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 "+$( andanalyzesamplesofstacktestemissionsaccordingtoTable3.Ifyouareusinganalyte ,&* spikingprocedures,youmustincludeequalnumbersofspikedand_unspiked_Ԁsamples. B  ` 8.3StorageandSamplingProceduresforTestingOtherWasteMedia.Youmust  analyzehalfofthereplicatesamplesattheproposedminimumstoragetimeandtheother   halfattheproposedmaximumstoragetimetoidentifytheeffectofstoragetimeson   analytesamples.Theminimumstoragetimeshouldbeassoonaspossible,butnolonger  ` than24hoursaftercollectionofthesample.Themaximumstoragetimeshouldbetwo z8  weeksorless. R   ` 8.4SampleStability.Afteryouhaveconductedsamplingandanalysisaccording *  to8.2or8.3,comparetheresultsattheminimumandmaximumstoragetimes.Calculate  thedifferenceintheresultsusingEquation3011.   `  l`8($`^ o `.E oo ol߀    0 p 0p(#p(#Eq.3011p(#(# Where0 _di_=differencebetweentheresultsofthe_ith_Ԁsample.$ (# (#  ` 0 _Rmini_=resultsfromthe_ith_Ԁsampleattheminimumstoragetime (# (# 0 ` 0 ` (#` (#_Rmaxi_=resultsfromthe_ith_Ԁsampleatthemaximumstoragetime. (# (#  ` 8.4.1StandardDeviation.Determinethestandarddeviation,_SDd_,ofthe "B differences,_di_'s,ofthepairedsamplesusingEquation3012. \$  mYIEz h p @Xdddddddd@E4&d\?% 4&" Where:r^X` hp x (#%'0*,.8135@8:<H?AXr B  `  _Vm_=0  validatedmethod(#(# 0 ` 0 ` (#` (#Pm=0 (# (#proposedalternativetestmethod (#(# 0 ` 0 ` (#` (#_di_=0 (# (#Thedifferencebetweenthe_i_Ԅthpairofsamples,_Vm_󀄀Pm   (#(#  `  dm=Themeanofthepairedsampledifferences.  `  `  n=totalnumberofpairedsamples z8   ` 8.4.2tTest.Testthedifferenceintheresultsforstatisticalsignificanceby R  calculatingthetstatisticanddeterminingifthemeanofthedifferencesbetweenthe *  initialresultsandtheresultsafterstorageissignificantatthe95percentconfidencelevel.  CalculatethevalueofthetstatisticusingEquation3013.  mEYIEz h p @Xdddddddd@E=pdu\?N p Where:0 nisthetotalnumberofpairedsamples.*! (# (#  ` Comparethecalculatedtstatisticwiththecriticalvalueofthetstatisticfrom # Table2.Ifthecalculatedtvalueislessthanthecriticalvalue,thedifferenceisnot $ statisticallysignificant,thus,thesamplingandanalysisprocedureensuresstability,and &p  youmaysubmitarequestforvalidationoftheproposedalternativetestmethod.Ifthe (H" calculatedtvalueisgreaterthanthecriticalvalue,thedifferenceisstatistically b* $  significantandyoumustrepeattheproceduresin8.2or8.3withnewsamplesusing :,%" shorterproposedmaximumstoragetimes. .'$   BiasandPrecision  B }y9.0Whataretherequirementsforbias?   ` Youmustestablishbiasbycomparingtheresultsofthesamplingusingthe   alternativetestmethodagainstareferencevalue. Thebiasmustbenomorethan+/10%   forthealternativetestmethodtobeacceptable.  ` 10.0Whataretherequirementsforprecision? z8   ` Ataminimum,youmustusepairedsamplingsystemstoestablishprecision.If R  youareusinganalytespiking,includingisotopicsamples,theprecisionexpressedasthe *  relativestandarddeviation(_RSD_),ofthealternativetestmethodatthelevelofthe  applicableemissionlimitationorstandardinthesubpartof40CFRPart63mustbeless  thanorequalto20percent.Ifyouarecomparingtoavalidatedtestmethod,the p alternativetestmethodmustbeatleastaspreciseasthevalidatedmethodatthelevelof H theapplicableemissionlimitationorstandardinthesubpartof40CFRPart63as b  determinedbyanFtest. : 11.0WhatcalculationsmustIperformforisotopicspiking?    ` Youmustanalyzethebias,precision,relativestandarddeviation,anddata ! acceptanceforisotopicspikingtestsaccordingtotheprovisionsinSections11.1through #  11.3. %X"  ` 11.1.NumericalBias.Calculatethenumericalvalueofthebiasusingtheresults r'0!$ fromtheanalysisoftheisotopicallyspikedfieldsamplesandthecalculatedvalueofthe J)#& isotopicallylabeledspikeaccordingtoEquation3014. "+$( mxyFXHDz h 0 @Xdddddddd@E,d\?, ,&* ЀWhere:  0 ` B=0 ` (#` (#Biasatthespikelevel.  (# (# 0 ` 0 ` (#` (# ` Sm=Meanofthemeasuredvaluesoftheisotopicallyspikedsamples.  (# (# 0 ` CS=0 ` (#` (#Calculatedvalueoftheisotopicallylabeledspike. ` (# (#  ` 11.2.StandardDeviation.CalculatethestandarddeviationoftheSivalues z8  accordingtoEquation3015. R  m|}JXHDz h 0 @Xdddddddd@E*8dap\m?^ *  Where: V  ` Si=0 Measuredvalueoftheisotopicallylabeledanalyteinthe_i_Ԅthfieldsample,p. (# (# 0 ` n=0 ` (#` (#Numberofisotopicallyspikedsamples,12.H (# (#  ` 11.3tTest.Testthebiasforstatisticalsignificancebycalculatingthet-statistic   usingEquation3016.UsethestandarddeviationdeterminedinSection11.2andthe   numericalbiasdeterminedinsection11.1. " mKYIEz h p @Xdddddddd@E$d2\?D$ $f Comparethecalculatedtvaluewiththecriticalvalueofthetwo-sidedt-distributionat T,& the95percentconfidencelevelandn-1degreesoffreedom.Whenspikingisconducted ,.'  accordingtotheproceduresspecifiedinSections7.2and7.4asrequired,thiscritical B valueis2.201fortheelevendegreesoffreedom.Ifthecalculatedtvalueislessthanthe  criticalvalue,thebiasisnotstatisticallysignificantandthedataareacceptable.Ifthe   calculatedtvalueisgreaterthanthecriticalvalue,thebiasisstatisticallysignificantand   youmustevaluatetherelativemagnitudeofthebiasusingEquation3017.  `  `  |`LF62p~1p `. !ERp& pERp| R  Where: 0  ` BR=Relativebias.  Iftherelativebiasislessthanorequalto10percent,thenthedataareacceptable.You  mayproceedtoevaluatetheprecision.Ifnotthecandidatemethodwillnotmeetthe v requirementsofMethod301. N  ` 11.4RelativeStandardDeviation.Calculatethe_RSD_ԀaccordingtoEquation301 h& 8 @! mABMWGCz h `X@Xdddddddd@E#d$\?" # whereSmisthemeasuredmeanoftheisotopicallylabeledspikedsamples.Thedataand (" alternativetestmethodareunacceptableifthe_RSD_Ԁisgreaterthan20percent. *$  12.0WhatcalculationsmustIperformforcomparisonwithavalidatedmethodifIam ,\&" usingpairedsamplingsystems? B  ` Youmustanalyzethedataforcomparisonwithavalidatedmethodaccordingto  Section12.Conducttheseprocedurestodetermineifanalternativetestmethodproduces   resultsequivalenttoavalidatedmethod.Ifthedatafromthealternativetestmethodfail   eitherthebiasorprecisiontest,thedataandthealternativetestmethodareunacceptable.   `  ` 12.1BiasAnalysis. z8   ` 12.1.1StandardDeviation.Determinethestandarddeviation,_SDd_,ofthe R  differences,_di_'s,ofthepairedsamplesusingEquation3012. *   ` 12.1.2tTest.Testthebiasforstatisticalsignificancebycalculatingthetstatistic  anddetermineifthemeanofthedifferencesbetweenthealternativetestmethodandthe  validatedmethodissignificantatthe95percentconfidencelevel.Calculatethevalueof p thetstatisticusingEquation3013.Forthespikingprocedureforpairedsampling H systems,accordingtoSection7.1andTable1,nequalsnine. b   ` Comparethecalculatedtstatisticwiththecriticalvalueofthetstatistic.When : ninerunsareconducted,asspecifiedinSection7.1andTable1,thecriticalvalueofthe   t-statisticis1.397foreightdegreesoffreedom.Ifthecalculatedtvalueislessthanthe ! criticalvalue,thebiasisnotstatisticallysignificantandthedataareacceptable.Ifthe #  calculatedtvalueisgreaterthanthecriticalvalue,thebiasisstatisticallysignificantand %X" youmustevaluatetherelativemagnitudeofthebiasusingEquation3019.Iftherelative r'0!$ biasislessthanorequalto10percent,thenthedataareacceptable.Proceedtoevaluate J)#&  precision. "+$( h`4 $ ` \0C `. EBCCBCh h  H      p     Eq.3019  B  Where:  L  ` B=Bias=meanofthe_di_s f $  ` VS=meanmeasuredbythevalidatedmethod   >  ` 12.2.Precision.Comparethevarianceofthealternativetestmethodtothatofthe   validatedmethod.IfasignificantdifferenceisdeterminedusingtheFtest,thealternative   testmethodandtheresultsarerejected.IftheFtestdoesnotshowasignificant   difference,thenthealternativetestmethodhasacceptableprecision.Thisprocedure \ requiresthatyouknowthestandarddeviationofthevalidatedmethod,_SDv_.Usethe v4 valuefurnishedwiththemethod.Ifthestandarddeviationofthevalidatedmethodisnot N  available,thepairedreplicatesamplingproceduremaynotbeused. &  ` 12.2.1Variance.Calculatethevarianceofthevalidatedmethod,Sv2,using  Equation30110.  mNY IEz h p @Xdddddddd@E!#d[\?J!  !l lO` hp !%'0*,.8135@8:<H?AXhXlWhere:  %  `  _SDv_=0  Standarddeviationprovidedwiththevalidatedmethod.'!(#(#  ` 12.2.2PooledVariance.Calculatethepooledvarianceofbothmethods,S2pooled, )`#   accordingtoEquation30111. z+8%" mWYO\ LHzl p @Xdddddddd@EBd~\?  B  Where:   0 ` 0 ` (#` (#_di_=Thedifferencebetweenthe_i_Ԅthpairofvalidatedandalternative   methodsamples.j  (# (# 0 ` 0 ` (#` (#n=Thenumberofpairsofsamples. p B  (# (# 12.2.3AlternativeTestMethodVariance.Calculatethevarianceofthealternativetest \  method,S2p,fromtheS2pooledusingEquation30112. 4  mPY IEz h p @Xdddddddd@E #d[\?    (IfS2v>S2pooled,letS2p=S2pooled/2). P  ` 12.2.4TheFtest.Determineifthevarianceofthealternativetestmethodis ( significantlydifferentfromthatofthevalidatedmethodbyperformingtheFtest. ! CalculatetheexperimentalFvalueusingEquation30113. " mQ\ LHzl p @Xdddddddd@E$_\?L$  $n ComparetheexperimentalFvaluewiththecriticalrangeofFata95percentconfidence ,r& level.WhentheprocedurespecifiedinSection7.1andTable1forpairedtrainsis B followedasrequired,thecriticalrangeis0.291to3.44.IfthecalculatedFisoutsidethe  criticalrange,thedifferenceinprecisionissignificantandthedataandalternativetest   methodareunacceptable.   13.0WhatcalculationsmustIperformforcomparisonwithavalidatedmethodifIam  ` usingquadrupletreplicatesamplingsystems? z8   ` Ifyouareusingquadrupletreplicatesamplingsystemstocompareanalternative R  testmethodtoavalidatedmethod,thenyoumustanalyzethedataaccordingtothe *  provisionsin13.0.Ifthedatafromthealternativetestmethodfaileitherthebiasor  precisiontest,thedataandthealternativetestmethodareunacceptable.Ifthe  Administratordeterminesthattheaffectedsourcehashighlyvariableemissionrates,the p Administratormayrequireadditionalprecisionchecks. H  ` 13.1BiasAnalysis.Testthebiasforstatisticalsignificanceatthe95percent b  confidencelevelbycalculatingthetstatistic. :  ` 13.1.1Bias.Determinethebias,whichisdefinedasthemeanofthedifferences   betweenthealternativetestmethodandthevalidatedmethod(dm).Calculate_di_according ! toEquation30114. #  mRX HDz h 0 @Xdddddddd@E%d @\?6% uR` hp !%'0*,.8135@8:<H?AX !%Xu %X" Where:     V1i=0 h Firstmeasuredvaluewiththevalidatedmethodinthe_i_Ԅth +f%$ sample.->'&h(#h(#  `    V2i=0 h Secondmeasuredvaluewiththevalidatedmethodinthe_i_Ԅ B thsample.h(#h(#  `    P1i=0 h Firstmeasuredvaluewiththealternativetestmethodinthe   _i_Ԅthsample. h(#h(#  `    P2i=0 h Secondmeasuredvaluewiththealternativetestmethodin  ` the_i_Ԅthsample.z8 h(#h(#  ` 13.1.2StandardDeviationoftheDifferences.Calculatethestandarddeviationof R  thedifferences,_SDd_,usingEquation3012. *   ` 13.1.3TTest.CalculatethetstatisticusingEquation3013,wherenisthetotal  numberoftestsampledifferences(_di_).Forthequadrupletsamplingsystemprocedurein  Section7.1andTable1,nequalsfour.Comparethecalculatedtstatisticwiththecritical p valuefromofthetstatisticanddetermineifthebiasissignificantatthe95percent H confidencelevel.Whenfourrunsareconducted,asspecifiedinSection7.2andTable1, b  thecriticalvalueofthet-statisticis1.638forthreedegreesoffreedom.Ifthecalculated : tvalueislessthanthecriticalvalue,thebiasisnotstatisticallysignificantandthedata   areacceptable.Ifthecalculatedtvalueisgreaterthanthecriticalvalue,thebiasis ! statisticallysignificantandyoumustevaluatetherelativemagnitudeofthebiasusing #  Equation3019.Iftherelativebiasislessthanorequalto10percent,thenthedataare %X" acceptable.Proceedtoevaluateprecisionofthealternativetestmethod. r'0!$  ` 13.2Precision.Comparethevarianceofthealternativetestmethodtothatofthe J)#& validatedmethod.IfasignificantdifferenceisdeterminedusingtheFtest,thealternative "+$( testmethodandtheresultsarerejected.IftheFtestdoesnotshowasignificant ,&* difference,thenthealternativetestmethodhasacceptableprecision.Thisprocedure B requiresthestandarddeviationofthevalidatedmethod,_SDv_,tobeknown.Usethevalue  furnishedwiththemethod.Iftherearenopublishedvalues,calculatethevarianceofthe   validatedmethodusingEquation30115.    ` 13.2.1AlternativeTestMethodVariance.Calculatethevarianceofthe  ` alternativetestmethod,Sp2,accordingtoEquation30115. z8  m#SYIEz h p @Xdddddddd@EROd!V\*? R  Where: J 0 ` 0 ` (#` (#_di_=Thedifferencebetweenthe_i_Ԅthpairofsamplescollectedwiththe d" alternativetestmethod.< (# (#  ` 13.2.2TheFtest.Determineifthevarianceofthealternativetestmethodis  greaterthanthatofthevalidatedmethodbycalculatingtheFvalueusingEquation301  13.ComparetheexperimentalFvaluewiththecriticalrangeofF.Thecriticalrangeis   0.264to3.79forthe95percentconfidencelevelwhentheprocedurespecifiedinSection "Z 7.1andTable1forquadruplettrainsisfollowed.IfthecalculatedFisoutsidethecritical t$2 range,thedifferenceinprecisionissignificant,andthedataandthealternativetest L&  methodareunacceptable. $(!  14.0WhatcalculationsmustIperformforanalytespiking? )#"  ` YoumustanalyzethedataforanalytespiketestingaccordingtoSection14. +%$  ` 14.1BiasAnalysis. -j'&  ` 14.1.1Bias.Calculatethenumericalvalueofthebiasusingtheresultsfromthe B analysisofthespikedfieldsamples,the_unspiked_Ԁfieldsamples,andthecalculatedvalue  ofthespikeusingEquation30116.   mTXHDz h 0 @Xdddddddd@E d\?f    Where: T  0 ` B=0 ` (#` (#Biasatthespikelevel.n,  (# (# 0 ` Sm=0 ` (#` (#Meanofthespikedsamples.F  (# (# 0 ` Mm=0 ` (#` (#Meanofthe_unspiked_Ԁsamples. (# (# 0 ` CS=0 ` (#` (#Calculatedvalueofthespikedlevel. (# (#  ` 14.1.2TTest.Testthebiasforstatisticalsignificancebycalculatingthe  t-statisticusingEquation30117andcomparingitwiththecriticalvalueofthetwo-sided d t-distributionatthe95percentconfidencelevelandn-2degreesoffreedom.Thiscritical ~< valueis2.228forthetendegreesoffreedom. V m;XHDz h 0 @Xdddddddd@E. p,dh\?8 !  .  Where: *$ 0 ` 0 ` (#` (#S2u=(_SDu_)2,_SDu_iscalculatedinEquation301_Ԅ19.,z&  (# (# 0 ` 0 ` (#` (#S2s=(_SDs_)2,_SDs_iscalculatedinEquation30118.B (# (# Ifthecalculatedtvalueislessthanthecriticalvalue,thebiasisnotstatistically  significantandthedataareacceptable.Ifthecalculatedtvalueisgreaterthanthecritical   value,thebiasisstatisticallysignificantandyoumustevaluatetherelativemagnitudeof   thebiasusingEquation3017.Iftherelativebiasislessthanorequalto10percent,then  ` thedataareacceptable.Youmayproceedtoevaluateprecision. z8   ` 14.2Precision.Calculatethestandarddeviationandthe_RSD_Ԁofthealternative R  testmethod. *   ` 14.2.1SpikedSamples.Calculatethedifference,_di_,betweenthepairsofthe  spikedalternativetestmethodmeasurementsforeachreplicatesampleset.Determinethe  standarddeviation(_SDs_)ofthespikedvaluesusingEquation30118. p mVXHDz h 0 @Xdddddddd@E8Zd p\7?&=. H Where:  * * dis=Differencebetweenthe_i_Ԅthpairofspikedsamples.   ` ` `   z z n=Numberofpairedsamples. "  ` 14.2.2_Unspiked_ԀSamples.Calculatethestandarddeviationofthe_unspiked_ $f valuesusingEquation30119. &>  m\^_[KGzl 0 @Xdddddddd@EX(^ pT|'&0 !  X(" !(#!(# Where:    _diu_=Differencebetweenthe_i_Ԅthpairof_unspiked_Ԁsamples. B ` ` `   z z n=Numberofpairedsamples.   ` 14.2.3PooledStandardDeviation.Calculatethepooledstandarddeviationofthe   spikedand_unspiked_Ԁsamplesifthestandarddeviationsarenotsignificantlydifferent.   TestforthisdifferenceusingEquation30120.  ` mUXHDz h 0 @Xdddddddd@Ez]d_\I?% z8  WhereSu2andSs2aredefinedinEquation30117. 2  Forthecasewheren=6anda95percentconfidencelevel,thestandarddeviationsmay   bepooledifthecalculatedFliesbetween0.139and7.146.Calculatethepooledstandard  deviation(_SDpooled_)usingEquation30121. x mXXHDz h 0 @Xdddddddd@E8Qdp\7?. P Ifthevariancesaresignificantlydifferentandcannotbepooled,usethestandard $ deviationofthespikedsamplesforthebiasanalysisinSection14.1.2. %  ` 14.2.4RelativeStandardDeviation.Calculatethe_RSD_Ԁofthealternativetest 'n! methodusingEquation3018andthepooledstandarddeviationdeterminedfrom )F# Section14.2.3.Ifthepooledstandarddeviationorthestandarddeviationfromthe `+% _unspiked_Ԁsamplesisused,Smisthemeanofthe_unspiked_Ԁsamples.Ifthestandard 8-&  deviationofthespikedsamplesisused,Smisthemeanofthespikedsamples.Thedata B andalternativetestmethodareunacceptableifthe_RSD_Ԁisgreaterthan20percent.   15.0HowdoIconducttestsatsimilarsources?    ` IftheAdministratorhasapprovedtheuseofanalternativetestmethodtoatest   methodrequiredin40CFRPart63foranaffectedsource,andtheAdministratorhas  ` approvedtheuseofthealternativetestmethodatyoursimilarsourceaccordingtothe z8  proceduresin19.1.1,youmustmeettherequirementsinthissection.Youmusthaveat R  leastthreereplicatesamplesforeachtestthatyouconductatthesimilarsource.You *  mustaveragetheresultsofthesamplestodeterminethepollutantconcentration.    OptionalRequirements  p 16.0HowdoIuseandconductruggednesstesting? H  ` Ifyouwanttouseavalidatedtestmethodataconcentrationthatisdifferentfrom b  theconcentrationintheapplicableemissionlimitationinthesubpartof40CFRPart63 : orforasourcecategorythatisdifferentfromthesourcecategorythatthetestmethod   specifies,thenyoumustconductruggednesstestingaccordingtotheproceduresin ! Citation10ofSection18.0andsubmitarequestforawaiveraccordingto19.1.1. #   ` Ruggednesstestingisalaboratorystudytodeterminethesensitivityofamethod %X" toparameterssuchassamplecollectionrate,_interferant_Ԁconcentration,collectingmedium r'0!$ temperature,andsamplerecoverytemperature.Youconductruggednesstestingby J)#& changingseveralvariablessimultaneouslyinsteadofchangingonevariableatatime. "+$( Forexample,youcandeterminetheeffectofsevenvariablesineightexperimentsinstead ,&* _ofone.(_W.J._Ԁ_Youden_,StatisticalManualoftheAssociationofOfficialAnalytical B Chemists,AssociationofOfficialAnalyticalChemists,Washington,DC,1975,pp.  33-36).   17.0HowdoIdeterminetheLimitofDetectionforthealternativemethod?      ` 17.1LimitofDetection.TheLimitofDetection(_LOD_)isthelowestlevelabove  ` whichyoumayobtainquantitativeresultswithanacceptabledegreeofconfidence.For z8  thisprotocol,the_LOD_Ԁisdefinedas3timesthestandarddeviation,So,attheblanklevel. R  This_LOD_Ԁcorrespondstoanuncertaintyof30%atthe99percentconfidencelevel. *  Ѐ ` 17.2Purpose.The_LOD_Ԁwillbeusedtoestablishthelowerlimitofthetest  method.Iftheestimated_LOD_Ԁisnomorethantwicethecalculated_LOD_,useProcedureI  inTable4todetermineSo.Ifthe_LOD_Ԁisgreaterthantwicethecalculated_LOD_,use p ProcedureIIinTable4todetermineSo. H   OtherRequirementsandInformation  b  18.0HowdoIapplyforapprovalofanalternativetestmethod? :  ` 18.1SubmittingRequests.Youmustrequesttouseanalternativetestmethod   accordingtotheproceduresin63.7(f).Youmaynotuseanalternativetestmethodto ! meetanyrequirementunder40CFRPart63untiltheAdministratorhasapprovedyour #  request.Therequestmustincludeafieldvalidationreportingcontainingtheinformation %X" in18.2.TherequestmustbesubmittedtotheDirector,EmissionsMonitoringand r'0!$ AnalysisDivision,U.S.EnvironmentalProtectionAgency,C30402,ResearchTriangle J)#& Park,NC27711.  "+$(  ` `/18.2FieldValidationReport.Thefieldvalidationreportmustcontainthe ,&* /5 TRY,3' LetterY,3' Letter 3' Letter 3' LetterT   informationin18.2.1through18.2.9. B  ` 18.2.1V  WRegulatoryobjectivesforthetesting,includingadescriptionofthereasons  forthetest,applicableemissionlimits,andadescriptionofthesource.V  WQ     ` 18.2.2V  WSummaryoftheresultsandcalculationsshowninSections7.0through17,   asapplicable.V  W*  `  ` 18.2.3V  WrAnalytecertificationandvalue(s).V  W z8   ` 18.2.4V  WLaboratorydemonstrationofthequalityofthespikingsystem.V  W_ R   ` 18.2.5V  WDiscussionoflaboratoryevaluations.V  W *   ` 18.2.6V  W3Discussionoffieldsampling.V  Wo   ` 18.2.7V  WDiscussionofsamplepreparationsandanalysis.V  W   ` 18.2.8V  WLStoragetimesofsamples(andextracts,ifapplicable).V  W p  ` 18.2.9V  WReasonsforeliminatinganyresults.V  W, H 19.0HowdoIrequestawaiver?  b   ` 19.1ConditionsforWaivers.Ifyoumeetoneofthecriteriain19.1.1through : 19.1.3,theAdministratormaywaivetherequirementtousetheproceduresinthismethod   tovalidateanalternativetestmethod.Inaddition,iftheEPAcurrentlyrecognizesan ! appropriatetestmethodorconsiderstheanalyststestmethodtobesatisfactoryfora #  particularsource,theAdministratormaywaivetheuseofthisprotocolormayspecifya %X" lessrigorousvalidationprocedure. r'0!$  ` 19.1.1SimilarSources.Ifthealternativetestmethodthatyouwanttousehas J)#& beenvalidatedatanothersourceandyoucandemonstratetotheAdministrators "+$( satisfactionthatyouraffectedsourceissimilartothatsource,thentheAdministratormay ,&* `6 TRY,3' LetterY,3' Letter 3' Letter 3' LetterT   waivetherequirementforyoutovalidatethealternativetestmethod.Oneprocedureyou Q mayusetodemonstratetheapplicabilityofthemethodtoyouraffectedsourceisby ) conductingaruggednesstestasdescribedin16.0.    ` 19.1.2DocumentedMethods.Ifthebiasandprecisionofthealternativetest   methodthatyouareproposinghavebeendemonstratedthroughlaboratorytestsor  ` protocolsdifferentfromthismethod,andyoucandemonstratetotheAdministrators 8  satisfactionthatthebiasandprecisionapplytoyourapplication,thentheAdministrator a  maywaivetherequirementtousethismethodortousepartofthismethod. 9   ` 19.1.3ConditionalTestMethods.Ifthealternativetestmethodhasbeen  demonstratedtobevalidatseveralsources,youmayasktheAdministratortodesignate  thealternativetestmethodasaconditionaltestmethod.IftheAdministratorhas p designatedatestmethodasaconditionaltestmethodandyouareusingtheconditional H methodwithinitsstatedapplicability,youdonothavetovalidateitaccordingtothe q  proceduresinthismethod.Youcanfindalistofconditionaltestmethodsat I 4 O  5  http://www.epa.gov/ttn/emc/ctm.html.6O  7  !   ` 19.2SubmittingApplicationsforWaivers.Youmustsignandsubmiteach ! requestforawaiverfromtherequirementsinthismethodinwriting.Therequestmust #  besubmittedtotheDirector,EmissionsMonitoringandAnalysisDivision,U.S. %X" EnvironmentalProtectionAgency,C30402,ResearchTrianglePark,NC27711. '0!$  ` 19.3InformationApplicationforWaiver.Therequestforawaivermustcontain Y)#& athoroughdescriptionofthetestmethod,theintendedapplication,andresultsofany 1+$( validationorothersupportingdocuments.Therequestforawaivermustcontain,at_a  -&* minimum,theinformationin19.3.1through19.3.4.TheAdministratormayrequest Q additionalinformationifnecessarytodeterminewhetherthismethodcanbewaivedfora ) particularapplication.     ` 19.3.1AClearlyWrittenTestMethod.Themethodshouldbewrittenpreferably   intheformatof40CFR60,AppendixATestMethods.Itmustincludeanapplicability  ` statement,concentrationrange,precision,bias(accuracy),andminimumandmaximum 8  storagetimeinwhichsamplesmustbeanalyzed. a   ` 19.3.2V  W-Summaries(seeSection18.3)ofpreviousvalidationtestsorother 9  supportingdocuments.V  WԀIfadifferentprocedurefromthatdescribedinthismethodwas  used,youmustsubmitdocumentssubstantiatingthebiasandprecisionvaluestothe  Administratorssatisfaction.  p   ` 19.3.3RuggednessTestingResults.Youmustsubmit resultsofruggedness H testingconductedaccordingtoSection16,samplestabilityconductedaccordingto q  Section8,anddetectionlimitsconductedaccordingtoSection17,asapplicable.For I example,youwouldnotneedtosubmitruggednesstestingresultsifyouwillbeusingthe !  methodatthesameconcentrationlevelastheconcentrationlevelatwhichitwas ! validated. #    ` 19.3.4ApplicabilityStatementandArgumentsforWaiverApproval.Discussion %X" oftheapplicabilitystatementandargumentsforapprovalofthewaiver.Thisdiscussion '0!$ shouldaddressasapplicablethefollowing:applicableregulation,emissionstandards, Y)#& effluentcharacteristics,andprocessoperations. 1+$( 20.0Whatdefinitionsapplytothismethod?   -&* _ ` Affectedsourcemeansaffectedsourceasdefinedin40CFR63.2andinthe Q relevantsubpartunder40CFRPart63. )  ` Alternativetestmethodmeansthesamplingandanalyticalmethodologyselected   forfieldvalidationusingthemethoddescribedinthisappendix.      ` Pairedsamplingsystemmeansasamplingsystemcapableofobtainingtwo  ` replicatesamplesthatwerecollectedascloselyaspossibleinsamplingtimeandsampling 8  location. a   ` Quadrupletsamplingsystemmeansasamplingsystemcapableofobtainingfour 9  replicatesamplesthatwerecollectedascloselyaspossibleinsamplingtimeandsampling  location.   ` Surrogatecompoundmeansacompoundthatservesasamodelforthetypesof p compoundsbeinganalyzed(i.e.,similarchemicalstructure,properties,behavior).The H modelcanbedistinguishedbythemethodfromthecompoundsbeinganalyzed. q  21.0WherecanIfindadditionalinformation?  I  ` Youcanfindadditionalinformationinthereferencesinparagraphs21.1through !  21.12. ! Ѐ21.1_Albritton_,_J.R._,G.B.Howe,S.B._Tompkins_,_R.K.M._Ԁ_Jayanty_,andC.E.Decker. #  1989.StabilityofPartsPerMillionOrganicCylinderGasesandResultsofSourceTest %X" AnalysisAudits,StatusReportNo.11.EnvironmentalProtectionAgencyContract6802 '0!$ 4125.ResearchTriangleInstitute,ResearchTrianglePark,NC.September. Y)#& Ѐ21.2DeWees,W.G.,P.M._Grohse_,_K.K._Ԁ_Luk_,and_F.E._ԀButler.1989.Laboratoryand 1+$( FieldEvaluationofaMethodologyfor_Speciating_ԀNickelEmissionsfromStationary  -&* Sources.EPAContract68024442.PreparedforAtmosphericResearchand Q EnvironmentalAssessmentLaboratory,OfficeofResearchandDevelopment,U.S. ) EnvironmentalProtectionAgency,ResearchTrianglePark,NC27711.January.   Ѐ21.3Keith,L.H.,W._Crummer_,J._Deegan_ԀJr.,R.A.Libby,_J.K._ԀTaylor,andG._Wentler_.   1983.PrinciplesofEnvironmentalAnalysis.AmericanChemicalSociety,Washington,  ` DC. 8  Ѐ21.4Maxwell,_E.A._Ԁ1974.Estimatingvariancesfromoneortwomeasurementson a  eachsample.Amer.Statistician28:9697. 9  Ѐ21.5_Midgett_,_M.R._Ԁ1977.HowEPAValidatesNSPSMethodology.Environ.Sci.&  Technol.11(7):655659.  Ѐ21.6Mitchell,_W.J._,and_M.R._Ԁ_Midgett_.1976.Meanstoevaluateperformanceof p stationarysourcetestmethods.Environ.Sci.&Technol.10:8588. H Ѐ21.7_Plackett_,_R.L._,andJ.P._Burman_.1946.Thedesignofoptimum_multifactorial_ q  experiments._Biometrika_,33:305. I Ѐ21.8Taylor,_J.K._Ԁ1987.QualityAssuranceofChemicalMeasurements.Lewis !  Publishers,Inc.,pp.7981. ! Ѐ21.9U.S.EnvironmentalProtectionAgency.1978.QualityAssuranceHandbookfor #  AirPollutionMeasurementSystems:VolumeIII.StationarySourceSpecificMethods. %X" PublicationNo.EPA600/477027b.OfficeofResearchandDevelopmentPublications, '0!$ 26WestSt.ClairSt.,Cincinnati,OH45268. Y)#& Ѐ21.10U.S.EnvironmentalProtectionAgency.1981.AProcedureforEstablishing 1+$( TraceabilityofGasMixturestoCertainNationalBureauofStandardsStandardReference  -&* Materials.PublicationNo.EPA600/781010.AvailablefromtheU.S.EPA,Quality Q AssuranceDivision(MD77),ResearchTrianglePark,NC27711. ) Ѐ21.11U.S.EnvironmentalProtectionAgency.1991.ProtocolforTheField   ValidationofEmissionConcentrationsFromStationarySources.PublicationNo.450/4   90015.AvailablefromtheU.S.EPA,EmissionMeasurementTechnicalInformation  ` Center,TechnicalSupportDivision(MD14),ResearchTrianglePark,NC27711. 8  Ѐ21.12_Youden_,_W.J._ԀStatisticaltechniquesforcollaborativetests.In:StatisticalManual a  oftheAssociationofOfficialAnalyticalChemists,AssociationofOfficialAnalytical 9  Chemists,Washington,DC,1975,pp.33-36.     *"dd9dd 9z dd z dd dd k"l(#(#, dd ,dd +  'QQ ' Table1ofAppendixA.SamplingProcedures D""3 d   DIfyouare... @""/!5"" @Youmustcollect..." 5+&5  "" 5(GX(Xcomparingagainstavalidatedmethod ' d  'ninesetsofreplicatesamplesusingapairedsampling  d system(atotalof18samples)orfoursetsofreplicate y ( samplesusingaquadrupletsamplingsystem(atotalof16 =  samples).Ineachsampleset,youmustusethevalidated   testmethodtocollectandanalyzehalfofthesamples. ."" t  .#usingisotopicspiking#(XX(G$#(GX(XԀ(canonlybeused   forproceduresrequiringmass   spectrometry#(XX(Ge&#(GX(X)#(XX(G '#(GX(X .""T "" .atotalof12replicatesamples.Youmaycollectthe   sampleseitherbyobtainingsixsetsofpairedsamplesor  threesetsofquadrupletsamples.#(XX(GO'# ."T "" .(GX(Xusinganalytespiking#(XX(G(#(GX(X ." " .atotalof24samplesusingthequadrupletsamplingsystem   (atotalof6setsofreplicatesamples).#(XX(G(#&(p   " () `  d  *x"dd dd  dd "(#(#x,dd ,dd +  0&QQ 0Table2.ofAppendixA.CriticalValuesoftforthetwotailed95percent d confidencelimit @"3)P   @T+  Degreesoffreedom 3"&!!  " 3,,  t95 `"S&!    "  ?1?`1 }"p? P"  ?1 ?" 9v@3.0789v@}3=078 ""pC P" 9v@3.078 9v@"  @2@2 ""p?! "  @2 @"" V-?1.886V-?1=886 zpC! " V-?1.886 V-?""  @3@z3 zp? P "  @3 @ h|?5?1.638h|?5?z1=638 ""pC P " h|?5?1.638 h|?5?  @4@4 ""p?! "  @4 @"" I +?1.533I +?1=533 zpC! " I +?1.533 I +?""  @5@z5 zp?P "  @5 @ V-?1.476V-?z1=476 ""pCP " V-?1.476 V-?  @6@6 ""p?! "  @6 @""  ףp= ?1.440 ףp= ?1=44 zpC! "  ףp= ?1.440  ףp= ?""  @7@z7 zp?P "  @7 @ p= ף?1.415p= ף?z1=415 ""pCP " p= ף?1.415 p= ף?   @8 @8 ""p?!"   @8  @"" '1Z?1.397'1Z?1=397 zpC!" '1Z?1.397 '1Z?""  "@9"@z9 zp?P"  "@9 "@ T㥛 ?1.383T㥛 ?z1=383 ~"qCP" T㥛 ?1.383 T㥛 ?  $@10$@~10 ~"q@!"  $@10 $@" ʡE?1.372ʡE?~1=372SIG!" ʡE?1.372 ʡE?" S   *"d ddd dd "(#(#,dd ,4dd , dd +  'QQ ' Table3ofAppendixA.StorageandSamplingProceduresforStackTest d Emissions D""3 P   D7Ifyouare... @""/!! "" @W%  ith... @""/!! "" @Thenyoumust... 5+&!   "" 5(GX(Xusingisotopicoranalyte  P spikingprocedures 'e   'samplecontainer(bagor  P canister)andimpinger e   samplingsystems ')    'analyzesixofthesamplesattheproposed  P  minimumstoragetimeandthenanalyze e   thesamesixsamplesattheproposed )   maximumstoragetime. '  ' .""E .sorbentandimpinger E samplingsystemsthat   requireextractionor |  digestion .""@ "" .extractordigestsixofthesamplesatthe E proposedminimumstoragetimeand   extractordigestsixothersamplesatthe |  proposedmaximumstoragetime.Analyze @  analiquotofthefirstsixextracts U  (_digestates_)atboththeproposedminimum   andproposedmaximumstoragetimes.   Thiswillallowanalysisofextractstorage P  impacts. 'e"" ' 'l  'sorbentsamplingsystems l thatrequirethermal 0 desorption 'E   'analyzesixsamplesattheproposed l! minimumstoragetime.Analyzeanother 0" setofsixsamplesattheproposed E# maximumstoragetime. *" $ *comparinganalternative a% testmethodagainsta %& validatedtestmethod *"' " *samplingmethodthatdoes a(  not includesorbentand %) impingersamplingsystems * thatrequireextractionor ^+ digestion#(XX(G9#(GX(X *"s", " *analyzehalfofthesamples(8or9)atthe a- proposedminimumstoragetimeandhalf %. ofthesamples(8or9)attheproposed / maximumstoragetime. ."\0 " . .""z1" .sorbentandimpinger z2 samplingsystemsthat >3 requireextractionor S4 digestion ."" 5"" .extractordigestsixofthesamplesatthe z6 proposedminimumstoragetimeand >7 extractordigestsixothersamplesatthe S8 proposedmaximumstoragetime.Analyze  9 analiquotofthefirstsixextracts  : (_digestates_)atboththeproposedminimum !N; andproposedmaximumstoragetimes. c"< Thiswillallowanalysisofextractstorage '#= impacts.#(XX(GA#(#>  "" (8_  $> *"dddd 4dd 4 dd  "(#(#,dd ,dd +  +! +Table4.toAppendixA.ProceduresforEstimatingSo C""2$< C(&m%X(XIftheestimated_LOD_Ԁisnomorethan l twicethecalculated_LOD_,useProcedureI D  asfollows. @""/! l"" @Ifthe_LOD_Ԁisgreaterthantwicethe l calculated_LOD_,useProcedureIIas D  follows. 0&! l "" 0#(XX%(&m"H#(GX(XAHEstimatethe_LOD_Ԁandprepareateststandardat    thislevel.Theteststandardcouldconsistofa L   dilutionoftheanalytedescribedinSection5.0. ' `  'Preparetwoadditionalstandardsatconcentration    levelslowerthanthestandardusedinProcedureI. *"L  *Usingthenormalsamplingandanalytical h  proceduresforthemethod,sampleandanalyze ,|  thisstandardatleastseventimesinthelaboratory. *"@ " *Sampleandanalyzeeachofthesestandardsat h  leastseventimes. *",| " *Calculatethestandarddeviation,So,ofthe H  measuredvalues. *" \ " *Calculatethestandarddeviationforeach H  concentrationlevel. *" \ " *Calculatethe_LOD_Ԁas3timesSo. *"d" *Plotthestandarddeviationsofthethreetest d standardsasafunctionofthestandard (x concentrations. *"<" * *"D" *Drawabest-fitstraightlinethroughthedatapoints D andextrapolatetozeroconcentration.The X standarddeviationatzeroconcentrationisSo. .""" . .""$t "" .Calculatethe_LOD_Ԁas3timesSo.J($t!  "" (#(XX(GaJ# `  ` ̀  *@