Document gyXyOGKM6Re03Vbk14BJgQvV

ngs JeanB. Sweeney pp3M Environmental, Health and aSrims 3M Center, Buiding 0224-0 hs 3M conan var 000 Zo Jen 0578-0537 A226 3937 oem RErPOoA PPoron maa East -- Room 6428 Attn: i) Section 8() US EPA Re: T TSCA 80) Sue bsanial Rise k Noe: Suphpleemenmt toDecketiNom. aSEHQv9er8o:375 I carboxylate-based fluorochemicals and more specifically, our September 5, 2006 submission on `water samples taken from groundwaterwells and from the water distribution system at the 3M HN ---- an on-going site-related environmental assessment of fluorochemicals that 3M is performing for its 3M Cordova, Illinois manufacturing facility. As part ofthis effort, which is being done with es Boel enh Ay Tere received the enclosed well water data taken from various sites on and in the vicinity of the 3M closeA d lee ndR E aapedin eim a ng ans(lin5gA locoatrisoAna, dnaE. dsua amayoblw en,Lorndyof `analytical report (Interim Report #2-Analysis of3M Cordova Groundwater Samples: December A dPeEeesi oor.iL Shm eeePnI neOo A RpanPehWrBo -- aonYeoowmemn enerAe-- eeTso(oaePcRPgomsahteecotn placing these results in the 8(c) docketas a supplement to previous submissions. CONTAINS NO CBI 225470 Page 1 0f2 2 L1uycobulehraavte(a6n5y1)qu7e3s7t-i1o3n7s4ororwdouillduelbikkeearn@ymamdmd.itcioomnal information, please contact Deanna Sincerely, See a3. Sunset (0%) Jekn B. Sweeney Staff Vice President, 3M Environmental, Health and Safety Operations Enclosures (3) Page2 of2 Sct rSemrepote 1 ee [osm][omT[ r Tm eme --m-- e[r-- m] [PLANTAREAWELLS | mwies | Macoos | | 1"oecooos | |wwio | Marcos| 175 | oss | NR ise | ses | toa 110 | 039 | 53 1 | oes | ota | | eos | ais | | oes | 125 | ee[ssw | sss | ero 5 |__mwze0 | waroos | | 1" Dec2oos | [__wweeom | warooos | [1oec200s| [_mwiss | maroo0e | [1Dec200s | [_wwssse | marzoos | | | Dec2oos | 831 | 23 | oe | 220 | 446 | see | 45 | 7s4 | 65 | so1 | dos | 17 | 2&7 | 247 | 272 | 572 | sos |" 761 | as | tor | 22 | 0709 | oar | 378 | asa | fo7 | odor | 0217 | 16 | 575 | 736 | 761 | 120 | 11a | sis | 200 | 666 | 23 | eer | 762 | | wwi7s | Maoos | 135 | 66 | 25 | er | 22 | eho ae [at sa|s aes | [wws7s | Mazoos | 32 | 217 | ore | ses | 32 | [ [oec2oos | mii | a1 | tes | 78s | tes | |wwa7s | Wao | 122 | 00s | oo | oosss | cores| [| Decaoos | 835 | 0123 | 00533 | 0046 | ota | |___wws7s | Warooos | 04 | <oo2e6 | <00249 | <0024 | <00250 | | 1Decooos | <5 | ooses | oos67 | <00250 | Oos4s | [__wwa2e1 | warooos | 234 | <oooes| 026 | <00203 | <00250 | | |"Dec2oos | 604 | 00344 | 087 | <00250 | 0038 | [_wwse1 |waroos| 413 | ase | ois | a3 | ses | peo | 4a [sts | omer | sa | isi | [weer |waroos| das | 121 | ose | 116 | 137 | eae iss|e | rie es ais | [__mwssr |Maroo0s| [ 1"Dec2009 | [__Ww7es | Mmarco0s | [1oec2009 | |wwsse | wa2o0s | [| | oecaoos | |wwese | Maoo0s | | | Dec2oos | [FormerAg.Well(#22580) Dec2009 | |PRODUCTIONWELLS [ Pwa1 |warcoos | | |oec2oos | [ Pwa2 |Warco08 | | 1Decaoos | [_Pwas | maroo08 | [1 Decooos | 0135 0091 537 634 984 ere 148 635 511 222 200 369 441 608 574 | <00208 | <00249 | <00244| <00250 | | <00303 | <00255 | <00250 | <00253 | | 245 | os21 | ass [ 11 | | 725[19[768 | 208 | | 4 | dos | NR | 134 | | 22 | toa | 13 | 127 | | oosss | oie | 076s | ooers | | 48 | oss | e691 | 193 | | <00303 | 00604 | <oo02s0 | <00253 | 1 | ooese | <ooass | ooss | 0266 | | ote | <ooass| oti | oars | | 05 | <0024s| 053 | 291 | | 13s | oossr | vas J v13 | 46 | 1e2 | asa | 114 | | 703 | 163 | eas | tas | S crmtpoerit, e [= ra rare FwaT i 1wbaercszoooss|| 2r6as1 || oasss || <ooooemasss||oeasms || osaro || [ Pwar | wa2o08 | 139 | oass | <oo4s| 0283 | 0383 | [| opecooos | 139 | 032 | <00255| oa40r | 0698 | [Commercwrwerts||| [11 |_Rierstone(C-1) | Dec200s| 0788 | <00303 | <002s5 | <002s0 | <00253| |WCeshtiwcays()C2) || Dbeecc2z0o00ss | | o4or5e1r | | <<o0o03s3s|| <0o1u4s5s| | <<oooo2msso0 | | <<0o0oz2s5s3| | 6 ort naycri [[_--_ccrriiccs4)) | I Dbeeccazooooss|| o02s1t1 | | ooussr | | <<oo0o2zssss||<<0o0o22ss00| | 0<0ou4z1s3s| | TCTh nA eoa e sa Se EE.o-- a"_ 23 i a BR ;: 0 8 HAE. me Lg) i \ G t T RY po -- l=] 5 38 fPRCTTgememVaie ce H NRE ayRY pt A es SON.Be | OE A lige Hyi c : |H See BONA hE . "rg NN eh a: EN 7 [RE kN iy NE i 9. 3s aN 23 ... SAS EERE x aD cA a "5 aR A a LN CL Bel iN ER ER A - PN "Na hs ERAN Pore iL ` BR po. RET on Rec | ie fl 5: ns r-- (PertF uoirnGiuO riaaAncrvaeSueifyorsnsUt)osefiP(negFfFLBu)cR.rbGPuatrahnfuScortcoAtuhhadda3yn(eTPsiPFutEol)hne,sPerer(hPocFHr5co)o,channdceAisPcsAomeddscsdirmoePccnFitOaRln)c,rs-kulPColnas)neo ho 3 Cordon. I.Facily EPATSCAGoadLabDoarattaorRyPeraqcutiiosrSetmanednartds 40 CFR Part762 sWaSetistunodnyKSoosDalirtriiPes.c,Et.ionOcr.EE WPehso1tn4e0C:0heW6se1ts0et-ro7Pn0A1W-a135y736610 SM EnvoSnAumuseatnnthlWoLorarbortory Report Completion Date Date of signing aMEnvPieoerrfmoenramlHienagthLnadbSoaraattOopreryations a0ECnaornem,e8n6gaZLa0b0or5sNtoAyT Mapiewod, WN 55144 ProjectEIodreonttiefication Total us Number of Pages SU ocronrGo:avnn aSperrn 00 Pu as p.7 cowenTAL Trispagehasbeenreservedfospecticcountyrequirements. 31 Cor0d7o.n0G14 irnaRaopere re2o:008 Pas20tas carves Sfoa FGT LPoTeCOMmP:TnLeIdANe neCE tSeTr A4 TEMeENT Cnn0ne 5sG CGo aRPeS SerrDrTe0roy Damampem s nser rcs org TokSG 580 Al : %0 = Te 212410 EcaTm miT n sans ps cowpea QUALITYASSURANCE STATEMENT ReportTH:InrimRr#2Analysis of 3 CortovsGourdeSami:Decarber2000 StudyTide:Analysisof PerfuorobutanoicAdd (PFBA), Perfuorooctancic Add (PFOA). Perfluorobutanesutionate (PFBS), Perfuorohexanesulionats (PHS), and Perfsorooctanesuifonate (hPoFOCS)ionGrrountdIwLaFotaecr,UisyingLC/MS/MSforthe "3MFluorochemical (FC)AssessmentWorkPianfor T2a0ibisntayrinmcalanaphnahosaetavokgasoenenadugstmtodyeabeynoTchhtero.3MnEdinngsvweererpLoabroealbooryhQeupaiycAasu)rmavnecseiUgrs (A(PU1)),. [EE [mmm Jiemn[wn Joon] To D2oe-320, CorConoG rvinnBgeema100 Fra iotras como A PES ; o te 04 0 ommrgcitn 00 EL ee r --. E ner et 8 rr career CoS Oe Tremes SampleDescriptionKeyCode. S-------------- mn at oor Tats, tonContss EE" TE il, AeE A ire --0 `Table 5continued.LaboratoryControlSpikeRecovery .... Ld Tabl7e.SAMPIECONCRMGIONS cori ---] TTeIsDUCa tOeLMArN nPA.AR SEE Table8. FieldMatrixSpikeCONOBNUIBIONS.......vm messes 2 TeoeescCoovvPommaSRRmPaAL `Table 12. COIL-GW-(MPlWan-tA2re-a 90 Wel)... TTaass. ccovoamvamesPsvAen messmo mae Sl ow" on eo TEEN, pens como TiA 1OLMSTED EToEwn cover pun -- em Feo t -- -- Ti COLHMNTAPHD. Ip a ---- eo A Fe ---- A-- 30 TS, COLA PR COUGH PAID. Tah.Cova RAED. A o--n- Oo OO -- i E 3S 88 -- pS ew enSEE nn ras p13 coupe oS a) sponsor 3M Company Sponsor Representative GESnpareocyrimHPernietaecM,naEnNagSeGrporstons BSPlhoahn2ea:2845u51n0)S7s3t7a3s570000 sStaudryhDeirnecstoarn@mcInn WWJeeossmkCnanSKtoesnrasrP,,AP1En6,d38O0EE PFraoxne0:106/170017-0714307161 LStiusdyaiLo@cuateisonosoiioonms Tosting Factty SSDMMuEEnHngSTvOp0eerNaArtoTrLsabotoy Maplowod WN 55105 Study Personnel SuWitfeonmaWcoKyt,RPreRgDelne,cPmhviDe,cstiLagRbeeolrvraGetoriy MBanagercom:phon 651-755.9851 Jonathan icege;anayst Study Dates IISrryanneAAvrvaa:cyaa11CaAotpmop2ni0n007:81D4Jecaembnera200y0100 ILorcaatniRoenopfoArCcohmipvteosn: toof iri Roped iin ALToosragainasblarsmaocweodnoatrtaiarnsagsna1r0dc4htti0hveGednFosRalBhratersJ7y0a3EpnTtvhihraovtneesmbesonuotbnsLatraacnbicvoeeardnaadtaahrceael3yoMbanElnvtoieo4rr0emnGacPreiRaaPlnoda7r02 cnerroGr inngEE ramsarris p14 Cowen FS RS TPorehareikhn3oroooEfcomndiaonongnomoesfs(neGC(tMFldGaLCA.a)oyOb.Co.rfPFeIuyScTeIso3oc-cmhaW15n1e5o1css)ossSp(aePcrmFsOpeoAan)snfPweaeoyrrnusaeopaurcvneaptnrasarineeedsrans1.d3fa, o2nnc0alh0u0edSoPsgFnoEcgSr)ow.sitDoof e CPoemotrtoenryseenfsootnaol E(0PE7H01S4a0n.dPrhcrsiane toate(FOS) ur 3Enionmertl Fe THRA e FT SSTLSTRTET PeTrrhtoucotrfaocntsviweoenosftlhsocsmatsaetusow.ensS1MaCnaolyzaecolalecctyed rtoeusrevatcirnsdamplefcoamrmbooronreiagnadnd The3M EnvioomentlLabor rare samplecatsinrs 250miplot aSiolnes)ewrhcsh `were shipped tothe 3M Cordova faciity priortofield sampling. Sample contfor each sampling locationincluded a fieldsample,fieldsampleduplicate,andthreefieldmatrixspikesamples. Each C`CSoeoomntpctotaiyinoncnoenrats0ardi1einseinreggnwfaatpshemadrafarofrkroafreibdebewlddsimtomehfbMaai"oxtfrisseptitoik,heeesprraevimo"rpillneebstaowiepnrrsoefdrourtctei0fiaefhdiwnifatlhsdaanmpoalrpepsrvaoopllruiemacetleomefac2tir0oi0nx.mspLi.5k0e0 CSaamnpalresywemreepireoparEeTSnd15n4ayDsetsecmaonrsaincgnoclhPeprrrveacteedeAdced,nAcoMhoEsn,vAorrimone,rosnld VSCSpouttemfcp,ooonauuStmneoesdtinsnyWaEStTetSir.emb8yo/b1ySn1oLl0bi:dyOPMLheaGtMshMeoESSdxMtorAfSacrtSaianond:yeaEcnTsDodSHn.it5rAg.vh0rc4PD4eey0rtafDoaorntmaarinmociennLitoqofuniPdooCfrhPriromtuaectoisgnCroaepmdhpyo/uMnadsss n Semobilvtbo7crsosurmnmrtastpcisoseptsthPsraomppelreraonut2ssr7ou0n2g4hweians Samleothowdisdepntoerd abaovde,dAalecss fr re Psa -- 4Tet& Control Substances TNT R sven ti tst, rere YLeTm Sr 5" ReferenceSubstance7s | J TET TTT TRI 0 tt OagmsTTeE TRY [[[rostSuomcorosocommsaumen| ce||PoGrorinmooao| | | eobrmruooa c| | | etcomsrasonin||| = Kirma: [[sCowmeoro | vSoemr| | omweemse| | onwems || [SoopoCondtons | Fon| Fon| fom | [[[CorPohmrosnotiecoheumser| | | owworavatosonni| | | wvor swws| o|uooe wnrrmr|| || Fo ww 1wm wm] [te] me Tw|www | ame | [[[CCrwommcaairtiaammes||PotucrGohresoanseosurton| st |Partuooroocransisuko| nse| Paorfuorroocoanose ||Pertucsroorcanesouns|| corms|Saveae: BR bSaivin): [[[SEwSme moeo[m|TcoTmwaWmemgnmor| [ | s wwerm gnen| | | wfmwoatm| || ooewnwe ||| Trosom |mn| [ToRMamber | Toroeobis|Tomsoor| vorim |Tomes | [PCrmeocaDosoptoT n| w CoaneT |w Gratis| 1inkwepmonserT |w Waapow] ar | eocra pons reso -- rDS e eiRmr Eme r rma r tsrt Se tnocote [Sogtimbw Jowgowown TEeSEaasme-- | " SEf SnEr n R 71 MaR tas SATE R fp E E a orer n o E pe mm T nhes eT Ceeres 7.2. SampleCollection fS rmE Er E e Sampleswerecollectedin250mLNeigeneTM(high-ensitypolyethylene)botespreparedatthe3M 7.3 Sample Preparation i 731 ETS81104 : `Sampleswerepreparedbyremoving a 1mLaliquotofthewellmixedsampleand diutingit with 9mLof --m C E mTcrsm vee yE 5T a4E 13tde ge s cen, `methanol (dilutionfactorof 10). E wamR mn J se -- H AA Er A TER STAl samplesandqualitycontrol samples wereanalyzedforthetargetanalytes listed previouslyusing r EuniteE er instrumentparameters,the liquidchomatography gradient prograrm, and thespecificmass ransiions S ES T E iwe Sow [osuomantiome1 ersomge | credo | [ouscotmn | peneommxa|oi wein Cio(e i00mi mX4ss mme 5,| [Asscsicstmn | bemsicrooommxzimmy8 | sensicis100mmxenmmsu| [1 ones gem TT ew | re erro a] [rPorm -- eaez wuetees]| bel m0 J we 1 CC mee eo Tw 1] CT weTee Tw 1 30] weESReE ots ee as rte [oma [T Ep =r Em oe | we | ime | IT ame] mew | [mm| | I I [own| 8.1 Calibration - e EE E E t ECeR aiR rcnamy T R T nEe o E nS isLsa includedin the finalcalibrationcurvemetthemethodcalibrationaccuracyrequirementof125% BE aBE I SEr E EgEaEeTErc S aAe a E S oE k E r :L S CEeSSs ERi preparedInrevers(ReO)-purcifisedlamboroatosryiwatser.Calibrationstandardswerepreparedby EE p19 pr 13 ETseaus 1{0ao1r3l0tfaanniaosetsapndlaerddassatwabenrsdaptrrerdpraparrneegdpibanrgyefadorpmeg0.l02eo5uringaaim.tou1en2rt5snocfgaosis(nrogiancachoawenrascnaarnaaabngnengsos.hieaT.hoA a2e105l.1tc0o,,uartcslw2ba5rsnatugonscvaveoeofpo0rdeist2aw6fo0orfaGhcahsbareaater.FpTFeheBekScaattormaweescrtoouorostlufdoerfo ehrrahmaa8vaenscainnpg,o0s0 cfavilentrgraapicroonolctceursrav.iCoanctcoaunrtvfamtneagcnahdcocrusretaawcnydaorffdrcsoosnccchcecuntrtavrtay.tpMoorosru.hsEdRCEtlhcbapveeapairnewaaaaicscyu sfaeradrn onrvesad egr i1r0v0e1.2T5%he1c00o1l30o%nfocroshfoiocwenets(cwevsgproens)owrearenm0e.t98f5oraorhPaErGaSt.e cednecokoraon Mdu8.to2imoSnysscttiaeanmts osSfuolatvcarabblarlaliutttotynyasbstiaenydaArcdvaemrpsaonazmedestthhaecboengtinainncgeorfatthaacnacsslbsaeqnuentceu0 1m05e%eavestandart(RSD) ope Sr ad sshana cu 1 30 RSDfor tern 8.3 Limitof Quantitation (LOQ) TahnedLsOcuGrfaocrytreiqsunireameyntss haenloowewshtinchrhzoarecaaCtoerattosnstandeasrdtinithc1cu0rvs tofttmetaspinpary `blanks.Thenominal LOGforanalytesbyenalysisdatecanbefoundinTable4. `Table4.LimitofQuantitation(LOQ) CS TTT [nee Terssrior | 0 |7o0 |oom | ite|oam |our| [[--i oowTgeorTsersssotsueso|[+1 [owoao|]wwaaT [wao[m amw |s | wm]aa]] 84 ContinuingCalibration a`C Dnusryinzgatdhieoccoa ournskemorfeaearcm hhaeonfaa1ly0mt0ice%al5e ns2e5qru%eesnwpcoienn,shcel oanatnidnbuhoinwgckas lasixbcrcaatapilionoovnresro:inficcaatvioenwsaemrplies (GCCrVo)lweArle: 1rC 2a1ck1e0t8arnO epao l7-s5SaeaA vmeeraisoeeetcnsCCoOL nVOsoLveGrsAsNo5z4.CdOoLgSWaAcNurseo76f,thOLunG.OWnACOfoorrPVFBS bBr1la2a7cr2kk2ae1,t0ae9ndadpnTotprBleo-srakom.pvlehenosdCoalCseVCcOoveLrr-ysaGofnYs2C.4(%6.arnidngWSh.acCoOrLseGWhGe,uCnO,IOLCnWGSC ,fEoarPvpFmOeArt Amehoddviaton has baanininchourdoed CocrtoornSo ma gSeerr080 ron otras p20 cowpama a8s5i BlEaTnSkse01 `SrSrivaey:aasFscOeonGtabrapsrak8rskdoafww0ee1rs0saaotdhroaoanatrvreoadveiarnsmdcaonadyopaerwoifhmeardrowseeaaerdriws1a.reeannssze1d PLr0oGgor00h [rope TSoheorsinypeesaoaLrOrkGksExasecrchshrapknaoreeada1nsdnavi 80hdhohdsa1mpslaesk:meambebha'npksreacT0 ark, uss ETSs0u0 Tw2vd oeyrpesaoofbbr aeorLksOsvGi veoerrrospn eheorawesgedhdeci.dcanyowehhooadmplneds:sasdch0edovorakts amrodtSoodlpd robmaraknsc.e 86 LabControlSpikes (LCS) La saercoaEsSstoneegtvorHpoefeerferdenncchmaaraesvsocadoorncaratva eof.(PTFaOiRnealdcoPnEceOnSar f50 renepeaieeeniasnhoatnareraCa:om,LcoOasaSGsfahemqoensaotoofebCsvSo.pnernoteaneatpaePnazdatrrawarennlccohrSsaaPc,FmOelAhwoseworeadovsP.UeF:M OOSCcwelroEsTa5rS8ego pca1roe1msp0cad 1seGoroosaf Goor 2S ahaveragerecov wih 100%32075.waRSD S2:08. AlLCS routs et se aes Esa CLSooowienmnnahogswhcioa8armecodounrsctoiloofkee0e.rsA,wneiyTroSpsaroSopfEedADrpicLaclenataoSvnSarnayrsoishsnceawomopioveimsscEsiaptTpna.Solce8Leex.Cndrd1Slob6scsv4weleda.srTaoGnyhpoorasmvenveaphattazhleroeaed0deds1 0ho eG S naiao nrr meCSco3hhwv vastiaaoa lS1eava 7tsrs9oe%mr.eothwn tecAhrLmsLoeroCSadoWvsereoogpastraianycreoordoosoLwmiCiSnhg ebceeaepneiaoynnfOiP0cE%lGUAr2wo0hri%tcawhiyha.c8aASnmOato EAFasPotOi.heToarofertreFrnsroOeasStgmveaerrtecsevovpaserrtueypsfaesrrdaedmooprllqeruaaatrncoincea,adtoomPnpwFofOeoPSdwFoOonhfAbcaaaonncudahPtbeFoddOsoSaiamcmravreesh,rleiLoctCocmSoihspenaapanndcrylencaaloreb,orraaannwdcinhhhaeaan l veageremyof 58%, Arena deseo lodwihDerow a. eS Pontes p21 conerenTAL 863 ETS80MU0 LsaopilwkoiangndakinnogdwhMnaaagbmnoceuosnnittuosml,osfp0hipkeerasownaecyrsteepshrieedipaeorasebedaadracntodonrcayen-natplrryaeztpeiadorinen.dTsylhnaethtsepetii.kcegdLrwCoaSusenwdrewSaratemepprcrloeenstpwaaienrrienebgdy en p`fromreetpthamerseeetdsahaonmddpalanecasolesypxzicenedaeicdnectehdertsh aacmatelhtemraanilgnohneLrrCaanSsgtaeht.e Tsahgmepmlmeetsc.huoDdduaecncotoetbpttheeacnaNckgecuhaertaecdu,rv2aebveihrenaaggreeGosecfaaob1ueLntdOs0S msehtuhiodbaecWceiptnan1c0ec0%er20.% wihan RSO S20%.Th averagerecoveryfrth lowsetof LOSmet Thefollowingcautionswereusdfo generatedaainTable for aboratrycontolspikes. OSPR + [meCr onno-- n LoxORRep andrmdaetiConarOSmtoc. MCartonGi Some808 Fan tsortts Cet | de I ni | ffoe]n [||[Feeef| {|eecisaz eg 3 i FLEE Hh : k= dgpoof|J i ies $8 lanai pant nl if i J! 2 ices 2l | ed tes fFtoeoe]t | HcEe fforroe [= || [Jeose rt 1 "ee[Lhte] pes] |Jee | letTJYoreseya i eli fi | ogRasqaa) see JReenssy | [eee] pJpe]a| [iefese sp fll | i i |A mingd |! HE 84484) 8s | | Wp I Jo i] 1 fe oJ if gr 2 4 334284] ieee p28 coon Table continued. Laboratory Control Spike Recovery [ro eeee| ee | L[Scosse-rroiiaoernassTs |Seriorse [LCS-1001134 [LCS-100113-5. OvSaooosni ||| oooammne | || 1w0e8 510 NAP ae fo5.10 | NwAeP | a we areas Fr myR ttrenscR cetace t 10f.t vet set0 T8e.7 rAanailyticeatlaMreytvhaosd Uencrerrtaibntay diron OCdat ht idooamebod `accaundrpreacicsioyn. Themethoduncertaintyiscalculated followingETS-12-012.2. The analytical m n erroe aebyco ova p SooihSuoSi ta sarite oG5od%t.oeR wba eSnan e p3a an rTmsrasso ab' `uncertaintywas determinedbythestatisticalevaluationoftherecoveriesfortheindividualanalyteas ere may oyran Table. Anayta Mthod Uncaranty [rCr ooomrorm T|emseeomnomnooor srs[| [orinrm[|Jwor rmms ]|-- Tor eoet-- rne]| [ome Com | eonor mews [so m | wt s | iu inn|] [Ch[ooommsee e eoTems m s[ww e ToS|s eoT mw i | T|ius mt| e]| omeTreo --TaT twa ia] a aro a ot 8.8 SampleResults `Table 7summarizesthesampleresuitsusingtheanalyticalmethods identifiedabove.Alresultsfor oncorr mm gn J. p26 connpem Table7. SampleConcantrations CC eemmcoemmmgs| I fBausnses[Fsochvonowm||mwrooas[[arssosn[oo[roesono [[soeoni nws[[e aewoass s|| E[ rase koa veoomw nm|emwweee iT|osse mwu|[nawroJToed w osn[a |awn rl r | [ fw orraamemf o ps o ov vo onn ||a0m o0rm [[|i eosm nnmm [[|o owwo oesd [[[om raeoswn n [[|oawne se |]|] [ [ wmos w mommaas e raJ|eoosrop|[oo wwrmp[e oi wen[[e swaee dn|] Frau Frown f fo orvoom e m||owmsz||oawl nos [|ravo or ||n ood ann n [[ose d wn|| [Ew [ CmConos s ow o momwsum|ww1o s7e T||n maeospwno ||[o ocmvoi s2ror[J|s oooaomnnn|[|msaoaawm 0nn||] F[ ranson ea osnmoenw w u|msdnoe[|eowe owne [Tonvore o[|ad sarzn||eoen med|| [ FFrraew aimmwf poo ovvoon||m i10m e aa0|[|m i oo0em0n [m [[oo5o mmo d [[|rw 1owsm sm |||sswe wu||| [r [ oo osmw ertoe r[[p o4w i [Jo0an[[0g ow2ne [[o0] e|| 0ENR i eCsawtPiETm e aESeATe o taevs rm geonyoePt PcEhWEnCe Topci no eLDr dSas.hoSAmhyn 050dTrthsmepd dned101e.0n08T1e 1 1 SS on e eosrroimaayy--5n0--TosBHonbrdh ETE1543 10 ETS A ator 8,$0 0 RD 50) Ro pprome ortvreinahalrya5ree]iE2e5a0ms04rcoeddiic.utE1o55O0K. eh a 3 Ener cboonnGan remogSseer2pen08 Preniais ---- Ts. SC BC oss JT om Tw [ror[rn m|om[rn| [ErrososEoro|mmomw[sas[owm[mno| FC rown boramml esscnsos |mo oToorw[|omwn[w feanm[|eere|| ow -- mses 12TeoTsTos |o| brroovneerrse EEovoommmnemmsom|| mm0w [|nomwso{[woeou[[awwrr[n[omrrs|| E own eoe ar[[o0e rTTowm[ad rwon[[0| Cae [ow orl [owe[wr| mwosumpwsom a |p2e 4 |o1g 0 |u40e|nood| Ca urine voe wr [JwoorJfaoonl [[0o0on|[om2e0r|] braves on--om--m|peauyr|Psooen [oroaeony Fvrreems|poormsey| -- E CECE m Te u H estosi ar0enJto two T, Cewe letwd [0pen] E EE EEr E e e T E ETREeReLe SnEen E T EE E Te -- t omarsms ei p28 cowpema Ta7cbontlineed. SampleConcentrations [1 semmcoommnomy | puso [oemeomevn [ron[ron Toros Tomo J eros| [poewwn Eros l----ovamm |se m[soei[ocmel e [oomm|aone s | [ [ oms a mov ow n0s [w [ooom ns[[n oo amo[[r ooo mwo [m [oom mwme|| ffemroraam__fooftomo ma sncvom om||waw w rs||asew[|oomwp a [ssiwn||evwadm|] [ w [ wosmpuo2m6[[powwve n[[2oneam[[o0wn|[rae|| Frown_foouo|wm w s|mena|n voo w [oo m [mwom d| [ [ wwosw emvsw0e0m[|ep a14 e |[ao wu p |[owk re|[eooor|| [ wo d sme voe mboor n"[oi wnf i [eanme [zomd een| [ pErorws ouFsoev _boomr1om |[m2oor seu[[[ms11wl r2ans[ o[|vs awasmco [[[evoe 0ocw[[|owaanmnen||| [ s [ mwor smve s0m0 |[oroawn r[|oo wannw |[re an|[eoewl ur|| N0 kPoeeCttptemie:nnnohrorTsoEorbtino earieLoAn5oLyAoOmPrOETAcEO11090v%ePtLtOtSoSDA oyLOf5R 0nc0awTeB SrphaltoT1Lo0.k0Th C 0@ SFn oaa pwsedasneaom aovereschar5ov0e n1 lvrS eosmdtt reae 1s ETE 13.E1561544 HA 5 RO,SB PH tn 5(0[PrmaepsaemsntaastehSrrohoennlo8pnpo0es1ai5mr0e0e3 hdstortset.Eo1.0kn MEnters CotoonnaGon i neSpoeter2r 00 [-- corsa "T7acob ntil nueed. SampleConcentrations fC ons [omer [ToTT m [wvose[7me| sno[| Mma memodoown[[uroTonor [Tuor[oae]| wmmlm o5rT[o 2o7[m a5me[Te eoen|[d ar|| Cl Towno [oom Loom [omer | [CC wosmpos12m | we a |owem |i w |nwd m | [oomotonwos -- EC ranan bmol newnosams e aw |ooo wmJfaammse o[n voew|[eome]| [ mommm0r0o 0 m we[oa w|d n] Eormonsbo[lxoian |n[omw nJooaommmL[omnno[osrrs]| m 3 J Ee E E 0n La[0_d T enLu] J Ea E esTE oa I Ea ETTTL cami eR roves p30 cowanm Table?continued.SampleConcentrations. [swore| pumo [swmwomcoem [roa[ron[eres|me |mon| [rosomwn wwe [oer [i [ew [wr| [ swosmwstre [ip s [ean[oem |ewl u | from bovovwasonm | vo | os {ams|oes|om| framfovov[1w20a|ocm|oomso s|onwe s |emn s| [wo in [ovo er [ome[od ar[omr| [ wwosmwso00p [ve v [ownn[2e2[aowd| from foovovmsrcoman |1 | owe[wuss|ome |ome| [ iamaed onTose Jaume[ior [omen| [ woosmws3m s |p00i|owa p | wi u |nswd| [commemwae ~~~~ | Eos bovoncrowm |or |owes [ams[comm |ams| [helLe oon[omn en[comm e [omer| [ swososos a |ewmwe[wam p [wme| [re[ol or [owe foi m [wom | r rrosemse 12r |wi a |oon |nwm e |wd m] C 1) PeC eep: erorCErTrg1erttn ehslbo dribcnfawTdE4E0hnn1dea1hs(v31t50oaSoe aLyC)v 5k0roTtehh tpicfmeeemd310.h E0@mSSoomrre aerrstaovearstbym k0hiad noeryraerre1ETS 143 E6154 GR Sn . So isci (50 Fe r Torneedsrpgea pa eiSmtereeaordgm at isrnSiEro31e5ns3sm00c6ecmd cmitrhteE1S50e0 kadanEres CorCtoornon maarRSgemis20 Press J-- SN bC mTns[omeT r {mew Torose[rmeLonn e [o]w| Ffoermos fom evesimm T|ooonm[[oeon[[caomTTeae|sTeam| --m -- re2r 1 p0re w pr y wpr [powry I E amos 0o [[oooor[sour[ooawr|[su]| CEooavesbovToooumrw[focoomos[aaormmssr[oesuonoe|[nmwaosrm|| [ m S EEy TES Ho--EeRs T ,rm erpoee emss s cemuopm ommO mn m E |no 2m2 p |Ce Owi m a|n n etwmdd |0w0m E FE reiey , r eemranTen.ssmarts 3 S E Es E RES m T S eee a a a roma J-- 8.9 Field Matrix Spikes (FMS) 8E 3 HAAMeSSSM EiNe S)rparenree eiorSy rriirirere goemrrciienn cnsters, donotsignificantly interfere withtheextractionandanalysisofthe analytesofinterest.Fieldmatrix ev Smete,s tsa) `spikesarepresented inthesecton 9ofthisreport. TT ems Table 8. FleldMatrixSpikeConcentrations. 150% b rr a [w0o0[|e m oewm[[oomm[]e a n0oorm|] rereFarrasmaann |to0|oo|r|no[w0o[|ow0s|| Bs Conmrcoi e [0e[o| |a [w0o0[|wr|| br m a es s 0|e wan||ont e [|wooos || ewn|| AHETH onrreesstnuemses || 012503||cowo[ovon||51 |[ovewo|| GAS |laosuera||520o0[|n0w300a|[oonwm|pw0o0e||oozsmo|| m CEIbf sre ms e e te a L|Twor eo[||S oonorm ||Loe o0|||wmee e n[lwsnm]| Ee 8.10 Laboratory Matrix Spike (LMS) "Thehighfieldmatrixspikeconcentrationwasnotsufficientforsamplelocation COIL-GW-MW-1-88for T D ee e e i oTaens, 110.1. Thepreparationof laboratorymatrix spikewasinadvertnetlymissedforlocationMW-9-84. A Trr e ne mr re Tabl9e.Laboratorymatrixspikeswerepreparedonthefollowingsamples: n-- i, ans 5.33 conmoenTAL Table9.LabMatrix Spike Concentrations. C C COO OUO U GM105N G 0aN0bL0iA A LoNMaa2rrN R kSSS8pppaan||| EECTTOONNB1TZTSS EC70140133 =w E conor ve7n52s600LaoMae eno PS seamen (0 Sarg ConTisAtvovgeaecCaarincciinnoon: SarisBSASPRDI) Sa SR NT LR 1 bed l"oTchaetitoanlsesabsewleolwassutmmhaTrriizpeBltherkssa.mpRelseulrtosuatnsdaanvdefrakgemvaalluroxssapokroruecnodveerdiebstfro ehsegsnaimcpainntg if2gsu3er0ed%si,acdncoomrortdnaiswnhtgdaaftteoa.tEhFPaiAtetrlhodeumnmadaitlnhigosucpisisk).ewsBe(erFcoMaaSup)psrreoepocrfoivraeotduenefdsoimrnetgah,iveiagnliguvteeshnmemamateyrtivxhaaoynddaitcghcheetptraernsopcmeeccttihevoerseaof r`Qsuatnimataitvehrsaangceesp.aInncehoGseaitns,tarnciescwhaerechaetmastaappberaopiacahteMatsricxasprk reacnovderrieescdadlact W`sCapOisIkeLhG(eWLoM-nSMi)Wa:atp55p.0r90o0ppRrp:eTswhesespipkrhlaefrvoekld.am3acTtohrmiepxrsaepcrokevedewraytsohnfeoshtaesLumMfefSccioenotrcefPnotFrPrBaFAtBiWAoan,S,tth1he4era8en%fao.ryS,ticnaaaclebthmeaLttMeS u`ncerGisitOyforIPFELA ThhLeesbMeGeSnsaWamcpulsAifoodrAP1E1H0WS0h%a1&d4a8%.r.eco7very5of13:3%. Tha recoofvhoeHrS fyor PcFonHcSanwtaatso9n0,.i8n%e,aSnianycteatlhuenMceSrtwaainstythfeomroPsFtHaSphprospbrieaetnesadpjkustleovde0210c0o%mpa3r9e%d.othesample "WTsapahiestdepilrgioehvpetfualoi1raese0sdcm.0Toai%mhtpooar4srep5cdeiod%kvee0wryiaosfsntaohmtepsLluUfefSiccoifneonctefPnoiFaBPiAoFwnAa, ,sthDe1ear4ne5afl%ry.etSi,icnalcuaonbchearatLatIinxStywsaposrktP(hFLeBMoASnh)yastap2br5o0oeppnrgite PcF`onCOcOaISnLwt.aGatWsi-oM7nW5,-.3h7.o%7.a9n:SaiTltyhtceiecahMleSunMscaSemwdpaalnsettfyohfreoPmFPoOFsStOahSpafpdraosprrbicoaoetvensearpdyukosfil6ee9vde.l10%as1.0cT0oh%moprar3ee1%dc.ooohfevtshaeemHprSlefyor cF (onCcOeIntLB wrGeaWstAi1oMS n0W,6-t%A,e8a1Sn:ialnTychteietcahMleSuMnscSaemwrtpaalisenfttoyhrfeomProFPsFStEahpSaphrdaopsarbrieeacteoenveaprdiyuesoltfee1vd3e1lta%o.s1cT0o0hm%eprar3ee1d%c.0 otohfevshaeemHplrSefyor Pp`FCaOOIrLLdwCo1a:nsT8h0e.2L5S%asananmpdpll8e5o.cf4oo%rnPrkFeasOpkSoohcnta,vdol8ar.eacSoivnnecreyaohfouL6n6S.cw0aa%ts.atTyhhoefmoroPstFeaOpSpchroospfrotbiaheteevMnpSicaekhnldireHvdeSlyofaosr100% + Cortoonrr o ronReDa nocnom1b2e.r r2000 Panzsoiels oo pefracas o| i: oE bft pes t me cf FA ft 1iHl fi ii) p : H HH] H inHiH Lhbihf R EEE Eii i [nieyd| Jesesli]Jeeves Ho Meltrfl 1 hol [nb f Bele, iH Babe bs am FEE | i , i afoty|i | E fool tied | ; i ]elereid | ` rmse ili il Eil EhiEi IE |3 f poet 1 Jor] he I te ded JI ETUC TE ott fi HilT] gtfieenes {cainny it he |Lpifna! d Hy g i i i Jesll |]Jessie 1 dtd {| LD fe fod od | {de ST Fesrda|| |yrezeq Bl: | aE i2 A [geeiesd Ei giiit ltd | For fJfooonssod||| Le fn| Pol fet i; fateid] ail] i i | [a fo Fed | od EE poses] H JL EE he H}i ii | (| Elglx | EQ fn HIRE i EEEEEH felis | jab iEle dn Rt H l RL EEEEE| sic cece (mfhz]Co Bedted Fol eesds |i |g I i oYat pl Ji i Ht dat 5 gfage 1 Be BHEHR [HE HT HER pgiEREy Iii HiE]LIEi Jedd 1|H pel Jit | -- H3E ; n Hedfl igidh ETE gl lezeids 1g] ifieiHs IEEE dd Bl LL HgiriTtHlhN l} JE fil fFiaeld l|| eb be dtd | i IH HH i 40LB Saaiti] | go ol5ededt 4]1jl Jost Jeet 1 feide Nl bode wi . sd 5[| fgiians flMILE kIfh | Jit A il ETE TLL fed | Fall dtd Ff] Fad | fit] | Jess] bat i {{aIn | de {iLLpy aset iECo prised | Jef] Jd | Ifood fy | fe | 5{| y8y {LE IERIE anl TIT ht fJody||o|q oIse fe | Dedo t efl] niTami i | iL] aHA l ne EE La RRERE 2 23 i Ed ollie bose {folafft i 4) {LH HE 1 | gh gael|| |yrane El goo J: ed 1ii fi | ndikemdi | I] |ei`zgz giiidgyl fil | HIER TTL ae : 1idt! ; Hd feet H1i] Jellies HHL be Bessa lleessl 110 TeTiell Tardrat W1H1 HR HEE HR HIETE : Baad] THTiL ft go 5 it Eelyrel1] odie lf { In ff i! : Joie Jl i ll EEE, Hi CARI EEELARA EEEEEE file PLR]|| Ji] i LL at ELef yoo [Efiyo lIi . bob bey E{T| eres pLeiarlntl] Tee 1i 3 nfant g111 {| JR IEE EiIz I Bess Hezoyg 1i] . Jes] anznzs H i Best pet 11 } Jee fsszualy Hi i {ial isl |! ie gieeal || Jegasak hbli HIETTHIE TE EEfFeod|| ne pellet | i EB prt presi 1 RE| tE gHtRIl : CEREHE ssid i feo | od fei i Jett] ferent epoe e ||| | lk ll i jseseid Le fees LE 4d 1 : i H | i ii Hl fo |i] o JDeti)lfdeet |h: i fod | iLllt1tI i sEaEEE | th il ii fJperest 1i} Jess] |]Jerse) |] Jo ol | Eio |Jrvig|] feres1 J 11d |il iol 1)! t:H] dsl] et fB {ljie RL R HH RE EI] aaeE | laa fli ETE TRE go gid | Jess] Jey 1 fod | { I lH B dtd i Eo [Jedd] Jerse by | 3 geil gaaagd Hi i ii Hi il 3 gt i id Fe | i | es | ltd | | EE no ET frm EH) pr it i i Hil| |i il it Juoisseddi |E||j] Jorssfd|Feed 1] : elf [1 le] Ii | Jers ey dLiik : !| Hgirees HTHiEi i Li! Tl ili Cp hflorol esh i 1i fied | ] | BH ITE ET i fold 1} 2 i HIETTIETEL Bail) | heciad pn {|i ii fi Jed{p| pd {le1s oor] [for|d | [Je: TTI 1 pe: d1 Sine 1 17F il |Ji [|TEE EE EO 8 ii Hf ; bili di: if | bh |G iit | giz gf LL V Dbereee hepa il p63 r-- HoCgon RL TIT Laabcoarrotcoyrayncdopnrtecikoensoaranldafneademast.iAcsryoesvweerssussauodceisconmsepitlseedaahnoaulnlgymSeMthod EnvrLaboroatornymemh edesnoieadhelrs ORS Rar 5 FERRE ET Aplolrremainingsamples andassociated projectddaattaa (har(hdardcopy copyandelect)wrilobenarichicve)d:according 5RRL ae SI FTTTRTTERA A`ttAaacctrhmmaeenncttCh::TTAeenrssatttecPPrarnolotttohtcooosltAhmoesndment . AncrmentsFema CronossanddCatronGrves re Fasestar is p.6t cower Report Approval. Sosa,> WPS.Ly 3 23/2070 iiEaS KRoagen-- ,Ph--. 3--EmvirormmertlLaboratoryMarge: J[Er 2To0e/0 ly PhD, HyTochvic Favow . " Sons Representa ; Tekin Ketan, Sud Dicer s3a lefle 2000 To 27, % Zelo Ton 0 ColEoomnaGverennfaSpoen2r200 Pre stes p.65 cowenTaL ATTACHMENT A: TesT PROTOCOL SMCord0o7n0G10r: utinntRaCgooo2.s 2000 Page00t 148 p.66 IMENVIRONMENTAL LABORATORY COWETA. {ab Raquest Number: E07-0149 ANALYTICAL STUDY PROTOCOL APnearlfylsuiosroofbuPtearnfelsuuolrfoobnuattaenc(iPcFABcSSi)td,u(PdPeyFrBfTAli)tul,oerPoehrefxlaunoersouolcftoannactiec A(PdHdS()P,FOaRn)d, PeFrlfulouroorcohoecmtiacnaels(uFfCo)naAtses(ePsFsOmSe)ntinWGorrokunPidawnaftoerrthUesi3ngMLCCo/rdMoSvIaM,SILfoFractihleit"y"3.M Data Requirement GLP AprilD1a1t,e:2007 3M EnvironmePnetraflo,rHmeianltghL,aabnodraStaofretyy Operations 33MMECnevnitreorn,meBnitdagl2L6a0b-o5rNa-t1o7ry St.Paul, MN 55144 Laboratory PEr0o7j-e0c1t4I9dentification SMCarbronoGurovvaermDnpcombes 2008 Foon as p.67 IM ENVIRONMENTAL LABORATORY COFOENTAL 5)Roguagt Number: E07-0140 Study Identification Analysis of Perfluorobutanaic ACid (PFBA), Perfluorooctanoic Acid (PFOA), PerPfelrufolruooorcotbaunteasnuetsfuolnfaotnea(tePF(OPSFB)Si)n,GPreorufnlduwoartoheerxUanseisnuglLfoCn/aMteS/(MPFSHfSo)r,thaend"3M Fluorochemical (FC) Assessment Work Plan for the 3M Cordova, IL. Facility". Test Substance `Sponsor `Sponsor Roprosentative Study Director aTchied t(ePsFtBmAa)t,erpiearlfsluaorreopoecrtfalnuooircoabcuitdanoic (pePrFfOlAo)r,opheerxfalnueosruolbfuotnaanteesu(lPfFoHnaSt)e, (aPnFdBS), perfluorooctanesulfonale (PFOS). 3M Corporation St Paul, MN 55144. Gry Hohenstein 3M Environmental Health and Safety Operations Bldg 4202-627 St.Paul, MN 55144 Phone: (651) 778-5150 Fax (651) 778-7203 gahohenstein@mmm.com Jai Kesar Weston Solutions 1400 Weston Way West Chester, PA 19380 Phone: (610) 701-3761 Fax: (610-701-7401 jkesari@westonsolutons.com Cor0n7s0G14r6aiminaRoCpoecro2on 008 Page F201a10s1o4s p68 IM ENVIRONMENTAL LABORATORY COMIOENTI |o Roguagt Number: 07.0149 PrincipalAnalytical Investigator (PAI) Susan Wolf 3M Environmental Health and Safety Operations 3M Center, Bidg. 260-05-N-17 St Paul, MN 55144 Phone: (651) 733-9851 Fax (651) 733-4687 stwolf@mmm.com Study Location(s) . Testing Facilty +. Proposed Study Timetable oy ExperimentalStertDate... Experimental Termination Date, 3OpMerEantviiornosnmental, Health, and Safety 33MM CEennvtierro,nmBelndtgal26L0a-b5oNr-a1to7ry St.Paul, MN 55144 Sample Receipt: Early Apr, 2007 May 31, 2007 NMConEt0o7s.rmmainnReSpoartb8o2 2808 PagParlo1S03ot 14s 3M ENVIRONMENTAL LABORATORY CONFIDENTIAL |31) Request Number: E07-0149 1. Stor Analysis of Perfluorobutanoic Acid (PFBA), Perfluorooctanoic Acid (PFOA), Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Groundwater Using LC/MS/MS for the "3M Fluorochemical (FC) Assessment Work Planforthe 3M Cordova, IL Facility". 2. PURPOSE The purpose of this study Is to analyze groundwater samples from seventeen monitoring wells and five production wells from the 3M Cordova facility, for perfluorobutanoic acid (PFBA), perfluorooctanoic acid (PFOA), (PFBS), perfluorchexariesulfonate (PFHS), and perfluorooctanesulfonate (PFOS). The samples `will be prepared and analyzed using the current version 3M Environmental Laboratory analytical method ETS-8-154: "Determination of Perfluorinated Acids, Alcohols, Amides, aChnrdoSmualtfoognartaepshyIn/MWaastserSpBeyctSroolmiedtPryh"a.seTEhxetrtaacrtgieotnedanlidmiHtiogfhquPaenrtfiotartmiaonncweilLibqeuid 0.025ng/mL (ppb) for all compounds of interest. 3. REGULATORY COMPLIANCE The analytical portion will be conducted in accordance with the United States Environmental Protection Agency Good Laboratory Practice Regulations for Non-clinical Laboratory Studies, 40 CFR 792. 4. QUALITYASSURANCE "The 3M Environmental Laboratory Quality Assurance Unit will audit the study conduct, raw data, and final reportto determine compliance with Good Laboratory Practice Regulations, this protocol, and 3M Environmental Laboratory Standard Operating Procedures. IE 5. TEST SUBSTANCES TS NSSS [ownctrom | = cr=co |e Torrwl oeo |" orsoi | weelarnsvin gunz Poo bias p.70 IMENVIRONMENTAL LABORATORY "ENA gb Roquost Number: E070149 [morons | oor | rio] [[rossubsmnce[pe T w ross| ||Cromeca Namo|Portuooheranssutonst |Fetumroocian sonst | sSuabmsptlaenscef,oratthainsystpuadrytiacurlear"rreaatle.worTlhde"resfaomrpsleosn,lyntohtedaonsaleydtiwciatlhpahsapseeciofficthfost sotfutdeystwil be performed under the GLP standards. kTnhoewtnestsosuurbcset,aenxcpeisraftoirotnhidsaslet,udsytoarraegenoc!ontdeisttiosnusb,stcahnecmeiscailn ltohtenculmabsesric,sTeCnsRe.nuTmhbeer, tpehsytsiscyasltdeemscarrisptniootn,kannodwnpuarsitythoefywthoeutlesdtbseu,bksntoawnncefsortthahte arreefebreeinncge msounbisttoarnecdesi.n the MCroCosroGn rownm pBeonca2 208 P08 eBanes TET 33 lil! I . Ji Tl SEITE: 3 1.83 1s) |g it ; | Ji i i if Ci il kifil Hel nei pie LJ p.72 IMENVIRONMENTAL LABORATORY COWONMAL |gbRaquastNumber: 07-0149 7. TesrSvsrew STehcettieosntssy4s0tCeFmRis7g9r2o.u1n2d0wa(t6)e,r(.9).Ad(d1i0t)ioannadl (s1o1u)rcarees nmoatyapbpeliacdadbleedaassornelqytuehsetaenda.lytical phaseofthis study is under the Good Laboratory Practices. 3`TMheCtoersdtosvyas,telimnsowlserfeaccithyo,seanndtoaraeccdeesfsintehdeinitmhpeacwtoorfkthpiearn.efeTrheencseasmupblsetsawniclesbein the wciollllbecetepdrebpyarWeedstboynthSeoltuetsitoinngs faanciditsyh.ipped to the testing facilly. The conlrol samples lPraiboorrattoocryolslaecmipolne, reeafcehresnacmepnluembboetrtl.e sTehnits (r0eftehreetnecsetinnugmlboecartiwoilnlwbilel ubneiqidueentainfidedwiwlilth a dCihsrtoimngautiosghreaapchhicladbaotraatwoirlybseaimdpelnteiftiheadt bisy ctahrerileadbotrhartoourgyhstahmepalnealryetfiecarlenpcreocneudmubreer.. 8. Specimen RecerT , pTrhoedugcrtoiuonndwwealtlesrfsraommptlhees3wMillCboerdcoovllaecfatceiditfyr.omWasteevrenstaemepnlemosnwiitlolrbiengcwoelllelcstaedndbfyive wWiellstboenkeSpotlurteifornisgepreartesdonante2lCa-nd8sChifprpoemd tthoetthiem3e MofEsnavmiprloenmreencteailptLuanbti.lonanaicley. siSsamples 9. EXPERIMENTALDESIGN ! `Sam9p.1lesPwrielpbareaptroerpyaarneddAnaanldyatniaclaylzeMdeuishiongdETS-8-154: "Determination of PExetrrfalcutoiroinnaatnedd AHciigdhs,PAelrcfoohromlsa,ncAemiLdiequsi,daCnhdiSoumlaftoongartaepshIyn/WMaalsesrSBpeyctSorloimdetPrhya".se mExattrcahceteddwcaatleirb)rattoiobnesdteatnedramridnsewdilallboengprweipthartehde QinCa ssaimmipllaersm.atrix (Mill Q or matrix fASiloellmcdoednutspailitiencseartmseauaysnehddaavfteoreaawdsadtittetirwonosaallmefpvleleledscsoopflilfkeeeclstiditosonpibwkriaelcsbkoeefttsehhaiecphppeosdsasmtipobllteehecwioslnlacmbepenltcreoalltloiecocantteido.n. A PraFnHgSesaonfdanPaFlOytSe.s Tinhae lfoiecladtisopni.keTshweilfllbeedusspeidketsowdieltceornmtianien tPhFeBApr,ecPiFsiOoAn,anPdFSac,curacy noofttbheemaectohmodpofnoernetaocfhthsiitse sstaumdpylebdu.t,iLfanbeocreastsoarryy,spciaknesbaenddolnaebowriatthorayppdruoplviaclatoers byw.ill request of the study director. tRheecofvoretriifieesdolfovfeilesl.d mIafttrhiexrsepciokveesri(eFsMoSf)tahreefiaenltdiscippiakteesdf1a0lboeutbseidtewetehen a7c0c%epatanbdle13ra0n%geo,f the sample result will be reported as "NR" (not reported duetoQC failures). aMCarCoonnoGrronceerCnncom8b2er 208 Pore ars p73 IMENVIRONMENTAL LABORATORY SONOBNTAL obRoguagt Number: 07.0140 . tFroirpleicaactehleaxbtrcaocnttiroonl bsaptickehsatalteaasmtitnhirmeeummoeftthwood bdilfafnekresnwtilclonbceenptrreaptairoends.arIentaodibleion, performed with each extraction batch. 9.2 Methodsfor ControlofBias. mCoentthroodl aocfcubiraascyisanadccpormepclisiisohne)danudsinbglanlkasb.oraLtaobroyractoonrtryolcon:tsraomlplseasmp(laessiandriecautsoerds of to dwieltlebreminuesetdhetooveprraelpladraetathuenclearboarianttoyryfocroentarcohl bsaatmcphl.esM.iliTQripolricmataetrliaxbmoraattcohryedcownattreorl esxatmrpalcteisonatbaatchm.inTihmeumreolfatitvweosdtiafnfdearerndtdceovnicaetnitornoatfitohnes aproeolteodbreecpoevrerfioersmemduswtitbheelaecshs tsphiaknesorwiellqubaelptroep2a0re%daatncdontoheenairvaetriaognes raepcporvoexriymamtueslytfbivee 8to0-t1en20t%i.mesLhoiwghelrabthcaonnttrhoel targeted LOQ and high laboratory control the mid-point of the calibration curve. spikes will be prepared at concentrations near MFeortheoadchblaananlkystimcuasltbbaetcdhoonfesawmitphleesa,chsoelxvternatctainodn mbaettchho.dAblraannkgsewoilfltbe hantaolesyezveede.n amneatlhyozdedbltahnrkosugmhoutu btehpersaenpalayt rteidcalinsteeqrusepnecrsee.dTthheromueghaonutatrheeaecxotruancttifoorn ebaactchhaananldyte in tmheeamneatrheoad cboluanntkssomfutshte bmeetlhesosdtbhlaannk5s0e%xcoefetdhe5a0r%eaofctouhnetoLfOtQhestLaOndQarsdt,antdhaernd.theIfthe ALlOteQrnmatuisvetlby,etrhaeismeedtthootdheblfarnsktsstcaounlddarbdeleevvealluinattehde sctuartvisetitchaaltlymteoedtestcerrimteirniea.outers or Ttehcehncirciatlerjiuasaiirfeictahteionnatpopelliiemdianagtaeina(b0leavnaklmuaatye bmeetmhaoddebwlahnekncdoemtpeliramnicnei.ng ItfhaenLyOmQe.thod abslaanpkpsroaprreiartee.moved from the LOQ determination, document in the reportorthe raw data 10. DaTA QUALITY OBuECTIVES aMcectohroddanpceerwfiotrhmaEnTcS-e8-c1r5it4e,riaThweilalppbreoprdieamteonlsatbroaratteodry fcoorntreoalchsamapnalleystipcralepabraeidchwitihn emeatchhods'est porfecsiasmiopnleIsswisthhoiunld2v0er%ifryeltahteivemsettahnodda'rsd adcevciuartaicony. is 100% + 20%, and the 11. StasmicaL ANALYSIS `pArvoevriadgeedsinanEdTSs-t8a-n4d3a.rd deviations wil be calculated. Additional calculations are 12. Report A`Threeproerptoorfttwhilel irnecsluuldtes,obfutthenosttubdeylwiimlitbedetpo,retphaerfeodllboywi3ngM, wEnhveinroanpmpelinctaablleL:aboratory. 12.1 Name and addroefsthse faciity performing the study. SM CarEo0n7G01rran ogGooca2mon 008 Pogo Pgorle1s0ton 7s IMENVIRONMENTAL LABORATORY "DENTAL Lab RouastNumber: 07-0149 1122..23 DAatsestupaontowhficecohmmptlhieeasntncuedbtyywatsheiSntautdyedDairnedctcoormapdlderteesds.ing any exceptions 12.4 tOobjGeoctoidveLsabaonrdatporroycPerdaucrteisceasStsatnadtaerddisn.the approved protocol, including any 12.5 aTohmdeeentdensmutemsbnuetbrss,ttsaotntrcheenegiotdrhei,ngtipinfuairlctapytr,iooatnoncbdoylc.noampmoes,itcihoenmiocraoltahbesriarpapcrtospnriuamtbeeror 1+2.6 cSahdtamaribanlciitstetyrriaastntidiocnts,,heifspproroolvvuiidbdeeiddoblfybitytthiehyneeteSSspptoonsnsusoborsr.t.ances under the conditioonfs 111222...978 AAAdddeeessscccrrriiippptttiiiooonnnooofffattnhhayectimerescttsuhmoydsssttauensmce.eds.tt.hoact+onmdauychtahveeteasfif(esc)t.ed thequaityorthe: ~ 12.10 iTpnrhtoeefgernsisatiymooenfoatlfhst,ehadeantdSat.suudpyerDviirseocrt+yor+paenrdsotnhneelnainmveoslovfedotinhethressctieundtyi.sts,. 12.11 Athdeedsactrai,ptaiosnuomfmtahreytraanndsfaornmataiolnsy;tschaelicaunslaal:tyitooincsfa,locrhoepmeirsattriyondsatpae,arfnodrmaed on 12.12 sStattiastticealmomefetnthhteodcsonucsleudstioonesvadlruaswtneftohematthae,anifaalpypsieisc.able. 1213 12.14 TpTrhhoeefeslsoiscgianotenidaolnaswnihdnevdroaeltrveeaddwridenpa'ottrhetasso:tfuaedtynah,cdefhfoaipnfpaltirhceeapboilnred.tiavrieduatto scientistsoother be stored. 12.15 AsretpusodtryattieendmsetpnoetctthpieroenSpstauardneyddbaDyuirdteichttesorwQeuaarnleditmyMaaadnseasaguernmadenncteth.eundiattleissotifnag nthyefdiantdeisngtshat 12.16 biIfseisetuniesdnacbecyceeptsthseeadrS,ytuttdhoeymDacihkraeecntcgooerr.sreTcwhitleilonabsmeeornmdaadmddeeinttiionnwsitlhteoclfaeoafrrilmnyaloifrdeepanotnrityaamtfheteenrdpatmrethansot.f twihlel bfienaslirgenpeodrtbythtahteISstbuediyngDiaremcetnorded, the reasons for the amendment, and Of1ar3ci.iglitnLaaOtleCdAaaTutdIaiOtoNsrOofcFoRtphaieewssDttAuhTderyAe,dofu,RriEwnCigOlRibsDepSr,aovAgatirFileIasbNsleaAnaLtd3RbEMePfEOonrRveTiarcocnempetntaanlceLaobfotrhaetofirnyalto rliesptoerdt.bWelhoewnwitllhebefinraeltraeipnoerdtiInstchoemppleertmeadn,enaltl orreicgoirndalapracphievredsatoaf,3IMncEinuvdiinrgontmheonstealtems Laboratory folowing signing of the report 13.1 Tarhcehifvoellsoawcicngorrdaiwngdattoa3aMndEnrveicroorndmsenwtialllbLearbeotraaitnoerdyinSttahnedsatruddyOpfeorladterinignthe 1133P..r11o..c12eduASrtpeupsdr.yovceodrmpersotpoocnodlenacned amendments 1133..11..34 13.1.5 SARhpaipwprpodivanetgadrfeicnoalrdrseport (orginal signed copy) CoebrosoGsovwn genr6o2 r200 Pose artes p75 IMENVIRONMENTAL LABORATORY SONOMA oocyst Number: 07.0149 13.1.6 Electronic copiesofdata 13.2 fTohledefroilnlotwhiengarscuhpipvoerstiancgcorredcionrgdsfowil3lbeMrEentvaiironnemdensteaplaLraabeolryatforroymStthaensdtaurddy 13O:p2e1ratiTnrgaiPnrinogcerdeucroersd:s ' 1133.2232 CIanlsitbrruamteinotnmraeicnotrednsancelogs 13.24 13.25 SAptparnodparridatOepesrpaetciinmgePnrsocedures, Equipment Procedures, and Methods 14.DATA/ SaNPLE RETENTION A portionofthetest substance used inthis study will be retained foar period not less trehtaanin1e0d5ye0arosnfgolalsowtihneglrthqeuaalpipyliacfaftoirodnsoefvatlhueaftiinoanl.test rule. The extracts will only be 15.PROTOCOL AMENDMENTS AND DEVIATIONS Planned changes to the protocol will b in the form of written amendments signed by tahsepSarttuodfytDhierepcrtootroaconldatnhde Swiplolnbseoart'tsacRheepdrestetnhteatifvinea.l Aprmoetoncdoml,enAtnsywoiltlhebrecchoannsigdeesred f(luendplwaintnhetdh)erwiallwbdaetian.thAellfocrhmaonfgwersitttoetnhedepxrioaltoicoonls,asnidgtnheed rbeyatshoenSftorudtyheDicrheacntogresanwdill ba indicated n the final report. 16. SioNATURES %A i Jai Kesan, Study Director 4 77 Date GaryA. Hohenstein, Sponsor Representative Date Zz -- Silos illam K, Reagan, 3M Environmental Laboratory Management Date CoocsorGnsr:moanmoGpiennn2ie2009 Poe 102Bares p.76 SMENVIRONMENTAL LABORATORY cone Lab Request Number: E070149 13.1.6 Electronic copies of data 13.2 TfholedfeorlIlntowhienagrcshupipvoerstaicncgorredcionrgdstowi3lMbeErnevtiarionnmeednsteaplarLaatbeolryatforroymStthaensdtaurddy 13O.pe2r1atiTnragiPnrinogcerdeucroersd:s 1133.22.32 ICanlsitbrruamteinotn mraeicnortdesnance logs. 1133..2245 ASptparnodparridatOepesrpaetciinmgePnrsocedures, Equipment Procedures, and Methods 14.DaTA/SAWPLE RETENTION Athpaonrt1i0oyneoafrtshfeoflelsotwsiungbtshteanacppeluiscaetdioinnUofYthsetfuidnyawtielsbtreurlee.taTinheedefoxr atperrwiiaoldlconnolttylbesses retained so long as their quaity affords evaluation. 15.PROTOCOL AMENDMENATNSD DEVIATIONS: PlthaenSnteuddcyhDainregcetsortoatnhdetphreoStpoocnolsowirl'lsbReepirn etsheenftoartmivoef.wrAimtetnednammeenntdsmweilnltbsesciognnseiddbeyred 2(5upnpalratnonfetdh)ewpilrobteocionltahnedfowrimlobfewatrtiatcehneddeviatthieofnisn,asipgrnoetodcboyl.tAhenSytoutdhyeDricrheacntogreasnd flbeedIwniditchatthederian wthdeatfian.alArlelpocrhta.ngestotheprotocolandthereasonforthechanges wil 16.SicHATURES JaiKesa,Study Director Gary AfHoh4enstein, Sponsor Representative: Dawe 17, 200 Date Willam K. Reagen, 3M Environmental Laboratory Management Date CaiEo07G0 oomm iagCoearrb2ar 200 Page 100110 Pasa Tot145 p77 conneNTAL "ATTACHMENT B: TEST PROTOCOL AMENDMENT 2MCoEr0s7o.n0G14r5ootmmerBgoocromb2er 200 Page T2ot us conan p78 IM Prot"ocAomleEn0d7:m0e1#n42t9 Study Title PerfuoroAoncPatelarynuseiassuroloofbnPuaataenef(sFuuOfoSor)naolenb(rPuFoAsBtucSa)nm,(ndPPeceeFrriAfUnu)cso,irntoPgheoLxafnooCsurlooSnfaoolsctA(htPeGFSaH(SMP)nF,FOcnuAc)icr,achemical FC)AsseWsorkPlanforthe SM Cordova IL. Facil PROTOCOL AMENDMENT NO. 2 NAomveenmdbmeern1t9,D2a0te0:8 3M Enviro3nmMePneEtnravflio,rroHmneiamnlegtnhtL,aalabnoLdarbaSotarofaerttyoyryOperations MapleBwuioloddi,ngM2N60-555N1-4147-1000 Laboratory PEr0o7j-e0c1t4I9dentification - Coron, amann12r PoPeaaaTor 145 p.79 conroeNTAL 3MProt"oAcmoelnEd0m7e-n0t1#429 `This amendment modifiesthefollowing portion of protocol: APnearlyfsuiosroobfuPtearnsfsuuofronoablust(aPnFABodSi)c, (PPeFrBfAu)c,roPheerxlaunoersouolcitoannactisc (APFcHS()P.FOaAn)d. Perfuoroocianes(uFtfCo)nAate (sPFOsS) iWneoGrroksuPnidawsnatfoermtUhseien3gMCLnoCrMdSotIvaM,SIfLorFatchieit"y3"M Fluorochemical PROTOCOL READS: 6. REFERENGE SUBSTANCE [Cromoncesipsmnce Teron | pron | eres) |coamicaitame |PerhuorobiancicAd|Perroccanox Ac |Putucrobvinendonss_| [CoemesiFomus | eFo00 TT Grated |ocarsn at | cass 2020493 [saw 1 mw [ow |ow | [SomertonTomei| wen|owes | [StageCondtors | Frozen | Pwr|Fown | [orementotNumbee[owrrsee| se | 2 | [CT eRWemos [7 wera | vemm | tones | |PyvcuOmran| vi omy| Whepowder |Goodiecys__| I J EY.SU SCS [sow | Wommeionwlete| saw |save | [RowncosubmanceTesTwos] [ChomciNeme |Pecuoronemaneeutorats| Peuorocumeslonse | [Cwmesifomia| orSe |GRsor | Sam 7Tw [ Eommnome 1 enamine| [ SoogeCo TTnsFtewons| |Chomattottumbor| Ngraooeres | [ ToRMebw TTvoRoss | tore | |PoicuOmergion 1 Wego | Vitepowier | [py7 Twos [ew soma owomut|navesoinete| eSi" PagPe2olsdoet4d8 p80 conpama IMProt"oAcmoleEn0d7:m0e1n41t29 AMETO RNEADD: 6. REFERENCESUBSTANCE [G[rRoofmorkwenciaNSuabsmtaence| | _Po_rf_uorroobuaan| skAcu|b_Pesrtuou prorodoniaan"iccAced_|Peorobuwisenesssi_ion_at_e|] [_c[roRmieceifNae me r||Poen rtcuproiars shex||aPneretusropunctarnoesonufsosntst]e| S(11)4Twos0fcaonrdccoentsauibnisntganrcaesncwhsebdeHuosmeedrfsx. PFOAandPFOS,00 containsmarty neesomes, uTRomEbaAleSlOrowoNf:torhtrhhulstehoofsreesftearteendceisutbhsepiraontooscotlh.atmaybedenied by TCR number oot PROTOCOL READS: `S9Aa.dm1d.pslP,ersapwcaorhhaotbloor,yArmainoddssApn,aaalanyndtdiSracunallafelomyniazdtteehdsoudsininWgaEtTerSB.8y-S1a54i;d"PDhaalseermEixtnraatcitnioofn PaonrdfuHoirgihnaiod PerformanceLiquidChromatographyMassSpectrometry". 9A.4.PMrETOeNREpADDaa:ndrAnaalytticoalmrethyod `oS2fa0mPpaHlfieogshrwniPaleltrbeoedrpArmceacpnsac,reLAdilqcauonihddoCalhnsr,aoAlmycazeleosdbg,ryaapLnhCdy//MSMuSlaIfsMosSnSafptoeelscloinwrioWngmaEelteTySB"8y-S1o5l4.d3PhDaetseerErnxirneatcitoonn Atormately, samplosmybeanayiedby ETS-8:044.0 `Detarmicatonof Perorinated PC`eorGmfpouoorujnneacdltsisodnnCaAontmapleyosubinysdHosfgIEnTWa Sa.le0r-,1S10i.`1aMnedtSheoddioCmfelAnntabyysLsCfIoMrStIheMSD'e.termeinnaotiroonf! RMeo ElAhSon OdNE:Tc S-8-ra1en5g4eifsnotympici0a.l0ly2u5rsaegdiaftr1s.:eo 2m5pnlinsnta.tcPontarinpaeenraulvoyrnaitofedgocrooumunpdowuasntedrs ithe V`maSoerayrimihspnolgredcssofEnorTcoeSmns-ttht5rhaa.entCt12io0o5ranednsno.gdviramEaTLSr.-oT8.h0e(4rn46e,arwshoincrehfoporrtehib#e1aa)mprarnodduumlceeendtsfoasmt{hp0ealalenorawelsyusolirsstohotf useavsmeolplofetsaotf SM CorctoonrG o reo nrCioan ne2008 Pda p61 i7io! ot Gary Hon7enslan, Spjojnsor cooerma Amendment Approval Repramaine IMProt"oAcomleE0n7d-m0e1#n42t9 l2z,44 Doi0 C ior lg `SusanWolf,Principal sigator [19/2009 Date Wikp a Regez n,EF--SOpsEnvironabmMeannagtemaenlt [EF ned2Oa0ts98 Tw DEE. StudyDrocior Toe Corton Go Soon 800 Pagodars Fheicae p.82 conFoENTIAL ATTACHMENT C: EXTRACTION AND ANALYTICAL METHODS 0Cors0o7n.0G14r%ommiintReSpooco2er 2000 pagoeters p.63 Dossiecropmambeaeuysed if current. on 14days from 022372010 - 3M Environmental Laboratory mea Analysis of Fluorochemicals in Extracts Using HPLC-ElectrosprayMass Spectrometry/Mass Spectrometry Method Number: ETS-8-110.01 Adoption Date: 08 Sept 1999 Revision Date: Upon signing Eftoctive Date: [0/13fey Approved: WienKHEResgon Manager Toe osdef Ansyss of FluorpochramEiiTcSanl8s1tn10Eex0t1rrac)ts sing LCMSMS. CornsSoman Sob 200 Page 1ct10 Pree Thorsis p84 CosecolnpmenTBiLe esed rant foi 14doys fore 02032010 1_Scopeand Application Tahnedmsieftohnoatdedse)sucsriibnegstHPhLaCa-nTalmyassisssofpoorcockheomimcalest(syypiecncaklaoympseetrsyfu.cronated acs,soto, mies, WS`oSarpnkedcshoearen)t,y)san,doones(ppaerresnmteaenrdsdwoi ubgehode)fmniaetidcis,hseolvreorsc,csootuhessa,mqpulaletyocpeornatsi,on mel AMSgeparttucmoa.st:TlheTeCooimmnopctouudnew,dlsb:btaBndeoectftiomnsepddrbayy k05,nazbosbrol,leaSoacroecshsaemmsipccloaelnpsrs.e,poerrgaatnnwosraksvheerest,ss)o.ls,sues, nd 2 Method Summary " -'" -- . {npidsmaeetmeharoesdsdcesbscarpirbeeosnohce(Pao(rFaHrOPoSacL)iaCmnEoiaofSaonMfd,StwnevMozcSy=to)o49yT9shooeBrzpfaesrnouocaxfualaionscipyiraarssaneooorsinmtes(5dPbFyouOA)g,fm HoPlL=Cl4z hdw1e mi3eaAnscgsoy Cporomdpuocutondns6peqcuianprtoadulctmoonntiocrreesdt.ed Trough ghenergycolisons, ndtheCreston fhe FTo5e1rc1henx0iaq(mucpehlraeer,dctuthcressribacanocfikCognrFo)urnomdrna4ni9se9ir>5ein9scm(ecashreairnaodcrteeenrdhisfatonirccPeoFsfOFaASn.OaT.lh)cisassmlseoenlndesrciehtdyfa.fooPrFdeOdSbaytnidsthe 13 3 Definitions 3.1 Atmospheric Pressure lonization (API): CIioonzmimizeantrgiconiva(lEtS)ya,vAaotifmstsoisooprLhceeCrsMi,cSpPrronebesdse,uLarnCsdcMhSemMriaSccasleylssat.reiTmzhasteiasolne(oiAwnPcfGlo)uvd.aeTrbihuoteusroemectnhtadszoenfdhnea0is:zeaEpteritcoorcneobssnyspersa.y `occursststmosphri pressure(.0.,NoneavacuwT). 3.2 Electrospray lonization (ES, ES): eAhlemcgetatihcsaopldhfoaefsler.viiTzyaptinocynacplh,earsrogresmddefrdooapritehstemsao.nTsahlpyehssieesrodfTpofrupeoserstoucrahee,mwpihrceoalrdseu.bcyedobnys ihesaopupoicnaatoon oafnasfreoendgto 3.3 Mass Spectrometer (MS) or Tandem Mass Spectrometer (MS/MS): `qSnindgslueumbsaaespcsmlesdaonpsyetsecyustddeoelmecptecbtteiissvcoei(.dsMetpSAle)ecstiocoergrhlTso.ainMocdSnefmsmaoamgyoabmsselseeesnmcppoiiolmvcaoaerytytmeGoeodetnncoo.rrrmosi(nnaVdtSeoMdtSebc)ytsmnyasotsretsmastnodacerhmareMgqSeui(apSpoeA(dSmwz)i)h maybeem 4 Warnings and Cautions 4.1 HeaanldSatfehty A2wDaryrOsPwseeaGroapipnrogprwiahteepwoosrokninaglpfrohloBctivIeeHqpmMaOtritcess,iScvhe33np, cShemicGalOsVE, ye Analysisof3FlCuoaroEoc5sh7EeGTTmeri5cso6arln-ea1ei1rnn0Ee0xOto1rnancct:os Urs2in0g5LCIMSMS olen,and Pege201l0 PagnToct es p85 Documcenotnmsayebre used. i curnent, for 14aye hom 02005.20%0 Pmaraancdttencss,isuomireorcIthaetEonnnv.irFooonrmrpeonltmeaalnsatLaaapbtophrarazotoaoprrrdyni's.Chmeamtiocna fHarzatrodmRaetveiceawls,ahloty3MdaGtuasihdeeteLapbaocrkaitnogry 42 Cautions "mnTheee,adnitahi,svhtoemlLtuasgete,ofafincdavoagcacawlimasytthseetrelmiasv,aoRtvoerenyse1,quthihphmaelnamtpapenrdspptoulrreen,tproamehesanzuptarrzpdrarsodcceaildsuirnaeangod,rsbatuoptlaneeronttt mana for acdiona infomation and cations. 5_ Interferences Tcomionimnizeanhteemsraemriepnec(enssw)haoeexntescnsosz)ingsamples, usacarinersandntuamentspasthatwlxt CsopeaxcrraocmteetdrmTahtessceomeposnenatrosmmaiynenehdarucsniongrasnuSpPprEefsethcemheaa,sburdeidhaenpdreycissiionnaandi tshcaemnacsysof 3pproserrte.sus usbe vatedfoposseafcof o-ercied a irrenceshetmybo _ Instrumentation, Supplies, and Materials 6.1 Instrumentation EcqounptmuresnttoinsnetdhbeoroawwGmtaaybanedmind2eAnianlaydteer EpqiupcmosntShyesstyesmtseGmo.cDumearctauttnmhoeatnchtlr `equivalentdocumentation sys. AgHlPLC1o100nsysttem: Peumqp: nQuatemaryPump, Aglont,Model 613114 orBinaryPurp,AQlantDModel 1312 or StventDogassrAglot,ModelG1322A orequivalent Auftorsoammpaes,Agiont,Model 13134,orTemostatedAutosample,Aghen,Model G1320Aor Ascoidseanmtp.ethemosta usedwthheThermestaledAutosamper,Aglent,ModelG1330A ConCompartment Tamporat.reConroe,Agent,ModelG1316Aorequivalent. DiodeAayDetect,(DAD)Agent,Model #G1318A oequivalent. `Controle, HandHol,Aglont,Model# G1323A oeutalent. Uma, TandemMS,iramaosrQsuatr,o,TandemMS,Mcromoarsqsuvsle,rt CaptaryPump,Waters,Model CAPLC,o equivalent Capt Autosamplr,SparkHotan,Model SPF,orequivalent. CamperHard Drive,Campa AP200 abeter, orequivalent. `Systemcontaonallyscissaottwaar: MasVesrsioLn3.4yorbmet,corsqTMuale,nt. Omer instrasunemodeed, dnoctumeantataipproopinate AnalysisofFiBsEPoTssr8r 1g1Ine0E0xahn g1acetmUsiingcLOaMSlIsMS SUCorson GoraGovmbae1e000 Page301t0 Pretaorres p86 aumeciommapyabe Use f EUITL 14 day fren IAIN 6.2 Supplies, ! FeTrubmiinge:sPaEnEdKo,tshtearicnloesnsnsteeecl,tpeaitrcvt.se. Autoavnid clapss. 6.3 Materials Highpuritygradenitrogen gasregulatedtoapproximately100psi (orothersuitablegassystem). Highpurity gradecollisiongas,argon. HPLC analyticalcolumns. Cimpers 7 Reagents andStandards. M 7.1 eReatgHePnhLtCsa .gradn e.oo requilval, ent. ut `AndSecTqmMuaaTytyebpdaeocpur| moWevaniltdraetdoibrocynauoMflhQees.ouTrAOclGe.wPautesrSuyssedtoimo5rbym.nofthihodeshyosuldebmsoASveTndToy,ppero|viodeeqdutivearlenits, AamdmiotniscucmorAdcentgalt.e;reagent grade oevant Whenpreparingferentauntshan hosestd, Vt2o.lo0ummmmoalrAL.aaskm .Admdwoaacteneta1tietshou elmuatm riokna.Wnediighxarpparolxismaotlelsya0.3s00egosfa.mmoinoriumaoceotmat.e tc 8 21. OtWohroksheveto)n.tDaarcdimsoaknttoansSm0ahyenbtesuasneddSaOLtOalNeUs1etdhepr0o0taopproo 1 helsoagmspolfe eprdeap.aration 7.2 Calibration Standards Typical, aminimumof8standendsre zedWohrcachgoupofsamples. 8 SampleHandling aid hi C`Satranfdoargdes,hsiaem,polfeoexetrracstas,baindpcroonpianraordssa1mplnesymsaeybosored icappedautos,capped 15mL IfvSanatpaysi oplinlob4creeaCdsulenoetyty-ec,hvoaessatenaabnmdladyasrkd,esac;vasdnatbwmeippbleesrarm0y0serd,s.saeArdppnprrotoppaaPlrreodscsaaommplploleresbstyo1araygabenocaroyfnsfdgtioionrntesewdiwatbe dataandor propworksheets. ? 9 QualityControl `PTrhnoeictfeyodlcuowrioensgunqsiunealttdihtiyosrrmc1eonotthrosolda.ismFrpoer,cnooamrnmyeQGnLudPeasdykfoPirreotscheiwsdmiuetrteoshuotddPo.rooctIfreacbnodaoerprnppkrr oetopco eolcoev rdeexnte crsacotd vioenr he ren EIST) Ae oFCorb Gia ragarisenr25600 Page dot 10 Pann oties p.67 Cogacnomeeg be sn unent for 16 dave fiom QUGE0%G `hexetrancatliornompetehtods, documentthechosen qualitycontrolonthesamplepreperationworksheetsandof 9.1 Blanks 94.1 SolventBlank Scolovennttbalmnkisonrcaeantmoyitoveoxetrnr.acTthede.sTahveeyaurseeadnssyhzsadwinshocmocoaspapmrpossaetoondreeptraeisennst `s7ch0veknt5us1e0d9forhhoes5t0a%ndoafrhdaarveo aconrokohf hsskanmwp sacacbsr.aonSsaacarlr,kv8708eccns `S5oo0nl%sveeoncftubvlaensrkooslsvheconoutulbdnabonefktasonmaalvyyezbesedtpnrceiaocreltsasotaeoraync.hscStaoallnivbcerenattipborniacourroverb.eaIcfocuencatosnmsohyfiosuokadnbpvorfoweebnslrsemthan samples. 942 MethodBlank Maentcthhoedrcbaormkmsearridxytacvtaelaeasnodvaenrldy.zsdwin achgroupofsamples, consistingcfwero TlhaerparostohcooldonejeescteesacouwnitldesfisnePthsu5m0b%eorahcrocaueunnctyooffthhesloswseasmtpclaelsb.raMoenthod Sarr 94.3 MatrixBlank Miantcrliuxdeblaonekssaarreexsterraacstaemdpalensd.anEanlcyzoegdnwiotuhseeavchegsroofutpaorgfestaamnpalbeiso.sTchoersaeingerdouipnshwoould `saomupglehmhatorinxatroeeevxavlaucaitaendbpyrtoackeisnsgoanngaleiiqueotthofsbiaanmk e(u.nexposed)matrixandcamying it D`aaThnnedkparsrost.hocooulodirheprvojoeackrteplaecoaoduswnistlsedeefcsiaen0e0tashwnehno5ur0me%bohefreanadrrfoerdeaeqcluoceuinractyblfoefhtevhesssweeosfsamtnpcclaeobsgr.aeMonantcrsix tharognet avnaalyite pressaemnptiinotdhaeamaatnridxG, tshuesn etheedendthogeonwoudostlaev.els shoud be taken into account 9.2 Surrogate Asuogatesandardmaybe sedforquatycone.Th suogatfs sedto qualtathely ovakite stGhpetkernattairotenahnaaalnbyoetigciarlipnrgoocefduaresianmclpuldeinpgospaamrpalteopnrsepnarsahtoiuokndanadlaWnailyisish.eTohews1ur0ro-ga3teshouolfd hbee 9.3 Post-Extraction Control Sample P{soastrtyga)xotaaanncaitaoennatcoytoznhetdotloasdlaeemtpxolameicsntmgaaxnyrdbaaecfpherorenapsnayraeydfoo.rnTgahchssaansoieesxaactperdespaamrepdlbey ascpeplacadbseioonse Poasstseoxraciwoinncon0traonls0aYm3p4leTchuepscsastaemspmeasyshbeopurdabasre3d0p0riciicantyhtsoammeessu8rsthopLrecpikeend oPGorosntsceehxnatiiaracbttooonpnsrscoohpnatorredodlso1anm5p-l5heecmoeonwcsaannhtegaatenooinfossghaaonunckuislfccllobinnrchaaetnoanoonv3ofnegeoeafnxtaayhtmons.koSwPcaOlebvcealtornaive veces Anatysis of FuBoEoTrss8ar-a1c1nE0xh0tar1gacaet0s.Umsiing LcOMaSMlS MoronGorovear Semebn1900 Pagos1a0 Pazva 1es p88 ocucmoennnaetyb.e sed, current, for 14 days fiom 6210372070 10 Calibration and Standardization 104 InstrumentCalibration ArenMgaryesozssitonshe(so=otramndhxLaer+rdscy)uuorirvarebUslpsBociftwracTMrof6.a(cyTh=h6seec0aotfsrbaaxtmo+en0nc,.uwreTvihegeshmstteadayn1dxnac0rhrduudUenvbweuotigsatheyodbu,edUpnogttbee fboyrcneedar cronosuigstha2nt0yh.oTuhgehmoauthtemastticya.AmeytchhoadnsgedshfoocudobleTtrohuagahbrdocumceurrdveedsihnhoedrboowsGptia.ed eiwhestcaanfctiraartdounrcuerve(fdnoecsesnsoatrym)eaentd8ceoa0npataynzcsa"crapor ounmarkenance orproper 8 Faeopnprdrpoouxritpmhoastceelasyboa1ft0apcocnburcoaufcryvnwearhatetenh,earugteananeinraatihne g8uolcawrtalnaegvteeol.snEcouravnxeaconsWaihsteminanmgysobtfietpenhneecpsettlsagsnoadraqeyradfsonfut:osaemsthpe lbow 1 t1b0a0ptpbatthneetahranrotghesusilornawnegiegohftitnhgeoGfriegh (co9n0ce1nt0ra1t0i0o0npsptba)n.daTrhdsi.wlrch nacsecy LHrioagwnhglaeeanvpdpeorcrouplrroviweappteiittostshsmhacaoytubadeoarlxsbocebhcdeaueesdxecruhosemeydthedfcnahoellibrmrearteeotantcchouerupvressoretoelpneronoivtinadeeodaaabctectweeiprtcaoftnhocaverereofrhiehaef.ner moeetd hodbland ks.Anayd cwurvteep.oatsmaaybienreojrecctedcnue10cabard tfecticoniovfpaoproesiwbllep0reip eorcan Aomwinimum of 8pont wilbeused i consethe cabratoncrv. 102 Intornal Standard IL beintnitwenerteesontmaThlhesetIraaSnodsaohrofduak(nd5b)ameisaopyfiobksoepdosantesaadnia1mSqououaprnpohshateewaitlanrdgleltakwnnioanwenthsceobnymciocnrttaaantsgotenioonfgftheaocalantaarlraytsoonf curve. TheISshoukdboaddedsie he xractonproses andbeforeanalysis 103 ContinuingCalibration Verification (CCV) cGaolnbtrrawteinngacavlber,ationverfcatons (COV)aroanaelryzedtoveryhecontinuedaccuracyofhe ba`oAnnbkaolscy,zoenistihmdieacrmeiadnnaigcmecuecpmatolafbbrloaent.eTopnhesatrcasaneldrbarriadotssoetntc.umCrvaieraintdo)tnahfvleearrseftvpceaarstysoiennrngeChcsCkaVomwnpilseml,uesponttbiernwacchikienntg2so5l%vent `crooewpdlaattal.esamples.MulipleCOV evel maybe used.TheCOV usedshoukdbodocumenitnethde 11 Procedures ET FWnoilrbsnosrtteucmouerundsetimdsnoegtneMutpha,ensrientfssetrytusom.tehneCtopniadnntouuoatnlsst:hmTaathpyeerbptesrionaos3oufdosuttrhee,spthpreeotdvlceiodnwsadtareucmfueosntmte.MAiOcCckoemlsapaseredameters ETS 8.11001 A P WCati on GrommapBaono208 MOMS Page8ol 10 Fasessoties rn Bw1T 1E.=1 TuneI Page Nr,t acmaar ne es E = e : | (eschanve j20 [maRez 1| eS n Srte Rs [oE me Jeteom r [aREe, I]S 11.2 InletEditor mmi --m _ -- OvenTempRIG ate of FraiSalasJengLOMSIMS `3M CordovsGroundvwler -Decamber2000 Page sect 145 oe p.90 AtosanmilpCoindoonr TovumecrontoienaTyALbo i "open! fr 4days fom 62703128 EjectSpeed (uUmin)_|200| [SropeTinpe (amee)y_|[1o0080_|| isrecommended,foconsistencyr , 2Saveousm SLAG=Pump Aandtheorganicsavers shvays Pump. " `Savetho method wit anappropiate methodname. Checkteshen ves ihereservoirsan ofl necossay Loadthemethodandtumon hesaver ow: 11.3 Functionlisteditor : `"CiGrueliadtseeiTanoMgDSaeatfcsoqlAuocwi.saiIuooinnmsnentofhmooardtsaopcpnororspenri)oatfterftoomerattheonod,atSahneeeercdmeeeddr.pcSuesaetPhroeseMaiacnrodmonmaesiosftiMenactrsaeesmsmLtraeynnmddxseTMfdhe Gaugerions. VS nilConditons: vt wis a AM [Tees can B[ E l F L "e --L s 17A s| 12 Data Analysis and Calculations Calculations(nckuing,bt otred 0: CKolRcolcootevmeartyt spiOkepobrRtosrseucolvae-rBiaemcsrkuegsirnnvogunhedeRooswduitn,g1eq0u0ation acu percentfrancous he folowingequaton: ortorance o CEcUBted C"oEnxcapnotcrtaotdonCo--nEcxapnetcrttieodnConcantraton . AnalysisofFSiToErTiso8.1rci1nrE0hxR0tor1eapcetrsUsiincg LaOMlSMsS, 0CortonGsm nreer200 Page8ol 10 Page1s45 p91 Documcenotnmaamybaeused. if current, for 14 days fon 22032045 13 Method Performance Cpertoacd,irsatewddientaaparnoloorclwheilrespuopretr.cadstismethod.Documentanychangesfrom hemethodinthe oHremtnsdSaimpnlessomnetshyozdpoodrcrrcmhaenrcceosenctsionosardanoatmmeiln,dmayiPnteonanace.mayDbeopercoomusecdomntehe row {aHbdiaetsaasntdodbaecruespsoerdteidwthheetnepxetroffohmearnocpect.rahavenolbeenmet.hedatamustbefocinctedon 134 System Sultabliity TAyrpmiicnailmutmhoosfetsraempelseyssiearrhsuintapbriitoyr ostamhpelceasbwrialtiboen cfurvced.Tahieshybsegisinugoftaachjabecntdioyniscfmaulysutn. haveorga coun wihanRSDof6%andaelenton meRSDof 2%, 132 Quantitation T0.h8e9c0o,eEfaicchepnotionftdenteermcinrateiomnu(s)tvbaewkioftorth2e5ca%lobfrattheotncheucrrveeimcuaslctobnecgerneaattieorntwheinhortheeqeuxcaelption oftheLLOQ,which maybewithin30%. 13.3 LowerLimitof Quantitation cTonhceeLroiwreartoini'tssoeflQeucaendiaa3ttohn(lLow0eGst)aicscaenpallbytleeannondzmearroxsapndeacri.nFtohremcoasbtaotonncutrvtehs.eLL,OQ c`aSialbvreano,nmcautrivea.nTdHmeitshnoodbkaavkayrsepaocsoeuinitsomrumsattbrioxb<a5nkhs,twohfatrhstlhoewresstmsatyabnedadrfdeucsietdienheveel of fdoartgaeatnadndayiis.sThcoieuntnhdseogrseownedouadsoav, fanyshoukdbetakennkocoun whenevaluatingsample 14 _Pollution Prevention and Waste Management `wSaasmptlieexdtirsapcosweadsitbearonkdefnrgamsabcolntsaivneerns icsadtisponsedhinliaghboBrTaU.corkainers,an glasspipes 15 Records Recorddotaperth laboratory sstandardoperatingprocedures. 16 Attachments None 17_Roferences EwTSi-h9A-024m, "OoperPartsieosnsapunrdeMhaniiznateteinonarnSocueorscfeM'i.cromass TreQuadrupoleMassSpectometersled err A SMo CorionsGn romer.pCancpemabesc2008 LOMSMS Pegoef1s0 Panesores p92 Cocuacroomnmeiny tbe use we| fe Adanrsan HOH 18 Affected Documents None. 19 Rovisions NRuevmibsieorn "17" Updatedto henewformat. Cha`ngSedutemromferatanargleyoswformoretypesofmates 0 Rbeatmeostveedd. oRremvicedathtehmedtahfotdotonsnciundSeechteonnewrequirementsof he n'ow omet. AnyiofMoFiroroacnEharmriimmscaeelsiea0t0p Stoaa r 3s028 cmsCMON Page 100110 Paan7ot a8 Doccuomwepnatmmaay be sed. p93 current, for 14 ays fem 12/03/20 3M Environmental Laboratory TT heed Determination of Perfiuorinated Acids, Alcohols, Amides, and Sulfonates In Water By SoliCdhrPohmaasteoEgxrtarpahcyti/oMnasasndSpHeicgthrPoemreftorrymance Liquid Method Number: ETS3.164.3 Adoption Date: 28Apr2000 Revision Date: Upon Signing Effective Date: 08/24/07 Approved By: St iVonasgmeKr Resgen : 0Te8e opis OolermaisraaisonvoafPresn oHonhPAcsas,aAriosnoE,wArmCiheaasmaanndsSaucbyiResas inSWpaoptcaog9meesSyot20 CoctoornovSeo.mvannRaBporie 1000 Prctmarnis p94 DsccounmreonetnTrAaLaybeusea, cures for 14 0a; from 020312016 1_Scope and Application "eTxrqtiurisadcmtecihtorhnoo(mdSadtPooEag)cfrraoiplbhoeyswtmehadebseyxstssropacpetecirioanotmonfe,aryge(enHttPfLncGaaMttSne),sonrodtmqawnaduteemrmamaastrrsuissciipensegucstHoiinmggahestpokeytdrhooisanence Wpa(etrFetPruL,oCarModoScMtiSan)nke.isnTugkhwniaytmleeartmshiaodmdeplh(eaFssO.bSoATo),anavnmaleditpdheaortfdeuidosfcroooonpcseiitaduneorrsoetcdsc(atPpaFanOerAsf)oionnrgmeroaunn(cdPveOaS-t)ebm,,aestsuhfeoadcds So`uannndmadatyebeeraspSptelaetratmnhetamdheietidhsenotdmgi8isnnracgtvo0anlokTafetoetdhfleorrnpeCrobmOupcCrodiunnaodtesds8t6a0ssd, tthoesnecoo,pesaomfidhuees,oarirgdnal pATrhnoiatsoimcseostl.hfoodritsbDaestedenintpeirotnoonfthPoeScMha oErngovvoicrioannmeesnuttablnLaatboeratory re(pPFtOSE),0P1er-f0ur4o5oc4i,an`sMethodof v`basyluEkfdxosmytygaaedmnisdRieen(sgePaaFrAOcAhD()Lo.smaaenmrdpPleeCraoukanrueooAcnfigrmhnfeoixecataelc(LtaPbnOoAraaAnt)odrines,iallIonacr)k,.oT8n3hdivesovmleulmoeepoedtfwaenSshd.voaroiiTdghanedtaseled Vholauprmoejsemctaieysbd.eAcchcaenpgteadbloenreapcoeveprirejseocftababsoirsatIormy eqtutahleCootnaqsuaakmtpyldebsfwecitvdeesmsoentstortahtebtyhat heextractionandeonvolesdonot pacthe aitofthe method `Samplecolcton isnotcoveredune isanalyticalprocedure. 2 JUNG, iirosimirmimmsismemmmmmerereeeeeeeee `P``sWeaarmtcupelorearssnauramsutpsitleinnedggasiscamoireddketsdhc,oaohnlooaeelso.cetSoeed,pxreaaormcamittdioaesonsn,e(aSlonPdfEdei)nnscftaceorraneitsctotgneae,nssa.dnrhTdeihmepeexpcaaescdutro0eetdmhfemenaotnmaaplryurseaoscshcsofuemoapdfclfithnos.emhewddahebtyeSsrPE HTdiiegfghihvnppeederGrfCmosmeaonnmcceeenkltusdalreccshhrraoommiaattdoogcrrnaadpphmhyeyeitmtaasnsdtsehsmepdemecattsraosmqseutpareiylct(coHbmPeecLtiCyvIeM(sSHc)uPmiLanCyebMdSeiMnsSte)hdeangafelhnyeersails. projectaie forthegivenproject "rhTehesepcuooannnscieetonatftrtoahnteiioqonuonefonertetscauhomndmoeenndtf(eodrascuoomfmmmpuoentdeicnttiolsnosmf)eMspusruotdreuecdoebndybsc)yomptpraaotrcciconegmdtphboyeutnhMdeSsoratemhseepMonSsof `compound nenexrectedcatratonstander (extemalstandard). 3 Definitions 3.1 SPE cartridge Acomncontainingan opensolventresevor, retainingft,sorbentbed,retainianndg, `c9So.emppTeorhauetnsedodrsfbooefmnnttohreeedwseittsdbeeorpmneadntediidcnselgsioacnnwtdhhiercsfhooldvueGcneotsdcgonnnkeddoonn0ssae.plTperchotpiervciealtyerosooavmneontrpeoofdrtoasnealushyestisnc.andbe 3.2 Analytical Sample Aportonofanextractedlaboratory samplepreparedforanaes. DPhaeseExttracotofiPoenrstmnucdriHingathePdneArEdfdTosa r5,ma8Anl1ctoe5hL4lisqo 3u,iAddCnehsr,aonmdaSlougorainpnSWphaaetycPerMtarogbameeeys2tS0syso1.2d0 aMCortE0onn01G4rs oonvmeCpaorc#a2o208 Pgetbat ies ccoanwepeaay Teer. fener ive cag p95 fan, E01 3.3 ApCnraoladicebutreeacmtuiisnsoendoaSmktooaunnptrdeaopfraAdrSeTdbMytysppoin|Wgalakan,oHwPnLCvoglruamdeeorfotohgaeWntewrakisg,Sotraondharrsdl(aWbSi)ervootaer Fhe.umoonrstaerwavteeo, a0ndcaexbraalcingotneiuomunarc0ceoprodnisn6gWtoiirompeetchto0da.Tnhae caClobnrcaetnotnrasttiaonndard 3.4 `LAaaltsbbsoorreaaxttaocoytrdeuydpisDcuuapdtlaeiscnaamyptleaSisap&maparlpaealr(wtLiDahSl)ountoaflapsaomcpeldeu,rsask.enAtnh anoafahLyOclSalcaoybmopratsroerdy DuTthewoihhesafrmepakccuocltaciivon,8mreeasseuvratoofn(,heoKpraogcseonPraoscsacceuaotse.dwinlaboratory procecres, 3.5AsCFoSlinTtecalMiodnTneByiroplnneasna,wkas(atrFbo,rcBar)Hga/ePtT,rLryCriaepsgnerBdravldvaaeetanirloekenaadgne8ndtoawsfaatamep,nloeycialaplrrsroecsuopeccubtrs,ew.Tcahhreipsngplapc0eod8of11thases0aFmsBpaiolmep0ing GStaarmmeisntfessetsrubestda1nc.e8so.fTophBltaekr.rence ar present hefkovicrment: This 3.6 Fleld Duplicate Sample (FDS) IoAo1f5sbtpahlomaerpcpoleedencciopslreoloenrccsetsdeesudnroitecnsadi.ullApcelndricsawauiytmhesasstatotfmahpcehleesesacFamonDeldSetcvcieoimaomenlpf,eardrroeemdastehctenotshaatDamooeonsflataonchmdaetiFrosronaasugsaegtm,hphe2ltsewafemlevpedlasesaa.nTmidheheosFuDrSs. laboratoryprocedres. 3.7f`SlFaAiemedsploladtapmnMutathstoetrwiblhaxobcoSrhadpkteinorokdywebnoet(khFerMnssSia1)emspotficteohsnetaarianregsreowtnitathn1oau1teFsnsorilodg.a.dATdkh.enadomw0na,yhSbpseeaacmicpeclvoeomblpoultmiesiohnfbehdyo "masainpg Fprte4s05o1v0etrrineesoineehxopaecutecdaonfalthyetseacmoprlceacnoartnoenr1.ThsoaFmpMlSe.sIhhoopbesuepicded rangeofanalyte concentrationsisunknown, multiplespikesatvarying volsmaybeprepared to iosnpFcisrkaeemaspreletehpherieBpknaergleindomoordotcehaaocthnassaepmipskieabngtsalno1acppharosparTnihaayteeilFceIavSerlieisssmauansda.ey.aTdyp1icsasllcyar8kionw amnadtiachaigfhc 3.8 Field Spike Control Sample (FSCS)/TripBlankMatrix Spike C`Aowanlhbioaclcshiikqtounonrotwp(osnfoAqauSatnTatoMpitpThiryeosspphoreiifpt|mwheaecnttoatenrcrfeg(neHtotrPaanLctaCoillgoylnrteaec1stdbiaeororneebdaaoegdreedemnestdi.wTinanhettdeehrbeFoyfSireColadtShapeitrrastosuhftiectattaiclbmialeeedowd)afatosneadnrammnpnalaeelyyuzseedd) to `aSSxpaaacmieesdhosoraamgspealamecpnldoernosdceetponmeitnreasnwsathudetentsoih.tkeAonrlonows0wn.rTodifhsahsnaamFplSlCecmSomauyabyobseaopbarodovperdeiaodhw0hn8anTmHDe, BlakMatixSpike. 3.9 Laboratory Control Sample (LCS) AWrneahcliokqnuno.otwoAnfllAqeSuaTasnMwToyploeefvt|wlhaestaaerrog(eHclPaeLnCdagr,easodnerereegaaagdneedrneatdwlayntaehrtoearorotmwhoeerrnsyudiottfahblheewcialmtbeerrmaofoasnyacumusprelvdee)to DetrminatonofPertuoratedAEcrss,aAlo1h54a3,Amides,andSufonates inWPataegMrbeays3Ss0o1n2a0 PhaseExtractionandHighPerformance Liquid ChromatograpShpeyc/trometry WMCoretonnGornaieamsoaanron 609 Posesocr sas Decnmiaymheesard. cuanto coneema p96 18 Ce fon bu CGI a5ndoa nleanbeoraetrhesmamiploeuopdpeertarainngsewohfetthhecrurvteh.amTehtehoLdCSfnarcoexna.ctLeCd Sansdhoanualybzeedprspxaacrleyd 3.4`0eacL h daaysbad mMapraretel rxitirxeact Stsepdi.o ke (rLMyS) d`2ldeadberdiisntrnnyemlaaebborasepikelThaoenLsMaSuvics eooxfacsstaemdspan iooswhnicyDhoksneoxiwancccyaermaeasssoofrTatharogeetSraaongmaepenosoouasre `icoonmceeantsruartieodnsoafkthseanntahleyLeMsSntchoemseciaedefomatreisxpmcuosntcbeentdaettoenrsm.inedin separatealquot and 3.41ALpoarbtoonraostioqruoytSfasmspleemplefromotche odiorvfeestdng. 342 _Lubitof Quantita(tLiQo)n" - . GQ"Touhnaedrtiookwrsest.dTiwotitosficliunlaenystpidaaatctioaenrde(pLoLrs.i0oQn),ffoarroLdcLeOSsGnefasngden9he0ercaullroawcsye0:lcoocnoncdgeoTrsiorhateoenonChpeaestrcaratonngnbe2r6o0by G`Seipaennddaerndtn.thecalbraon uvehat meetsmeodr7ea.SampleLLOQSaemats TQGhoueraudnpopntsea.rTmwhtieofHniqguehsetsiptaseticoatnn(eddeLrdOnntGsthofoefrcpl8sdicarstaaotsnoenatircsurovsecchhulrsomy:eeGctuosnnmcgeonoinradteornptohcrticnangdboofnreodobs y theULOQ. Ro 313 MethodBlank {`ArSnavtaelarku,aottnoedfdAreSxeTaacgMteTynyWtpeheta| waabarotresuts(ceHndPyWLSChamgrpOalldehecrraiebaongregnattwrxyaspeaormsploebs0e.TrahsegmtGeaitsohwovadorl,eerqmkuaiyps Uessnded,) Geomisoo rfibeosaspbpsa,nrc.esoowbere1 wenxerseCn1 cesaereset helabortryemicnmer, he 3.44 Sample es sample melorioncalcdfo argaGanttofmateri Fendarepresentthe `original sourcematerial. 3.45cocSomnptcooeuncntkrda.tSetdasonudtaorndSofolsuntgionna(tSSiSp)r:e-par:..ed n reeera.lory wih an assayedrforence 316 Surrogate Acampoundsiriartoth large oo nai(s) inchemicalcomposifonandbehav thatsnot oSnanompmslaeas 6cfoonutnaQdiunnianyegcoosnnatmrspce(osspa)im.cpAislsus(rbeoxocgeeadpttSsscuhooemrptnobu.nadriksusysaiencdda,hlTa 0ofoarhgoetgaronopraaehr8e0ds0wmiedhtoh)fooeldast Blanka). Surogee(s)ar acid o uanttatvelyeval hootro anlyal procedure iGonpactmliueodrnisanlgpcsoaumiplceoconllaecmltieooan,steuxrtwracahtnideon,raNnOOdT1ar0neaql8yosrTiosO.d.GITnhcleusCpiOroonmjopofectnaesaudrwrslohlgboaetuepaannrahocyftee0isaannhyes. `DePthoamsineaEtxtornacotfioPnernoddnHsiigehdPoAErcrtems,aanAiccoesnLiouss,dAiCders,oamnadStuonagiresapISnhpeaycoPMkroabamays4tSgsoyofw2ea0 CatEonnoGn:oiimmRepSoooeo2na2c00 er DuccuomnreonetnTmaLay be 156 cartenl for 16 6a p.o7 02 54707 347 Working Standard(WS) pArsepoalrteoncaoffosreaveornasltannadtaerdssparnedpatrheedrirnohquerleadbarnataoryfsrooumtSoSnSs anddiedasneeded10 4_ Warningsand Cautions 4.1 HealthandSafety d"oTthaercmuinteeda;nhdocwehvveorn,ct0aocihshvfitdhbsetaonadtaerddsasoratphoitsemnettalhohdeahtahvehnazoatrbde.enprecisely cUonnktanionwernsssahmopluedsbmeaoypceonnetadini haihgohocdoanncednhtraantidoendsowivhoglotveetsfco prceovmepnotuenxdpso.suSraem.ple mt"oaTchteaelriaeblgousrlaaaftteoitroyyndisaereagsasphroeinenstgistb(heMefhSoarDnmSda)iisnnhagnuoidtnbhgeaecashavefamelibcairlksu0esarelndpmneerisnsontneaentidndvao.luvreAderinentfteahrweeansrceeefnleesosfof analyses. 42 Cautions n"fsToyhtselotaienmmrasil.eymdRsa0toam0nf,udtosctfhaoiebuuhtosieofenaanospmf.pirsoopfwrvietraitste,hspeqreluaspbsmoureraintzotreydprgeoaqcsueaidpnumrdeenotrvaoenpndetrpnaotstoer,mtaainlguhhavalzofatorardagsecn,acounnddnvga,cbuuutm 5 Interferences D`u5r0ikngpheaxstereaxctkroancatinodnadneavliycseiss,.beawareofpotanalcontawminantsrcesfom reagent and `AcoSnmdaittieornisaolfs uasneadly1tbhyanuarliynsegsmsehtalhlobdebaermkso.nsated 6Foefomnereroncesunder PairtnsanedsruapnfpdlleoosrtchoeanttcanmoinncaatnieoTn.etTohnessehmoauydbnecauvdoei,dbeddoarr irnoiiizeedddue:wtatshhebpootsss,i of "TTeefunseionfeidscpoopssa,taluetoviicerlopciappest,iHesPoLfCpppaettessocto.suostandardsoluonsis recommendedto makecolbratonstandardsand atxspikes. 6 _ Instrumentation, Supplies, and Materials DpNeeomrtofano:smtBraranatcniedonnmaamoyfeebsq,eusaiucvphaipleeevnretse,rasonridmgparantpcperaur(mtqbuuesraasynacrdoenmtfaroorrlisuaasmtplatethsvsmpteuheratpinonsgemsseoetlshypo.adEcqaeucdicveapeltreaenn.tce rior)is herosponsiiyofth laborerperitheanalysis. 6.1 Instrumentation Balance,analytical (display atleast0.0001),Metter HPLGMSMSorHPLCIMSsystem, sdescribedinSecton 10. 6.2 Supplies and Materials. DetPorrimsienEaxitornacotfioPnearuncdriHngahtePdeAErctcTrsm,SaAnlcc1oe5hLo4ilq3su,iAdmiCdhesr,aonmdaSutfoongalreos npSpWhePacytaerMrgoBmaeeystsSrsyo12a0 0CorEsoonnGrmnnpncanet2er 309 Pageszot 1s Bataan may he coneoeNTAL degre p98 fo Naa En pli D`SoamrpkleucsoeleTceifolnonbbotttieosso--rLTOoPtEon(0n.5e, dNcaalpgee.naTM) naw botswihscrowcap, Nota: (Coolersorbosforsampleshipment. AE utoTracesuB tommaatyedbSaPED werkostsason,SCaeesrLieSTciaenrcese. AFEmmaaSPdnEmrauencfosildnwlih Vacuumpump, Bch. Visiropvocuum mend,Supelco. 15m.disposatiopolyocapnetbeesn,WRs. Om iiposatiopolyprceontprye lbses,nWAeR So`SuepPrakVac6ocof(10r) e(Cr18cartviedlgesapyaen #WdATS0e36n7d55),oWenleords.et(aCqatrytcwiicdhgooevesr ho 16mLdeposatleculetes(17 x 100mm), VAR(CatNo.60616.626). Disposablemicropipeties (50-100, 100-2004),Drummond. x Class Appetos ndvolumetric ask,yarous. LDPEnaoumauthbots,Nalgene(`okiesmayvarydependingonanalyte!needs), 2m clearHPLCvial kit(cat# 5181-3400),AgheriHewettPackard. `Standard ab equipment(racuated ines, disposable bes,oc),vrous. 7_ ReagandeStnantdarsds Noaty :bSaucphpiteevresdaunsdicnagcthaelmogincualmsbecrbisaainefrfmsoteatrospupuprlpioersse.sDolnyo.EtqUsueaalesseprtroardmeaonfce chetmhanithocseaetle. 7.1 Chemicals Methanol(MeOH), HPLCgrade,JTBaker,CatalogNo! 9083-2. AmmoniumAcetate,Reagentrads, Sgme-Arch,CatalogNo.A-730. aAiSsTobMeTuyspeed|)Water,preparedin-house (HPLC radereagentwater oroersufatlewatermay SocumThiosufats,Reagentgrace,JTBaker': : w 7.2 Standards so PFBA,HeptafAuc,o(rCPeortbuodunattedyAcck) NFPA,NonafuorAod(pCsePenrhtuiaetnsdoAcst) PFHA,ParuooAchid e(CsrPerauorninacteidAcc) TOMA,TrcocatuoAr,ohCrePeprttuoarnnatoedAicc) PFOA,Ammonium perfuorc(oCscPeiruacrninceleedAtdd,) CsAck,HeptadecaltuorononanAcicd PFDA,NonadecatuAccd(rCroo PderefucorananedAccck) DetonationofPeruoinatedAEdTs,SA8l1oo5h4ls3,Aides, ndSufonates In tPeraBySgoofb2ea0 PhaseExtraction andHighPortmanceLid ChormatorapShpeycMioamsetsy Cori Goran Sono 600 Freese x Osccioumrepnetnm.ay te seg + creat, for 14 Gays fom 021032610 CCynAcck PPeetuuoorruodnoddeaccaannAAdciccictt FFBO8SAA,,PPeedruicuroorbcuatnaenseustuoonnyaimaimdiede PFBS,PotassiumPortucrobutanestorate PRLOS,rPotassiu--mpo--tuc--roo--ctanesuons TTHHPPFOFSD,SH,H,,HH,,224H,,2p24r+HtpuerohdoerccoacannssssuuonoircAiAccck ` : PPRFOOAS[1(20"3C,),0;sC tioctiocpicallyabaeblleeddAmpmeornoiruomaPcearnudocraocodc,aPiaenrsunfoEnismieer Othesereqruirsed. 7.3 R25e0amgoemn.tsProepuarthaotsiuolnitesoon -- Disc 259ofsodum biosufls in 00mreagent 22a0mtWeoafmrmeoangeinutmwaatct:a cuton(Ansyse--Weigh 0.3 ofamareaceatsand dsslve1 mNaet:aAneldmasvolumes eybeprepared slong 8 4 aos oftesole 1 kderasaro 7.4 Stock Standard Solution (S88) and Working Standard Solution T\POhrueaompewasriamntagiyobsnetacnhdaarndgredoa0srstepnroeceeddusroefserpvreisculsaarsnexyampFloercWeredaiao.umvrolduspmaensmd,ayal fp`b1eoe0rxs0cipgemkneemtrds.ailtntttaaoasrvgno.elTdutprmauaernrtnatrsilychy)tflataSnosdSkaesSci1we2h--6eWktneo.dLgi0Dht0PinEmugb.tso1twto0ichmkomgsarootlcufhiteeienornlssyttioocaaoalplbpeeraroncpsdroiaanartalenle(e.cvseoolmPsveo.ecprta,ernofsaor 00 `SuSnnoatabenspacssisoiacnganmoecrdieoaanccheradnvaaneyctnebslEAoxwhprBoartroPnaFdOayStSsaannddesrorpaagreaonngdpioocnsoofrseo.Acknecxhaomnplseof arenaacctoor= Teeccaunvewiegihgthotfofaisoanl 2708 Kotcomatontr =2305275 10mgCoFuSO5K"withpurity90% =8.35mgCaF rS05TM (10mg*0.600.8275+8m.g3)5 40p0nm.vo(m0e0#0tncgiflmaLskmaindseidwgor0kpin0gvsotkamnedawrhd--sAcdivder1t..0m oachofhe 100g.$55 108 `0S:anpdgormLs0(u1o00nnm5)10m0imx,evdwoormkiEng15st.sa8kn.dn1ad5rdb0--i3nAgdUp 01.0ummofehWei 1s.e0nptg.LmiPnaegdew7o0rk120 Dot"aPmhaisnetExotnracoftiPoencatncddHnisgthnPdeArcfoor,mAanocenLoiq,uiAdiCdheis,oamndaStoongartaepShpVyiesc/ttaMoramBeystSsyo. Corteoxnr0G 1,iao m ganrn or200 [ p.100 Fcumest mag be Used, Surient fo 1 days fren 029500 come 0S.00l1upiogntmo8(1100n0gm/.mvoLl)ummeitxreicdsatsaknadnadrbdri--nAgdudp100.v0omlLuomfetwhei0hs.v1eL.moredwor standard `sSttaonrdaagredCoopnedraittiingopnrs--oScieodruerealolSISaSseafngdowroarokrinagts4t2a2ndaCrfdosri8nmacxoridmaunmcpeewnidhobf omraotnes romthe doteofpreparation. 7.5 Calibration Standards `WUasatinenrgv,eohakeitwnghoersrkaisnundtgaasrbtldaesnwdmaaatreydrsb,deeosscesrgitbheeedafbooolvmoewe,iplnrgte2pha0rceat8caalq8bguxuaatiyolnhsepoe.cktcNveonstsa:icnVoAsSosTlMeTduyonpmfwooea|tser gneeneederda. rejectune.Calbratonevlsche than hos iedbowcanboprepared 35 VetaorW3. - Erivct rrContr etowsneeenorf [ow Tw] [wo Tw [em] [wm Tw wT om | Cw wo TemT om [[wComw T To m7 17"0 01 oowm | | [[C[ Coomm 1 Tw o [w 7 0 o 7 10 T a o "0 . smm ]| ["od TemClbreate othioeT nlebnn oaraartadrsysa waompprloew cse,sTsheedcFYoougahn2e] "SocrftheG|xCraabncriaolrnprsoiaoamonddueatrrd_i(noSteh_ecfonna]1l1), xtactdeperetsonthevolumeexacted ndthe nalSionvolume. Final samoconcanaton factor =Vokumesxacted(nLYElufonVokume(ml) I`axSbttooarlcaetgdseisCunotnocvdoioblrsodnaastn--4cS6ew2iirCh.elaAibfoerrxataaolcryytssitsac,naadlratcrahdtioivpoeenasrltsainxndtgaarpcdrisoecidsnsct1uar5nemdsLa.prodlsywpirohptyhleesneampbleeso in 8_ Sample CollBoettlcePtrepiaroatinon parFeororsanmoonnscsetlpeirsoktjoetmcrawottsiir,nishcexagympaspihihelnege.lchaeDiocepoeplptceeenctdtdneoitbntnoshgtdoetisne:stlaehs cortsirconoea ppsefteoere.fdtTm bhuyeypppiiSrccoMp ajaeltEc,stn,vSoai, audcmrdsmpoee,pnratlsraoalwetpLeoalcbcdooalrteaaectsttooroxnyfsbhtpeike,s fleoevueldsfsaipmepadmlnaeatlnairdgfseicpskoemnscltebxnetsprokalelteascinmioogadneyfbtheeaedxdpecdiAaldssoa,mp1lecnooncuentnraticonsfooremaBddumiyounnoalkmondw:nof oLrotwadionenrssi:y(pVoolykeutmheysloenfet(heDPboEt)iewsimdae-ymvoaurtyhdNeaplegnedniengbootnehsoawremuuscehdsfaomrtpleeissarmcpluiecodleocmiooent DePtheramsineaEtxivoanocftPienrafnudrHiisgthePdeArEcfdTosr5,m8Aal-ncc1oeh5o4lqs3u,iAdiCdhsr,onmdaSutoonagtresaIpSnphWeaPytcaotMrgobaemyes8Sts0yo1m20 0CoErt0o71G4r,omtenrReponrets#t2or200 Pagessat ses oer fu conPoeNTAL p.101 SET Er for TA 0s am SHINE d`aahctoeatqotunaeelaistnysdobmojepettchtoainnvloeasla)nnTddhsaaorlteorwrieoedrtqsoouf.thTbeehfNeoaripegrajandedscibtnoeglatthdesimaplapcryobopermiismesudpkmnewshui.etclNoattheei:tfmeareislnswiintghof cufosloilmnepgcltaitoepn.evArotmleaumnmaeienwvtemllaybr,ekaoefntdTeysapcwioicrraelps,ep-omnoaderinkmgedlvooolfhutemhreeinl"diitncahteosrrcserm"aiawnyobnes ptduhoernecexhbtaeysruiesodir.onfg ahmeabrokleer `Foo`sritshndsoainm6aplldlcdeoeundocotaittnehrseaidoemnsyoiogfantanbatoregtdsesfta.onTramhlayettveosslopunimckeoeotsh,fesanpbiaokpeptsrosoproifalnteedvawodildhuemsdeasomhpfolmwekaotpreodspufkclientogheere tnohreedm.aai(tn1ialsspufiokteghsee)tt.aTorhgeentmc(aadtnoidxdssupfTiokrotignhageSprooajkpepocl,icoahbeiled)abTnooagpearseCp:aohrmoepwdeoviuenrds,sMtuabpds4aspviekbereasadondudetdontso mSaoyobnousoedoniatnh psparomperaisatmheiwsoerdkicnogmpSoannednatrdsstuansdeadrd1fscrecetlvtahlecea.lbTrhaekonasiatndakdxisn.gAn exampleofabotsspkeis venbelow. DFeisilroehdeFree"dvoSpliukmeeC=4o5n0cme.(nAt5=r00a0.m1tini./Noamlng.ene ttefsusec) bo484t ocfap1 gromLp ssepailnegdsoln(containing he targetanabtes) added 0he te ndthe sahsans oauldyssaiissofaomdadsSeuaimnpdoagpuapprtiloacpaartnieaesateaevmopssleiusnm.celuodfesd uTtohgeapersjaencdtaorbjdesctioveos,nhe0parlepaherabtoorty sandaelsyisgtnated sAp hiooudtleissooha dwoesaurpdlbt kyei,ncodere iaNciegthlsh. apebisekalee.mdp1I0ciakncodhiclcaaootcnastdioennstihgeannsacdteiifdoenur.seeGnt3deesaisgannaltaeeedestpokfrbsrlaiemveaepllsfe,olhraelga,beenl collectionsteaothen grouped getheri psi beg forCrganizatonal uposes. F"olTehrade.enaucFmohbrctehorloetcfpiopbnabnolvkaen,rktt,shaesstuarrsresoqtugoiarnteeedssfpotkr eoafitsvapednbdpaeredkc1stnhdewbiloptbtbelleca(on1mkmunarctiurdcieaxdsip)eiadknebsdyhrheoenppArgeSjpeTacrMted. h"TTeryrppeebia|nwraa.ktemTrah(toHbPasLtpCtkgercsaadprespraregepeplnaartcweeaddtabenyadod2rdpitenhgmeratshyuibtaaepbploelpawrcaietedteaerrvooeulynuudmseheeodfo)umitaetarideddsegpdein0fgthsheeofcoialpn1.0, fianngtheboth thedesiredvokumewth th appropriatewale andreplacingandseaingthe T"porTtehapelanprruatemipboaenrrwaootrfykbastnhtaeleeytss.ptrTsehhpeaurNieod,tdnouc0mubmFeelenrstohbfootsutaldemppnrceitupdassrt,hsethnelsnotawainNdnoagtrIdnfFdoeimnaettfioiorcnao:tndoanasnteuammpbrpeelpreasraedn,d 5dnapkthoaerpmvaotauomnnceesfekodsreetdhadefptoorgroprjreeeecpcatroosnpskiubcotisbh,eidathetya.T1heeNrost"evooFlulmeew,ialndbeancyudtehdrien rheefntel Det`ePrhmaisneaEtxitorancotfioPnearuncdriHniagihePdoArEdfdTosm,SaA8nlc1oe5Lh4iaq3,uAdmCirdreso,maarlodgSrualpoynMaaesssiSnWpPaetcaetgroBemyesStooyfk2a0 SMCorEn0s7r14 omon mpDooeanan2btor2e08 Pagesoot 18 S[onee --may C8 p.102 ee for 12 Say i 9 Quality Control and Data Quality Objectives An`o alyStiocy a rmues eaosrosferhaeFtB,waFhcMSu,hioLtsUaScm,pFalDr,6as6ndd.FnSC"SAsnhoauydabroeesvuasdfoetdhaestehceonctornoclicshiuopnicoafte 9.1 SolventBlanks x x Saeinveerrt,blSaonyekrssDeaarrkiesSyzheadkwihtav6eacahrsaatertsetitaold1etsf0msineaconnt5a0midoafthioenaorcdamcyuorvero.f In `Sivekbinssh beanal poto olowigsec cabraon uve,00hslof C`oosoyrrcsytttoeeovmneosfuroitlftoa.erbitirrtvyorslakaemHp,lanecrsak,snassneoodcruuasfiktaeesrmoneosmmror0be<at5rha0kn%so1ef0uynbkenonowewecnesssscaa=marpryla.etextirsacctcsaa.sreI;fipnhsortraourmoeantth.e 9.2Method Blanks i LU `AStamlmaetvoawreierem.aiyJbsooeseffd)nese chuytoSomtASSeTSHVApoe5vlre10ncdryansciaoonddpomscshwaiomeoe:mVaerrkecs xroaucgtohntsiareprrocmhodbfaorc8haparrdtacnlrysoscirapprescedMeotuhogdhtarhseaunabceo rsparcseed Tashtaerndaavcred,rsaTghetaersertaancdoaurrodtlsdesfvoipraateicconhuogfrhaoyeasrmeeiassctounlt1dsshoeruadhnb5e0sc%askou.fihatepeader.en aA scopuencd tisoifac%c0Re SLDOOof thaenmdeetrhoedvbleannkhexecueevde5t0h%tomfetshetrLOeG!rst.anNdaerdh,thDeanntkhesmLaOyQbmuesatibmeertaeisdedfltcohtvhiefcarlst justificationcanbeprovided (6.9. themethodblankwas analyzed afteran unexpectedlyhighlevel osamepalen). ron pr. Ifaymethodblanksareremovedfromthe LOQdetermination,documentin theraw 9.3 Laboratory Sample Repl/iFiceldaDutpliocaste Sample Grfoapiencnsoia,ngmaoosn.tIhe1sepcikoopaeaeomffytAlhfrefpiecatweasiracsraecncoenlteee,rsapilniecastssaaamynpbldionpegslxnesctceeedxhraoodcetnaogsncsIofnnodnor `aPmdrophplaersaisooanramnpoldaeinaalyyasnnidosattbbeedeocviodaino.sn e(TRhSeiDn)Gsohvrooue,p5Frecpoekscahfeaesnra2sm0p%lesk(RtnPhkDm)epoefrtfiancglae0o2f0sa%mple hdcre wi berevives andevita nacave case ass. 9.4dLoLtatobemoiraanratetgepoe,rrfyLoirkSMmeaarter1icxopMnSSrpesaihkmaeivssevfp(orrLevoMisSaoaursmsc)lpgyiabneceaunsptaocverv.seFGMfSo eltahevesnaowmopolreheesmoaratmtapp.araocpi.oen for TomnpaaryozsesedptiiakoearGfeecraovreeirtniegssashmhepmoluaedtafnloswfafimocpntloe2n3sm0pu%ktorfeeLcxoMpveSecrytreoedfvcpairnolcpsyroeffooracahcarsgamsplneaan. Lab CLMoSncoencsenetraotfosrpsseChHTtbeeYp4re1p0areneashpLOoG rcoenc0n.510 omfeesatchesennaco.gecs DetheremisnsatEixovnacofioPnrafunotnHsgthedPAEactTkos,aaAn1cc5eLo4i,3dAidCerso,naaongdrSauglohnyaMtaesssISnVpPeetacekgroeme1St0oy0k1a20 0catcoonrG n ia reBpeerasn r2 e208 Prerrorts `Document may be used,if conPoanTAL p.103 renfi 14 G7ys from 206320: 9.5 Laboratory Control Spike (LCS) Lsapprhbekcceissoisonnh.tooLusCdpSbikseepssrhaeorpuadrrbeeedpprarteeapacforonrecdaeanctthraeamxtironanciinimotuhnmeobaeflnwcghoeoflofvdeelplsperaronxidininenamtepetyihfcooduara,cLtaencyoabeacnsodwntol `iorenhlcateainveitsrhtaaatnntodhnaenredtadarervgtiehatetemidiodLn-O(pmcQieantnthdooftdhptreheeiccgiashliobanr)baoctfotnnhcteurporlvoepk.ieFkedoscrs6oh3oicuhllstapbriegkepetrsamopnsoarte,dboathaeepssertchaennotr {`feoqrugaettaon2al0y%teasncdutishideavoefrtahegelaebcooravteorryyc(omnveodsapcickueraacccye)ptmaunsctecber3e0a-2ar0e%n.cSk aemppolreadbae.a or 9.6 Field Matrix Spikes (FMSs) hfMookpSdrisonsgaarrtmosperaoenpfaesrrpeedkneftorrseeacamocpvhleseraamnefpdilsceaiaemnnpcldyoaemnfaaeltoycizhedtatrogdetetaonmian.g tGhsmeanx esfefaeccrhtsoanamdpslalmelpyolcea,ion F`sMcaSmipslaembgpohltFetseMiSrteahreaefspaermdepploaeriteofhwoheielcaahbcokhrnastaoomwrpnylbGienufgaornoechaselobonf.thTeshteaaieagtestoaeonnfatleyottnehseadfreeola.dgdaTeeyndpaiirlcoyatlchloeyuaflisoewd sspamlmokpselcteohniesceexenxptpreeacctttieeoddnsToaimbtsesle1a.cp0opnrngoc/pormniLta,atttehtieoona"spFpeoosrpsrasatmccpuarn.acgfye1tf8hoderefFeinMndSeoudgse3nesodusstpoplaersvmsealetsofasalarycac0ur5a1c0nyto1hf0e Tb`ooonasdosgpewnoouukpsdabnreaa4epop0sr1poxrd0emsateitimnaetlstmah0oe5raLboOoQoticwohne0cee1tn0alrrnagtegyoten.d.FLFoOorr,es1xahammpaplplepesr,otphfatithateaersroaenxngpeecaLotOreFdGbM0sSht0wa0voe2eu5 gSpianc,itadhreaapnpgrooopfrinataeyrlaengoencoerroirwateovnes FLMrSkwoawnd,mbei0p.1snSpiikes1a0l.2va5rnyingg e.veIshmeaybe propared 0increasethelkeloodhl spk atan propria ovismode. FFdMiPStMeSwmraaeastfcsstoNpvosihepetrkdRinoeaspmtooeuarettntshainobdaddelpepoa,rfcocFoer3opi0rtad%atnoscotefetcvrheoep,eeoxriapebesirclattemyefp,dol0vcesaorlavuomeerpouelftsewsmouairleydpnbonr+eot3erb0eda-e%easoxstfNrsaRech.seiwesedhexepdaernbcoedtNceraRdouivssaektee. `rooe-nsaaanmyapzll0yidsniogrfaaanindstortemaeenamelysstihsenFoalfMyaiSncaeaclwcmoesptakhmaopndlcmeecmaeeyrybbieaea,cp1polimespdaemopltlh.eeffsovsu-mleixpveri.alcbtAaotrnee,mparoetrsetalemydp,l3isnNg,Ra"nd (pot repoteddue to noncompOlCireasnust), Excaptions the 30%FMSacosptanca teriafordoaroportabityareasfolows: La1b)orHaFtoMrSyMreactorviexrSy cpouekd (nLcMSb)emaasysbesesseudbbsetcuatuesde.FALSV'Swfeorcaoveartiaens ainraoppwrkohpienat30o%vtehedhoetna ar reporiabe utfaggeda3 otmesting heFMSmethodacceptancecrea. as2ca)cmepHplteiamnmecetersatFnMhgSee'ts3hw0eed%roaepcarcaeerppotararenpeocdreotcnarbllaeserbaaulu8etaaagdn9ddebdhowneilchFoasnIese'txFpaMaonSdoeeuvdteaulndcteoetrhhtaeei3nrte0ypa%orntdedsnot mosingFMSmethodacceptarnicene. a3na)ieoHxrpihcaolnrFdoMepdSourrniecaceborivteaeFirnMiteSysasaanrmdpaclsutesorietdsmeuoetefstatihrenegaF3vM0ai%Slocacbrceatpfrtheeanacteamanagyebbeu eaptoeraisetdb20tafcaegpgieadbwlieh 10 Calibration and Standardization DotPohmaisnoEaxornaocifoPneraunarnHaitgehdPeAcEciTdmsaS,n8cc1eo5Lh4ioq3,uAdmiCdehs,raonmdSauafogareasIpnShpWePaycateMrrgoaBmeeystS1rsyo10b1a20 SMCarEoonnoGun r mmaRaSpocnmo2mona008 Pacesoct165 p.104 a coneroenTAL 10.1NotI:nIsnttriusmeexanmtpSlee,taunpApple BiosystemsSciexAPY4000TandemMassSpectrometer SS{CppapLclliCorrmAse,MpteaSrrissMn(uusLSmoCbd)Me.rSOs)t,mhoeanrydbbmreoandsdeessdofaarLfCooMngSMu0sSta3hievm5ewetehlpoodsrSetlsaoenya.rqoaEmdqeuulpa.oelBnrtamnadpsnerasfmoemsa,nce Gmfoaryonobnsasstpcathoovonneofdfshusescbaiuovneirglaeettprprteyyrp.eetrTufshoernmadpnomcresakhoarrtmmlueseitthsoepthihiazrneeqauonisdreeGmoepcneutcmteofnettdsthhemsee,ctpharomdesntdheand saings used. Estabieh he LCMSIMS systemand operat conditionsequivalent1 theflowing: MoansSsoSuprceec::TAppuledbBoSoplasyyo(AsBnASPe)!4m0s00 Scan Type:MRM (Mule ReectonMondor) Harvardinfusionpump (Harvard psiuments)fortring `Computer: DetOHM RB 3 Sofware:Windows2000 orWindowsXP,Anat14.1 HPLC: AglontSores1100 AghertQustomaryPump : Agler VacuumDegasser Agha Autosamper . S`Nuoatmnad)S:omOpanayerbsoetramantoiyrarecehsGe1cdoueHnPooLnCtadafmeniraciainoaslphuca somvaamlyvbe(oa2.n11dhmbeemfomxro1b0d0heep7Sl,easmeyaemnndoerrc2t.Ho1PnmLpmCosxry5s0tre1emmt.mar,d HPLCColi:Botas C18,2. fmm 100mm, 5m(ThemoeCocrptoraotionn) Cotumn Temperate: 36C, S| : InfectionVolume: Si. > Mobi Phase(A):2m AmmoniumActasinASTM Type [water(Ses 7.3) Mobi Phase 8): Methangl+ =~ <1 DetPehrmaisneatEixotnroocftoPnafnucdrHiingahePdAocEakdTas,SnA8cc1oe5rLn4is3u,AiCdehs,oamnadStuoongsrieaspISnhpWPeaycsaMeigroabomyse1Srs2cyi0120 SW Cat0o7.0G14m0.iinmaReSgoeanm12es200 Poansactris `LiquidChromatGroadgierntaPrpoghraym, CoToTw1wo1me [21 was [a0 | we 1 00 eT es a0| wo 1 20 | AmHnenEenSsa ste msTposieeeenpprratocie Note:OtherHPLCgradientsmaybeusedaslongasthemethodcriteriaandprojectdataquality [ me || me | | [ocams ano |wo 1 = [Pracasn | sso | sservee | ws | [ors 1 wo Juwnwam4 es]| [oa [pres | wre | meTw | | 20 | seme | es | [meros | [eros 1 [Proanzig | [erosion | aso T 5030. | asses | |__soarer|o ee 00, ow] ren cEonEsn i te srpm t es `PhaseExtraction and HighPerformanceLiquidChromatography Mass Spectrometry p.106 Pocumens may be vee *orient, (5 44 5s Hom 6202315 conoema SrManoiantlunbanncaaiosvnsfgorafmmsnaoremreasirnrdgalhteTmorararsucstoeosoefJsi.eacdahtyeogsnhNorUosRnudfmositSncagadmpuaatyehtmveansrhicooanscmiady V`sSienusnitnivhigtayaeissoarccihPiFepeOvSde.di,pGrumoavaniydibeadottoChnhaotmsreeytnebnstetiophneetrdiomcaermcereiidtoenursiiaonafgritesmhaenttatilyoasatos.nsmucaryseoasmdvaeatqaurgaartaemsp(GecI'isCic)iftoyr. `aDg6iveofntahnaslygtpee.Fsoerdperxaimmpelye,othnesPFreOcAoTmImeCnwdoeudl.dsRuelmeanliltohnrSeeeosfmthaeymvonairtyoSreGdb,anscintoanso.y- `tuos-eddaeytbca.siDrsi,fdteipnernedteinntgioonnttihmeesbaitscahccoefpmtoabbilleewpithhaisneananandatlhyetigcraaldriuenn,ta,csolkounmgna,3gtuhaerddcrotlumn(s) oncontinuesthroughthe entreanalysisendthestandardsareinterspersedthroughout theanalytical 10.2 Method Acquisition Parameters - Troeharupmf,oelnstoiotwniirgnloiggeervnxaaampltreueuremsiisemssareretnz.nptumrAsoiesvreyi,.ddeehIdefsasa,siemnvngueahiesrSrpcaoyobnofioSmsicouihtsmaheneo,grdeetasdacfchoonspmrtAinocedtmpaavrayalmmhoeoaetvsemresraaiyeofrvrlar0seydfggoelms, TompaendronSrey vaBgEn [[c ro emmopmwommnTe Tahineangsn|| [om2ummeosmmToarosns)| [ [e rmtmaocoorvono[ mTom 0wer|| 10.3`SAtnasnCydazalaritdbcerasratvtaeinosdnhaorCuduurbrvpeeotretuaeach rtaoeffstawmepilgehsTheTvratterwdemietghhoedsHpoawceverah,to he CU`oZssotimrann.gtdsaTreahdbcelumraehvtrehsomeucamgayahtaorilucst.ao8TbmrSeeeutpclchyoa.tlAtubersrdbeaytcyoh1qhucaacrdavrskasatSdihmcafoatuy(2ybc=csalBexbo'rrab+otbudoxgnh+ac)dvd,oweceuiihmgtohetuneodkde1bd/roioxnaoobpdfpoultnoerwoewuiggdhhotaed, Ifthecaltrationcurve ossnotmeetacceptancerere, peo routemainlenanceorprepare. Fnoerpwusrtpaonsdeasrodfcsurcvae(cifynewcheessnaqruya)raitnadtrienganoalwyzee.ve ofana,may benecessary ouse `lqSoawunedanadnroctaffatpohpemrcoaxl0ii.bmr2aat5teinlooyn0cm.ui0r5vge1ra0nthenrotfghan.nathteehfurlgltrehananrngeeh.eFoCrae alntrgxaeifnachuwerm hvceenacpvaatetnl (e0smp0te l2i5nog,fgthoieno 12Co5m.v0e0nntga/imLo)n.sTahnidsewrilsl,reduce inaccuracyattributed10 linearregressionweightingofhigh. `CaHaiatg0rhoafsSn9dpLiroorowltaoewntvpdoeiatnotntvshmefoapGsyoobtroesteesxbchelocuuadaremkde.8fAr0oremytyheexvcrcaeullicboermadnatfieomneackyurbrvreeesraotcooopouorrodvidddreosacab8cektc0taeetpr0RfaitsrotvfWecritSohne. DeFtearmsinoatEioancotfoPnerahnodr+siiedPAErd1os3,8anc1co5sL0ha3,AdiOdeas,ramndaSuiloaraptets ybSnVphPeeaictigsaoemse1Srs4y0b120 Coreornra s,ise ReSr geaanr 208 Paoats Fr irenmeet say as 2 om conven p07 Jas fon an `orc`sfaahlsietnotgnctoaoonhmsftonecraueubsdctrabtatahceiecouecnrrxaacccdyluirebvesdqpr.uiiaTrthcteuismrosewvenniG.tlosNbsosoofnnm+toe2prode%rt1haaatnhne2do:5roa3%ww0oda%oftntafch.oeirgtAhhaellLeLemvOxeQlas)c.ttiheaodJtfumcmasalptioyabinrntuaetotseniwdofinmlo0rbbes I`ndtseatnideeddt0oa8cphipoyv1eamnidacoucruvresptooicnutrsvce nn.theconcanason rangeof hesamples, rater, 1s 104ConCotnitgicnaulibnragtoCnavleirbfrcaatiionosn(VCeCrVi)faircatainoalnyz(eCdCfoVv)eryth accuracyofhecalbration hmcuoreCi.abArnaonitfvonzonieceravemomri,sdfarmaaupnmlgeemsiceta.uraCatalofbnrrasatovanenrvdyaetrrdof,cnoaniseoaonmfplhjeoe,scniaoomntsenmsutuasnntdbgaersdwsvitesiondB2a5rc%kosn,0sbtisuncta Caocncseipdtaebrleedsaacmcpelpetsa.blNeu.iTihpolceCalCbVraleovnels mvaeyabnodtuhseda.!passingCCVwil then bracket 105 Systom Suitability ' Aoumnai,rnptirhieor moiolefetvaehnloasolsfyystsihtseoecfmabhsrteaactboointcruarvaomnpaciurersvreav:piTeybpaielcdajlncetcetthdieosnastShoaemmbpelogenissnriaunetgoosofaaemcpaolcnehcraevnniaty.aiicoTanhle oyfs2% ulbaecompnljioacnitonsmusthave roacourtsWhanRSDof5% a areentontimeRD. 11_Procedures 114 Extraction Scheme Thafolowingslop represent atypicalextraction scheme.Sampleexavocuetsaond nal elton voumesmaybeadjusted 0meet ataQualtyojectves. `lsoamwpslaebmoptlee.s to eqstrae 0oom emperatre,Thoroughly ixsamplesbygendyinvert he Mcoaosnurgo at4ub0ensL(rSpoirkeetseenlatbaemaatuicspoifktehsae 8erkequeredd',saremppllaecreiodaanSdmOiLxpwoeyp.roAplyeemantee Vfoolauhmexsrmaacyhobnesuasneddddoecpuenmdeinntgoonnhteesa6cmopaeopfrotpesphreoejetct.Use 8consilentsamplevome A`sGoSdi4u0mptLhoiofs2ut5a0tmesiomoinsoadddedtofsaukleramtastesscamipolne ov4o0lumm.eosfasraomupsleed.. AThodhreoasmmuoiuxgnsttahomplflye. `(Noyouitice:abl*eySsaapmpippklreeodsrismmtamatyoenoye0te.hde1n00obn1ee0 pmrveeeslsc,trlhooeewnsieadnmgpiolfodecttohenercmiiennneetpaaentrnoap)prp.ireoAspsrtiiaketerlmeaavelttlhisoebpsveakeemkpelilvneyeeslied. m`i`ConniCdimtuiOomun)LntfhoeAilyoG.w1fe8idcbSoPyEapcparroGixodeisgmeartnel(y1hS,yGaeimc.o)nadbiyiapomansi.sniSnugPmaE)pcpArSaoTmMerlTsypyctea1n|n0wrometLtbmsia.eotDvdheoarnngcodot(neeadt:oansed Lhomeacdaatrthreinhadgnaeav,iloybtsiekcceaalnsiltaohmaepddelade.roiDtidosctohfreodCm1ut8ahSteePV.EaOccpuareutnmimcagnaed.wnOandtosvutavhaeeselnatsnradempspuallmelspoalvneahchauesuvlmaoocaunduehmdooro `SPEcaticgesforapprormately3mirdesfo emo rescualwat fomthSPE carte chaEnetresfcwuvtgeehntewbxiealsclt.ayTv5hemitsihieoSfthP1eE00ac%romgueltnehh.aunoTonlea.wCciolloennc(ttianuafsltcvotuthmoCeagarcpadpcaruoixaoienmdsat1e5almyn.y4pw5oamoy.psayi6nlcneeonhtsolof DePdoamisnaotEixotnraoctfiPonetaunodrHnaoihedPeAEcriTmdSsa,0nc.co1e5hL4ou3,dAmCidreas,ramndaSulfoongatresaipnSWphaPotycaetMrgobaemyes1eSsy5o.t20 MCorEtsurnonnannReoann1o2 n1009 Page02a 145 p.108 Gacurert may be uss + i le 14 08,8 on BLED conroenTa. `cSamulusrteoonvvorkeautmeesdn)e,edNsotte:obtehuessekifnorvaosmamepmleas,ycbaolabfaotroen sftoamnedaertdpsr,oajencdtGnCoasacm.pTlhees. Intrspers hemethodbarksfcughoutthe exvactonbach "Transtrwelmedahauosofhetna extract 1 beled util. fitz oreofbo rt tnaconhr ig gat Scio HPLCHSINS NFointa:lVSoalm=p6lems ar concertedby actorofeight ing th esrachon; it Voi =40mL > 11.2`SetSuapampnleaAlsnaamylpylsseiqisuesue.Method lrksmu: stbenerspersedtvcughout heanayical sequence. InIfnescitmtheensta(mursevsoskoanmeo(nb-esttwuemeen5n-ts2a5m1p)loefdeaocnhsstadnodeorr,)an.alytesampleendbark nothe Anlalsaemxpaictefsaadec1 wriotdhucinaccooatpottaoienra>uUlLO(GogisotobroMiStrdencdeorvetase.rorgi6inhaeolnasomfph)lee andrea ho"; * 12 Data Analysis and Calculations STahmerclheveoxmtartaoctqsruaspitnygatnhaelyestabsloisaherdcdaRlbryapbiocnaCluvcaek.uatshe amountoftargetnal nthe Cauat thepercentrecovery ofthLCS singhefowingecuaton LCSHo--rrLoS--eCeocmcoenvoiieB((no8L3rn))y10s0% alotthepercent recovery of iFSCS sig heflow equation: FSCstrCesoTvery n kEESrCoonk tneneti(2r2o58n)) 005s `Cacuattheprcentrecovery ofheFMSusing he folowingequation: FMS recovery = Fr MSCone centrp uon () 2).AverageConcenratonofSampl/Semple Duplicaa te (2&) oom. SpikeConcenra(t"noL5n : DetePrhmaisneatExitornacotfiPoontunodriHniagthePdeAErcfcTosm,Sa8nc.co1en5Ls4u3,dAmCidhoso, amndatSuoongertoaspISnhpWPeyecaeMigroabemyse1Ses6oy.i0120 MCorEt7s01G4r:oim mRaSpeb1e2r208 Page 1030145 p.108 Document may be vies. went or 14 Gays fom CLTHOIC coven 13 Method Performance PorAfoytfmcetdtaohtaao.ddNcpohnrocomasaoesrnm0caerppcoaerra1mheeatdneayrstsptoaotfaerdepnacracmeeevresdmumsutstbebdceosncsoideedrasnddtishcuasvsaeladtfiohne . o`ncStnaahletyssatypsrtotpeedmcatinneaddh.issammDpelteohsorceeanraulmyaazmcenkdo,cneosefscn0eitcetorrnaoaacwroGenlano.ttamkeen,am8aldreelneamnionaedmbayyhbespero fcooittnooterdoonblotrioespeerndeddwohcuesnspordonmahnceexroefhaorhaevpetctbeen me,the datamust be 134 System Suitability - PuaAvnmeeTahreesacosofautmnrpelweeistyharasnrRuSnupDrtoioafr5t5%oshaamncpalaersosvloilnabcnourfve.caTRheSaasDyohtfee5bm2gs%iura0ibbniegtcyoofminpefaaecrchttso.nasmtuast! 13.2 Quantitation GCraoelnlsorstanotrtiaoatnonnoCwuairtqvheu:haTe1he0xcc9oeep0ftf0iiocnEiaeoncfttohfhpadiLenLeOmnGi,nhWahdiGocnvhem()ayuvbosletwbieotWr 1i0$n3c0a%2l.l5v%aotfnthcurhvcermeutstcbao `ADsimonns3i7r6atoifosntaonfdSarpde)acnidf2y:mSpaescispecisderm9on0sntrsaetoefd ubryicchroomnast.ographic retain ma 133 Sensitivity : `SDSaotmlpvolefenhstBloaconaiktbsraasnttodannMsdatatarhdnudoadsrBddlanmnakhys:hcaSavolovboantotoarecnoudurmneet.tshrSoaodtbleernnthbalanaan5k0sc%aonouraftlshzeeudlsoatwbecseti<ga5hn0de%avrel SoammpneGtCumseanntpclamdyemoornesatsroantghalsisuobesemqueentnscchaeydovaerriisadncarloyazeednbgobarcek 11enxepexctted Liomaviact.aoflQuianctuiravtei;ohnep(LeOaGk:erTehsefowoerLLLOOQQ(mLuLsOQ3) .heelsotwe2sXtnrantozfehoeacmtiaveosdtabnrdka(rsd)i,n Bycaiaton, themeasure valuecf2LLOQ us bewih30% fh oralvas. 134 Accuracy CoVParormance:Cobra vefcaoninecionsmus bowitin26% oboconsidered `cV`caiecpckelpatitabCilCe.aVTnhveoeclavlembrrayaytboanetcuhusrevem.eLaniCdoStdhriescoa1vsetorpiaresslssehodonCuaCdgbVeovnwlidtiaihyne.2br8a%ckeotbaecccoenpslaibdlerseadmples. LaibbCon0t-r1o2l0S%pakneds:hTehpeoarvoeorntaegearveceovseray rfhaedpeocveidnLCfSheorreceoavecrhiteasrgetsatn blesshhoaunobre equato20%- : 135RneprPoradeucociifysbsilamotpynsl:esR.eprAoRcuPcDiiatryRSofDhoaf m52t0h%odwisl dbeefcionnesdbidyetrheedraocuclpsloaf dupolrcraopolocratlplcato 5c5oViarlabsipthyes. Bhoeceaxuysascftoknsparmopclee)p,RlFeDoraRccSoDuyntaokr vsamraaybbisy H1isgahmspieRloecatpohneo(R2PrwOetOlr PeatsaeExmtracoiftiPoennartnuadorHntahiePdoeAErcnTocms,a8An1coe5nL4ou3,dAmiCdheso,arnmdSaoongersapinShpVeycPeMtaogamBoyseS1ns7yo0k/20 Cot0o7n.0G10o, mmarneRaBpearer2508 FreTor nte Bo ent may be Le tL Le Tt oe conan p.110 bn CHL fRoSlDdmoaftsasmeplreeccupoivcaetorssaarn,yd.discussin hereport fgreeterthan20% and he mpecton 13.6 Analytical Method Uncertainty/ Data Acceptability `Ac`aunprparaoycaycahaumnsodetshphroiosdctoiursnioccnea,rlbtaaLisGnSeddaoltnaaypbtrhoecledsedfuironeresdtadeonfcdihrnreeipdeoidrntaEenTdSdi-n1sn2.so0eo1df2.wfoIonewEvaTaySas-.t12eT.mh0e1e2tf,hirosdt detaled `e`nsCtdoimmApantoiauoynnodssfbtoyfnHcPioegrrahuioPnroyirnmlaeimooasdnuAcrcoesmLi,eqnAutiosdwnCeos,vpAoemkimdoeamse,ldSooufngoErTraSe-a5sS.app2n3eyd1c.oMo2tm,aheSrtsoyFls"ud.oPdThaahtsespdErxotceadcutroen `uaEciTcSne5pet.da2bi3ln1e21.psIrmneohtachtetovidakzeueeastmtoihnenswgaaamsnaettypetrrkoamplairnmaeeidtotnhhoodnudnhceaenrastlaeyisnoitfsysc.tAoerlptisaoacsshtaowtessrewtdsedananiaepdorts are `oeciunreedawsh2extuhsisniganidsamrdedtehvoidsfboordoefttehrempienricngeanntarleyctoivcearliuensceorfttahientpyo.oTehdem8ebtohondocapidkaes. fs `dWehtoiremaiiLngCShdoomtapooidntusrrceercaonnttryo.lcharted, nly themostreceTntFydtaposare sedfor `aWnhdeFnMfeSsGs ChadneltwoemnitnyeLtChSeddaataapaocicnetptshabaivteyb. oIofnFgMeSnsermaetee!dtfheo a 3g0i%verneacnovaer,yrtheebaaktchaLeCvSel aurnepccpeorrvoteparriyinacttyeeortfoatthh,eeadneandtdahoiisgstedonreioecuamlseFedMvaSec,dcaounrtadattdehofeeoLswnCioStnmexe1ie0s!0tt:hh2ee0%$a.n2a0l%FircMeaScoduvneorcnyarottaemirney,esthhveean3lh0ei%don case-by-casebasisand a cussion incudedin he alanalyalreport 14 Pollution Prevention and Waste Management P`eSatmpeleweaxstrtacftswdassctaeradneddfIlnabmrmoakbelnegslaasvsceontiasidniesrcsardceadteidn iinghthBeTlaUbcoornattaoirnye.rs,andglass 15 Records i} Etarhceofhcodloalwntianspgaicnekmacogsfte:gsbheotindeetyrtyaoatr.eIpdnrfooojrremcaatsthniuuomdnbfemorut,shSetdpInocetkauadpenoacdlkSastugapenpmdauarrstdtnrgneicnpufSdoheme,aebttiusotrnescfoonrrds, ted10 iinnsseertt ruensfuos (fisesu, cmehrrbotmchactorcodaslg,iarntsoaRnamnesvnet,asc,aaunidsiGoonamceiahkoadt,sonusmarypage). 16 Attachments None. 17 References "sFMlueafthoehnroyyda.moSifcAcen(aPyNFsuOsmSbfAeorr,t0ah2en3D-de0tP0e2re,mirnGaetuiioosnoArrfaPoleyftou(aoPlcrOLoAaaAobo)cnraahntncooWrsaiatueebsrt,n"e,entEcs.S(WaPvtFeOeS)Cr,oelPeesgueoi,ranonondc.eiane Penryn, encery2000. urEG1a-0t45e4:(PVaFlOiSd)a,tPioanrfpoorrotfoocithne"slMleotrhyoldaomfidAen(sPyFsOsSAfo)r,tahneDdePfoefrumoinraotaocniaonfcPaetret(iPcOroAoRc)iiamne DPetaersmionaEtxitornacotiPonearnudoHiiegthePdoArEcfTsom,SaAn8oc1en5Lo4i,3dAiCdehsr,oamndaStufoogatroasIpnShpWeyPaca/eigrrMoeaBmyes1St8soy0k1a20 CEor7s0on1G0.o mimmopaeca na52 :2000 Page 10st 145 pot Pozument may te used, icuranl, for 14 days from 020031201 CONFIOENTAL `LWatear,Eb.Woinkcsr,eStmaaetesiCioalnlnoehdgeJer,.PFeanehnerstysyv,anS,itau.dy Number023-002,Centre Anaiytal 18_AffectedDocuments None. 19_Revisions Revision `Num1ber Updotahenteweformdat. Ch`aSnugmemdaTrhyoe.fChanges :. t`hSaecttsinono1o:Sntgaotresaptphleivcaabllied.ationof3 analytes, omoiesreference fo EPAdocument `tSheocutsioono2:faPrLoCv/iMdSedsfyosrttehme,enxottraocntlioyntohfemLoSroMSthMaSn pthreev3ivoaulisdlaytmeednatrioineeds., aows m``eSSeetcchttiiooodnn53b::laRRnekov,wio8srnedddodMdefDihLno.itIinotnesrffoerrefniceelsd,m8a0rd|iesdpirkeec,ommeledndcaotniroon s(p0iukes,oLdLisOpQo.sable `pSiepcettitoens6. : Section7: Re-caleagnodprariedzdoewdn. Changedstorage time {o 6months. Addedmoro calibproiantts(i0othne `aSebclt.ion8:Addedstatement adtsssinglabelingrequirementsandspiking. p`rSooccetdiuorn9o:sN.aEwxSpeacntdieodnsoction 8.8. `Section 10: Changedsomeofthe parametersinthe table. Alloforwuseeodf efxtreonsnitveilnystrrouvmiesnetda.tion. Addedinformation fomsection12ofprevious version, V`Soelcutimoen o1f1el(sueacltiions 59minL,prreevviiosuesdvsetrasnidoanr)d:izCaltairofnicpartoiconeossf,wraesmhovtoepd,rsetqautierdeemxeanctt(0 us`eSLeOc1M2St(MsiSoc.olonn Sec1t3i(seoclnon 1143innpproevviioouussvveerrssiioonn)::nEocxhtanegness irevwerilteyn. ``rSSeoeccqttuiiioornne1me15n4t((ssss.eccltiioonn 1156innpprreovviioouussvveerrssiioonn))::Mniocnohracnghesantorgecoerdisng `SSeceticon1t176(is(saecocttinioonn 1178iinnpprroovviioouussvveerrssiioonn))::RReemmoovveeddartoofcorhomnecnot(,o EPA document 2 t`hatSnoel1o8cn:gNetreawpipsieociteidnotno this Sectio1n: Added emphasis SOF. thatthemethod is 8performance-bmeatsheodd. `SAdedcetdisot2na:tRomeemnotvtheadsttheitsommeetnhtotdhdetossamnpoltecsoavreorsshamipelodcoclolldecatsiohnis nolonger tSthheeaptcrotatichote3inr.ceexM.tirRnaeocmtrioeovneaddndrelfsuerteon/ncveoctlou[sompseoaecsivmfeirarcaylCb1fde8efuSiscPnelEdioc.naasr.tArtidddgeei.dsAudordoegdnasltaealsonmdent `SPEcartarsiadefdinigtieonE.TRSe.m8o1v5e4dr3oforoncos(0LOD and MOLPasatgheis 190120 DelPahmainsaetEixornaocftoPneraunordinHailgehPdeArcfiodrsm,aAnccoenLoisq,iAdmCihdreosm,aatnodgrSaufpohnyMataosssInSWpaetcetrrobmyeStroyld Corso07n.C01r4o8m rnRaCgeonc8o2 a 200 Page 10801148 meal May ba sa come p.112 Tn G1 cag om GAN la`bSoercattioo6rny.dAoedsdendotfreorpoerntceLCoDaauntdolmoartMeDdLSPvEalwuoersk.steton 0`oSxeamcptlso.7n. Addedaddtional analytes andupdatedstandardproperation `ESnavcitrioonn8m.enRtaelmLoavbepdevresrobineeglettyhpaiclaplerdtaoinnoedflcooslacmtpslaemcopllleecst.iAonddarsetshseedIsHample Sboactttlieopnr5o.paCrhsatning.edmethodblankcrlorie,LMS and FMSacceptance criteriafrom 1d`0Se0et2cet2ri5mo5in%n1e0a.0cUc1pe0dp0at2at3ne0cd%ea,.ilanexdaLmCplSecriintsrtirauwmheentrceopnodiotlieodnrsfecoorvSecriieesxianrseturusmeedntfaotion = raocmtoivoen1d1M.icCrloamroisosdreefxetrraecntcieonsprocedurs =removedinclusion of 840% methanol w`aSeschtisolno12p.. Minoredt. p`Socetiorn 13f. Acodrdtreerdasmaoscatsopnpnoronpcrdieeeteer.mination ofanalytical ncertanty andchanged 3 Section 11.1. Addeduseofsodium thiosuato Deta`rPmhiansaetEixotrnaocftioPn eandrHitghuPeAorEcifTdroSsm.,ai8Anl.ccn1oehL5oail4su3,itAdmCaiidvedosm,aatnodgSrapuhyMfasnsISnpWaPeatcaeitgrobmeeyo2tS0yos0r1c20 MCorto0n7.G0o1:morrsmaRaOgnoca2ner2000 Page 10701145 p13 Document may be Led, current for 14 days from (203/201 r-- 3M Environmental Laboratory Method MethodofAnalysis for the DeterminationofPerfiuorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis Method Number: ETS-8-044.0 Adoption Date: Upon Signing, Effective Date: 04/12 [0] Approved By: PE Willa K. Ragen. Loboralos Manager taDfatee MethodofAnalysis forte DeterminCationocofiEPGerrrrBsnfsoR0nbniEael0ReDdAuCormprou5n0c0sinWaterPabgyeL1A01S11SPr: Dtiroectns Soret nay be coneroenTL p14 nS eran ka 14at Pom LOM 1_Scope and Application "PPTeirfsmueoertorhnoondfasnotiubcAeccosdde((drFPNHoAAoq))u.,ePnPheterlrfytuPeuoeorororrodoeebpcuatanatcnaionncccAAiccddAc((iiPPdFFDH(AOcP)AF,)B.PAe.PrPfeeurorfrouoruoonpdreeroctaaannccciAiiAcdGAad(nGF(cOP(RiFP)UFcR,PAe))., P`MaeinrsdfPuseoSrrpfeoucdotorrdooeomcdeaitnsrcniieccsDAuelctoedncet(toPsrF((DLFodCO)MS.SP)IebMrfySuH)ciirgnohcbPlueetaarnnwosamsluaolnroscnaaomtLpol(ieFsdB,SCW)ha,itoPmeetrsouagomrrpaolphehseysccaoonnustpsaluieondngaohteaea(fvPayFnHdSo)m, PpBeaerrrftfoisrcomudalnenamctaeeLdyAirqcuesdc,CioAvlpocrmooehptoaolrg,arAtamopindhbeyys/a,MnaaasnsdbSSpaueltcoierramoimeeettshyIo'nd.WsaulcehBaysESTcSk-d3P*-h1a5s4e"EDxettrearcmtiinoantiaonn dofHgh "ToisemetO hodsa considaere aspaogrormaonr cepera-pmeestheocd.Dat isconsideredaccept5 angbssle `Samp callecionlsnotcoveredunder isnatal procedure. 2 Method Summary CpSlhaeoaurnacbqaeucemeoanuytssnaomtpbleperssiolararfeobarsneafmlooryvaiznnegadlbayyssasmbrpyeltchteirasjimeaecuttoohn,ouods.nSeagrmLpelC.eMsScAoVntSa.iSnainmgplseusspceonndteadipianrgihueiaavtye ITaahcbiorsraiasotyaoypfoeorrretfaroclhrssmpaiamkpnelsceaebt-memdbueeatttseheroemcddio.nnMceeednuttshriaontdgioancskc.udrTamhcaiybsmixsesdpteihtkoeerdsmiiosnvoeedorolUryeFtahcahtstheaamtmpheletepshreoctduisssisonpnglucsantdipe to ``Xepacahnsdamplscecmuartaicy.sSltaammpelnetrse),suorswfiolrsnptibkeosroeuptosritdeeddof7e0%1ntoon1-3c0o%m;pkmaanytbqeuflatygcgoendtr6ossuacmhp(leWs.h eFanodrotcgceantcoofnuosurelavenvreaesllfayaontrdefclrieeesdssymutash,tatn s10pSkmeessanhdefeonrlcaiboogreantooruysmeaveiltosbpeieUsssedh1o0uddebtoatilansteht s0a%teofmtehnetof 3Defntons 3.1 Calibration Standard Asolfonpreparedbysping knownvokume of theWorking Standard(WS) no peceterined `mcaoemntocuhenontdiorCfaaAolnSb.TraMtToynpseta|n.dHaPrLdsagrorasdewdattoe,Caolbortahte tsheunasruvamteen,raensdpoannsaelwyizehdraecscpoercdti0nganatlhfitse 3.2 Laboratory Duplicate Sample (LDS, or Lab Dup) Alaborstry upicatosample i separa aauotof sampl akeninthe nal aborstrytats `pamnaerlaysezuerdsesoeepfaortrrhsestvpclrryeaawciigtsteihpoirnonaocseisdcnouacrie,aspt.oecdowdiuhrelsa,bAonraleyrspirsoocfedLuOrSeSsc,obrutpnaortedwi1hhsaamtpolftehceoflesctksokn,u Give 3.3 Field Blank (FB)Trip Blank aApnSdTrrMiTeyspaes8IaaenHdsParLaCmapnvglaraleadynecowaaitltperreiros,cpeeoodcruttrshne,eisnr.csuTudhiitneagpblueerwxpapotoseseorflt1ahsceeaFdmBpili1nsgadmieptiaeccoinodnnittaiifonfneso,srtHnsotu@hbegstelaa,nbocreastoorry `ner ereroncos ar presentnthefieldenvionment.Thssampleisalso ofored10.8 a TrpBlanc. MethodofAnalysisfor theDeterminationofE"jPToecStriu8oon0rAi4nn4aalt0yesdisCompoinuWantPedrabsgyoL2C0MS1M1S; Direct aMCoocrorsGtesrmeraReCvpoocoe2 2e009 Page1080115 p15 Document may be used curren, for 14 daysfrom GIUSEIC coneoenTAL 3.4 Field Duplicate Sample (FDS, Field Dup) hAparsoncademedupdruencs.odlelArendcatleeyndsiiinsadolufopfrieccuaFtmDestSatactnohcemespsaaarmneeddvemoatelhfeadoeomfxttahhceesftahtmesseaakmmopcelateighooinue8gsshhoaeumsteaafmsiuplrlaen.odTftlhhaeebpcFrrOelcSairissyion ssocitedwi samplecollection, presenvatonandstorage, 38wel 8wih aboraoryprocedures. 3.5 Field Matrix Spike (FMS) bseAafsmoaprmlptelhmeeutbsootwtbtioecshadrdkonsdoew0ntqtuheatsnhaetmfpielloedfcfoornitecatoialnreegcerttwoainnhoaolfuyatqesunaeerogeus.asdTadmhepidlmeosat.yeAbseKaanmocpwlcne,bsoptmecpniiltcbviyeomskaabmhkoeiorenafgid&ry "oipkflpaalrinoohatiolmoystadettechevoalnetycr5aes0in%preakoatonnnahts e1a0naGumpuroipksdnretoowhonefp,emrhxepauseiclaiomeeJlpdssmaapacnivdokaeneei.aseiocTnfoshvnreac.FeyTniMhtgSrolaiFetsviMaeonSlnassnmlhyhyozeeubsddaotbmpepalrseecpp.eiarretfeadhdibnefeofetaxwnpneceyrecmonteasetedirxhaenge fects,intrfrences,orstabiyissuesmayccmplcateth rdoprotakonofhesampleanaly. 3.6ATnri8p BklaoqnfkAuSSpTiMokTeypt(eF|i.elLd CSpgirakdeewCaotnet,roolotShaempsulieta,blFeWSaCteS,)10whichknownquant ofte {eWaxhrtegrteahtcetraendaaalynstdessaoanfraaolnayadzledydedecxiaoncuthldyeblkeaebaotartsauttuoidneydsacormhapoldtihnteghsiepmlempd,esenattemompfilneneeicotorhloeegmceeaitnohdnoodrtiesssh1i.cpTmohenneitrFlsaSunCedSsi.s A lleoawsatncdroisgehpFaSrCaS,aurr-e+appipkreodpsraimstpelwehmeunsetxbpoetcaikoednsaamtphleescaonmcoeriimroaiaonndsaprlaocneatskanocwhnFoHfSm.ayvary. AL 37Laboratory Control Sample(LCS) Aceanltabmruaetocofnocfsucaromvnpeteloeneldxmotaonctetnostneo.rwAtihlcehemakdnto0wwonulpeqpvueearlnstaianrgeonofcfkttuhhdeeeeud,vroeene.agTneahlnyeetreLsaClaSestaatdoedeeodwtnenred loscfanbhdoetarnsaoelryzadted ``axchcdaykse aalabomraatpoorylesxtaermapcltseed.fo deteminewhetherthe mehodisincontol.LCSsshboepruepadred 3.8 Laboratory Matrix Spike (LMS) imnltaabhboeerlacatbooorrrayrtmoaertys.riTbxhisespLfkoIiShsaeinaananakalqylutyiozctealdoferxeasscuatsmy,pTklheetaoewanhbdioocrhgaektnnrcoyuwssnacmapuolaennifosdeoestoeefrmatifrnerttwaohnaaeatlntyhateeerosshreniesnaasdmhodpelde f`osramhpelsemsactorniaxemnuisratiboendse.LleImSiSnaedrienGptsneaplaroersaonqaluyositsoonfdaqhueeoMuesassuarnepdiveasl.ues intheLMS camecied 3.9 Laboratory Sample Aportiono auof asamplereceivedfom th fledfortesting. 3.40 LiofQmuantiitattion (LOG) T`ushiaemnpllaoywteceradtmwirtieopnofrtutihanengsi,ptehaetcoLinLe(OLkRLiiOtsGsg)eofnfoerprraaedclaitssialoseneactniidedahcaescutrwhaecslytowcuoteniscntegnnotornautzeinonotspaaerntadtcaiarnngdbcnotnrdhoietlciaaobnbsay.tiToon unothatmetsmooclarda. SampleLLOGSarematsSopandert TPuhiaheneiusptptaostraenidwdiiattriodnfiqtuhahenestpciteaalctttiroeand(toUmnLicOtusQro)vffoptrraeactimsteiaeontsasenmidesatchhceoudrhaicgcehyredsiutarcioninsgccreeonutfrteaitndieo2nospteharaetticLnagOnbcGoe.nrdlioinesb.yThe Math ofAnsfyo tshe DtomiofEnPToSra8t0uo4r4an0td Compound i WPaobgyoLOt 3M01SH1r1MS; Dec SMCarbcoonlGd n roe Dmnconete2r000 Page 11001145 Gomer copy a eid Fern, Fi comer p.116 Gusds STN 311GaAsnMaoewutarhcso,odsfqBculpomaecnnmkt,asoxarts,sanedsrteeadgeexnatcst)thBahorsaulsabeodritrysoaemrpabnourlnrygSeaxrpeoseu,rTeheomlethad leanknouistohodfensa8gmaomtns,aforsh!nosudbotsptRarn,caess.orovrrererencos re present the aborstry 342 "A Sample samp ia ntbl re m o v ed o m' gerquantofmeri nln" rprese the rightsource 343 StockStandardSolution(688) - a "Aconcentrated sonof 8singe-analieprepared in ihelaboratorywit ansssayed reference 344 Surrogate toe CCoAoocnrarimlau pnosnuanean dcsnssasa,cmrd csSuiTc)noagbcheyesemsbeiue)coaegldreectsaoemcpodnomspotoaucandduussepafdi,aalsluvrvortgareesgeesta)ratrgnhoaaarndidaweeidshaJn)aoat,llobecusaelttasoplrvreaotscsraotonocmmrdasqluyay Qeerliyngosnamlpmleeacsoulreeciaonnd,pireNpOerTatriooncuarneda: na.1CLSnof8suoihgele nae 3an ptnsl 345 WorkingStandard(WS) !: CAasb0rtaitoonnosftsaenvdearradlsanaanlyoteesrpreeprareeddinantahellyabooraktotry.fr.o.mSSSs+and.died 8sneededtoprepare 4_ WarnanidCnautgiosns om 41PToHwheoeavalectruh,teas0nncddhscShharofouneidtcabyecetsioefd5he8s&tapnodtaerds fHoea8 nmaeztahr .Thahveeannoatlbyeesnheoicuidswleystdetveasi,neadi:a Gos,andsfey he abrstori asses10prevent exposure responsiblefotmassing 1hic sof work ayiiaotmnimgohnttboapnrdesceuntter awareness of cal. TouaiaSbhoonessr(eHgaSi)nsthhahanbdinvgeadfabl ochesmipcaelrssuosneelnnoivsemeinlrd.sAanfeareensc.e leofmotelsey 4.21C"0Tah,ua1at6niauoltynesstomfSusVtbE,fampirlearsettzheedlgaabsoa}ranteovesrqtpnmeesn,tagnhdptoalgenet,aahnadzvaarcdsnuynsgi,sb.tRerfeirteodo appropriatesqupmentprooadur ofoparstor manualforatonal omatonandcautons 5 Interferences Lo oOudatviomnargarsseao,rAfpIisonmparaoprabsaty3o0nvdain n1agn1raeyashinosa,dmeBoasrrk$spdobteadlomcoornteaymaiineadnttosoousrcFeosear1ormeageednetrseanncdesunder MethodofAnalystsfo theDetentionoEfTPesfu8or0inua0lsd CompoundsinWaterPbay LgCoeMfS1sI1V;Direct Mento Govnar n aSponen o 808 Pre rors p17 Document may be used. if rent, for 14 days from 0200372610 coe Pcoiarptnes,amtnodedasrualpncpfdollpoeer,creHonPtteLacmoCninpntaaactirinoesnT.otTcnh.essehmoauydibneclaudve,beutoarrmeinontiizmeitdeddtuoe:wtahsahpbootsiieis,tTyeofifon ined TchoeorusseofsdiaspnosaabledmicaropeisStoeskeosp.iates aolstandard soon recommendedfo ake 6 _ Instrumentation, Supplies, and Equipment 6.1 Instrumentation and Equipment . VAarhiiagbhlpeevroflourmmeainjceectqouricdacpharbolmeaotfoignrjaepcthicnag5p-a1b0l0eofpcuomnpniencgteudptotoattwaonsdoelmveMnatssasnSdpeeqcutirpopmeeddewrith a Acvmistmasl)b.lan|ca capabe olreading 1000001 * Adevistocolectraw atafor peek integrationand quandtatcn 15m andSOLdisposablepopropyinsceiigs bss. GfaisnktipgahtssysriHnPgeLsC,a2u6t4o,5014, 100uL.,250uL,500L. ,10004L. Disposablo pets, poypropytensor ass 2propriety Centrifugecapableofspinning 15-mLandS0-mLpolypropylenetubesat3000 rpm. 6.2 Chromatographic System GuardColom Prism RP,48mm x50mm, Sp Ansyica Column:Betas C10, 48mm x 100mm, 5 om MToebmipePrhaatsee:(A1)0:2CmMAmmoAcentatieiuWatmer MoblePh(8a):Msehaenct Grdert Program: [ome | wa [we [Tm] CCoomsoSoT T -- sTSr & w -- 5s--T T--7t0o] Commoe--T To w 5T 1110 10]] rQeuacnotnatoVn:omPe:ak1A0re0.~cua avei. weighed. Run Time:~17mines. pTrhoveipdreedvihouas idnoftoramqaatliotny ibijnotceinvdeesdarasemogtu.ide; atmateconions adequipmentmaybeused Mothod ofAnalysisfrtheDeterminationoiEfreTPcosif8uoo.nrA0ir4na0atdiCompoundsinWatePrabgyoLsOoMfS1M1S;Direct CotcoorniGmoe mASaeeannpr1900 Pre izanes p.118 Daze may be sed, eur 1514 Gage fo SOHPO1Y conan 6.3 MS/MS System 631 Mode: BoctospoyNegatveon,MRMmode,monn he lowingYaris: [[ I p-- p r. eA a---- Sussmrrms2w8d3a5s2m1i8 i-- aiie|| [[[PPPFFFOAAA1d9#61333819,s49o8n31.4613.2t41o000aaa3nnnaaa 413693 521076000 [P[FPOFAOGTA81536613305dt1eho90.,,565611333 -f2e21600gaaennadn5s6td33e>t23161a900 [[Pprro>ss--| |Swoo-28m600,84o906 m0909ms2na0a>0800w51a30w_|_| WQiuinacnrieltaasterdoasnnoeaifinosnossm.eorsTFhhooautntmtoeooregfCol1noaesaealryuigmeahtisceh1oesnoNniaMspaRcndc.aapaaiaabnerd mimaneynghomadvuestleneenadsdnesedibboaencnshmitavoeyfprovide Providedhe etnton imecra roMat10 8s8roadequate spec. Theprov fommasonis tend as agi,ame sinnersandequprmentmybeusc 7_ Reagents and Standards . 7.4 Chemicals, Wotor Mi,HPL rade,o oerstablyapprosporreis AMmemtoenniduimHAcPeLtCagtrea-deACS ReagentGrade ve 7.2PoSrttacnrdoabrudtasnccAc (FEA -C4sc);OakwoodProducts, nc i PoProreoperrtatnducAAccc((PPFrFHPAe-oAC~8Ch5aacek);,OaraoioaondoPwnoc3sdusNE,cPIA,:nonshorsperandcac AleAsso PortucrcheptanicActPFHpA - G700d,asina8TOHA, daca roneptanoi ac,Oskvood PPePorrocrutssu,uIencAorAdcdorP(oPFFcOcNAAt~nCCaB9oan3cdi)ln;cOaaclacnaadPcrnoceidss,coc PPoaerrrttfouAurccAAccdiar(ddP(F(rPuoDPFAFU-OondCA1--da0dCCa11o12cdeaa;ccecO])s;OaOcoaaokknadwwooPooornddoPPirrcsoo,dducuiicctn,,:cIinnc:. PPPoorrttourccrhooecbstu(a(aFPanEEnHSnaeS---sssCCuuu48ssttttooonrnnnasataat)t)tt;eSssM MethPodoorftAnsuiyesirsfoorteDe(tPeFrmOiSnatCio8nsuoftoPaeEtfeTu;osr8na0t1ed4C0 ompinWaetrubynLPCagMdeSgMosSl:11Direc ction SMCocoosoGn mreenGoeanna r208 Faeries p19 ! Frame may oe red Con Br tes fon LONI conFoenTAL "uTsheedp.revious information is intendedas aguide. Reagentsandstandards romatematesources maybe 7.3 Reagent Preparation 2watmer.Ammonikamacetatesoon(Analysis}--Weigh 0.39ofAmmeriumacetateanddissolve in 201ofreagent ole: Atamatvevolumesmaybsprepareda ong sth atsof hesolvent 0sceralcs re makrianed 7.4 Stock Standard Solution (SSS) and Working Standard Solution Preparation TcWhhhaeennfgoGelioduwttionnsggusstiaohncedkansreodlepudtriseopnoesfra0tpaipaopnrrtourpolrciresduurcao.svaeFsvoersoxeaampnle,xaLm.vpolel.uWmeeisgmhaedy:baemospuinktesanndofvaolkuvmoeliurmefsamsaksy.be p`1u1r02i05tpym).gLamDnPdtEakrbogdtettteoaona1rl0oyt0thmoe.8rws8iu8ihtsamboltWehecaionngtohaoionruecr.1hP0ermresgpoaufreaanassaoeSlpvaaenlnostt,tsisanonduaafr1od0n0cfmoor.rrveeoaclctuhemdnefoaepae.srkcE.expniTtrrsaatinitosnadn1ad0te8s apnrodcsetdourrea.geAconnedxitaimopnsloefosftpoucrktysaonodsnllschooeucdboenasgsvedbonloawcocraPnFcOeSW,eh boraorysander parsing on Ber =moloecceuclualrawrewiegihgthotfoafnsiaotn PROS (K*Jstcoacmtoa c322t0o.52n75 10mgCFESOK withpurty 90% =8.355CF S05(10mg0008275+6.35mg) H5apsmka.ndb(i60n0g0unpgt/omvoLlmuimxeewdiwhorskaivnge,standard--Add 0 Si.eachofhe 100pgin.SSSsfo a 10m.voumetic: 2v6o0lunmge/smL.fmlaisxkeadnwdorriknignUgpstavnodlaurmed--wAidhds1ol2v5enmtl. ofthe mi isedworkingsandardsolutionto. 25mL f1a2s6knangdb.rimnigxpedostvaonldumaerwdi--hAdsdob62e5r.4.of he pOLThsedworkingsandardsoon 0. 25m volumetric p`rSotcoerdaugreeCoonrdnitaioenfsi--gSeiaotroeraatl S4'S8S2sCaonrdwaomrakxiingmsutmrpdaerrdcsionfa6cmcoonrtdahncerwotmhlhesbaertaotrofysrteapnardaatriodnoperating MethodofAnayssfo theDetermination ofPerEtTuoSr.i8na.t0e4d4C0ompounds inWaterby PLCaMSgIoMefS17:1Direct nection SM CartCoonsroGnroememrtCocamon2008 Puan vastris p.120 Bucumant nay bo ueed cured for 14 ug bo 02030 conFioeNTAL 7.5 Calibration Stahdards bUosteihnaegcrustsuhkieaewbedlrfekowiamntogeorst,thuaseindngedthsaeduefesocllrtoiywbciebndjgoabcbotlvvee,s8ap5dr.de8prgaeurisedseealdilniei.tahNseogte:snVoeorkoupmrseojsneocAftSwcaTutMteirTeay.npCdewa|awakltienbrg,srHtPeaLavnedtsawraotdthsenmerr,aoyr then thoselistedbelowcanbeprepared83needed. Coolebrryse ctoAienssShouniynpsew,Wmeagrtme, [w[ m Tw e [ oom r [ To em ms 7] [ [ws mw = [ ofoaan m.s| i om om 7] [C Cmw[ Tw e [ . aowm} [[C mow eoT [1ow wwo[ | | = owwy[ T |e R om m] ] [ow Co w ow === T [7w om] 8 _ Sample Handling ca 8.1 WaterSamplePreparation `Tsamnetabhyoltdhiiyssamspeptiihcoasdb.leStaomcplelaenswcaotnetrasnaimpglwessp.eSnadmepdlpeasrcionctuaaitneinsghhoeuadvbyepcaernctifautgeepmoarytnootrbeemosvuifanbglae for `sample luo, orfered "Thorpourghelydmioxvsearmtphleubseefoofrer8emsoavuitnogvaianl,a1l0uproetvaenntdpahceipnogssiia loafbeflcexdopcahesmtiacuatosvcakli,nPgloaschisgass. Diesample, fnecessary, witASTMType|,HPLCwate, oroersulatiewater. Preparemethod QCsamples andmultiplemethodblanksandaliquot ntlabeledpast autovels. Proparo tlesstfivemethod banks. 9 Sample Analysis - LCIMSIMS ```Aswnoeafilwgyahzrteeet.dhTe1/hsxteoacrnauidnlawrreaidtgcihuotrnevcder,pvroeribosymtoaQeuyaacdnrhcaskteuidctfeolfu(sytas=mphaxlo'eus+.bnToxhte+bsect)f,aownredciaegrdhdttcherudoru1vg/ehxmOzafeuyrnobw.eeTipghohettmeeaddt,uhusesiminangtgisauctanalebmalerethod tsheordou1ghclaylcduosctuemtehntceadiibntrhaetoanwcudrevteas.houdbeappliedconsistant EYoughoutasay. Anychangeshoudbe H``aippgophriospasrnihdaotoeurtdoostwhsepoodbianettsaemxoacrlbyuobdceeadeuxscehlteuhrdeeyaddreiradocnomouttnhtmeseceaatrbtorhnaecpsroent-cdlueeratvseterstmwitioncpeerdohavacitcdoeefpttbhaeentcmeeerrthfetoaidv.eanrLdtoohrwaseraavnvegelerc.ubvaneks. pioiontcoisftihceiceunrtovfemGuesttembeiwnaionn(21)5v%aobfefhorettheeccrlebtrcaaltocnonccuernvteramtuiosntwbtehgtrhoeteoxrcehpatnioonroefquhael L0L0O.Q9,9w0.icEhacmhay Meotf Anahlysios fodrte OtarmoifPnerEatTuSio.r8oi.a0ne0d4C0ompoundsinWabytLPOaegMeABrSal;11Direct injection MCoicnosroGrmocnnDpn:cwarnra20r00 Parises p21 Diocament may be used. cirent for 14 cays fom GLIE00 cone bpoeiwsivnil2b3e0u%s,eJdusfobicoantsiionncfto heexccaslioorngtoofnccaurrvaet curvepointswil benotedntherwdeta. Aminimuofm8 ciurhveec(alntxeatocnceursvaensddoaresarnnaoyyz)ee.etacceptancecr,pro utemaintenanceorpropa anewsandard `amCfoienrrtaeinvuigrneygcfcoaarlbtarhtastoaonmnpsvlteea,nrndcoaatrtdn,ocnousnd(eonCfgCtsVec)easrnaetmabneaarlsktysazn,edwdar0hdvsuesrmeyidrt1ih0meuaCmocncosuftroucncyeophfeetrhaselacbmarplalbterosaneoc.nurcCvuear,lveta.lra@Amininanilmyuzame V(eCrOfVcwaitlotnhenjebcriaocnksemtuasctboeswpisanabmp2le6se%.oMbuecloensCiCdeVrleedvealcsomepaaytlbee.uTsheed.cabratoncurv andthelstpassing `Sa`mpulersecsonhtoauinibnegafnualtyhteers tuhtaetadarnsqduraenatniaallyezdeadb.ovetheCanosaoftheighest standardinthe 10_QualityControl 10 Data Quality Objectives hTLhoOirsamoeftd0ha.ot0a2da6anngddiefloc.oubAcnteydqGu1ealtviahtytcofonrnastforrloopmsatahmepqlueasldecsoingrneldmteogseneersatspdedeesdoaucctubreatleowtowil3b0o%dwoictuhmetnatregdetiend 102 Method Blanks MMmeoetithhhooddbbbllaaannnkkkss.mmAualsyatmbbeienprrueecmpta.erdmemedtwuhttohdebeaacmnhekassn,aablruyestainnsaolmeytozcrehed.ptArhtiaoenrg3sntijnesvcteirmoanemsetsnhhtocodabuladtbratkeosrn,emursotvrbeed0fp1roempaaarnseaidyn.sgse of `CCVsamples, andatihe endoftheanalyalrun. Tshtaendmaerad.nTahreesatcaonudnatrfdordoavcihtaonnaolfi1e2i8th1e6mceotuhnotsdobfatnhkessemmuesttbhoedlbeasntkhsasnh5o0u% obfehceaacrieatoedoatndofre1phorLteOdG. I 1fsar0tsstmsietcaaanntdayarr1edadoecvfoeournImtsihonegfcctuuhrtevemeret,thhaotoedmcbohartniskccsarelixoscate,ieocdra5t0o%mnoatotfetllmoiyLn,aOltQehesomteaentdohaorMdd,obrahenerknsohmsoussLstOhbQooumauvsbatalbmaotaedrdee.ed 0h. 10.3 Sample Replicates. f`eSasmupllessgeusptlcrattheasna2r0%colillebctefdlanggeedeinct.heTehpeorre,labtiuvewpielrnceonbtefeexruendceed,fRoPm,rsephoortuidngb.eTrhepearreiqeudi.reRmFeDnt or Tepicatesexcudes eldbanks. 10.4 Surrogate Spikes `Sutogatespikesaronotequi butmaybsusedonproectspec requirements, 105 Lab Control Sample tTabrraptgccehat.teLedolLawOblQacaboncndtoonhltgspohiskapebksaectsoar$mhtioonuikimbkueempsrohefpowaurodebdfsaerperonenptcaceroenntcaaetoicnrosnacoe1nnsthreartroiaonngsbenaoefaprrtohpeatormeedinpwiotmihaetasocfHhhigpehrecaruparhrvaaent.ohn e TlSohestesotfhlsaaanmvpoeleesqstusaanhldoa1ur2dddb0ve%iaea-onnndftochifeadhveecoroaongteporrlesecppoiavkreeresy5mvuasptglrblooper8ii0tn-ed1.e2p0e%n.de1nt aaboavcehccroencdarreanoontmetve,lhuesenboe MethodofAnalysisfor theDeterminationofPerEuTo5ri.n8a0to0d4Co0mpoundsinWaterbyLPCIaMSgMoSfo1:D1irect injection SMCarEonmGonrbion Cnmoceoemon2r008 Page 180145 p22 Lumet may te ue, fcutent for 14 dafyrso 92032010 conmoemAL 10.8 Flold Matrix Spikes/ Lab Matrix Spikes aRfecrccouevredarcieyevssaetsoof.mSenaldtmmspa)lt,eroirrxowsuiptiknseofskobrasenrpdeklpaeobsrotroaeutdtodruyemofaoft7r0cn%s-pctiook1me3p0laar%no,tamqnauypabayeefoldnattgoogbleesdabamesptslwueecseh.n(7w0th%eaxnpadn1d3e0d%ofthe e"Tnhdeotgaerngoetuesdefvretlcaftobioonuesveedlwitshhoouutkdibsectatlieoenst5o0d%eotfeihes8tnhdeosgteantoeumsenetvoelfaacncdulreascy fhoans1l0ytesfhoouls. Theeverageofhesamplean thfk cupicatsshoudbeused10caluatethe recovery. 1_Data AnalanydCaslculiatisons Usstaontdahrfdocluorwvien(gneeqouratrioognrtosoicoanlpooraotmtehleears)mgeunaorfatnodibysanouanpdp(r7oivei.bwaasresdpornopgerak:ree) using he Analytefound (ngiml) = PekAreSoapeI.ntercept ip # DF =factorbywhich hefn vkamevs td, necessary. pFeorrcseanmtprelceosvfeorryd.ed wihknownamountsofanalyte rr10Extraction,usethe folowing equation tcatethe Recover Totalanalytefound (ng"/AmnLa)i-yAevaedrdageeda(navlytte)found insample (n/m) w 12_ MethodPerformance `A`GNnLoyPnsmcoehrtfyhoo)rdomperenSrcfeoytromDaaninyvceescppoaerrca(fmGeeLdtPpesarursochm)eathaaorssmneuosstSobchreideeesvsecdrmiuhbesedtdiabtenac.dodnissicduesrseedd nftthhaeTeevcahsiicoanlMoafntahgedearta(.ron saomtptleslrietaandaliynzeids,moetthhoedrcpeornorsmaankceensaeceopnparorprniitckemeDtmaoilecnaofnucaecmoamnynbtaehpeenarwmdetedtaon hesysemand dfatiaasr itcnohbeourteepsrorotlsedowrehoapndoprerf+riancecrihavenobeenme,thedetamustbefootnotedonabiesand 12.1 System Sultability `Sytem Sutabity standardsaro not required component of hsmethod. reqbyupriotornoebydthe cueaclnhbpvrraiitcoiarolnomctauchnravageea.tndaarimeinrocioumpruevnmseot.efdTrypjoieoccaksloynsstfheersoSmsoAanmDpoiaReusisoaasrmaopmlptleaescavorinelre,reiTcrthaeotdosnyasntteoahmrsbtethgaeibnmiiidngnaovefe ceoatfcthiheaomnusnyssitcal aveaoacountswihan RSD of56%and tection ime RSDof 2% tobecomplet. 122`GalQiuraanttointCautriveo:nThecoeffcentofdemeintton()vakeforthecalibrationcve mustbe restr hanof * ehqeuaLlL1O9O0,.w9h9i0c,hEamcahypboionwtiinnhe1c30a%v.emustbgwin25% of he hecretclconosriraton wih heexceptionof ```voCacOluhVacPiaaerdvfeo2prsmocanontncmteuu:siTntghbceeaclwabiatrtiainto2on5nv%osrotffacnahdetaorhndessorihenatatcdaalrivoanelrufosbp(eeWiErhnsigan3pdeH0rot%uogffhoerhoeluoctwoelhs!becrauarntvnaecpatroav)es..eTqhSueeanaccercatuleraaetocafysre bracketedbyCCV notmeetingthesecrteriamustberoanohzed. MothodofAnalysisfortheDatrminationofPrEfTuSoi8n.t0e4dC0ompoundsinWaterbPyagLeO1S0S01;11Direct rjection CatcoonG nanrainngCosocoan2009 pagn 1701148 p23 Socamant may vs Ll Ta an for 14 caps from CHORE0AG coenTAL s`iDoenmdoanrsdt)raatniotnheomfaSspsescpiecftyr:aSepsepconseoifsudnemiounestornast.edbychromatographic retentionte(win 4%of 123 Sensitivity t`"oTdoeSepeteacnrdoginentg1oe0nditomhreiaodofvdequltaunistkoaodtneniotoafanlpflepo,rraopfraanatlsybtaesrks0o.n02d5tnhgeimacLc.urTahceyofLOGhefoorwadneyvselpcaelctrnatanvcuermvaepyovanrty. Refer 124 Accuracy . "SSepTcistemosenatnh1d0olcdoatanadibnrseoaqudrmidraiaettdoiqtnuaasollpiitiryknefcysoa.mnatrilosnaremgpalredisnagrohdesriegqunierdetdoagceanuerraactyeodfaatbaotrhsattarryecaocnctuorastpeik0es+,1f3e0d%m.atrix 125 Precision R`rPSeaqDmupirlreeesmsseunhstogfruoardtrbeeepricotahltaecnst2e0exc%dundwdelusbpoiecladabglgnaetndhkiesn toiheedn.rsTeehpbera,rnbeklusat.iwvielpesobseexfuedreendcfer,oRmPrOep,osrhtoiunlgd.bTehreeported. `Section 10containsaddons ifomtionregardingtherequiredpreciscnoflaboratorycool spkes. 13 Pollution Prevention and Waste Management Waarcshtivsegdeantetrhaete3dMwEhnevniproenrmfeontrailnLtabiormaettorhyoidnawclcboerddiasnpcoewstehd oifralpeprmoaprpiarteolcy.eTsh.eorignal sampleswil bs. 14 Records E`Iasnacfmohpmladteeiatoannpdafsoctrkatanhgdaedrgadetpnareporapactskehaedgfsetosmrfauesscttruddnsyc,miiduness,itrbunumcteusndntsoratnllosiugtpep(danrosttrnhugemifenofnloorbwmeiattnigonreefmcosorr:rdessc,tounnsdisyrouurcmipeornnotojefaccthqneuudimesbtieaor.n, method, summarypages),instrumentrestsfles, chromatograms,calibrationcuves,anddaacaciations 15_AffoctedDocuments Nore. 16_Rovisions Revision Humber `Sumomf Chaanrgyes Math ofAnalysis oteDolominatnofPrETuSo.8s.a0t04d.0CompoundsinWaterbyPLCaM11gSoIfo1:1Dict foci SM CarcoonnaGn nrmiaDocmonona 2008 pageieorras p.12 cowroenTaL ATTACHMENT D: SAMPLE CHROMATOGRAMS AND CALIBRATION CURVES WMCordo0w7s0G10r,ormnerRCoorcom12ber2009 Page 119011 p25 rr =] =] 8 Ee f: a 2' 5i3 } rl EY } i3 . |2 | ot of J |: SEERRERRRRRRRRNA RULE L Hn ae g BRh 1Gon osu RA flocks,pr Hci pp ptJg heaislCls 5 igifiie1 g --1Biifllaiio s 1gY ifi. iasn iI | i . T= 5 J id . A 8} + L |3 s `og . | ol J Tree reer J 2B ge Bou i bof a i 2 ah i Be uhl nn iiedh a,lidEe at5i2 E lal ih as Bilis i Tit :i: i - ! p.126 3 2 |2 ih :i FITIIIIIIIVTiTIiiiiaeTh i Tee H BH, ge lf sf lhile gi5 HHHISHI] i i fe pin an bis GH RE TBihat dHitSL lias lle isd i 5 " BH | Lt l& 3 : |-- b K lo: | rr TITRE h REEREREEEREREEEEERIR FE iH fil} Ho bielt pd ap ddsn,npnni [RE lsIJsf 242 5h2i8: bPoli oof dHiEeS T Bidoigl 1 iii i RH GRE di tildes i adit 355 p27 * JE flo8 .| ihi TTT Bo te il White dfL eelaE t gy Bilis lt i k1i THT i Woe am HHle 5 F i! liltlegtsit t :: . Lf : A 3 > | | rrr re Blip: a BE PoLaAaT Hi EEEEERRRERERERRRINY ET i Loh ah Bl Fi Bhltl a i ii p.128 + : @ ) LS 1 - 323 L A t i RE ! FEEEEEEEEEEEEEREERRRERERER hi rn : ne B 3-- hoo Feo MoLdE brat le bhjat dlaili 1 ifn iidsihiikidi di :-- bi dali i 3 i= fo Me ae : ifwialsdate, Ble a lo : ili india: dsl 1| = -- =g Ii i A hr |3 i i : ER fiw Hl il mn | TIT J POR Blige opa t gOeF fPgEeTn Eds sae ii Bohbll,i fhhE es d iHliEif:E it iirir p.129 + :i flo | |# : . Im ! TIT TI hr 5 MfhilBosgon swi pgs hjile a 8 ' h le T r rrr i i ii eg [RhE E f 2 Bjlis if H0 d0 : | | .: ; : A LE | h bi $i IE ii | il FrgTiTiaaiisaae:TH di IT |: 4 2 i sh li [cohli, ffihe A= 3 fhpolfla Gatdaany BaHli iFI itt hitgy ed iHHH \| i: { '! I iB Li 4 : 3| \ i 2 } | } ld PR OTTTIIIITITIITIIaTiEBei : a suns sary 52: | i oF ot 4 1! 1| Is 8i I 2? i | .: if * ld PPE f TIIEEIIIARIIRRRIREIAILE Lf Ji:i |!Joili | |iE PRTITIITIITIIIIIAIEY ]Hl \ ; | i /or 1h |s i NJ J !i ]i 1pr " | : NJ ] p13 TRI R -------- ee -- Lys gratis C 15% i leb 7BEAN b 8 C i{ + ua-- fo GAL 23:] dSE E] .| # Fee - $y [1 | :: i . [ 2 NE HI f Hy + Lk A FH if - rr ! A 8 TIT il ie fj EN Hn ai Bi Bf tie a TYTI TIT I iiaiie | pcsaf fhena fshde J figspilal, ipHien5 s aliiid 2H BHEE als WT p1a ` ge ERE11 iri I 8 A 4NfLETTT rr ":it > t - FF i - :4 L & l: il x of: | EEEEEEEEREEEREEEEITETHEITIE hy TETRA TI avon aii) 3 i He E FiO LlL i1t wih plisegi Eii: Bhltl, 1 dy a fr HH p.136 3 EE fe h 3 : -- Le I Int : le sy tk ! lr og = Lz b ILl ea ! } Lad Blo Bbw ge i 1 REEERREEREREEREENNFnfori+ n= t = MBoEul pin a EE IoEn ts i i ia t Ay i ieiwfliile E np bh Gi Blike iais be Fy 0 k' : . v } i: =|ffeg5 oo: [ = 3 Bi EEEEEEEEREREEERNEN a i mre||g4 iP: oHEBEnu aa EE if]iifbitiyFgf Fiki if PB 3 o OPp Ra EiaLnE B({lIHl E iHiidz : 8 i) Pho TTT Fo ee hfaotsHoGmens batlhii Sdiitg:i Hpn4i p.137 : TTT ee q : s oe : Fr 8 - i# I i i Th -- TTT HoPohd ar mde id ilHiin iifs gs ie Ih : il 8 le A fr fj rrr EET F2I bhE i aoo pl bopfl,a ddad sf ece---- : |) LELELUBLELI UIEBURLILI I FT HH IjR o dEomCS iki:: pilhi, Hheihge fat ifiie p.138 i" os Pe : | 1 A Li a C: h PnWoT nie errr Bo ey filo feel, IE8a FLaenagntBeEsD 8Enli233l00 d saile s i Ba ar Bot wo l| e 2 r 5 alia Chl iid i ed A : Co H`|i: aT 0 i i: i PI | thy | TTI3T2nT3TIIIIIII ITT nTTI 3 2 oR ih jl brn, i fg hs, il he Jen BER : i DB iH iii L ldaitthh di iw A ls biirhte, Bit: Je Lith i instil E dy dude |i aii|,i A iii iHiH iii . . : os ol? Ths . = 10 I i Cl i LEEREEEEEREEREEEREEE TERTTRARE AERA RR IRANI ilo i 0g bpjes sa pis fhi: a l1E. { Bib5i 1 fd Bibi 5 . i fialt tfSiF bs iisdsoggin : i le il OE b " loz !| --C3 A 4|:: REREREREREEREEEEMS | TEE EaT v iavE avaR ni| 8 Eio fl fjto Ff pli bi: BPohlidl ddfd Bhil Hi2t iie:: ) H it ! | i od : 22g gl =i C Ce o |} | fe ik aE A g: plmiviTiiiiiaiaiiie Lo \ | i: +4 f if Hl :} \. | | \3 | RR Hy 1 [ )i) | | ! | | |! { TrTTTT RIT IRIEL 4 vf] | Hh Cf H 1 i 44 i gE | . 1 Po : i Td Pi TET i iia fh CS , [| i : W+ idl Hl 1) ! :| | Nf I NO j Ni PE - gf p.145 s : s o5 le i C 1 Ha ih i [ nl IEERERERREERRRERENS 1 | TEN ifj sHtoau pag miEthNty 14 : ipetboshwpsg li i 5otE ed0 : " : ' oAfi gal # C [|- LF FE =f. 3 H i Is &f :i = b | | mom O: ME a ge - bikes 5h gg L Pob T m Ilae ) :! Brrr : i PIAA RRINT | 2 M ; o Poulg i2:3 il en pe 8: i|sgt bwiidihet ! iHih Ble SR HH TT if L : Ly - 3 : a fd Hi iy I : | `| :Hlf iGi PR TIITIIREIEIRIIIIIL p.147 conrioeNTAL ATTACHMENT E: PROTOCOL AND METHOD DEVIATIONS 3MCord0o7n0G1r0o,mpesianraGpooca5m2oe 2000 Poe zattas p.148 aMContents RECORD OF DEVIATcoIneOsNTNONCONFORMANCE SOwai sytoTntmPypNsr.a0 zSOP Sac0rE)aaofpcOmooecmunimtannPscrneod:ced0u0r1e080@ SaTScAeIErANS e Motrad cckom;" 0 Prowes Il, Description _ _(D GsPOtaexctraphages 0 ss Ober: nesde) "Met351hodFCCGCiRSVserrqeaucnoivoreeenrmyrewencicwtosiv:oyno5f%01r%0o0sf%1teo20na5ls.5.64680 10.4) Actu(a1)lSperqouceendcuer0e0l1p2r2o2c0essn:wo hesevr CCV (2)LCSofsurcndPOSandPFOAbo hda sfoarrPeFgOeAhcaovder3yeocfov1e2r9y%o.f 2.4% (8)P78 FS C5reco fo ocaton CON-OW.C1vas68.6%. ll.ActionsTaken (such asamendmentissued,SOPrevision,ele.) Corrective Action (0 Yes (2No) Reference: `Acc1)epBtEC oavbeeinlCCiotrOfyE Vatwheer53nmaomnns acaaortnafaondrdumnignISghewocorovku:rr tahnarwnarihshctr oCO PaFOPNF.OSArocnvwacakt 24%b.e 2) 3) STeE oranaair:esneePpUnESeDcswg cnoda1eo5a3o0ef5PprL0aSr0sxlTofPosUahSsiaaeknmrgCtOesoLnn-eGciWoCvH opfot1r%egardlonmPFnSaa4PdCPrSEhAawvere etmeh scapecawth Actions: 5mOaHtahireirao:nh3Do3if5Wne%oragkdvc$l5wii4Gl5irb.aassnnStaotNtsnoetidvhreinsfottoriaosnnreiesrd13.WsorekocRekcoalal l0)sWoitcohroeolfdR1enhpngt$0 Project Lead/PAI Study Director (1 Approval: GLP): Susan NY Wolf i oDaattesi;;lhtnl SponsorApproval (for GLP protocol deviations): NA Date: NA Technical Reviewer (optnal): Date: Laborajgry Department Manager Approva Dre are atingofvk cuIrV.oAusthtotrktiostz RetasbutmseioWnooernkby `LaboratoryDepartment ManagerApproval:NA oe: 29 Fraud Lars Date: NA' srs SusyDvDervoiaFtiooniNo.T __E ~___T ___ AtscomentA Documeniatono,QeuEEHe15.R4E00M0I7 oncontorTmeisngtP,agePiogft42615 p.149 am Content RECORD OF DEVIATIONINGNCONFORMANCE 1._Identification O`oSEtvruadayto7Ponryoap.jecemtNo.RepPSoOr?Pes DSaotqeuQ(asn)cEaoafGuOOmc1ceEun1r1rtaePnarcnoec:e1d0ur0o1. 7@. `MEDoTotcSruo1md1en0t4Number: DB GPO 8 Ghar Viet1.hoCdORVeqauciorremnewnittisn: 25%oftu vale (acton 103) Actual proceduralprocess: (1)Oo ne fht evrat COV orPFA 40 FES 0d ik mtmeh accstan tr iccs sess amino ott, SOPmvs CorrectiveAction (O Yes Hl. Actions Taken (No)Reference: Acce1p)taQabCiclciotlyrrnofwStruhemeavnsoinecwooncfaoddrmoyitnmogowtPorrEk:aAcoondpFaEncBSrGLt:hoctrvts g Ra edLCaScacnc apdatncaslc, earU.S. rat var Acton: @OHmoetri:ngcofoWvodrakvaio0n ClloenatrNoolteation e0r).WorkRecall WadingofReport n Project LeadiPAI Approval: Susan Woll | `Study Director(If GLP): Tv v iA `Sponsor Approval (for GLP protocol deviations): NA Date:i130 Date:2lzlio Date: NA `Technical Reviewer (optional): Date: oY LaboratoryDepartment ManagerApproval: D2ate9: 770 TaboraUtoareyDepaatin rtomfewnetMtoacncauIgVre.rAAPuptmIheOoVmrBieEzsNatAiovkntomgResusmteoWonrk etnDate:aNnaA (e DinDceavc ioastmioontNoor . FEAP=u TT Aachen A Ers40087 Page 1011 `Documentationof evil#haeanfiepetHonconforming Testing Page 144of 145. p.150 aMContdantal RECORD OF DEVIATIONINONCONFORMANCE SSiiTe PFuGmio ts DCevriaactikoonnttyyp.e 0 PSrOoPcess S 5)oe fOecuean nsceo:otg 000Ts DoETcSuEmIIe0NT r 0O GPOEquipmentProcedure 0 OMemtahrod Meth1.odiReaqmuaitremsehnets:cian 91 ofProc `Actual procedure/process: (1) LoecatiyonCOaILc-ssGWaa-abMrWee-owW 3n-84eadsisdnaptapharabvoei oliimdFtmaahttrisi xa5sop5ailkresTleolvelsaEpiprBospr.iCatOnsLfoCer PFhHBAa.rSAee3ve4:r)Sawleosther ACorcrecctivee Apcoiftotnhae[nbonVceiosnifo@rtNmioyn)gRweofrekr:en_ce: ; -- - 1) Daa beg ih ort nkhaving a olma sk Actons: 0GHinaertioD fWnorgkeibCv olninotto Ninorttan tiortn. )Work Recall 0 WithoolfdRenpogrt wren gl ry ProjectLeadlPAI Approval: Susgn Wail ' rector !: `SponsorApproval orGLPprotocol deviations): Yong A Fela Technical Reviewer (optonal): ole Bote, ai"e,2120 One: 750 Dae: oS -- Laboratory Department Manager Approval: D2at9e: < abi of rt cIVu.t A mpuumitonhaoerhtioRzetasmutmeisWoorrnrk Labret Hank LaboratoryDepaMar nagterm Appe rovn alt NA. / = Date: NA = enorSiy oeorviationaNeos.FTST Jr-- Oocumenatonof EE1saRoerS oncotomingTes PagPe 1e011450145