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Final Report
Analysis of PFOA, PFOS, PFHS, and PFBS From Newly Constructed Wells at the Oakdale, Minnesota
Disposal Site
Laboratory Request Number: E06-0151
Method Requirement: 3M Method ETS-8-154.1 (modified)
Testing Laboratory 3M EHS Operations
3M Environmental Laboratory
Building 2-3E-09
935 Bush Avenue St. Paul, MN 55106
Requester Gary Hohenstein
3M Building 42-02-E-27
PO Box 3331
Saint Paul, MN 55133-3331 Phone: (651) 778-5150 Fax: (651) 778-7203
a
Corticato #2052.01
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33MMEEnnvviicroomnamennttlaLlabLcarbsotroartoMraynager.Wiliam KResgen,PhD.
RSeSMMpEToecAhniucral:vLoMaidc:rLhaebloclrhaoNatloarlyMePnarnsosfymeySs,suPnshealoaDl.Snlencs Ptersolnne
`Gabriel Mchuty,Pace Analytical,Lab Ops.
.
Cindy Carison,PaceAnalytiLacbaOlps,
Analytical ReportE06-0151
`GroundWaterSamplesfrom arch 13,2008 NewlyConstructedWellsnear the Oakdale,MinnesotaDisposalSite. HsdueoSmman ETE TL E RE E E
`MSTohles3ioiMnEs.nvinSnrci.ocnpsmeeeprnsotosanllsnLesaobton.rMSaataromcrphylee2x.st5rW,a2ec0tr0e6deafknoadmamnenacleyowzhecdeogOnrMotuEcnnidvawiadrotneemlrelsnsatmoanpllLaeansbodcrooalrtlnoeercaytredoibryaOWnaeaksdtaolen,
ofperfuo(PFrOAo),poerfucoroioctaznesnulfoonaate (tPFOeS),perfurohexanesulfonate (PFHS), .
AamEnindcvperesor,fnlmauenorndoSabLuoateabnoserstuslofnonMaWetaett(hePoFbdBESTS)Soukn5d1eP5rh4la.a1sbeoDErexattlrosraiycntpirdooijnoescnatnnodufHmPibegerhrPfEoe0rr8a-ot0me1ad5n1AccuecssiLn,giA3acM h.
Chromatography/MassSpectrometry".
TheSMEnvironmentalLaboratory eepardsts ofsamplecontainers rinesampinglocations
Eachsamplesetconsistedof afieldsample, fieldsample dupiicate,low fieldspike (1.0ng/mL)and
hCigh ofieldrspikse (a1p0nign/aomlLv)on.luEmacecohfeem5p0tcyMc.onCtoanitnaeriwnearsmreasrekrevdewdiftrhfea dfiml taohrersep"kiensewwheriechrtd `wiktdhafonsapapmrpolpreiaotelmaactriinxspikesolution containing thefourtargetanalytes priortobeingsenttothe. A sampleswere tractedonMarch3,2006 ndanayzedon arch ,2006andonMarch, 2006
`Table 1belowsumma thersai mplzereesulsts.Allresults forquaiitycontrolsamplespreparedand. `analyzedwith thesamples willbe reportedanddiscussedelsewhere in this report.
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Table 1. Sample Resuits Summary.
em me[STETEEETEE emowion
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Table 3. Sample Description Key Code.
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Tabl4e.Sample Observations.
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pAS2ri.ol2scoeardmauEprtexoestsurcWlaaiacnrtteiaedotrnyESTsSot5an.d1Pr5hd4as1,sae`nEDxdettsaescmsiuatocanststoaendndoqHfuailPgiethyucorononnamrllaesndacAmepclseL,sewAedorCnovxoaa,raAcirioddgusps,tiynaghdihae ss erwSaepreccihiooannlcy(S'eP.Ed)Bwrciiahsr,5t4me0.moSLfeompfePhsaaaknm.cp1ll.e0Tw3eir.ss6el)okuaasdcienidgeonapovraocachpeurdmoucrmoeancdrioitnoioonan.neTrdhaelele5r6ssoa1m8SpalPseEcsdceaoyhread5.sgdees hsfpeiacescoo,lmtfeeecotieghrdhotgdr(HoauIrnakdswv,aoatkenurdmsaerm+ppb4l0lemasnLck.osniatamalpilnveeoadlniudmlepy=iSe5gs7a)fe.caoTnhtoaexmraoafucbntrteasatoosnfdsseenodccmidbemencdps,ahHrobcvies.aoeBn,eechaeuse 4cCm0ooanmdLrrelaslosianiqmupsolttewhnsa.SdsTPNcheEonehtcrreiiamfadurigmneeidaanfgtosr3o5osx0dpr0ksarcwpiempofenoorsretbtaoeainremnxeiordnaunctrieeoscenfaorArracslrlxosaaHncmsiploarencsw,aiasrsadompalngmheddeeuaplsnipcrbasatrreeosay,llnuowofy,ieelsd ET5.0.1541 doesnatdescr samp caniigaton pioio xsacion This trodmStatiwoans
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necessaryasthesedimentcompletelycloggedthe SPEcartridgesaimostimmediatelypreventing
CcRoonmecpctlueagtraehloooaondfiSanegbpoafGltihoenywkamStaetirts:casmappelces.aTnhpedafceikndalsmamemtiphlnaendomlapstearmcpsrlhmeaeensxctrecaoctmsohnasdyaaislighotykellowishcolor. Saplswo extractedand ial anayzedan arch3,200,Th ipHark ies oraor S`SaTaannnaclecyatroedscpwruwaoeoedssru1eco5ve6tbddrheeec0Seopvannremerp6ieae00rs.e0o6sh0f%ua.spUepUpdrpe1oolrnxToAiapmnegaaotr6etf0lih0%y.ecCoAlloeofcdttaahkd nbdoci ati,nmtoeAswkti afeeniseMo Gl.adesrOnaonemnNa p.nalre3al cm0ha0t6l 6ara,tinxa2ysd0n0po6ni,,kdteenriosw C`opelxtircarictoendecbawlaiipntbrneaastaipnovenecrwsuc.rvrMeeevwta,hsAopddrbSeiapoaknreeadalun.sdtihnagtichpebrsaaormkea(neneswreiarp)B|santrakgnFd.earladamunsaet1dt0oSpprimkeepsawsraaettrhe in t12wosmamapelsesp(kE0eBs-a0115a1n-0d9180anndLE08w-e01r51p-r0e11p0a)rweerre1a0lsworoe-sexrirasctesde.leFctuedrotthreelromw0aconodrn.heiFg,ohr
thelabmatrixspikedsamples,anappropriateamountofspiking standardwasaddedtothe40 mL.
`samplealiquotbeforeitwascentrifugedtoremove thesolids.Analysisofselected calibraptoiinotns.
SaVfnermormaeathhieetfnigresaatncanusa:ryovfzehee5(n-Mea3Srw0cA7hcTwa3lS,ab2rsa0a0tmro6en)aasgneaCtieiunn.set0t.heAt5lhreunnetawyscsup.rrveAesla(tMSeaadrncmhee6e,axr2e0e0c8Fs)odreommmeoMnaasrrtchr6,ta,ht22a0e0t00ad88
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2.3 Analysis
All sampleandqualitycontrolextractswereanalyzedforthetargetanalytesusinghighperformance
liiMnqtuhiledc asbh csrbor maaGno aram pthayna dreamdt meantso Pssopg eact,r roamnea tdry(p HsPpLh eCc/iMy eS/Ma! Ss).FPaenrstiionennstainnsatyreuemedntwepadraemwesteoresd,
Tabl5e. Instrument Parametars
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Table6. Liquid Chromatography Gradient Program
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3.1 Calibration
ET e rey pene `Calibrationstandards werepreparedbyspikingknownamountsofmethanolicstocksolutions RE S B Se EeAII AA A T t e SE He TA ECSn S EgEnBrt, A re,e 3.2 Limit ofQuantitation (LOQ) SE E a SMADAD SeEsrsrr `curveinwhichtheareacountsaretwicethoseofthemethodbiank(s). The limitofquantitatifoonr EE T St 3.3 System Suitability Ar E E EE3E0nS C c ee no e . C S e Me srS n arL tsnrareipes 3.4 Continuing Calibration
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T3h5reetyBpleasnokfbslankswerepreparedandanalyzedwiththesamples:methodbanks,solvent lanks, andhepblanks, Eachbanktype isdescribebleowd. 351 MethodBlanks cSaervteirdaglemaentdheoldutbilnagnwkiswther5empir.eopfamretehdabnyolloausdiinngg4th0msiamoefeAxStrTaMctTiyonpepr|owcaetdeurroeratso haeCs1a8mpSiPeEs.. M`eexttrhaoctdibolnparnokcswesesre(rperaegpeanrtweadtteore,vgailausastweatrhee,leSvPeElscaorftbiadcgkegsr,ouincd)coTnatbamein8atisitosnthin tahreeoavceoruanltlsforthe methodbanksandtheLOQstandardassociatedwihhegiven dataset.
Tabl8e. Method Blank Area Counts for Extractions performed on 3/6/2006.
ron | pros | ems | Pres
so0s6005300s8i02255 MMaercsssaankz | vMoooonssz || wvweem || mwoz || s2w% || saemw
sestoss0t2s0eazt2r8 MMeeccssmsaurnksa || Mveooceweesa || woiwn || eomw || swoen | |amee
006600330088103020 MVeecrsistnass | wveocoess || ssszs || weso || ewse || aorn
pr06e0s20e8t0051 MMaorroostobuanncrs || vwoococoeness || msosrs || wwee || esam || wvemn
[area Counts of ighestmethodblankmuttpledbyowo |asso | goes | 1mm| wrens|
[amecomsroqumoms
| somes | sae |awe | ses |
[toocomcentasonogm.
| oom |oous| ess | ooowr |
((1B)aOwvroemeiensdiobo sateoutro86codon vegCtr Hest.Arnvertusodoathbo
352 SoiventBlanks `cSaemvyeorvaelrm.etAhnaanloyltespolevaekntabrleaanckosuwneirseiannaallbylzaendksfoamapssleessswseyrseteemscsotnhtaanmihnaaltfitohneaarnedaocrouinntstsroufmtehnet Gaftration standardusedto estabish the LOQ. 353 FlopBlanks P`rainodrsthoispapemdpltoechoellseactmiponl,eocnoeliseacmiopnlsetcoentlaoinngerwwiathsthfeleemdwpittyhco4n5t0aimneLrosf.ATShTi MsTaymppelewwaatsera,nsaelaylzeedd. `acsofndltdioinspabnldanokr.hTolhdeitnigpSbmieanisksseuresvtehsaastahensaadmiptloensamlameytehxopderbieanncke.thTthaectcaorugnettsafnoraaensyswteorreagneot etectedabovethesated LOQinthe rpbank.
F3o.r6thLeaextbraCcotinotnsrpoerlfSoprmiekdeosnM(aLrCcShs3), 2008,low (0.26ngimLnominalconceniraton)andhigh(7.5 ndpgeriseimpraLerndecodombniycnesanpltirckaoitnncigeoknnnt.roTawhtnieosanpm)ioakubendctwosnaottfreotrlhssepaaimnkpaellsyewtseewrseeirpnetroteh4pe0anrmeeix.dtaorfnadAcatSenTdaaMlnyTdzyepadneianlIwyrazitepedirciatotteph.reosLdaCumSceewtehree manashnesaemplres. Anayssofrlcate LCSs a the wospeciied levelscrossvaliatesthe
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Table 9. "Lab Control Spike Results.
samp pes
(op |_ tog) |p polm | (ropyty | ce
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ftmOmpubsCnoCnoemirssspnhee || Lioosasmoennss|| 1o0r1 || s1e0s0 || mworr | [oomme|| owms || swoe
tfomboluabbsCCoonnvmihsipsngeha || c(cCsaosoomness|| t0o1r || 9os%s || werse || eomw|| ooms || aern
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3.7 Analytical Uncertainty
`Boththe accuracy (percentrecovery)andprecision(%RSD)ofthelab controlspikeswereusedto
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