WPCx Cό@*x|mXE'#`BG3[*{wS`'m]&[feDsF >>>|??|2@@ABCDEFGHFIJdK 15L 72L1L 1Md MN AS\O D+OOOfOOaPPP 0OP 0EQfJQaLQ AY`QQ AR 0K*S*S*S:uS\SX T T TcTdg~T~T~T3TdUU6VdVV@WoAWpxZZZZZZZZ jndvnnnnn0od0o0o&odppKpdppppp@rro3rdvvKvdvv1gxd xxxxxx'ydyy8uzdDzzr{fc|J|f}a}f)}a+}pj?}Ffa : dEf!a#d7m <6X9`("Courier 10cpiX'     0 .   ;S9Z+Courier  Level 1Level 2Level 3Level 4Level 5(O$3|x<6X9`("Courier 10cpiXx6X@8;X@<6X`(4Line Draw 12cpiFull-Crd6X@J'@( T$  x12NOMWgmacr Mark WilsongmARush ##Xd#(uH Z6Times New Roman Regular\\US_EPA\EMAD_D230 HP4200dtn.PARK.OAQPS.RTP.EAST.EPA0,2 >U*OLE* S_p^2~=~{SUM{d_i^2}}over{2n}),-./012x3MQUY]aeiLarge BulletWPC. . !.  y  .  @@ &  & MathType-  PP Times New Roman[wdw0- 2 JBy 2 OBy 2 VS 2 pxS YTimes New Roman[wdw0- 2 9RSSymbolw@" [wdw0- 2 U=STimes New Roman[wdw0- 2 } 100%@ &  "System 0- 5HCEKQW]cioAutoList1I.A.I.I.I.I.I.I.WPWin 6.0/OLE 1.0 Prefix Information MarkerEquation.COEE2ࡱ> Root EntryFKSsOle CompObjjBOlePart  FMicrosoft Equation 2.0 DS EquationEquation.COEE29q y  .  @@ &  & MathType-  POlePres0004Equation Native lP Times New Roman[wdw0- 2 JBy 2 OBy 2 VS 2 pxS YTimes New Roman[wdw0- 2 9RSSymbolw@" [wdw0- 2 U=STimes New Roman[wdw0- 2 } 100%@ &  "System 0-NANIPD B R =BVSabx100%R =BVSab~x~100%0Courier New TUR#Lucida Console # METAFILEPICTQ y  .  @@ &  & MathType-  PP Times New Roman[wdw0- 2 JBy 2 OBy 2 VS 2 pxS YTimes New Roman[wdw0- 2 9RSSymbolw@" [wdw0- 2 U=STimes New Roman[wdw0- 2 } 100%@ &  "System 0-3#37=CIQYag1.a.i.(1)(a)(i)1)a)i)(EGMSY_ekqAutoList34A.A.A.A.A.A.A.A.http://www.epa.gov/edocket.Courier New Regular dXX"S<2pXX`aXqXXEIXXxd2HiXXJ2XXFJn1, 2, 3,Level 1Level 2Level 3Level 4Level 5 \\R3' Letter\%2A`Arial2 Z(Times New Roman (;3$2#  0  .3  0  Level 1Level 2Level 3Level 4Level 5(O;$0  2#  a  .3  0` (#(#(b$0  0` (#(#2#   .3  0 ` (#` (#(xir$0  0` (#(#0 ` (#` (#2#(  0  )3  0 (# (#($0  0` (#(#0 ` (#` (#0 (# (#2#(  a  )3  0h(#(#(F$0  0` (#(#0 ` (#` (#0 (# (#0h(#(#2#(   )3  0h(#h(#($0  0` (#(#0 ` (#` (#0 (# (#0h(#(#0h(#h(#2#  0  )3  0(#(#({$0  0` (#(#0 ` (#` (#0 (# (#0h(#(#0h(#h(#0(#(#2#  a  )3  0p(#(#(F$0  0` (#(#0 ` (#` (#0 (# (#0h(#(#0h(#h(#0(#(#0p(#(#2#     )3  0p(#p(# ((3m$  T!    i#   __fR` hp !%'0*,.8135@8:<H?AXf_ԀEq._Ԁ301_Ԅ17_ԄLevel 1Level 2Level 3Level 4Level 54#02Quick 1.$  .0 $   2 +RSD~=~left(SDoverS_mright)~times~100XX RSDXX XXEhXXjXXjXXiXXwEoXXwqXXwqXXwpXN3XXlxSDXX}}S8mXXL 'XX 100 i#   __r^X` hp x (#%'0*,.8135@8:<H?AXr_Eq._Ԁ301_Ԅ3 r i#   ___ԀEq._Ԁ3014(EGMSY_ekqAutoList36I.I.I.I.I.I.I.I. i#   ___ԀEq._Ԁ3015   r i#   ___ԀEq._Ԁ3016 ___Ԁ____Eq._Ԁ3017 r i#   ___ԀEq._Ԁ3018  i#   __r^X` hp x (#%'0*,.8135@8:<H?AXr_ԀEq._Ԁ301_Ԅ10_ i#   __cO` hp !%'0*,.8135@8:<H?AXc_ԀEq._Ԁ301_Ԅ11_ i#   __cO` hp !%'0*,.8135@8:<H?AXc_ԀEq._Ԁ301_Ԅ12   i#   __cO` hp !%'0*,.8135@8:<H?AXc_ԀEq._Ԁ301_Ԅ13_ i#   _cO` hp !%'0*,.8135@8:<H?AXc_ԀEq._Ԁ301_Ԅ14_   i#   __fR` hp !%'0*,.8135@8:<H?AXf_ԀEq._Ԁ301_Ԅ15 i#   __fR` hp !%'0*,.8135@8:<H?AXf_ԀEq._Ԁ301_Ԅ16_  i#   __fR` hp !%'0*,.8135@8:<H?AXf_=.ԀEq._Ԁ301_Ԅ20_ i#   _fR` hp !%'0*,.8135@8:<H?AXf_ԀEq._Ԁ301_Ԅ18_ <{S^2}_{pooled}~=~{{sumfromitoN{d_i}^2}over{2(n1)}}  i#   __fR` hp !%'0*,.8135@8:<H?AXf_=.ԀEq._Ԁ301_Ԅ21_XXS$2pooledXX2mXCXXIN3iXXdiW"2XXaJ2XXJ(XXMJnXXJXX_J1XXJ)(EGMSY_ekqAutoList37A.A.A.A.A.A.A.A.ZA. 'SD_u~=~sqrt{{sum~{{d_iu}^2}}over{2n}}),-./012x͋Gaeimquy}Bullet ListBullets ListXXSDuXXQ XSXXTXXSXXESXXSXXSXXR XpXXEIXXmxd3iu2XX=J2XXJn _____Eq._Ԁ301_Ԅ19_iM -, dc'dxdl Level 1 Level 2 Level 3 Level 4 Level 5TABLE A('2$  T!   ($ (    ) bTABLE BeijaM << deUULevel 1Level 2Level 3Level 4Level 5nipa&OLE 2.0 Box <=8C HKKKK( $ Figure  1  http://www.epa.gov/ttn/oarpghttp://www.epa.gov/ttn/emc/audit/audreqr1.pdfhttp://www.epa.gov/ttn/emc/email.html#audit B~=~{S}_{m}~~CSXX}BXX}XX}SL8mXX}XX}CS )SD~=~sqrt{{SUM(S_iS_m)^2}over{(n1)}}XXSDXXXwXXXLTXXLSXXLESXXLSXXLSXXLRXXX9EIXXx(XX6xS3iXXxXXxS3mXXhx)2XXJ(XXpJnXXJXXJ1XXJ) ,t=~{{lineBline}over{{SD}over{sqrtn}}}XXtXXX(XXm XX!mBXXm X-XXrSD gX OXXgJn*OLE*WPC. . ! .  r  .  @@& & MathType-<JJ:: 0Courier New  ~ ~ ~0- 2 (By 2 <Ry 2  2  2 B 2 ,CS2 h x Symbol~@b Y  ~ ~ ~0- 2  =S0Courier New w  ~ ~ ~0- 2  100% & "System ! ~-WPWin 6.0/OLE 1.0 Prefix Information MarkerEquation.COEE2ࡱ> Root EntryFD^@Ole CompObjjBOlePart  FMicrosoft Equation 2.0 DS EquationEquation.COEE29q*zlculatedtvaluewiththecriticalvalueof r  .  @@& & MathType-<JOlePres000&Equation Native J:: 0Courier New  ~ ~ ~0- 2 (By 2 <Ry 2  2  2 B 2 ,CS2 h x Symbol~@b Y  ~ ~ ~0- 2  =S0Courier New w  ~ ~ ~0- 2  100% & "System ! ~-NANIæC Courier New eB  eR  e =  e  eB  eCS ab e x Courier New~1~0~0~% METAFILEPICTQ r  .  @@& & MathType-<JJ:: 0Courier New  ~ ~ ~0- 2 (By 2 <Ry 2  2  2 B 2 ,CS2 h x Symbol~@b Y  ~ ~ ~0- 2  =S0Courier New w  ~ ~ ~0- 2  100% & "System ! ~- S_{v}^2~=~{{SD}_{v}^2}XX}S2MvXXR}XXF}SD222Mv &{S^2}_p~=~{{S^2}_{pooled}~~SSUBv^2}XX}S28pXX}XX}SA28pooledXX}XX}SS28Mv F~=~{{S_p}^2}over{{S_v}^2}XX"/FXX/XWXXSp2XX}S8v2 Ad_i~=~{({V_1_i}~+~{V_2_i})}over2~~{({P_1_i}~+~{P_2_i})}over2XX1diXXTXeXX(XXVoY1,,+iXXSXXGVY2,, +iXXI)XXfJ2XX6XGXXe(XXPQ Y1,, +iXX5 XX) P Y2,, +iXX+ )XXH J2*OLE* B~=~S_m~~M_m~~CSWPC.B .B ! .B  k  .   &  & MathTypeP Times New Roman  ~ ~ ~0- 2 `4dy 2 `Ry 2 `*Ry [Times New Roman  ~ ~ ~0- 2 iy? 2 Jiy? 2  iy?Symbol~@  ~ ~ ~0- 2 `=y 2 `-y [Times New Roman  ~ ~ ~0- 2 min?p 2 maxpb & "System !, ~-XX}BXX}XX}SQ8mXX}XX}Mh8mXX}XX}CS At~=~{LINEBLINE}over{sqrt{{{S_u^2}~+~{S_s^2}}over{12}}}XX"tXXXXX XXBXXl XXXTXXSXXSXXESXXSXXSXXRfXXX xS2HuXXJxXX>xS2HsXX"J12 'SD_s~=~sqrt{{SUM~{{d_is}^2}}over{2n}}XXSDsXXQ XSXXTXXSXXESXXSXXSXXR XpXXEIXXmxd3is2XX=J2XXJn F~=~{{S_u}^2}over{{S_s}^2}XX"/FXX/XWXXSu2XX}S8s2 .SD_{pooled}~=~sqrt{{{S_s}^2+{S_u}^2}over2}XXSDpooledXX8 XXX,TXX,SXX,ESXX,SXX,SXX,RXXXxS3s2XX4xXXxSK3u2XXGJ2 h\R3' Letter\   \\R3' Letter\http://www.epa.gov/ttn/emc/ctm.html.vTABLE B8TABLE AWPWin 6.0/OLE 1.0 Prefix Information MarkerEquation.COEE2ࡱ> Root EntryFa֌_Ole CompObjjBOlePart  FMicrosoft Equation 2.0 DS EquationEquation.COEE29q) 4 k  .   &  & MathTypeP Times New Roman  ~ ~ ~0OlePres000Equation Native l- 2 `4dy 2 `Ry 2 `*Ry [Times New Roman  ~ ~ ~0- 2 iy? 2 Jiy? 2  iy?Symbol~@  ~ ~ ~0- 2 `=y 2 `-y [Times New Roman  ~ ~ ~0- 2 min?p 2 maxpb & "System !, ~-NANIPC d i =R mini -R maxi METAFILEPICT) ) 4 k  .   &  & MathTypeP Times New Roman  ~ ~ ~0- 2 `4dy 2 `Ry 2 `*Ry [Times New Roman  ~ ~ ~0- 2 iy? 2 Jiy? 2  iy?Symbol~@  ~ ~ ~0- 2 `=y 2 `-y [Times New Roman  ~ ~ ~0- 2 min?p 2 maxpb & "System !, ~- <SD_d~=~sqrt{{sumfromitoN{({d_id_m)}^2}}over{n1}}xTABLE CH 0t~=~{lined_mline}over{{SD_d}over{sqrtn}}XX"3tXX3Z X[XX? XXdmXXR tX<-XXZSDK`d X OXXJn0&TABLE A XXSD dXXwXXXXTXXSXXSXX4SXXSXXSXXMSXXSXXRXu'XXIN^iXX(XXd iXX[XXdrmXX)8q2XXAnXX@AXXA1 c i#   __?Eq.3012  T!   _8    ?,8EXXdd8р@B(# B XEXXX(XXXXE@@  ENVIRONMENTALPROTECTIONAGENCY  @@&40CFRPart63  l @@*[OAR20040080,FRL78519]  D @@((+_RIN_Ԁ2060AF00 ^  NationalEmissionStandardsforHazardousAirPollutants:AppendixATest 6  Methods;Method301forthe "  @@(( FieldValidationofPollutantMeasurementMethodsfromVariousWasteMedia    A  AGENCY: EnvironmentalProtectionAgency(EPA).    ACTION: Proposedrule. p  SUMMARY: Thisactionproposestoamendproceduresforvalidatingalternative P emissionstestmethods,torewritetheEPAsMethod301inplainlanguage,reorganize r0 themethodforclarity,correcttechnicalerrors,andrevisethetechnicalprocedures.The J revisionstothetechnicalproceduresincludereplacingquantitationlimitswithdetection " limits,revisingthebiasacceptancecriteriaandeliminatingthecorrectionfactors,revising  theprecisionacceptancecriteria,andallowinganalytespikingasanoptionevenwhen   thereisanexistingtestmethod. "h  DATES: Comments.Commentsmustbereceivedonorbefore[INSERTDATE60 $@! DAYSAFTERPUBLICATIONINTHEFEDERALREGISTER]. b& # PublicHearing.IfanyonecontactstheEPArequestingapublichearingby[INSERT :(!% DATE20DAYSAFTERPUBLICATIONINTHEFEDERALREGISTER],apublic *#' hearingwillbeheldon[INSERTDATE30DAYSAFTERPUBLICATIONINTHE +%) FEDERALREGISTER]. -'+  ADDRESSES :Comments.Submityourcomments,identifiedbyDocketIDNo.OAR B 20040080,byoneofthefollowingmethods. "  ]),-./012(͋x3")3"  )3 2͋3  0 `   Federal_eRulemaking_ԀPortal:http:///www.regulations.gov.Followtheonline   instructionsforsubmittingcomments.)3  ݌ ` (#` (# Ќ  ")3"  )3C 2͋3  0 `   AgencyWebsite:http://www.epa.gov/edocket._EDOCKET_,EPAselectronic  h publicdocketandcommentsystem,isEPAspreferredmethodforreceiving @  comments.Followtheonlineinstructionsforsubmittingcomments.)3C p ݌Z ` (#` (# Ќ  ")3"  )3 2͋3  0 `   Mail:AirandRadiationDocketandInformationCenter(MailCode6102T), 2  AttentionDocketNumberOAR20040080,RoomB108,U.S.EPA,1301   ConstitutionAvenue,NW.,Washington,DC20460.TheEPArequeststhata  separatecopyalsobesenttothecontactpersonlistedbelow(seeFORFURTHER x INFORMATIONCONTACT).Sendsubmissionscontainingsuchproprietaryor P confidentialbusinessinformation(CBI)directlytothefollowingaddress,andnot j( tothepublicdocket,toensurethatproprietaryorCBIisnotinadvertentlyplaced B inthepublicdocket:Attention:Mr.RobertoMorales,U.S.Environmental   ProtectionAgency,OAQPSDocumentControlOfficer,109_TW_ԀAlexander ! Drive,RoomC40402,_RTP_,NC,27711.)3 H ݌# ` (#` (# Ќ  ")3"  )32͋3  0 `   HandDelivery:AirandRadiationDocketandInformationCenter(MailCode %`" 6102T),AttentionDocketNumberOAR20040080,RoomB102,U.S.EPA, z'8!$ 1301ConstitutionAvenue,NW,Washington,DC20460.Suchdeliveriesare R)#& onlyacceptedduringtheDocketsnormalhoursofoperation,andspecial *+$( arrangementsshouldbemadefordeliveriesofboxedinformation.TheEPA -&* requestsaseparatecopyalsobesenttothecontactpersonlistedbelow(seeFOR B FURTHERINFORMATIONCONTACT).)3݌` (#` (# Ќ  Instructions.DirectyourcommentstoDocketIDNo.OAR20040080.TheEPAs   policyisthatallcommentsreceivedwillbeincludedinthepublicdocketwithoutchange   andmaybemadeavailableonlineat4  O  5  http://www.epa.gov/edocket6ORL]  7n,includinganypersonal  ` informationprovided,unlessthecommentincludesinformationclaimedtobe z8  ConfidentialBusinessInformation(CBI)orotherinformationwhosedisclosureis R  restrictedbystatute.DonotsubmitinformationthatyouconsidertobeCBIorotherwise *  protectedthrough_EDOCKET_,_regulations.gov_Ԁ_websites_,oremail.TheEPA_EDOCKET_  andtheFederal_regulations.gov_Ԁ_websites_Ԁare anonymousaccesssystems,whichmeans  theEPAwillnotknowyouridentityorcontactinformationunlessyouprovideitinthe p bodyofyourcomment.IfyousendanemailcommentdirectlytotheEPAwithoutgoing H through_EDOCKET_ԀOR_regulations.gov_,youremailaddresswillbeautomatically b  capturedandincludedaspartofthecommentthatisplacedinthepublicdocketandmade : availableontheinternet.Ifyousubmitanelectroniccomment,theEPArecommends   thatyouincludeyournameandothercontactinformationinthebodyofyourcomment ! andwithanydiskorCDROMyousubmit.IftheEPAcannotreadyourcommentdueto #  technicaldifficultiesandcannotcontactyouforclarification,theEPAmaynotbeableto %X" consideryourcomment.Electronicfilesshouldavoidtheuseofspecialcharacters,any r'0!$ formofencryption,andbefreeofanydefectsorviruses.Foradditionalinformation J)#& aboutEPAspublicdocketvisit_EDOCKET_ԀonlineorseetheFederalRegisterofMay "+$( 31,2002(67FR38102). ,&* Docket.Alldocumentsinthedocketarelistedinthe_EDOCKET_Ԁindexat B http://www.epa.gov/edocket.Althoughlistedintheindex,someinformationisnot  publiclyavailable,i.e.,CBIorotherinformationwhosedisclosureisrestrictedbystatute.   Certainothermaterial,suchascopyrightedmaterial,isnotplacedontheinternetandwill   bepubliclyavailableonlyin_hardcopy_Ԁform.Publiclyavailabledocketmaterialsare  ` availableeitherelectronicallyin_EDOCKET_ԀorinhardcopyattheEPADocketCenter z8  (AirDocket),EPAWest,RoomB108,1301ConstitutionAvenue,NW.,Washington, R  DC20004.TheDocketCenterisopenfrom8:30a.m.to4:30p.m.,Mondaythrough *  Friday,excludinglegalholidays.ThetelephonenumberforthePublicReadingRoomis  (202)5661744,andthetelephonenumberfortheAirDocketis(202)5661742.  PublicHearing.Peopleinterestedinpresentingoraltestimonyorinquiringastowhether p ahearingistobeheldshouldcontactMs.CorlisMcCormick,SourceMeasurement H TechnologyGroup,EmissionMeasurementCenter(D24302),U.S.Environmental b  ProtectionAgency,ResearchTrianglePark,NC,27711,telephonenumber: : (919)541-5545,atleast2daysinadvanceofthepublichearing.Peopleinterestedin   attendingthepublichearingmustalsocallMs.McCormicktoverifythetime,date,and ! locationofthehearing.Thepublichearingwillprovideinterestedpartiestheopportunity #  topresentdata,views,orargumentsconcerningtheproposedchangestoMethod301.If %X" apublichearingisheld,itwillbeheldat10:00a.m.intheEPA'sAuditoriuminResearch r'0!$ TrianglePark,NorthCarolina,oratanalternatesitenearby. J)#&  FORFURTHERINFORMATIONCONTACT :Forinformationconcerningthe "+$( proposedstandards,contactMr.GaryMcAlister,SourceMeasurementTechnology -&* Group,EmissionMeasurementCenter(D24302),U.S.EnvironmentalProtection B Agency,ResearchTrianglePark,NorthCarolina27711,telephonenumber:(919)541  1062,electronicmailaddress:mcalister.gary@epa.gov.    SUPPLEMENTARYINFORMATION :   PreambleOutline  h  ` Theinformationinthispreambleisorganizedasfollows. @  I.GeneralInformation Z  A.DoesthisActionApplytoMe? F  B.WhatShouldIConsiderasIPrepareMyCommentsfortheEPA? 2  C.AvailabilityoftheProposedRule   II.Introduction   III.WhatchangesAreWeProposing?   (8x]),-./012A.UsePlainLanguage  B.ReorganizeMethod301  C.CorrectTechnicalErrors x D.MakeTechnicalRevisions d IV.WhataretheAdministrativeRequirements? P A.ExecutiveOrder12866RegulatoryPlanningandReview ~< B.PaperworkReductionAct j( C.RegulatoryFlexibilityAct(_RFA_) V D.UnfundedMandatesReformAct B E.ExecutiveOrder13132Federalism . F.ExecutiveOrder13175ConsultationandCoordinationwithIndianTribal   Governments ! G.ExecutiveOrder13045ProtectionofChildrenfromEnvironmentalHealthRisksand ! SafetyRisks "  G(88H.ExecutiveOrder13211,ActionsConcerningRegulationsThatSignificantlyAffect #  EnergySupply,Distribution,orUse $t! I.NationalTechnologyTransferandAdvancementActof1995 %`"  I.GeneralInformation  z'8!$ A.DoesthisActionApplytoMe? R)#&  ` Method301affects/appliestoyouifyouwanttoproposeatestmethodtomeetan *+$( EPArequirementinabsenceofavalidatedmethod. -&* B.WhatShouldIConsiderasIPrepareMyCommentsfortheEPA? B  ` 1.SubmittingCBI.DonotsubmitthisinformationtotheEPAthrough  _EDOCKET_,_regulations.gov_,oremail.Clearlymarkthepartoralloftheinformation   thatyouclaimtobeCBI.ForCBIinformationinadiskorCDROMthatyoumailtothe   EPA,marktheoutsideofthediskorCDROMasCBIandthenidentifyelectronically  ` withinthediskorCDROMthespecificinformationthatisclaimedasCBI.Inaddition z8  toonecompleteversionofthecommentthatincludesinformationclaimedasCBI,acopy R  ofthecommentthatdoesnotcontaintheinformationclaimedasCBImustbesubmitted *  forinclusioninthepublicdocket.Informationsomarkedwillnotbedisclosedexceptin  accordancewithproceduressetforthin40CFRPart2.   ` 2.TipsforPreparingYourComments.Whensubmittingcomments,remember p to: H  ` _i_.Identifytherulemakingbydocketnumberandotheridentifyinginformation b  (e.g.,subjectheading,FederalRegisterproposalpublicationdateandreferencepage : number(s)).    ` ii.FollowdirectionsTheEPAmayaskyoutorespondtospecificquestionsor ! organizecommentsbyreferencingaCodeofFederalRegulations(CFR)partorsection #  number. %X"  ` iii.Explainwhyyouagreeordisagree;suggestalternativesandprovidesubstitute r'0!$ languageforyourrequestedchanges. J)#&  ` iv.Describeanyassumptionsandprovideanytechnicalinformationand/ordata "+$( thatyouused. ,&*  ` v.Ifyouestimatepotentialcostsorburdens,explainhowyouarrivedatyour B estimateinsufficientdetailtoallowforittobereproduced.   ` vi.Providespecificexamplestoillustrateyourconcerns,andsuggestalternatives.    ` vii.Explainyourviewsasclearlyaspossible,avoidingtheuseofprofanityor   personalthreats.  `  ` viii.Makesuretosubmityourcommentsbythespecifiedcommentperiod z8  deadline. R   ` _Commenters_Ԁwishingtosubmitproprietaryinformationforconsiderationmust *  clearlydistinguishsuchinformationfromothercommentsandclearlylabelitasCBI.  Sendsubmissionscontainingsuchproprietaryinformationdirectlytothefollowing  address,andnottothepublicdocket,toensurethatproprietaryinformationisnot p inadvertentlyplacedinthedocket:Attention:Mr.RobertoMorales,U.S.Environmental H ProtectionAgency,OAQPSDocumentControlOfficer,109_TW_ԀAlexanderDrive,Room b  C40402,_RTP_,NC,27711.TheEPAwilldiscloseinformationidentifiedasCBIonlyto : theextentallowedbytheproceduressetforthin40CFRPart2.Ifnoclaimof   confidentialityaccompaniesasubmissionwhenitisreceivedbytheEPA,theinformation ! maybemadeavailabletothepublicwithoutfurthernoticetothe_commenter_. #  C.AvailabilityoftheProposedRule %X"  ` Inadditiontobeingavailableinthedocket,anelectroniccopyoftheproposed r'0!$ changestoMethod301isalsoavailableontheInternetthroughtheTechnologyTransfer J)#& Network(TTN).Followingsignature,acopyofMethod301willbepostedontheTTNs "+$( policyandguidance_pagefornewlyproposedorpromulgatedrules ,&* http://www.epa.gov/ttn/oarpg.TheTTNprovidesinformationandtechnologyexchange B invariousareasofairpollutioncontrol.IfmoreinformationregardingtheTTNis  needed,calltheTTNHELPlineat(919)541-5384.     II.Introduction     XXX ` TodaysactionproposestoamendEPAsMethod301;FieldValidationof  ` PollutantMeasurementMethodsfromVariousWasteMedia.Method301canbefound z8  inAppendixAof40CFR,Part63(TestMethods).Method301waspromulgatedwith R  40CFR,Part63,SubpartD(RegulationsGoverningComplianceExtensionsforEarly *  ReductionsofHazardousAirPollutants)(58FR27338,June13,1991)pursuantto  Section112oftheCleanAirAct(asamendedin1990).YouwoulduseMethod301  wheneveryouproposetouseatestmethodtomeetanEPArequirementinabsenceofa p validatedmethod.Themethodspecifiesproceduresfordetermininganddocumentingthe H precisionandbiasofmeasuredconcentrationsfromvariousmedia(e.g.,sludge,exhaust b  gas,wastewater)atthelevelofanapplicablestandardforasource.Bias(orsystemic : error)isestablishedbycomparingyourproposedmethodagainstareferencevalue.A   correctionfactorisemployedtoeliminate/minimizebias.Thiscorrectionfactoris ! establishedfromdataobtainedduringyourvalidationtest.Methodsthathavebias #  correctionfactorsoutsideaspecifiedrangeareconsideredunacceptable.Method %X" precision(orrandomerror)atthelevelofthestandardmustbedemonstratedtobeas r'0!$ preciseasthevalidatedmethodforacceptance. J)#&  ` Todaysactionproposestoamendthoseprovisionsbycorrectingtechnicalerrors, "+$( andsimplifyingandclarifyingprocedures.SectionIIofthispreamblediscussesthe ,&* proposedMethod301rule,andSectionIIIpresentstheadministrativerequirementsfor B thisaction.  &  III.WhatChangesAreWeProposing?  C   A.UsePlainLanguage' K    ` IncompliancewithPresidentClintonsJune1,1998,ExecutiveMemorandumon  ` PlainLanguageingovernmentwriting,Method301hasbeenrewritteninplainlanguage. z8  TheuseofplainlanguageclarifiestherequirementsofMethod301,thus,reducingthe R  burden(time)associatedwithunderstandingtheMethod.WhenMethod301refersto *   you,itmeanstheowneroroperatoroftheaffectedsource.  B.ReorganizeMethod301   ` WehavereorganizedtheinformationinMethod301tomakeiteasiertofollow p therequirementsandtounderstandtherelationshipsamongthevariousrequirements. H Thereorganizationdidnotcreatenewrequirements,butitdoesincorporatevarious b  correctionstotechnicalerrorsandtechnicalrevisions.Thesecorrectionsandrevisions,as : wellastherationaleforthechanges,arediscussedinSectionsIIICandDofthis   preamble. !  ` Section17.0oftodaysrule(WhatdetectionlimitsmustIuse?)shallapply #  insteadofSection9.0(PracticalQuantitationLimits)ofthepromulgatedMethod301 %X" rule.WehaveretainedallothersectionsfromthepromulgatedMethod301,butyouwill r'0!$ findtheminnewplaces.Wherenecessaryforclarity,wehaveputtheinformationfrom J)#& onesectionofPromulgatedMethod301intoseveralnewsections.Someinformationhas "+$( beenputintotablesattheendoftheMethod.Section2.0presentsnewinformation.It ,&* hasbeenaddedtoexplainwhenyoumustuseMethod301andtoidentifytherequirement B forreceivingwrittenapprovalfromtheAdministratorbeforeusingthealternativetest  method.Table1ofthispreamblespecifieswherethesectionsinthepromulgated   Method301arefoundintheproposedMethod301rule.    ` TheequationsofthepromulgatedMethod301havealsobeenamended.Someof  ` thepromulgatedequationshavebeenmodified;somehavebeenreplacedbyother z8  equations,andsomehavesimplybeenrenumberedorreordered.Thetechnicalreasons R  forthechangestotheequationsarediscussedinSectionIII.Dofthispreamble.Table2 *  indicateswhethereachequationintheproposedamendedrulehaschangedfromthe  promulgatedrule.Equations3015and30110(correctionfactorswhenusingisotopic  spikingandpairedsamplingsystemswithavalidatedtestmethod_comparison)of p promulgatedMethod301rulehavebeenremovedforthereasonsdiscussedinSectionIII H Dofthispreamble. b  _    *d"fddd Xdd Xdd X(#(#,Xdd , dd ,dd ," dd +  0&BB 0Table1.ComparisonofSectionsinProposedMethod301.toThosein d PromulgatedMethod301. Q""@)P"   QProposedNewSection G""6$ "" GPromulgatedMethodSection E;)   "" E(GX(X  UsingMethod301 3)$ P  3d[ ' P '#(XX(GE[# K"> P ?1.0?K(GX(X1.0 J"=8  ?1.0 ?" JWhatisthepurposeofMethod301? K">  " ?1.1?K1.1 J"=8   ?1.1 ?" JApplicability P"C  " i@2.0@P2.0 J"=8j (  @2.0 @" JWhenmustIuseMethod301? *"j ( " *None *"j (" * P"Cj ( i " @3.0@P3.0 J"=8 @3.0 @" JWhatdoesMethod301include?#(XX(G^\#(GX(X *"" *1.1.2#(XX(G~_#(GX(X *"" * K">" @4.0@K4.0 J"=8+  @4.0 @" JHowdoIperformMethod301? K">+ " 333333?1.2333333?K1.2 J"=8+  333333?1.2 333333?" JPrinciple 7"*+ " 7  ReferenceMaterialsandPerformanceAudits 6")$A  " 6a *"A " * K">A " @5.0@K5.0 J"=8  @5.0 @" JWhatreferencematerialsmustIuse? K"> " @3.0@K3.0 J"=8  @3.0 @" JReferenceMaterials K"> " @6.0@K6.0 J"=83  @6.0 @" JHowdoIconducttheperformanceaudit? K">3 " @4.0@K4.0 J"=83 ! @4.0 @" JEPAPerformanceAuditMaterials ."!3 "" .  SamplingProcedures 6")$I# " 6{e *"I$" * K">I%" @7.0@K7.0 J"=8& @7.0 @" JWhatsamplingproceduresmustIuse? K">'" @5.0@K5.0 J"=8( @5.0 @" JProcedureforDeterminationofBias ) andPrecisionintheField K">e*"  @8.0 @K8.0 J"=8+  @8.0  @" JHowdoIensuresamplestability? I"<,"   @8 @I8 H";6-   @8  @" HProcedureforSampleStabilityinBias . andPrecisionEvaluations ."!/" .  BiasandPrecision 6")$0 " 6i *"1" * K">2" "@9.0"@K9.0 J"=8s13 "@9.0 "@" JWhataretherequirementsforbias? *"s14" *1.2.1 *"s15" *Bias L"?s16" $@10.0$@L10.0 K">97 $@10.0 $@" KWhataretherequirementsforprecision? *"8" *1.2.2 *"9" *Precision L"?:" &@11.0&@L11.0#(XX(G_#(GX(X K">9#; &@11.0 &@" KWhatcalculationsmustIperformfor #< isotopicsampling?#(XX(Gl#(GX(X K">=" ffffff@6.1ffffff@K6.1 J"=8#> ffffff@6.1 ffffff@" JIsotopicSampling L"?#?" (@12.0(@L12.0 K">9?!@ (@12.0 (@" KWhatcalculationsmustIperformfor ?!A comparisonwithavalidatedmethodifI "B amusingpairedsamplingsystems? *""C" *6.2.1 *"?!D" *Comparisonwithavalidatedmethod: ?!E PairedSamplingSystems I?"F" *@13.0*@I13.0 H>9$G *@13.0 *@ HWhatcalculationsmustIperformfor $H comparisonwithavalidatedmethodifI $I amusing#(XX(Gm#(GX(XԀquadrupletreplicatesampling %eJ systems? 'k&) K '6.2.2 '$L 'Comparisonwithavalidatedmethod:#(XX(Gvq#(GX(X $M QuadrupletReplicateSampling $N Systems L"?%eO ,@14.0,@L_14.0 K">9'!P ,@14.0 ,@" KWhatcalculationsmustIperformfor#(XX(Gir#(GX(X '!Q analytespiking? K">(E"R" 333333@6.3333333@K6.3 J"=8'!S 333333@6.3 333333@" JAnalyteSpiking L"?'!T" .@15.0.@L15.0 K">9)#U .@15.0 .@" KHowdoIconductfollowuptests? J"=)#V"  &@11&@J11 I"<7)#W  &@11 &@" IFollowupTesting *")#X" * *"7+$Y" *  OptionalRequirements 3"&!7+$Z " 3gv *"7+$[" * L"?7+$\" 0@16.00@L16.0 K">9,M&] 0@16.0 0@" KHowdoIuseandconductruggedness ,M&^ testing? I"<S-'_"  @7@I7 H";6,M&`  @7 @" HRuggedness_Testing P""?,M&a" 1@17.01@P__17.0_ O"">9 d 1@17.0 1@"" O WhatdetectionlimitsmustIuse? M""< d""  "@9"@M9 L"";6 d  "@9 "@"" LPracticalLimitofQuantitation ' d"" ' '  '  OtherRequirementsandInformation 0&!   0z '  ' L"?  2@18.02@L18.0 K">9B   2@18.0 2@" KHowdoIapplyforapprovaltousean B   alternativemethod? J"= "  $@10$@J10 I"<7B    $@10 $@" IFieldValidationReportRequirements B    L"?" 3@19.03@L19.0 K">9^0 3@19.0 3@" KHowdoIrequestawaiver? *"^0" *1.1.1 ^0 and12 *""" *ProcedureforObtainingaWaiver L"?^0" 4@20.04@L20.0 K">9zL 4@20.0 4@" KWhatdefinitionsapplytothismethod? I"<zL"  @2@I2 H";6zL  @2 @" HDefinitions P""?zL" 5@21.05@P21.0 O"">9 5@21.0 5@"" OWherecanIfindadditionalinformation? N""=""  *@13*@N13 M""<7  *@13 *@"" M#(XX(Gs#(GX(XBibliography#(XX(G#(  "" (    %/*k"lddXdd X dd dd " dd " d"f(#(#,9dd ,z dd ,dd ,dd +  +!BB +(&m%X(X Table2.EquationsinProposedMethod301 L"";$d" LThefollowingequationinproposedMethod301...#(XX%(&m#(&m%X(X C""2$"" Cis... @""/!"" @#(XX%(&m#(&m%X(XThefollowing  equationin  promulgated   Method301... 5+& X  "" 53011 '  'DifferenceinSampleResults '   'new '   ' .""   .3017 .""r 0 "" .RelativeMagnitudeofBias .""r 0 "" .new .""r 0"" . 7"&r 0"" 7  3019 @"/!" @RelativeMagnitudeofBiasforComparing  AgainstValidatedMethodsUsingPaired t  SamplingSystems @"/!L " @  new @"/!" @ D"3!"" D#(XX%(&m# @ (GX(X EquationsWhenUsingIsotopicSpiking #(XX(G# 3)$ "" 3(GX(X3014 'P  'NumericalValueofBias#(XX(G#(GX(X 'P  'arevisionof 'P  '3011#(XX(G&#(GX(X *"P  *3015 *"f" *StandardDeviation#(XX(GȊ#(GX(X *"f" *thesameas *"f" *3012#(XX(Gu#(GX(X *"f" *3016 *"" *tTest *" " *areplacementfor *"!" *#(XX(G#(GX(X3013and3014#(XX(G!#(GX(X *""" *3018 *"X#" *RelativeStandardDeviation *"X$" *arevisionof *"X%" *#(XX(Gr#(GX(X3016#(XX(G#(GX(X 7"*X&" 7 @ #(XX(GЎ# @ (GX(X EquationsWhenComparingAgainstValidatedMethod#(XX(Ga#(GX(XԀUsing #(XX(G׏#(GX(XԀ PairedSamplingSystems 6")$n'"" 63012#(XX(G"#(GX(X *" (" *StandardDeviation *" )" *forpairedsampling  * systems,a + replacementfor#(XX(G#(GX(X *"P," *#(XX(G#(GX(X3012#(XX(G'#(GX(X *" -" *3013#(XX(Gn#(GX(X *"." *tTest *"/" *thesameas#(XX(Gߒ#(GX(X *"0" *#(XX(G#(GX(X3019#(XX(G#(GX(X *"1" *30110#(XX(G9#(GX(X *"B2" *Variance *"B3" *areplacementfor#(XX(G#(GX(X *"B4" *#(XX(GZ#(GX(X3017#(XX(Gƕ#(GX(X *"B5" *30111#(XX(G #(GX(X *"X6" *PooledVariance *"X7" *new *"X8" * *"X9" *30112#(XX(G#(GX(X *" :" *AlternativeTestMethodVariance *" ;" *areplacementfor#(XX(G#(GX(X *" <" *3019a *" =" *30113#(XX(GH#(GX(X *"J">" *Ftest *"J"?" *thesameas#(XX(G#(GX(X *"J"@" *#(XX(G#(GX(X3018#(XX(G#(GX(X 7"*J"A" 7 EquationsWhenComparingAgainstValidatedMethodUsing #(XX(GD#(GX(XԀ QuadrupletReplicateSampling #`B Systems #(XX(G#(GX(X 6")$h$&C"" 630114#(XX(G|#(GX(X *"%|D" *Bias *"%|E" *thesameas#(XX(G#(GX(X *"%|F" *#(XX(G#(GX(X30112#(XX(G #(GX(X *"%|G" *30115#(XX(GS#(GX(X *"' H" *AlternativeTestMethodVariance#(XX(Gŝ#(GX(X *"' I" *thesameas#(XX(GQ#(GX(X *"' J" *#(XX(GȞ#(GX(X30111#(XX(G4#(GX(X 4*' K" 4EquationsWhenUsingAnalyteSpiking 6")$n(,"L" 630116#(XX(G|#(GX(X *")#M" *Bias *")#N" *thesameas#(XX(GR#(GX(X *")#O" *#(XX(G#(GX(X30114#(XX(Gc#(GX(X *")#P" *30117#(XX(G#(GX(X *"+$Q" *tTest#(XX(G#(GX(X *"+$R" *areplacementfor#(XX(G#(GX(X *"+$S" *#(XX(G #(GX(X3014#(XX(Gx#(GX(X *"+$T" *30118#(XX(G#(GX(X *"t,2&U" *StandardDeviation#(XX(G1#(GX(XԀforSpikedSamples *"t,2&V" *arevisionof *"t,2&W" *#(XX(G#(GX(X30113#(XX(Ge#(GX(X *"t,2&X" *30119#(XX(G#(GX(X *"-'Y" *StandardDeviation#(XX(G#(GX(XԀfor_Unspiked_ԀSamples#(XX(G#(GX(X *"-'Z" *areplacementfor#(XX(G#(GX(X *"-'[" *#(XX(G#(GX(X30113#(XX(G#(GX(XԀand3016#(XX(GE#(GX(X *"-'\" *30120#(XX(G#(GX(X *" d" *#(XX(G#(GX(XFtest *" d" *new *" d" * ."" d" .30121 ."" "" .PooledStandardDeviation#(XX(Go#(GX(X ."" "" .areplacementfor#(XX(G#(GX(X ."" "" .#(XX(G #(GX(X30115#(XX(Gz#(GX(X(   "" (#(XX(G«#    C.CorrectTechnicalErrors B  ` SomeoftheequationsinpromulgatedMethod301areincorrect.Weare  proposingtocorrecttheseequationswithtodaysaction.Foradiscussionofnew   equationsduetotechnicalrevisions,seeSectionIIIDofthispreamble.Werevised   severalequationstoclarifytheirintent.Underthenewnumberingsystem,therevised  ` equationsare3014(numericalvalueofbias),3016(tTest),3018(relativestandard z8  deviation),30118(standarddeviationforspikedsamples),and30119(standard R  deviationforunspikedsamples).Thesechangeswereeditorial/definingchangesandnot *  technicalchanges.Forexample,weaddedorchangedsubscriptsorredefinedavariable.   ` WeaddedEquations3011,3017,and3019.Equation3011isusedtocalculate  thedifferenceinminimumandmaximumstoragetimesunderthenewsamplestability p procedures.Equation3017isusedtocalculaterelativemagnitudeofbiasforisotopic H spiking.Thisnewequationwasneededwhenwedroppedtheuseofcorrectionfactors. b  Likewise,Equation3019wasneededforcalculatingrelativemagnitudeofbiaswhen : comparingagainstavalidatedmethodusingpairedsamplingsystems.    ` WealsoaddedEquation30111andchangedEquations30112,30117,30118, ! and30119tocorrecttechnicalerrorsinpromulgatedMethod301.Equations30111 #  (PooledVariance)and30112(AlternativeTestMethodVariance)arebeingproposedto %X" correctatechnicalerrorinthepromulgatedmethod.Additionandsubtractioncanonly r'0!$ beperformedonthevariance.Itcannotbeperformedonthestandarddeviation.The J)#& proposedEquation30111isanewequationthatcalculatesthepooledvarianceofboth "+$( methodswhencomparingagainstvalidatedmethodsusingpairedsamplingsystems.The ,&* proposedEquation30112replacesthestandarddeviationwiththevariance. B  ` Equations30117(calculationofthetest tstatistic)and30121(calculationof  thepooledstandarddeviation)werechangedbecausethedivisorwaswrong.Equation   30120(Ftest)wasaddedsothatthetestercoulddetermineifthespikedand_unspiked_   sampleshadthesameprecision,therebyallowingthemtobepooledtocalculatethe  ` overallprecision. z8   ` TheproposedEquation3012(StandardDeviation)replacesthepromulgated R  Equation3012whencomparingagainstvalidatedmethodsusingpairedsampling *  systems.Thetextinpromulgated6.2.1.4directstheanalysttodeterminethemeanofthe  pairedsampledifferencesbysubstitutingdm(meanofthepairedsampledifferences)and  _di_(standarddeviationofthedifferences)forSiandSmintheproposedEquation3012. p WecreatedtheproposedEquation3012toincorporatethesechanges. H ! !D.MakeTechnicalRevisions b   ` WeareproposingfivemajortechnicalchangestoMethod301.Thesetechnical : changesincludethefollowing:    ` (1)ReplacingthePracticalLimitofQuantitation(PLQ)withaprocedureto ! determinetheLimitofDetection, #   ` (2)Revisingthebiasacceptancecriteriaandeliminatingcorrectionfactors, %X"  ` (3)Revisingprecisionacceptancecriteriawhenusinganalytespiking, r'0!$  ` (4)Allowinganalytespikingevenwhenthereisanexistingtestmethod,and J)#&  ` (5)Establishingnewproceduresforensuringsamplestability. "+$(  ` 1.PracticalLimitofQuantitation.Weareproposingtoreplacethedetermination ,&* %/ %TRY,3' LetterX3' Letter 3' Letter3'T %  ofthePLQwithaproceduretodeterminetheLimitofdetection(_LOD_).Thepurposeof B establishingameasurementlimitistoensurethatatestmethodisappropriateforits  intendeduse.The_LOD_Ԁisabetterparameterforthispurpose.    ` ThePLQisdefinedasthelevelorconcentrationatwhichtheprecisionofatest   methodreachesanacceptablevalue.Thereareseveralproblemswiththisconcept.The  ` firstistheideathatthereisanabsolutevalueforacceptableprecision.Toacertain z8  extent,atestercancompensateforimprecisionbycollectingadditionaldatasothereisno R  absolutelevelatwhichtheimprecisionofatestmethodbecomessogreatthatthemethod *  isnolongeruseful.Thisconceptworksbestwhentheprecisionofthetestmethodis  independentoftheconcentrationoftheanalytebeingmeasured.Astheconcentrationof  theanalyteincreases,theimprecisionofthemethodasapercentageofthemeasured p quantitydecreases.Inthiscase,therelativeimprecisionwillactuallydecreaseasthe H quantitymeasuredincreases. b   ` However,formostenvironmentalmeasurements,itappearsthattheprecisionisa : functionoftheconcentrationoftheanalytebeingmeasured.Thus,therelative   imprecisionwillnotdecreaseasthequantitymeasuredincreases.Inthiscase,thePLQ ! hasnomeaning. #   ` The_LOD_Ԁistheminimumlevelorconcentrationofananalytethatproducesa %X" signalorresponsethatisdistinguishablefromthesignalorresponseproducedwhenno r'0!$ analyteispresent.Thisisameasurablequantitythatcanbedeterminedregardlessofthe J)#& methodsprecisionorwhetherthatprecisionvarieswiththeleveloftheanalyte.Forall "+$( ofthesereasons,webelievethatthe_LOD_Ԁisamoreusefulparametertocharacterizeatest ,&* methodsperformance. B  ` 2.BiasAcceptanceCriteria.Wearealsoproposingtochangetheacceptance  criteriaforthebiasinaproposedalternativemethodfrom+30%to+10%and   concurrentlytoeliminatetherequirementforcorrectingalldatacollectedwiththe   method.Webelievethattwelvepairsofresultsfromasinglesourcearenotsufficientto  ` allowustoestablishacorrectionfactorthatcanorshouldbeappliedtoallfutureusesof z8  themethod.Inaddition,keepingtrackofcorrectionfactorstoensurethattheyareapplied R  tofutureusesofthemethodisahugeadministrativeburdenbothfortheusersofthe *  methodandtheregulatoryagencieswhooverseeitsuse.Ifwedonotusecorrection  factors,methodbiasesofupto30percentareundesirablylarge.Therefore,weare  proposingtoreducetheacceptablebiasto+10%andeliminatetherequirementtocorrect p thedata.Withthischange,thebiasofalternativemethodswillbeacceptable;thecriteria H forusingthealternativetestmethodatsimilarsourceswillbeclear,andthe b  administrativeburdenwillbereduced. :  ` 3.PrecisionAcceptanceCriteria.Weareproposingtochangetheacceptance   criteriaformethodprecisionwhenusinganalytespikingfrom+50%to+20%.In ! addition,weareproposingtoeliminatetherequirementfordifferentnumbersofreplicate #  samplesdependingonthemethodsrelativeprecision.Allfuturetestingusingan %X" alternativetestmethodatsimilarsourceswillrequireonlythreereplicatesamples.The r'0!$ requirementintheexistingprocedurewasanattempttocompensateforthepoorer J)#& precisionofsomecandidatealternativetestmethodsbyincreasingtheamountofdatathat "+$( theuserwasrequiredtocollect.Whilemoredatadoescompensatefortheimprecisionof ,&* anyfuturedatacollectedwiththemethod,allowingcandidatealternativetestmethods B withpoorprecisioncreatesotherproblems.Oneproblemisthatpoorprecisionmakesit  moredifficulttodetectpotentialbiasinatestmethod.Forthisreason,weareproposing   totightentheacceptancecriteriafortheprecisionofcandidatealternativetestmethods.    ` 4.AnalyteSpiking.Wearealsoproposingtoallowthetestertouseanalyte  ` spikingtoevaluateanalternativetestmethodevenwhenthereisanexistingcompliance z8  testmethod.IftheNESHAPspecifiesatestmethod,promulgatedMethod301requires R  thetestertoevaluateanalternativemethodbydirectcomparison.Webelievethatthisis *  toorestrictiveinsomecases.Forexample,achangeinprocesstechnologymaycausea  previouslyunbiasedtestmethodtodevelopaninterferencethatbiasesitsresults.Ifthe  testerisrequiredtocomparethealternativetestmethodtotheexistingtestmethod,the p alternativemethodcouldneverdemonstrateacceptableperformanceifitwereunbiased. H Webelievethatitissufficientforanalternativemethodtodemonstrateacceptable b  performancebyusingtheanalytespikingprocedureandthatthisisareasonable : alternativetodirectcomparison.    ` 5.SampleStability.Finally,weareproposingproceduresforsamplestability. ! Method301previouslylackedspecificproceduresforensuringthatsamplescollected #  underproposedalternativemethodswereanalyzedwithinanappropriatetime.New %X" Section8.4includesarequirementtocalculatethedifferenceinthesamplingresultsat r'0!$ theminimumandmaximumstoragetimes,determinethestandarddeviationofthe J)#& differences,andtestthedifferenceintheresultsforstatisticalsignificancebycalculating "+$( thetstatisticanddeterminingifthemeanofthedifferencesbetweentheinitialresults ,&* andtheresultsafterstorageissignificantatthe95percentconfidencelevel.Wehave B alsoaddedTable1tocomparethecalculatedtstatisticwiththecriticalvalueofthet  statistic.Theseproceduresarenecessarytoensuresamplestabilityandshouldhavebeen   includedinpromulgatedMethod301.     III.WhatAreTheAdministrativeRequirements  ?   `   A.ExecutiveOrder12866RegulatoryPlanningandReview   z8   ` UnderExecutiveOrder12866(58FR51735,October4,1993),theEPAmust R  determinewhethertheregulatoryactionis"significant"and,therefore,subjecttoreview *  bytheOfficeofManagementandBudget(OMB)andtherequirementsoftheExecutive  Order.TheExecutiveOrderdefines"significantregulatoryaction"asonethatislikelyto  resultinarulethatmay: p  ` (1)Haveanannualeffectontheeconomyof$100millionormoreoradversely H affectinamaterialwaytheeconomy,asectoroftheeconomy,productivity,competition, b  jobs,theenvironment,publichealthorsafety,orState,local,ortribalgovernmentsor : communities;    ` (2)Createaseriousinconsistencyorotherwiseinterferewithanactiontakenor ! plannedbyanotheragency; #   ` (3)Materiallyalterthebudgetaryimpactofentitlements,grants,userfees,orloan %X" programs,ortherightsandobligationofrecipientsthereof;or r'0!$  ` (4)Raisenovellegalorpolicyissuesarisingoutoflegalmandates,thePresident's J)#& priorities,ortheprinciplessetforthintheExecutiveOrder. "+$(  ` Ithasbeendeterminedthatthisproposedregulatoryactionisnota"significant ,&* regulatoryaction"underthetermsofExecutiveOrder12866andis,therefore,notsubject B toOMBreview.   Z(88G! !B.  PaperworkReductionAct    ` Thisactiondoesnotimposeorchangetheinformationcollectionburdenunderthe   provisionsofthePaperworkReductionAct44U.S.C.3501,etseq.Burdenmeansthe  ` totaltime,effort,orfinancialresourcesexpendedbypersonstogenerate,maintain,retain, z8  ordiscloseorprovideinformationtoorforaFederalagency.Thisincludesthetime R  neededtoreviewinstructions;develop,acquire,install,andutilizetechnologyand *  systemsforthepurposesofcollecting,validating,andverifyinginformation,processing  andmaintaininginformation,anddisclosingandprovidinginformation;adjustthe  existingwaystocomplywithanypreviouslyapplicableinstructionsandrequirements; p trainpersonneltobeabletorespondtoacollectionofinformation;searchdatasources; H completeandreviewthecollectionofinformation;andtransmitorotherwisedisclosethe b  collectionofinformation. :  ` Anagencymaynotconductorsponsor,andapersonisnotrequiredtorespondto   acollectionofinformationunlessitdisplaysacurrentlyvalidOMBcontrolnumber.The ! OMBcontrolnumbersforEPAsregulationsarelistedin40CFRPart9and48CFR #  Chapter15.   %X" C.RegulatoryFlexibilityAct(_RFA_) r'0!$  ` The_RFA_Ԁgenerallyrequiresanagencytopreparearegulatoryflexibilityanalysis J)#& ofanyrulesubjecttonoticeandcommentrulemakingrequirementsunderthe "+$( AdministrativeProcedureActoranyotherstatuteunlesstheagencycertifiesthattherule ,&* willnothaveasignificanteconomicimpactonasubstantialnumberofsmallentities. B Smallentitiesincludesmallbusinesses,smallorganizations,andsmallgovernmental  jurisdictions.    ` Forthepurposesofassessingtheimpactsoftoday'sproposedruleonsmall   entities,smallentityisdefinedas:(1)Asmallbusinessthatmeetsthedefinitionsfor  ` smallbusinessbasedontheSmallBusinessAssociation(SBA)sizestandardswhich,for z8  thisproposedaction,areoperationsthathavefewerthan1,000employees;(2)Asmall R  governmentaljurisdictionthatisagovernmentofacity,county,town,schooldistrictor *  specialdistrictwithapopulationoflessthan50,000;and(3)Asmallorganizationthatis  anynotforprofitenterprisewhichisindependentlyownedandoperatedandisnot  dominantinitsfield. p  ` Afterconsideringtheeconomicimpactsoftodaysproposedruleonsmallentities, H Icertifythatthisproposedactionwillnothaveasignificanteconomicimpactona b  substantialnumberofsmallentities.Indeterminingwhetherarulehassignificant : economicimpactonasubstantialnumberofsmallentities,theimpactofconcernisany   significantadverseeconomicimpactonsmallentitiessincetheprimarypurposeofthe ! regulatoryflexibilityanalysisistoidentifyandaddressregulatoryalternatives which #  minimizeanysignificanteconomicimpactoftheproposedruleonsmallentities,(5 %X" U.S.C.603and604).Thus,anagencymaycertifythatarulewillnothaveasignificant r'0!$ economicimpactonasubstantialnumberofsmallentitiesiftherulerelievesregulatory J)#& burden,orotherwisehasapositiveeconomiceffectonallofthesmallentitiessubjectto "+$( therule.Thisproposedrulewillnotimposeanyrequirementsonsmallentities.Thisrule ,&* establishesproceduresforusingalternativemethods.Assuch,smallentitiesandother B sourcesarenotrequiredtocomplywiththisproposedrule,butmayelecttouseMethod  301.Theproposedruleoffersadditionalflexibilitytoallsources,includingsmallentities   thatmaybesubjecttorequirementsundertheCAA.Additionally,thisproposed   amendedruleclarifiesandsimplifiestheproceduresforusingalternativemethods. XXX(X We  ` continuetobeinterestedinthepotentialimpactsoftheproposedruleonsmallentities z8  andwelcomecommentsonissuesrelatedtosuchimpacts.#(XXXX#Ԁ R    D.UnfundedMandatesReformAct *   ` TitleIIoftheUnfundedMandatesReformActof1995(_UMRA_),PublicLaw  1044,establishesrequirementsforFederalagenciestoassesstheeffectsoftheir  regulatoryactionsonState,local,andtribalgovernmentsandtheprivatesector.Under p Section202ofthe_UMRA_,theEPAgenerallymustprepareawrittenstatement,including H costbenefitanalysis,forproposedandfinalruleswith"Federalmandates"thatmayresult b  inexpenditurestoState,local,andtribalgovernments,intheaggregate,ortotheprivate : sector,of$100millionormoreinanyoneyear.BeforepromulgatinganEPArulefor   whichawrittenstatementisneeded,Section205ofthe_UMRA_Ԁgenerallyrequiresthe ! EPAtoidentifyandconsiderareasonablenumberofregulatoryalternativesandadoptthe #  leastcostly,mostcosteffective,orleastburdensomealternativeiftheAdministrator %X" publisheswiththefinalruleanexplanationwhythatalternativewasnotadopted.Before r'0!$ EPAestablishesanyregulatoryrequirementsthatmaysignificantlyoruniquelyaffect J)#& smallgovernments,includingtribalgovernments,itmusthavedevelopedunderSection "+$( 203ofthe_UMRA_Ԁasmallgovernmentagencyplan.Theplanmustprovidefornotifying ,&* potentiallyaffectedsmallgovernments,enablingofficialofaffectedsmallgovernmentsto B havemeaningfulandtimelyinputinthedevelopmentofEPAregulatoryproposalswith  significantFederalintergovernmentalmandates,andinforming,educating,andadvising   smallgovernmentsoncompliancewiththeregulatoryrequirements.    ` WehavedeterminedthattodaysproposedamendedruledoesnotcontainFederal  ` mandatesforState,local,ortribalgovernmentsortheprivatesector.Therefore,this z8  proposedamendedruleisnotsubjecttotherequirementsofSections202and205ofthe R  _UMRA_.    *    E.ExecutiveOrder13132Federalism     ` ExecutiveOrder13132,entitled"Federalism"(64FR43255,August10,1999),  requirestheEPAtodevelopanaccountableprocesstoensure meaningfulandtimely p inputbyStateandlocalofficialsinthedevelopmentofregulatorypoliciesthathave H federalismimplications.""Policiesthathavefederalismimplications"isdefinedinthe b  ExecutiveOrdertoincluderegulationsthathave"substantialdirecteffectsontheStates, : ontherelationshipbetweenthenationalgovernmentandtheStates,oronthedistribution   ofpowerandresponsibilitiesamongthevariouslevelsofgovernment." !  ` UnderExecutiveOrder13132,theEPAmaynotissuearegulationthathas #  federalismimplications,thatimposessubstantialdirectcompliancecosts,andthatisnot %X" requiredbystatute,unlesstheFederalgovernmentprovidesthefundsnecessarytopaythe r'0!$ directcompliancecostsincurredbyStateandlocalgovernments,ortheEPAconsults J)#& withStateandlocalofficialsearlyintheprocessofdevelopingtheproposedregulation. "+$( TheEPAalsomaynotissuearegulationthathasfederalismimplicationsandthat ,&* preemptsStatelawunlesstheAgencyconsultswithStateandlocalofficialsearlyinthe B processofdevelopingtheproposedregulation. p    (5H08Z ` Todaysproposedamendedrulewillnothavefederalismimplications.Theywill   nothavesubstantialdirecteffectsontheStates,ontherelationshipbetweenthenational   governmentandtheStates,oronthedistributionofpowerandresponsibilitiesamongthe  ` variouslevelsofgovernment,asspecifiedinExecutiveOrder13132.Todaysproposed z8  amendedruleclarifiesandsimplifiestheproceduresforusingalternativemethods.Thus, R  therequirementsofSection6oftheExecutiveOrderdonotapply.  *    F.  [ ExecutiveOrder13175ConsultationandCoordinationwithIndianTribal  Governments   ` ExecutiveOrder13175,entitled ConsultationandCoordinationwithIndian p TribalGovernments(65FR67249,November9,2000),requiresEPAtodevelopan H accountableprocesstoensure meaningfulandtimelyinputbytribalofficialsinthe b  developmentofregulatorypoliciesthathavetribalimplications.Theproposedamended : ruledoesnothavetribalimplications,asspecifiedinExecutiveOrder13175.The   proposedactionservestoclarifyandsimplifyproceduresforusingalternativemethods. ! Therefore,ExecutiveOrder13175doesnotapplytotheproposedamendedrule. #    G. SExecutiveOrder13045ProtectionofChildrenfromEnvironmentalHealthRisks %X" andSafetyRisks r'0!$  ` ExecutiveOrder13045, ProtectionofChildrenfromEnvironmentalHealthRisks J)#& andSafetyRisks(62FR19885,April23,1997),appliestoanyrulethattheEPA "+$( determinesis:(1)"economicallysignificant"asdefinedunderE.O.12866;and(2) ,&* concernsanenvironmentalhealthorsafetyriskthattheEPAhasreasontobelievemay B haveadisproportionateeffectonchildren.Iftheregulatoryactionmeetsbothcriteria,the  EPAmustevaluatetheenvironmentalhealthorsafetyeffectsoftheplannedruleon   childrenandexplainwhytheplannedregulationispreferabletootherpotentially   effectiveandreasonablealternativesconsideredbytheEPA.  `  ` TheEPAinterpretsExecutiveOrder13045asapplyingonlytothoseregulatory z8  actionsthatarebasedonhealthorsafetyrisks,suchthattheanalysisrequiredunder R  Section5501oftheExecutiveOrderhasthepotentialtoinfluencetheregulation.The *  proposedamendedruleisnotsubjecttoExecutiveOrder13045becauseitisnot  economicallysignificantasdefinedinExecutiveOrder12866,andbecausethisproposed  amendedruleisnotbasedonhealthorsafetyrisks.Thus,ExecutiveOrder13045does p notapplytothisproposedamendedrule. H   H.ExecutiveOrder13211,ActionsConcerningRegulationsThatSignificantlyAffect b  EnergySupply,Distribution,orUse :  ` ThisruleisnotsubjecttoExecutiveOrder13211, ActionsConcerning   RegulationsThatSignificantlyAffectEnergySupply,Distribution,orUse ! (66FR28355(May22,2001))becauseitisnotasignificantregulatoryactionunder #  ExecutiveOrder12866. %X" I.NationalTechnologyTransferandAdvancementActof1995   r'0!$  ` Section112(d)oftheNationalTechnologyTransferandAdvancementActof J)#& 1995(_NTTAA_),PublicLawNo.104113,Section12(d)915U.S.C.272note),directsall "+$( Federalagenciestousevoluntaryconsensusstandardsinsteadofgovernmentunique_ ,&* Ї Method301Page24of62  B standardsintheirregulatoryactivitiesunlesstodosowouldbeinconsistentwith  applicablelaworotherwiseimpractical.    ` Voluntaryconsensusstandardsaretechnicalstandards(e.g.,materials   specifications,testmethods,samplingprocedures,andbusinesspractices,etc.)thatare  ` developedoradoptedbyoneormorevoluntaryconsensusstandardsbodies.Examplesof z8  organizations,generallyregardedasvoluntaryconsensusstandardsbodies,includethe R  AmericanSocietyforTestingandMaterials(ASTM),theNationalFireProtection *  Association(_NFPA_),andtheSocietyofAutomotiveEngineers(_SAE_).The_NTTAA_  requiresFederalagencieslikeEPAtoprovideCongressthroughOMBwithexplanations  whenanagencydecidesnottouseavailableandapplicablevoluntaryconsensus p standards.Thisproposedamendedruleclarifiesandsimplifies,alreadypromulgated, H proceduresforuseofalternativestandards.TheintentoftheMethod301istoallow b  ownersandoperatorsofsourcesregulatedbyPart63standardstheflexibilityandoption : tousealternativestandards.Todaysproposedamendedruleisintendedtosimplifyand   clarifytheproceduresforusingalternativestandards.Therefore,theEPAisnot ! consideringtheuseofanyvoluntaryconsensusstandardswithtodaysproposedaction. #   ,&*  ListofSubjectsin40CFRPart63  B  ` Environmentalprotection,Alternativetestmethod,Airpollutioncontrol,Field  validation,Hazardousairpollutants,Method301.   򀀀  t Dated:December16,2004.  ` ̀0 ` 0 ` (#` (#0 (# (#0h(#(#0h(#h(#z8 (#(# 򀀀 R  MichaelO.Leavitt, >  Administrator.  *   ` Forthereasonsstatedinthepreamble,Title40,ChapterI,Part63,oftheCodeof B theFederalRegulationsisproposedtobeamendedasfollows:  PART63[AMENDED]   1.TheauthoritycitationforPart63continuestoreadasfollows:   Authority:42U.S.C.7401,etseq.  ` 2.Part63isamendedbyrevisingAppendixAtoreadasfollows: z8  AppendixAtoPart62TestMethods R  Method301FieldValidationofPollutantMeasurementMethodsFromVariousWaste *  Media  Sec.   UsingMethod301 p  1.0WhatisthepurposeofMethod301? H 2.0WhenmustIuseMethod301? b  3.0WhatdoesMethod301include?  :  4.0HowdoIperformMethod301?    ReferenceMaterialsandPerformanceAudits  ! 5.0WhatreferencematerialsmustIuse? #  6.0HowdoIconducttheperformanceaudit? %X"  SamplingProcedures  r'0!$ 7.0WhatsamplingproceduresmustIuse? J)#& 8.0HowdoIensuresamplestability? "+$(  BiasandPrecision  ,&* 9.0Whataretherequirementsforbias? B 10.0Whataretherequirementsforprecision?  11.0WhatcalculationsmustIperformforisotopicspiking?   12.0WhatcalculationsmustIperformforcomparisonwithavalidatedmethodifIam   usingpairedsamplingsystems?  ` 13.0WhatcalculationsmustIperformforcomparisonwithavalidatedmethodifIam z8  usingquadrupletreplicatesamplingsystems? R  14.0WhatcalculationsmustIperformforanalytespiking? *  15.0HowdoIconducttestsatsimilarsources?   OptionalRequirements   16.0HowdoIuseandconductruggednesstesting?  p 17.0WhatdetectionlimitsmustIuse?  H  OtherRequirementsandInformation  b  18.0HowdoIapplyforapprovaltouseanalternativetestmethod?  : 19.0HowdoIrequestawaiver?    20.0Whatdefinitionsapplytothismethod?  ! 21.0WherecanIfindadditionalinformation?  #    UsingMethod301  %X" .1.0WhatisthepurposeofMethod301? r'0!$  ` Thismethoddescribestheminimumproceduresthatyou,theowneroroperatorof J)#& anaffectedsourcesubjecttorequirementsunder40CFRPart63,mustusetovalidatean "+$( alternativetestmethodtoatestmethodrequiredin40CFRPart63. ,&* ?, ? ?  _2.0WhenmustIuseMethod301? B  ` Ifyouwanttorequesttouseanalternativetestmethodtomeetrequirementsina  subpartof40CFRPart63,youmustuseMethod301tovalidatethealternativetest   method.Youmustrequestapprovaltousethealternativetestmethodaccordingtothe   proceduresinSection18and63.7(f).YoumustreceivetheAdministratorswritten  ` approvaltousethealternativetestmethodbeforeyouusethealternativetestmethodto z8  meetrequirementsunder40CFRPart63.Insomecases,theAdministratormaydecide R  towaivetherequirementtouseMethod301.Section19describestherequirementsfor *  obtainingawaiver.    3.0WhatdoesMethod301include?0  (#(#  ` Thismethodincludesminimumprocedurestodetermineanddocumentsystematic p error(bias)andrandomerror(precision)ofmeasuredconcentrationsfromexhaustgases, H wastewater,sludge,andothermedia.Itcontainsproceduresforensuringsamplestability b  ifsuchproceduresarenotincludedinthetestmethod.Thismethodalsoincludes : optionalproceduresforruggednessanddetectionlimits.    4.0HowdoIperformMethod301? !  ` First,youintroduceaknownconcentrationofananalyteorcomparethe #  alternativetestmethodagainstavalidatedtestmethodtodeterminethealternativetest %X" method'sbias.Then,youcollectmultiple,collocatedsimultaneoussamplestodetermine r'0!$ thealternativetestmethod'sprecision.Sections5.0through17.0describethese J)#& proceduresindetail.   "+$(   ReferenceMaterialsandPerformance_Audits  ,&* }85.0WhatreferencematerialsmustIuse? B  ` Youmustusereferencematerials(thatis,analytes) atthelevel oftheapplicable  emissionlimitationorstandardthatthesubpartin40CFRPart63requires.Ifyouwant   toexpandtheapplicablerangeofthemethod,youmustconductadditionalrunswith   higherandloweranalyteconcentrations.Theadditionalrunsmustbeconducted  ` accordingtotheruggednessproceduresin16.0.Youmustusetheanalytesaccordingto z8  theproceduresin5.1through5.4. R   ` 5.1ExhaustGasTests.Youmustgetaknownconcentrationofeachanalyte *  fromanindependentsourcesuchasaspecialitygasmanufacturer,specialtychemical  company,orchemicallaboratory.Youmustalsogetthemanufacturersstabilitydatafor  theanalyteconcentrationandrecommendationsfor_recertification_.  p  ` 5.2TestsforOtherWasteMedia.Youmustgetthepureliquidcomponentsof H eachanalytefromanindependentmanufacturer.Themanufacturermustcertifythepurity b  andshelflifeofthepureliquidcomponents.Youmustdilutethepureliquidcomponents : inthesametypemedium asthewastefromtheaffectedsource.Youmustverifythe   accuracyoftheconcentrationofeachdilutedanalytebycomparingitsresponsetothe ! pureliquidcomponents. #   ` 5.3SurrogateAnalytes.IfyoudemonstratetotheAdministratorssatisfaction %X" thatasurrogatecompoundbehavesastheanalytedoes,thenyoumayusesurrogate r'0!$ compoundsforhighlytoxicorreactivecompounds.Asurrogatemaybeanisotopeor J)#& onethatcontainsauniqueelement(forexample,chlorine)thatisnotpresentinthesource "+$( oraderivationofthetoxicorreactivecompound,ifthederivativeformationispartofthe ,&* methodsprocedure.Youmayuselaboratoryexperimentsorliteraturedatatoshow B behavioralacceptability.   ` &  5.4IsotopicallyLabeledMaterials.Isotopemixturesmaycontaintheisotopeand   thenaturalanalyte.The' |Bisotopelabeledanalyteconcentrationmustbemorethanfive   timesthenaturalconcentrationoftheanalyte.   ` 6.0HowdoIconducttheperformanceaudit? z8   ` 6.1GettingPerformanceAuditMaterial.IfEPAhasperformanceauditmaterial R  fortheanalytesthatyouaretesting,youmustuseittoassessmethodbias.Youcangeta *  listofperformanceauditmaterialsat4s O  5  6EO+E  7 YE4t O  5  6EOE  7 EԀ4u O  5  http://www.epa.gov/ttn/emc/email.html#audit6bFOvF  7 !FԀorby  contactingEMCat(919)5415545.Youmustrequesttheperformanceauditmaterialat  least30daysbeforethevalidationtest. p  ` 6.2SamplingandAnalyzingPerformanceAuditMaterial.Youmustsampleand H analyzetheperformanceauditmaterialthreetimesaccordingtotheinstructionsprovided b  withtheauditsample.Youmustsubmitthethreeresultswiththefieldvalidationreport. : Althoughtherearenoacceptancecriteriafortheseperformanceauditresults,youandthe   Administratormayusethemtoassesstherelativeerrorofsamplerecovery,sample ! preparation,andanalyticalproceduresandthenconsidertherelativeerrorinevaluating #  themeasuredemissions. %X"   &   @`  @  @  @h  @ SamplingProcedures  r'0!$ J7.0WhatsamplingproceduresmustIuse? J)#&  ` Youmaydeterminebiasandprecisionbycomparing'r'Jagainstavalidatedtest "+$( method,usingisotopicsampling,orusinganalytespiking.Isotopicsamplingcanonlybe ,&* _usedforproceduresrequiringmassspectrometry(GX(X.#(XX(GL#ԀYoumustcollectsamplesaccordingto B therequirementsinTable1.Youmustperformthesamplingaccordingtotheprocedures  inSections7.1through7.5.    ` 7.1ComparisonAgainstaValidatedTestMethod.Ifyouarecomparingthe   resultsfromthevalidatedtestmethod,itisrecommendedthatyouconductaperformance  ` auditaccordingtotheproceduresinSection6. z8   ` 7.2IsotopicSpiking.Spikeall12sampleswiththeanalyteattheconcentration R  intheapplicableemissionlimitationorstandardinthesubpartof40CFRPart63.If *  thereisnoapplicableemissionlimitationorstandard,spikeattheexpectedlevelofthe  samples.Followtheappropriatespikingproceduresin7.4.1through7.4.2forthe  applicablewastemedium. h  p  ` 7.3AnalyteSpiking.Ineachquadrupletset,spikehalfofthesamples(twooutof H thefour)withtheanalyteaccordingtotheapplicableprocedureinSection7.4. b   ` 7.4SpikingProcedure. :  ` 7.4.1GaseousAnalytewithSorbentorImpingerSamplingTrains.Samplethe   analyte(inthelaboratoryorinthefield)ataconcentrationthatisclosetothe ! concentrationintheapplicableemissionlimitationorstandardinthesubpartof40CFR #  Part63(ortheexpectedsampleconcentrationwherethereisnostandard)forthetime %X" requiredbythemethod,andthensamplethegasstreamforanequalamountoftime.The r'0!$ timeforsamplingboththeanalyteandgasstreamshouldbeequal;however,thetime J)#& shouldbeadjustedtoavoidsorbentbreakthrough.Thestackgasandthegaseousanalyte "+$( maybesampledatthesametime.Theanalytemustbeintroducedasclosetothetipof ,&* thesamplingtrainaspossible. B  ` 7.4.2GaseousAnalytewithSampleContainer(BagorCanister).Spikethe  samplecontainersaftercompletionofeachtestrunwithanamountequaltothe(GX(X' (G?+ 4 <DL!XX?   #(G 'V##(XX(GbV#concentrationintheapplicableemissionlimitationorstandardinthesubpartof40CFR   Part63(ortheexpectedsampleconcentrationwherethereisnostandard).Thefinal  ` concentrationoftheanalyteshallapproximatetheleveloftheemissionconcentrationin z8  thestack.Thevolumeamountofanalyteshallbelessthan10percentofthesample R  volume. *   ` 7.4.3LiquidandSolidAnalytewithSorbentorImpingerTrains.Spikethetrains  withanamountequaltotheconcentrationintheapplicableemissionlimitationor  standardinthesubpartof40CFRPart63(ortheexpectedsampleconcentrationwhere p thereisnostandard)beforesamplingthestackgas.Ifpossible,dothespikinginthe H field.Ifitisnotpossibletodothespikinginthefield,youcandoitinthelaboratory. b   ` 7.4.4LiquidandSolidAnalytewithSampleContainer(BagorCanister).Spike : thecontainersatthecompletionofeachtestrunwithanamountequaltothe   concentrationintheapplicableemissionlimitationorstandardinthesubpartof40CFR ! Part63(ortheexpectedsampleconcentrationwherethereisnostandard). #   ` 7.5ProbePlacementandArrangementforStationarySourceStackorDuct %X" Sampling.Tosampleastationarysourceasdefinedin40CFR63.2 ,youmustplacethe r'0!$ probeaccordingtotheproceduresin7.5.Youmustplacetheprobesinthesame J)#& horizontalplane. "+$(  ` 7.5.1ForPairedSampleProbes,thesampleprobetipshouldbe2.5cmfromthe ,&* outsideedgeoftheothersampleprobe,witha_pitot_Ԁtubeontheoutsideofeachprobe. B TheAdministratormayapproveavalidationrequestwhereotherpairedarrangementsfor  the_pitot_Ԁtubeareused.    ` 7.5.2ForQuadrupletSamplingProbes,thetipsshouldbeina6.0cmx6.0cm   squareareameasuredfromthecenterlineoftheopeningoftheprobetipwithasingle  ` _pitot_Ԁtubeinthecenterortwo_pitot_Ԁtubeswiththeirlocationoneithersideoftheprobetip z8  configuration.Youmustproposeanalternativearrangementwheneverthecross R  sectionalareaoftheprobetipconfigurationisapproximately5percentormoreofthe *  stackorductcrosssectionalarea.  8.0HowdoIensuresamplestability?   ` 8.1DevelopingStorageandAnalysisProcedures.Ifthealternativetestmethod p includeswellestablishedproceduressupportedbyexperimentaldataforsamplestorage H andthetimewithinwhichthecollectedsamplesmustbeanalyzed,youmuststorethe b  samplesaccordingtotheproceduresinthealternativetestmethod.Youarenotrequired : toconducttheproceduresinSection8.2or8.3.Ifthealternativetestmethoddoesnot   includesuchprocedures,youmustproposeproceduresforstoringandanalyzingsamples ! toensuresamplestability.Ataminimum,yourproposedproceduresmustmeetthe #  requirementsinSection8.2or8.3.  Theminimumstoragetimeshouldbeassoonas %X" possible,butnolongerthan24hoursaftercollectionofthesample.Themaximum r'0!$ storagetimeshouldbefourweeksorless. J)#&  ` 8.2StorageandSamplingProceduresforStackTestEmissions.Youmuststore "+$( andanalyzesamplesofstacktestemissionsaccordingtoTable3.Ifyouareusinganalyte ,&* spikingprocedures,youmustincludeequalnumbersofspikedand_unspiked_Ԁsamples. B  ` 8.3StorageandSamplingProceduresforTestingOtherWasteMedia.Youmust  analyzehalfofthereplicatesamplesattheproposedminimumstoragetimeandtheother   halfattheproposedmaximumstoragetimetoidentifytheeffectofstoragetimeson   analytesamples.Theminimumstoragetimeshouldbeassoonaspossible,butnolonger  ` than24hoursaftercollectionofthesample.Themaximumstoragetimeshouldbetwo z8  weeksorless.