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Laboratory Report
LCMSMS Analysis of Extracts reported in: "Preliminary Report Analysis of
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Perfluorinated Compounds in Environmental Samples" by P. Jones and K. Kannan
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Report number: FACT-GEN-008
Testing Laboratory
3M Environmental Technology & Safety Services 3MEnvironmental Laboratory
Fluorine Analytical Chemistry Team (FACT) 2-3E-09
935 Bush Avenue,
00St. Paul, MN 55106_ Laboratory Contact
Kris Hansen, PhD. Bldg. 2-3E-09 P.O. Box 3331
St. Paul, MN 55133-3331
Phone: (651) 778-6018
nnReguenner FAX: (651) 778-6176
3M/Battelle Exposure Team (c/o Susan. Beach) 3M Company
Environmental Lab 2-3E-09
St. Paul, MN
000514
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MENTHReOrEoNnTsAriiegroCResTnOaRS
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"
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1. Introduction
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MMSiiaccmrrpoolmmeaaessxsstQPrulaaacdt,oprrroneIp,a1area sbpiylngPql.eaJqodunpaedorslanpeodlieKn.LsKtCarMnuSnmea.nnTth(aLecCsIoeSarMEmnSe)0e,xwrFhaAicCcsThwpMerro4ev0ird,eesw-etrmerosrnerdsebinyeeFdvAeuCsaTinngiaaegsa
tbheaen lsiniglmeqwuiiadhnitnhsaeiLmCtumMeSenM.Sdn.ieferences atmayprovide flepositiveresponsein CMS analystsen
PthRExoOtsreSacdutsseifnrgoemthsreamLupisOlieMnsngSoLMfeCsSeMdInc.nlg1eesnleka,esPy,RtbOhSadtlmecvaeltlsiedeitnletaerrmafie,nreeandncbeyatsLohrwCaerMrouaVnndwalryczesesd4qp3p9rucoosamipailtielcyahfaotfrhoef
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o`rsgmipnlaelsFLoCrMthSe LaClyMsSisM.TShansaltyyspieso,fqmuaanttitiatmieonrwfaersebnaseneedaarnmtahses449999h5a9s9b,e1c3adbsaergve ionncshersspbinosgiecal
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cVIaanultsheeesdLaarOneManSopMmioSlcaonauaslylsyiblsi,ogwlheorwtelhseapvnoenlshseooiefnrPhFeeOLpSO(tM<bS5yapJpnob)eswsea.rnedeKtaencntaendin1seveerallyoftthhatefisehssamipleese;tnhesse
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`NAogaPinR,OShiasb5ove tchoealsittootfhdeiLcOtMiEoSnvaansydse.c inte rein fh samples needbyLCMSME,
Additonal, allsamplesofclepasawerescreened fore followingflucrochersicals PFOSA,
:1
PPVFReOOySSlAAoAAw,,MMv35e87s60,,(<MP5SOpSAb6A,),PooOrfAMPA3F,7OP0SHwAwaSes,rdaeenctdhescPetFrvDenS(asiyneteshAeupNppoerentdh.iAxmBefroircdaenfbinaitdioansgoefpFlaAsCTascrpoineysms.).No
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'ePFHSlwasadeltf aectedineeveryB)alticseaneadgleplcasvmassNamphle,whilePeFnDa Swas y prelimnay (0oo%standard
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"Thisdaiscreeuanl innlgy.Only
`wereextractedandanalyzed.
2bigh level (250)POS
tix
kesupe (eagleplasm)
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aPn.sJloynzeesdabytKheKmansnianng adnelEinvveirreodnsmaemnptlaelsLoabtLeEOMnvianrMaornchs1L5b-.19T,h1e99s9.plAftewreLrCeMxStaancailoydsiasntdhe
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`xiatchtthsewseamrpelseusb.miItiedatsouFmAeCdTtfaorsaLmCpMlSevMoSalnealaynsidsf.aThleerxetwraacstnvooetxterawcetrieontpaepsearnweo.rk submited.
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ERdg E Te E T E T
+ Theres oholding timereissocistewiththesesamples forLC/ESMSM aris.
000515
Pacezors
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wesiREPgORoTNOn. FrCToGinasn
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4 Methods - AnalayndtPriepcaraatolry
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AaaflrFyoAtmCiTSc-eaMrl:um3emt1oh,roOEdtshxertFlruiodaffcoProAtinaasosliyunsmisPUseinrgHuPoLCr-EoleoccrotsparnaoryeOMtashsesuSlpFelfucotorrooncmhaeemttiyc:eaml CoodmpioubfnydiNs.eOdT
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foSofXrmUqoTuAsaCnttnoigftatathimeoaant.rrgiTexhctiusfrmuvooerdfoiocbrhceuamstieicioannlqwuialrnltoiamtvahteiteohfnei.shgArtepiarstese-useetxiesfrfteeiclntigokcenulrtyvhteeo,fbeexhtSrgasncatimecpdlafenrslo.ymExrtlarobawbceittrisoenaraen,hwteahssonusiscesd.
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fFcFrlAouCoimTdt-UnhMs4ei.spn1l,giatHosbdmAeanm.eaP`ilFnyrosiritLmeshuiimdsPr.Coetaasso-sn,iuLmCPEMSSepMelcSrrroefempoernltyec:domvadlrruiesofooobrortyOhqstceahfreisdtrhpiFttlaiiasonsargunoescsuheameympmplisleceassMllsvihnoefSaueelrdobu8seman.onrdaOsathreer
curve racedfrom rabbitsea,nofrom thesamplemai.
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H1PHPLCL,anOaalnidqEuEotPoLSf CexEtMSraMcSiSMinSjctdan column.Basedonthe afinity of theanalyte
fpoasthseedsatthiroonuagrhyprheavseerisnepthheac:oiluimdn
rcehlraotimvaettoograpfhiiqcuid
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msaoonlabulityiltoeenpehPxatFsreOa,cStmtehdaefarynoaclmhygtereaoutinrd8ew0tamatiienertdiefnosrh.iaRscahenaratalacytsieirsniwsttieimrceaesmmbaeottucwhreeeodfnoanvsteah.neFdHoaPrrLdPaCmFspyOsltese,omutiniowSoinatahcidnrt1eh%e
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odrFegtoaelncltioiwcoicnnoogmHfmpPooLluCencduslespaiarnracotnhisoinn,giEsBgSoenMreaSrcaMhlleSympoirpocevraialdtsee.dEaaltrcealopasitdpiaevnaedlyy,amciarladtteenizato mepaesrfeaor.canMahloyuzalinegeiacwaizqrudaoelnsroyaengf,soeor f
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a`dnseduacbspierdqiumeanrty onco,llcisihonasrraactteersimsalolfertshenealctso,finsosiedelreaacgtrr.mTeynhtissuonniqiusetbootmhbeaprderdwiitihozhni,gwahh-iercnehryagrygas
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`For example,for PFOS (CJF,SOy)analysis, ion 499isselected asthe characteristic primaryion. Thision
ithsefsreagsmeecnotnedadirnyftrooatghmeernitosnisssduetcehcatesd8a0aemcua(nbcoeruresspdotnoddiinfgetroeSnOty),aPnRdO1S3f0oamm (heCcFom;pSouEOnadycsht)oa.ft
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smeicgohntdhaarvyeftoensfaagmmeecnhtaaraicotnerpisatticem4s9.9amapriaryion,butdifferentchemical compositions and
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5.1 FrQuoatnthittaetiLvVeSAnaanldyLsCisVISSsys quiverssd poncompan aye
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+ pTPaelhaaesktmeaaxrrcpaacitenwilitoohnteehsfslifaniimtchpliemlerneacawetyniogtiefehovsaPcnfReaqyOleu.ySatfnetrlpioaemtaissokena.rreoaIfssgotelhnieekreralayntitehmdaautlstsihnegaesxatbsraeacntniddoaendtesfriemcxiianeecndtceytdofbfrePobRmetOrwSaefbebrniotms7cc5aa..9g5e%
| a 52 Qualitative Analysis
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PHmEaSgl,oepalnaandnsamlPayFistDeaSmr.epttDleuenrtoeiionxngairctmhtees.waeOrtrahleyeqsraslt,thaahivereexltlarytasicvctesrcweoeemnrpeeadrbiorsraocPknEe,tOnSobAy,aaPrFmOitSnAieAm,ruemMs5ut5m6sb,aeeMrSo7vf0as,atbaPnlOdeaA.rAd,s t
response of3reasonabledaughic ons (599-580,59, 130) atareasonableeenton ime.
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000516
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Paceaces
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WeWIRO ETL aoRuTORY
REPORTNO. FACT.-GEN-008
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53 Blanks
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pTrweopacroendt.NaionearabllyatneksswweerreedperteocvtieddeidatnhdeexxaaccttseodfbeyileJrontehse aCnodKnannneanr. sExotrracrteieonbelannkssiwertealso
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5.4 Matrix Spikes
`sOpinkeePssRhOoSwmeadtgrixespikse at25800e%pporbowvaensrypreparedforcachoftwoeagleplasmasamples.Bothmatrix
55 Laboratory Control Samples
LaboratoryControlSamples renot componentof hissy.
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5.6 Sample Related Comments
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vAelrldparreliisimisnacryr, aesteqhueanlidtiryoannclgoy.neAflfilcaineanlcyytoicfaltrheetsurseoffforhotchsemeicexatlracftsosmhouhledsbemeacosnosnisdeeredctobe
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Pt`FhEoxOtsreSadcutesstifenrrogmTminhseeadmLpuClseiMsnSogMLfSC.MaSIa.ngIglteespnlearse,ulaPy,tFbhOalStmldeacvategliespdneattfseeamri,enanecndedbafytisoLhrwCaeMrrSoeuManEndamwlaeyszrsed4aq5pu9panrctoixotaitmmievptelyyafaotrafeof
rLeCsMpoSnsaen.aMlyastisi.xForrtfherLeOnMeaStM4S99anbaalsyseies,nquhanatviteatdioinnwaos basieodloognictahlest4a9p9l>es 99, 130daughterions
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aHln`oiaLwgolwehyrlzeeetsvdhpebaolnyntoshLfeoCisPnMrFteOhSpSeao(Lrnt<Cde5MdLpSbCypaVn)JaSwolMyneseSrisess.d.neTdtheKicatsnetndyaipneno.sIfetvaeniroamlakolefylhtehhafstiseahseanmtciphleert;vrtehfdersyeovtFalAcuCeaTsnoadrnes4oighsnimfciccuamtplyle
NoPFOSabovethlimitofdetectionwasdetected the remaining fishspl analbyyLCzMSeMSd.
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F`AVAFdegdOraiySitlinAo,ontAwah,lielMsiyvS,sei7asn0lc(l,o<unMmt5SrpSapise6bts,t)oPooftOfehAaePgF,LiOCSPMlFAaSwHsSea,nraaelwnyeodsbrisPeses.FrDevSee(dmsieensdtAhfepoNpotehrnetdhfioAxlmlBeforwoiircndgaeSnfubioanrlidoticcohnaesomgiefcpalFlaAssC:mTsPaFscOraSoAmm,yms).
'PFOSAA, M556,POAA,or S70wasdecidinanyspies.
p. No
were exascndtanaelyded materialavailableforconfimmation)detectedinevery NothAmericanbald eagleplasmasample.
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`Thisdataisscreening quality only. `Only 2highlevel(250-ppb)PFOSmatrixspikesamples (cagleplasma)
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BBi pman RE TE E
`Samplesandextractswillberetained forfutureevaluation,if necessary.
000517
raceaces
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WERREPEORNTNTG FLuAsGoemCToaTRss
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AA en RE I RE
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8.1
82
AAthtamchementt AB:TaabblleeooffLFCACMTSaMScResyults fortrhemAnsalysisofEagle PlasmaandFishTissue.
8843 AAttttaachcmhemnetCnDt:: LDaCtMaSarepsortsbywoi.tJchoLneCisMaSandMKSt.aKneaalymsdaisn:
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Fdahro.ld Jonson, =n
2 7 Nh
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Ph.D, FACTGroupLeader
lala
Dae [2/99
Date.
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000518
Paaesoes
3M Environmental Lab - Fluorine Analytical Chemistry Team
FACT-GEN-008
WWIIEEAA-SSWWEE9-933.-001270 SSeeaa EEaaggllee PPllaassmmaa. WIE6A2S9W38E29633012 SBaeladEaEgalgelPelPalsamsama
662295308721614 BBalddEEaagglleePPllaassmmaa 6622993365358497 BBaallddEEaagglleePPllaassmmaa 6622993377002310 BBaalldd EEaaggllee PPllaassmmaa.
BBaaltiicc N.BAamleircica NN.. AAnmcerriica NN. AAmnerciaa NN.. AAmneerriiaa
59 ddeetsccitedd
1A6s5 detcted detected
1998
ddeetteeccteedd
120647
ddeetteecctteedd
Emn
ddeettesccteedd
| fr totqumsmm soncopy |
FFOS8700038152 LCaarkpe,Twrhooultewbhoodlye body PiSinsekiRwiivte,r,MMIU BBLDD
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FO0310
1998095
Lake Trout whole body Siskivit, MI
Brown Trout muscle Detroit River, MI
BLD
BLD
1F979880795 CBirsocwonweTtrmouuscLliever DeLmakietSRuipveerr,ioMrI BBLLQD
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11999986006644 CChaammeellCCaaftfishheegggg LLaakkeeSSttCChliirm,,MMII BBLLQQ
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FFBSO80001008811 LLWaakkieeTTsrroouuw,,hwwihhooellheebbooddyy PDiLanakmeeRiiSvuRepree,riMsolrd BBBLLQDD
1998064 Chanel Catfish muscle Lake St Claire, MI BLD
BLD =limitofdetection (approximately 1ppb)
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