

h10 0 g o f silic agel i n a scre w cappe dglas s bottl e an dagitat e thoroughly
. Dispers e solid s withastirrin g ro d unti l aunifor

mmixture i s obtained
. Store th e mixture .i n glas s containe r

wit haTeflon-line d scre w cap . 3.3.1 7 Carbon/Celite
. Combin e 10. 7 g o f AX-2 1 carbo n wit

h12 4 g o f Celite 54 5 i n a 250-m l glas s bottl e wit

haTeflon-line dscre w cap . Agitat e th e mixture thoroughl y unti l a unifor mmixture i s obtained
. Store i n th e glas s container
. 3.3.1 8 Nitrogen
. Ultr ahighpurity
. 3.3.1 9 Hydrogen
. Ultrahighpurity
. 3.3.2 0 Interna l Standar dSolution
. Prepar e astoc k standar dsolutio n containin g th e isotopicall y labelle dPCDD' s an dPCDF' s a t th e concentration s show n i n Tabl e 1 unde r th e headin g "Internal'Standards " i n 1 0 m l o f nonane . 3.3.2 1 Surrogate Standar dSolution
. Prepar e astoc k

standar dsolutio n containin g th e isotopicall y labelle dPCDD' s an dPCDF s at Ih e concentration s show n i n Tabl e 1 unde r Ih e headin g "Surrogate Standards " i n 1 0 m l o f nonane . 3.3.2 2 Recover

y Standar dSolution
. Prepar e astoc k

standar dsolutio n containin g the isotopicall y labelle dPCDD' s an dPCDF' s at th e concentration s show n i n Tabl e 1 unde r th e headin g "Recover

y Standards " in 1 0 .m

l o f nonane . 4. Procedure 4. 1 .Sampling
. Th e complexit y o f thi s metho di s suc hthat,,i n orde r t o obtai n reliabl e results, tester s shoul db e traine dan d experience dwithth e tes t

procedures
. 4.1. 1 Pretes t

Preparation
. 4.1.1. 1 Cleanin g Glassware
. All glas s component s *o

f th e trai n upstreamo

f an d includin g th e adsorben t

.module , shal l b e cleane da s describe di n sectio n 3 A o f th e "Manual o

f Analytica l Method s fo

r th e Analysi s o

f Pesticide s i n Human an d Environmental Samples. " Special car e shal l b e devote dt o th e removal o f residua l silicon e greas e sealant s o n groun dglas s connection s o f use dglassware
. Any residu e shal l b e remove dt y soakin g th e glasswar e for severa l hour s i n achromi c aci dcleanin g .solutio n prio r t o cleanin g a s describe dabove
. 4.1.1. 2 Adsorben t Trap
. Th e trap s mus t

b e loade di n aclean are at o avoi d contamination
. The y ma

y not b e loade din th e field. Fill atra p wit

h2 0 t o 4 0 g o f XAD-2
. Follo w th e XAD- 2 withglas s woo l an d tightly cap bot

hend s o f th e trap
. Ad d10

0 /i l o f th e surrogat e standar dsolutio n (sectio n 3.3.21 } t o eac htrap
. 4.1.1. 3 Sampl e Train
. It

i s suggeste dtha t al l component s b e maintaine daccordin g t o th e procedur e describe di n APTD-0578
. 4.1.1. 4 Silic aGel
. Weighsevera l 20 0 to 30 0 g portion s o

f silic agel in a n ai r

tight containe r t o th e neares t

0. 5 g . Recordth e tota l weight

o f th e silic age l plu s container , o n eac hcontainer
. A s a n alternative , th e silic agel may b e weighe ddirectl y i n it s impinger o r samplin g holde r

jus t prio r t o sampling
. 4.1.1. 5 Filter
. Chec k

eac hfilter

agains t ligh t for irregularitie s an dflaw s o r pinhol e leaks
. Pac k

th e filter s fla

t i n aclean glas s container
. 4.1. 2 Preliminary Determinations
. Same a s sectio n 4.1. 2 o

f Metho d5
. 4.1. 3 Preparatio n o

f Collectio n Train
. 4.1.3. 1 During preparatio n an dassembl y o f th e samplin g train , kee p al l trai n opening s wher e contaminatio n ca n enter , seale dunti l jus t prio r t o assembl y o r

unti l samplin g i s about"to begin
. Note : D o no t

us e sealan t

greas e i n assemblin g th e train
. 4.1.3. 2 Plac e approximatel y 10 0 m l o f wate r in th e secon dan dthirdimpingers , leav e th e firs t

an dfourt himpinger s empty , an dtransfe r

approximatel y 20

0 t o 30 0 g o f preweighe dsilic agel iro mit s containe r t o th e fift himpinger
. 4.1.3. 3 Plac e th e silic agel containe r i n a clean plac e fo

r late r us e i n th e sampl e recovery . Alternatively , th e weigh t o f th e silic agel plu s impinger

may b e determine dt o th e neares t

0. 5 g an drecorded
. 4.1.3. 4 Assembl e th e trai n a s show n in Figur e 23-1
. 4.1.3. 5 Tur n o n th e adsorben t modul e an d condense r coi l recirculatin g pum

p an dbegi n monitorin g th e adsorben t

modul e .ga s entry temperature
. Ensure prope r sorben t temperatur e ga s entry temperatur e before proceedin g an dbefore samplin g i s initiated
. It i s extremel y importan t

tha t the'Xu\D- 2 adsorben t resi n temperatur e neve r

excee d5 0 °C .becaus e thermal decompositio n wil l occur . During testing , th e XAD- 2 temperatur e mus t no t excee d2 0 °C fo r efficien t captur e o

f th e PCDD' s an dPCDFs
. .4.1.4 Leak-Check

Procedure
. Same a s Metho d5 , sectio n 4.1.4
. 4.1. 5 Sampl e Trai n Operation
. Same a s Metho d5 , sectio n 4.1.5
. 4. 2 Sampl e Recovery
. Prope r cleanu p procedur e begin s a s soo n a s th e prob e i s remove dfro

mth e stac k

at th e en do f th e samplin g period
. Seal th e nozzl e en do f th e samplin g proh e wit

hTeflo n tap e o r

aluminum foil
. Whe n th e prob e can b e safel y handled , wip e of f al l externa l particulat e matte r nea r th e ti p o f th e probe
. Remov e th e prob e fro m the trai n an dclos e of

f bothend s wit

h aluminumfoi

LSeal of f th e inle t t o th e trai n wit hTeflon tape , agroun dglas s cap , o r aluminu mfoil
. Transfe r th e prob e an dimpinger

assembl y t o th e cleanu p area . Thi s are ashal l b e clea n an denclose ds o tha t

th e chance s o

f losin g o r contaminatin g th e sampl e ar e minimized
. Smoking , whic hcoul dcontaminat e th e sample , shal l no t

b e allowe di n th e cleanu p area . Inspec t th e trai n prio r

t o an ddurin g disassembl y an dnot e an y abnorma l conditions , e.g. , broke n filters, colore d impinger liquid , etc
. Trea t

th e sample s a s follows : 4.2. 1 Containe r

No
. 1
. Either

sea l th e filter holde r o r carefully remove th e filter fromth e filter holde r an dplac e it

in it s identifie d container
. Us e apai r

o f cleane dtweezer s t o handl e th e filter. I

f it i s necessar y t o foldth e filter , d o s o suc htha t

th e particulat e cak e i s insid e th e fold
. Carefully transfe r t o th e containe r an y particulat e matte r

an dfilter fibers whic hadher e t o th e filter holde r gasket , b y usin g adr

y inert bristl e brus han d asharp-edge dblade
. Sea l th e container
. 4.2. 2 Adsorben t

Module
. Remov e th e modul e fro

mth e train , tightly cop bot hends , labe l it , cover

wit haluminu mfoil , an dstor e i t o n ic e fo r transport t o th e laboratory
. 4.2. 3 Containe r

No
. 2
. Quantitativel y recove r materia l deposite di n th e nozzle , prob e transfer

lines , th e front

hal f o f th e filter holder , an dth e cyclone , i

f used , first, b y brushin g whil e rinsin g thre e time s eac hwit h aceton e an dthen , b y rinsin g th e prob e thre s time s wit hmethylen e chloride
. Collec t al l th e rinse s in Containe r

No
. 2
. Rins e th e bec k

hal f o f th e filter holde r thre e time s withacetone
. Rins e th e connectin g lin e betwee n th e filter

an dth e condense r

thre e time s wit hacetone
. Soa

k th e connectin g lin e wit hthre e separat e portion s O f methylen e chlorid e fo

r 5 minute s each
. I

f usin g a separat e condense r

an dadsorben t

trap , rins e th e condense r

in th e sam e manne r

a s th e connectin g line
. Collec t

al l th e rinse s i n Containe r No
. 2 an dmar

k th e leve l o

f th e liqui do n th e container
. 4.2. 4 Containe r

No
. 8
. Repeat

th e methylen e chloride-Tinsing describe din Section4.2. 3 usin g toluen e a s th e rins e solvent
. Collec t

th e rinse s in Containe r

No
. 3 an dmar k th e leve l o

f th e liqui don-th e container
. 4.2. 5 Impinge

r Water
. Measur e th e liqui d in th e firs t thre e impinger s t o withi n .± 1 m l b y usin g agraduate dcylinde r o r b y weighin g it t o withi n ±0: 5 g b y usin g abalance
. Record th e volume or

weight o f liqui dpresent
. Thi s informatio n i s require dt o calculat e th e moisture conten t

o f th e effluen

t gas . Discar dth e liqui dafter

measurin g an d recordin g th e volume o r

weight
. 4:2. 7 Silic aGel
. Note th e colo r o f th e indicatin g silic agel to determin e i f i t ha s bee n completel y spen t

an dmake amentio n o f it s condition
. Transfe r

the silic agel fro

m th e fift himpinger

to it s original containe r

an d seal
. 5. Analysis All,glasswar e shal l b e cleane da s describe din sectio n 3 A o

f th e "Manue l o

f Analytica l Method s fo

r th e Analysi s o

f Pesticide s i n Human an dEnvironmental Samples. " Al l sample s mus t b e extracte dP.1 1 

### 576 8 Federal Registe r/Vol . 56 , No
. 3 0 / Wednesday,-
. Februar y 13 , 199,1; / Rule s and : Regulation s withi n 3 0 day s o

f collectio n an danalyze d withi n 4 5 day s o

f extraction
. 5. 1 Sampl e Extraction
. 5.1. 1 Extractio n System
. Plac e a n extractio n thimbl e (sectio n 2.3.4) , 1 g o f silic a gel , an daplu g o

f glas s woo l into th e Soxhle t apparatus , charg e th e apparatu s wit htoluene , an dreflux fo

r aminimumo

f 3 hours
. Remov e th e toluen e an ddiscar dit , bu t retai n th e silic agel
. Remov e th e extractio n thimbl e fro mth e extractio n syste man dplac e i t i n a glas s beake r

t o catc hth e solven t

rinses. 5.1. 2 Containe r

No
. 1 (Filter)
. Transfe r

th e content s directl y t o th e glas s thimbl e o f th e extractio n syste man dextrac t the m simultaneousl y withth e XAD- 2 resin
. 5.1. 3 Adsorben t

Cartridge
. Suspen dth e adsorben t modul e directl y over

th e extractio n thimbl e i n th e beake r

(Se e sectio n 5.1.1)
. Th e glas s fri t o f th e modul e shoul db e in th e up position
. Usin g aTeflo n squeez e bottl e containin g toluene , flushth e XAD- 2 int o th e thimbl e ont o th e be do

f cleane dsilic agel
. Thoroughl y rins e th e glas s modul e catchin g th e rinsing s i n th e beake r

containin g th e thimble
. I f th e resi n i s wet , effectiv e extractio n ca n b e accomplishe db y loosel y packin g th e resi n i n th e thimble
. Ad dth e XAD- 2 glas s woo l plu g int o th e thimble
. 5.1.4 Containe r

No
. 2 (Aceton e an d Methylen e Chloride)
. Concentrat e th e sampl e t o avolume o

f abou t 1- 5 m l usin g th e rotar y evaporato r

apparatus , a t

atemperatur e o

f les s tha n 3 7 °C
. Rins e th e sampl e containe r thre e time s wit

hsmal l portion s o

f methylen e chlorid e an dad dthes e t o th e concentrate d solutio n an dconcentrat e further t o nea r dryness
. Thi s residu e contain s particulat e matte r remove di n th e rins e o

f th e trai n prob e an dnozzle
. Ad dth e concentrat e t o th e filter an dth e XAD- 2 resi n i n th e Soxhle t apparatu s describe di n sectio n 5.1.1
. ' 5.1. 5 Extraction
. Ad d10

0 ji l o f th e interna l standar dsolutio n (Sectio n 3.3.20 ) t o th e extractio n thimbl e containin g th e content s o

f th e adsorben t

cartridge , th e content s o

f Containe r

No
. 1 , an dth e concentrat e fromsectio n 5.1.4
. Cover th e content s o

f th e extractio n thimbl e wit hth e cleane dglas s woo l plu g t o preven t th e XAD

2 resi n from floating int o th e solven t reservoi r o f th e extractor
. Plac e th e thimbl e in th e extractor, an dad dth e toluen e containe din th e beake r

t o th e solven t

reservoir
. Pour additiona l toluen e t o fill th e reservoi r approximatel y 2/ 3 full
. Ad dTeflon boilin g chip s an dassembl e th e apparatus
. Adjus t th e hea t sourc e t o caus e th e extracto r to cycl e thre e time s pe r

hour
. Extrac t

th e sampl e fo

r 1 6 hours
. Afte

r extraction , allo w th e Soxhle t t o cool
. Transfe r

th e toluen e extrac t

an d thre e 10-m

l rinse s t o th e rotar y evaporator
. Concentrat e th e extrac t

t o approximatel y 1 0 ml
. At thi s poin t th e analys t

ma y choos e to spli t th e sampl e i n half

. I f so , spli t th e sample , stor e on e half

fo r futur e use , an danalyz e th e othe r accordin g t o th e procedure s in section s 5. 2 an d5.3
. I

n eithe r case , us e anitroge n evaporativ e concentrato r

to reduc e th e volume o f th e sampl e bein g analyze dt o nea r dryness
. Dissolv e th e residu e i n 5 m l o f hexane
. 5.1. 6 Containe r

No
. 3 (Toluen e Rinse)
. Ad d10 0 fi l o f th e Interna l Standar dsolutio n (sectio n 3.3.2] to th e content s o f th e container
. Concentrat e th e sampl e to a volume o f abou t 1- 5 m l usin g th e rotar y evaporato r

apparatu s at

atemperatur e o

f les s tha n 3 7 °C
. Rins e th e sampl e containe r apparatu s at

atemperatur e o

f les s tha n 3 7 °C
. Rins e th e sampl e containe r thre e time s with smal l portion s o

f toluen e an dad dthes e t o th e concentrate dsolutio n an dconcentrat e further t o nea r dryness
. Analyz e th e extrac t separatel y accordin g t o th e procedure s i n section s 5. 2 an d5.3 , bu t

concentrat e th e solutio n in arotary evaporato r apparatu s rathe r tha n anitroge n evaporativ e concentrator
. 5. 2 Sampl e Cleanu p an dFractionation
. 5.2. 1 Silic aGe

l Column
. Pac k

on e en do

f a glas s column , 2

0 m mx 23 0 mm , withglas s wool
. Ad din sequence , 1 g silic agel , 2 g o f sodiu mhydroxid e impregnate dsilic agel , 1 g silic agel , 4 g o

f acid-modifie dsilic agel , an d1 g o f silic agel
. Was hth e colum n with3 0 m

l o f hexan e an ddiscar dit
. Ad dth e sampl e extrac t dissolve di n 5 m

l o f hexan e to th e colum n wit htw o additiona l 5-m

l rinses
. Elute th e colum n wit ha n additiona l 90 m

l o f hexan e an dretai n th e entir e eluate
. Concentrat e thi s solutio n t o avolume o f abou t 1 m l usin g th e nitroge n evaporativ e concentrato r

(sectio n 2.3.7)
. 5.2. 2 Basi c Alumin aColumn
. Shorte n a 25-m l disposabl e Pasteu r

pipette t o abou t

1 6 ml
. Pac k th e lowe r sectio n withglas s woo l an d1 2 g o

f basi c alumina
. Transfe r

th e concentrate dextrac t

fromth e silic agel colum n t o th e to p o

f th e basi c alumin a colum n an delut e th e colum

n sequentiall y wit h12 0 m l o f 0. 5 percen t

methylen e chlorid e i n hexan e followe db y 12

0 m l o f 3 5 percen t methylen e chlorid e in hexane
. Discar dth e firs t 12 0 m l o f eluate
. Collec t

th e secon d12

0 m l o f eluat e an dconcentrat e i t t o abou t 0. 5 m l usin g th e nitroge n evaporativ e concentrator
. 5.2. 3 AX-2 1 Carbon/Celit e 545 Column
. Remov e th e botto n 0. 5 in
. fro mth e ti p o

f a9

- m l disposabl e Pasteu r

pipette
. Insert

aglas s fiber filte r dis k in th e to p o

f th e pipette 2. 5 c

m fromth e constriction
. Ad dsufficien t carbon / celit e mixture t o for

ma2 c mcolumn
. To p wit haglas s woo l plug
. I

n some case s AX-21
. carbo n fine s ma

y was hthroug hth e glas s woo l plu g an dente r

th e sample
. Thi s ma

y b e prevente db y addin g acelit e plu g t o th e exi t en do f th e column
. Rins e th e colum n in sequenc e wit

h2 m l o f 5 0 percen t

benzen e in ethy l acetate , 1 m

l o f 5 0 percen t

methylen e chlorid e in cyclohexane , an d2 m l o f hexane
. Discar dthes e rinses
. Transfe r th e concentrat e i n 1 m

l o f hexan e fro

mth e basi c alumin acolum

n to th e carbon/celit e colum n alon g wit h1 m l o f hexan e rinse
. Elute th e colum n sequentiall y wit

h2 m l o f 5 0 percen t methylen e chlorid e in hexan e an d2 m l o f 5 0 percen t benzen e in ethy l acetat e an ddiscar d thes e eluates
. Inver

t th e colum

n an delute in th e revers e directio n wit

h1 3 m l o f toluene
. Collec t thi s eluate
. Concentrat e th e eluat e in arotary evaporato r

at 5 0 °C t o abou t

1 ml
. Transfe r th e concentrat e t o aReacti-vial usin g atoluen e rinse an dconcentrat e t o a volume o f 20 0 fi l usin g astrea mo

f Na
. Store extract s at

roo mtemperature , shielde dfrom light , unti l th e analysi s i s performed
. 5. 3 Analysis
. Analyz e th e sampl e wit ha ga s chromatograp hcouple dt o amas s spectromete r

(GC/MS ) usin g th e instrumenta l parameter s i n section s 5.3. 1 an d5.3.2
. Immediatel y prio r

t o analysis , ad da2

0 *x l aliquo t

o f th e Recover

y Standar dsolutio n fro mTabl e 1 t o eac hsample
. A 2 -i l aliquo t o f th e extrac t

i s injecte dint o th e GC
. Sampl e extract s ar e firs t

analyze dusin g th e DB- 5 capillary colum

n t o determin e th e concentratio n o

f eac hisomer

o f PCDD' s an d PCDF' s (tetra-throug hocta-)
. I f tetra
chlorinate ddibenzofuran s ar e detecte din thi s analysis , the n analyz e anothe r aliquo t o f ' th e sampl e in aseparat e run , usin g th e DB

22 5 colum n t o measur e th e 2,3,7, 8 tetra-chlor o dibenzofuran isomer
. Othe r colum n system s may b e used , provide dthat th e use r i s abl e t o demonstrat e usin g calibratio n an d performanc e check s tha t

th e colum

n syste m i s abl e to mee t

th e specification s o

f sectio n 6.1.2.2
. 5.3. 1 Gas Chromatograp hOperatin g Conditions
. 5.3.1. 1 Injector
. Configure dfo r capillary column , splitless , 250°C
. 5.3.1. 2 Carrie r

Gas
. Helium , 1- 2 ml/min
. 5.3.1. 3 Oven
. Initiall y a t

150°C
. Rais e b y a t leas t 40°C/mi n t o 190° C an dthe n at 3"C / min up t o 300°C
. 5.3. 2 HighResolutio n Mas s Spectrometer
. 5.3.2. 1 Resolution
. 1000

0 m/e
. 5.3.2. 2 Ionizatio n Mode
. Electro n impact
. 5.3.2. 3 Sourc e Temperatur e 250°C
. 5.3.2. 4 Monitorin g Mode
. Selecte dio n monitoring
. A lis t

o f th e variou s ion s t o b e monitore di s summarize di n Tabl e 3
. 5.3.2. 5 Identificatio n Criteria
. Th e following identificatio n criteri ashal l b e use d fo r th e characterizatio n o

f polychlorinate d dibenzodioxin s an ddibenzofurans
. 1
. Th e integrate dion-abundanc e rati o (M/ M+ 2 o r M+2/M+4 ) shal l b e withi n 1 5 percen t o f th e theoretica l value
. Th e acceptabl e ion-abundanc e rati o range s fo r th e identificatio n o

f chlorine-containin g compound s ar e give n in Tabl e 4
. 2
. Th e retentio n time fo

r th e analyte s mus t b e withi n 3 second s o

f th e correspondin g 1 3 C-labele dinterna l standard , surrogat e o r alternat e standard
. 3
. Th e monitore dions , show n in Tabl e 3 fo r agiven analyte , shal l reac hthei r maximum withi n 2 second s o

f eac hother
. 4
. Th e identificatio n o

f specifi c isomer s tha t d o no t hav e correspondin g 1 3 C-labele d standard s i s don e b y compariso n o f th e relativ e retentio n tim

e (RRT ) o f th e analyt e t o th e neares t

interna l standar dretentio n time wit hreferenc e (i.e. , withi n 0.00 5 RR T units ) t o th e comparabl e RRT s foun di n th e continuin g calibration
. 5
. Th e signal to nois e rati o fo r al l monitore dion s mus t

b e greate r

tha n 2.5
. 6
. Th e confirmatio n o

f 2 , 3 , 7 , 8-TCDD an d 2 , 3 , 7 , 8-TCDFshal l satisf y al l o f th e abov e identificatio n criteria
. 7
. For th e identificatio n o

f PCDFs , n o signal ma y b e foundin th e correspondin g PCDP Echannels
. 5.3.2. 8 Quantification
. Th e peak area s fo r th e tw o ion s monitore dfo r eac hanalyt e ar e summe dto yiel dth e tota l respons e fo r eac h analyte
. Eac hinterna l standar di s use dt o quantif y th e indigenou s PCDD' s or PCDF' s in it s homologou s series
. For example , th e 1 3 C u-2,3,7,8-tetr achlorinate ddibenzodioxi n i s use dt o calculat e th e concentration s o f al l othe r tetr achlorinate disomers
. Recoverie s o f th e tetra
- an dpenta
- interna l standard s ar eP.1 2



### ""*- . Ffedera

l Registe r*/

- Vdl
. \56, ! 

### No
. 30 '

. / • Wednesday ; •'February

- J13,1991 ' / Rifle s arid ; Regulation s 376 7
calculate dusin g th e 1 3 C i2-l,2,3,4-TCDD
. Recoverie s o f

th e hexa

- throug hocta
- interna l standard s ar e calculate dusin g aC i2 — 1,2,3,7,8,9-HxCDD
. Recoverie s o f th e surrogat e standard s ar e calculate dusin g th e correspondin g homolo g fromth e interna l standard
. ft Calibration Sam e a s Metho d5 wit hth e followin g additions
. 6. 1 GC/M S System
. 6.1. 1 Initia l Calibration
. Calibrat e th e GC / M S syste musin g th e se t o f five standard s show n i n Tabl e 2
. Th e relativ e standar d deviatio n fo r

th e mea n respons e facto r from eac ho f th e unlabele danalyte s (Tabl e 2 ) an d o f th e internal , surrogate , an dalternat e standard s shal l b e les s tha n o r equa l t o th e value s i n Tabl e 5
. Th e signa l t o nois e rati o fo r th e G C signa l presen t

i n ever y selecte dio n curren t profil e shal l b e greate r tha n o r equa l t o 2.5
. Th e io n abundanc e ratio s shal l b e withi n th e contro l limit s i n Tabl e 4
. 6.1. 2 Dail y Performanc e Check
. 6.1.2. 1 Calibratio n Check
. Injec t o n fil.o f solutio n Numbe r

3 fro mTabl e 2
. Calculat e th e relativ e respons e facto r (RRF ) fo r

eac h compoun dan dcompar e eac hRR Ft o th e correspondin g mea n RR Fobtaine ddurin g th e initia l calibration
. Th e analyze r performanc e i s acceptabl e if

th e measure dRRF' s fo r th e labele dan dunlabele dcompound s fo r th e dail y ru n ar e withi n th e limit s o f th e mea n value s show n i n Tabl e 5
. I n addition , th e ion

- . abundanc e ratio s shal l b e withi n th e allowabl e contro l limit s show n i n Tabl e 4
. 6.1.2. 2 Colum n Separatio n Check
. Injec t a solutio n o f

amixtur e o f

PCDD' s an dPCDF' s tha t document s resolutio n betwee n 2,3,7,8

- TCD D an dothe r

TCD D isomers
. Resolutio n i s define da s avalle y betwee n peak s tha t i s les s tha n 2 5 percen t

o f th e lowe r

o f th e tw o peaks
. Identif y an drecor dth e retentio n tim e window s fo r

eac hhomologou s series
. Perfor masimila r

resolutio n chec k

o n th e confirmatio n colum n t o documen t th e resolutio n betwee n 2,3,7, 8 TCD Fan dothe r TCD Fisomers
. 6. 2 Loc k

Channels
. Se t

mas s spectromete r loc k channel s a s specifie di n Tabl e 3
. Monito r th e qualit y contro l chec k channel s specifie d i n Tabl e 3 t o verif

y instrumen t

stabilit y durin g th e analysis
. 7. Quality Control 7. 1 Samplin g Trai n Collectio n Efficienc y Check
. Ad d10 0 fi l o f

th e surrogat e standard s i n Tabl e 1 t o th e absorben t cartridg e o f

eac h trai n befor e collectin g th e fiel dsamples
. 7. 2 Interna l Standar dPercen t Recoveries
. A grou p o f

nin e carbo n labele dPCDD' s an d PCDF' s representing , th e terra-throug h octachlorinate dhomologues , i s adde dt o ever y sampl e prio r

t o extraction
. Th e rol e o f th e interna l standard s i s t o quantif y th e nativ e PCDD' s an dPCDF' s presen t i n th e sampl e a s wel l a s t o determin e th e overal l metho defficiency
. Recoverie s o f th e interna l standard s mus t

b e betwee n 4 0 t o 13 0 percen t fo r th e tetra-throug hhexachlorinate d compound s whil e th e rang e i s 2 5 t o 13 0 percen t fo r th e highe r

hepta

- an d octachlorinate dhomologues
. 7. 3 Surrogat e Recoveries
. Th e fiv e surrogat e compound s i n Tabl e 2 ar e adde dt o th e resi n i n th e adsorben t samplin g cartridg e befor e th e sampl e i s collected
. Th e surrogat e recoverie s ar e measure drelativ e t o th e interna l standard s an dar e ameasur e o f collectio n efficiency
. The y ar e no t use dt o measur e nativ e PCDD' s an dPCDFs
. Al l recoverie s shal l b e betwee n 7 0 an d13 0 percent
. Poo r

recoverie s fo r

al l th e surrogate s ma y b e a n indicatio n o f breakthroug hi n th e samplin g train
. I

f th e recover y o f

al l standard s i s belo w 7 0 percent , th e samplin g run s mus t

b e repeated
. A s a n alternative , th e samplin g run s d o no t

hav e t o b e repeate dif th e final result s ar e divide db y th e fractio n o f surrogat e recovery . Poo r recoverie s o f isolate dsurrogat e compound s shoul dno t b e ground s fo r

rejectin g a n entir e se t

o f th e samples
. 7. 4 Toluen e Q A Rinse
. Repor t th e result s o f th e toluen e Q A rins e separatel y fro mth e tota l sampl e catch
. D o no t ad di t t o th e tota l sample
. 8. Quality Assurance 8. 1 Applicability
. Whe n th e metho di s use dt o analyz e sample s t o demonstrat e complianc e wit hasourc e emissio n - regulation , a n audi t

sampl e mus t

b e analyzed , subjec t t o availability
. 8. 2 Audi t

Procedure
. Analyz e a n audi t sampl e wit heac hse t

o f complianc e samples
. Th e audi t

sampl e contain s tetr athroug hoct a isomer s o f

PCD D an dPCDF
. Concurrently , analyz e th e audi t

sampl e an dase t

o f complianc e sample s i n th e sam e manne r t o evaluat e th e techniqu e o f th e analys t

an dth e standard s preparation
. Th e sam e analyst , analytica l reagents , an danalytica l syste m shal l b e use dbot hfo r

th e complianc e sample s an dth e EP A audi t sample
. 8. 3 Audi t

Sampl e Availability
. Audi t sample s wil l b e supplie donl y t o enforcemen t agencie s fo r

complianc e tests
. Th e availabilit y o f

audi t sample s ma y b e obtaine d b y writing : Sourc e Tes t Audi t Coordinato r (MD-77B) , Qualit y Assuranc e Division , Atmospheri c Researc han dExposur e Assessmen t

Laboratory , U.S
. Environmenta l Protectio n Agency , Researc hTriangl e Park , N C 27711 , o r

b y callin g th e Sourc e Tes t Audi t Coordinato r

(STAC ) a t

(919 ) 541-7834
. Th e reques t fo r th e audi t

sampl e mus t

b e mad e a t leas t 3 0 day s prio r

t o th e schedule d complianc e sampl e analysis
. 8. 4 Audi t

Results
. Calculat e th e audi t sampl e concentratio n accordin g t o th e calculatio n procedur e describe di n th e audi t instruction s include dwit hth e audi t sample
. Fil l i n th e audi t

sampl e concentratio n an dth e analyst' s nam e o n th e audi t respons e for m include dwit hth e audi t instructions
. Sen d on e cop y t o th e EP A Regiona l Offic e o r th e appropriat e enforcemen t agenc y an da secon dcop y t o th e STAC
. Th e EP A Regiona l offic e o r th e appropriat e enforcemen t agenc y wil l repor t

th e result s o f

th e audi t

t o th e laborator y bein g audited
. Includ e thi s respons e wit hth e result s o f th e complianc e sample s i n relevan t

report s t o th e EP A Regiona l Offic e o r

th e appropriat e enforcemen t

agency . 9. Calculations Sam e a s Metho d5 , sectio n 6 wit hth e followin g additions
. 9. 1 Nomenclature
. A ai =Integrate dio n curren t o f th e nois e a t th e retentio n tim e o f

th e analyte
. A* cl =Integrate dio n curren t o f th e tw o ion s characteristi c o f

th e interna l standar di i n th e calibratio n standard
. A c U= Integrate dio n curren t o f th e tw o ion s characteristi c o f

compoun di i n th e jt h calibratio n standard
. A*dj=Integrate dio n curren t o f th e tw o ion s characteristi c o f

th e interna l standar di i n th e jt hcalibratio n standard
. Aci=Integrate dio n curren t o f th e tw o ion s characteristi c o f

surrogat e compoun di i n th e calibratio n standard
. A,=Integrate dio n curren t o f th e tw o ion s characteristi c o f

compoun di i n th e sample
. A*i=Integrate dio n curren t o f th e tw o ion s characteristi c o f

interna l standar di i n th e sample
. A re =Integrate dio n curren t o f th e tw o ion s characteristi c o f

th e recover y standard
. A,i=Integrate dio n curren t o f th e tw o ion s characteristi c o f

surrogat e compoun di i n th e sample
. C,=Concentratio n o f

PCD D o r

PCD Fi i n th e sample , pg/ M 3

. C T =Tota l concentratio n o f PCDD' s o r PCDF' s i n th e sample , pg/ M 3

. m c) =Mas s o f

compoun di i n th e calibratio n standar dinjecte dint o th e analyzer , pg . m„=Mas s of

recover y standar di n th e calibratio n standar dinjecte dint o th e analyzer , pg . m,i=Mas s of

surrogat e compoun di i n th e calibratio n standard , pg . RRFi=Relativ e respons e factor
. RRF„=Recover y standar drespons e factor
. RRF,=Surrogat e compoun drespons e factor
. 9. 2 Averag e Relativ e Respons e Factor
. 1 n Ad

j m* d RRF, = —2 n j= l A*d , m d Eq
. 23- 1

9. 3 Concentratio n o f

th e PCDD' s an d PCDFs
.

m /

A , Eq
. 23- 2 A| * RRF i V mBt d
9. 4 Recover y Standar dRespons e Factor
. A c i*m „ RRF„ = Eq
. 23- 3

A „ m d *
9. 5 Recover y o f

Interna l Standard s (R*). A, * m „ A „ RF „ m, * Eq
. 23- 4

9. 6 Surrogat e Compoun dRespons e Factor
.P.1 3 

### S|^8 8 Federa

l tRpgiste i /^Vo i 56, , No
. 3 0 /

,Wednesday t



### ffetaujaiy -1.3, .1-951 J

Rule s gn dRegulation s

RRF„ = Ad * m .

Atunva * Eq
. 23- 5
9. 7 Recover y o f

Surrogat e Compound s (R»)

- A„m, * A, * RRF , m , X100 % Eq
. 23- 6

9. 8 Minimu mDetectabl e Limi t (MDL)
.

MDL = 2. 5 A, ! m! *

Ad * RRF , Eq
. 23- 7

9. 9 Tota l Concentratio n o f PCDD' s an d PCDF' s i n th e Sample
.

n VuXr~ •

—lu j i = l Eq
. 23- 8 Agency
. Washingto n DC
. Decembe r 1984
. 2 5 P

2
. America n Societ y o f Mechanica l Engineers
. Analytica l Procedure s t o Assa y Stac k Effluen t Sample s an dResidua l Combustio n Product s fo r Polychlorinate d Dibenzo-p-Dioxin s (PCDD ) an d Polychlorinate dDibenzofuran s (PCDF)
. Prepare dfo r

th e U.S
. Departmen t

o f Energ y an dU.S
. Environmenta l Protectio n Agency
. Washington , DC
. Decembe r 1984
. 2 3 p . 3
. Thompson , J
. R
. (ed.)
. Analysi s o f Pesticid e Residue s i n Huma n an d Environmenta l Samples
. U.S
. Environmenta l Protectio n Agency
. Researc hTriangl e Park , N G1974
. 4
. Triangl e Laboratories
. Cas e Study : Analysi s o f

Sample s fo r

th e Presenc e o f

Tetr a Throug hOctachloro-p-Dibenzodioxin s an d Dibenzofurans
. Researc hTriangl e Park , NC
. 1988
. 2 6 p . 5
. U.S
. Environmenta l Protectio n Agency
. i Metho d8290—Th e Analysi s o f Polychlorinate dDibenzo-p-dioxi n an d Polychlorinate dDibenzofuran s b y High

Resolutio n Ga s Chromotography/High

Resolutio n Mas s Spectrometry
. In : Tes t Method s fo r

Evaluatin g Soli dWaste
. Washington , DC
. SW-846
. TABL E 1.—COMPOSITIO N O F TH E SAMPL E FORTIFICATIO N AN D RECOVER YSTAND
ARD S SOLUTION S An y PCDD' s o r

PCDF s tha t

ar e reporte da s nondetecte d(belo w th e MDL ) shal l b e counte da s zer o fo r

th e purpos e o f

calculatin g th e tota l concentratio n o f PCDD' s an dPCDF' s i n th e sample
. 10. Bibliography 1
. America n Societ y o f Mechanica l Engineers
. Samplin g fo r th e Determinatio n o f Chlorinate dOrgani c Compound s i n Stac k Emissions
. Prepare dfo r U.S
. Departmen t

o f Energ y an dU.S
. Environmenta l Protectio n

. TABL E 3.—ELEMENTA L COMPOSITION S AN D EXAC TMASSE S O F TH E ION S MONITORE D B Y HIG H RESOLUTIO N MAS S SPECTROMETR Y FO R PCDD' S AN D PCDF S Analyt e Interna l Standards : 1: C ls -2,3,7,8-TCD D l! C,2-1,2,3,7,8-PeCD D "C l 2-1,2,3,6,7,8-HxCD D "C»-1,2,3,4,6,7,8-HpCD D •*C 12-OCD D '. Concentra tio n (pg/|il )

•10 0 10 0 10 0 10 0 10 0 TABL E 1 .—COMPOSITIO N O F TH E SAMPL E

FORTIFICATIO N AN D RECOVER YSTAND
ARD S SOLUTIONS—Continue d

Analyte

I: C,2-2,3,7,8-TCD F - "C„-1,2,3,7,8-PeCD F „ •'Cii-1,2,3,6,7,8-HxCD F "Ci2-1,2,3,4,6,7,8-HpCD F Surrogat e Standards : sl Cl4-2,3,7,8-TCD D "Ci2-1,2,3,4,7,8-HxCDD.. , la Ci 2 -2,3,4,7,8-PeCD F •-Cia-1,2,3,4,7,8-HxCD F l 'Ci2-1,2,3,4,7,8,9-HpCD F Recover y Standards: . "C la -1,2,3,4-TCD D "C,2-1,2,3,7,8,9-HxCD D Concentratio n (pg/jd ) 10 0 10 0 10 0 10 0 10 0 10 0 10 0 10 0 10 0 50 0 50 0
TABL E 2.—COMPOSITIO N O F TH E INITIA L

CALIBRATIO N SOLUTION S

Compoun d

Alternate Standard : •*C,2- 1,2,3,7,8,9 - HxCDF „ Recover y Standards : "C l3 -1,2,3,4 - TCD D •-C.2- 1,2,3,7,8,9 - HxCD D Concentration s (pg/jiL ) Solutio n No . 1

2. 5

10 0
10 0 2

5

10 0
10 0 3

2 5

10 0
10 0 4

25 0

10 0
10 0 5

50 0

10 0
10 0

Descripto r No . 2

3 Accurat

e mass 292.982 5 303.901 6 305.898 7 315.941 9 317.938 9 319.896 5 321.893 6 327.884 7 330.979 2 331.936 8 333.933 9 339.859 7 341.856 7 351.900 0 353.897 0 355.854 6 357.851 6 367.894 9 369.891 9 375.836 4 409.797 4 373.820 8 375.817 8 383.863 9 385.861 0 389.815 7 391.812 7 392.976 0 Io n type

LOC K M M+ 2 M M+ 2 M M+ 2 M Q C M M+ 2 M+ 2 M+ 4 M+ 2 M+ 4 M+ 2 M+ 4 M+ 2 M+ 4 M+ 2 M+ 2 M+ 2 M+ 4 M M+ 2 M+ 2 M+ 4 LOC K . Elementa l compositio n CF „ Ci2Hu?

5 CluO C, 2 m*CT O

- a C,2H 4 "Ct 1 0 1 'C,sH4 M Cl3 ,1 CI O C, 2 H4*CIO , Ci,H 4 M CI. 3, a0 2 C,2H < "CUO . CF w *-C 12 H. M Clu.02 "CsHuaCTCIO j Ci2H 3 M CU ,7 CI O CaHs^Cla^Clj O "C,zH 3 'K,U"C\0 1 ^C 12 H>«CI 3M1 CI 2 0 C 1I H, M Cl s 37a0 2 C,2H, M CI, lr Cl20 2 "CuHjaCU'lCIO * "CHjKVWl * c„H, 3: ek*"ci o C, 2 H s MCl6S7CI O C 12 H 2 35CI 5 3, CI O c 1 2 H 2 M ciu s , ei 2 o ia C,2H! 31 CI« 0 1J Ci 2 H 2 »wei o C l 2 H 2 3 WC!0 2 CnHa'WCI-. a C,F „ Analyt e PF K TCD F TCD F TCD F (S ) TCD F (S ) TCD D TCD D TCD D (S ) PF K TCD D (S ) TCD D (S ) PECD F PeCD F PeCD F (S ) PeCD F (S ) PeCD D PeCD D PeCD D (S ) PeCD D (S ) HxCDP E HpCPD E HxCD F HxCD F HxCD F (S ) HxCD F (S ) HxCD D HxCD D PF KP.1 4



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TABL E 3.—ELEMENTA L COMPOSITION S AN D EXAC TMASSE S O F TH E ION S MONITORE D B Y HIG H RESOLUTIO N MAS S SPECTROMETR Y FO R PCDD' S AN D PCDF's—Continue d Descripto r No .

4 Accurat

e mass 401.855 9 403.852 9 445.755 5 430.972 9 407.781 8 409.778 9 417.825 3 419.822 0 423.776 6 425.773 7 435.816 9 437.814 0 479.716 5 430.972 9 441.742 8 443.739 9 457.737 7 459.734 8 469.777 9 471.775 0 513.677 5 442.972 8 Io n type

M+ 2 M+ 4 M+ 4 Q C M+ 2 M+ 4 M M+ 2 M+ 2 M+ 4 M+ 2 M+ 4 M+ 4 LOC K M+ 2 M+ 4 M+ 2 M+ 4 M+ 2 M+ 4 M+ 4 - Q C Elementa l compositio n

' a C, 2 H 2 M Ct l ' ,1 CI0 2 "CuHj'WCfe O 

### c-jH-^wa o C F „ CJH^WCI O C 12 H :w CI» sl Cl2 0 '•CSH-^CIT O "CuH'WCI O CIH^CIG'KJIO J CJH"CU S , CI 2 0 2 "CKH'WCIO: . "CnH'WCfeQ , CuH^WW ) CF, , C 1J S5 CI, sl CI O Cu'WCW D Cia'WCIO- ! Ci^le^CliO j '-WWCIO * •-WWCkQ . C,2 M CI, ; "CI 2 0 2 CloF] 7 Analyte HxCD D (S ) HxCD D (S ) OCDP E PF K HpCD F HpCD F HpCD F (S ) HpCD F (S ) HpCD D HpCD D HpCD D (S ) HpCD D (S ) NCPD E PF K OCD F OCD F OCD D OCD D OCD D (S ) OCD D (S ) DCDP E PF K (a ) Th e followin g nuclidi c masses were used : H = 1.00782 5 C = 12.00000 0 " C = 13.00335 5 F = 18.998 4 O = 15.99491 5 "C l = 34.96885 3 "T O = 36.96590 3 S —Labele d Standard Q C = Io n selecte d fo r monitorin g instrument stabilit y durin g th e GC/M S analysis . TABL E 4.—ACCEPTABL E RANGE S FO R ION
ABUNDANC E RATIO S O F PCDD' S AN D PCDF' S NO . O f chlorin e atom s 4 5 6 6 " 7 " 7 8 Io n type
M/M+ 2 M+2 /

. M+ 4 M+2 / M+ 4 M/M+ 2 M/M+ 2 M+2 / M+ 4 M+2 / M+ 4 Theo retica l rati o 0.7 7 1.55 1.2 4 0.5 1 0.4 4 1.04 0.8 9 Contro l limit

s Lowe r 0.6 5 1.3 2
• 1.05 0.4 3 0.3 7 0.8 8 0.7 6 Uppe r

0.8 9 1.78 1.43 0.5 9 0.5 1 1.2 0 1.02 •Use d only fo r "C-HxCDF . " Used only fo r 13 C-HpCDF . TABL E 5.—MINIMU M REQUIREMENT S FO R INITIA L AN D DAIL YCALIBRATIO N RE
SPONS E FACTOR S
Compoun d

Unlabele d Analytes : 2,3,7,8-TCD D 2,3,7,8-TCD F 1,2,3,7,8 - PeCD D 1,2,3,7,8 - PeCD F Relativ e response factors Initia l calibratio n RS D

2 5 2 5 2 5 ? 5 Dail y calibratio n % difference

2 5

2 5 2 5 2 5 TABL E 5.—MINIMU M REQUIREMENT S FO R INITIA L AN D DAIL YCALIBRATIO N RE
SPONS E FACTORS—Continue d
Compoun d
2,3,4,7,8 - PeCD F 1,2,4,5,7,8 - HxCD D 1,2,3,6,7,8 - HxCD D 1,2,3,7,8,9 - HxCD D 1,2,3,4,7,8 - HxCD F 1,2,3,6,7,8 - HxCD F 1,2,3,7,8,9 -

. HxCD F 2,3,4,6,7,8 - HxCD F 1,2,3,4,6,7,8 - HpCD D 1,2,3,4,6,7,8 - HpCD F OCD D OCD F Interna l Standards : • 3 C 12 -2,3,7,8 - TCD D ,3 C,2-1,2,3,7,8 - PeCD D 13 C l2 - 1,2,3,6,7,8 - HxCD D Relativ e response factors Initia l calibratio n RS D
2 5 2 5 2 5 2 5 2 5 2 5 2 5 2 5 2 5 2 5 2 5 3 0

2 5 3 0
2 5 Dail y calibratio n % difference
2 5

2 5 2 5 2 5 2 5 2 5 2 5 2 5 2 5 2 5 2 5 3 0

2 5 3 0
2 5 TABL E 5.—MINIMU M REQUIREMENT S FO R

INITIA L AN D

. DAIL YCALIBRATIO N RE
SPONS E FACTORS—Continue d
Compoun d

13 C, 2 - 1,2,3,4,6,7,8 - HpCD D > 3 C 12 -OCD D 13 C 12 -2,3,7,8 - TCD F 13 C,2-1,2,3,7,8 - PeCD F •**C, 2 - 1,2,3,6,7,8 - HxCD F"Cn1,2.3,4,6,7,8 - HpCD F Surrogat e Standards : 37 CU-2,3,7,8 - TCD D 13 C, 2 -2,3,4,7,8 - PeCD F * 3 C 12 - 1,2,3,4,7,8 - HxCD D 13 C, 2 - 1,2,3,4,7,8 - HxCD F • 3 C 12 - 1,2,3,4,7,8,9 - HpCD F Relativ e response factor

s Initia l calibratio n RS D

3 0 3 0 3 0 3 0
3 0
3 0

2 5 2 5
2 5
2 5
2 5 Dail y calibratio n % difference

3 0

3 0 3 0 3 0
3 0
3 0

2 5 2 5
2 5
2 5
2 5

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TABL E 5.—MINIMU M REQUIREMENT S FO R INITIA L AN D DAILYCALIBRATIO N RE
SPONS E FACTORS—Continue d
Compoun d

Alternate Standard ,3 C 12 - 1,2,3,7,8.9 - HxCD F Relativ e response factors Initia l calibratio n RS D

2 5 Dail y

calibratio n % difference

2 5

Metho d28—Determinatio n o f Hydroge n Chlorid e Emission s Fro mStationary Source s 1. Applicability, Principle, Interferences, Precision, Bias, and

Stability 1. 1 Applicability
. Thi s metho di s applicabl e fo

r determinin g hydroge n chlorid e (HCl ) emission s fro

mstationar y sources . 1.2 Principle
. An integrate dsampl e i s extracte dfro

mth e stac k

an dpasse dthroug h dilut e sulfuri c acid
. I

n th e dilute acid , th e HC l ga s i s dissolve dan dform s chlorid e (Cl" ) ions
. Th e Cl " i s analyze db y io n chromatograph y (IC)
. 1. 3 Interferences
. Volatil e material s whic hproduc e chlorid e ion s upo n dissolutio n durin g samplin g ar e obviou s interferences
. Anothe r likel y interferent

i s diatomi c chlorin e (Cl 2 ) ga s whic hreact s t o for mHC l an d hypochlordu s aci d(HOCl ) upo n dissolvin g i n water
. However , CI

2 ga s exhibit s alo w solubilit y i n wate r

an dth e us e o

f acidic , rathe r tha n neutra l o r

basi c collectio n solutions , greatl y reduce s th e chanc e o f dissolvin g an y chlorin e present
. Thi s metho d doe s no t experienc e asignificant

bia s whe n samplin g a40

0 pp mHC l ga s strea m containin g 5 0 pp mCl 2 . Samplin g a22 0 pp m HC l ga s strea mcontainin g 180 pp mCI 2 ' result s i n apositiv e bia s o f 3.4 percen t

i n th e HC l measurement
. 1. 4 Precisio n an dBias
. Th e within

laborator y relativ e standar ddeviation s ar e 6. 2 an d3. 2 percen t

a t HC l concentration s o

f 3. 9 an d15. 3 ppm , respectively
. Th e metho d doe s no t exhibi t abia s t o CI

2 whe n samplin g at concentration s les s tha n 5 0 ppm . 1.5 Stability
. Th e collecte dsample s ca n b e store dfo

r u p t o 4 week s before analysis
. 1. 6 Detectio n Limit
. Th e analytica l detectio n limi t

o f th e metho di s 0. 1 •xg/ml
. 2. Apparatus 2. 1 Sampling
. Th e samplin g trai n i s show n i n Figur e 26-1 , an dcomponent

part s ar e discusse dbelow
. 2.1. 1 Probe
. Borosilicat e glass , approximatel y %-in
. (9-mm ) I.D
. wit ha heatin g syste mt o preven t moistur e condensation
. A %-i n I.D
. Teflo n elbo w shoul db e attache dt o th e inle t o f th e prob e an da1-in
. (25-mm

) lengt ho f %-in
. I.D
. Teflon tubin g shoul db e attache dt o th e ope n en do f th e elbo w t o permi t

th e openin g o

f th e prob e t o b e turne dawa y fromth e ga s stream
. Thi s reduce s th e amoun t

o f particulat e enterin g th e train
. Thi s prob e configuratio n shoul db e use dwhe n th e concentratio n o f particulat e matte r i n th e emission s i s high
. Whe n high concentration s ar e no t

present , th e Teflo n elbo w i s no t

necessary , an dth e prob e inle t may b e perpendicular

t o th e ga s stream
. A glas s woo l plu g shoul dnot b e use dt o remov e particulat e matte r

sinc e anegativ e bia s i n th e dat acoul dresult
. Instead , aTeflo n filter (se e Sectio n 2.1.5 ] shoul db e installe dat th e inle t (fo r stac k temperature s 00 0 °F

) o r outle t (fo r stac k temperature s >30 0 °F

) o f th e probe
. 2.1. 2 Three-way Stopcock
. A borosilicate , three-way glas s stopcoc k withaheatin g syste mt o preven t

moistur e condensation
. Th e heate dstopcoc k

shoul dconnec t

directl y t o th e outle t

o f th e prob e an dth e inle t

o f th e firs t impinger
. Th e heatin g syste mshoul db e capabl e o f preventin g condensatio n up t o th e inle t o f th e firs t impinger
. Silicon e greas e may b e used , i f necessary , t o preven t

leakage
. BILLING COD E 6560-50- MP.1 6



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## ZZZZZZZZZZ 2 

# g
£ c o c o
C M



# t

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Wednesday , Februar y 13 , 199 1 / Rule s an dRegulation s
2.1. 3 Impingers . Fou r30-m l midge t impinger s wit h leak-fre e glas s connectors . Silicon e greas e ma y b e used , i f necessary , t o preven tleakage . Fo rsamplin g a thig h moistur e source s o rfo rsamplin g time s greate rtha n 1 hour , amidge timpinge rwit h a shortene d ste m (suc h tha tth e ga s sampl e doe s no tbubbl e throug h th e collecte d condensate ) shoul d b e use d i n fronto f th e firs timpinger . 2.1. 4 Dryin g Tub e o rImpinger . Tub e o r impinger , o f

Ma e Wes tdesign , filled wit h 6 - t o 16-mes h indicatin g typ e silic agel , o r equivalent , t o dr y th e ga s sampl e an d t o protec tth e dr y ga s mete ran d pump . I f th e silic age l ha s bee n use d previously , dr y a t17 5 ° C (35 0 °F) fo r2 hours . Ne w silic age l ma y b e use d a s received . Alternatively , othe rtype s o f desiccant s (equivalen to rbetter ) ma y b e used . 2.1. 5 Filter . A 25-m m Teflo n mat , Pallfle x TX40H17 5 o requivalent . Locat e betwee n th e prob e line ran d Teflo n elbo w i n aglas s o r quart z filte rholde ri n afilte rbo x heate d t o 25 0 °F . 2.1. 6 Sampl e Line . Leak-free , wit h compatibl e fitting s t o connec tth e las t impinge rt o th e needl e valve . 2.1. 7 Rat e Meter . Rotameter , o r equivalent , capabl e o f

measurin g flo w rat e t o withi n 2 percen to f

th e selecte d flo w rat e o f 2 liters/min . 2.1. 8 Purg e Pump , Purg e Line , Dryin g Tube , Needl e Valve , an d Rat e Meter . Pum p capabl e o f

purgin g th e samplin g prob e a t2 liters/min , wit h dryin g tube , fille d wit h silic a ge l o requivalent , t o protec tpump , an d arat e mete rcapabl e o f

measurin g 0 t o 5 liters/min . 2.1 5 Stopcoc kGrease , Valve , Pump , Volum e Meter , Barometer , an d Vacuu m Gauge . Sam e a s i n Metho d 6 , Section s 2.1.4 , 2.1.7 , 2.1.8 , 2.1.10 , 2.1.11 , an d 2.1.12 . 2. 2 Sampl e Recovery . 2.2. 1 Was h Bottles . Polyethylen e o rglass , 500-m l o rlarger , two . 2.2. 2 Storag e Bottles . 100-m l glass , wit h Teflon-line d lids , t o stor e impinge rsample s (tw o pe rsamplin g run) . Durin g clean-up , th e tw o frontimpinge rcontent s (0. 1 N H2SO4) shoul d b e combined . Th e content s o f th e tw o rea rimpinge r(0. 1 N NaOH ) ma y b e discarded , a s thes e solution s ar e include d onl y t o absor b Cl 2 , an d thu s protec tth e pump . 2. 3 Sampl e Preparatio n an d Analysis . Th e material s require d fo rvolumetri cdilutio n an d chromatographi canalysi s o f sample s ar e describe d below . 2.3. 1 Volumetri cFlasks . Clas s A , 100-m l size . 2.3. 2 Volumetri cPipets . Clas s A . assortmen tT o dilut e sample s int o th e calibratio n rang e o f

th e instrumen t 2.3. 3 Io n Chromatograph . Suppresse d o r nonsuppressed , wit h aconductivit y detecto r an d electroni cintegrato roperatin g i n th e pea kare amode . Othe rdetectors , stri p char t recorders , an d pea kheigh tmeasurement s ma y b e use d provide d th e 5 percen t repeatabilit y criteri afo rsampl e analysi s an d th e linearit y criteri afo rth e calibratio n curv e ca n b e met . 3. Reagents Unles s otherwis e indicated , al l reagent s mus tconfor m t o th e specification s establishe d b y th e Committe e o n Analytica l Reagent s o f

th e America n Chemica l Societ y (AC S reagen tgrade) . Whe n suc h specification s ar e no tavailable , th e bes t availabl e grad e shal l b e used . 3.1 . Sampling . 3.1. 1 Water . Deionized , distille d wate r tha tconform s t o AST M Specificatio n D1193 - 77 , Typ e 3 . 3.1. 2 Absorbin g solution , 0. 1 N Sulfuri c Aci d (H2SO4) . T o prepar e 10 0 ml o f th e absorbin g solutio n fo rth e fron timpinge rpair , slowl y ad d 0.2 8 ml o f

concentrate d H2SO

4 t o abou t9 0 ml o f

wate rwhil e stirring , an d adjus tth e final volum e t o 10 0 m l usin g additiona l water . Shak e wel l t o mi x th e solution . 3.1.3 . Chlorin e Scrubbe rSolution , 0. 1 N Sodiu m Hydroxid e (NaOH) . T o prepar e 10 0 m l o f th e scrubbe rsolutio n fo rth e bac kpai r -o f impingers , dissolv e 0.4 0 g o f soli d NaO H i n abou t9 0 ml o f

water , an d adjus tth e fina l solutio n volum e t o 10 0 m l usin g additiona l water . Shak e wel l t o mi x th e solution . 3. 2 Sampl e Preparatio n an d Analysis . 3.2. 1 Water . Sam e a s i n Sectio n 3.1.1 . 3.2. 2 Blan kSolution . A separat e blan k solutio n o f

th e absorbin g reagen tshoul d b e prepare d fo ranalysi s wit h th e field samples . Dilut e 3 0 ml o f

absorbin g solutio n t o 10 0 ml wit h wate ri n aseparat e volumetri cflask . 3.2. 3 Sodiu m Chlorid e (NaCI ) Stoc k Standar d Solution . Solution s containin g a nomina l certifie d concentratio n o f 100 0 mg/ 1 ar e commerciall y availabl e a s convenien t stoc ksolution s from whic h workin g standard s ca n b e mad e b y appropriat e volumetri cdilution . Alternately , concentrate d stoc ksolution s ma y b e produce d from reagen tgrad e NaCI . Th e NaC I shoul d b e drie d a t10 0 ° C fo r2 o rmor e hour s an d coole d t o roo m temperatur e i n adesiccato r immediatel y befor e weighing . Accuratel y weig h 1. 8 t o 1.7 g o f

th e drie d NaC I t o withi n 0. 1 mg , dissolv e i n water , an d dilut e t o 1 liter . Th e exac tC l concentratio n ca n b e calculate d usin g Eq . 26-1 . ji g Cl"/m l = g o f

NaClX10 s X35.453/58.4 4

Eq . 26- 1 Refrigerat e th e stoc kstandar d solutio n an d stor e n o longe rtha n 1 month . 3.2. 4 Chromatographi cEluen tEffectiv e eluent s fo rnonsuppresse d I C usin g aresin - o r silica-base d wea kio n exchang e colum n ar e a 4 mM potassiu m hydroge n phthalat e solution , adjuste d t o p H 4. 0 usin g asaturate d sodiu m borat e solution , an d a4 m M 4-hydrox y benzoat e solution , adjuste d t o p H 8. 6 usin g 1 N NaOH . A n effectiv e eluen tfo rsuppresse d io n chromatograph y i s asolutio n containin g 3 m M sodiu m bicarbonat e an d 2. 4 m M sodiu m carbonate . Othe rdilut e solution s buffere d t o asimila rp H an d containin g n o interferin g ion s ma y b e used . Whe n usin g suppresse d io n chromatography , i f th e "wate rdip " resultin g from sampl e injectio n interfere s wit h th e chlorid e peak , us e a2 mM NaOH/2. 4 mM sodiu m bicarbonat e eluent . 4. Procedure 4. 1 Sampling . 4.1. 1 Preparatio n o f

Collectio n Train . Prepar e th e samplin g trai n a s follows : Pou r1 5 m l o f th e absorbin g solutio n int o eac h o f th e firs ttw o impingers , an d ad d 1 5 m l o f scrubbe rsolutio n t o th e thir d an d fourth impingers . Connec tth e impinger s i n serie s wit h th e knockou timpinge rfirst , followe d b y th e tw o impinger s containin g absorbin g solutio n an d th e tw o containin g th e scrubbe r solution . Plac e afres h charg e o f silic agel , o r equivalen ti n th e dryin g tub e o rMa e Wes t impinger . 4.1. 2 Leak-Chec kProcedures . Leak-chec k th e prob e an d three-wa y stopcoc kbefor e insertin g th e prob e int o th e stack . Connec t th e stopcoc kt o the . outle to f th e probe , an d connec tth e sampl e lin e t o th e needl e valve . Plu g th e prob e inlet , turn o n th e sampl e pump , an d pul l avacuu m o f

a tleas t25 0 m m H g (1 0 in . Hg) . Tur n of

f th e needl e valve , an d not e th e vacuu m gaug e reading . Th e vacuu m shoul d remai n stabl e fo ra tleas t3 0 seconds . Plac e th e prob e i n th e stac ka tth e samplin g location , an d adjus tth e prob e an d stopcock :
WCt g of

NaCI XWX35A53 ml 58.4 4 Eq . 26- 1 Refrigerat e th e stoc kstandar d solutio n an d stor e n o longe rtha n 1 month . 3.2. 4 Chromatographi cEluent. Effectiv e eluent s fo rnonsuppresse d I C usin g aresin - o r silica-base d wea kio n exchang e colum n ar e a 4 m M potassiu m hydroge n phthalat e solution , adjuste d t o p H 4. 0 usin g asaturate d sodiu m borat e solution , an d a4 mM 4-hydrox y benzoat e solution , adjuste d t o p H 8. 6 usin g 1 N NaOH . A n effectiv e eluen tfo rsuppresse d io n chromatograph y i s asolutio n containin g 3 mM sodiu m bicarbonat e an d 2. 4 m M sodiu mP.1 8



### Federa l Registe r

/ Vol
. 56 , No
. 3 0 /

Wednesday , February 13 , 199 1 / Rule s an dRegulation s 577 3 carbonate
. Othe r

dilut e solution s buffere dt o asimila r p H an dcontainin g n o interferin g ion s ma y b e used
. Whe n usin g suppresse d ion chromatography , i

f th e "wate r

dip " resultin g fro

msampl e injectio n interfere s wit hth e chlorid e peak , us e a2 m M NaOH/2. 4 m M sodiumbicarbonat e eluent
. 4. Procedure 4. 1 Sampling
. 4.1. 1 Preparatio n of

Collectio n Train
. Prepar e th e samplin g trai n a s follows : Pou r 1 5 m l o f th e abortin g solutio n int o eac ho f th e first tw o impingers , an dad d1 5 m l o f scrubbe r solutio n to th e thirdan dfourt h impingers
. Connec t

th e impinger s i n serie s wit hth e knockou t

impinge r first , followe db y th e tw o impinger s containin g absorbin g solutio n an dth e tw o containin g th e scrubbe r solution
. Plac e afreshcharg e o f silic agel , o r equivalent , i n th e dryin g tub e o r Ma e Wes t impinger
. 4.1. 2 Leak-Check

Procedures
. Leak-chec k th e prob e an dthree-way stopcoc k before insertin g th e prob e int o th e stack
. Connec t th e stopcoc k

t o th e outle t

o f th e probe , an d connec t th e sampl e lin e t o th e needl e valve
. Plug th e prob e inlet , tur

n o n th e sampl e pump , an dpul l avacuu mo

f a t leas t 25 0 m mH g (1 0 in
. Hg)
. Tur

n of f th e needl e valve , an dnot e th e vacuu mgaug e reading
. Th e vacuu m shoul dremai n stabl e fo

r a t leas t 3 0 seconds
. Plac e th e prob e in th e stac k a t th e samplin g location , an dadjus t

th e prob e an dstopcoc k heatin g syste mt o atemperatur e sufficien t t o preven t wate r condensation
. Connec t

th e firs t impinge r to th e stopcock , an dconnec t th e sampl e lin e t o th e las t

impinger an dth e needl e valve
. Upo n completio n o f asamplin g run , remov e th e prob e fromth e stac k an d leak-chec k

a s describe dabove
. I

f aleak ha s occurred , th e samplin g ru n mus t b e voided
. Alternately , th e portio n o

f th e trai n behin d th e prob e may b e leak-checke dbetwee n multipl e run s a t

th e sam e site a s follows : Clos e th e stopcoc k

t o th e firs t

impinger (se e Figur e 1 A o f Figur e 26-1) , an dturn o n th e samplin g pump . Pull avacuu mo f a t leas t 25 0 m mHg , turn of

f th e needl e valve , an dnot e th e vacuu mgaug e reading
. Th e vacuu m shoul dremai n stabl e for

a t leas t 3 0 seconds
. Releas e th e vacuu mo n th e impinge r trai n b y turnin g th e stopcoc k

t o th e ven t

positio n t o permi t ambien t ai r t o ente r (se e Figur

e I B o f Figur e 26-2)
. I f thi s procedur e i s used , th e ful l trai n leak-chec k

describe dabov e mus t

b e conducte dfollowing th e fina l run , an dal l precedin g samplin g run s mus t b e voide di

f a lea k ha s occurred
. 4.1. 3 Purg e Procedure
. Immediatel y before sampling , connec t

th e purg e lin e t o th e stopcock , an dtur

n th e stopcoc k

t o permi t th e purg e pum

p to purg e th e prob e (se e Figur e I A o f Figur e 26-1)
. Tur

n o n th e purg e pump , an d adjus t th e purg e rat e t o 2 liters/min
. Purg e fo r a t leas t 5 minute s befor

e sampling
. 4.1. 4 Sampl e Collection
. Tur n o n th e samplin g pump , pul l aslight vacuu mo f approximatel y 2

5 m mH g ( 1 in
. Hg) o n th e impinger train , an dturn th e stopcoc k t o permi t stac k ga s t o b e pulle dthroug hth e impinger trai n (se e Figur

e l C o f Figur e 26-3)
. Adjus t th e samplin g rat e t o 2 liters/min , a s indicate db y th e rat e meter , an dmaintai n thi s rat e t o withi n 1 0 percen t

durin g th e entir e samplin g run . Tak e reading s o f th e dry ga s mete r

volume an dtemperature , rat e meter , an dvacuu mgaug e at

leas t onc e every 5 minute s durin g th e run . A samplin g time o f 1 hour i s recommended
. Shorte r samplin g time s ma y introduc e asignificant

negativ e bia s i n th e HC l concentration
. A t th e conclusio n o

f th e samplin g run , remov e th e trai n fromth e stack , cool , an dperfor

maleak-chec k

a s describe di n sectio n 4.1.2
. 4. 2 Sampl e Recovery
. Disconnec t th e impinger s after

sampling
. Quantitativel y transfe r th e content s o

f th e first thre e impinger s (th e knockou t

impinger an dth e tw o absorbin g solutio n impingers ) to aleak

free storag e bottle
. Ad dth e wate r rinse s o f eac ho f thes e impinger s an dconnectin g glasswar e to th e storag e bottle
. Th e content s o f th e scrubbe r

impinger s an dconnectin g glasswar e rinses may b e discarded
. Th e sampl e bottl e shoul db e sealed , shake n t o mix , an dlabeled
. Th e flui dleve l shoul db e marke ds o tha t

i f an y sampl e i s los t

durin g transpor t acorrectio n proportiona l t o th e los t volume can b e applied
. 4. 3 Sampl e Preparatio n fo r Analysis
. Chec k th e liqui dleve l in eac hsample , an d determin e i

f an y sampl e wa s los t

durin g shipment
. I

f anoticeabl e amoun t

of leakag e ha s occurred , th e volume los t ca n b e determine dfromth e differenc e betwee n th e initial an dfina

l solutio n levels , an dthi s valu e ca n b e use dto correc t

th e analytica l results
. Quantitativel y transfe r

th e sampl e solutio n t o a100-m l volumetri c flask , an ddilute th e solutio n t o 10

0 m l withwater
. 4. 4 Sampl e Analysis
. 4.4. 1 Th e IC condition s wil l depen dupo n analytica l colum

n typ e an dwhethe r suppresse do r

nonsuppresse dIC i s used
. An exampl e chromatogramfrom a nonsuppresse dsyste musin g a150-m m Hamilto n PRP-X100 anio n column , a* * *
. 2 l/mi n flow rat e o

f a4 m M 4-hydrox y benzoat e solutio n adjuste dt o ap H o f 8. 6 usin g 1 N NaOH , a5 0 -i

l sampl e loop , an da conductivity detector

se t o n 1.0 ji S ful

l scal e i s show n i n Figure 26-2
. 4.4. 2 Befor

e sampl e analysis , establis ha stabl e baseline
. Nex t

injec t asampl e o

f water , an ddetermin e i

f an y Cl " appear s i n th e chromatogram
. I

f Cl " i s presen t

repea t th e load/injectio n procedur e unti l n o Cl " i s present
. At

thi s point , th e instrumen t i s read y fo r use . 4.4. 3 Firs t

injec t th e calibratio n standard s coverin g a n appropriat e concentratio n range , startin g wit

hth e lowes t

concentratio n standard
. Nex t

injec t i n duplicate , aQC sampl e followe db y awate r blan k an dth e fieldsamples
. Finally , repea t th e injectio n o

f calibratio n standard s t o allo w compensatio n fo r an y drif t in th e instrumen t

durin g analysi s o f th e fieldsamples
. Measur e th e Cl " peak area s o r height s o f th e samples
. Us e th e averag e respons e fromth e duplicat e injection s to determin e th e fieldsampl e concentration s usin g alinear calibratio n curv e generate dfromth e standards
. 4. 5 Audi t

Analysis
. An audi t

sampl e mus t b e analyzed , subjec t

t o availability
. 

## 0.79 9 0.94 4

1.95 7 Chlorid e

Figur e 26-2

. Exampl e Chromatogra m

5. Calibration 5. 1 Dr y Gas Meterin g System , Thermometers , Rate Meter , an dBarometer
. Same a s in Metho d6 , section s 5.1 , 5.2 , 5.3 , an d5.4
. 5. 2 Calibratio n Curv e fo

r Io n Chromatograph
. T o prepar e calibratio n standards , dilut e given volume s (1. 0 m l o r greater ) o f th e stoc k standar dsolution , wit

h 0. 1 N H2SO

4 (sectio n 3.1.2

) t o convenien t volumes
. Prepar e a t

leas t fou r standard s that ar e withi n th e linear

rang e o f th e instrumen t an dwhic hcove r

th e expecte dconcentratio n rang e o f th e fieldsamples
. Analyz e th e standard s a s instructe din sectio n 4.4.3 , beginnin g wit

hth e lowes t

concentratio n standard
. Determin e th e peak measurements , an dplo t individual value s versu s Cl ' concentratio n in fig/ml
. Draw asmoot hcurv e throughth e points
. Us e linear regressio n t oP.1 9 

### 577 4 Federa

l Registe r/

Vol
. 56,
. No
. 3 0 /

Wednesday,
. Februar y 13 , 1991* / Rule s andiRegulatiGh s
calculat e aformul adescribin g th e resultin g linea rcurve . ftQuality Assurance 6. 1 Applicability . Whe n th e metho d i s use d t o analyz e sample s t o demonstrat e complianc e wit h asourc e emissio n regulation , ase to f

tw o audi tsample s mus tb e analyzed . 6. 2 Audi tProcedure . Th e audi tsampl e ar e chlorid e solutions . Concurrentl y analyz e th e tw o audi tsample s an d ase to f complianc e sample s i n th e sam e manne rt o evaluat e th e techniqu e o f

th e analys tan d th e standard s preparation . Th e sam e analyst , analytica l reagents , an d analytica l syste m shal l b e use d bot h fo rcomplianc e sample s an d th e EP A audi tsamples . I

f thi s conditio n i s met , auditin g th e subsequen tcomplianc e analyse s fo rth e sam e enforcemen tagenc y withi n 3 0 day s i s no trequired . A n audi tsampl e se tma y no tb e use d t o validat e differen tset s o f complianc e sample s unde rth e jurisdictio n o f differen tenforcemen tagencies , unles s prio r arrangement s ar e mad e wit h bot h enforcemen tagencies . 6. 3 Audi tSampl e Availability . Th e audi t sample s ma y b e obtaine d b y writin g o r callin g th e EP

A Regiona l Offic e o rth e appropriat e enforcemen tagency . Th e reques t fo rth e audi tsample s mus tb e mad e a tleas t 3 0 day s prio rt o th e schedule d complianc e sampl e analyses . ' 6. 4 Audi tResults . Calculat e th e concentration s i n mg/dsc m usin g th e specifie d sampl e volum e i n th e audi t instructions . Nots * Indicatio n o f

acceptabl e result s ma y b e obtaine d immediatel y b y reportin g th e audi tresult s i n mg/dsc m an d complianc e result s i n tota l fi g HCl / sampl e t o th e responsibl e enforcemen tagency . Includ e th e result s o f

bot h audi tsamples , thei r identificatio n numbers , an d th e analyst' s nam e wit h th e result s o f th e complianc e determinatio n sample s i n appropriat e report s t o th e EP A Regiona l Offic e o rth e appropriat e enforcemen tagency . Includ e thi s informatio n wit h subsequen tanalyse s fo rth e sam e enforcemen tagenc y durin g th e 30-da y period . Th e concentration s o f

th e audi tsample s obtaine d b y th e analys tshal l agre e withi n 1 0 percen to f

th e actua l concentrations . I f th e 1 0 percen tspecificatio n i s no tmet , reanalyz e th e complianc e sample s an d audi tsamples , an d includ e initia l an d reanalysi s value s i n th e tes treport . Failur e t o mee tth e 1 0 percen tspecificatio n ma y requir e retest s unti l th e audi tproblem s ar e resolved . However , if th e audi tresult s d o Ino taffec tth e complianc e o rnoncomplianc e statu s o f th e affecte d facility , th e Administrato rma y waiv e th e reanalysi s requiremen tfurthe raudits , o rretest s an d accep tth e result s o f

th e complianc e test . Whil e step s ar e bein g take n t o resolv e audi t analysi s problems , th e Administrato rma y als o choos e t o us e th e dat at o determin e th e complianc e o rnoncomplianc e statu s o f th e affecte d facility . 7. Calculations Retai n a tleas ton e extr adecima l figure beyon d thos e containe d i n th e availabl e dat a i n intermediat e calculations , an d roun d of f onl y th e fina l answe rappropriately . 7. 1 Sampl e Volume , Dry Basis , Correcte d t o Standar d Conditions . Calculat e th e sampl e volum e usin g Eq . 6- 1 o f Metho d 6 . 7. 2 Tota l fi g HC l Pe rSample . (S-fl)(100)(36.46) (35.453 ) = (102.84)(S-5 ) Eq . 26- 2 where : m = Mas s o f

Hc l i n sample , fig . S = Concentratio n o f

sample , fi g Cl'/ml . * B = Concentratio n o f

blank , fi g Cl'/m L 10 0 = Volum e o f

filtere d an d dilute d sample , ml . 36.4 6 - = Molecula rweigh to f

HCl , fig/fig mole . 35.45 3 = Atomi cweigh to f Cl , fig/fig-mole . 7. 3 Concentratio n o f

HC l i n th e Flu e Gas . K m VmUld ) Eq . 26- 3

where : C = Concentratio n o f

HCl , dry basis , mg / dscm . K= 10'mg/fig . m = Mas s o f

HC l i n sample , fig . V m (rtd ) = Dry ga s volum e measure d b y th e dry ga s meter , correcte d t o standar d conditions , dscm . ftBibliography 1 . Steinsberger , S.C . an d J.H . Margeson . "Laborator y an d Fiel d Evaluatio n o f a Methodolog y fo rDeterminatio n o f Hydroge n Chlorid e Emission s from Municipa l an d Hazardou s Wast e Incinerators. " U.S . Environmenta l Protectio n Agency , Offic e o f Researc h an d Development . Repor tNo . , 1989 . 2 . Stat e o f

California , Ai rResource s Board . Metho d 421 . "Determinatio n o f Hydrochlori c Aci d Emission s from Stationar y Sources. " Marc h 18,1987 . 3 . Entrop y Environmentalist s Inc . "Laborator y Evaluatio n o f aSamplin g an d Analysi s Metho d fo rHydroge n Chlorid e Emission s from Stationar y Sources : Interi m Report. " EP

A Contrac tNo . 68-02-4442 . Researc h Triangl e Park , Nort h Carolina . January 22,1988 . Appendi x A [Amended ] 3 . Metho d 1 9 o f

appendi x A par t6 0 i s amende d b y addin g paragraph s 4. 3 an d 5. 4 a s follows : Metho d 19—Determinatio n o f Sulfu r Dioxid e Remova l Efficienc y an d Particulat e Matter , Sulfu rDioxide , an d Nitroge n Oxide s Emissio n Rate s **** * 4. 3 Dail y Geometri cAverag e Pollutan t Rate s fro m Hourl y Values . Th e geometri c averag e pollutan trat e (E m ) i s compute d usin g th e followin g equation :

E« . = EXP[(1/n ) 2 [lnfEJ] ]



### 1= 1 Eq . 19 -

20 a where : E r a= dail y geometri caverag e pollutan trate , ng/ J (lbs/millio n Btu ) o rpp m correcte d t o 7 percen tO2 . Eh j = hourl y arithmeti caverag e pollutan trat e fo rhou r"j, " ng/

J (lb/millio n Btu ) o rpp m correcte d t o 7 percen tO2 . n = tota l numbe ro f

hourl y average s fo r whic h pollutan trate s ar e availabl e withi n th e 2 4 h rmidnigh tt o midnigh t dail y period . I n = natura l lo g o f

indicate d value . EXP= th e natura l logarithmi cbas e (2.718 ) raise d t o th e valu e enclose d b y brackets . • * * * * 5. 4 Dail y Geometri cAverag e Percen t Reductio n fro m Hourl y Values . Th e geometri c averag e percen treductio n (%R„) i s compute d usin g th e followin g equation : 

### :

!P.2 0
Federa l Riegister
. /

£Vol
. "56* 'No
. "3 0 >/' We'dries'day , - Februar y 13 , 199 1 7 Rule s an dReguMtori s 5775 :

%R „ = 10 0 1-EX P [(1/n ) 2 I n (Ej 0

/E M ) ] 1 j= l ' Eq
. 19

- 24a where : %R „ = dail y geometri c averag e percen t
. reduction
. Ejo , E M = matche dpai r

hourl y arithmeti c averag e pollutan t

rate , outle t

an dinlet , respectively , ng/

J (lb/millio n Btu) o r

pp m correcte dt o 7 percen t

0 2 . n = tota l number

o f hourly average s fo

r whic hpaire dinle t

an doutle t

pollutan t rate s ar e availabl e withi n th e 24-h r midnight t o midnight

dail y period
. In=natura l log o

f indicate dvalue
. EX P= th e natura l logarithmi c bas e (2.718) raise dt o th e valu e enclose db y brackets
. Note : Th e calculatio n include s only paire d dat aset s (hourly average ) fo r th e inle t an d outle t pollutan t measurements
. 

### * * ' * * * [F RDoc
. 91-139 9 File d2-12-91 ; 8:4 5 am] BILLING COD E 6560-50- M DEPARTMEN TO F COMMERC E Nationa l Oceani c an d Atmospheri c Administratio n 5 0 CF R Part s 67 2 an d 67 5 [Docke t No . 90899-1019 ] Groundfis h o f th e Gui f o f Alaska ; Groundfis h o f th e Berin g Se a an d Aleutia n Island s AGENCY: Nationa l Marin e Fisherie s Servic e (NMFS) , NOAA , Commerce
. ACTION : Fina l rule , technica l amendment
. SUMMARY

: Th e Secretar y o f

Commerc e issue s thi s fina l rul e implementin g a technica l amendmen t

t o reinstat e regulator y languag e tha t wa s unintentionall y delete db y regulation s implementin g Amendmen t 1 3 t o th e Fisher y Managemen t

Pla n fo r th e Berin g Sea/Aleutia n Island s Groundfis h (Berin g FMP ) an dAmendmen t 1 8 t o th e Fisher y Managemen t

Pla n fo r th e Gul f o f Alask aGroundfis hFisher y (Gul f FMP ) (5 4 FR50386 , Decembe r 6,1989)
. EFFECTIV EDATE : Februar y 8,1991
. FO R FURTHE R INFORMATIO N CONTACT : Patrici aPeacoc k

(Fisher y Managemen t Specialist) , NMFS , Plan s an d Regulation s Division , 133 5 East-Wes t Highway , Silve r

Spring , Marylan d20910 , telephon e 301-427-2343
. SUPPLEMENTAR Y INFORMATION : Groundfis hfisherie s i n th e Exclusiv e Economi c Zon e of

f Alask aar e governe d b y Federa l regulation s a t 5 0 CFRpart s 611 , 620 , 672 , an d67 5 tha t implemen t

th e Berin g an dth e Gul f

FMPs
. Thes e FMP s wer e prepare db y th e Nort hPacifi c Fisher y Managemen t

Counci l an d approve db y th e Secretar y o f Commerc e (Secretary ) unde r

provision s o f

th e Magnuso n Fisher y Conservatio n an d Managemen t

Act
. Thi s fina l rul e implement s atechnica l amendmen t

tha t (1 ) reinstate s languag e unintentionall y delete db y amendator y languag e i n 5 4 FR5038 3 (Decembe r 6 , 1989 ) an d(2 ) retain s th e amendator y languag e o f

5 6 FR49 2 (Januar y 7,1991)
. O n Decembe r

6,1989 , afina l rul e wa s publishe di n th e Federa l Registe r (5 4 F R 50386 ) tha t

wa s intende donl y t o amen d th e introductor y languag e o f § § 672.20(a)(2 ) an d675.20(a)(2)
. Ite m1 1 o f thi s amendator y languag e state s tha t * * * paragraph s (a)(2 ) an d(f)(1 ) ar e revise d* * * ; ite m2 0 state s tha t * * * paragrap h(a)(2 ) i s revise d* * *
. Thi s amendator y languag e revise dth e introductor y tex t

o f paragrap h(a)(2 ) i n thes e section s bu t

delete dth e remainde r o f th e regulator y languag e i n § § 672.20(a)(2 ) an d675.20(a)(2)
. Paragraph s i n § 672.2 0 tha t wer e unintentionall y delete dwer e (a)(2)(i) , (a)(2)(H) , (a)(2)(ii)(A) , an d(a)(2)(ii)(B)
. Tabl e 1 i n § 672.2 0 als o wa s unintentionall y deleted
. Paragraph s tha t wer e unintentionall y delete di n § 675.2 0 wer e a s follows : (a)(2)(i) , (a)(2)(i)(A) , an d(a)(2)(i)(B)
. O n Januar y 1,1991 , fina l rules ' implementin g Amendmen t 1 4 t o th e Berin g FM Pan dAmendmen t 1 9 t o th e Gul f FM Pals o revise dtex t

i n § § 672.20(a)(2 ) an d675.20(a)(2 ) (5 6 FR 492 , Januar y 7,1991)
. Thi s rul e retain s th e change s t o thes e section s resultin g fro mAmendment s 1 4 an d19
. Th e Gul f an dBerin g FMP s wer e implemente dusin g procedure s specifie d b y th e Magnuso n Ac t

an dth e Administrativ e Procedur e Act
. However , a s explaine dabove , th e languag e currentl y i n § § 672.20(a ) an d675.20(a ) doe s no t correctl y reflec t

th e Gul f o r Berin g FMP s an dsubsequen t amendments
. Thi s fina l rule , technica l amendment , i s reinstatin g regulator y languag e neede dt o implemen t

correctl y th e Berin g an dGul f

FMP s a s amended
. Classificatio n Thi s fina l rule , technica l amendment , i s issue dunde r

part s 67 2 an d675
. Becaus e thi s rul e reinstate s regulator y tex t tha t wa s inadvertentl y delete d durin g a n earlie r

rulemakin g proceedin g an dmake s n o substantiv e change s othe r tha n change s determine di n rulemakin g fo r Amendment s 1 4 an d19 , i t i s unnecessar y unde r

5 U.S.C
. 553(b)(B ) t o provid e fo r

prio r publi c commen t

an d ther e i s goo dcaus e unde r 5 U.S.C
. 553(d ) no t t o dela y fo r

3 0 day s it s effectiv e date
. Becaus e thi s rul e i s bein g issue d withou t prio r comment , aregulator y flexibilit y analysi s i s no t require dunde r th e Regulator y Flexibilit y Ac t an dnon e ha s bee n prepared
. Thi s rul e reinstate s languag e tha t ha s bee n determine dno t

t o b e amajo r

rul e unde r Executiv e Orde r

12291 , doe s no t contai n policie s wit hfederalis m implication s sufficien t

t o warran t preparatio n o f

afederalis massessmen t unde r E.0.12612 , an ddoe s no t contai n a collection-of-informatio n requiremen t fo r th e purpose s o f

th e Paperwor k Reductio n Act
. Ther e i s n o chang e i n th e regulator y impact s previousl y reviewe d an danalyzed
. Lis t o f Subject s i n 5 0 CF RPart s 67 2 an d 67 5 Fisheries , Genera l limitations
. Dated : February 7,1991
. Michae l F
. Tillman , Acting Assistant

Administrator

for Fisheries, National Marine Fisheries Service. Fo r reason s se t

ou t i n th e preamble , 5 0 CFRpart s 67 2 an d67 5 ar e amende da s follows : PAR T672—GROUNDFIS H O F TH E GUL F O F ALASK

A 1
. Th e authorit y citatio n fo r par t 67 2 continue s t o rea da s follows : Authority : 1 6 U.S.C
. 180 1 et seq. 2
. Sectio n 672.20(a)(2 ) i s revise dan d Tabl e 1 i s adde dt o th e sectio n t o rea d a s follows :