Document JrOBb5wrvzmkVmMMzMpaoDEza

_ `E a o ` - a a - L 4 - n Proc ReseRarEchS, EARCH AR22- 1933 Analytical Report 3M Company Analysis of PFOA and PFOS in Water Samples from Oakdale Municipality E04-0911 Exygen Report No. L0004145 Revised Testing Laboratory Exygen Research 3058 Research Drive `State College, PA 16801 Requester Gary A. Hohenstein Manager, Environmental Operations EHS Operations. Bui3lMdiCngo4m2p-a2n6-y27 St. Paul, MN 55106 - - .- pastors io00m81c20 ee - . - " a a a " Ll - - - - - - err------------ 1 Introduction FpInthosobeversofnSoasMpCotor,mproaeons(nyuP.sFaoOTrSha)ercriompwpoaetlrdwfossraartmhopevnaeansaald1ye1os00ips0vaoseftdaeufrtuoBrxofyoogqecuntooaasnstoerienFqaoucremdasa(ttePidoOlnbRya)nGoaadrnyad Tmaokoemninorchangesfo ho ex ofthoreport. Anaica rosswore norchanged ie TahnaelBogqenuproajenctotnruambesiraamospsoidsg.ned 1 thosamplesisLOOO4145. Table | ls ttharget `Table |. TargetAnaflory Quat ntie tatison Parameter Perfluorooctanoic Acid Acronym PFOA Formula. CrFsCOOH Perfluorooctanesulfonate PFOS CeFrSOH 2 Sample Receipt "pATwterhntaoyr-cssueivenesaAntstoarafmcphi3mlMee,onswtlaAlersearmepcleeisvweedartaaExnyagyeznodin.50Ac0ompLywohfiatelplsaasmtpilcenarorgowm-mooumtahbtottolens6. Tshamopslaemspwleersoswiorreedrrociaivgerdioandf12o7m240i4. Tofhraosaomplesawenrassl.hedambientvia UPS. The 3 Methods - AnalayndtPriepcaraatolry 3.1 Water Sample Preparation `Solidphaseextraction (SPE)wasusedtopreparethewatersamplesforLC/MS/MSanalysis. FWo1ar0st0hy%amidmlewttiehhrans5oolf.thAoefpwoa4tre0nr%soamfmetptlheeanwadassa0tcrt%awnwsafaserrraewdnass10ihe;arTCdhysa1SGPaEdrcoiacsrgtaormiwpdageesr. vTvihileecdaarwntidrhaidnSgaeylwiaoosfd using dactoapry LOMSMS 32 SampleAnalysisbyLC/MS/MS ItnhrHoiugghhPraelsiqsuuirde-LpihqasueicdhCrhormoamtaotgorgaprhaipchyco(lHuPmLnC.),Baansaeldiqouonttohfeeaxftfriancittiyosfintjhecetaendaalnytdepfaosrstehde `stationaryphaseinthecolumnrelativetothe liquid mobile phase,the analyteisretainedfor a racezoes : a 4 - `fahnradarcaaceugirsamilooaemannedamdtneosteeofucofdtreani,dnma.tely.TsihFnogoloaowniinsdgocHharPraLagCcesteaoprfairsatrtogoiaofin,cmtchaosmscpsoosmuppencodtusrn.odmMsetaroryokpreoebvsircdeoensueradiezraeaspdni,dd Qanagiaisit exaactetdstoandadrds. " ASnamHpPo1o100xsysrftoermaciunaanctttaacstaodn 1an AppledBiosytams APY4000was usedfoanalyzeth - 2I1asnomamlemyr.sexpa5ra3tmicoonlwumens.obTtahinesduumsinogfthaegsraodmeenrtseilsornoptooieudgh2 aaTshienrgmevoaFlluoephfoar sascRhPo,f50ngx Thefolowing gradientvaspero: . MMoobbolPohPahseas(8Ao)Y 2MmotMhaAnmclmoniumAcetatenWaar Tiam0e 10 5&A & x5% 3 50 2 7s 111000 180 2& b3e] 3 "Thefolowingparameters wreusedfor operationofthe mass spectrometer: - Pontozatmoneode Polarty sEelouctospray Nogatio . Transions Meitorad GasTomperatre 4341153055336790((F"OCRP)R,OA9)9-80(PFOS), DryingGas(2) 70Unin " 4 Analysis = 41 Calibration . A 7-pointcalbraten curv wasanalyzed ial andtoghouttheanatcalsequencefor a yPseFaansOmdAeP,1S0lPP0t0FEOnpSfogarrno(dcooph"t)CpcufPoosrFoeOL.dAfGcU.oMTsrShusoMacmrSnapliabsesrnsa.atiTlo.hnrpooisCsnaittlsnrbwuraWmatrahinoptnr1resetpisaapnroidenadsrnaodvtse,0ra,sr2ue5s,sp5r0ipe,peac1ro0,e0nd,c2av5sr0iin,ag5ct0eib0oo,nt a0n3d6c5,oeffofidecterimienatniotn(7)were determined. A calcburvreisaaccteptaibleof 7n - Forthtohrearwodsauttas ianpAotrtadchhemreo,ncGta.Bratoncroraworeme.Thecabvcuravestarie coludned a rrasscrs - -_-- - a 42 Surrogates - soaCmspPlheOocAotrIatsauanseoorkdsebaensfeors1turhoongbaeotwtaifho wttrohrasvosaatpnat.satmhplols.doCsPaFmOApw.asa1dhdfedl,ot1hoobomiys CPFOAocovorie canbofound intachment8. " 43 Laboratory Control Spikes Laboratory contol kos i neanatasotwero proparod acinga ownconcentration a w1`aoi3sfn80P0%F8OoshAmo,atsth"cohCGco-aodPtpFaaaOcicAsou,rrraaaanccndyge.PedT..OhFSeoltxaobtolhraabrtooerrasytuocsroynrrtereaogplesrnpteishk.eesLma,buosrhtaotsobhrooywcrorneetcrroovclesorpiieokslebseaatrpweeeuessnwedo7r0toe- . 44 FleldMatrixSpikes a SAWsalOmooLpwlsiacnsngi.hdeModhwaiTrgorhocmhosvaoeitarimsepslbpayekowseoUwaasanamsd7o00pca.roesTpns3ate0raes%nds.ofrmFosrtobehrveoe1rdr.ysawfcaco1utar0elarcbssyoa6im0tnp0sol1oew0iem8nrhitorhcse,.ofnlTtehde1m.0maCanoetsmspToaskuknlegdossf WooWith ho acceptable ange,oxcap a5 cled inSocio ourepr. - 45 SampleRelated Comments - AlhvoastaomrplsearmepaluetsswnoArstaccohomloendtBn.ica, Dupatosaa susar ropedalongwin o 5 DataSummary - PilneaarsesspooorbAtlanch(mnegnmtL8)ffoorrPadFeOtAalaendidsPiRnOgSo.fthoanatarouts.Thoreasr rueporsted 6 StatoefmAcecunratcy . aBnsaaesiosidcoaanndarcecfsulruascmoyafforliaPboRrpOaitSkoraeysncdsoPhnFotOwoeAdprirekesocsuo,vsefirai.eds5W0mi%a.lkiLshpiaakceesb, angoceonssrt,uorlwrasioogabttses,opakosrru,esysha capone: w + SSTaphmoepPcoFwOoaAdsanonvodetrPb3FomOcaSarselcroleveesredyrbironacOna-iuWsSa-st1ph2ie7n2g8n7oSLrooawnoSspraimakpnola.encdanOcWeBn.t5a7t2i6n08Lroew + Tha PROS recoveryfosampleO-W7-463534LowSpowas46%. + ThePFOArecovery forsample 0-2208463 LowSpkewas 1%. . racescrs - a Sms AS, 7 Data/Sample Retention . SrapaosbediamhaadtSsanmpardoioa3a1mt6e0eidnyroforrorsoro.tTihngSi.rl sisPrAl Ge'ssGabc ysrvoadncn . om 8 Attachments [ 73 desta aise - 7732 AasmofaCoasyFnorms Atta B:ScpikheRm ecoe vern yDat ta. - 74 AtachRmaweAnanlyttcalDDa:ta. o 9 Signatures " eerdrFcml for Loren Aisha =Yafes a ALL oAi AS a . Z o ---- d Section A ---------------------------- . n pT [Suu " RESEARCH Pot. a " `Summary of PFOA and PFOS in Water Samples E04-0911 8Acid PFAnOaAiyto FoundC(8ngSiumitf)onate PFOS " o ELxy4ge5n3ID OWrS.a2m0p8l4e62ID.y Dup Porfivor0oo0c9t6a5ncleAcid e Perfluorooooctsaenessulfonate ' LLL4eit1ii4ss5aa71 OOw-aoWw2.s-2a2z00r88a44a6r36up3 00.000870168s40 0NN8saat " LL1i6s51125 OWOSwr1-2d72e8s7sDsup 0053020 0i2o5r0 ` LLAeisStA?8 OoWwT4e6s25T%a4eDup oosaer 00s2s25 be L4LL1ei4tsa5s-2a12i8 0-OWW8O-aw52a72o06a808d4DsD8uup4p. 0NN6Do77 0Nn.8oD69 Ll 1414525 E04:0011 Trip Blank ND NO [] NNDQ ==NQoNuotatdnqettuieaacttnoentdf(at0bo0l=r)Mawebhaovsceuhr0e.Rd02Oc5onDgn/cmRnLB.r.La.trbabon 0.025 nim. and ha iiof a a - - o \ - 3S0E58EfR ogsDrRivhea, usn - OSr ahe Section B "`E rHeh aerRtEhSnEARCH 4 Msi SpeRacoerySummaryforPFOAsndPES inWistarE0491 a . SPpeoR FTE E| a fmcos"cioreon Ti rcaosutg ormmrarrcs " owT S s nss un | or | oom Jen om ws| oom sew |e ow eo rw cmDssItsEioSrtEots er fem www [a ew we ` oTvEEeSnia [---- Le em me ow oe ew SITE a ene ome com ow [O-WTTS-E1E--27ET287--IIHiEEghS--SSpike | o |e ae ar om om | am oe am om ow om ow P) [ TA-- RE | [em sw ow em ss ow [ED--I--E a | em amc [om ems ` PM Oo-BWsTe-t5E7i2E6oE08nHIisEghoEStpieke | em we we we om an em ow | wa ow . -- CEE-- RI tan pow1 Lee ws mw am we CEE La |e am oe | 0 ow ow - . TEI E04-0911 Trip Blank High Spk |e ae me se wm 4 m ESI Eiee n mce ntrsssceriee a ara i ) a 30E5i5aEnnBnD,rlive.n, in a `eogencom --- PB`E - " a a ` a a a - . " a ` . en 7orRReES.EARCH Surrogate Spike Recovery Summary for "*C-PFOA in Water E04-0911 jp mm---- ExgBonectSaomplne --HSpoikread ReRZcCooPvueFrtOedA Recovery (amt) om) od LLL41Si4Ss5:,s3 owoi0w-ziWiz1m0-z200ie8o24n6bs2uep k 00055s o0o.5os70 1i111ms4 L41456 O-W1-208462 High Spk. 05 0583 "7 Lo1t4u5ss oow-awazos2d0s84s6o3w o0ss ooesms im0 LL4i1s4T59o O-OWw2-o20x8e46m3 HLowSSKpk 0055 os 0379 17s6 L4WL1tS4e5Is-i1Sz1 Liste OOWwoSOsw-usiWTiszrI-aT1Tr2zLH7eo2gr8wno7suopkk 00o55s 05 Oo0.ss48ee6 ams im83ge ise Lasts owas 0s ost ws L4L1e45a-s1t6 OwOr-Wd7o-w4s63a5l3o4wDsuppc 0055 o0.s55s1 i11z0 L4145-2 (O-W7-463534 High Spk- 05 0.541 108 ULsii4aSsrTtea oWooswTswTsB0eL0o0s0wusppk 0005ss oomsee 055 11007s 11g WiS20 OwesTsmHGhSK | 05 os 107 sat owsaomess os oss ms L4LL1Hs4s52-22432 Oo0ww-sWs3xa-em2i0S8si4il5Ho4wgDsnuppSki O00s55 0oo.5ss8ee1 ii1o1zs6 LLLe55142252857 EEO0kD0EoN1a1 TTriippBnTlapknBkFLaonkwSSpkk 005s 05 0osstt 0sr4 1o0d8 X=BBoson, sn ES 33 BN Se