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+ AARRA2A2G-6-33663335 SHENVIROMERNeTArLoLAR0BOERAoTOsRY Final Report Analysis of PFOA, PFOS, PFHS, and PFBS From Newly Constructed Wells at the Oakdale, Minnesota Disposal Site Laboratory Request Number: E08-0151 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 xa Contitcate #2052.01 ThEaiteTstia ngreapotrttedKherooisncrm5oe0non SctateshOieofrneSSquoaiikrRemEmeonttssCofuwISbOiMeEsD P1b7o0ar26tm-1o9nr99"sGSenaesrraclrsiiSnec ih -- once ror 000006 MenvROErNToAtBooREAxToOnRsY 333MMMTEeEcnnhvviicreoanlomLenenamtda:elbMrLiaacirbhaoeartlaeltMoaMralyniagse,rP:IW.ika K Reagen, PD. ReSpMoErnvtiArGounatmoiernlMtialechLtaebloyerNa.taoirPnyasPcireoyAfSeusssniaonnWaaolSlLyleabcOapssPrscnne! `Grd Caron,PacoAnalyicaLabOps Analytical ReportE06-0151 (GroundWaterSample omNewlyConsMtraurccthedV13i,e200n6eartheOakdale,MinnesotaDisposalSte E ST E I TMSihonenlGeosMnoEt,naiIicnnmGpepneotsarallsLsaooboon.rMnSaataonmcrpyhele2ex.lst5r,ae2cr0toe0rd0aarnodmananaelwtylozy1ecd0goSrnWouEnnnidvwieactwremerelsnatmoanpllaLeansbciootlreneecirefobhrye WnOeasakteosn, oaEf1ppenrefrufcuvrooroocibaLdnaacbnoaoslrseaut(nloPfFonOmaMAt)ee.he(poPedFrEBfrSuT)rSnoto6ec.t1ral5nl4ea1sbouDroantoaertysprl(ojPeRcaOSo)mfmpoPeereifiuuoct0nri5on.ha0aatx1ea5dn1AtevcscoisonAnoktenn(FS), Amide. andSuloaies IWalesbySoldPhas Extactonsand HighPaiomenceLous Chromatography/MassSpectrometry". H"iETgshhech3fsMeadmEpSnplvieikreeonl1me0cnonntisagilnsLtLae)db.oEorfaaatcohryekpdmrpsotapymapcrloeeid.asfeietnsedorsfwasamapsmlmpealcrukpceoidncttwaeiin,heoraswffore0idhnseeprsoia:mlp(lo1in0wgihlcomhca)tioannsd fGetdhoafonrasrparoemper0isc:toleemrpceiaoovnxosnpmkdeosf oe45o0ndTcLo.ntCaoinntinagnrhseofsouerargefloarfneademsarrisrp0kebsewngesrott1ebde A spiesweroextractedonMarch 8,2006andanalyzedon March3, 2008andonMarch ,2006 `aTnaballeyz1ebdewliotwtsheusam mplmesa wtihlersbeai mrpelpzeorrte eesdis ans.Adlilscreussusitesdfsoruqumaleitry conntsrolrseapmoplespreparedand aa saan RoDhoeoAtemEmstin anCg ororrietdohCior ormi0me1e0sTotehnsTnTc ihniagrrstnotrdeeCo,foSwliOhIaEsoDL17a0o261oo858n"Gonsrsdrtnes wih wo i cows mez 900005 swenvmowEf NTALaAsOme ATORY eeoe Tabl1e. Samplo Results Summary. -- EEE Coanon|| oCins s|| Cpointyaaton||Coontgatanton cmon | camonsrwoosoonee | cow | ome | ome | cow IC ll ll ll ll pussmnois | a Soon |oamousuzoomems| aus | owe| ows| oom I Ws I a - - Semon | camonsnusvooone. | com. | cue | ous | eww re 0 |45 poses - Py Sous |camonsmsoeteoe | "amo | aoe | ous| opw oe ea 2TSF [ me Te eet]]| Soom | comonsropsoasvuerwes||_ oam Somaru |amonsromomons || om || om | o-ws | w-o ods ||ome | cow E060151.099 | |'OKMNGWSPC45DB060303 ost | oss||" oosar 0.037 %4RsbSemplarSaimpDluepLab Dup| mre | camorpesapamues | ems. | awe | ous | eww eeSPB ol ta | wa Pry EEEEE ETE] Eonar |comonsmscsomun | use pre vs -- we [Gamowspmasroaneun| ose | ser | oam | o=wn G Seoon ||ocmaomsomvmsomooomenwess|| ooomme || msne || eommsa || <owww mE LE|B ) Eos0181114 CI E060151:115 _%RSD Sample/SamDpluepiLab Dug OKMN GIVSPLAT 060003 OKMNGIVSPL41DB080003 50 ores 00796. Rt "ons. 00240 - NA 00282 - NA <0037 - 0 pT r o POAva s a05Lsothnoc orEAi yra ebpecee nsSevnSss ccio ronns swcowroam Forous orcesors 000008 Wf ny auemronENrTAoL LtisoEroTboOrReYs SeOrEnacd Svtnsommayyytmro tfp vovnPEs OKpti r.Fe.osSa (G0og tnetso rtioss 0 TSeoiSrs esr mttnr onmeoThntaPmliEonSVvyaaSErPo0aAy0ta2ep7LSnCiao)vsnoddHLAOmNRasEDRnOc..roFyeaS srdda roec,SrSoa seescspbed a O03no oy inFOS er,Fs Tn 103 nthe TBehctr eonnsScpiarottnsveTsshPmrEreiSt ynwoaEyP1rA0o0Fg1LoisOrOevteascs.nS0a 3e 0c OTEk.hay B we.SseaedisonRSSonvSAcsAiov3o7eSnn Fo 25no ytmo tvsPES rer:Fess Pn 58 srt hes 9 TShierohscrecartpteyTerPliEnSwe o1aA0k1o0n.0 Bec oan osoeyiyFo CeOdsoCnpOPTDdlseaRroeechadm en.ASOo Ss atiesn.h Bt50 wa.Sa SEA 2S a O03ro yo th FESpo. es Po 5oeacs ) Seoemosrweercbocsy xkrc. er n.Shnati an evan(KRSO) epuodh (6)LTEhaGavnvansosapARconvcretrion 0sago e sanAr tsePrrocnknss 2.1 Sample Collection `Sampleswere collectedin NalgeneTM(low-densitypolyethylene)bottiespreparedatthe3M E`naspvniikareoedinsmnoetfnhtneaillraLbeaosrbaot(roaPrtFyoOwriyA.t,hPPraFikoOnrSot,owPsnFavHmoSpll,ueamcenooldlfePcaFtniBaoSpn)p,.rbooCtpotrllieeacsttdeaemdsaistgraniamxtpsepdifkboirtngifiseeosllduwmteaitrorneicrxosenptuiamkieneisdnwgoettrhheee lacSbtoersaotoTraybrlaot3aespmrpboikvseeindlteecsvpoehnldesikofioeoryencsanoocndhMdsaaarmrcpiihinn5gsn2la0om0cp6aglteodTnea.bsSlceerrpm2tbpoelrelsso.wwedreeacdolteceibeodftioems ppirnepamraediadna!he Table 2. SampleCollection and Spike Information. CC rwcommsonioy| sore I rwo) w T w= w= oncPhisaaSotukna wwo || owmme aasso 0o1n osamz oy obmtonanne | 0 | o-me ose wor oaz pmunnssoie | 0 | oo am wr om r-- Proves mrasacr 000009. SW EWIROWEeNTrArLnLAoBOERvAaTrOeRrY Tabl3e. Sample DescriptionKeyCode. [Sanp[poltieoniocose| [fT ooowurme ts euomw sm movna s| | [[e [speesatpsoresommo somnenwsss|| FT YT [[[T T looeor i o Tm em meee ws e||| fT s onge| "CToihlteecioesudesnaadmmwepanlteerpssrwaeemsrpenldtecwseh,nsctahfmcgpleaedrodeurpeihmcaoeevwse,apaarrnidsualimaeptdlemebawefhtoeresnespxhatarskacertnieot1nu.SdmieespefeoSrsaenhaeleyss2icos2daisolo.rhmaAdolnre Tfhoemtaatloenb.lAodwdtdeosncarliyb,eisnaedsdaomnpslesobassesrovcaitaitoendsnwohteRWfSor?egaecnheorfatheedsaamfpaltesloocnatgoprse.rleu odor. Tabl4e. SampleObservations. [WC erigosteston | SodimentColer || T Sedombeneteamnoeunwt | omer | [avoo | mewn TC Age Tw | F[[T oroono [7 r mmweboewnn a POOuwweeessdes |n owwm || [rote EE1 Riamunmbo dO| SS IfPnnSoS T|R__A_w_lm | @ Coar 0msc oesitspss nbmi 2.2 Extraction ABplSrpiloofscocaenvmdapoullmroeeesstc,ynu'ctWa.ilaniBtbererdeatfnbiyEoy,nSTs4oS0tla1mndd5LPa4rohd.fasss1,aema"EnDpxedlttareeswarscmeoilrcnoieanatsltiaooendandoqduefadHPloeinhtftyuPoocerornitpfnreoao-ltmceas odnnAcdcieia Ltdoisnq,weuAm eddlrWCceahoetp xnretaorr,smaCAcl amt1tie8oddsgeue ossaki,pdneghps ntyhdhaaessse `Wioevraetctihooofennicgr(huS.tPEe)idncwfaiiatlhivao5mgleuLm(oeSfa=pm-e4Pt0ahlma,nLc,1l..0n.Ta9h,li6vs.oe5lx)utUrmaesct=dionmapLvr)ao.ccueTudhumermceaaciobnnacoteln.otnrTashtteealsndthaeorsda,malSpaPlbEcedoscbnaytreoialdgdes S4pr0iekmcetas.i,aemciqiehdodwroabuasnncdkewsn,atatinuegdseandmpsptl3lea5sn0cko0snatomampilnfeeodavnedinsbpmlikSnegensswfiefcroarenealxatrsmaaocmutpneltdessoa,sfadsmeespccmriecbnueldpplaaabrtoievsue,.atoBeewcfhaeeulsde emaadt ispnkteotsahendSPhEgch akrdmdaolrisuprkacetsopnrisormtoeaxtroatcteiocna.lAberratcosteandiardus anhgdeasbauopreamotaotrannqutavi,es E7o5ni.r5o.l1s5a4m.p1leose.sTnhoetrdeemsaciningssaomdpslewcearnetruagianteodn fpriotrhreexxtaraccttino.nwThaissdmeeetmheoddnmeocdeiscsaatriyon was anconrooma QO aA mt prcesorts 000010 i suewROWENTAL LisoREsTOeRY RCoenmcepoceretaesteslaooaadfrtinhbygasoreftdiohemnewnmtatrcoxmsplsapeitlkeelesyaTcnoodgggfeiadlhSeatSPhlEamclaaStraelksesmrGaoecsmramnamdatdeStdtehyykplreovrtingsc. `centrifugation stepdid not significantly impact the method performance. a`TSnaamepelsecpwrweooederueeovsbxdteeraeecoctnodnva6ene0rd-s6os0f%sa.l Upapnoranyozeueor6tne0Msi%ir.cA ho3f,2t08dd ,aTmhoositied fspeGdloaslraekmmsa plkemsaotr. aalnsocueerr SSoannadra weessnustedhopSaapcarethuseUppetraenpgeerof0heCCoallberacioopnCtusnSponee.tcOhn5.a2t0h05 0606o,tn1sw `extractedcalibrationcurvewaspreparedusingthe same (newer)standardusedtopreparethe RI`ocaoolmlSecapatmirponlbeaoetsptle(ersEs0p6ai.eok0w1e1s5n.c1Mnd-ie0v0t180h,o0AdGddbISliEaLa0nwnk5easOlraTyon.Spd1hrl0eae1pba1criopenbwtfearororlo1ksapainkotdesypast a1krnpga/cs1mesLs0a.eneFdsale10anrSg/remtLsrwroSeaorwcanetagaoplnwss,.iogEoh Snraomempatlehmsaritqteucsoubrlvefeo(draar1mchess3,,c2a0e0n6)noagapaiptn eshmaeohnentheewoScfoaskpv.e A(naaslfaytnsidso2f0ws0ee9ls)scaieacdmcconaesldtbteerd4a0pbtrtiois.ns SWeerahtnrsoseofa0n.3a0ag%awltahsyraenzseewnectrindve.fAL1a6n8yssr.eA sendRes ofxefoorHa o6nWMaarcel hn6, 0200088 `analysis against thenew calibratcuirovne. 2i.f3sidacumipAclnearhalnyrdsocioussmmtacaotannrdoorolalmsecmxetaarroascpptrsowngpgereraycema,oramnnedyta1ys(SHfppPoerLcCnhiMaSmAgyaIecS)ea.aPnnasortisonnesutsainnngsoiiemheedpnrttoopmaSraaonmevcteeeris.s prt dm Table 5. Instrument Parametors [iosomonthomeTeresa] [oE untcouma -- |Csor TicTisT esmmr osoumn m| [[tlsesemvcmromems[ r |L opmaenmerE eorion | [[o[ 1 noseowses ptuo bospmy | [Copoonayn 1TTT emgiae J| Tabl.e Liquid Chromatography Gradient Program [a= T | TotanleTyiT me |m "FlUowRyate | oPsercemnt A ee ' FC [ oTaeo T Te sow o mTT e sa e tooe s | w2w0ee0s ]| =eTes [aw | so | a0 | CT m0 Taw 1 wo 1 200] [r-- Siri meorn 000011 wy, F-- E-- Y Tite. a Trntons [om [m= Tommi] =) [ [o ow me e T Ts s] ] Pros [[e o[ wee T Tw as w ]| [om ws oTs s| FOR [ [e aswowsT|as 2s ] T oweT s TE eS s vse e e tt Tens E 3Data R AralysiA s TT D TIT EHh lg ] 3.1 Calibration P e m e e Shee s a r Co IE s TeLl,ATs e SeTcHOiDreiroee ,AgoAni va er , v eovAsg, `Calibrationstandardswerepreparedbyspikingknown amountsofmethanolicstocksolutions Sr e lrnhe CSrEE celrlrot srobe `correlationcoefficients (r) weregreaterthan0.999forall analytes. SrP3i.EeR2eOLyLNdiTmTiAOetPa oefPcQooSuaSnS atoirStraetHind onUe(LOieIQ)S a54:1oO nrSyo ad e nrs cca S serse nin P Si3.3SniyshStsemercSuirtaae biliatygnessceisLSce rTnsrTTorevsaoesrvyteuieongrfsenereirl E S3.4tCo2a ntinun ingCCaleSibrEats ionrpece p ssrtrs e r trrae onttten sr aereis -- Cragg E33 aero 000042 ECo TLnBORAoTORY T3h.e5roopBaelnasnodfkaslear.ksEwoerhparnokpapredadn aanalryz ewosiwhsame: thdbasrhekbla,rks 351 aodBlake SCeavebireaglsmaeatnhtoaadvbreargrskbwsiawhreerdpfiroeaerekndabtdeylhaedsiiSnnggt4s0 osLbmooeACSRTTaWcTiyotpnpeaOVGametrasciao5 1haeCo1Sv8eSriPsE r idsSarvcsaihacmtam ondGbe ssoiucaoen c,aStHeEtoicueav,nodk)tTo5e 16s a encoun oxo Tabl . MathodBlank AreaGourts forExtractions perfor on 81205. [empTot wrpun i |on r aee scums |e |s| owznss ray | wmoootus | wodbums |o[wroesm || |orsmns | vona || wn | vweze || we | wmwe || sw nweow |e eeaszsy e|Wnedndobwomss mama |||voWrooossumwrrsas ||| wwwm sun || | woom ws || | mwsa ww || | wamw wm omamy | a|atieanss |[uvoouoers || mooms || wwwee || asww || seenw oimeCCousrscgossttnsadik dps || stoormne|| oeswses |osviemsr| soemn]] 1B1. aDartmsuetioossetter 35krn angDsGe i ert 352 soventBlanks SoeveoratlrontBhaaoylndspcvoeensttbstasrokastnwseshrooraanL2eo6s410Soaslso erseto0ncohantrlatoarorGeatnoft 353 For Banks oereltipsaemdplirekcaoTcoooni,lcnrtsoacsmhpalseichoosioanminbriwtainsof)l ewyiinoc4o5a0atsonftATSaHTscMceTaysn orwaaaylseAs arsanegzld, aihoonsoewtakarsmLO sinkop oarSos my vp. Th gtaafwaeresck Foeo3.6mparcLogamob csCoksoniotnprowonalorSepiskBeonshrtca(soLcnoChtfSsS)2ak0n0y6a,weIaswr(l0oa24p5na0g..BofAynSomTiHaloTcnac0cen1atten0).aL5nCdSGhWi7t.5 edraamSaamnesTAnrsypkeeaowfatkrestamspLeCsSw%aaterhaarpvaacioddaenvdaal noysss v1i1hteama8 RECs 1000013 auemmomeeNrTLLisomsTORY aFn5e8astetcaoamelthfoaeeatasofsodmaiooaeafoorrcavnyr8,m m2e0t0h0oodxa raccairaasa k.nLSCfiSa oromnEeT37Sc.n 81To6fa4ol.vm1s,heAsadMudreromcniahalce,2bL0seC0S8 Cation a kv ers 51 sa es ir 06141 36. Table 9. "Lab Control Spike Results. poi I Ee =I ] Tnoinmooamiripse inom ||Li|ooLsstsoiaosammnsrs||| aowoe|| owe | otomo || own | wo | o[omw || wa | ow | tioer || io | mwwew Immooiimmcmosmoms|| |LLicccooovmmoounnmsse||| aasmmm||| saomww||| wmwiee || | esww || ow | owme || wwe wi | iw [agosmucomyenmsn |wows| seme | 1 PHS ic [pes| TomtaoGanton | cso?| 1m | ts | dw [os | tor | ws TT1IpropobmmLmiaobimCtocmnmetororomltmSopmiknemm |||| LiiiCcccSss0s6ooo0uu3usm0m6nn2ssd. | || td1[.ooo0rrn1 ||| omvmme || om | wo0wr | [0a9o0m2 || we | sm | 1oi0w8 || ow | 08 swso amon | ico| 1 | sos | oa | om | oe | wr fl rehag dtl ep (1) Aresultsandaveragevalues sted1gtoesigricartfigures: 10EPAfounding ies. or RSDvaluesgivenfo wo. Sp ---- Los! ONY = piaConcentration 10 Loren. Sstaodiotn Sctsppilcoeas. SSe3Co.ah7TonaeicAnsvaamoslnnyosartrvaiecraaplemnrUconeoncdrtesrPrtecOaon ivnebtrya)saenprLoa dCsSiroeno(ek4as5vgDao es)nGf7sh4n6aa.b3c5oF4nr.toTal hpenseswhseeeerosuv,sepreredciosion RSSDa)mOir:asses ceemin 2325 range he sons. 7443281007, 974-326=0420 ween ER motsorn 000014 wenoHLsomSos Thusa,nLdOsStaccruraacysrowuhtesnrcaangmepfemd 6S402551e10s7%s,Tao aback irofhocwd Tio0cmtuemss00% E GBohTRaEGnSFiSToarnsa.oS. orarvia uatracnayte ion.PoEsOKdGarn,e 101040S257%5f,y b09e4n50s and 100 6.6%,respectively. 3.8 FieldMatrix Spikes (FMS) Low (nominal concentrationof1.0ng/mL) andhigh (nominalconcentration 10 ng/L) field matrix `spikes werecollected at eachsampiing pointto verify thatthe analytical methodisapplicableto the pCraielismtirroofynuetr.cnoFmapomaratrhsoskaosleAsmatmiinc5eGnMreLaesbro armioTnhgtoatsooc snswoTiRhOPLaDclcroonnn .(loutaedSampleConcentration-AverageConcentration:FedSample&FeldSampleDup) . Th le Tbe1010) blow smthsrlrut fold mati cours an ah `matrixspikereovoeries(ifapplicable)fortheninelocationsas wellastheTripBlank. Eachtable providestheaverageconcentrationandtherelativepercentdifference (RPD)orrelative percent `standarddeviation (RSD)ofthe sampleandsampleduplicate (andlaboratorydupiicate ~ifapplicable). Allfieldmatrixspikerecoverieswerewithin 100:30%forallanalytesexceptforthehighlevel PFOS Tiotmreaancssescsroeomoera iPhFFOASrLeMsSaIDsF EcO8o015t100wwailnaeoohaniodnoo 1% lowfieldmatrixspike, aswelasthe lowandhigh levellabmatrixspikes,producedrecoverieswithin compos JHE macros 000015 ---------- NY VE Dfo o[dae]llyl feanllel 5J] woldiil tplbyl))ii jlafl u)el Fpthe]ein ii i 2 2 Hib y EEL Eo fied Pl PLE LE : dEaiilii l F| L if BETH 000016 or oFodoewll ll el egllI. Hl jel ad Sl ded ha it e it BEl lpisan 3H ) gHn rte AE i HE i Fi ied ; Li i : : 8 deeifh foore i | i to141] : jiiii il : 1 fut]Llil | ia : FT i HE ; bE Fooldmd Teele 8 g |Bg Jet et ; dFidl (feill) ell Tae stl Le 1 Hae ik jl) gfe ih A J: d(uIEiEE2i)| dioifiian 22 i fairio i iid i | LES gi : Bde 3 jg2228 ig tl fitt1e9r) H :i odor or 1 gees=e 3L1E fg om4 {iC Li HE| R pRE aa :RR L BrrreI n qiE d en i FHL =e i IE | | oa el | im | [ae | { | - i . Lo L | ord soy ig i i : ol ) :a [B olJii elodaki i i |i) Wi ii i 3 Ji: if dais HH on MENROWENeTrAaLLtAeBOREAxoTrOeRnY .= LPTaFhbOoerAaa,tcoePreRyaOccSoyn,atPnoHldpSsrp,eicaeinssdiwoenPwrFeeBurSostrehedestnuousdsfeeoerdtrfhmoeiecnsoelitlmheacetmteeedhtsheaoamdpnalaecysctuwcreaalrceuypnarcneedsrteparneitcneisdiioornntThafebolrraeelsl1uatnasl(y1t0e0s.+ 5Sp.i6k%eroecroPveFrOieAs w1i0t0i2n31.070%%3or0P%RdOeSro,n1s0t0e+te6.d6t9h%aflorhePaFnHaSl,ytaincdalm1e0t0h1o.6d6w%asforapPpFrBoSp)r.itFeifeolrdhmeatix givensamplemat. A0l3rMemEaniinsionngsmaemnptalleLaanbdoarsastoocriysattaenddparorjdecotpdearattai(ngarpdoocoepcyiaensd.electronic) ilbearchivedaccording scone moe rrorse 000022 Ea 7." Signatures d [yy Sodo TVS S3 SLiTte SwenvRonEE NTA. gon raTOnY | | | i i vy Zefos |i 4 i NY BiL e rLiga y 3a;, i ! Wii ka KCReagen,PhD.. EndronyentalaboieyManagement R Toer ii| pTihcek2MyEnvironmentalLabeotory s Quaity Assurance Unithasaudited heda and resort frTis ii Se AN BEGOO S eesmrt E Se divers ail. 00023