Document ypNkKMz6m26e6GGN14GzbLyVX

S1uEenyvepoanrmioonntss, athsnd S0C FCoarM,N 5k1i6n8g100202025017 aM MMaayy 55~.22001155 UPS Next Day RMer.meGdairaytiKornueDigveirsion M5RMi2cni0mnnnLeceasdsfo[oaatt~yaaoePPtnooellDlR:iu~ovtaiiisodoinnoNaC Coornattnhro.lt AAggeennccyy S5t20PaLual~, yMeN~e 55155 Road Nor~: St, Paul, MN 55155 Re: 323M 0M14CCooAf*nranagugaeelGGrPreoorvvfeeTaSSoiirteeos((hSSeiimtteei))cal (PFC) Groundwaer, Pore Water and Surface Water Report `And2014 At~d Response to Comments on Aarma[ Perfla~roehemical Response to Commems on the 2013 Annual Groundwater Monitoring Report (PFC) Groundwater. Pore Wat~:~ a~d Sur!hee Water the 2~ t 3 Aanual Groundwate~ Mot~iloAng Report Repe~ Dear Mr. Krueger: EGEnr~coclu~onosdseweddatppellree,aassPeeorffiiennddWaSttarereereea((n33d)) eSllueerccfi~uoocneniiWceacctooeppriieeRssepaao~nrddt~tfhhorrreeeeth((e33))3hhMaarrCddocctooappgiieeessoGorffottvhheee S22t00e~1.44 AAnnn~uuaNl PPFFCC Groundwater. Pore Wa~er and Surface Water Repo~ {~r the 3 M Coemge Grove Site. IG1:nr: oaauddndddiiwttaiiootnne,.r,:t:i:Pisosrel[eeUWeaer:t'epprrraoonvvdiiddSeeussrfaaacrreeessWppaootnnesr~e R:teoopoArAtEE,CCwOhOiMMchccwooammsmmteernaa~tn:sssmooi~nt:cdtthhteeo 232{0M71133viaAAnerrnoaumiaall:daPPtFFeCCd GOOprcrcitotmoeoabnbredierwlrya11mi33n,r:_2t2h00Pe11o44fr,eorWf:m?rooaor~fmeesr1tumhhmeeumdMMaSPrPuCyrCPAAad.ci.escWTTushhaseetieorAAnsREE.eCC~OSoOprMeMLciwccfhoiocimmem:tm:eewenmntastsss i~onoannt:shttmhehreeiad22ei00ds~1c3:3uossaa3innMonnnuusvaali:aa erreeemppiaodo~retltntdwwifaeeir~reeed aa1p0nrnidMmdaPaCrrreiAelsys.ppooinnnFss1oeehreiisscrrraeeselfe}:eeorrfeeonnfrceeseefmdderbbneyymncppaeaaw,ggceedocuimsumcmmubesbnesetirrosaannnos,rdd dtooSipppsicieccuislff?irioccomnmitttethmheeemsirrsS~SepeprNthtoeevemiimrdbbedeedirrscb88ue,.sl22so00iw1o:4n4a,s.rmemae~femomol:odlrroeaNwmne::ddd~uuebmmdy at3~noMMdPMa'sssP~rCaeeApsspp.rpoonopFsr~eoi..rateeC~C,ls~aeiarn~oitfif~hyreiienn~aggtrte~ianncBfchoe~erd,maea2toti0oim1on4nmarreneenngg~uaaarrolddriirnndeggpisottcrhhtue.esss~eieecnoomimtmm-e-ensmtpssrowwvaais~dei~dnncebl[euulddoeewdd,.wwwehheefroreello~pwosseisdbib~bleye and as approp~ate, in the ~ttached 2014 annuaI repot. AECOMComments Hi[{neetemmrpr11e-(tapt(ipaoagngoeef11ro,eGsGurlros~un=tdh~waaapttreeesrrenEEtl|seevvfaaitn{id~oinnnsgs,s, o11~n ppthaaerraapggr~roa'dapupchht))i::onTTwhheeerlreelsiissab~riooliddtiyisstccouusspssriiooovnnidooerr mggrr~ooueu~nnddrewwtaaatttieeorrnppotlmfu~mrmeesuccioo~nnstt~aaiqinNnmmepenrntet.s.ents f~ndings on the productio~ well's ability to provide `3GMrouRnedswpaotnerseSamtopliCnogmPmleanntf:orthIenSiatec,caorPdearnfcoermwaintche EtvhaeluMatPiConAReappoprrtowvieldl bbineetsesruucbbemmpititi~toeenddstty#osttthehmee MMhaPPsCCbAAeeononninaasnntaaallnnennduuaaanlldbbaaisssiif.~sulaaljfy~eeorrpettrhhaeeticcnoogm~.p&lTeh,tteee Pggerrroofuuonnrddmwwaaanttceeerr tEinhvaatlpuraotvitiioodnneRs~eapvosstretumwimhlalmbs eaobefsreutnbhymeiingtstrtaeoldulenidndwaaadndtdietriisoqgnu~atdloityatynodpAaetrn~a Hafonlrg.tMho~enaSittePo.reirnfogrRmeapnoeret AAEvssadldiuissacctuuissossneeRddeiipnnortth~eewiGGlrrooiutntncnldduwwdaaettehererfSSoaalmmlpoplwliiinnnggg PPiln&afnnorf~moarrtitto[htnee:SSiittee,, t[htee PPeer~foorrmmaannccee AnneRvaelpuoartti~onio!tfisnictleu-dweitdheehyy~dHroogwe#otl~ogi~icfoarnmdar#e~mmediation systems. ~ AAnn ea~ssaetusasm#etmntooffsPitFe-Cwimdiegrhaktdi~oongienolgorgoiuenadnwadter. orion system. + An asses.~ment ,~PFC m n in groundwater. Exhibit 3630 33663300..00000011 MMeE.CGAary Krueger Page 204 May 5,2015 An evaluation ofthegroundwater remediation systems with respect to: TT_h~ee eefJf)~eccttiivveenneess~so~foplluummee ccaappttuurree bbyy ~thee eexxiissttiinngg s~yysstteemm((ss)).. increase in pumping. MMoodidfifiiccaattiioonnssttoo ppuummppiinngg,, bi~fnneecceessssaarOy,,, iinncclluuddiinngg tthhee rreedduuccttiioonn oorr iTnhcereaefsfeegcnt pfurmompinagn,y of the removal actions that have been cTohmepleted.t from a~, ~f the removal action~ th~ ~ave been A discussionof the effectsof remediation including sediment removal fArodmiscthuessEiaosnt oCofvtheeanefd[~gcr~ouondfwraetmeerdeigxttiroanctiinocnlfurdoinmgPWse-d0i9m,ePnWt -re1m0oavnadl ferxoim stitnkgopEroadsutcCtoivoen wells. a~d grou~dwate~ extractio~j~m PW.O~ PW-IO and Doecxuismteinngtpa~toidounetiot.h~atwt~rllesa.ted groundwater is discharged in accordance with state requirements as stated in the RD/RA Plan. AA20nn13exttoendFd~eeddbrppuiilaioorttyppu2um0~1p4tteetssott pdreotegrrmaimnew~,aatssheppeengruffomorbrmemree,dd aaattnt~dhheeflSSioittwee~frarotom ems,FPeo~bfbrewuueaalrrlyys 2013 t~ February 20!4 to ine the number, ~nd flow rate.~ of well~ nmeeceeessssaar~yttooffM ulffi!llll 33AM'!'ss ccoommmmiittmmeenntt uunnddeerr tthhee sseelleecctteedd ggrroouunnddwwaa~tee~r aal#teerr~naattiivvee J`oprrotghreamSiatned(ArletecronmatmievnedGeWd-1g)r.ounTdhweatreesrulitnsteorfcetphteioenxtseynsdteedm pwielorte pduimscpustseesdt sdduuurmriimnnaggriaazpperrdeessieennnttaaattdiioooncnummmaeadndete tttooilttehhdeeEMxPteCnAdeiidnn GJJurutonnueenaadtnwtdadt~NeovrvePemimlbboteerrP2u200m11p44,,Taaesnntddaaanrrdee Design of GroundwaterRecovery System, CottageGroveSite, providetdo MPCA summarized in a document titled Extended Groundwater PHot Pump T~t and Design of Groundwater Recovery ,~.~em. Cottage Grove Site, p~vided ~ oo~n MMaar~cqh~ t17Z, 2200115. oInteomn2c --fi(gpuargee(2c,urGrrenotulyndtwheasteeArrQeuaasliatey,i1denptiafriaegd ruaspihn)g:diBfyfeirdeennttimfaypinsgseyamcbhoolfsthoenAtrheraese ossseenyDpsaoatrrneaamc~teeafinfgfdiig~gpuucrrree(osscv))ui~utd~esaesniitnnglggyressathhhtaaeeddrseiidnnAegggrooerraesoooufwuttcelloiinnniidsinneiggns_,ttiefttinhheceedyrreeubsewwitonowuguelledddniffbbtceeerxc!aan~assnii~mdmappfplilisigffuiisereyeddms iibddoeelnnsttiioffniiccatahttirioconen ays~em and provide a greater degree of consistency be|wee~ re{ a~d figures 33apMMprRRoexesisppmoaontnseseelottecoaCCtio~ommnommefneeatnct::h Aarffieigaguurrreeefewwriirlleldbbteeoaaiddnddteehdde tttooeffxtuttttuurree reports reports 0to show show the tl~e approximme location of eae~ area referred to in the t~:t. slIihteoeunmld33 ---pr({oppvaiadggeee 22a,, rGGerfrooeruuennndcdwewaattoteerMriqqnuunaM elsitoi~yt,,a44D~e' pppaaarrrtaamggerrnaatpphho)tf---HeGGarmlotu~hndd(wwMaaDt~eHerr)qquuRaialsliikttyy L~biblmileetsss should provide a reference m Minnesota Depa~mem ~f Health (MDH) Risk I~Jmits (HRL). 3coMmpRaersipnognstheetSoitCeogmrmoeunndtw:atAesr pdarteasetnoteMdDinHprHeRvLioSusisrneostpoanpspersoptroiactoemfmoernttsh,e Site since the groundwater is not comparing t~e Site groundwater Site since t&e gg~undwater is nat bing used data to being used aass drinking IIRLs ~ drinking water. not app water. te fo~ the 33663300..00000022 S3MUMNMON105195955995511 MMrB. CGAary Krueger Page3ofd May 5,2015 May 5~ 20 i 5 pI|trteeersnmen33te--d((ippnaaS~geeect22i,,oGGnrr3oo.1uunndddowewasatnteoetrr iqqnutcmallhuitdtyey~,un$5i"t~sppraaerrpaargegsrreaanptphih)n)g---tThTehheenuhhmyyeddrrriaacuOall~iccvagglrruaaedd.imenmt vvaaliuuee ~resemed in Section 3. t does not ~c~ude ~dts representing the numeriea~ t33eMMxt;RRehesoswppeoovnnessree,tt~tohiCCso~mmismmeaenrt~d:it:menTTshhieeonualennsiits~s'ffepeeaetrtappmeeerrtffeeereettaO(nf~dif!)u)nwiwit~lstl[ abbreeeaaddndodeteddattloowatthyhsee rt~epto;rt~edo.wever, t~ i~ a dLmensionles~ p~ra~ter and ~ni~ are nat Mways III~ntecemlmud44in-g ((appnaaaggdeedi22t,,ioPPno~arlreeseW\Vnattaee~nrec/er/SStuourtrffhaaeccleeatWWapaat~reearrgrQQaupuahaloliifttyyS,'e, c11t~ioppnaar3r.aa3ggirnraadippchha,.t33irn7agassneennnutetanelcnepc}oer--)e wai~nlcat~~eeneuxtrd~aitnondgdpeassrnuufrrafNodarcdcmeeitaiwdoadntiateliro~ssnnaaa~mlmepapnlniciniennuggatolwwtsiihatlelmcpclaoolsmnittnipigr~n.auaraee~ii-~nap22h00~o15fwSwoeoucutlliddonpprr3{o.~3vviiiddneedicclaartiinfgic~atuioM n onpothree. ~mem m ~rfo~ addJti onaf annum sampling. 3`aMnd RinesmpeoentsiengtsohCeoldmmwietnhtt:heAsMPpCreAs,en3tMe'dsinpopsrietviioonuiss rtheastpotnhseesefffoecctoivmemneenstsso,f atdheeqSuiatteelrye.meadsisaelsascetdiviutseistnhgatghraovuendbweaetnercomeplleevtaetdi,onanadnadregcroonutnidnuwiantge,rcaPnFbCe msmoaonmnipitltoiornriignnggwiddlaaltta~p.r33oMM vidddoeoeessannotatetcaahggnrireceeaetltlhkyaatsaaodddudintidtiioobnnaaasltippsoorrteeo wweavgaaelruaaanttneddssteuuhrOef~rarcceeemwewadatiteaerrl alternativesws~ellepcrtoevdifdoer taheteSicthen. &Asalplyres~eonutnedd 1h0ats~he" MmPCA in tthee ptahset,rweimtehdtihae! occboolmmipgpla&ettitiiooon~ns rso~eefgfattrhhdeeinSSfgoeeppprottrteehemmebwbSaeeitrtreer.22/A00ssu1!r44pfrassecasaeem~wnpalltietindenrggtosarrtmkoopeuulnniddn,,g,33aMsMisnphheaatc~ssiefmmpiee~edttti,nMawlSltietc~ttthhiteehoiinerr 4.2ofthe MPCA-approved SamplingPlan for the Sit. obligations regarding pare water/su~kce water sampling, 4.2 of the ~PCA.approved Sampling Plan ~r the Site. as sp in Section M~Iitesemsmis5si---pp((ippRaaiggveee22r,,PPPoororereeWaWWtaeatrieerar/n.,Sd'SuSuruffrfuafcaceceeW WWaaatt~eeerrr QQSuauamalpiilitteyy,,Re22s*ul~tpsaard~aogegrsraanopohht,,inI1c~lu~sdenenttteeh~encueen))it---s ~pMrreeisssseeinnsttseeipddpbbiyyRttilhv~eeernnuPummoereerriWicc avvtaaellruuaeenssdiinnSccullurufddaeecdde iW i~n NtthheeertrSuaabbqlneep.~ e Resu|ls does not include ~e mnits p33rMMeseRRnetessspptoohnnessveealtt~uoesCCoomfmtnmhmeenenntut::merCCioocmmvmmaelenunetts nnaoosttpeeaddr,,tsaaprreeervviibssieledldiottanabb(llpeepbi~)s.aattttaacchheedd aanndd pre.~en~" the va!ae~ of the numeric values ax parts per bitTion (ppb)o RIetpeomr6t in(dpiacagtees2,tFhiatndbiansgelsi/nFeutgurroeunCdowuartesre,opfAocretiwoant,er1apnadrsaugrrfaupceh,wa1tesrenstaemnpclee)s~wTehree aconldlescutrefdacien wOactteorbebras2e0l1i2n.e Asalmtphloeusghwetrhiescioslalceccutreadteinf2o0r0g6ro(uwnidtwhattheeresxacmepplteiso,n poofrIeWw-a2t5e4r amnudd )wwiit~hhaa coommpplIecttee ssaammpplliinngg eevveenntt ppeerr~fobr~meedd iinn 22001I11.. 3evMenRtepseprofnosremetdo CinomOcmteonbte:r 2T0h1e2rperpioorrttuosetshethsetatretrupmo"fbatsheeleixnet"enadsetdhepsialomtppluimnpg testprogram in February 2013. 33663300..00000033 3M_MNOt595952 3M MN01595952 MMeP.CGaAry Krueger Page dof4 May's,2015 IIAtteEemCm O77M-- s((uppgaagggeeest22,,thFFaitinnfddoilinlngosgw/siFn/u~gtucurormeeplCCeootuuirrossneeaoonffdAApcrctetiisooennn,t,a1tt'i"~onppaaorrfaagtghrreaappehxh,t,e33n~daedsseenpn~tueemnnpccee~t)es--t `ArreepEssuuumCllpttOsis nMtgtoo sruMMagtPegPsCeCsA~Aa,n.~dht*ahh~taah~tteblffaliuaobttiwuulrriieetnygaanno~nnfouwmatalhlpelrreeetpipr~ooonrrdttusmsc~tiidinnoccpnllrueudsdweeeenlVlaasadtditioiossnccuueefssffsseiitochotneniveroe~xlff~yepparprdooredodduvucicptdtiuieoomnnpplwwuteemelsielIt p`cMcouPommnCtNpAaiin,nnmmgaeensrnta.utt.mesFFmuuatarrunoyrdroeeftaahnnaennnuunaaaub~laillmritpeyFop~or>roet~fsswa~sSthhheeooruupallrnddoddaa~lslassucoortfioiainnnccce~luwwuddaeeetl~,elsraasss~oappmrrepeeflvvfeeiiocorutueisssvluleylyltysr>.eepqqruuoeevsstitdeeedd bbpyylum~theee MPCA. a summa# of annuN pore wmer ~nd s~h~ water sample resnlts. 3M Response to Comment: See respo1n0slteesm 1 and Item 4. Ithteemre8su--lt(spoafgeth3e, GeexnteernadeldRpepuomrpt Cteostmmweilnltsb,e 1d*ispcaurssaegdraupnhd,er3"sespeanrtaetnececo)v-erA,ltahobruigehf dtddhiiiessscccuuruesssssssuiieoo~dnnsotohforftfothul1ngeheheoeeuextxt~teetennhnedddeereddedmppauupimmunpmdpiepinnrogg{fetst~eetsshttwewwirloeloupuolbtreddt Npprrsoocvviuiddsees~ccoonunt~teaedxxettr ffsooerrp~tahreeatrreeevvciioeevwweere,rr aaassbii~tt eiissf discussed througho~t the remainder of the repo~ MPCA 3waMsfRoersptohnes2e01to3Cmoonmimteonritn:gTphreorgerpaomrtadnidatthweeaxstseunbdmeidtptieldoitnp2u0m1p4tteostthhead not Sbbeee~pennteccmoobemrpl20e1t4aeaswdsiotqfhft~thhteee eceonnlddloe~cftf2i20o01not33.f,tTThh~eeefienxatlepndodeerddeppwiialltootetrppau~nmdppsttueerssftta~wceaasswCcatoemrpslaemteptdlieiindnng. SR`TReeespsMtueealtmt.n~sdobosefDfrteths2hti0eeg1ppn4uuowmmfippGtthrteeotshsuttenaadcrr~weeasstuuemmrm~aRnrerc~iiozzfveetehddre3yiinn~SnttyahhsgeetpEeoxmrrteeepnwoddareettdderGsGrau~obnomuduinstndutdwrewafdaattcteeoer~MPwPiPalffCtooetAr PPsavuuimma ppcover. eTtetsetradnadteDdeMsiagrnc~hf1G7,ro2u01n5d.~ater ~eeoveO, ~o~ submitted to via cover letter March 17, 2015. 1you haveany questions regarding his information, pleasecall me at (651) 737-3477. have aay questions regarding this h~|brma~km, p[ea~ earl me at {65I) 73%3477 Sincerely, EKanrviieroBnlmoemnqtuailstE,ngPiEn.eering Specialist CCBEouo~riqvpl3iodrorioran~atgmtee2e2EEnn4ntva-vil5irrEWoo-~nn1gmm7ienenenttlaralilnPPgrroSoggprreacamimasslist Building 224~5W~ i 7 Enclosures Ce: MMirr.. SForenddeCsapmpBbeulln--MmPMaCPACnA MMes.. GVeirrgailndiaShYiankglein-gM-PMCDAH 33663300..00000044 3M_MNO1595953 3M MN01595953 bee: GJ.AK.esHaornie-nsWteesitno--n 2So2l4u-t5iWon-s03(cover rly) FM.AA.. TNeaysahb -- 2Bi2c0k9eEl-&02Brewer MJCR. KYotesamgietrh--22220495E-W0-217 33663300..00000055 3M_MNO1595954 3M MN01595954 eprosimate rHEn Sm Senna sdScWat Sem ee SEE TEE [ wm~E~ EL E rE EEEE EE EEe Eo= EEatEm E taee eS]aSS] Elz Pa | Foote fw eo ae a PFOS FEE EL I3MM__MMNNO011550955095555 33663300..00000066 enoAEmR Tr een i 08 fre ona eT ~~Ere [~F ~ E Te Le E TE EE CeRbbanibalg Elite Et Hm. Tm mr ens IETS mins re -- 33MM__MMNNO011550955995566 33663300..00000077 GROU2200N11D44WAAANNTNNEUURAA,LLPPPOEERRREFFWLLUAUOOTRREOORCCAHHNEEDMMISICCUAARLLFSSA(C(PPEFFCCWssA))TER REPORT FOR THE GROUNDWATER, PORE REPORT FOR THE 33WMMATCCEOORTTTTAAANGGDEESGGURRROOFVVAEECESSIIWTTEEATER CCOoTl-TrAAGGEE GGRROOVVEE,, MMNN AAPPRRIILL 22001155 PPrreeppaarreedd ffoorr: 33MM CCoommppaannyy PPrreeppaarreedd bbyy.: WesWWtEECShSeTTsOOteNNr,SSOPOeLLnUUnTTsIyIOOlNvNSaSn,,iaIINN1CC.9.380 West Chester, Pennsylvania 19380 WW..0O.. ##0022118811..000022..119977 33663300..00000088 SW_MNO1895957 3M MN01595957 TTAABBLLEE OOFF CCOONNTTEENNTTSS SeScetcitioonn PPaaggee 1 INTRODUCTION ummmmsssmmmsassssssssmansansammsmsonmonnassons 1 INTRODUCTION.......................................................................................................... 1-1 11 PURPOSE AND OBJECTIVES OF THE SAMPLING PLAN 13 1.1 PURPOSE AND OBJECTIVES OF THE SAMPLING PLAN .......................... 1-3 2 SAMPLING PROGRAM cocormmmmensmomsmsmsmssmmomsssmsmssemmssonssons BL SAMPLING PROGRAM .............................................................................................. 2-1 21 GROUNDWATER 21 2.1 GROUNDWATER .............................................................................................. 2-1 22 PORE WATER AND SURFACE WATER 23 2.2 PORE WATER AND SURFACE WATER ........................................................ 2-3 3. WATER MONITORING AND RESULTS cuvovsmsssrsmsmmsmssssmmsssssmsssnss3in-s1 o WATER MONITORING AND RESULTS ................................................................. 3-1 31 GROUNDWATER ELEVATIONS 31 3.1 GROLVNDWATER ELEVATIONS .................................................................... 3-1 32 EXTENDED PILOT PUMP TEST 32 3.2 EXTENDED PILOT PUMP TEST ..................................................................... 3-2 33 GROUNDWATER QUALITY 33 3.3 GROUNDWATER QUALITY ........................................................................... 3-3 331 Background 34 3.3.1 332 DUD2 Ares 35 3.3.2 333 D9Awa 36 3.3.3 334 WWTP Area 36 3.3.4 335 DSArea 37 3.3.5 336 DSArea 37 3.3.6 337 EastCove Area 38 3.3.7 Background ........................................................................................... 3-4 D1/D2 Area ........................................................................................... 3-5 D9 Area ................................................................................................. 3-6 WWTP Area .......................................................................................... 3-6 D5 Area ................................................................................................. 3-7 D8 Area ................................................................................................. 3-7 East Cove Area ..................................................................................... 3-8 34 PORE WATER'SURFACE WATER QUALITY. 38 3.4 PORE WATER/SURFACE WATER QUALITY ............................................... 3-8 4 TINDIISmmmmssssssmsisssmmmmmssmntel o FINDINGS ...................................................................................................................... 4-1 41 GROUNDWATER ANALYTICAL DATA a 4.1 GROLVNDWATER ANALYTICAL DATA ....................................................... 4-1 42 SURFACE WATER / PORE WATER ANALYTICAL DATA a2 4.2 SURFACE WATER / PORE WATER ANALYTICAL DATA ......................... 4-2 43 SITE HYDROGEOLOGIC CONDITIONS. a2 4.3 SITE HYDROGEOLOGIC CONDITIONS ........................................................ 4-2 5. FUTURE COURSE OF ACTION ceovovsnmmmsssmsmsssssmssssmsssmssssssnssnss$n1s FUTURE COURSE OF ACTION ................................................................................ 5-1 LE TR -- | REFERENCES ............................................................................................................... 6-1 33663300~.00000099 3M_MNO1595955 3M MN01595958 FFiigguurree FFIIGGUURREESS PPaaggee Figure 1-1 Site Location Map ................................................................................................ 1-4 Figure 2-1 Groundwater Monitoring Network ...................................................................... 2-5 Figure 2-2 Pore Water and Surface Water Sampling Locations - 3M Cottage Grove Site.. 2-6 Figure 3-1 Well Locations and Site Geologic Map ............................................................. 3-10 Figure 3-2 Groundwater Elevation Contour Map, January 2014 ........................................ 3-11 Figure 3-3 Groundwater Elevation Contour Map, April 2014 ............................................ 3-12 Figure 3-4 Groundwater Elevation Contour Map, August 2014 ......................................... 3-13 Figure 3-5 Groundwater Elevation Contour Map, December 2014 .................................... 3-14 33663300..00001100 3M MN01595959 TaTabbllee Table 2-1 Table 3-1 Table 3-2 Table 3-3 Table 3-4 TTAABBLLEESS PPaaggee PFCs Groundwater Monitoring Plan ................................................................... 2-7 Depth-to-Groundwater and Groundwater Elevation Data - October 2012 - December 2014 ...................................................................................... 3-15 Summary of Groundwater PFC Analytical Data - October 2012 through October 2014 ...................................................................................................... 3-16 Mann-Kendall Trend Test Summary ................................................................. 3-19 Summary of Pore Water and Surface Water PFC Analytical Data ................... 3-20 AATTTTAACCHHMMEENNTTSS ATTACHMENT A SUMMARY OF WELL CONSTRUCTION INFORMATION ATTACHMENTB PORE WATER AND SURFACE WATER SAMPLING SHEETS SEPTEMBER/OCTOBER 2014 SAMPLING EVENT ATTACHMENT C HYDROGRAPHS FOR SITE MONITORING WELLS ATTACHMENT D LABORATORY ANALYTICAL PACKAGES AND CHAIN-OF-CUSTODY DOCUMENTATION FOR GROUNDWATER SAMPLING EVENTS ATTACHMENT E PFBA, PFOA AND PFOS TREND GRAPHS ATTACHMENTF LABORATORY ANALYTICAL PACKAGES FOR PORE WATER AND SURFACE WATER SAMPLINGSEPTEMBER/OCTOBER 2014 ES 33663300..00001111 3M MN01595960 11.. IINNTTRROODDUUCCTTIIOONN Ths anal 208 prt ha repr by Wes Slatin, ne. (WESTON) for This annual 2014 report has been prepared by Weston Solutions, Inc. (WESTON) for 3M Compan (3M, ad includes an ssn fperusoshemis (PECs) n grote, Company (3M), and includes an assessment of pertluorochemicals (PFCs) in groundwater, pore tr, fice wate he 3 CoteGrove, Mines fi (Se The Sie pore water, and surface water at the 3M Cottage Grove, Minnesota facility (Site). The Site hhaass bbeeeenn iinn ooppeerraattiioonn ssiinnccee 11994477,, aanndd ccuurrrreennttllyy mmaannuuffaaccttuurreess aa rraannggee ooff pprroodduuccttss iinncclluuddiinngg ihe pred, pci per. industil polymers, bri, ad fc rod sis adhesive products, specialty paper, industrial polymers, abrasives, and reflective road sign mal. Resch and desclopmet of a propria nature are lo poformed at he materials. Research and development of a proprietary nature are also performed at the fet Th Ses oad proxi mils ss fh Cty of Cot Grove, facility. The Site is located approximately 3 miles southeast of the City of Cottage Grove, MMiinnnneessoottaa,, aanndd iiss aapppprrooxxiimmaatteellyy 11,,770000 aaccrreess iinn ssiizzee.. TThhee iinndduussttrriiaall,, ddeevveellooppeedd ppoorrttiioonn ooff tthhee ssiittee iiss aapppprrooxxiimmaatteellyy 220000 aaccrreessaass sshhoowwnn iinn FFiigguurree 11--11. Sine he cy 1950 3 a kad cooper ith he Mins Polson Contol Since the early 1980s, 3M has worked cooperatively with the Minnesota Pollution Control Agen (MPCA) in conocing inven to charac eniommensl mata te Agency (MPCA) in conducting investigations to characterize environmental media at the Site. More ren, 2 cay 2 Desenber 2004, 30 fad worked ith the MCA 10 Site. More recently, as early as December 2004, 3M had worked with the MPCA to vvoolluunnttaarriillyy aasssseessss tthhee pprreesseennccee ooff PPFFCCss aatt tthhee SSiittee.. TThhiiss iinncclluuddeedd ffiieelldd aaccttiivviittiieess ttoo hunts el nd router lt 3 wel 3 sediment an sis wae ul characterize site soil and groundwater quality as well as sediment and surface water quality atthe Ea Coe I ddd eld actives 0 charter sine, sufice water, at the East Cove. It also included field activities to characterize sediment, surface water, aanndd ppoorree wwaatteerr qquuaalliittyy iinn tthhee MMiissssiissssiippppii RRiivveerr.. SSuubbsseeqquueenntltlyy,, 33MM eenntteerreedd iinnttoo aa Stim Agrsment snd Consent Order Gh Agen) in My 2007 he purpose of Settlement Agreement and Consent Order (the Agreement) in May 2007 for the purpose of peroming he etl inscagainodn sponse actos 0 acres PC eS. performing the remedial investigations and response actions to address PFCs at the Site. IInn SSeepptteemmbbeerr aanndd OOccttoobbeerr 22000088,, ttwwoo ggrroouunnddwwaatteerr pprroodduuccttiioonn wweellllss ((PPWW--09 and PWW--1100)) wir elo the Sh a 3.44 pumping ts erm sah. The ei were installed at the Site and a 48-hour pumping test was performed on each. The results ofthe shorten pup tests were tized to deci aundwae emedil Almas of the short-term pump tests were utilized to develop groundwater remedial Alternative GV.1 ich omits ofan panded rounder nation sont fo pres ffs GW-1, which consists of an expanded groundwater extraction network to prevent off-site ition of groundtr bench te East Discs] Aves (rcs DI, D2 nd D9) nd migration of groundwater beneath the Eastern Disposal Areas (Areas D1, D2 and D9) and th ast Con, well the stern portionof he plant en. Tos re as show the East Cove, as well as the eastern portion of the main plant area. These areas are shown on Figie 12. The exact poundustr woud be red hough 2 new ganar on Figure 1-2. The extracted groundwater would be routed through a new granular civited cubon (GAC) tenet hiding and ssc used in manucuing activated carbon (GAC) treatment building and subsequently used in manufacturing perions iro dhe operations prior to discharge. 33663300..00001122 3M MN01595961 ESE AAss ddeessccrriibbeedd iinn tthhee MMPPCCAA-a-apppprroovveedd FFeeaassiibbiilliittyy SSttuuddyy ((FFSS)) RReeppoorrtt ((WWEESSTTOONN,, 22000088)) aanndd tthhee RReemmeeddiiaall DDeessiiggnn//RReessppoonnssee AAccttiioonn ((RRDD//RRAA)) PPllaann ((WWEESSTTOONN,, 22000099)) ffoorr tthhee SSiittee,, 33MM aanndd MMPPCCAA aaggrreeeedd tthhaast tthhee rreemmeeddiiaall AAlltteerrnnaattiivvee GGWW--11 wwoouulldd bbee iimmpplleemmeenntteedd iinn aa pphhaasseedd mmaannnnere.r. TThhee pphhaasseedd iimmpplleemmeennttaattiioonn ooff tthhee rreemmeeddiiaall AAlliteermnaattiivvee GGWW--11 iinnvvoollvveess tthhee ppeerrffoorrmmaanncceeooffaann eexxtteennddeedd ppiilloott ppuummpp tteesstt oonn tthhee ttwwoo nneeww pprroodduuccttiioonn wweellllss ((PPWW--0099 aanndd PPWW-1-100)),, ttoorreeffiinneeaanndd ooppttiimmiizzee tthhee lloonngg--tteerrmm ppuummppiinngg ssyysstteemm ooppeerraattiioonnaall ppaarraammeetteerrss,, aanndd to iiddeennttiiffyy iiff aaddddiittiioonnaall pprroodduuccttiioonn wweellllss aarree nneeeeddeedd.. SSaoiill aanndd EEaasstt CCoovvee sseeddiimmeenntt rreessppoonnssee aaccttiioonnss aallssoo hhaavvee bbeeeenn ccoommpplleetteedd iinn aaccccoorrddaannccee wwiitthh tthhee AAggrreeeemmeenntt aanndd MMPPCCAA-a-apppprroovveedd RRDD//RRAA PPllaann ttoo aaddddrreessss tthhee PPFFCCss ffoouunndd iinn tthheessee mmeeddiaia,. IInn JJuunnee 22001111,, pprriioorr ttoo tthhee iimmpplleemmeennttaattiioonn ooff rreemmeeddiiaall mmeeaassuurreess iinn tthhee EEaasstt CCoovvee,, ppoorree wwaatteerr ((iinntteerrssttiittiiaall wwaatteerr ((IIWW))) aanndd ssuurrffaaccee wwaatteerr ssaammpplliinngg wwaass ppeerrffoorrmmeedd iinn tthhee MMisisssiissssiippppii RRiivveerr aatt aa ssuubbsseettoofftthhee llooccaattiioonnss pprreevviioouussllyy ssaammpplleedd iinn 22000066.. PPFFBBAA,, PPFFOOAA,, aanndd PPFFOOSS ccoonncceennttrraattiioonnss iinn ppoorree wwaatteerr aanndd ssuurrffaaccee wwaatteerr wweerree oobbttaaiinneedd aatt ffoouurr itrraannsseesctt llooccaattiioonnss ttoo cchhaarraaccteteririzzee. pprree--rreemmeeddiiaattioinn ccoonnddiittiioonnss ffoorr ccoommppaarriissoonn ttoo ffuutuurree PPFFCC ccoonncceennttrraattiioonnss ddeetteecctteedd iinn tthheessee mmeedaia. AAtt aa mmeeeettiinngg wwiitthh tthhee MMPPCCAA oonn MMaarrcchh 1155,, 22001122,, 33MM aaggrreeeedd ttoo pprreeppaarree aa mmoonniittoorriinngg ppllaann ffoorr PPFECCss iinn ggrroouunnddwwaatteerr aatt tthhee SSiittee,, wwhhiicchh aallssoo wwoouulldd iinncclluuddee ppoorree wwaatteerr aanndd ssuurrffaaccee wwaatteerr ssaammpplliinngg iinn tthhee MMisisssiissssiippppii RRiivveerr pprriioorr ttoo,, dduurriinngg,, aanndd aafftterr tthhee eexxtteennddeedd ppuummpp tteesstt. "TThhee GGrroouunnddwwataeterr,, PPoorree WWaatteerr aanndd SSuurrffaaccee WWaatteerr SSaammpplliinngg PPllaann ffoorr PPeer~ffhl,u~oorroocchheemmicicaallss ((PPFICCSs))-- 33~M1 CCoortttaaggee GGrroovvee SSiittee ((SSaammpplliinngg PPllaann)) wwaass ssuubbmmiittteedd ttoo tthhee MMPPCCAA oonn MMaayy 44,, 22001122. AAfftteerr rreessoolluuttiioonn ooff MMPPCCAA aanndd AAEECCOOMM ccoommmmeennttss oonn tthhee SSaammpplliinngg PPllaann,, tthhee PPFFCCss bbaasseelliinnee ((ii.ce.. pprriioorr ttoo tthhee eexxtteennddeedd ppuummpp tteesstt)) ggrroouunnddwwataetre,r, ppoorree wwaatrer,, aanndd ssuurrffaaccee wwaatteerr ssaammpplliinngg wwaass ppeerrffoorrmmeedd iinn OOccttoobbeerr 22001122.. TThhee rreessuullttssoofftthhee OOccttoobbeerr 22001122 ssaammpplliinngg eevveenntt wweerree pprroovviiddeedd ttoo MMPPCCAA iinn tthhee JJuunnee 22001133 iinn tthhee BBaasseelliinnee MMoonniittoorriinngg RReeppoorrtt ffoorr PPeertfflluuoorrooechheemmiiccaallss ((PPFFCCss')) iinn GGrroouunndawha,,taeterr,, PPoorree WWataeterr,, aanndd SS~urlrffaaccee WWaatteerr,, 33MM CCoottttaaggee GGrroovvee SSiittee, CCoottttaaggee GGrroovvee,, MMNN ((WWEESSTTOONN,, 22001133)). "TThheeeexxtteennddeedd ppiilloott ppuummpp tteesstt wwaass iinniitiiaatteedd iinn FFeebbrruuaarryy 22001133 wwiitthh tthhee ssttaarrmtupp ooff pprroodduuccttiioonn wweellllss PPWW--0099 aanndd PPWW-1-100.. GGrroouunnddwwaatteerr eexxttrraacctteedd ffrroomm PPWW--0099 aanndd PPWW--1100 wwaass rroouutteedd ttoo 12 33663300..00001133 3M_MNO1595962 3M MN01595962 tthhee nneeww GGAACC ttrreeaattmmeenntt ffaacciilliittyy.. TThhee ffiieelldd ddaattaa ccoolllleeccttiioonn ppeerriioodd ooff tthhee eexxtteennddeedd ppiilloott ppuummpp tteesstt ccoonnttiinnuueedd unnitlil FFeebbrruuaarryy 22001144,. TThhee ddeettaaiillss ooff tthhee eexxtteennddeedd ppiilloott ppuummpp tteesstt wweerree ssuubbmmitittteedd t(o0 MMPPCCAA iinn MMaarrcchh 22001155 iinn aa sseeppaarraattee rreeppoortr.t. IInn aaccccoorrddaannccee wwiitthh tthhee RRDD/RRAA PPllaann,, PPWW--0099 aanndd PPWW--1100 ccoonnttiinnuuee ttoo ooppeerraattee iinn ccoonnjjuunnccttiioonn wwiitthh eexxiissttiinngg SSiittee pprroodduuccttiioonn wwelels otoliinntlteerrccseepptt ggrroouunnddwwaatteerr mmiiggrraattiinngg ttoowwaarrdd tthhee MMisisssiissssiippppii RRiivveerr. 11.11 PPUURRPPOOSSEE AANNDD OOBBJJEECCTTIIVVEESS OOFF TTHHEE SSAAMMPPLLIINNGG PPLLAANN IInn aaddddiittiioonn ttoo tthhee bbaasseelliinnee ggrroouunnddwwaatteerr ssaammpplilinngg,, tthhee SSaammpplliinngg PPllaann iinncclluuddeess aa rreeqquuiirreemmeenntt ffoorr qquuaarrtteerrllyy ((ffoorr ffoouurr yyeeaarrss aafftteerr ccoommpplleettiioonnooff tthhee eexxtteennddeedd ppiilloott ppuummpp tteesstt)) aanndd aannnnuuaall ggrroouunnddwwaatteerr ssaammpplliinngg ffoorr PPFFCCss.. TThhee mmoonniittoorriinngg ffoorr PPFECCss iiss bbeeiinngg iimmpplleemmeenntteedd iinn aaccccoorrddaannccee wwiitthh tthhee pprroovviissiioonnss ooff tthhee MMPPCCAA-a-apppprroovveedd RRDD/iRRAA PPllaann ttoo pprroovviiddee ggrroouunnddwwaatteerr qquuaalliittyy ddaattaa ttoo aasssseessss tthhee iimmppaacctt ooff tthhee ccoommpplleetteedd PPFFCCss ssooiill aanndd sseeddiimmeenntt rreemmeeddiiaattiioonn aaccttiivviittiieess,, aanndd tthhee eeffffeeccttiivveenneessss ooff oonn--ggooiinngg ggrroouunnddwwaatteerr rreemmeeddiiaattiioonn aaccttiivviittiieess.. TThhee SSaammpplliinngg PPllaann iinncclluuddeess MMisisssiissssiippppii RRiivveerr ppoorree wwaatteerr aanndd ssuurrffaaccee wwaatteerr ssaammpplliinngg ffoorr PPFFCCss pprriioorr ttoo,, dduurriinngg,, aanndd aafftteer tthhee eexxtteennddeedd ppiilloott ppuummpp tteesstt ttoo aasssseessss wwhheetthheerr aannyy ttrreennddss aarree aappppaarreenntt ffoorr tthheessee eennvviirroonnmmeennttaall mmeeddiiaa. "TThhee ccoommppoonneennttssoofftthhee SSaammpplliinngg PPllaann iinncclluuddee: + rIIdadteeinnottniiaffliicec,aattiioonnooffssaammppllee ttyyppee aanndd llooccaattiioonnss,, mmoonniittoorriinngg ffrreeqquueennccyy,, aanndd mmoonniittoorriinngg + rPartoiocnedauler,es for sample collection, Procedures for sample collection, + PPrroocceedduurreess foorr ddooccuummenentatattiioonn aanndd qquuaalliittyy sassssuurraannccee//qquuaalliityt ccoonnttrrooll ((QQAA//QQCC)),, + SSaammppllee aannaallyyssiiss aanndd aannaallyyttiiccaall ppaarraammeetteerrss,, aanndd + Reporting Reporting. "TThhiiss iiss tthhee sseeccoonndd aannnnuuaall mmoonnititoorriinngg rreeppoorrtt ssiinnccee bbaasseelliinnee ssaammpplliinngg aaccttiivviittieess wweerree ccoonndduucctteedd iinn OOccttoobbeerr 22001122.. ITti ccoonnttaaiinnss aa ddeessccrriippttiioonnooffssaammpplliinngg mmeetthhooddoollooggiieess aanndd tthhee rreessuultss ooff ggrroouunnddwwataeterr,, ppoorree wwaatteerr aanndd ssuurrffaaccee wwaatteerr ssaammpplliinngg ppeerrffoorrmmeedd iinn 22001144 iinn SSeeccttiioonnss 22 aanndd 33.. AA ssuummmmaarryy ooff tthhee ffiinnddiinnggssoofftthhee gsrroouunnddwwataeterr,, ppoorree wwaatteerr aanndd ssuurrffaaccee wwaatteerr iinnvveessttiiggaattiioonnss iiss pprroovviiddeedd iinn SSeeccttiioonn 44 aanndd ffuuttuurree ccoouurrssee ooff aaccttiioonn iiss pprreesseenntteedd iinn SSeeccttioinon55.. 15 33663300..00001144 W_MNO1595963 3M MN01595963 FeO Smee VER wan i hi i Ge ERE os) mL i Ne CnOG AE SE 2 CiEE Bi Nh I Aerial Source: ESKI Imagery Ma!oping Selwlce. 2013 cei Lig ce To SN TE : CV x Ee 3 weilS Bit mE fi Rot ie eiEi LrSASe SeNdgEs x Figure 1-1 Site Location ]~lap Cotlage Grove Site 3M_MN01595964 33663300..00001155 [ZEEE EY ww Logond 3M Cottage Grcve Property LJnes ~ Buildings RDe .IRN TRTANuG e A GramTM NE L 0 xs a WE ah EN & aN aL 3 pe BFZoe SNE UB Figure 1-2 Site Layout Cottage Grove Site 3M_MN01595965 33663300..00001166 22.. SSAAMMPPLLIINNGG PPRROOGGRRAAMM The PFC Sampling Plan contains the monitoring program for the Site. As indicated in the Sampling Plan, 3M implemented baseline groundwater monitoring for PFCs in October 2012, prior to the startup of the extended pilot pump test. These baseline monitoring results aarree uusseeddaass aa rreeffeerreennccee ppooiinntt ffoor commppaarriison ttoo ffuuttuure mmoonintitoorriinngg.. TThhe2200114 PFC sammpplliing program that was conducted to assess groundwater, pore water, and surface water conditions at the Site is described in the following sections. 22.11 GGRROOUUNNDDWWAATTEERR The current groundwater monitoring network at the Site consists of 33 monitoring wells and one piezometer. In addition, there are six existing production wells (PW-01 through PW-05/PW-06), one infrequently used production well (PW-07), and two new production wells (PW-09 and PW-10). Production wells PW-02 and PW-05 are currently the primary production wells used for water supply (not used for drinking water) at the Cottage Grove Plant. Production wells PW-01, PW-03, PW-04 and PW-05/PW-06 are not routinely pumped, but are available for use on an as-needed basis. Former production well PW-08 was abandoned in April 2012 as it was no longer used. The monitoring wells and production wells that are included in the annual and quarterly sampling network for PFCs are presented in Table 2-1 and shown on Figure 2-1. A table summarizing available well construction and other information for the Site wells is included in Attachment A. In accordance with the Sampling Plan, the annual groundwater sampling event was ppeerrffoorrmmeedd iinn AApprriill 22001144 aanndd iinncclluuddeedd tthhee aannaallyyssiissoofftthhee ffoolllloowwiinngg 1122 PPFFCCs:s: * PPeerrffluluoorrooooccttaannooiicc aacciidd ((PPFFOOAA)) Pertluorooctane sulfonate (PFOS) Perfluorobutane sulfonate (PFBS) * PPeerrfflluuoorroohheexxaannee ssuullffoonnaattee ((PPFFHHSS)) = PPeerrfflluuoorroobbuuttaannooiicc aacciidd ((PPFFBBAA)) * PPeerrffluluoorrooppeennttaannooiicc aacciidd ((PPFFPPeeAA)) * PePrfelurorfolheuxoanroiocahacceiiddx((aPPnFFHHoxxiAAc)) Ta 33663300..00001177 3M MN01595966 WEEE * PPeerrfflluuoorroohheeppttaanncoiiccaacciidd ((PPFFHHppAA)) * PPeerrfflluuoorroonnocnnooiiccaacciidd ((PPFFNNAA)) * PPeerfrluforloudeocarnooidcaeaccicidda((nPPFFcDDiAAc)) + PPeerrfflulouroorunoduencdaencoaicnacaciicdd ((PPFFUURnAA)) + PPeerrfflulouroordooddeocdaencoaicnacaciicdd ((PPFFDDooAA)) QQuuaarrtteerrllyy ggrroouunnddwwaatteerr ssaammpplliinngg wwaass ppeerrffoorrmmeedd iinn JJaannuuaarryy,, JJuullyy aanndd OOccttoobbeerr 22001144,, aanndd iinncclluuddeedd aannaallyyssiiss ffoorr:: PPFFBBAA,, PPFFBBSS,, PPFFHHSS,, PPFFOOSS aanndd PPFFOOAA.. AAss nnootteedd iinn TTaabbllee 22--11,, aa ffeeww mmooddififiiccaattiioonnss ttoo tthhee SSiittee mmoonniittoorriinngg wweellll nneettwwoorrkk hhaavvee ooccccuurrrreedd ssiinnccee tthhee iimmpplleemmeennttaattiioonnooftf thhee GGrroouunnddwwaatteerr SSaammpplliinngg PPllaann.. AA ssuummmmaarryyooff tthheessee mmooddififiiccaattiioonnss aarreepprorovviiddeeddiinn tthhee ffoolllloowwiinngg ppaarraaggrraapphhss.. MMoonnititoorriinngg wweellllss MMWW--0066 aanndd MMWW--1144 wweerree aabbaannddoonneedd iinn MMaayy 22001133 iinn aaccccoorrddaannccee wwiitthh MMiinnnneessoottaa DDeeppaarrttmmeenntt ooff HHeeaalltthh ((MMDDHH)) rreegguullaattiioonnss.. AAtttteemmppttss ttoo rreehhaabbiilliittaattee bbootthh mmoonniittoorriinngg wweellllss wweerree mmaaddee pprriioorr ttoo aabbaannddoonnmmeenntt TThhee ssccrreeeenneedd iinntteerrvvaall ooff mmoonniittoofriinngg wweellll MMWW--1144 wwaass ccllooggggeedd aanndd ccoouulldd nnoott bbee rreessttoorreedd ttoo aa uusseeaabbllee ccoonnddititiioonn.. AAnn oobbssttrruuccttiioonn wwaass pprreesseenntt iinn mmoonniittoorriinngg w~evlelll MMWW--0066 aatt aapppprrooxxiimmaatteellyy 8855 ffeeeett bbeellooww ggrroouunndd ssuurrffaaccee ((fftt bbges)) tthhaatt ccoouulldd nnoott bbee rreemmoovveedd.. AA nneeww mmoonniittoorriinngg wweellll ttoo rreeppllaaccee MMWW--0066 wwaass nnoott iinnssttaalllleedd bbeeccaauussee MMWW--0066 wwaass aann uuppggrraaddiieenntt mmoonniittoorriinngg wweellll aanndd aannootthheerr uuppggrraaddiieenntt lmnoonniittoorriinngg wweellll MMWW--0055 iiss bbeeiinngg uusseedd ttoo aasssseessss uuppggrraaddiieenntt ccoonnddititiioonnss.. NNeeww mmoonniittoorriinngg wweellllss MMWW-0-044RR,, MMWW--1144RR aanndd MMWW-1-l1l22 wweerree iinnssttaalllleedd iinn MMaayy 22001133. MMoonnititoorriinngg wweellll MMWW--0044RR wwaass iinnssttaalllleedd aass aa rreeppllaacceemmeenntt wweellll ffoorr aaddjjaacceenntt mmoonniittoorriinngg wweellll MMWW-0-404.. TThhee ooppeenn bboorreehhoollee iinntteerrvvaall ooff mmoonniittoorriinngg wweellll MMWW--0044 hhaadd ppaarrttiiaallllyy ccoollllaappsseedd lliimmiittiinngg tthhee ffllooww ooff ggrroouunnddwwaatteerr iinnttoo tthhiiss wwelell.l. TThhiiss wweellll ccoouulldd nnoott bbee aabbaannddoonneedd dduuee ttoo oovveerrhheeaadd ppoowweerr lliinneess tthhaatt pprreevveenntt aacccceessss ttoo tthhee llooccaattiioonn bbyy aa ddrriilllliinngg rriigg.. MMoonnititoorriinngg wweellll MMWW--1144RR wwaass iinnssttaalllleedd aass aa rreeppllaacceemmeenntt ffoorr mmoonniittoorriinngg wweellll MMWW--1144 ttoo pprroovviiddee ggrroouunnddwwaatteerr qquuaalliittyy aanndd eelleevvaattiioonn ddaattaa iinn tthhee vviicciinniittyy ooff pprroodduuccttiioonn wweellllss PPWW--0055 aanndd PPWW--00S5//PPWW-0-066.. PPeerr MMPPCCAA aapppprroovvaall rreecceeiivveedd bbyy 33MM iinn JJaannuuaarryy 22001144,, mmoonniittoorriinngg wweellll MMWW--1144RR wwiillll rreeppllaaccee pprroodduuccttiioonn wweellll PPW W--0055//PPWW--0066,, wwhhiicchh iiss nnoott rroouuttiinneellyy ppuummppeedd,, aass aa g`grorouunnddwwaatteerr mmoonniittoorriinngg ppooiinntt iinn tthhee ssaammpplliinngg pprrooggrraamm.. FFiinnaallllyy,, mmoonnititoorriinngg wweellll MMWW--111122 wwaassiinnssttaalllleedd iinn tthhee eeaasstteerrnn SSiittee aarreeaa ttoo pprroovviiddee aann aaddddiittiioonnaall ggrroouunnddwwaatteerr mmoonniittoorriinngg ppooiinntt bbeettwweeeenn tthhee EEaasstt CCoovvee aanndd tthhee ffoorrmmeerr DD1l//DD22 AArreeaa.. GGrroouunnddwwaatteerr ssaammpplleess wweerree ccoolllleecctteedd Re 33663300..00001188 3M_MNO1595967 3M MN01595967 in July 2013 from monitoring wells MW-04R, MW-14R and MW-112 to provide baseline PFC groundwater quality data at these locations. 22..22 PPOORREE W WAATTEERR AANNDD SSUURRFFAACCEE WWAATTEERR Paired pore water and surface water samples were collected from the Mississippi River during the xveek of September 29, 2014. This sampling event was performed after the extended pilot pumping test was completed at production wells PW-09 and PW-10. This pore water and surface water sampling event could not be performed until after water levels in the Mississippi River had subsided due to above normal precipitation that caused high water conditions in the river. Samples were collected from the same locations as the September/October 2006, June 2011 (pro-East Cove remediation), October 2012 (pre-extended pilot pump test), and AAuugguusstt 22001133 ((mmiidd--ppooiinntt ooff eexxtteennddeedd ppiilloott ppuummpp tteesstt)) ssaammpplliinngg eevveenntsts.. TThhee ssaammpplleess wweerree ccoolllleecctteedd ffrroomm tthhee ffoouurr ttrraannsseecctt llooccaattiioonnss iinn tthhee MMisisssiissssiippppii RRiivveerr ppeerrppeennddiiccuullaarr ttoo tthhee shoreline to assess the current distribution of PFCs in surface water and groundwater beneath the river (Figure 2-2). As shown in Figure 2-2, four samples were collected from eeaacchh ooff tthhee ffoouurr ttrraannsseeccttss ((IIWW--0099,, IIWW--1144,, IIWW--1199 aanndd IIWW--2255)).. TThhee ssaammpplliinngg llooccaattiioonnss wweerree approximately 50 feet (ft), 100 ft, 300 ft and 500 ft from the shoreline. These transects were selected based on their proximity to the following Site areas: IW-09 transect located near the D5 Area; IW- 14 - transect near the wastewater treatment plant (WWTP) Area; IW-19 - transect near the D1/D2/D9 Areas; IW-25 - transect near the East Cove. Pore water and surface water sampling protocols and standard operating procedures are contained in the Sampling Plan. Modifications to the pore water and surface water ssaammpplliinngg pprroottooccoollss wweerree ddeettaaiilleedd iinn aa rreessppoonnssee ttoo MMPPCCAA ccoommmmeennttss ddaatteedd AAuugguusstt 2211,, 22001122.. AA bbooaatt wwaass uusseedd ttoo ggaaiinn aacccceessss ttoo ceaacchh ooff tthhee ssaammpplliinngg ppooiinntsts.. SSaammpplliinngg wwaass performed from downstream to upstream transect locations. A GPS with submeter accuracy was used to establish each sampling location. As agreed with MPCA, surface wwaatteerr ssaammpplleess wweerree ccoolllleecctteedd ffiirrsstt.. BBaasseedd oonn ssiimmililaarriittiieess iinn tthhee 22000066 ssuurrffaaccee wwaatteerr rreessuullttss ee 33663300..00001199 3M MN01595968 WEEE ffrroomm ddiissccrreettee ddeepptthhss ccoorrrreessppoonnddiinngg ttoo 2200 aanndd 8800 ppeerrcceenntt ooff tthhee wwaatteerr ccoolluummnn,, tthhee ssuurrffaaccee wwaatteerr ssaammpplleess ccoolllleecctteedd dduurriinngg tthhee SSeepptteemmbbeerr//OOccttoobbeerr 22001144 ssaammpplliinngg eevveenntt ccoonnssiisstteedd ooffaa ssiinnggllee ccoommppoosisittee ssaammppllee ooff eeqquuaall pprrooppoorrttiioonnss ffrroomm tthheessee ssaammee ddeepptthhss ((2200 aanndd 8800 ppeerrcceenntt)) ttoo rreepprreesseenntt tthhee aavveerraaggee wwaatteerr ccoolluummnn ccoonncceenntrtraattiioonn.. FFoolllloowwiinngg tthhee ccoolllleeccttiioonn ooff tthhee ssuurrffaaccee wwaatteerr ssaammppllee,,aa ccoo--llooccaatteedd ppoorree wwaatteerr ssaammppllee wwaass ccoolllleecctteedd.. TThhee ppoorree wwaatteerr ssaammpplleess wweerree ccoolllleecctteedd uussiinngg aa ddeeccoonnttaammiinnaatteedd ssttaaiinnlleessss sstteeeell ssaammpplliinngg pprroobbee wwiitthh 00..55 fftt ooff 00O01l--iinncchh ssllootttteedd ssccrreeeenn aanndd ssuuffffiicciieenntt riisseerr t1o0 eexxtteenndd aabboovvee tthhee ssuurrffaacceeoofftthhee wwaatteerr.. TThhee ssaammpplliinngg pprroobbee wwaass ddrriivveenn aapppprrooxxiimmaatteellyy oonnee ffoooott iinnttoo tthhee bboottttoomm sseeddiimmeenntt ssoo tthhaatt tthhee ssccrreeeenn wwaass ppllaacceedd aatt aann aapppprrooxxiimmaattee ddeepptthh ooff0.50.5 fftt t1o0 11..00 fftt bbeellooww tthhee ttoopp ooff sseeddiimmeentn.t. GGrroouunnddwwaatteerr wwiitthhiinn tthhee pprroobbee wwaass ppuurrggeedd uussiinngg aa ppeerriissttaallttiicc ppuummpp aanndd ddiissppoossaabbllee ppoollyyeetthhyylleennee ttuubbiinngg. SSaammpplleess wweerree ccoolllleecctteedd ffrroomm tthhee ppoorree wwaatteerr pprroobbeess aafftteer eeiitthheerr 33 wweellll vvoolluummeess wweerree rreemmoovveedd,, oorr aafftteerr tthhee wwaatteerr lleevveell hhaadd ssuuffffiicciieennttllyy rreecchhaarrggeedd aafftteerr ppuummppiinngg ddrryy.. W Whheenn ppoossssiibbllee,, tthhee ppoorree wwaatteerr ssaammpplliinngg pprroobbeess wweerree aalllloowweedd t0o rreeccoovveerr aa mmiinniimmuumm ooff 2244 hhoouurrss pprriioorr ttoo ssaammpplliinngg;; hhoowweevveerr,, dduuee ttoo hhiigghh wwiinnddss aanndd tthhee ffoorreeccaasstt ffoorr hheeaavvyy pprreecciippiittaattiioonn tthhaatt wwoouulldd ppootteennttiiaallllyy ccoommpprroommiissee ssaammppllee iinntteeggrriittyy,, ssoommee ooff tthhee ppoorree wwaatteerr llooccaattiioonnss wweerree ssaammpplleedd sslliigghhttllyy lleessss tthhaann 2244. hhoouurrss aafftteerr ppuurrggiinngg. CCoolllleecctteedd ssaammpplleess wweerree aannaallyyzzeedd tfborr PPFEBBAA,, PPFFOOSS aanndd PPFFOOAA bbyy tthhee 33MM EEnnvviirroonnmmeennttaall LLaabboorraattoorryy iinn SSt.t. PPaauul,l: MMininnneseostoata.. PPoorree wwaatteerr aanndd ssuurrffaaccee wwaatteerr ssaammpplliinngg ffiieelldd sshheeeettss aarree pprroovviiddeedd iinn AAttttaacchhmmeennttBB. nmin 33663300..00002200 33MM_MMNNO011559955996699 3 PR 7 NN ERA Ri i NE patil WT eae po Ee # bY voli. - jo oN pa mEEE 3M_MN01595970 33663300..00002211 RET a B00 J Guin b5h NPY hi 5aFE = eT iiON 3 Xta =ro oy en es 5 Sy fe Se wm Feet ~ore W~ter and Su~ace Water 3M_MN01595971 33663300..00002222 Well ID EWREa ~lonitoring Wella IVBV-O 1 MW-02 outers HstCerCCroCmiCmoSptTtruenseetGaESmrmoenvenptSkhieTPPYargn ot October 2012 hi FwoAi Tnuwi [wiheT wwaor | (Baseline) Table 2-1 PFCs Groundwater Monitoring Plan 3M Cottage Grove Site Cottage Grove, MN Quarterly Sampling until 4 Years after Completion of Extended Pump Test 1Q 2Q(1) 3Q 4Q WL WL IV~V-03 MW-04 va MW_04R(2) mncae| 1VBV-05 " w0!r wio wo5 W W W W iw5oELELL ~r_06 MW-07 et ~V-08 he~V-09 ni ~V 10 ni~V- 11 AN ~V-12 WL, 12 PFCs wrwuiwiiree WL, 12 PFCs WL, 5 PI;Cs iWL wiWL wrWL iWL wr Sve WL, 5 PFCs WL, 12 PFCs iWL wiWL wiWL uiWL ve | "~%, 12 PFCs WL, 5 PI, Cs e ir WL i a WL he ui WL hi hs WL |r Ses WL, 5 PFCs WL, 5 H, Cs WL WL WL WL WL, 5 PFCs heii -- | | res owl"1 ~V-13 ~r_ 14~~ MW- 14R ~-15 we WL, 12 PFCs 1WL, 5 1 PFCs WL, 5 PFCg WL, 12 PFCs {re WL, 12 PFCs WL, 5 I PFCs WL, Se5 PI~Cs WL, 5 I PFCs res WL, 5 Pl~Cs WL ~V-16 MW-17 Wie w wr ur bi bi ~V-18 hs bi ui wi i ui ~-19 rw |e | he ~-101 Mid | Weimer |e| ol ~-102 MEER He 5 ~V-103 mits | wii | wie | wee | wine | wisi | ~-104 nm nf cm nf ~-105 Avis Wns | mee | mee| Wee | Wes | ~-108 i Wr i i i ~-109 we. | wi sie, | wwe,| wtme, | withes | ~-110 HE -- if i i i ~-112 i ui u; ji i ECPZ-01 rs |r Wi wi wi ECPZ-02R(?~ WL, 12 PFCs WL WL, 12 PFCs WL, 12 PFCs WL, 12 PFCs WL, 12 PFCs WL, 12 PFCs WL, 12 PFCs WL, 12 PFCs serine| wr i wr foro 7 va ECPZ-03R(3~ poo~ -PZ 01 ZPZT-14SPS WL Production We~ EA rere Tw wr PW-06 WL(5), 12 PFCs ri | wo ime, | wom| wi cs | wise| wiosne PW-09 WL(5), 12 PFCs Pus | wine: | wiv sme | wire] wi ime| wine| PW-10 WI~(5), 12 PFCs WL, 5 PFCg WL WL, 12 PFCs WL WL, 5 PFCs WL WL, 5 PFCs WL, 5 PFCs WL, 5 PFCs WL, 5 PFCs WL, 5 PFCs WL, 12 PFCs "~%, 12 PFCs ~%, 12 PFCs "~%, 12 PFCs WL, 12 PFCs "~%, 12 PFCs "~%, 12 PFCs WL, 5 PFCs WL WL, 5 PFCs WL, 5 PFCs WL, 5 PFCs WL, 5 PFCs WL, 5 PFCs WL WE WL WL, 5 PFCs WL, 5 PFCs WL, 5 PFCs WL, 5 PECs WL, 5 PFCs WL wa Te we a IWS L WPLR SS WLSU SWP L I WL(5) V~rL(5) WL(5) W-L(5) WL(5), 5 PFCs WE(5), 5 PFCs WL~5;', 12 PFCs ~TJ5;', 12 PFCs WL'5~, 5 PFCs ~,VIJ5;', 5 PFCs WL(5), 5 PFCs Vql,(5), 5 PFCs Rationale for Sampling after Baseline Upgradient v~ell a D5 Area (RD/RA) D9 Area (RD/RA) | i D8 Area, replaced PW-06 D5 Area ram D1 Area (RD/RA) Diniry D1 Area (RD/RA) DiAmabED D2 Area (RD/RA) pieoony D2 Area (RD/RA) mr D9 Area (RD/RA) war meee WWTP Area (RD/RA) psamavny D5 Area (RD/RA) arcs East Cove Area owns East Cove Area toss East Cove Area 1 SrD8 Area (RD/RA) ram D9 Area cocks East Cove Area Not=s: WL Water level measurement VWV]P - V~agtewaler Trea[m~nt Plant a v t m tami 12 PFCs- PFBA PFPeA, PFH~, PFHpA, PFOA, PFNA PFDA, PFUnDA PFDeA, PFBS, PFHS, and PFOS. 5 PFCs - PFBA, PFBS, PFH S, PFOS, and PFOA. (~) The annual groundvcater s~npling event will ~e performed in 2Q sampling event. (2) In May 2013, monitoring wellg MW-06 and MJV-f,I were abandoned, and monitoring wellg M~V-0a,R, MW-] dR, and MW-I 12 were (3) Realassified a~ monitoring wells since theyare registered with the IVinnesota Department of Health ('vlDH) with unique well (4) PW-06 is currently not in use; therefore, a sample cannot be collected from this well. N earby monitoring well rvlN-~4R has been added to the sampling program to replace PW-OS. (5) I/Vater level measurement will be recorded if pump is not operating. 33663300.'00002233 awmnorsssor2 3M MN01595972 33.. WWAATTEERR MMOONNIITTOORRIINNGG AANNDD RREESSUULLTTSS 3.1 GROUNDWATER ELEVATIONS Figure 3-1 shows the locations of the production wells, monitoring wells and piezometer oonn tthhee MMiinnnneessoottaa GGeeoollooggiicc SSuurrvveeyy ((MMGGSS)) ggeeoollooggiicc mmaapp ffoorr tthhee SSiittee.. BBeenneeaatthh tthhee mmaaiinn plant area, the uppermost water-bearing unit is the Oneota Dolomite. Where the Oneota Dolomite is absent, the uppermost water-bearing unit occurs within the unconsolidated gladofluvial sediments. As shown in Figure 3-1, the Oneota Dolomite (blue) is eroded in a ssiiggnniiffiiccaanntt aarreeaa ttoo tthhee ssoouutthh aanndd eeaasstt ooff tthhee MMaaiinn PPllaanntt aarreeaa wwhheerreaea bbeeddrroocckk vvaalllleeyy ((yyeellllooww and green) is present. Site production wells PW-05 and PW-05/PW-06, in addition to new production wells PW-09 and PW-10, are all screened within the unconsolidated sediments within the limits of the bedrock valley. Depth-to-groundwater measurements were measured on a quarterly basis at the monitoring well and piezometer locations shown in Figure 2-1. Water level measurements recorded in groundwater monitoring wells are presented in Table 3-1. Hydrographs were constructed for select monitoring points, and are included in Attachment C. As discussed previously in Section 2.1, monitoring wells lVlW-04R, MW-14R and MW-112 were installed in May 2013, while monitoring wells MW-06 and MW-14 were deemed unusable due to well integrity issues and abandoned at the same time in accordance with MDH regulations. EEffffoorrttss wweerree aallssoo ccoommpplleetteedd iinn MMaayy 22001133 ttoo rreehhaabbiilliittaattee mmoonniittoorriinngg wweellll MMWW--1122 aass tthhee screened interval of" this well is clogged. The rehabilitation efforts could not completely cclleeaarr tthhee ssccrreeeenneedd iinntteerrvvaall ooff tthhiiss wweellll aass iitt ccoonnttiinnuueess ttoo ppuummpp ddrryy dduurriinngg ssaammpplliinngg eevveennttss;; however, the water level in this monitoring well recovers sufficiently within 24 hours to aallllooww tthhee ccoolllleeccttiioonnooff aa rreepprreesseennttaattiivvee ggrroouunnddwwaatteerr ssaammpplele.. TThheerreeffoorree,, mmoonniittoorriinngg wweellll a MW-12 continues to be included in the quarterly groundwater sampling program for the SSiittee., bbuutt tthhee wwaatteerr lleevveell rreeccoorrddeedd iinn tthhiiss wweellll iiss nnoott uusseedd ttoo ccoonnssttrruucctt ggrroouunnddwwaatteerr elevation contours. As shown in Table 3-1, the water levels in monitoring wells more distant from the Mississippi SRiver E(e.g. monitoring wells MW-01, Z:~FOL DE R-G O-9\3m-c~ttage~qrove\WE~TON-Reports~20144Q-AnnuaI-G~/~CGMN_2014_Ann ual_Report.docx 3-1 MW-02, MW-03, MW-09, MW-17 and 3M MN01595973 33663300..00002244 WEEE MMWW-1-188)) eexxhhiibbiitteedd ggrreeaatteerr cchhaannggee iinn wwaatteerr lleevveell tthhaann mmoonniittoorriinngg wweellllss cclloosseerr ttoo tthhee rriivveerr.. ~Trhheessee fMlluuccttuuaattiioonnss iinn wwaatteerr lleevveellss aarree aallssoo sshhoowwnn iinn tthhee hhyyddrrooggrraapphhss pprreesseenntteedd iinn AAttttaacchhmmeenntt CC.. IInnccrreeaasseess iinn wwaatteerr lleevveellss ooccccuurr iinn rreessppoonnssee ttoo ssiiggnniiffiiccaanntt pprreecciippiittaattiioonn eevveenntsts,, aanndd aafftteerr tthhee sspprriinngg mmeletl.t. GGrorouunnddwwataeterrlelevveellss ssuubbsseeqquueennttllyy ddeecclliinnee iinn rreessppoonnssee ttoo lToowweerr rreecchhaarrggee dduurriinngg tthhee wwiinntteerr mmoontnhths.s. TThhee ggrroouunnddwwaatteerr eelleevvaattiioonn ddaattaa ccoolllleecctteedd ffrioomm tthhee nneettwwoorrkk ooff wweellllss sshhoowwnn iinn TTaabbllee 33--11 wweerree uusseedd t1o0 pprreeppaarree ggrroouunnddwwaatteerr eelleevvaattiioonn ccoonnttoouurr mmaappss.. FFiigguurreess 33--22 tthhrroouugghh 33--55 pprreesseenntt ggrroouunnddwwaatteerr eelleevvaattiioonn ccoonnttoouurr mmaappss ccoonnssttrruucctteeddffoorr JJaannuuaaryry,, AApprirli,l, AAuugguusstt,, aanndd DDeecceemmbbeerr 22001144.. AAss sshhoowwnn iinn FFiigguurreess 33--22 tthhrroouugghh 33--55,, tthhee ddiirreeccttiioonn ooff ggrroouunnddwwaatteerr ffllooww iiss ccoonnssiisstteennttllyy ttoo tthhee ssoouutthh ttoowwaarrdd tthhee MMisisssiissssiippppii RRiivveerr.. AA mmooddeerraattee hhyyddrraauulliicc ggrraaddiieenntt ooff 00..000099 ((fUt/Rft)) iiss ccaallccuullaatteedd aalloonngg tthhee iinntteerrpprreetteedd ddiirreeccttiioonn ooff ggrroouunnddwwaatteerr ffllooww ffrroomm mmoonniittoorriinngg wweellll MMWW--0011 ttoo tthhee MMisisssiissssiippppii RRiivveerr.. AArreeaass ooff ddeepprreessssiioonn iinn tthhee ggrroouunnddwwaatteerr ssuurrffaaccee iinndduucceedd bbyy tthhee ppuummppiinngg ooff pprroodduuccttiioonn wweellllss PPWW--0022,, PPWW--0035,, PPWW--0009 aanndd PPWW--1100 aarree eevviiddeenntt iinn aallllooff tthhee ggrroouunnddwwaatteerr eelleevvaattiioonn ccoonnttoouurr mmaappss.. AAss ppaarrtt ooff tthhee eexxtteennddeedd ppiilloott ppuummpp tteesstt,, pprroodduuccttiioonn wweellll PPWW--0099 wwaass ooppeerraattiinngg aatt 990000 ggppmm oonn JJaannuuaarryy 2222,, 22001144.. AAss sshhoowwnn iinn FFiigguurree 33--22,, tthhee eeffffeecctt ooff pprroodduuccttiioonn wweellll PPWW--0099 ooppeerraattiinngg aatt tthhiiss hhiigghh ffllooww rraattee ccrreeaatteess aa llaarrggeerr ccoonnee ooff ddeepprreessssiioonn iinn tthhee ggrroouunnddwwaatteerr ssuurrffaaccee ccoommppaarreedd ttoo tthhee ggrroouunnddwwaatteerr eelleevvaattiioonn ccoonnttoouurr mmaappss ffoorr tthhee ootthheerr ddaatteess;; hhoowweevvere,r, tthhee eeffffeecctt ooff ccoonnttiinnuuoouuss ppuummppiinnggooff pprroodduuccttiioonn wweellllss PPWW--0099 aanndd PPWW--1100 iiss aallssoo eevviiddeenntt iinn tthhee ggrroouunnddwwaatteerr eelleevvaattiioonn mmaappss ccoonnssttrruucctteedd ffoorr AApprirli,l AAuugguusstt aanndd DDeecceemmbbeerr 22001144.. 33.22 EEXXTTEENNDDEEDD PPIILLOOTT PPUUMMPP TTEESSTT TThhee eexxtteennddeedd ppiilloott ppuummpp tteesstt wwaass ppeerrffoorrmmeedd aatt tthhee SSiittee ffrroomm FFeebbrruuaarryy 22001133 tthhrroouugghh FFeebbrruuaarryy 22001144.. TThhee pprriimmaarryy ppuurrppoossee ooff tthhee ppuummpp tteesstt wwaass ttoo pprroovviiddee iinnffoorrmmaattiioonn ttoo `ccoommpplleettee tthhee ddeessiiggnnooff aa ggrroouunnddwwaatteerr iinntteerrcceeppttiioonn ssyysstteemm iinn aaccccoorrddaannccee wwiitthh tthhee aapppprroovveedd RRDD//RRAA PPllaann aanndd tthhee MMiinnnneessoottaa DDeecciissiioonn DDooccuummeenntt ((MMDDDD)) ffoorr tthhee SSiittee.. "TThhee ccuurrrreenntt ggrroouunnddwwaatteerr rreeccoovveerryy nneettwwoorrkk ccoonnssiissttss ooff SSiittee pprroodduuccttiioonn wweellllss PPWW--0055,, PPWW-0099 aanndd PPWW-1-100.. TThhee eexxtteennddeedd ppiilloott ppuummpp tteesstt ccoonnssiisstteedd ooff ccoonnttiinnuuiinngg ttoo ppuummpp pprroodduuccttiioonn Z:~FOL DE R-G O-9\3m-c~ttage~rove\WE~TON-Reports~2O 14~Q-AnnuaI-G~/~CGMN_2014_Ann ual_Report.docx 33-22 33663300..00002255 3M_MNO1595974 3M MN01595974 WEEE wweellll PPWW--0055,, aanndd vvaarryyiinngg tthhee ffllooww rraatteess aatt pprroodduuccttiioonn wweellllss PPWW--0099 aanndd PPWW--1100 wwhhiillee ccoolllleeccttiinngg wwaatteerr lleevveell ddaattaa aatt nneeaarrbbyy mmoonnititoorriinngg wweellllss.. TThhee wwaatteerr lleevveell ddaattaa wweerree uusseedd ttoo ccaallccuullaattee tthhee aarreeaa ooff ggrroouunnddwwaatteerr ccaappttuurree zzoonneess iinndduucceedd bbyy pprroodduuccttiioonn wweellllss PPWW--0099 aanndd PPWW--1100 aatt vvaarriioouuss ffllooww rraatteess.. 'Tlhhee ppuummpp tfeesstt wwaass ccoonndduucctteedd iinn aaccccoorrddaannccee wwiitthh tthhee aapppprroovveedd ppuummpp tteesstt wwoorrkk ppllaann ((WWEESSTTOONN,, 22001133)) aanndd ccoonnttiinnuueedd uunnttiill ssuuffffiicciieenntt ooppeerraattiioonnaall ddaattaa wweerree ccaolllleecctteedd t1o0 aallllooww ccoommpplelettiioonnooff tthhee ffiinnaall ddeessiiggnn ooff tthhee ggrroouunnddwwaatteerr iinntteerrcceeppttiioonn ssyysstteemm wwiitthh rreessppeecctt ttoo tthhee nnuummbbeerr,, ssppaacciinngg aanndd ppuummppiinngg rraatteess ffoorr tthhee pprroodduuccttiioonn ((eexxttrraaccttiioonn)) wweellll nneettwwoorrkk.. "TThhee pprrooppoosseedd ffiinnaall ddeessiiggnn ooft'tthhee ggrroouunnddwwaatteerr iinntteerrcceeppttiioonn ssyysstieemm wwaass ddeetteerrmmiinneedd uussiinngg aa ccoommbbiinnaattiioonn ooff ggrroouunnddwwaatteerr eelleevvaattiioonn ddaattaa ccoolllleecctteedd dduurriinngg tthhee eexxtteennddeedd ppiilloott ppuummpp tteesstt aanndd ppeerrffoorrmmiinngg pprreeddiiccttiivvee ssiimmuullaattiioonnss uussiinngg aa ggrroouunnddwwaatteerr ffllooww mmooddeell ccaalliibbrraatteedd ttoo SSiittee hhyyddrrooggeeoollooggiiec ccoonnddititiioonnss.. TThhee rreessuullttss ooff tthhiiss aannaallyyssiiss iinnddiiccaatteedd tthhaatt tthhee rreeccoommmmeennddeedd ggrroouunnddwwaatteerr iinntteerrcceeppttiioonn ssyysstteemm wwoouulldd ccoonnssiisstt ooff pprroodduuccttiioonn wweellll PPWWO0S5//PPWW--0066 ((oorr aa rreeppllaacceemmeenntt)),, PPWW--0099,, PPWW--1100 aanndd oonnee aaddddiittiioonnaall nneeww wweellll bbeettwweeeenn pprroodduuccttiioonn wweellllss PPW W--S5//PPWW--0066 aanndd PPWW-0-099.. DDeettaaiillss ooff tthhiiss aannaallyyssiiss wweerree pprroovviiddeedd iinn aa sseeppaarraattee ddooccuummeenntt tthhaatt wwaass ssuubbmmiitttteedd ttoo tthhee MMPPCCAA iinn MMaarrcchh 22001155 ((WWEESSTTOONN,, 22001155)). 33..33 GGRROOUUNNDDWWAATTEERR QQUUAALLIITTYY QQuuaarriteerrllyy ggrroouunnddwwaatteerr ssaammpplliinngg eevveennttss wweerree ppeerrffoorrmmeedd iinn JJaannuuaarryy,, JJuullyy aanndd OOccttoobbeerr 22001144.. TThhee aannnnuuaall ggrroouunnddwwaatteerr ssaammpplliinngg eevveenntt wwaass ppeerrffoorrmmeedd iinn AApprriill 22001144.. TTaabbllee 33--22 ccoonnttaaiinnss aa ssuummmmaarryy ooff ggrroouunnddwwaatteerr PPFFCC aannaallyyttiiccaall ddaattaa ffoorr tthhee ggrroouunnddwwaatteerr ssaammpplliinngg ppeerrffoorrmmeedd ssiinnccee tthhee OOccttoobbeerr 22001122 bbaasseelliinnee ssaammpplliinngg eevveennt.t. LLaabboorraattoorryy aannaallyyttiiccaall ppaacckkaaggeess aanndd cchhaaiinn--ooff--ccuussitooddyy ddooccuummenetnatattiioonn If'oorr tthhee 22001144 ssaammpplliinngg eevveennttss aarree iinncclluuddeedd iinn AAttttaacchhmmeenntt DD.. PPFBBAA,, PPFFOOAA aanndd PPFFOOSS ccoonncceennttrraattiioonnss ffoorr sseellceectt wweellllss aarree ppllootttteedd oonn ttrreenndd ggrraapphhss aanndd pprroovviiddeedd iinn AAttttaacchhmmeenntt EE.. TThhee PPFFCC aannaallyyttiiccaall ddaattaa wweerree eevvaalluuaatteedd bbyy aappppllyyiinngg tthhee MMaannnnKKeennddaallll ttrreenndd tteesstt ((aatt aann a~z == 00.00S5 ssiiggnniiffiiccaannccee lleevveell)) ttoo PPFFBBAA,, PPFFOOAA,, PPFFOOSS aanndd PPFFHHSS ccoonncceennttrraattiioonnss ffoorr tthhoossee SSiittee mmoonniittoorriinngg wweellllss wwhheerree ssuuffffiicciieenntt hhiissttoorriiccaall ggrroouunnddwwaatteerr aannaallyyttiiccaall ddaattaa aarree aavvaaiillaabbllee ((ii.ce.. nn>>=-55)).. TThhee MMaannnn--KKenendadlalll trreenndd tteesstt iiss aa nnoonn--ppaarraammeettrriicc ssttaattiissttiiccaall pprroocceedduurree tthhaatt iiss uusseedd ffoorr aannaallyyzziinngg ttrreennddss iinn ddaattaa oovveerr ttiimmee ((GGiillbbeerr:t,, 11998877)). Z:~FOL DE R-G O-9\3m-c~ttage~qrove\WE-~TON-Reports~2(] 14~Q-AnnuaI-GV~CGMN_2014_Ann ual_Report.docx 33-33 33663300..00002266 3M_MNO1595975 3M MN01595975 Nonparametric methods require no assumptions regarding the underlying statistical distribution of the data. The outcome of the procedure depends on the ranking of individual data points and not the overall magnitude of the data points. The Mann-Kendall procedure can be used for data sets that include irregular sampling intervals, data below the detection limit, and trace or missing data. The method may be applied to track data trends for purpose of groundwater compliance monitoring, site assessment, and monitoring of the perrffoorrmmance of groundwwaatteerr coorrrreccttiivve accttiioons ((UUSEPAA,, 2000099)).. MMaannnn--KKeennddaallll tteesstt outcomes consist of the identification of statistically significant increasing trends, no statistically significant trend or a statistically significant decreasing trend at the specified significance level. Table 3-3 provides a summary of the results of the Mann-Kendall analysis, and a ddiissccuussssiioonn ooff tthhee ggrroouunnddwwaatteerr aannaallyyttiiccaall rreessuullttss iiss pprroovviiddeedd iinn tthhee ffoolllloowwiinngg ssuubbsseeccttiioonnss.. `TThhee ddiissccuussssiioonnoofgf rgorouunnddwwataeterr aannaallyyttiiccaall rreessuullttss iiss oorrggaanniizzeedd bbyy tthhee llooccaattiioonn ooff wweellllss bbyy Site area and focused primarily on the PFBA, PFOS and PFOA results. However, the analytical results for other PFCs are discussed where pertinent. 33..3..11 BBaacckgrroouunndd TTaabbllee 33--22 pprroovviiddeess aa ssuummmmaarryy ooff bbaacckkggrroouunndd ggrroouunnddwwaatteerr aannaallyyttiiccaall rreessuullttss ccoolllleecctteedd from monitoring well MW-07. As shown on Figure 2-1, monitoring well MW-07 is llooccaatteedd ttoo tthhee nnoorrtthheeaassttooff tthhee CCoottttaaggee GGrroovvee PPllaanntt nneeaarr HHiigghhwwaayy 6611. TThhee ggrroouunnddwwaatteerr aannaallyyttiiccaall ddaattaa ffoorr tthhee ppeerriioodd OOccttoobbeerr 22001122 tthhrroouugghh OOccttoobbeerr 22001144 indicates PFBA, PFOA and PFOS are consistently detected in the samples collected from monitoring well MW-07. PFBS, PFHA, PFHpA, PFHS and PFPeA were also detected. The Mann-Kendall results presented in Table 3-3 indicate a statistically significant increasing trend for PFOS, PFOA, PFBS and PFHS, while no statistically significant trend was identified for PFBA in the period October 2012 through October 2014. Groundwater elevation data for the Site have consistently shown that monitoring well MW-07 is hhyyddrraauulliiccaallllyy uuppggrraaddiieeanttooff tthhee ppllaanntt aanndd tthhee ffoorrmmeerr ddiissppoossaall aarreeaass oonn SSiittee ((sseeee FFiigguurreess 33--22 Z:~FOL DE R-G O-9\3m-c~ttage~rove\WE~TON-Reports~2014~Q-AnnuaI-G~/~CGMN_2014_Ann ual_Report.docx 3-4 33663300..00002277 3M MN01595976 ESE tthhrroouugghh 33--55)).. 33MM iiss nnoott aawwaarree ooff tthhee ssoouurrccee ffoorr PPFFCCss iinn ggrroouunnddwwaatteerr aatt tthhiiss uuppggrraaddiieenntt llooccaattiioonn. 333.3..22 DDUI/DD22 AArreeaa SSooiill eexxccaavvaattiioonn aaccttiivviittiieess wweerree ppeerrffoorrmmeedd tf'rroomm DDeecceemmbbeerr 22000099 tthhrroouugghh MMaayy 22001100 iinn tthhee DDI1//DD22 AArreeaa tthhaatt iinncclluuddeedd tthhee rreemmoovvaall,, aanndd ooffff-ssiittee ddiissppoossaall aatt aa ppeerrmmiitttteedd ffaacciilliittyy,, ooff aapppprrooxxiimmaatteellyy 1155~.000000 ccuubbiicc yyaarrddss ((yydd3)) ooff" PPFFCCc-ocnotnataiinniinngg ssooiill. WWeellllss MMWW-1-10011,, MW- MW- 110022,, MMWW--110033 aanndd MMWW--110044 mmoonniittoorr ggrroouunnddwwaatteerr ccoonnddiittiioonnss nneeaarr tthhee DDI1//DD22 AArreeaa. MMoonnititoorriinngg wweellll MMWW--111122 wwaass iinnssttaalllleedd ttoo tthhee eeaasstt ooff tthhee DDI1//DD22 AArreeaa iinn MMaayy 22001133. AAlltthhoouugghh nnoott iinncclluuddeedd iinn tthhee lliisstt ooff mmoonniittoorriinngg wweellllss iinn tthhee lloonngg--tteerrmm ssaammpplliinngg pprrooggrraamm ffoorr tthhee SSiittee,, aa ggrroouunnddwwaatteerr ssaammppllee wwaass ccoolllleecctteedd ffrroomm nneewwllyy iinnssttaalllleedd mmoonniittoorriinngg wweellll MMWW--111122 dduurriinngg tthhee JJuullyy 22001133 ssaammpplliinngg eevveenntt ttoo pprroovviiddee bbaasseelliinnee PPFFCCss ggrroouunnddwwaatteerr qquuaalliittyy ddaattaa. AAss sshhoowwnn iinn TTaabbllee 33--22,, PPFFBBAA,, PPFFBBSS,, PPFFOOAA,, PPFEHHAA,, PPFFHHppAA,, PPFFHHSS,, PPFENNAA,, PPFFOOAA,, PPFFOOSS aanndd PPFEPPeeAA aarree ccoonnssiisstteennttllyy ddeetteecctteedd iinn ggrroouunnddwwaatteerr ssaammpplleess ccoolllleecctteedd ffrroomm mmoonniittoorriinngg wweellllss MMWW-1-10011,, MMWW-1-10022,, MMWW--110033 aanndd MMWW-1-01404.. IInn aaccccoorrddaannccee wwiitthh tthhee GGrroouunnddwwaatteerr SSaammpplliinngg PPllaann,, qquuaarrtteerrllyy ggrroouunnddwwaatteerr ssaammpplleess aarree ccoolllleecctteedd ffrroomm mmoonniittoorriinngg wweellllss MMWW-- 110011 aanndd MMWW-1-10044,, wwhhiillee mmoonniittoorriinngg wweellllss MMWW--110022 aanndd MMWW--110033 aarree ssaammpplleedd aannnnuuaallllyy.. DDeetteecctteedd PPFFCC ccoonncceennttrraattiioonnss aarree ggeenneerraallllyy hhiigghheesstt iinn MMWW-1-0110.1. PPFFBBAA aanndd PPFFIHISS ccoonncceennttrraattiioonnss aarree hhiigghheerr iinn MMWW--110011 aanndd MMWW--110022 ((DD11 AArreeea)) ccoommppaarreed ttoo tthhee rreessuullttss ffoorr lmnoonniittoorriinngg wweellllss MMWW--110033 aanndd MMWW-1-10044 ((DD22 AArreeaa)).. PPFFOOAA ccoonncceennttrraattiioonnss iinn tthhee ppeerriioodd OOccttoobbeerr 22001122 tthhrroouugghh OOccttoobbeerr 22001144 rraannggeedd ffrroomm 3355..11 gugg//LL ((MMWW--110044)) ttoo 147 147 pg/L ~ag/L (MW- (MW- 110011)).. PPFROOSS ccoonncceennttrraattiioonnss aarree ccoonnssiissteennttllyy lloowweesstt iinn mmoonniittoorriinngg wweellll MMWW--110033 ((11..5555 ttoo 77..8822 ~ugtg//LL))., wwhhiillee tthhee PPFFOOSS rreessuullttss ffoorr mmoonniittoorriinngg wweellllss MMWW-1-10011,, MMWW--110022 aanndd MMWW--110044 wweerreeccoommppaarraabbllee ((110077 t1o0 225500 ~g/gL/L.)). TThhee MMaannnn--KKeennddaallll trreenndd tteesstt iinnddiiccaatteedd nnoo ssttaattiissttiiccaallllyy ssiiggnniiffiiccaanntt ttrreenndd ffoorr PPFEOOSS,, PPFFOOAA,, PPFEBBAA oorr PPFFHHSS ffoorr mmoonniittoorriinngg wweellll MMWW--110044 ((TTaabbllee 33--33)).. AA ssutattiissitiiccaallllyy ssiiggnniiffiiccaanntt ddeeccrreeaassiinngg PPFFOOSS,, PPFFOOAA,, PPFFBBAA aanndd PPFFHHSS ttrreenndd wwaass iiddeennttiiffiieedd iinn mmoonniittoorriinngg wweellll MMWW-110011,, wwhhiillee aa ssttaattiissttiiccaallllyy ssiiggnniiffiiccaanntt ddeeccrreeaassiinngg PPFFBBSS ttrreenndd wwaass ddeetteerrmmiinneedd ffoorr mmoonniittoorriinngg wweellll MMWW-1-01044.. AA ssttaattiissttiiccaallllyy ssiiggnniiffiiccaanntt iinnccrreeaassiinngg PPFFBBSS ttrreenndd wwaass ddeetteerrmmiinneedd ffborr Z:~FOL DE R-G O-9\3m-cottage_grove\WE-~TON-Reports~2(] 14~Q-AnnuaI-GV~CGMN_2014_Ann ual_Report.docx 33-s5 33663300..00002288 3M_MNotS5977 3M MN01595977 mmoonniittoorriinngg wweellll MMWW-1-10011,, aalltthhoouugghh PPFFBBSS ccoonncceennttrraattiioonnss hhaavvee fflluuccttuuaatteedd iinn aa rreellaattiivveellyy nnaarrrrooww rraannggee ooff 1199..55 ttoo 337.78.8 u~ayg/.L. IInnssuuffffiicciieenntt ddaattaa iiss ccuurrrreennttllyy aavvaaiillaabbllee t1o0 eessitaabblliisshh aa ttrreenndd aappppllyyiinngg tthhee MMaannnn--KKeennddaallll tteesstt ttoo PPFECCss ddeetteecctteedd iinn mmoonniittoorriinngg wweellllss MMWW--110022 aanndd MMWW-1-0130.3. AA ccuurrssoorryy rreevviieeww ooff tthhee rreessuullttss iinn TTaabbllee 33--22 ffoorr mmoonniittoorriinngg wweellllss MMWW--110022 aanndd MMWW--110033 iinnddiiccaatteess tthhaatt tthhee PPFFCC ccoonncceennttrraattiioonnss fflluuccttuuaattee wwiitthh nnoodidsicsceerrnniibbllee ttrreenndd.. 33.33.33 DD99 AArreeaa IInntthhee DD99 AArreeaa,, ssooiill eexxccaavvaattiioonn aaccttiivviittiieess wweerree ppeerrffoorrmmeedd ffrroomm MMaayy tthhrroouugghh AAuugguusstt 22001100 wwiitthh tthhee rreemmoovvaall,, aanndd ooffff-ssiittee ddiissppoossaall aatt aa ppeerrmmiittteedd ffaacciilliittyy,, ooff aapppprrooxxiimmaatteellyy 48,04000 yydd"3 ooff ssooili.l. W Welelllss MMWW--110055 aanndd MMWW--1133 mmoorniittoorr ggrroouunnddwwaatteerr qquuaalliittyy ccoonnddiittiioonnss nneeaarr tthhee DDO9 AArreeaa.. TThhee ccoonnttiinnuueedd ppuummppiinngg ooff pprroodduuccttiioonn wweellll PPWW--0099 iiss rreemmeeddiiaattiinngg PPFFCCss iinn gsrroouunnddwwaatteerr iinn tthhee DD99 AArreeaa (aanndd aa ppoorrtiioonnooff tthhee WWWWTTPP aanndd DDI1//DD22 AArreeaass)).. AA ccoommppaarriissoonn ooff tthhee PPFFCC aannaallyyttiiccaall ddaattaa ssuummmmarariizzeedd iinn TTaabbllee 33--22 ffoorr mmoonniittoorriinngg wweellllss MMWW--1133 aanndd MMWW--110055 iinnddiiccaatteess hhiigghheerr PPFFCC ccoonncceennttrraattiioonnss iinn mmoonniittoorriinngg wweellll MMWW--110055 ccoommppaarreedd ttoo MMWW-1-31.3. MMoonnititoorriinngg wweellll MMWW--110055 iiss iimmmmedeidaiatteellyy ddoowwnnggrraaddiieennttooff tthhee DDO9 AArreeaa wwhhiillee mmoonniittoorriinngg wweellll MMWW--1133 iiss sslliigghhttllyy ttoo tthhee wweessttoofftthhee lliimmiittss oofftthhee DDO9 AArreeaa. AA vviissuuaall iinnssppeeccttiioonnooff tthhee PPFFCC rreessuultss ffoorr pprroodduuccttiioonn wweellll PPWW--0099 iinn TTaabbllee 33--22 ssuuggggeessttss aann iinnccrreeaassee iinn PPFFCC ccoonncceennttrraattiioonnss aatt tthhiiss ppuummppiinngg cceenntteerr,, aanndd tthhee MMaannnn--KKeennddaallll ttrreenndd tteesstt iiddeenntiiffieess aa ssttaattiissttiiccaallllyy ssiiggnniiffiiccaanntt iinnccrreeaassiinngg ttrreenndd iinn PPFFOOSS aanndd PPFFOOAA ccoonncceennttrraattiioonn ffoorr pprroodduuccttiioonn wweellll PPWW-0-099.. AAss sshhoowwnn iinn TTaabbllee 33--33,, aa ssatattiissttiiccaallllyy ssiiggnniiffiiccaanntt ddeeccrreeaassiinngg ttrreenndd wwaass iiddeennttiiffiieedd ffoorr PPFFOOAA aanndd PPFFBBSS ffoorr mmoonnititoorriinngg wweellll MMWW-1-01055.. NNoo. ssutattiisstticcaallllyy ssiiggnniiffiiccaanntt ttrreenndd wwaass iiddeennitiiffiieedd ffoorr tthhee rreemmaaiinniinngg PPFFCCss ffoorr tthhee MMaannnn--KKeennddaallll aannaallyyssiiss ppeerrffoorrmmeedd ffoorr mmoonniittoorriinngg wweellllss MMWW--110055 aanndd pprroodduuccttiioonn wweellll PPWW-0-099.. FFuurrtthheerr,, nnoo sstaattisstticcaalllyy ssiiggnniiffiiccaanntt ttrreenndd iinn PPFFCCss wwaass iiddeennttiiffiieedd ffoorr mmoonniittoorriinngg wweellll MMWW--1133. 333.3..44 VWVWWTTPP AArreeaa MMoonnititoorriinngg wweellll MMWW--110088 iiss iinncclluuddeedd iinn tthhee qquuaarrtteerrllyy ggrroouunnddwwaatteerr ssaammpplliinngg pprrooggrraamm ttoo pprroovviiddee ggrroouunnddwwaatteerr qquuaalliittyy ddaattaa ddoowwnnggraraddiieenntt ooff tthhee SSiittee wwaassttee wwaatteerr ttrreeaattmmeenntt ppllaanntt ((WWWWTTPP)) aarreeaa.. AAss sshhoowwnn iinntthhee PPFFCC aannaallyyttiiccaall ddaataa pprroovviiddeedd iinn TTaabbllee 33--22 aanndd ttrreenndd ggrraapphh pprreesseenntteedd iinn AAtttaacchhmmeenntt EE,, PPFFCC ccoonncceennttrraattiioonnss ccoonnttiinnuuee ttoo fflluuccttuuaattee iinn mmoonniittoorriinngg wweellll corms Z:~FOL DE R-G O-9\3m-c~ttage~rove\WE~TON-Reports~2014~Q-AnnuaI-G~/~CGMN_2014_Ann ual_Report.docx 3-6 SW_MNo1S95078 3M MN01595978 33663300..00002299 MW-108 with a temporary increase in PFCs in July 2014. Prior to July 2014, PFC concentrations showed a general decline over time. The Mann-Kendall trend analysis for monitoring well MW-108 indicated a statistically significant decreasing trend in PFHS and no statistically significant trend tbr the remaining PFr2s analyzed. 3.3.5 D5 Area Monitoring wells MW-ll0~ MW-12 and MW-16 provide groundwater quality and eelleevvaattiioonn ddaattaa ffoorr tthhee DDS5 AArreeaa.. MMoonnititoorriinngg wweellll MMWW--1122 iiss llooccaatteedd wwiitthhiinn tthheelilmimititss ooff tthhee D5 Area, while monitoring wells MW-ll0 and MW-16 are located immediately south to southeast (downgradient) of the D5 Area (see Figure 2-1). As shown in Table 3-23 prior to 2014, PFBA, PFOS and PFOA concentrations for monitoring well MW-12 are higher ccoommppaarreedd ttoo mmoonniittoorriinngg wweellllss MMWW--111100 aanndd MMWW-1-616.. CCoommppaarriinngg tthhee PPFFCC rreessuullttss ffoorr 22001144 to previous PFC data for D5 area monitoring wells, PFC concentrations have decreased for monitoring well MW-12 while an increase in some PFCs (e.g. PFOA) were apparent in monitoring wells MW- 110 and MW- 16. The Mann-Kendall trend test provides the following results: Monitoring well MW-12: Statistically significant decreasing trend for PFOS, PFOA, PFBA, PFBS and PFHS. * MMoonniittoorriinngg wweellll MMWW-1-1101:0: SSttaattiissttiiccaallllyy ssiiggnniiffiiccaanntt ddeeccrreeaassiinngg ttrreenndd ffoorr PPFFOOSS.. SSttaattiissttiiccaallllyy ssiiggnniiffiiccaanntt iinnccrreeaassiinngg ttrreenndd iinn PPFFOOAA,, PPFFBBAA,, PPFBBSS aanndd PPFFHHSS.. + MMoonintitoorriinngg wweellll MMWW-1-166:: NNoo ssttaattiissttiiccaallllyy ssiiggnniiffiiccaanntt ttrreenndd ffoorr PPFFOOSS oorr PPFFBBAA.. AA statistically significant increasing trend for PFOA, PFBS and PFHS. In the final design of the groundwater interception system for the Site, discussed in ssuubbsseeccttiioonn 33..22,, aann aaddddiittiioonnaall pprroodduuccttiioonn ((rreeccoovveerryy)) wweellll iiss rreeccoommmmeennddeedd ttoo bbee iinnssttaalllleedd between existing production wells PW-05/PW-06 and PW-09. 3.3.6 D8 Area As discussed in Section 2.1, quarterly groundwater samples were to be collected from pprroodduuccttiioonn wweellll PPWW--0055//PPWW-0-066.. HHoowweevveerr,, dduuee ttoo aa ddeecclliinniinngg yyiieelldd,, tthhee uussee ooff pprroodduuccttiioonn ee well PW-05iPW-06 was scaled back in March 2013 to intermittent use. To compensate for Z:~FOL DE R-G O-9\3m-c~ttage~rove\WE~TON-Reports~20144Q-AnnuaI-G~/~CGMN_2014_Ann ual_Report.docx 3-7 3M MN01595979 33663300..00003300 the reduction in flow of production well PW-06, the plant water supply demands were met by pumping nearby production well PW-05 at a higher average flow rate. In 2014, production well PW-05 operated at an average flow rate of 916 gpm, which represents the highest flow rate for all the Site production wells. Monitoring well MW-14R is located between production wells PW-05 and PW-06 to the southwest (hydraulically downgradient) of the D8 Area. Following MPCA approval in January 2014, quarterly groundwwaatteerr sammppllees wweerre coolllleectteed ffrroomm mmoonniittoorriinng wweellll MMWW-1-144RR,, as a rreeppllaacceemmeenntt monitoring point for production xvell PW-06. A review of the PFC analytical data provided in Table 3-2, and trend graphs provided in Attachment E, for monitoring well MW-14R visually indicates an increasing trend in PFC concentrations. However, as shown in Table 3-3, the Mann-Kendall analysis identified no statistically significant trend for PFCs except fbr a statistically significant increasing trend 257 Emcoers forPFBS. 3.3.7 East Cove Area RReemmeeddiaiall aaccttiivviittiieess iinn tthhee EEaasstt CCoovvee aarreeaa iinncclluuddeedd tthhee rreemmoovvaall,, aanndd ooffff--ssiittee ddiissppoossaall aatt a permmiitttteed lannddfiflill,l, ooff appprroxxiimmaatteelly 16,,5500 yd~' ooff seddiimmeennt.t. TThheesse accttivviitiiees wweerre performed from August 2011 through January 2012. Production well PW-10 was installed to contain and remove groundwater potentially impacted with PFCs in the East Cove area. TTaabbllee 33--22,, aanndd tthhee ttrreenndd ggrraapphhss pprroovviiddeedd iinn AAttttaacchhlmneenntt EE., pprreesseenntt tthhee ggrroouunnddwwaatteerr analytical results through October 2014 for production well PW-10. A cursory review of the PFC analytical results for PW-10 indicates generally stable concentrations. This observation is confirmed by the Mann-Kendall trend test that indicated no statistically ssiiggnniiffiiccaanntt ttrreennddss ffoorr tthhee PPFFCCss aannaallyyzzeedd eexxcceepptt ffoorr PPFFHHSS wwhheerree aa ssttaattiissttiiccaallllyy ssiiggnniiffiiccaanntt 44 PORE WATERSWUARTEFRQRURGLITEY decreasing trend was identified. 3.4 PORE WATER/SURFACE WATER QUALITY As described in the Groundwater, Pore Wawr, and Surface Wawr Sampling Plan for PPeertfflluuoorroocchheemmiiccaallss ((PPFFCCs~)9 ((SSaammpplliinngg PPllaann)) ssuubbmmitittteedd ttoo tthhee M MPPCCAA iinn AApprriill 22001122,, tthhrreeee pore water/surface water sampling events were conducted at the same locations where ee Z:~FOL DE R-G O-9\3m-c~ttage~qrove\WE~TON-Reports~2O 14~Q-AnnuaI-G~/~CGMN_2014_Ann ual_Rep~rt.docx 3-8 3M MN01595980 33663300..00003311 WEEE ssaammpplliinngg wwaass ppeerrffoorrmmeedd. pprreevviioouussllyy iinn SSeepptteemmbbeerr//OOccttoobbeerr 22000066 aanndd JJuunnee 2200111.1. TThhee aaddddiittiioonnaall tthhrreeee ssaammpplliinngg eevveennttss wweerree ccoonndduucctteedd pprriioorr t(o0 ((OOccttoobbeerr 22001122)),, dduurriinngg ((AAuugguusstt 22001133)),, aanndd aaffteerr ((SSeepptteemmbbeerr//OOccttoobbeerr 22001144)) tthhee eexxtteennddeedd ppiilloott ppuummpp tteesstt.. TThheessee ppoorree wwaatteerr ssaammpplliinngg eevveennttss ccoommpplleettee tthhee ppoorree wwaatteerr aanndd ssuurrffaaccee ssaammpplliinngg ccoommmmititmmeenntt mmaaddee ttoo MMPPCCAA iinn tthhee SSaammpplliinngg PPllaann.. "TThhee llaabboorraattoorryy PPFFCC aannaallyyttiiccaall ddaattaa ppaacckkaaggee ffoorr tthhee SSeepptteemmbbeerr//OOccttoobbeerr 22001144 ssaammpplliinngg eevveenntt iiss pprroovviiddeedd iinn AAttttaacchhmmeenntt FF.. AA ssuummmmaariyy ooff tthhee ppoorree wwaatteerr aanndd ssuurrffaaccee wwaatteerr aannaallyyttiiccaall rreessuullttss ffrroomm tthhee pprree--,, mmiidd--,, aanndd ppoosstt eexxtteennddeedd ppiilloott ppuummpp tteesstt ssaammpplliinngg eevveennttss aarree pprroovviiddeedd iinn TTaabbllee 33--44.. TThhee PPFFCC aannaallyyttiiccaall rreessuullttss ffoorr tthhee SSeepptteemmbbeerr//OOccttoobbeerr 22000066 aanndd JJuunnee 22001111 ssaammpplliinngg eevveennttss ffoorr tthhee ssaammee llooccaattiioonnss aarree aallssoo pprroovviiddeedd iinn TTaabbllee 33--44 ffoorr ccoommppaarriissoonn ppuurrppoosseess.. TThhee ppoorree wwaatteerr aanndd ssuurrffaaccee wwaatteerr ssaammpplliinngg llooccaattiioonnss aarree pprroovviiddeedd iinn FFiigguurree 22--22.. AAss sshhoowwnn iinn FFiigguurree 22--22,, tthhee ppoorree wwaatteerr aanndd ssuurrffaaccee wwaatteerr ttrraannsseeccttss aarree llooccaatteedd ddowongrwadinentgoofftrthheefafoolllldoowwiiinnggSeSiitteenaarretesass:: + TTrraannsseeectt IIWW--0099:: ddoowwnnggraraddiieenntt ooff tthhee ffoorrmmeerr DDS5 AArreeaa o TTrraannsseeectt IIWW--1144:: ddoowwnnggraraddiieennttooff tthhee WWWWTTPP AArreeaa + TTrraannsseecctt IIWW--1199:: ddoowwnnggraraddiieenntt oofftthhee ffoorrmmeerr DDI1//DD22 AArreeaa TTrraannsseecctt lIWW--2255:: ddoowwnnggraraddiieenntt oofftthhee EEaasstt CCoovvee AArreeaa. "TThhee ffoolllloowwiinngg oobbsseerrvvaattiioonnss ffoorr tthhee ppoorree wwaatteerr aanndd ssuurrffaaccee wwaatteerr ddaattaa pprreesseenntteedd iinn TTaabbllee 33-44aarree pprroovviiddeedd: PFC concentrations PcoFnCcentrcaotnicoenns.trations iinn ppoorree wwaatteerr aarree hhiigghheerr tthhaann ssuurrffaaccee wwaatteerr PPFFCC concentrations. LoLtchoaactnaitliooocnnassticoclnloosssmeerorrt1eo0 dttihhseetassnhthoofrrreeolliimnneeshoggreeenn.eerraallllyy hhaadd hhiigghheerr ppoorree wwaatteerr ccoonncceennttrraattiioonnss than locations more distant from shore. PoProree wwaatteerr PPFFCCccooncnecnetnrtraattiioonnssfflluuccttuuaattee oovveerr tiimmee wwiitthh nnoo ddiisscceerrrniibbllee ttrreenndd.. + W Winhhteehrereerddeepetoteerccttiteenddg,,pPPerFFiCCosds iipnnrossvuuirrdffaaeccdeeiwwnaTatateebrrlhheaav3v-e4ef.lfluuccttuuaatteedd bbuutt hhaavvee ggeenneerraallllyy ddeecclliinneedd in the reporting period provided in Table 3-4. Z:~FOL DE R,S O-8\3m-cottage_grove\WE-~TON-Reports~2(] 14~O-AnnuaI-GV~GGMN_2014_Ann ual_Report.docx 33-09 33663300..00003322 3M_MNO1595981 3M MN01595981 Tamm EINESO J fa ONG Stee i NET CEE Hp AEE NE cil mE Se TA LE i=ae em f u - elLeo ati slwoe [To--m=e= plume Bo 4 ST Well L~catio{~s I3MM__MMNNO011559955096822 33663300..00003333 BE cee See NGL Legend ' Tehee .......... Gmu~dwate Elevation Cont,~ur Fas aN a eeSr I NFNNo YT A R= E ae SSELT - ce : 5N hk | "=m slSiaen Figure 3-2 Ela Bo "BL EE Groundwater ]~leva llon Contour Map 22 Janualw 2014 PW-02, PW~-05 ~ld PW-09 operating Cottage Grove Site Cottage Grove, _Minnesota 3M_MN01595983 33663300..000034 SE TESN Se ESs E SEaa te IW se nh Fy N CE NEEe Eree : Waee wa Pa L hirie # tom Piezometer Loca~io~t (PZ) &x b= ES aaAnaaWaLW EE Ed = rowers Figure 3-3 Groundwater Elevation Contour Map | wih 14 April 2014 em. Cottage Grove Eacili/y Cottage Grove, l~linuesota 3M_MN01595984 33663300..00003355 = LE BL EER - ENCE: EE BEE CN i NE ~ EET | LEE TR " IN X=Sr Er a EiL 3 TX AE Ea = \ CLAN Ef = ee RE oe) wm I wna |= ------ 2N ' on ne Ts blaEne s | Figure 3-4 Groundwater Elevation Contour Map en 6 Augusl 2014 PW-02, PW-05, PW-09 and PW-IO Operathtg Collage Grove Fadlity Cottage Grove~ Minnesota 3M_MN01595985 33663300..00003366 ENNELY EN EEE : SrvEsmmo oe me EEE ' Ne y Tas == N E: o S ikTaEhse=e5 : Thoraen GroulKiwat~r Ele~ aLlon Comeur (contour inter- M: || ar N a = 3 pS NoS e L w o T h EhEe = aSa] EEEET E Figure3-5 == SEE | Groul|dwater Elevation Contour Map 29 Decem her 2014 a ae EE and PW-10 Operating SE by Ee -- Cottage Grove Facility Cottage Grove, 1Minnesota 3M_MN01595986 33663300..00003377 October 2012 - De~ember 2014 Cottage Grove Site, Cottage Grove, 3,Iinnesota lE lzlesE lE=eTeEseE Tersslle E EEilsls==a=lEseEs=if sraEEclesiEas s aol] B HE eD eE EE E aE E EE E EE [LEEE e EE1 e e 2Sr1 e e iRI: R B 33MM__MMNNO011559955998877 33663300..00003388 a ~fable 3-1 (cont'd) Depth-to-Groundwater and Gro.ndw,~ter Elevation Data October 2012 - De ember 2014 TCC E L E EEB EEE E IREES a E IeSe E SlESE e sEa I eAe E E RE EsSeEEE he S= ee e EeE EIsREs SR Ee a a sRoe E E SFe Et[ Er E e N IeE | BSES| TR8e1S Elevation Jan.14 Depth to Groundwater Groundwater Igevation Cottage Grove Site, Cottage Grove, ~,~innesota Apr-~4 Depth to Groundwate[ Groundw=tl~ Elevation gug-14 Depth to Groundwater Groundwater Ele~ration Dec-t4 Depth Io Gr~ndwater Groundwater Elevati~ Groundwater Elevation Data Sta.dard 33MM__MMNNO011559955998888 33663300..00003399 SumofGmrosanTTdawarbteleesr3y2-P2FC Ausyica Data Summary of Groundwater PFC Analytical Data Cottag"e GrOovec2S0t2a,-OCcobtttoabgeeerGr0ro1v4e, MN October 2012 - October 2014 Cottage Grove Site, Cottage Grove, MN [so Well ID MW-07 tocinTon rese so for txsror--sp s er] Location Date PFBA PFBS PFDA PFDoA PFC Groundwater Results (ppb, ~tg/L) PIZHA PFHpA PFHS PFNA PFOA PFOS PFPeA PFUnA Background 10/15/2012 2.55 <0.0250 <00250 <0.0250 0.076 0.025 <0.0500 <0.0500 0.298 0.026 0.165 <0.0250 1/29/2013 209 < 0.0250 < 00250 0.259 0044 4/22/2013 2.61 0.027 < 0,0250 < 0.0250 0.064 0.265 < 0.0250 < 0.0250 0.240 0.046 0.153 < 0.0250 Ei 7/23/2013 1.71 10/28/2013 3.07 0.040 0.029 1/13/2014 2.88 <0.100 0.026 < 0.0250 0.045 0.303 0.428 0.390 0.241 0.104 0.104 4/23/2014 2.48 0.036 <(I.0250 <0.0250 0.078 <0.0250 <0.0250 <0.0250 0.344 0.049 0.153 <0.0250 7/16/2014 305 0.0762 00416 0.602 0237 10/28/2014 3.01 0.070 0.050 0.581 0.191 MW-101 D1/D2 M~V- 102 DI/D2 [| IVIV~- 103 D1/D2 10/18/2012 1860 23.9 0.424 1/30/2013 1630 25.2 4/23/2013 1830 19.5 0.365 7/25/2013 1680 24.0 10/28/2013 1020 25.5 1/15/2014 1510 25.4 4/25/2014 1330 37.8 0.241 7/17/2014 1460 29.3 10/29/2014 1410 29.6 10/18/2012 648 5.52 0.262 ova r ow | nr ove 4/25/2013 621 4/25/2014 919 4.57 7.12 0.345 0.136 10i18/2012 226 7.16 0.036 4/25/2013 241 7.01 <0.0250 4/25/2014 241 6.51 <11.0250 <0.0250 121 101 427 11.6 147 154 98.9 455 124 206 < 0.0250 85.4 85.6 459 9 I. I 121 188 96.4 464 112 189 314 86.7 158 398 79.4 159 <0.0250 61.1 62.3 364 6.96 76.0 135 72.2 480 83,9 193 452 74.8 170 <0.0250 14.8 9.52 129 3.2 42.2 1(17 18.2 {awe ewstewo rwiomr|r si er s | wr < 0.0250 18.7 13.3 401 12.0 62.0 250 23.2 <0.0250 28.8 16,0 147 1.87 58,1 67.4 30.7 <0.0250 54.9 29.7 26.2 0.045 115 4.02 25.5 <0.0250 49.5 25.6 24.7 8.01 126 1.55 26.7 <0.0250 57.4 30,9 21.8 0.053 121 7.82 28.2 <0.0250 0.046 <0.0250 <0.0250 eww 0.075 <0.0250 <0.0250 <0.0250 <0.0250 Page 1 or 6 SM_uno1695989 CGMN All FC data Cros~ah~hru-20$4~7-ZT(ISO-14).l~T~l~-O2-Data 3M_MN01595989 33663300..00004400 Tale 32 conti Table 3-2 (cont'd) SumofGmrounrdwayter PEC Anaya Dna Summary of Groundwater PFC Analytical Data ocaber 2013- October 2004 October 2012 - October 2014 Cottage Grove Sit, Cotage Grove, MN Cottage Grove Site, Cottage Grove, MN [esercinToes Well ID Location Date PFBA MacV- 104 DI/D2 10/18/2012 36.0 IE 1/'30/2013 4/2512013 36.3 74.7 7/'25/2013 54.3 10/'28/2013 53.6 1/15/2014 202 4/25/2014 107 7/17/2014 47.9 10/29/2014 30.9 MacV- 112 DIED2 7/'24/2013 4.42 PFBS 12.6 11.4 9.75 8.16 7.95 7.5(I g. 10 8.68 7.72 0.166 PFDA 2.78 2.90 3.26 srr PFDoA reso PFC Groundwater Results (ppb, pg/L) PIZHA PFHpA PFHS PFNA --sror--so--poeere| PFOA PFOS PFPeA PFUnA <0.0250 3.89 2.51 8.69 2.26 42.0 127 3.10 0.052 9.07 44.8 201 <0.0250 12.1 7.11 13.4 10.8 60,7 185 7.64 0.196 11.8 74.7 176 10.1 72.5 165 ]4.2 35.1 4.25 <0.0250 19.7 9.11 12.6 2.59 82.1 234 12.6 0.056 895 6.24 76.5 233 50.0 177 0.367 1.18 0.96 MW-105 D9 10/19/2012 52.7 9.46 0.991 <0.0250 16.2 14.7 18.9 0.836 98,3 120 6.11 <0.0250 1/'30/2013 54.4 8.03 21.1 119 129 4/'25/2013 57.1) 5.72 0.683 <0.0250 11.4 9.64 16.0 9.22 104 95.0 5.13 0.116 7/'25/2013 71.6 6.49 6.35 70.6 92.3 Ei 10/28/2013 1/14/2014 38.9 55.6 4.98 6.15 6.01 12.6 87.2 467 68,3 152 4/25/2014 71.0 7.68 0.334 <0.0250 11.8 8.64 8.59 0.583 44,3 58.7 6.05 <0,0250 7/17/2014 39.2 4.89 6.65 277 36.2 10/29/2014 46.3 4.01 18.9 92,8 73.5 SM_uno1895950 Page CGMN All FC data Cm~tab-thru-2014-07-17( -14) xIs; TblQ~-02-Data Ta~le~(ISO$4) 3M_MN01595990 33663300..00004411 Tale 32 conti Table 3-2 (cont'd) SumofGmrounrdwayter PEC Anaya Dna Summary of Groundwater PFC Analytical Data ocaber 2013- October 2004 October 2012 - October 2014 Cottage Grove Sit, Cotage Grove, MN Cottage Grove Site, Cottage Grove, MN [cso Well ID rcinToe res so w fot --sror ss ome] Location Date PFBA PFBS PFDA PFDoA PFC Groundwater Results (ppb, pg/L) PIZHA PFHpA PFHS PFNA PFOA PFOS PFPeA PFUnA MW-13 D9 10/17/2012 7.10 0.619 0.040 <0.0250 0.330 0.101 0.487 0.060 3.33 3.85 0.544 <0.0250 Ee 1/'29/2013 4/'24/2013 5.60 9.34 0560 0.972 7/'23/2013 8.30 1.07 0.033 <0.0250 0.227 0.116 0.396 0.931 1.05 ii 0.050 2.56 5.46 392 4.05 0.569 6.17 4.02 <0.0250 10/'28/2013 6.48 0.571 0.366 4.01 1.40 1/14/2014 9.80 1.20 0.969 9.78 3.08 4/24/2014 7.14 0.752 <[I.0250 <0.0250 0.257 0.078 0.556 0.045 8.63 2.33 0.465 <0.0250 7/16/2014 8.08 0.973 0.713 14.4 4.48 Bei PW-09 10/28/2014 9.64 1.09 0.720 10.0 4.89 D9 4/'25/2013 3.72 < 0.0250 < 0.0250 < 0.0250 0.0627 < 0.0250 < 0.0250 < 0.0250 0.223 0.324 0.191 < 0.0250 6/19/2013tl) 0.462 0376 7/24/2013 2.95 0.058 0.040 0.624 (I.622 8/29/2013(b 9/30/2013~b 0.605 0.87q 0.818 1.38 10/'28/2013 4.53 0.137 0.076 1.02 1.52 1/15/2014 4.76 0.173 0.109 1.33 2.13 4/25/2014 4.14 0.148 <[I.0250 <0.0250 0.135 0.0471 0.084 0.037 1.05 1.60 0.272 <0.0250 7/17/2014 4.32 0.155 0.081 1.16 1.79 10/30/2014 3.87 0.106 0.054 0.701 0.838 Sw_no1895081 CGMN All FC data Cros~tab-thru-2014-07-17( -14) xIs; TblQ~-02-Data Ta~les(ISO$4) 3M_MN01595991 33663300..00004422 Ta2 coent Table 3-2 (cont'd) Summaryof GroPFCvAneisDa Summary of Groundwater PFC Analytical Data om 03e omerot October 2012 - October 2014 Cote Grae Se Cone Grove MN Cottage Grove Site, Cottage Grove, MN Well ID [raeJrowcwiron TodaesaT] or| rore|oonw MTV=108 Location WWTP Date PFBA 10/18/2012 1/3{1/2013 4/25/2013 155 101 42.5 PFBS 30.5 26.5 16.1 PFDA {1.615 0.470 7/24/2013 38.0 14.6 10/28/2013 51.7 21.6 1/14/2014 51.6 17.0 4/25/2014 65.4 17.4 {1.562 7/17/2014 222 60.7 10/29/2014 87.0 22.7 ran PFDoA <0.0250 |<omo| <0.0250 <0.0250 vemPFC PIZHA psem Groundwater Results (ppb, PFHpA PFHS even pg/L) PFNA pPrFOoAx proper PFOS PFPeA wPeFeUnrA] 31.1 17.6 ew | wo | 6.90 4.50 10.2 4.15 21).7 2.76 551) a | wa | om | ] 1.1 348 4.95 83.2 201 4.94 202 4.47 218 4.13 169 3.58 1.26 164 11.3 522 8.50 268 55.2 ms | 45.5 37.3 26.8 33.2 33.5 43.3 58 42.0 25.4 <0.0250 0 | om 7.43 0.049 11.5 <0.0250 MTV-110 D5 10/18/2012 144 39.6 0.062 <0.0250 22.1 12.2 17.6 0.115 193 21.6 15.7 <0.0250 1/30/2013 171 46.6 10.3 141 28.6 4/25/2013 183 747 {1.085 <00250 26.4 105 11.8 843 160 264 20.7 <00250 Bie 7/24/2013 304 10/28/2013 174 43.8 94.8 1/14/2014 179 85.1 9.41 15.3 19.4 144 17.8 190 21.1 248 12.1 4/24/2014 189 86.1 <0.0250 <0.0250 32.9 12.7 20.9 0.194 310 12.5 24.0 <0.0250 7/16/2014 185 82.3 24.1 390 15.4 10/28/2014 294 576 23.5 417 129 awmorsseez CGMN All FC data Cros~tab-thru-2014-07-17( -14) xIs; TblQ~-02-Data Ta~les(ISO$4) 3M_MN01595992 33663300..00004433 [cso Well ID MW-12 rocinToes Location Date PFBA D5 10/19/2012 975 1/30/2013 484 4/'25/2013 622 7/'24/2013 1110 10/28/2013 408 1/16/2014 312 4/25/2014 220 7/17/2014 154 10/30/2014 127 M3,V-16 D5 10/18/2012 33.6 1/'29/2013 31.5 4/24/2013 33.2 7/'24/2013 || vias] 10/28/2013 1/14/2014 26.3 | 45.0 42.9 4/24/2014 40.7 7/16/2014 45.7 10/28/2014 38.9 PFBS 94.3 91.4 105 175 87.7 82.1 68.9 50.4 46.1 25.7 28.3 27.5 29.6 wo42.1 40.0 37.9 37.9 33.9 PW-06 D8 UL 10/23/2012 on 2/1/2013 7/'26/2013 82.2 26.4 ms | ne 85.0 82.5 3'7.5 42.9 Ta32lconeti Table 3-2 (cont'd) Summryof GrounPEdC AwnaaytaeDnra Summary of Groundwater PFC Analytical Data oc2a013-bOctoeber2r004 October 2012 - October 2014 Cottage Grove Sit, Cotage Grove, MN Cottage Grove Site, Cottage Grove, MN PFDA srr PFDoA res PFC Groundwater PIZHA PFHpA so fotx--sror--so--poeere Results (ppb, pg/L) PFHS PFNA PFOA PFOS PFPeA PFUnA | 3.38 <0.0250 93.3 33.3 20.9 3.95 1390 122 84.9 0.105 2.65 <0.0250 61.1 20.9 13.7 16.4 84.0 = 946 143 1020 145 72.7 0.625 23.9 2000 204 13.0 954 131 13.1 668 121 1.85 0.162 26.8 11.7 9.82 1.76 548 117 24.8 0.424 8.11 7.78 402 96.9 348 92.5 0.198 <0.0250 5.02 1.88 2.71 0.283 45.9 23.1 6.43 <0.0250 2.54 42.6 20.2 0.173 <0.0250 4.43 1.83 2.74 8.47 43.8 21.8 6.11 <0.0250 || 2.83 FT)3.95 5.52 39.9 20.1 wo | m| 73.9 382 91.0 53.1 0.334 <0.0250 6.50 3.30 4.49 0.535 85.7 51.9 6.72 <0.0250 5.46 4.58 98.3 75.8 57 42.6 0.497 <0.0250 13.4 4.52 4.90 pit4.74 4.16 0.598 172 37.9 woe 188 35.5 217 42.3 12.9 <0.0250 Page 5 or 6 SM_No1695955 CGMN All FC data Cmggtab-thru-2014-07-17( N-14)~ls; TblQ~-02-Data Ta~le~(ISO$4) 3M_MN01595993 33663300..00004444 win| Well ID veo| Location N~V- 14R D8 jg wDaotee[pePaFBrA 7/'24/2013 219 1/13/2014 295 4/23/2014 650 7/16/2014 671 10/29/2014 570 PW-10 EAST COVE 4/25/2013 6/19/2013~1) 7/24/2013 8/29/2013~v' 9/30/2013~b 10/28/2013 1/22/2014 4/25/2014 ECPZ-02R E. COVE 7/17/2014 10/30/2014 7/24/2013 ECPZ-03R E. COVE 7/24/2013 4.25 3.37 6.09 4.40 5.07 4.9 4.43 7.8{) 3.58 M~V-04R PLANT ---------- Notes: ppb - parts per bllhon 7/25/2013 3.72 rem dat. I~ ~ff, - nlicrou'qm a per liter "-" - not analyzed Sampled as part of extended pumping test program. Tatons Table 3-2 (cont'd) Summaryof GromPiCvAantieDarta Summary of Groundwater PFC Analytical Data caberneots October 2012 - October 2014 Cutan roe Sh oto ome, MN Cottage Grove Site, Cottage Grove, MN eee PFBS 10.9 17.5 18.2 29.6 38.1 vem Tru RnEeepee pre PFDA PFDoA PFC YH Groundwater Results (ppb, pg/L) PIZHA PFHpA PFHS PFNA PFOA PFOS PFPeA 6.23 91.7 13.2 12.3 139 249 2.10 <0.0250 197 26,1 20.0 1.72 543 353 278 20.1 16.6 426 158 353 82.6 FePFUnA <0.0250 0.594 <0.0250 <0.0250 0.153 0.540 0.703 0.261 O471 0.54 0.400 1.61 0.379 <0.0250 <0.0250 0.151 0.049 0.047 0.197 <0.0250 0.185 0.193 0.049 0.110 0.104 0.0777 0.939 0.205 <0.i}250 0.428 0.415 0.420 0.378 0.528 0.524 0.212 0.421 0.484 0.376 1.17 0.41 0.396 (I.4111 0.380 0.315 0.465 0.458 0.124 0.437 0.503 0.337 1.46 0.892 0.290 <0.0250 0.252 <0.0250 0.223 0.886 0.301 0.200 Page 6 or 6 awnotsasons CGMN All FC data Cr~s~tab-thru-2014-07-~7( SO-14) xls; TblQ~-02-Data Ta~les(ISO$4) 3M_MN01595994 33663300..00004455 Mann KendallTTaaTbblrleee3d3-33Test Summary PPMRFOOaSn`S,Gn,Pr-PKoFFueOOnnAdAdw,aa,ltPPleFFTrBBrAAeAn,m,PdlPyTFFieBcSsaStlSaaunnDmddatmPPaFRaHrIySS CotiageGrove Sie Groundwaler Analytical Cottage Grove Site Data Pros Pren Pres PFO8 PFOA PFBA PFB8 PFH8 TeDeduaannse || rooumss |_Tins oPnoms| Tiena | Poomns Well ID WNT | bcos[2005 tara] 15 | mewsos| 13 | weessng| 8 | | 11 MW-07 Mwaor | owz [sows veo] 13 | omens| 13 owcemog| 9 | ovens| 12 MW-101 was | ovr fame. somore] 5 | ns 0 | ws |e | ww | 10 MW-104 Location Background DI/D2 DI/D2 Trend Analysis Data Range Number of Data Points Trend 3/2005- 10/2014 13 Increasing 3/2005- 10/2014 13 Decreasing 9/2006- 10/2014 9 NS Number of Data Points 13 13 10 Trend Increasing Decreasing NS Number of Data Points 9 9 9 Trend NS Decreasing NS~ Number of Data Points 11 12 10 Number Toons Trend mown| 13 | baesng Increasing coming| 13 | orem Increasing owes] 0 | ss Decreasing of Data Points 13 13 10 Trend Increasing Decreasing NS MW-13 D9 3/2005- 10/2014 10 NB 10 NS 9 NS 10 N$ 10 NS MW-105 Pos PW-09 wwaos | MW-108 mwto | MW-110 wiz | MW-12 mut | MW-16 D9 orD9 we WWTP osD5 0sD5 osD5 9/2006- 10/2014 fumomvzo| 4/2013- 10/2014 faze. vozore| 9/2006- 10/2014 foes sooo] 9/2006 10/2014 aos. vais] 3/2005- 10/2014 aos. ase] 3/2005- 10/2014 9 NS 0 [nes | 9 Increasing 3 | ns 9 NS 10 | owen] 10 Decreasing 10 |oesesson'| 10 Decreasing1 0 | ne 10 NS 9 Decreasing 10 NS 9 5 [wesw] 7 | ws | 7 9 Increasing 7 NS 7 o wow ow |e 9 NS2 10 NS 9 10 | wcrsop| | wees'| 10 10 Increasing 9 Increasing1 10 10 | oocemng| 9 | oeceasng| 10 10 Decreasing 9 Decreasing 10 10 | comog| | ne | 10 10 Increasing 9 NS 10 Decreasing ws | NS ws | NS csseg | Increasing oecesmog| Decreasing icesseg | Increasing 9 NS 7 | ne 7 NS 0 | owns 10 Decreasing 10 | wang 10 Increasing 10 | oeceason 10 Decreasing 10 | tcmosny 10 Increasing owi0 | emcon [saves] 5 | we we |v ve Jv we |e orm MW-14R D8 7/2013- 10/2014 5 NS4 5 NS4 5 NB4 5 Increasing 5 NS PW-10 East Cove 4/2013- 10/2014 9 NB 9 NS 7 NS 7 NS 9 Decreasing RenataPet ioe aet Notes: Trend analysis performed using PFC analytical data for each well from March 2005 through October 2014. Results are for the Mann-Kendall test for trend at a significance level of 0.05 Imre NS = No statistically significant trend identified 1 Previous trend was not statistically significant 2 Previous trend was decreasing 3 Previous trend was increasing 4 Previous not applicable M_NO1595985 3M_MN01595995 33663300..00004466 `SummaT ry of Fore Wn ate and Sut race Watere SampleRevwls Table 3-4 Summary. of Pore Water and Surface Water Sample Results September/October 2006 through October 2014 3M Cottage Grove Site Approximate POREWATER 0tg/L; ppb) SURFACE WATER (~tg/L; ppb) LOCATION distance from AANNAALLVYTTEE| SeptO Sept/Oct 96 | JJuunn-1I11 | OcOtc-t1-122|AAvuggl-133 OuOtcti-14| SSeepput/OOucit 0066 |JJuunni-lll| OuOctt-i1?2 |AwAgugt-1d3 |OOtct-t14| shoreline LoIW w ToIwW Tw IW [Iw W w 1W TSSho',dnlow DDe~pp|CCoommpepnoistitee CCoommpopnoisittee CCoommppuotsiete CCoommppoonsiitte | PFFIA 1.58 67.6 1.67 30.3 46.13 :0.1(2,0 <0.050 *0.100 0.553 *0.025 "-0.0500 l~V-O9b 50 feet PFOA 0.5~q5 43.2 2.03 109 g.10 0.050 0.530 0.025 0.187 0.024 0.030 PFOS 0.114 45.6 1.27 2.84 2.95 <0:050 <0.050 <0.050 0.124 <0.0232 <0.0232 PFBA 5.01 2.32 4.65 8.10 6.71 1.24 NR <0.100 0.300 <0.025 <0.0500 1~/-09 100 feet PFOA 2.69 1.25 1.41 5.74 1.39 0.192 0.187 0.025 0.139 0.024 " 0.0240 PI~)S 1.09 0.415 0.958 0.822 0.383 0A62 0.183 <0.050 0.088 <0.0232 <0.0232 PFBA 0.112 83.3 11.8 0.057 2.94 NR 0.200 0.100 0.158 0.025 0.0500 l~V-09d 300 foot PFOA PFOS <0.050 ~3.050 48.5 0.533 0.355 0.141 <0.0240 0.0232 0.789 0.027 0.065 0.050 NR <0.050 <0.025 :0.050 0.064 0.043 <0.024 0.0232 <0.0240 0.0232 PFFIA NR 2.98 ~0.0500 30.7 15.4 0.405 0.477 ~0.100 0.204 ~0.025 0.0500 l~V-09f 500 feet PFOA 0.054 0.158 -~0.0240 2.83 0.524 <0.0~0 0.054 -~0.025 0.085 -~0.024 c0.0240 PFOS <:0.050 0.090 <0.0232 0.061 0.024 "-0:050 <0.050 <0.050 0.051 ~ 0.0232 -0.0232 PFBA 695 79.9 24.9 32.1 24.4 NR 0.540 <0.100 0.345 0.0415 0.0500 DV-14b 50 feet PFOA 436 467 123 221 102 0.195 0.158 ~-0.025 1.36 0.061 0.0750 PFOS 122 64.9 40.9 25.5 37. I 0.063 0.058 <:0.050 0.780 ~ 0.0232 -0.0232 PFBA 281 l~V-14 100 feet PFOA 300 38.8 205 142 529 192 2.16 0.414 NR :0.100 0.0618 :0.025 0.0500 517 4.24 0.053 0.057 ~0.025 ~0.024 ~0.024 ~0.0240 PFOS 12 4 28.3 I 8.3 4.22 0.251 Nil <0.050 ~ 0.050 -40.0232 ~ 0.0232 ~:0.0232 W-14d 300 feet PFBA PFOA 0.282 <0.050 0.318 0.054 0.7,17 0.257 1.1'1 0.115 0.85,1 0.216 0.329 -0.100 0.318 <0.100 <0.100 --0.025 <0.050 ,--0.024 <0.025 --0.024 <0.0500 -0.0240 PFOS </I.050 0.089 11.947 0.032 0.095 <0.050 <0.050 <0.050 <0.0232 <0.0232 <0.0232 PFBA o. 178 33.3 78.4 39.1 76.1 ~0.0~0 <0.050 <0.100 *0.050 <0.025 <0.0500 IW-14I 500 feet PFOA <0.050 0.813 59.3 0.926 4.i9 "0.050 <0.050 -'0.025 "-0.024 -'0.024 -0.0240 PFOS <o.025 0.086 1.23 0.05 0.048 <0.050 <0.050 <0.050 <0.0232 <0.0232 <0.0232 ppb - parts per billioq I~g/L- micrograms per liter IW- Interslilial Water (Pore walor) NR - Not repoded due to quality control issues NS Nr~t sat ip ed Note In September/October 2006 t~,~9 sulface water samples were collected at discrete ceplh inlen/als at each location (i e, shallow and deep, 0 2 and 0 8 of the tolal depth of the water column) In June 2011, October 2012, August 2013, and October 2014 one composite ssmple was collected a[ each Iosa:ion, composited from the same deplh illelvals snors 3M_MN01595996 33663300..00004477 er oie r Table 3-4 (cont'd) Summary of Pore Wmer and Surface Water Sample Results T a e September/October 2006 through October 2014 3M Cottage Grove Site Approviemic| Approximate fonsSmo ma oe Pe] er] LOCATION distance from ANALYTE Jhordine Loo Ton ow Tow ow Shon Dep[ComposeCompute Composit'Compute] shoreline Sept/Out (;6 IW [om oe EeIePe ea) l~V-19b R = S E mt ee e a aa b e eE e e IW-19 50 t~et 100 tieet PFFIA PFOA P1TOS PFBA PFOA PFOS PFBA NR 118.5 5a I 866 289 NR 1.40 POREWATER (~g/L; ppb) Jun-I1 Oct-12 Aug-13 IW IW IW 198 154 157 34.4 10.5 6.96 43 2 95 6 40 4 i07 112 18.3 257 8.43 1.63 311.3 81. I 0.r~91 0.143 4.07 8.00 Oct-14 1W 69.2 147 31 9 62.6 9.15 92.3 13.4 SURFACE WATER (~g/L; ppb) Sept/Oct 06 Jun-ll Oct-12 Aug-13 Sh',dlow Deep Composite Composite Composite 2.81 1.96 :0.100 0.223 0.115 0.154 0 127 0.129 ~ 0Rq -~0.025 <:0 050 0.557 0 100 0.434 0 412 NR NR <:0.100 0.089 0.037 0.119 0.126 <0.025 0.041 0.108 0.105 {).()97 <0.050 -0.0232 < 0.0232 0.095 ~.117 <0.100 0.069 <0.025 Oct-14 Composite 0.068 0.203 0 137 :0.0500 0.091 -0.0232 0.0500 l~V-19d o[rTRT a Tb erL Ab Et A Pb PLe e Ee le ha ] IW-19f 300 l~ot 500 l~et PFOA PFOS PFBA PFOA PFOS PFBA 0,184 0.0S~ 118 6.84 i 7~ N~ 0.097 0. I 18 0.57 0.0250 <0 0500 56 0.206 0.246 141 15.3 I 26 1.47 0.206 0.207 47.1 185 10 9 37.2 0.114 <0.0232 51.5 231 0 913 53.9 0.050 <0.050 0.245 0.050 <0 050 i'IS 0.050 <0.050 ~3.516 NR <0 050 NS 0.025 <0.050 <0.100 0.025 <0 050 12.5 <0.024 <0.0232 0.051 0.028 <0 0232 0.686 0.024 <0.0232 <0.025 0.024 <0 0232 0.897 0.0240 :O.0232 ~0.0500 0.0240 ~:l~ 0232 0.553 IW-25b l~rV-25 orI~V 25d 50 t~et 100 li:et 300 IL'et PFOA PIOS TT 0 PFBA re PFOA PFOS ES J SC PFBA PFOA Shenae PFOS Lh ie Cb PFBA NS NS 23 1 129 206 NS 97.3 595 13.6 110 82.4 25 16.6 0.13 ~ 1.2 2.41 34.7 74.7 0.916 15.9 2.04 19.1 169 86 35.5 9.98 3.28 38.6 19.5 0.141 374 1300 58.9 23.6 16.2 10.8 36.7 0.094 r,JS ixIS NT~ 0.163 0.095 ]'IS r'JS ~,IS NS NS NI( ~J.146 ~).102 ixS NS NS 1.01 1.10 6.25 0.583 0.586 :0.100 <0.025 0.050 0.202 0.151 0.819 0.575 0.422 0.389 0.335 0.236 0.328 0.122 3.64 1.26 0.311 0.043 <0.024 0.0232 0.173 0.148 0.673 0.1~1 0.127 ~ 0.0500 0.045 "0.0232 IW-25f 500 t~et Dovefos Psa TomTow PFOA NS PFOS NS 1.25 2.64 0.482 0.201 5.18 2.18 ow 10.0 6.65 ow ToeTam Tour 1svunsTuo INS i",S <0.025 0.163 <0.024 <0.0240 ~,IS ~,-S 0.050 0.087 0.0232 0.0232 ppb - parts per billion ug/L- micrograms per liter os IW leterstitial Water (Pore water) NR - Not repraled due to qualfly control issues N$ - Not samp ed Note ~n~ep~ember/Q~..1~ber2~6tw~su~ac~.atersamp~eswerec~e~1eda~discretecep~hiIIie~/a~sateach~ca~i~n(i.e.'sha~wanddeep' 0.2and08ofthetulaldepthofthewatercolumn) 2013, and October 2014 one composite sample was collected a~ each Icoa:ion, composited from the same depth intervals In June 2011, Oclober2012, Augubt svar 3M_MN01595997 33663300..00004488 44.. FFIINNDDIINNGGSS The Groundwater, Pore Water and Surface Water PFC Sampling Plan (WESTON, 2012) was developed to collect analytical data that could be used to assess long-term groundwater and surface water conditions in the area within, and surrounding, the Cottage GGrroovvee SSiittee.. GGrroouunnddwwaatteerr eelleevvaattiioonn ddaattaa aarree aallssoo ccoolllleecctteedd ttoo ddeetteerrmmiinnee tthhee lloonngg--tteerrmm eeffffeecctt of the continuous pumping of the groundwater remediation system on water levels at the Site. In addition, pore water and surface water samples have been collected in the Mississippi River to determine whether any trends are apparent in PFC concentrations. The baseline groundwater, pore water, and surface water sampling event was performed in October 2012. The results and findings of this sampling were provided to the MPCA by 33MM iinn JJuunnee 22001133 ((WWEESSTTOONN,, 22001133)).. The following findings are summarized for groundwater analytical data, surface water and pore wwaatteerr annaallyyttiicaall ddaattaa,, and hyddrroggeeoollooggiic daatta coolllectteedd in 2014 aat tthhee SSiittee.. 4.1 GROUNDWATER ANALYTICAL DATA PFBA, PFOA, PFBS and PFHS are detected at low concentrations in background (upgradient) monitoring well MW-07. 3M is not aware of the source for PFCs in groundwwaatteerr aatt this uppggrraaddiieenntt llooccaattiioonn.. PFC concentrations are highest in groundwater samples collected from monitoring wweellllss iinn tthhee ffoorrmmeerr DDI1//DD22 ((MMWW-1-10011,, MMWW-1-10022,, MMWW--110033 aanndd MMWW-1-10044)) aanndd DDS5 ((MMWW--1122)) AArreeaass.. + TThhee MMaannnn--KKeennddaallll ssttaattiissttiiccaall ttrreenndd rreessuullttss iinnddiiccaatteedd aa ssttaattiissttiiccaallllyy ssiiggnniiffiiccaanntt increasing or decreasing trend at the following locations: o DDeeccrreeaassiinngg:: PFOS in monitoring wells MW-101, MW-110 and MW-12; PFOA in monitoring wells MW-101, MW-105 and MW-12; PFBA in monitoring wells MW-101 and MW-12; PFBS in monitoring wells MW-104, MW-105 and MW-12; Z:~FOL DE R-G O-9\3m-c~ttage~rove\WE~TON-Reports~2014~Q-AnnuaI-G~/~CGMN_2014_Ann ual_Report.docx 4-1 33663300..00004499 3M MN01595998  PFHS in monitoring wells MW-101, MW-108, MW-12 and production wells PW-10. Increasing: PFOS in monitoring wells MW-07 and production well PW-09. PFOA production well PW-09 and monitoring wells MW-07, MW110 and MW-16. PFBA in monitoring well MW-110. PFBS in monitoring wells MW-07, MW-101, MW-110, MW-16 and MW-14R, and production wells PW-09 and PW-10; PFHS in production well PW-10 and monitoring wells MW-07, MW-110 and MW-16. 44..22 SSUURRFFAACCEE W WAATTEERR// PPOORREE WWAATTEERR AANNAALLYYTTIICCAALL DDAATTAA * PPFFCC ccoonncceennttrraattiioonnss iinn ppoorree wwaatteerr aarree hhiigghheerr tthhaann ssuurrffaaccee wwaatteerr PPFFCC concentrations. Pore water PFC concentrations fluctuate with no discernible trend at this time. Surface water PFC concentrations were primarily below laboratory quantitation limits except for a few locations close to the shore at transects IW-19 and FW-25. At the maj ority of pore water sampling locations, PFBA was detected at the highest ccoonncceennttrraattiioonn ooftf thhee PPFFCC ccoommppoouunnddss.. 4.3 SITE HYDROGEOLOGIC CONDITIONS The direction of groundwater flow is from north to south towards the Mississippi River. The extended pilot pump test was completed in February 2014. Production wells PW-09 and PW-10 continued to operate at approximately 300 gpm. A report summarizing the results of the extended pilot pump test was provided to MPCA in March 2015 under separate cover. Groundwater levels in monitoring wells closest to the Mississippi River showed lleessss fflluuccttuuaattiioonn iinn rreessppoonnssee ttoo rreecchhaarrggee ffrroomm tthhee sspprriinngg mmeelltt tthhaann tthhoossee mmoonniittoorriinngg wells more distant from the river. FEZ:~FOL DE R-G O-9\3m-cottage~qrove\WE-~TON-Reports~2(] 14~Q-AnnuaI-GV~CGMN_2014_Ann ual_Report.docx 4-2 33663300..00005500 3M MN01595999 55.. FFUUTTUURREE CCOOUURRSSEE OOFF AACCTTIIOONN The analytical and hydraulic data resuling from the monioring of Site groundwater cTohneditainoanlsytiwcialll acnodnthinyuderautloicbedautasedrestuoltiensgtabflriosmh nthoermamlonciotoncrienngtraotfioSnitevargiraotuinondswaatnedr Hciosntdoritiiconsranwgeilsl, coasnstiensuse ptoossbiebleusetdrentods in the establish cnoonrcmenatlractoinocnesntroaftiocnertvaairniatiPoFnCss inand historic ranges, assess possible trends in the concentrations of certain PFCs in g`grroouunnddwwaatteerr,, aanndd ttoo aasssseessss tthhee iimmppaaccttoofflolonngg--tteerrmm ppuummppiinngg ooff tthhee SSiittee pprroodduuccttiioonn wweellllss on groundwater levels. Afte the groundwater interception system is expanded described in Soenctgiroonun3d.2w,acteornfleivrmealst.ioAnfttehratthgergoruonudnwdawteartecraipnttuerrceeipstiboeninsgysmteamintisaienxepdanovdeerd tdheescrreiqbueidreind aSreecatsionwil3l.2b,ecoprnofivrimdeadtioinn tthhaet agnrnouuanldwreaptoertrs.capItnuraecciosrbdeainncge mwiatihntatihneedSaomvpelrinthgePrleaqnu,irtehde areas will be provided in the annual reports. In accordance with the Sampling Plan, the ffoolllloowwiinngg aaccttiivviittiieess wwiillll bbee ppeerrffoorrmmeedd iinn tthhee aapppprrooxxiimmaattee ttiimmee--ffrraammeess nnootteedd:: Groundwater Monitoring Groundwater Monitoring + Quarterly groundwater sampling was completed in January 2015. The annual sQaumaprlteirnlgy egvreonutndiswastcehredsualmedplifnogr wAparsilco2m01p5letaendd inaddJiatniounaarly q2u0ar1t5e.rlTy hesamapnlniunagl esvaemnptslinwgillevbeenpterisfosrcmheeddiunleAdugfuosrtAanpdrilNo2v0e1m5bearnd201a5d.ditional quarterly sampling events will be performed in August and November 2015. + Groundwater elevation data willbe collected on aquarterly basis at a mirimum. Groundwater elevation data will be collected on a quarterly basis at a minimum. Future Submittals to MPCA presenting a summary of the groundwater analytical data collected at th Sit n the * TThhee 22001155 aannnnuuaall ggrroouunnddwwaatteerr mmoonniittoorriinngg rreeppoorrtt wwiillll bbee ssuubbmmiitttteedd ttoo MMPPCCAA presenting a summary of the groundwater analytical data collected at the Site in the ffiirrsstt qquuaarrtteerrooff 22001166.. ls Z:~FOL DE R-G O-9\3m-c~ttage~rove\WE~TON-Reports~2014~Q-AnnuaI-G~/~CGMN_2014_Ann ual_Report.docx 5-1 33663300..00005511 W_MNO1556000 3M MN01596000 66.. RREEFFEERREENNCCEESS GGililbbeertr,t, RR.OO.., 11998877.. SSttaattiissttiiccaall MMeetthhooddssffoorr EEnmv~iirroonnmmeennttaall PPoollhl~utiioonn MMoonnititoorriinngg.. NNeeww York, van Nostrand Reinhold. York, van Nostrand Reinhold. USEPA, 2009. Suaisical Anais of Groundwater Monitoring Data ai RCRA Facilities USEPA, 2009. Statistical Analysis of Grotmdwater Mortitoring Data at RCRA Facifities UUnniiffiieedd GGuuiiddaannccee.. ~U.SS.. EEnnvviirroonnmmeennttaall PPrrootteeccttiioonn AAggeennccyy., ~ EEPPAA'/5S3300/RR0/099--0O0077.. WWaasshhiinnggitoonn., DD..CC.., M Maarrcchh 22000099.. WESTON (Weston Solutions, Inc). 2008. Feasibility Study. Prepared by Weston WESTON (Weston Solutions, Inc.). 2008. Feasibifi(y Study. Prepared by Weston SSoolluuttiioonnss,, IInncc..,ffoorrtthhee 33MM CCoommpapnayn.y. MMaarrcchh 22000088.. WESTON (Weston Solutions, Inc) 2009. Remedial Design Response Action (RRA) WESTON (Weston Solutions, Inc.). 2009. Remedial Design/Response Aetimt (RD/2ZA) PPllaann.. PPrreeppaarreedd bbyy W Weessttoonn SSoolluuttiioonnss,, IInncc..,, ffoorr tthhee 33MM CCoommpapnanyy.. M Maarrcchh 22000088.. WESTON (Weston Solutions, Inc.). 2012. Grownbrater. Pore Water, and Surface Water WESTON (Weston Solutions, Inc.). 2012. Groundwater, Pore Water, attd Surface Water SSaammpplliinngg PPllaann ffoorr PPeertfflluuoorroocchheemmiiccaallss ((PPFFCCs)s.), 33MM CCoottttaaggee GGrroovvee SSiittee.. PPrreeppaarreedd bbyy W Weessttoonn SSoolluuttiioonnss,, IInncc..., ffoorr tthhee 33MM CCoommpapnanyy.. AApprriill 22001122. WESTON (Weston Solutions, Inc.). 2013. Groundwater Extraction Weil Eviended Pump. WESTON (Weston Solutions, Inc.). 2013. Grounchater Extraction Well ExtendedP~mp TTeesstt CCoonncceeppttuuaall WWoorrkk PPllaann,, 33MMCoCtotttaaggee GGrroovvee SSiitte.. PPrreeppaarreedd bbyy W Weessttoonn SSoolluuttiioonnss,, IInncc.., foforrtthhee 33MMCComompapnayny.. JJaannuuaarryy22001133. W WEESSTTOONN ((W Weessttoonn SSoolluuttiioonnss,, IInncc).).. 22001133.. BBaasscelfinnee M Moonnititoorriinngg RReeppoorrtt ffoorr PPeertfflluuoorroocchheemmiiccaallss ((PPFFCCss)) iinn GGrroouunndaw~a,'taeterr,, PPoorree WWaatteerr,, aanndd SSuurrffaaccee WWaatteerr,, 33MM CCoottttaaggee GGrroovvee SSiittee.. PPrreeppaarreedd bbyy W Weessttoonn SSoolluuttiioonnss,, IInncc.,, ffoorr tthhee 33MM CCoommppaannyy.. JJuunnee 22001133.. W WEESSTTOONN ((WWeessttoonn SSoolluuttiioonnss,, IInncc.).).. 22001155.. EExxtteennddeedd GGrroouunnddwwaateterr PPiilloott PPuummpp TTeesstt aanndd DDeessiiggnn ooff GGrroouunnddwwaatteerr RReeccoovveerryy SSyysstteemm,, 33MM CCoottttaaggee GGrroovvee SSiittee.. PPrreeppaarreedd bbyy W Weessttoonn SSoolluuttiioonnss,, IInncc..,ffoorrtthhee 33MM CCoommpapnayn.y. MMaarrcchh 22001155.. mrt mpi Z:~FOL DE R-G O-9\3m-c~tta9e~rove\WE~TON-Reports~2014~Q-AnnuaI-G~/~CGMN_2014_Ann ual_Rep~rt.docx 6-1 33663300..00005522 33MM_MMNNo011559966000011 SUMMARY OF WELAALTTTTCAAOCNCHSHMTMREEUNNCTTTAAION INFORMATION SUMMARY OF WELL CONSTRUCTION INFORMATION 33663300~.00005533 3M_MNO1596002 3M MN01596002 Summary of Well Information Cottage Grove Site, Cottage Grove, MN et rb eCrees Well ID Well T~/p~ A SL Li lima Production/Extraction Wells IVDH Unique Well Number TOC Elevation (ft MSL) Depth to Top of Screen/ Open Hole* (ft BGS) Depth to Bottom of Screen/ Bottom of Hole* (ft BG$) Total Boring Depth* (ft BGS) Well Diameter* Unit Monitored Northing Easting (UTM meters) (UTM meters) PW-01 Production 231867 804.35 NA reductin| oes | 148 a 205 205 14 2 a Ey NA Grow 4959573 ET 506968 SsBoEmon=eonnoon n[ER oSmmmoimioan ~W-08 PW.09 (EW01} ~:~6 i~6~i PRL le ~nitor Well~ LL ~-01 Em ~-02 Production Extraction ~nitoring ~nitoring .............~............. NA 767283 . . . . . . . . . . . . .~8~. . . . . . . . . . . . . 233567 233568 ...................~.................... .......................~........................ ...............~............... ............~.............................................~................................. 806.93 NA NA NA NA NA 1 781.23 =[ . . . . . . . . . . . . . . . . . . 164 . .~. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . i224 ~6 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Bon 225 12 ~=~5............... ............. . . . . . . . . . . . . . = == Seis Glaciofluvial sedimen:s 8i~i~i~i ~8=i~ ~ 822.92 NA 805.92 NA 200 200 6 192 192 6 Cj / Csl Cj / Csl 4960087 En 4959117 4961188 4960019 ......... 506742 Sn 507776 ~.......... 506875 ~07126 cSE SLE eoETEiE= Emi ZmEnm o LosEE m = LEoomCE bmooEnb: fpoRs2 ooonn a2 a EEs md esoeoae a an0== EEEmE=maoBa=sem rvivv-10 ToBm Eoo r oFn oF a =o: rvlw-12 TPmaEloRinamEEEIEEEEREEEeeeeTmE eT et n BSR eEE ~-14R PPooEmmmoomaonomoosnoowEo ofooamoasmmm oooon on r~w.17 Monitoring Monitoring 2335~4 233951 786.28 781.~3 ~nitoring 797616 703.~0 Monitoring 570322 785.16 198 122 59.1 92 ECDBBEDmE oEfE aoEm2 aEr BwE @ oe Sop Drm eosaminmm BaEoeUbOoE rVNV-102 Monitoring 680686 783.25 86 237 141 69.1 112 96 237 8 Cj / Csl 4959320 50741~ 141 ~ Glaciofluvial sedi ...... 4959193 ~07137 70 2 Glaciofluvial sedi ..... 4959174 506801 112 4 Cj 4959671 506505 96 2 Glaciofluvial eedimen:s 4959171 508072 EeBELTE rEEoEmEEmpf mmmDSmE im ooafTe SE ATsotoeooSomZotmnnIiDorTooe.oEnaTe EE5f T w fSo8 on s oov o D 0ES RaaE mmoaaooaaeaammmms mmistesmEnnnmmmoiaaoEota= mbnnnnoaoiimnn ECPZ-02(ABD)Monitoring Eizo son ro: v0 omen mom ~CP~-02R Monitoring FUE ma Bn 1 seem oe oo EGPZ-03R ~nitorin~ 747073 780910 780911 691.75 69331 69~.~0 33 35 30.2 43 45 40.2 46.5 47 42 2 Glaciofluvial sedi ..... 4958935 508452 2 Glaciofluvial sedi ..... 4958934 508452 2 Glaciofluvial sedimen:s 4958932 ~08517 i~:~2~. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .28~8~. . . . . . . . . . . . . .................~:2.................. .....................8~:28..................... .................88................ .............. ~.............. .......... ETrEem Notes: * - Inbrmation oblained from well completion reporls (ABD) - Well Abandoned, THEEEE Opo- One0ta Delomite q - Jordan Sandstone Cd - Sl. Lawrence Formation fl BGS- Feet below ground surface, Cf- Francenia Formation fl MSL- Feet above mean sea lev~. NA - Not Available 33663300..00005544 2014-02-CGMN-Well-lnfo Is; CGMN-WelIIr#o (RPT) 3M MN01596003 AATTTTAACCHHMMEENNTT BB PPOORREESW WEAPATTTEEEMRRBAAENNRDD/OSSCUUTRROFFBAAECCREE2W W0A1A4TTSEEARRMSSPAALMMIPNPLGLIINENGVGESSNHHTEEEETTSS SEPTEMBER/OCTOBER 2014 SAMPLING EVENT 33663300~.00005555 3M_MNO1596004 3M MN01596004 como -- rn Cottage Grove, MN PORE SAMPLE DATA SHEET Project No.: 02181-002-179 rll ol rm Drainage System: E TTo ee ---- GPS Latitude: 44.784685 Mississippi River County: Washington GPS Longitude: -92.909316 State: MN Location Description: IW-09 transect line Water Conditions: ( ) Low Turbidity I Water Conditions: re Weather Conditions: l-Oct Temp. 50 F ET Depth to Sediment: 13.7' (X) Moderate Turbidity ( ) High Turbidity ( ) Calm (X) Choppy ( ) Visible Current a ( ) Partly Sunny (} Cloudy (X) ftbws Sediment Bottom: mm Rain ( X ) Windy ( ) Firm (X) 5oft Water Sample Method: ( X ) Peristaltic Pump wsmpeom1] Water Sample Data supleoepmimsc |_ ompouezresassn| Sample Depth (ftbws1 Composite (2.74' and 9.96') Pownmeguonsop rgaen rmntel| Flow Rate (gallons per minute] 0.1 9pm ET Sample Date 10/01/2014 Sompetind we Sample Time 14:10 iscirac m | oy sso |owm ee o | y emo|r oml| pH / SC l "r (c) / DO (mg/L)/ORP 8.33 349 16.03 6.78 28 sper]comswmammorwon| Sample ID CG MN-SW-MRIW09-0-141001 owes comvewmamsoswen| Duplicate ID CGMN-SW-MRIW09-DB-141001 resmpegonoed 1] Field matrix spike (1.0 ng/mL1 ------ COMMENTS: Rinse Blank CGMN~W-MRIW09-RB-01-141001 EFoncmwaren Well Diameter (in) Depth to Sediment (ftbws) Em = Depth to Top of Screen (ftbws) -- Depth to Bottom of Screen (ftbws) 1 13.7 14.2 14.7 Water column 14.0' Well Volume (gal) 1.26' me 7 Purge Start (time) 14:29 ee -- Purge Stop (time) 14:37 a Volume Purged (gal) 1.2 gallons Tr ni TE Well Purged Dry? (X) Yes ( ) No fsa Sample Method: (X) Peristaltic Pump sponte umewn | Sample Depth Interval (ftbws] spond owas | Sample Date sper we | Sample Time miscisr m c | e aw o|owm e g | y emo|nas]| pH ! SC i T (C) / DO (rag/L)/ORP spon commamwmerin| Sample ID 8.32 299 Water Sample Data 14.20' to 14.70' 10/02/2014 09:05 15.92 C~MN-IW-MRIW09-0-141002 6.73 51.5 Fistmots sp (10x 1601 Duplicate ID Field matrix spike (10 or 100 ng/mL] CG MN-IW-MRIW09-DB-141002 CG MN-IW-M RIW09-FMS-141002 COMMENTS: Sampling- DTR: 1.10', DTW: 13:20; Not much water in point; Gray clay 33663300..00005566 3M MN01596005 como -- rn Cottage Grove, MN PORE SAMPLE DATA SHEET Project No.: 02181-002-179 rll HN Drainage System: Q TEE en os GPS Latitude: 44.784018 Mississippi River County: Washington GPS Longitude: -92.909633 State: MN Location Description: IW-09 transect line Water Conditions: ( ) Low Turbidity (X) Moderate Turbidity ( ) High Turbidity Ty a Water Conditions: ( ) Calm (X) Choppy ( ) Visible Current pe TL Weather Conditions: l-Oct Temp. 50 F ( ) Partly Sunny (X) Cloudy (X) Rain ( X ) Windy ET a mm Depth to Sediment: 11.7 ftbws Sediment Bottom: ( ) Firm (X) Soft Water Sample Method: ( X ) Peristaltic Pump supleoepmims|_ wscom mposmep simasse y om1|] Sample Depth (ftbws1 Pownmeguonsop sgee m rmntel| Flow Rate (gallons per minute] ET Sample Date Sompetind _ wes Sample Time iscircoyoomoyor ase | sw | we | we |ow | pH / SC l "r (c) / DO (mg/L)/ORP sompeo| comswwmwessorwor| Sample ID owtemerf comsmmmmososuen| Duplicate ID Feamatespe(1 Field matrix spike (1.0 ng/mL1 moose. Rinsate Sample ID 8.35 Water Sample Data Composite (2.34 and 9.36) 0.1 9pm 10/01/2014 13:25 328 15.6 7.16 57 CG MN-SW-MRIW09d-0-141001 CGM N-SW-MRIW09d-DB-141001 CG MN-SW-MRIW09d-FMS-141001 COMMENTS: DTR: 2.40'; DTW: 2.42'; Gray silty sand EfEoncwaren Well Diameter (in) Te Depth to Sediment (ftbws) -- Depth to Top of Screen (ftbws) es, Depth to Bottom of Screen (ftbws) moWell Volume (gal) fot Purge Start (time) mmm Purge Stop (time) -- Volume Purged (gal) TE TE Well Purged Dry? ( ) Yes (X) No psa Sample Method: (X) Peristaltic Pump 11.7' =H13.5' 14.0' --1.22 qallons =13:40 13:52 RE 1.80 gallons sopeowieatton meme | Sample Depth Interval (ftbws] spond owas | Sample Date spt we | Sample Time siseir 7sc|eeo n o | m weo|yo ww n |e am]| pH ! SC i T (C) / DO (rag/L)/ORP 7.5 377 Water Sample Data 13.5'-14.0' 10/01/2014 13:55 15.63 2.07 -112 Sample ID i Duplicate ID Fospa e om o ongmy Field matrix spike (10 or 100 ng/mL] Resa] Rinsate Sample ID COMMENTS: Gray silty sand CG MN-IW-M RIW09d-0-141001 cm-- CGMN-IW-M RIW09d-DB-141001 wows Not Applicable wompete Not Applicable | | | 33663300..00005577 3M MN01596006 como -- re cnn Cottage Grove, MN PORE SAMPLE DATA SHEET Project No.: 02181-002-179 rll AE Drainage System: i TTr ee a GPS Latitude: 44.784765 Mississippi River County: Washington GPS Longitude: -92.909144 State: MN Location Description: IW-09 Water Conditions: e mre Weather Conditions: Depth to Sediment: Ty transect line ( ) Low Turbidity Water Conditions: l-Oct Temp. 50 F 6.5' a his Kifer (X) Moderate Turbidity ( ) High Turbidity ( ) Calm (X) Choppy ( ) Visible Current ( ) Partly Sunny (X) Cloudy (X) Rain ( X ftbws Sediment Bottom: ( ) Firm ) Windy (X) Soft Water Sample Method: ( X ) Peristaltic Pump supleoepmimsw |_ e composmes romassy w| Sample Depth (ftbws1 Pownmeguonsop sgee m rmntel| Flow Rate (gallons per minute] J Sample Date Somperind we | Sample Time siscir axc|csi e | o. om| yo es r |s en]| pH / SC l "r (c) / DO (mg/L)/ORP sen]comnswwwwemowe| Sample ID owtemef comsmmmmomoswon| Duplicate ID resmpegonoed 1] Field matrix spike (1.0 ng/mL1 8.35 Water Sample Data Composite (1.70 and 6.80) 0.1 9pm 10/01/2014 14:50 346 16 6.9 6.1 CG MN-SW-MRIW09b-0-141001 CG MN-SW-MRIW09b-DB-141001 COMMENTS: [porewaren| EEWell Diameter (in) 1 fa = Depth to Sediment (ftbws) 8.50' --| = Depth to Top of Screen (ftbws) 11.0' eS Depth to Bottom of Screen (ftbws) 11.5' me -- Well Volume (gal) mm mm Purge Start (time) 1.03 qallons 16:02 mmm a Purge Stop (time) 15:09 a Volume Purged (gal) 1.05 gallons SE ni TE Well Purged Dry? (X) Yes ( ) No fsa Sample Method: (X) Peristaltic Pump SaDeem n tae na Sample Depth Interval (ftbws] spond owas | Sample Date spt wa | Sample Time sseir7c s e | oaw o|mwo w y | o ewn |e0]| pH ! SC i T (C) / DO (rag/L)/ORP 7.9 329 Water Sample Data 11.0'-11.5' 10/01/2014 09:25 15.88 6.36 -30 Sample ID CG MN-IW-M RIW09b-0-141002 i cm-- | Duplicate ID CGMN-IW-M RIW09b-DB-141002 Foam pegooongm | Field matrix spike (10 or 100 ng/mL] wees] Rinsate Sample ID -- -- COMMENTS: Gray clay, soft; DTR: 4.55'; DTW: 4.20' 33663300..00005588 3M MN01596007 como -- rn Cottage Grove, MN PORE SAMPLE DATA SHEET Project No.: 02181-002-179 rl A Drainage System: i TT ee en GPS Latitude: 44.783686 Mississippi River County: Washington GPS Longitude: -92.909899 State: MN Location Description: IW-09 transect line Water Conditions: ( ) Low Turbidity TR Water Conditions: em Weather Conditions: Temp. 50 F ET Depth to Sediment: 4.S0' Ty (X) Moderate Turbidity ( ) Calm (X) Choppy ( ) High Turbidity ( ) Visible Current a me ( ) Partly Sunny (X) Cloudy (X) Rain ( X ) Windy ftbws Sediment Bottom: ( ) Firm (X) Soft Water Sample Method: ( X ) Peristaltic Pump supleoepmimsw |_ e composmeps sosazen w| Sample Depth (ftbws1 Pownmeguonsop sgee m rmntel| Flow Rate (gallons per minute] ET Sample Date Sompetind _ ee Sample Time scirccioomyors] au | we | we | es | a| pH / SC l "r (c) / DO (mg/L)/ORP sampeo| comewwmomowen| Sample ID owtemer] comswwmmowosrwen| Duplicate ID resmpegonoed 1] Field matrix spike (1.0 ng/mL1 cer -- COMMENTS: 8.34 Water Sample Data Composite (0.98 and 3.92) 0.1 9pm 10/01/2014 12:65 359 15.65 5.3 -25 CG MN-SW-MRIW09f-0-141001 CG MN-SW-MRIW09f-DB-141001 [porewaren| Em Well Diameter (in) freDepth to Sediment (ftbws) re, Depth to Top of Screen (ftbws) a Depth to Bottom ot Screen (ftbws) Fa Well Volume (gal) FePurge Start (time) mm Purge Stop (time) mm Volume Purged (gal) E fsT a Well Purged Dry? (X) Yes ( ) No = =TE 0.405 13:07 =13:11 =0.6 1 4.90' 5.85' 6.35' Sample Method: (X) Peristaltic Pump smpogorm[ atton wweeswwepesonn || Sample Depth Interval (ftbws} Water Sample Data 6.86'-6.36' spool eww | Sample Date 10/02/2014 sper wes | Sample Time 08:55 suscirsc w c |iao n o |mwo e u |yao e | newm ]| pH / SC i T (C) / DO (mg/L)/ORP 8.38 277 14.69 8.5 37 samen]commumwoerw| Sample ID CG MN-IW-MRIW09f-0-141002 owen commamwmosr| Duplicate ID CGMN-IW-MRIW09f-DB-141002 fo Field matrix spike (10 or 100 ng/mL] mel ---- COMMENTS: Gray Clay; DTR: 4.15; DTW: 5.50 33663300..00005599 3M MN01596008 como -- re cnn Cottage Grove, MN PORE SAMPLE DATA SHEET Project No.: 02181-002-179 rm AE Drainage System: i TT ee en GPS Latitude: 44.783699 Mississippi River County: Washington GPS Longitude: -92.904236 State: MN Location Description: IW-14 transect line Water Conditions: ( ) Low Turbidity (X) Moderate Turbidity ( ) High Turbidity I SE Water Conditions: ( ) Calm (X) Choppy ( ) Visible Current en er Weather Conditions: Temp. 50 F ( )Sunny (X) Cloudy ( )Rain ( X ) Windy ee Depth to Sediment: mr Water Sample Method: 17.5 ( X ) Peristaltic Pump ftbws Sediment Bottom: ( ) Firm ( ) Soft supleoepmiums|__ comwpeoessepwpmsemoornny | Sample Depth (ftbws1 Pownmeguonsop sgee m rmntel| Flow Rate (gallons per minute] sopeond_ oseenwns | Sample Date Songer ee | Sample Time wiscisr u c | c wmi|ovo e m | y teo |r=]| pH / SC l "r (c) / DO (mg/L)/ORP sper]comswwewenowoms| Sample ID owtemef comvewmawmosuesn| Duplicate ID Fesmaphoeom comonamwicrwsoso| Field matrix spike (1.0 ng/mL1 cer -- COMMENTS: 8.44 Water Sample Data Composite (3.5' and 14') 0.1 9pm 0913012014 16:10 353 17.65 7.59 95 CG MN-SW-MRIW014-0-140930 CGMN-SW-MRIW14-DB-140930 CGMN-SW-MRIW14-FMS-140930 E[pormewaren| Well Diameter (in) Depth to Sediment (ftbws) -- Depth to Top of Screen (ftbws) r-- = Depth to Bottom of Screen (ftbws) 1 17.6 19.3' 19.8' Water column Well Volume (gal) mm a Purge Start (time) a Purge Stop (time) mn 5 Volume Purged (gal) PE TE Well Purged Dry? ( ) Yes (X) No pees Sample Method: (X) Peristaltic Pump 15.46 1.39 12:06 12:19 1.95 sponte wsaes | Sample Depth Interval (ftbws] spond owas | Sample Date sper we | Sample Time miscir 7sc|eeo w o | m weo|yo 1a n|ear]| pH ! 8C i T (C) / DO (rag/L)/ORP 7.9 sper commamwsion| Sample ID Water Sample Data 19.3'-19.8' 10/01/2014 633 12:20 14.86 7.2 -27 CGMN-IW-MRIWI 4-0-141001 mel Foam spegooongmd A | Duplicate ID Field matrix spike (10 or 100 ng/mL] COMMENTS: CG MN-IW-MRIW14-DB-141001 Sandy sediment; DTR: 1.16; DTW: 2.04 33663300..00006600 3M MN01596009 como -- re cnn Cottage Grove, MN PORE SAMPLE DATA SHEET Project No.: 02181-002-179 ri AE Drainage System: nTr E eo n -- GPS Latitude: 44.783879 Mississippi River County: Washington GPS Longitude: -92.904248 State: MN Location Description: IW-14 transect line Water Conditions: ( ) Low Turbidity (X) Moderate Turbidity ( ) High Turbidity I Water Conditions: ( ) Calm (X) Choppy ( ) Visible Current cm meee Weather Conditions: Temp. 50 F ( ) Sunny (X) Cloudy ( ) Rain (X) Windy E mrT Ta om Depth to Sediment: 6.6 ftbws Sediment Bottom: ( X ) Firm ( ) Soft Water Sample Method: ( X ) Peristaltic Pump supleoepmimsw |_ e compouepss zanasamy w| Sample Depth (ftbws1 Pownmeguonsop rgaen rmntel| Flow Rate (gallons per minute] sopeond_ oseenwns | Sample Date Comper ess | Sample Time oiscir saec|csi w v | o wam| yo wm r |eww]| pH / SC l "r (c) / DO (mg/L)/ORP sper]comowmmmouworesw| Sample ID owtemef comsmmmmmosuomo| Duplicate ID resmpegonoed 1] Field matrix spike (1.0 ng/mL1 cer -- COMMENTS: 8.46 Water Sample Data Composite (1.32' and 5.28') 0.1 9pm 0913012014 16:35 344 17.8 7.7 103 CG MN-SW-MRIW014 b-0-140930 CGMN-SW-MRIW14b-DB-140930 [porewaren| Em Well Diameter (in) -- Depth to Sediment (ftbws) r-- o, Depth to Top of Screen (ftbws) Depth to Bottom of Screen (ftbws) Water column = Well Volume (gal) me Purge Start (time) Purge Stop (time) mn Volume Purged (gal) PfE s TEia Well Purged Dry? (X) Yes ( ) No Sample Method: (X) Peristaltic Pump == 7.3' z0.67 12:31 --12:36 =0.75 1 6.6' 7.55' 6.05' `SaDepnctrtael Sample Depth Interval (ftbws] spond owas | Sample Date sper ww | Sample Time miscir rnc|eao s o | m weo|yo en n |ees]| pH ! SC i "r (c) / DO (rag/L)/ORP spon commammmsrn| Sample ID 7.74 Water Sample Data 7.55' to 8.05' 10/02/2014 08:40 405 15.36 CG MN-IW-M RIWI 4b-0-141002 7.74 -65 Foam spegooongmd Duplicate ID Field matrix spike (10 or 100 ng/mL] | CGMN-IW-M RIW14b-DB-141002 COMMENTS: Gray/brown sand; DTR: 4.45'; DTW: 4.70' 33663300..00006611 3M MN01596010 -- Cottage Grove, MN PORESANDAPTASLHEEET PORE SAMPLE DATA SHEET sims Project No.: 02181-002-179 i. premer Drainage System: Mississippi River rn wr GPS Latitude: 44.783114 Am---- Location Description: IW-14 transect line fw County: Washington Ek GPS Longitude: -92.904237 Water Conditions: ---- Weather Conditions: ( ) Low Turbidity (X) Moderate Turbidity ( ) High Turbidity a ta ry <a: Water Conditions: (X) Calm ( ) Choppy ( ) Visible Current boi Nalini Ap Temp. 60 F ( ) Sunny (X) Cloudy ( ) Rain (X) Windy State: MN conte " sansa rn (150 Depth to Sediment: Se -- Water Sample Method: 7.90' ( X ) Peristaltic Pump SupeDpmmlw _____ e comeseqs smmasn w| Sample Depth (ftbws1 Powmueguorspermtel orem | Flow Rate (gallons per minute] sopeond_ oseenwns | Sample Date Comper ws | Sample Time siscir ansc|cwi m o | o wam| yo ter |ewu]| pH / SC l "r (c) / DO (mg/L)/ORP women comowwmmouscweme| Sample ID owen comswammucosuome| Duplicate ID reamed. Field matrix spike (1.0 ng/mL1 cows -- COMMENTS: 8.43 ftbws Sediment Bottom: ( ) Firm ( ) Soft Water Sample Data Composite (1.58' and 6.32') 0.1 9pm 0913012014 15:95 373 17.8 7.47 84 CGMN-SW-MRIW014d-0-140930 CGMN-SW-MRIW14d-DB-140930 [Forever] ema ; Well Diameter (in) a rt pr Depth to Sediment (ftbws) r---- ry Depth to Top of Screen (ftbws) ovr i Depth to Bottom of Screen (ftbws) 1 7.90' 8.80' 9.3 Water column ero Well Volume (gal) | ---- Purge Start (time) rte aw Purge Stop (time) ire oe Volume Purged (gal) ream tr Well Purged Dry? (X) Yes ( ) No er Sample Method: (X) Peristaltic Pump 7.95 0.7 16:46 15:50 0.8 `SaDepnctrtael Sample Depth Interval (ftbws] -- | Sample Date nf] Sample Time wsseensommro oTmT we TmTw] pH ! 8C i T (C) / DO (rag/L)/ORP eeSample ID 8.42 Water Sample Data 7.9'-8.3' 10/01/2014 10:00 380 17.52 7.46 90 CG MN-IW-M RIWI 4d-0-141001 Duplicate ID CGMN-IW-M RIW14d-DB-141001 Field matrix spike (10 or 100 ng/mL] CG M N-IW-M RIW14d-FMS-141001 aa: A eR e T ] COMMENTS: Gray Clay; Some sediment in sample/sl, turbid; DTR: 1.70'; DTW: 3.05' 33663300..00006622 swmorssaors 3M MN01596011 como Cottage Grove, MN A PORE SAMPLE DATA SHEET frien Project No.: 02181-002-179 Si Els Drainage System: Mississippi River er wns GPS Latitude: 44.782683 nonts o Location Description: IW-14 transect line -- Water Conditions: Weather Conditions: ee ( ) Low Turbidity Water Conditions: Temp. 60 F rr ms County: Washington GPS Longitude: -92.904238 re amen (X) Moderate Turbidity ( ) Calm (X) Choppy Voor ( ) High Turbidity ( ) Visible Current ( )Sunny (X) Cloudy ( )Rain (X) Windy TE State: MN prS----" Depth to Sediment: Water Sample Method: =7.35 ( X ) Peristaltic Pump on sermnmm 4im tom ftbws Sediment Bottom: ( ) Firm ( ) Soft `SaDmepplwes wsmpeom1] Sample Depth (ftbws1 Pownmeguonspermntel osgem | Flow Rate (gallons per minute] sompreond ewnew | Sample Date Sompetind _ wes Sample Time iscirac u | oy wso|owm e | oy wso |rwml| pH / SC l "r (c) / DO (mg/L)/ORP sper]comewmmwowronwsw| Sample ID owtemer] comswmmwurosuesw| Duplicate ID resmpegonoey Field matrix spike (1.0 ng/mL1 Moose Rinsate Sample ID 8.44 Water Sample Data Composite (1.47' and 5.88') 0.1 0913012014 14:45 329 17.6 7.36 77 CGIV]N-SW-MRIW014f-0-140930 CGMN-SW-MRIW14f-DB-140930 COMMENTS: |E emrerr-- . Well Diameter (in) fin pr Depth to Sediment (ftbws) amr = Depth to Top of Screen (ftbws) resins po Depth to Bottom of Screen (ftbws) Water column i, i Well Volume (gal) -- Ta Purge Start (time) -- Purge Stop (time) eet 2 Volume Purged (gal) remand Well Purged Dry? (X) Yes ( ) No Sr mes Sample Method: (X) Peristaltic Pump 7.40' 0.66 15:05 15:09 0.6 1 7.35' 8.20' 8.70' n [CC p vowswmpe) om Sample Depth Interval (ftbws] a Sample Date re 8ample Time Water Sample Data 8.20' to 8.70' 10/02/2014 08:25 pH / SC ~ T (C) / DO (mg/Ly ORP 8.46 349 16.91 7.1 88 zi Sample ID CG MN-IW-MRIW14f-0-141002 oa] TT compe Duplicate ID CGMN-IW-MRIW14f-DB-141002 rtm aepa ee] Field matrix spike (10 or 100 ng/mL] rn] Rinsate Sample ID counts: ETT COMMENTS: Gray Clay; DTR: 2.30'; DTW: 3.60' 33663300..00006633 awsonra 3M MN01596012 J -- ee cnn Cottage Grove, MN PORE SAMPLE DATA SHEET Project No.: 02181-002-179 rm a Drainage System: i TEr ee -- GPS Latitude: 44.784036 Mississippi River County: Washington GPS Longitude: -92.899015 State: MN Location Description: IW-19 transect line Water Conditions: ( ) Low Turbidity (X) Moderate Turbidity ( ) High Turbidity I Water Conditions: ( ) Calm (X) Choppy ( ) Visible Current eT Weather Conditions: Temp. 60 F ( )Sunny (X) Cloudy ( )Rain (X) E mre Depth to Sediment: 4.4 ftbws Sediment Bottom: ( ) Windy Firm (X) 5oft Water Sample Method: ( X ) Peristaltic Pump supleoepmimsw c |_ ompoe sseic s ssamw sery| Sample Depth (ftbws1 Pownmeguonsop rgaen rmntel| Flow Rate (gallons per minute] sopeond_ oseenwns | Sample Date Somperind ee | Sample Time iscirccioomyors] as | sw | wm | en | w | pH / SC l "r (c) / DO (mg/L)/ORP 8.4 sper]comswwewenowoms| Sample ID owtemef comvewmawmosuesw| Duplicate ID resmpegonoed 1] Field matrix spike (1.0 ng/mL1 cer -- COMMENTS: Water Sample Data Composite (0.68' and 3.52") 0.1 9pm 0913012014 12:55 347 17.33 6.91 85 CG MN-SW-MRIW019-0-140930 CGIV]N-SW-MRIW19-DB-140930 [porewaren| Em Well Diameter (in) Depth to Sediment (ftbws) ---- Depth to Top of Screen (ftbws) -- --% Depth to Bottom of Screen (ftbws) Water column = = Well Volume (gal) rl -- Purge Start (time) mmm ee Purge Stop (time) mn 8 Volume Purged (gal) SE ni TE Well Purged Dry? (X) Yes ( ) No fsa Sample Method: (X) Peristaltic Pump 1 4.4' 6.8' 7.1' 4.75 0.42 13:17 13:19 0.4 speoientton _ egwre | Sample Depth Interval (ftbws} spond woos | Sample Date sper ww | Sample Time miscirr st c | e awo|owm e | oy emo |nmw]| pH / SC i T (C) / DO (rag/L)/ORP spon commamwesion| Sample ID 7.94 409 Water Sample Data 6.6' to 7.1' 10/01/2014 09:15 17.43 C~MN-IW-MRIWI 9-0-141001 5.69 -39 feDuplicate ID Field matrix spike (10 or 100 ng/mL} CG MN-IW-MRIW19-DB-141001 COMMENTS: Some sediment in sample/turbid; Gray sandy clay; DTR: 3.90'; DTW: 6.25' 33663300..00006644 3M MN01596013 como -- re cnn Cottage Grove, MN PORE SAMPLE DATA SHEET Project No.: 02181-002-179 ri AE Drainage System: i TT ee i GPS Latitude: 44.784180 Mississippi River County: Washington GPS Longitude: -92.899002 State: MN Location Description: IW-19 transect line Water Conditions: ( ) Low Turbidity I Water Conditions: en Weather Conditions: Temp. 50 F E mre Depth to Sediment: 5.6 (X) Moderate Turbidity ( ) High Turbidity ( ) Calm (X) Choppy ( ) Visible Current ( )Sunny (X) Cloudy ( )Rain ( X ) Windy ftbws Sediment Bottom: ( ) Firm (X) 5oft Water Sample Method: ( X ) Peristaltic Pump supleoepmimsc |_ omposse weeqswimei on pamasry| Sample Depth (ftbws1 Pownmeguonsop rgaen rmntel| Flow Rate (gallons per minute] sopeond_ oseenwns | Sample Date Songer we | Sample Time iscirccioomyore] siz | swe | um | im | w | pH / SC l "r (c) / DO (mg/L)/ORP sen]comowmmmowsoresws| Sample ID owtemef comsmmmmmosuomo| Duplicate ID reamed. Field matrix spike (1.0 ng/mL1 cer -- COMMENTS: 8.42 Water Sample Data Composite (1.12' and 4.50") 0.1 9pm 0913012014 13:40 349 17.81 7.32 52 CG MN-SW-MRIW019 b-0-140930 CGMN-SW-MRIW19b-DB-140930 [porewaren| Ee Probe Diameter (in) 1 Depth to Sediment (ftbws) 6.6 mm : Depth to Top of Screen (ftbws) 7.6 r-- = Depth to Bottom of Screen (ftbws) 8.1 Water column Well Volume (gal) me Purge Start (time) rmPurge Stop (time) mn Volume Purged (gal) TR Well Purged Dry? (X) Yes ( ) No psa Sample Method: (X) Peristaltic Pump o=s6.75 0.6 13:69 14:02 0.6 speonientton _ eesr | Sample Depth Interval (ftbws] spond woos | Sample Date sper we | Sample Time miscisr u c | e weo|om er o | y emo |nw]| pH / SC i "r (c) / DO (rag/L)/ORP 8.31 Water Sample Data 7.6' to 8.1' 10/01/2014 09:30 386 7.67 6.01 61 Sample ID a Duplicate ID Foam spegooongmd Field matrix spike (10 or 100 ng/mL] CG MN-IW-M RIWI 9b-0-141001 c---- || CGMN-IW-MRIW19b-DB-141001 COMMENTS: Gray clay; DTR: 2.5'; DTW: 4.25' 33663300..00006655 3M MN01596014 como -- rn Cottage Grove, MN PORE SAMPLE DATA SHEET Project No.: 02181-002-179 rll A Drainage System: s TTe ee ---- GPS Latitude: 44.783496 Mississippi River County: Washington GPS Longitude: -92.899104 State: MN Location Description: IW-19 transect line Water Conditions: ( ) Low Turbidity (X) Moderate Turbidity ( ) High Turbidity I Water Conditions: () Calm (X) Choppy ( ) Visible Current pe Vm Weather Conditions: Temp. 50 F ( )Sunny (X) Cloudy ( ) Rain ( X ) Windy ET a Depth to Sediment: 6.4 ftbws Sediment Bottom: ( ) Firm (X) 5oft Water Sample Method: ( X ) Peristaltic Pump wsmpeom1] Water Sample Data supleoepmimsc |_ ompouepmanassmy| Sample Depth (ftbws1 Composite (1.28' and 5.12') Pownmeguonsop rgaen rmntel| Flow Rate (gallons per minute] 0.1 9pm sompreond ewnew | Sample Date 0915012014 Sompetind ees Sample Time 12:05 iscirsc s | oy awo|owm a o |y eso |rwml| pH / SC l "r (c) / DO (mg/L)/ORP 8.38 326 17.2 6.8 79 sompeo| comswammonsorese| Sample ID CGMN-SW-MRIW019d-0-140930 owtemef comsmmmmseosuomo| Duplicate ID CGMN-SW-MRIW19d-DB-140930 reamed. Field matrix spike (1.0 ng/mL1 cer COMMENTS: EFoncmwaren Well Diameter (in) 1 Depth to Sediment (ftbws) 6.4 Em Depth to Top of Screen (ftbws) 8.0 Snr Depth to Bottom of Screen (ftbws) 8.5 Water column Well Volume (gal) mm a Purge Start (time) mmm em Purge Stop (time) mn 8 Volume Purged (gal) SE ni TE Well Purged Dry? (X) Yes ( ) No fsa Sample Method: (X) Peristaltic Pump 8.55 0.77 12:28 12:32 0.8 speoienttow _ soess | Sample Depth Interval (ftbws] spond owas | Sample Date sper we | Sample Time miscisr w c | e weo|oum m | oy emo |nwm]| pH ! SC i "r (c) / DO (rag/L)/ORP spon commammmsron| Sample ID 8.35 Water Sample Data 8.0' to 8.5' 10/01/2014 09:05 356 17.21 6.83 93 CG MN-IW-M RIWI 9d-0-141001 Faspm e oa o orgmd_____commie Duplicate ID Field matrix spike (10 or 100 ng/mL] GGMN-IW-MRIW19d-DB-141001 CGM N-IW-M RIW19d-FMS-141001 | COMMENTS: Soft Gray Clay; DTR: 2.45'; DTW: 3.77' 33663300..00006666 3M MN01596015 como -- rn Cottage Grove, MN PORE SAMPLE DATA SHEET Project No.: 02181-002-179 rm A Drainage System: i Tn r -- GPS Latitude: 44.782929 Mississippi River County: Washington GPS Longitude: -92.899194 State: MN Location Description: IW-19 transect line Water Conditions: ( ) Low Turbidity (X) Moderate Turbidity ( ) High Turbidity I Water Conditions: ( ) Calm (X) Choppy ( ) Visible Current en Weather Conditions: Temp. 46 F ( )Sunny (X) Cloudy ( )Rain ( X ) Windy ee Depth to Sediment: 12.1 ftbws Sediment Bottom: ( ) Firm ( ) Soft Water Sample Method: ( X ) Peristaltic Pump supleoepmimsw |_ e compouepus zanassn w| Sample Depth (ftbws1 Pownmeguonsop rgaen rmntel| Flow Rate (gallons per minute] sompreond ewnew | Sample Date Sompetind wes Sample Time iscirccioomyors] au | ww | we | en | wu | pH / SC l "r (c) / DO (mg/L)/ORP sompeo| comvewmwmoworesw| Sample ID owtemer] comswmmwmosuew| Duplicate ID reams Field matrix spike (1.0 ng/mL1 mowosawn] wns Rinsate Sample ID 8.34 Water Sample Data Composite (2.42' and 9.68') 0.1 0913012014 11:15 338 16.02 6.77 13 CGMN-SW-MRIW019f-0-140930 CGMN-SW-MRIW19f-DB-140930 Note Applicable COMMENTS: LiWell Diameter (in) Te, Depth to Sediment (ftbws) poe Depth to Top of Screen (ftbws) me Depth to Bottom of Screen (ftbws) ra u Total Probe Depth (ftbws) 1 12.1 13.6 14.1 14.1 Water column Well Volume (gal) mm i Purge Start (time) mm = Purge Stop (time) mn, % Volume Purged (gal) SE nT Well Purged Dry? (X) Yes ( ) No fee Sample Method: (X) Peristaltic Pump 13.0~; 1.2 8:45 8:54 1.35 wsmmeom ] Water Sample Data sopeogomeatton weer | Sample Depth Interval (ftbws] 13.6' to 14.1' speod wows | Sample Date 10/02/2014 sper we | Sample Time 08:06 miscivr e | co awi|owo e m |ouw o|nw]| pH / SC I T (C) / DO (mg/Ly ORP 7.67 498 14.47 4.1 .48 some] commumwmerw| Sample ID CG MN-IW-IVlRIW19f-0-141002 owen commammmosuwr| Duplicate ID CGM N-IW-MRIW19f-DB-141002 Foams ooonge | Field matrix spike (10 or 100 ng/mL] RoasteSavgien] dodges | Rinsate Sample ID Not Applicable COMMENTS: Gray Clay; DTR: 4.11'; DTW: 6.05' 33663300..00006677 3M MN01596016 como rn Cottage Grove, MN irl -- la Drainage System: ioTm =a GPS Latitude: PORE SAMPLE DATA SHEET Project No.: 02181-002-179 Mississippi River 44.78267 County: GPS Longitude: Washington -92.89306 State: MN Location Description: Water Conditions: cI Ti SaseeO TRe Weather Conditions: ERrRm orn rm Depth to Sediment: 2.3 IW-25 line ( ) Low Turbidity (X) Moderate Turbidity ( ) High Turbidity Water Conditions: ( ) Calm (X) Choppy ( ) Visible Current Temp. 46 F ( ) Sunny (X) Cloudy ( ) Rain (X) Windy ftbws Sediment Bottom: (X) Firm ( ) Soft Water Sample Method: ( X ) Peristaltic Pump supleoepmimsc |_ ompouewei esws meosn saarsn| Sample Depth (ftbws1 Pownmeguonsop rgaen rmntel| Flow Rate (gallons per minute] sompreond ewnew | Sample Date Sompetind ew Sample Time scirecioomyors] ax | ss | wm | ew |ow | pH / SC l "r (c) / DO (mg/L)/ORP sper]comswmmmasovew| Sample ID owtemef comvewmawasosuesw| Duplicate ID resmpegonoey Field matrix spike (1.0 ng/mL1 Mes] Rinsate Sample ID 8.36 Water Sample Data Composite (0.46' and 1.84') 0.1 9pm 0913012014 9:30 396 16.33 6.57 194 CG MN-SW-MRIW25-0-140930 CGMN-SW-MRIW25-DB-140930 COMMENTS: LiWell Diameter (in) fa : Depth to Sediment (ftbws) mm : Depth to Top of Screen (ftbws) -- 2 Depth to Bottom of Screen (ftbws) rm 2 Total Probe Depth (ftbws) 1 2.3 0.5 3.05 3.55 Water column Well Volume (gal) me Purge Start (time) mem Purge Stop (time) ne Volume Purged (gal) Fa, Well Purged Dry? ( ) Yes ( ) No AE Sample Meti~od: (X) Peristaltic Pump 9.61 0.855 =9:50 10:05 :1 sopeogomeatton w _ es swwasws w]| Sample Depth Interval (ftbws1 seo] omens | Sample Date spre ee | Sample Time miscist w| coew n|owo m | mo owo|nom]| pH ! SC i "1" (C) / DO (mg/L)/ORP some commummmonmo| Sample ID owen commummasosuome| Duplicate ID Foams ooonge | Field matrix spike (10 or 100 ng/mL1 moosawen| wages Rinsate Sample ID 6.95 Water Sample Data 3.05' to 3.55' 09/30/2014 10:10 692 15.78 CGMN-IW-MRIW25-0-140930 CG MN-IW-MRIW25-DB-140930 0.38 Not Applicable -122 I COMMENTS: Loose gray sand (f-m), litle silt and clay; DTR: 5.46'; DTW: 5.46' 33663300..00006688 3M MN01596017 como -- rn Cottage Grove, MN PORE SAMPLE DATA SHEET Project No.: 02181-002-179 rl A Drainage System: i TE ee -- GPS Latitude: 44.78281 Mississippi River County: Washington GPS Longitude: -92.89304 State: MN Location Description: IW-25 transect line Water Conditions: ( ) Low Turbidity (X) Moderate Turbidity ( ) High Turbidity ry ay Water Conditions: ( ) Calm (X) Choppy ( ) Visible Current pe Oe Se er Weather Conditions: Temp. 45 F ( ) Sunny (X) Cloudy ( ) Rain (X) Windy Ee Te Depth to Sediment: 1.05 ftbws Sediment Bottom: ( X ) Firm ( ) Soft Water Sample Method: ( X ) Peristaltic Pump spew oep e mw ews s|_ w __| Sample Depth (ftbws1 Pownmeguonsp eige en rmntel| Flow Rate (gallons per minute] sompreond ewnew | Sample Date Sompetind ess | Sample Time scireaxc|iao w | om wwy |o ewr|sw] m | pH / SC l "r (c) / DO (mg/L)/ORP sen]cownswwwamouess| Sample ID owtemef comsmmmmamosuomo| Duplicate ID resmpegonoed 1] Field matrix spike (1.0 ng/mL1 cer -- COMMENTS: 8.24 Water Sample Data 0.75 0.1 9pm 0913012014 10:25 335 16.14 6.56 20 CG MN-SW-MRIW25b-0-140930 CG MN-SW-MRIW25b-DB-140930 [porewaren| Em Well Diameter (in) Depth to Sediment (ftbws) ---- Depth to Top of Screen (ftbws) me Depth to Bottom of Screen (ftbws) Well Volume (gal) me Purge Start (time) frPurge Stop (time) mm Volume Purged (gal] re Well Purged Dry? ( ) Yes (X) No psa Sample Method: (X) Peristaltic Pump -1" 1.05 1.55 0.2 210:28 =410:40 2.05 11 smpogormatton wes wens w]| Sample Depth Interval (ftbws} Water Sample Data 1.05' to 1.55' spool owen | Sample Date 09/30/2014 sper es | Sample Time 10:45 siscir ssc|cwoo s o | m wwo| ueymo |nae]| pH / SC i T (C) / DO (mg/L)/ORP 6.85 1063 16.33 0.43 samen]commamvasorme| Sample ID CG MN-IW-M RIW25b-0-140930 owen commumomosuom| Duplicate ID CGMN-IW-M RIW25b-DB-140930 fr Field matrix spike (10 or 100 ng/mL} mel a COMMENTS: Poorly sorted light gray sand (f-~s), trace fines; DTR:3.27'; DTW: 3.22' -110 33663300..00006699 3M MN01596018 como -- rn Cottage Grove, MN PORE SAMPLE DATA SHEET Project No.: 02181-002-179 rll A Drainage System: Q TEE ee ---- GPS Latitude: 44.78204 Mississippi River County: Washington GPS Longitude: -92.89319 State: MN Location Description: IW-25 Water Conditions: pe Weather Conditions: ET Depth to Sediment: transect line ( ) Low Turbidity (X) Moderate Turbidity ( ) High Turbidity YE ay Water Conditions: ( ) Calm (X) Choppy ( ) Visible Current Oe er Temp. 45 F ( ) Sunny (X) Cloudy ( ) Rain (X) Windy a im 5.5 ftbws Sediment Bottom: ( ) Firm ( ) Soft Water Sample Method: ( X ) Peristaltic Pump supleoepmims|_ wscm ompouerp ranasse y om1|] Sample Depth (ftbws1 Pownmeguonsop rgaen rmntel| Flow Rate (gallons per minute] sompreond owen | Sample Date Sompetind _ es Sample Time iscirc swo|yso e o | msemo|yo es r |s aesl| pH / SC l "r (c) / DO (mg/L)/ORP sompeo| comswwmwossores| Sample ID owtemef comsmmmmascosuonms| Duplicate ID reams Field matrix spike (1.0 ng/mL1 mesgg ps ] Rinsate Sample ID 8.37 Water Sample Data Composite (1.1' and 4.4') 0.1 9pm 0913012014 8:25 350 16.72 6.5 CG MN-SW-MRIW25d-0-140929 CG MN-SW-MRIW25d-DB-140929 Not Applicable 200.3 COMMENTS: EfEoncwaren Well Diameter (in) 1 frDepth to Sediment (ftbws) 5.5 m , m ~:F Depth to Top of Screen (ftbws) 6 Depth to Bottom of Screen (ftbws) 6.5 Water column Well Volume (gal) tein = Purge Start (time) mm Purge Stop (time) mn 5 Volume Purged (gal) ro Well Purged Dry? (X) Yes ( ) No psa: Sample Method: (X) Peristaltic Pump 6.1 0.5~; 8:53 8:57 0.6 swpeogomeaiton [CC voawsvwempseom | Sample Depth Interval (ftbws] spend wees | Sample Date sper ww | Sample Time miseira3c|ep amo|owmao|yeo w n |swm ]| pH / SC ~ T (C) / DO (mg/Ly ORP 8.3 328 Water Sample Data 6.0' to 6.5' 10/01/2014 08:10 15.2 6.67 Sample ID owen]commumessosnuer| Duplicate ID Fodmspaeoaomge Field matrix spike (10 or 100 ng/mL1 sesame] togese | Rinsate Sample ID CG MN-IW-M RIW25d-0-141001 CGMN-IW-M RIW25d-DB-141001 Not Applicable COMMENTS: Gray sandy (v. fine- fine) silt/clay; DTW: 5.9'; DTR: 4.35' 33663300..00007700 3M MN01596019 como -- rn Cottage Grove, MN PORE SAMPLE DATA SHEET Project No.: 02181-002-179 rl AE Drainage System: i TT -- GPS Latitude: 44.78153 Mississippi River County: Washington GPS Longitude: -92.89331 State: MN Location Description: IW-25 transect line Water Conditions: ( ) Low Turbidity (X) Moderate Turbidity ( ) High Turbidity I Water Conditions: ( ) Calm (X) Choppy ( ) Visible Current eV ee Weather Conditions: Temp. 59 F ( ) Sunny (X) Cloudy (X) Rain ( ) Windy ET a im Depth to Sediment: 7.7 ftbws Sediment Bottom: ( ) Firm ( ) Soft Water Sample Method: ( X ) Peristaltic Pump Sumpleoeptaws|w come poues psesw asey| Sample Depths (ftbws1 Pownmeguonsop rgaen rmntel| Flow Rate (gallons per minute] sompreond een | Sample Date Sompetind ew | Sample Time iscirc amc|iwo m o | mema| yo amr |sws]| pH / SC l "r (c) / DO (mg/L)/ORP sen]comswwmwamonsss| Sample ID owtemer] comswwmwamosiess| Duplicate ID Fosmatcophioerom comswumwasewsuoss| Field matrix spike (1.0 ng/mL1 cer -- COMMENTS: 8.23 Water Sample Data Composite (1.54' and 6.16') 0.1 9pm 0912912014 16:40 378 19.36 7.13 196 CG MN-SW-MRIW25f-0-140929 CG MN-SW-MRIW25f-DB-140929 CG MN-SW-MRIWZSf-FMS-140929 [porewaren| Em Well Diameter (in) 1 m-- : Depth to Sediment (ftbws) 7.7 mm = Depth to Top of Screen (ftbws) nm SrDepth to Bottom of Screen (ftbws) nm ene = 1 Probe Volume (gal) 0.68 ee Purge Start (time) nm rm - Purge Stop (time) nm emir = Volume Purged (gal] nm ffe s Well Purged Dry? (X) Yes ( ) No Sample Method: (X) Peristaltic Pump smpogorn[ atton wwesawwpeonn || Sample Depth Interval (ftbws] Water Sample Data 7.9' sompteoe ewan | Sample Date sper wea | Sample Time siscicsmc|io sso|mwoeu|yoom | newm ]| pH / SC i T (C) / DO (mg/L)/ORP some] commumwmerin| Sample ID owes commammmosn| Duplicate ID Fam spe oo Orgmdc _ ommummsnsion| Field matrix spike (10 or 100 ng/mL] 8.25 10101/2014 08:25 345 18.98 7.26 nm CG MN-IW-MRIW25f-0-141001 CGMN-IW-MRIW26f-DB-141001 CG MN-IW-IVlRIW25f-FMS-141001 COMMENTS: Gray Clay; DTR: 1.05'; DTW: 2.41' 33663300..00007711 ssn 3M MN01596020 AATTTTAACCHHMMEENNTT CC HHYYDDRROOGGRRAAPPHHSS FFOORR SSIITTEE MMOONNIITTOORRIINNGG W WEELLLLSS 33663300~.00007722 3M_MND1596021 3M MN01596021 ICle a -- en -- y ~' 750.0 Groundwater Hydrograph Monitoring Wells MW-01, MW-05, and MW-07 October 2012 - December 2014 .nu 745.0 hee ~ 740.0 - PL ~ 735.0 O fn on LE 730.0 dd 725.0 a 720.0 Sep-12 Jan-13 Apr-13 Aug-14 Dec-14 LS L me ee e o",~ ~"~MW-01 ~ MW-05 Date ~MW-07 ~,'~ Daily Precipitation (inches) Te 3M_MN01596022 33663300..00007733 || 695.0 - ||| 692 0 |||| a ||[|I i | os | 3 | -o 683.0 |||| 680.0 Sep-12 |- | | ee mtv Hydrrooggraeph Groundwater Hydrograph Monitoring Wells MW-110 and MW-15 October 2012 - December 2014 |l| a| |||| ||| | i 1 Ll| | | | | | | - lh A AAR dil. ||| ------s -- -- 33MM__MMNON101559966002233 33663300..00007744 Groundwater Hydrograph | -- ae | Monitoring Wells MW-10, MW-11, MW-13 and MW-108 | Getober2012 December2014. | October 2012 - December 2014 710.0 705.0 700.0 | 7 695.0 || b-- e --.] | 685.0 |E yr r 570.0 [eh 665.0 bo660.0 coll 655.0 Sep-12 Jan-13 Apr-13 Aug-14 Dec-14 | ee Date ren | 3M_MN01596024 3630.0075 | - | 740.0 Groundwater Hydrograph Monitoring Wells MW-08, MW-09, MW-17, MW-18 and MW-19 October 2012 -December 2014 | 730 0 | 720.0 | -- -- %| 700.0 | Lh 600.0 Dhl 1 680.0 | far 670.0 ble 660.0 I ame CO 650.0 Sep-12 May-14 Aug-14 Dec-14 | cris. eD -- ST | Date Daily Precipitation (inches) Ce CGMN GWELEVs Hvdrof~raphs.xlslVW 8, 9, 17, 18, 1~ CHT 3M_MN01596025 33663300..00007766 | 730.0 Groundwateryrogropn Groundwater Hydrograph Monitoring Wells MW-02 and MW-03 October 2012 - December 2014 | 1. | 72510 | oo ------ | 720.0 | I 715.0 A 4 710.0 |b BP 705.0 a -- -- | 700.0 oo | - | o 695.0 |. WN ML, | 690.0 l| RNnar ms Ee e stan ei e || Sep-12 Jan-13 Apr-13 Date Aug-14 Dec-14 Ce 3M_MN01596026 33663300..00007777 E | e GroundwaterHydrograph .|| Groundwater Hydrograph Monitoring Wells ECPZ-01, ECPT-O2R, ECPZ-O3R and MW-112 | ns | October 2012 - December 2014 | = rr 694.0 ||| ae.T-- | 688.0 || E=685.0 |a682.0 1] . | 6 4b -- a | > = 3 A| = - 679 0 | 4 ] L | 676.0 ||| in -- hir.= ECro AT--otSACEo sst t ste Co * ||| Sep-12 Jan-13 Apr-13 ~ECPZ-02R Date Feb-14 Daily Precipitation (inches) Dec-14 33MM__MMNNO011559966002277 33663300..00007788 Groundwater Hydrograph Monitoring Wells MW-101, MW-102, MW-103, MW-104 and MW-105 m Sea| 695.0 694.0 6930 692.0 October 2012 - December 2014 688.0 687.0 686.0 685.0 Sop-12 Apr-13 Date Feb-14 3M_MN01596028 3630.0079 Groundwater Hydrograph Monitoring Wells MW-04, MW-04R, MW-14R and PZ-14 October 2012 - December 2014 7100 705.0 | | 700.0 So 695.0 -- E-- -- i [I 690.0 In 660.[I 675.0 670.0 Cl 665.0 ibd 660.0 | ln Te | Sep-12 Date Dec-14 3M_MN01596029 3630.0080 TL_ ABORATORYaAA_ ATNTTAALtCYaHTcIMmCEeANLnTtPD_ oACKAGES AND_ LCCAHHBAAOGIINNRR--AOOOTUFFON--CRDCUYWUSSAATTTNOOEADDRLYYYSDDTAOIOCMCCAPUULLMMIEPNENAGNTCTEAKAVTATEIGIONOETNNSSFFAOONRRD GROUNDWATER SAMPLING EVENTS 33663300~.00008811 _no1ss6030 3M MN01596030 JJAANNUUAARRYY 22001144. 33663300~.00008822 3M_MND1596031 3M MN01596031 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-13 FFiinnaall RReeppoorrtt AAnnaallyyssiissooff PPFFBBAA,, PPFFOOAA,, PPFFBBSS,, PPFFHHSS,, aanndd PPFFOOSS iinn AAqquueeoouuss SSaammpplleess,, CCoottttaaggee GGrroovvee GGrroouunnddwwaatteerr SSaammpplliinngg 1Is%t QQuuaarrtteerr 22001144 Laboratory Rogues Number 15011010313 Laboratory Request Number: ISO11-01-03-13 ero tans Report Date - Date of Last Signature TTeessttiinngg LLaabboorraattoorryy a sas poraions 3M EHS&S Operations 33MM EEnnvviirroonnmmeennttaall LLaabboorraattoorryy Sinn ST Building 260-5N-17 Moplonser NN. 351441060 Maplewood, MN 55144-1000 Requestor Requester SaStM SPuoitnMgn055s5u44s10s00 GGaarryy HHoohheennsstteeiinn 33MM EEHHSS&&SS OOppeerraattiioonnss 3M Building 224-5W-03 Saint Paul, MN 55144-1000 PPhhoonnee:: ((685511)) 773377--33557700 fBe >oeurWwoRm The testing reported herein meet the requirements of ANSI/ISO/IEC 17025:2005 TE eeete otsTye "General Requirements for the Competence of Testing and Calibration SEITRIRIREIILS Bonn Laboratories", in accordance with A2LA Certificate # 2052.01. Additionally, the iSaias s E al r, ThSeshE laboratory's quality system has been audited and was determined to be in conformance with the EPA GLPs (40 CFR 792) by an independent A2LA assessmenL 33663300..00008833 -- PAGE 1 OF 39 3M MN01596032 REPORTING1501 011s 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-13 3H3r~ EEnnvviirroonnmmeennttaall LLaabboorraattoorryy 333MMM PEErnnivnvicirrioopnanlmmeAennntataatll LcLaaablboorvraatitootrryyoTTerecch:hnniScicuaaslaDDneirWecocttlo:r: Wika K William K. Reagen, Reagen, PhD. Ph.D. Report Author Kove Eich 3M Principal Analytical Investigator: Report Author: Kevin Eich Susan Wolf AAnnaal~yytti#ccaalJ RReppoor~t ~ISSO01111-o0011-o0033-o1133 ``AACnnoaatllayysgs'oissGoorffoPPvFFeBAGA,r,oPPunFFdOOwAAa,,tePPrFFBSSSa,,mPPpFFiHHnSS-,g, aa1nnddQuPPaFFOOSS ii2nn0AA1q4quueoouss SSaammppleless,, Cottage Grove Groundwater Sampling - l't Quarter 2014 RReeppoorrtt aDtaete:: DDaateeooff LLaasstt Satie Signature 11 _IInnttrroodduuccttiioonn/S/Suummmmaarryy TTSohhloeut33iMMonsEEnnpvveiirrrosononmnmeeenlntataatlltLLaahbbo3oerMraatCtooorrtyytppargreeepGpaarrroeevddeaafnnaddciaaiynn.aallyySzzaeemddpgglrreoosuunnwddewwraeattecerorslsaeacmmtpepldoleesns ccJooallnleeucactreeyddb1by3y,WW1e4es,st1too,nn S1f16o6o,o,luaaatnnniodddnJs22a22pn.,eu22r0a0s1ro14yn4.3n.3e,SSl2aa0mta1tph4leemas3wMwopeeoCrmelortrtefeaoeitgumuerpmnsGooerrddoatvtooeutrthfhaefec3il3ittoMyh. EESannvnaviamirrloponynlemsmseieonwfsntteaParlleeLLrcaauobbololoerrracaottteouodrrtyyoaoonnnnJcJJaaaannnoududaaarry(ryPy1F113B77,A,,)122.400, 111445,oonn aPiPcnoeedrrafflPnuuedoorrrJfooauooancrcutaotanonrocyotiic2a3naa,ecc2idds0u1((fPP4oFFnaOOatAtAr)eo),,o(mPPPeFertOretfSlmuu)ooprrueoanrobaduuetuttraraenaneofbossoruurtlhfftoeonnaaantroeaoly((ePsPciFRstBBoSSf)m),P, oePProoeflrrurfloou1rorSorbOoouThht1eoa0xnaa1onnic0de5ass-cuu1ild3lffo.o(nPnaaFttBee A(()P,FFHHSS)) and Perfluorooctane sulfonate (PFOS) under laboratory project number ISO11-01-03-13. TsTahhmeop33lMeMsEEannvvciirrooonnnmmseeinndttaaollfLLaaabb0oordraattosorarymyppprlreeeppaaorrekeddsssaaammrpoeledccuoonncttaaaiilnn,eerrssafnfoowdreatwaverlvegelssanammpaplliyinnggolcodccaatmtoionanss.l. EsEpaakccehh. sEmElaaa.mcchhpCeleeommnpsttpeayttiycncceooornnsntsatirsaietinensedeerrrwovwfeadaassffoimermaldfarreskkdaeemddmwpwalierit,hhxfaiaeslp"fdfiklllsea0tsomeheperrleree"d" ufilipnnrloeicetahadtaelt,wccaioonhrdrraesanspptoaaopnrnpgdrdeoeetpddarin0taoat4layetfenminafaaileltldvvoosmluupaimmtkroeeioxsofsofpl22iuk00ie00o.n wcCmeooLrnn.ettaCifinnoirnnnggetatdhihneeewratisarhrrggeteesltearaavannealdalyfestoetsrsafnippecrrladiiorodrmrstoiaatbbrnieexdiinsnSgpgUirkssoeeegsnntatwttooeererteeh.cefoovf1riteeifrlideyfdfsoowtrmaistnhapdmaarnpldleaspccppoorrleolecopcitrrtooiiaontbn.e.amnAAgaIlltrssSiexaanmstmppiplkeehbbesotoftiltiuleeetissdonfor wSaemreplfeorctiofieledcwtoitnh internal standards and surrogate recovery standards prior to being sent to the field for sample collection. S5`S.aa0mm4pp4ll1eessMwaweierhreoodpprroeefppanarreadeyaasnndd aoarnnaalhlyeyzzeDaddtefoorrrmPiPFnFBaBAtA,o,nPPoEFfOOPAAo,,rPuPcFFrBSnS,a,tPPoEFdHHCSS,o,maapnnoddunPPdFFsOOSSn uuWssaiinntggammbeeyithhoodd ETS- ETS- 8-044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water by LadGjMecStIiMveSs;foDircetanbailcyhsoenofAsenleactssamptleosm, awesrteanadpapridcawbloere sod ta ad the co ually LC/MS/MS; Direct Injection Analysis". Internal standards were used to aid in the data quality objectives for the analysis of select samples, were applicable. TTuaaablbllleey 11csosuunmnrrlmaasirazizmeepssletthsheprsseaapmmapprlleeedrraeenssduultassnuuassyiiznngogdtthhweeiaahnntaahhelysttacicamalpl mlmeeetsthhooviddldibdeeeinpftiiafieerddteaasdboovavene.d. dAAilllsrcreusssusseltsdffoorr Ssntare nbs roprt quality control samples prepared elsewhere in this report. and analyzed with the samples will be reported and discussed RIA SToIwN R (RcoafE omis) se gpa rt gts. OG REE ]he testing reported herein meet the requirements of/~SI/ISO/IFC 17025:2005 "General Requirements for the Competence of Testing and Calibration rvssian fhASACae WEY, Abtthbym Laboratories", in accordance with A2LA Certificate # 2052.01. Additionally, the bebe cust tershisban soca 30d wsanomieto bo laboratory's quality system has been audited and was determined to be in ee ELT i by cn 3 conformance with the EPA GLPs (40 CFR 792) by an independent A2LA assessment. 33663300..00008844 encezors PAGE 2 OF 39 W_MNO1596033 3M MN01596033 TTaabbllee 11.. SSaammppllee RReessuullttss SSuummmmaarryy wes 3M ENVIRONMENTAL LAB ORA TORY REPORT NO. IS011-01-03-13 Concentration (n~llmL) EE rm le m EC=lWaFlEEaAElEL=] ISOll-01-03-13-001 l] ISOll-01-03-13-002 pl EA EA EF ISOll-01-03-13-004 ISOll-01-03-13-005 eim ETETETETE: ISOll-01-03-13-007 EE ISO11-01-03-13-008 E----a -- A-- ISOll-01-03-13-010 eS ISOll-01-03-13-011 ee LE[E215] ISOll-01-03-13-013 a rol I EE ISOll-01-03-13-614 I---- EE ISO1%01-03-13-016 EE Tme Eml se [EaAlFF aEelEA alEsA] ISO1%01-03-13-017 CGMN-MW07-0-140113 CGMN-MW07-DB-140113 Average %RPD SamplelSample Dup CGMN-MW12-0-140116 CGMN-MW12-DB-140116 Average %RPD Sample/Sample Dup CGMN-MW13-0-140114 CGMN-MW13-DB-140114 Average %RPD SamplelSample Dup CGMN-MW16-0-140114 CGMN-MW16-DB-140114 Average %RPD SamplelSample Dup CGMN-MW101-0-140115 CGMN-MW101-DB-140115 Average %RPD Sample/Sample Dup CGMN-MW104-0-140115 CGMN-MW104-DB-140115 Average %RPD Sample/Sample Dup 3.01 2.75 2.88(2) 9.0 327 297 312 9.6 9.69 9.90 9.80(z) 2.1 43.4 42.3 42.9(2) 2.6 1590 1430 1510 11 194 210 202 7.9 0.407 0.373 0.390(2} 8.7 682 653 668 4.3 9.65 9.90 9.78(2) 2.6 93.1 88.9 91.0(=~ 4.6 80.0 78.7 79.4 1.6 35.1 35.0 35.1 0.29 <0.100 <0.100 <0.100(2) NA 85.4 78.8 82.1 8.0 1.12 1.27 1.20(2) 13 41.1 38.8 40.0I=) 5.8 25.7 25.1 25.4 2.4 7.34 7.65 7.50 4.1 0.0508 0.0386 0.0447(2) 27(3) 14.1 12.1 13.1 15 0.857 1.08 0.969(2) 23(3) 5.51 5.52 5.52(=) 0.18 383 413 398 7.5 14.4 13.9 14.2 3.5 0.104 0.104 0.194(2) 0.0 129 113 121 13 3.02 3.14 3.08(2) 3.9 51.0 55.2 53.1(2/ 7.9 160 158 159 1.3 4.22 4.27 4.25 1.2 ISOll-01-03-13-019 CGMN-MW105-0-140114 56.0 68.5 6.48 12.4 152 ISOll-01-03-13-020 EpEeEl I PE ISOll-01-03-13-022 ISOll-01-03-13-023 e EEE TSee TTEaTa E[ET TE] ISOll-01-03-13-025 ER ETE TEE] ISOll-01-03-13-026 CGMN-MW105-DB-140114 Average %RPD Sample/Sample Dup CGMN-MW108-0-140114 CGMN-MW108-DB-140114 Average %RPD Sample/Sample Dup GGMN-MW11043-140114 CGMN-MW110-DB-140114 Average %RPD Sample/Sample Dup 55.1 55.6 1.6 48.9 54.2 51.6 10 177 181 179 2.2 68.0 68.3 0.73 171 166 169 3.0 247 248 248 0.40 5.81 6.15 11 18.1 15.9 17.0 13 884 81.7 85.1 7.9 12.8 12.6 3.2 4.19 4.06 4.13 3.2 202 18.6 19.4 8.2 152 152 0.0 33.2 33.7 33.5 1.5 120 12.2 12.1 1.7 E CZr en= NA = Not Applicable T BRERR (1) Samples v,~re reported by external standard calibration, except where noted. The analytical method uncertainties associated with the reported results by external standard calibration are as follows: PFBA + 19%, PFOA + 16%, PFBS + 14%, PFHS + 16%, and PFOS + E Em mm or e 20%. e e (2) Samples w~re reported by internal standard calibration. The analytical method uncertainties associated with the reported results by internal standard calibration are as fellows: PFBA _+ 14%, PFOA_+ 16%, PFBS _+ 18%, PFHS _+ 28%, and PFOS _+ 16%. (3) The sample/sample dup %RPD did not meet the method cdteria of <20%. eiPAGE 3 OF 39 33663300..00008855 3M MN01596034 Table 1 continued. Sample Results Summary (1) 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-13 3M LIMS ID a ISO11-01-03-13-031 r(E mmenaE erh e ISO11-01-03-13-032 Sample Description CGMN-PW09-0-140115 CGMN-PW09-DB-140115 Average %RPD Sample/Sample Dup 5.00 4.52 4.76(~) 10 Concentration {n~l/mL) 1.40 1.26 1.33(~ 11 0.167 O. 178 0.173(~) 6.4 0.117 O. 101 0.109(~) 15 2.29 1.97 2.13(~) 15 IS011-01-03-13-034 I SO 11-01-03-13-035 I m EE s eS d lI d dhry IS011-01-03-13-037 [-- TT : I SO 11-01-03-13-038 CGM N-PW10-0-140122 CGMN-PW10-DB-140122 Average %RPD Sample/Sample Dup CGMN-MW14R-0-140113 CGMN-MW14R-DB-140113 Average %RPD Sample/Sample Dup 4.03 4.77 4.40(2) 17 300 289 295 3.7 0.223 0.200 0.212(2~ 11 137 141 139 2.9 0.254 0.268 0.261~) 5.4 17.3 17.7 17.5 2.3 0.0426 0.0543 0.0485~2~ 24~3~ 12.1 12.4 12.3 2.4 0.121 0.126 0.124 4.0 25.0 24.8 24.9 0.80 E cESEeierr m esap r FrEeAsR, oE NA=NotApplicable n, (1) Samples were reported by external standard calibration, except where noted. The analytical method uncertainties associated with the reported results by external standard calibration are as follows: PFBA + 19%, PFOA + 16%, PFBS + 14%, PFHS + 16%, and PFOS + 20%. (2) Samples were reported by internal standard calibration. The analytical method uncertainties associated with the reported results by internal | EEE standard calibration are as fellows: PFBA _+ 14%, PFOA _+ 16%, PFBS + 18%, PFHS _+ 28%, and PFOS + 16%. (3) The sample/samole dup %RSD did not meet the method cntena of <20%. BrreSr RT 22 MMeetthhooddss --AAnnaallyyttiiccaall aanndd PPrreeppaarraattoorryy 2.1 Methods Analysis was completed following 3M Environmental Laboratory method ETS-8-044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis". Table 2. Target Analytes Target Analytes [Pumoutum|merogac|soouecewirn| [Petco soacarsy Perfluorobutanoic Acid (C4 Acid) Perfluorooctanoic Add (C8 Acid) |Potomtuanesstonsio 4Surat) | pres| umew | Perf]uorobutanesulfonate (C4 Sulfonate ) [Putoshomesstoran Cosme) |pevs | uoew | Penluorohexanesulfonate (C6 Sulfonate) [PutonomensotoCosutoratey | pros| mewr+Boches | PerfluorooctanesL=lfonate (C8 Sulfonate) Acron~ | pro | PFBA PFOA PFBS PFHS PFOS Reference Material Structure tmewrBmched | Linear Linear + Branched Linear Linear Linear + Branched 22.22 SSaammppllee CCoolllleeccttiioonn `E R SampleswerecoleocnJtaneuadry 13, 14, 15, 16, and22P ,2014 in NaigeneTM (nigh-density polyethylene) bots Samples were collected on January 13, 14, 15, 16, and 22, 2014 in NalgeneTM (high-density polyethylene) bottles A TEE A h ED prepared at the 3M Environmental Laborstory. Prior to sample collection, bottles designated for field matrix spikes A were spiked in the laboratory with a known volume of an appropriate matrix spiking solution containing the analytes of interest. Collected sample bottles were returned to the laboratory on ice on January 17, 2014 and at room temperature on January 23, 2014. 33663300..00008866 anPAGE 4 OF 39 3M MN01596035 REPORTING 1501101 50.13 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-13 2`2S.3a3mpleSScaaommncpeplnlieeraPPtrornoesppawaerrraaetteiioxopnnected 0 ange from <0.025 ng. 101000 nm. Sampirglocationsthal were. elSeoxxacppmaeetcpcitolteeendsdcho1to0antchneaawnvveteerraocctioooennxnccpseeewnncttiereaaredttiootennoxph<<ea11cv00te0e0dcnnotggnoi/cmemranLLtnrwwgaeeetrrifeeroonaamn>na1a<l0ly0y0z.z0een2ddg5bbynygii/nnwmtteeLerrmntoaoaalln>ssa1tila0ayn0rzd0ceaanrdrdgdb/mccyaaLelli.xbbtrrSaeatamtioamilnnpsalaitnnnaagalnlydylosasicrissad..ticoSSanalasrmmtaphptialiintnogwgn ere analysis. locations analysis. The folowing sampe that were expected to The following sample reparation procedureswere folowedforeach have concentration >100 ng/mL were analyzed preparation procedures were followed for each type of anayss. by external standard type of analysis. calibration rIInnettmeeormnvaai)lnsgsttaaann0dd.aa4rrdmd ccLaall_ibbrraaattilooonnfqaathnnueaayolwysosstlis:l: mSSiaaxmmepdpllseeassmaapnnlaaollyyazzneeddddoibyuyntninegtemrwnaialtsshttaa0nn.dd4aarmrddLcocafaslmiobreraattthiooannnweeer(redeapuptrreoepnpaafrreeaddcbbtyyofo2r) removing a 0.4 mL aliquot of the well mixed sample and diluting it with 0.4 mL of methanol (dilution factor of 2). DwDuaursriinnlggotthhdee pp0rreotpphaaerralatatiibooonnraootffottrhhyeceollanabtborororalattsooraryymcpcooennsttroo(llnossmaaimmnpaplllescs,o,naacnnonaatliaqluuiootnlofoffaa1ssereppmaarr)aat.tee iiTnnrfteeerrnnsaaallmssettaianonddbaaarrddttpsspkiwikiennrggosssooilukoteiondn wwcwoiialtlhhsecaaatndinodniien.ntdteeTrrtnohnaaetllhlsseattbaaloannrbddaotaaorrrarddytommcryxixocaaoltnatronsnloaosmmmaipinmlnaeaplslleccwsooenn(rcnceeeonnmttthrrianeatnatiilodocnnloooneffcd1e1 nwnntirggah/mmtiomLLnepptorrihfioo1arrnotnoagi/lbbnmeetiLinhn)geg. assTeanhnmtetestooamtmthhpeaflefiaebldadnostfftoloterrnhsssewaasmmeeaprpmelpleelsrepsik.ed collection. The laboratory control samples were then diluted with methanol in the same manner as the samples. ExaEtnxaotleymrsnaisal.l sstStaaannmddpaalrreddsccaaollqibburriaanttinoognn aaann1aal:yl1ys0sidsisl::uSStaaommnpwpleleersseaanpnaralelyypzzaeradedbdbybyyeexdxittleeurmtniaanlgl ss1ttamannLddaacrfrddaccwaaelliblbrkraamttiiiovonendrrseeaqqmuuipirreleded ddwilhuution9nmppLrroioifro(tro0 analysis. Samples requiring a 1:10 dilution were prepared by diluting 1 mL of a well-mixed sample with 9 mL of omfetmheatnhoal.nolSamples requiring 1:50 dluonwere peared by dling 0.2 mL ofa welkmixed samplevith 98 mL. methanol. Samples requiring a 1:50 dilution were prepared by diluting 0.2 mL of a well-mixed sample with 9.8 mL of methanol. 22ll.44sampAAlnnoasallayynssdiiassualty cotrl sampos wero analyzedforfve target analytes using high perormanc uid cAcchhhlrlrvosoomammamaatpttooolgeggrsrraaaappnphhdnyyy/qgttauranaanddldiieteyemnmctommpnaratrsosogsslrsssaappmme,eccpattlrnreoodsmmtewehteterrryyesp((eaHcHniPPafLiLlycCGzm/eMMadSSsIfs/oSMr)aSfi.nv).se ttPPaoerenrgrtsetiitnnaaeennnnatatllniyynsztseietsrrduuuammsreeiennngtdtepphsaiagcrrhraabmmpeeeetdrteefirornsrstm,h, 1tahnetcaellbiqallueiuqsiddubidelow. chromatography gradient program, and the specific mass transitions analyzed are described in the tables below. DcDuueetutootthheeronnfaamtrutrueuto(e~frfetthheeiensssoaammmepcrlpseloe,,fehttheheewwaiibddceerraraalonnrggyee'osoffaccnooanncceeesnnttrroafatteioornnesssffo,ouunntdhd iinnsttohhweeassraaommppulsleee,,daafnnoddrptthrhoeeceeennsvvsiiirrnoognnmmheeen.nttaall oaP`aencnccaaeullysyrstrtiaeccraanlylc.erreesoAsuuflllmttmssuaiilnstiupnnalooelttaiasnbobellmgeerettaorostccoooonnfnstishsiaestrtoeelannbpttolyeyrariintnomttereyegg'rrsdaattaeefnoattlhhloyeewteiaansnnagaloyltfythtiineicctaapelrlreoppsceetea,adkktu,h,remmeassanonouftuuawatlail rniiennettdeueggsirneraadmttieiofootnnrhooopffdrotthEncoeTeaSsan-sna1ilna2ygl.yt0titi1hcc0eaa.ll ppTeehaaekk. is is pccnoroenoncscesieisssssttsaeernrnycce.yyquAoorlfflettmdhheeafonllraauabbaloollrraimantattooenrrguyyr'a'assltiiioninnnttetseegggarrraraaetttioiipnooennsrissf,oeetrmnnesseuurdrereevfoddilelrtowhoworofuinuggmgahhtnhttuehhaeeplrrtroiaacnienendignggugaretoosfofroblasubobtrloyinartaeohtdoreryiynQAppmeeUerr,ssthooaonnndnndeewEllh,TethShre-ee1p2po-ne0eee1cr0err.seesvvTiaieherwewy hproorceosvsewreoqfuimreadnufoarlaillnlmoagrnauiaolnisntbeygrlaatbioonrast,otrhyemraenviaegwoomfomntanual integrations by the QAU, and where necessary the review of manual integrations by laboratory management. TThhee ffoollloowwiinngg aannaalylyttiiccaall urunnsswweerree uusseedd ttoo ggeenneerraatel tthheerreeppoorrtteeddrreessuultltss:: 124/14 -ntemal s1/24p/1f4or-eInPtFe)BrnAa,l standard calbraton; PsFtaOnAd,arPdFBcSa,librPaFtiHoSn,; MMP WWO0T7,F a, MnMWdW1sO 1u33r,,ogMMaS WWt1e16s6.,, PWOS, PW09, Rinsaate Rinseate and and Trp Trip Blanks Blanks (sample (sample and and iow low spike) for PFBA, PFOA, PFBS, PFHS, PFOS and surrogates. 1s1p2/2i88k//e11f44or-- EEFxFxttBeeArrnn,aalPlsFsttOaaAnn,ddaaPrrFddBccSaa,fliobPrrFaatHtiooSnn,;; aMMnWWd11P22R,,OMMSW;WAM100W11I,,4MMRWWAf1o10r044,P, FWMO1AW,01P50F5,B, SMM,WW1P1F00H88S,,,MMaWWn1d1l 10P0F,,OaaSnn.dd Trip "rrip Blank Blank high high spike for PFBA, PFOA, PFBS, PFHS, and PFOS; MW14R for PFOA, PFBS, PFHS, and PFOS. 1/30/14 - Internal standard coloration; PWD for PFBA, PFOA, PFS, PFHS, POS and surrogates. 1/30/14 -Internal standard calibration; PW10 for PFBA, PFOA, PFBS, PFHS, PFOS and surrogates. 1131/1-4 External standard caibration; MWR for PFBA. 1/31/14 - External standard calibration; MW14R for PFBA. 33663300..00008877 Prcescrs PAGE 5 OF 39 3M_MNO1596036 3M MN01596036 A 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-13 Table 3. nstrumnt Parameters. Table 3. Instrument Parameters. [i|meen ma ts| Instrument Name ETS Buster Liquid Chromato~lraph Lormpmaaros =| eeowr | Analysis Method I ---- TR-- Analysis Date [oon| gemichusrmroms, | Guard column [a|rpus mictusrmo rmms,n| Analytical column [itonvoone | omwoa | Injection Volume [tes pment | rpmsion | Mass Spectrometer I-- ---- Ion Source A~ilent 1100 ETS-8-044.1 1124114, 1/28/14, 1/30/14, 1/31/14 Betasil C18 (4.6 mm X 100 mr'n), 5 Betasil C18 (4.6 mm X 100 mm), 5 10, 30, 40 pL Applied Biosystems API 4000 Turbo Spra), [amas Polarity Sof~Nare 1 amie] Negative Analyst 1.6.1 Table 4. Liquid Chromatography Gradient Program. Table 4. Liquid Chromatography Gradient Program. Comms] ETS-8-044.1 Analysis Step Total Time Flow Rate Percent A Percent B Number (min) (!~L/min) (2 mM ammonium acetate) (Methanol) CoTwTmTw T--0--] 0 0.00 750 97.0 3.0 CwTwTwoTs] 2TaTmTmoTwo| 1 0.50 750 2 4.00 750 97.0 70.0 3.0 30.0 Co TwTmTmTw] 3 6.00 750 70.0 30.0 Como TmTmTwo] 4 11.0 750 20.0 80.0 Co TmTmo wo] 5 13.0 750 20.0 80.0 Coes me wo] 6 13.5 750 10.0 90.0 I ---- ----T-- 7 16.0 750 10.0 90.0 Cows TmTwo TT 0 --] 8 16.5 750 97.0 3.0 Co TwTwTwo Ta] 9 19.0 750 97.0 3.0 33663300..00008888 rrcescen PAGE 6 OF 39 _Motsesos7 3M MN01596037 Table 5. Mass Transitions Table 5. Mass Transitions A 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-13 Com Analyte PFBA |e PFOA Mass Transition Internal Standard (1} QIlQ3 we | fopm 213/169 som] 4131369 am] reseron 413/219 II:~C4]-p FBA [13Cs]-PFOA Mass Transition [ m--| Q11Q3 2171172 421/376 ow1 PFBS [me Eo2w 2] PFHS | [re e = a2n2] PFOS 413/169 299/80 299/99 399/99 399/80 499/99 499/80 corms come Foros [13C~] PFOS 303184 402/99 507/80 499/130 IS Sc S---- 216/172 [13C4]-P FBA 217/172 IE TS ------ 417/372 [I~C~]-PFOA 421/376 [reposTomo 1 eros 1 som | 503/80 [I~Cs]-PFOS 507/80 St 0 Tr aeor a To Se do Dwell time was 50 or 100 msec for each transition. The individual transitions were summed to produce aan 0 wevaet a "total ion chromatogram" (TIC), which was used for quantitation. ) mtn tance sis ro her onto sors. (1) Internal standard was not used for the samples analyzed by solvent dilution external standard a calibration. 33 DDaattaa AAnnaallyyssiiss 31 Calibration 3.1 Calibration Soon luton analy using tama standardcarson: Samp wer anayzed or snes agit a Solvent dilution analysis using internal standard calibration: Samples were analyzed for all analytes against a a malhd site scape tema sancard clan i, Calarndrae eirsJoPAn by SIG matrix-matched stable isotope internal standard calibration curve. Calibration standards were prepared by spiking Koo amof soe ck sos utons mo Sof 050 metvantabreoagrenstwaekyer Tne cao known amounts of stock solutions into 50 m L of 50:50 methanol:laboratory reagent water. The calibration Sanda cone an emo tncard iat a nol concenra0b3onmoL Catbrton sandr standards contained an internal standard mix at a nominal concentration of 0.5 ng/mL. Calibration standards rraannggiinnggffrroomm 00..00112255nnggi/mmL.Lttoo5500 nnggi/mmLL ((nnoommiinnaall))wweerree aannaallyyzzeedd ((00..00112255nngg//mmLLttoo 1100 nnggi/mmLL ((nnomoimnail)fnfooarrtlthh)ee SRE Lowor ign portsmay hveboon debi 0 motmaccrea. Ausra, Tweihed, carson SRSs). Low or high points may have been disabled to meet method criteria. A quadratic, 1Ix weighted, calibration Ce vf oe lard pk a oa ove In hal avr pk ara GS as 0s 10 ho curve of the ratio of the standard peak area counts over the internal standard peak area counts was used to fil lhe ta each aona. Th Gtavers toca NUN 20 ung hefin process Calasaing ns sans data for each analyte. The data were not forced through zero during the fitting process. Calculating the standard ConcanvatonsUs ha peak aaasa 0ToSatCASALL Cue Cored 20oOIF 6a00CSvYe concentrations using the peak area ratios and the resultant calibration curve confirmed accuracy of each curve pontpoint. Soven diuon analy using arma standard cacao: Samples war analyzed gaanrosma sandard Solvent dilution analysis using external standard calibration: Samples were analyzed against an external standard Caltrabon cue. Calbaton sannaodproprre by pcg Known amooufnttocsk soir io80ml calibration curve. Calibration standards were prepared by spiking known amounts of the stock solution into 50 mL GF9010metro: aborMILiovante Garton sda ang fom 0.1 gLa 100 (roma) of 90:10 methanol: laboratory Milli-QTM water. Calibration standards ranging from 0.1 ng/mL to 100 ng/mL (nominal) ore ana Aquadote Xgl carnv tfhostanndard pro d co wie sued 4sne were analyzed. A quadratic, 1/x weighted, calibration curve of the standard peak area counts was used to fit the nao22h ana Low hgh POSwere sane 0 eet method cr.Ths data arsno {rc ugh data for each analyte. Low or high points were disabled to meet method criteria. The data were not forced through ZoroGuhnefigng srocess. Casheasanldr concenkalons wn 1h pes ares counts and zero during the fitting process. Calculating the standard concentrations using the peak area counts and the estan cabratonau confimedacaracy of och cae po resultant calibration curve confirmed accuracy of each curve point. Forbob method of nays, each curvepitwas quate stih ovgeralcalbaion cuanrdrevvieew for For both method of analysis, each curve point was quantitated using the overall calibration curve and reviewed for Scrat. Mth caoraion accra qurana 1004255 (1002307 or ne lowest oun por were it accuracy. Method calibration accuracy requirements of 100+25% (100+30% for the lowest curve point) were met {oral mb. Tho conan coaio(1 grotr an 0995 oral race. for all analytes. The correlation coefficient (r) was greater than 0.995 for all analytes. 33663300..00008899 orcercen PAGE 7 OF 39 a_Motsesoss 3M MN01596038 3M ENVIRONMENTAL LABORA TORY a maEosCrs seat REPORTNO. IS011-0!-93-13 3.2 System Suitability A calibration standard was analyzed four times at the beginning of the analytical sequence to demonstrate overall system suitability. The acceptance criteria for system suitability samples of less than or equal to 5% relative standard deviation (RSD) for peak are counts or peak area ratio and retention time criteria of less than or equal to 2% RSD were met for all analytes with the following exceptions: 1/24/14 Analysis: The system suitability area counts exceeded 5% for PFBA (7.7%), PFBS (6.5%), and PFHS 6(63.3%%).). 111/3300//1144 AAnnaallyyss'iss:: TThhee ssyysstteemmssuuiittaabbilliytyaarreeaa ccoouunnttss eexxcceeeeddeedd 55%% PPFFBBAA ((77..33%%)),, PPFFBBSS ((55..66%%)),, aanndd 1"3CC.4P-PFFOOAA ((77.11%%).). Se -------- A method deviation is included with the raw data. EEEEl ere _--" 3.3 Limit ofQuantitation (LOQ) The LOQ as defined in method ETS-8-044.1 is the lowest non-zero calibration standard in the curve that meets linearity and accuracy requirements and for which the area counts are at least twice those of the appropriate blanks. The LOQs associated with the sample analysis are listed in the Table 6 below. eT Table 6. LOQ Analyte LOQ, ng/mL !1) LOQ, ng/mL (2) LOQ, ng/mL(1) LOQ, nglmL 1124/14 Analysis 1/28/14 Analysis [eon 1 oao[om | oom | om | PFBA 0.200 0.250 [pron 1 oowo |oss |ow | wa | PFOA 0.0480 0.0958 [ees 1 ow |ow | ooo | wa | PFBS 0.100 0.100 [ews T omso |ow | omw | wm | PFHS 0.0250 0.100 lHSea so1 m omeToor 1 ome | wm | PFOS 0.0232 mt NA - Not Applicable s (1) A dilution factor of 2 was applied to the LOQ. 0.0927 1~14Anal~is 0.0~0 0.0~0 0.0~0 0.0~0 0.0~2 1/31/14 Anal)sis 0.250 NA NA NA NA (2) A dilution factor was not applied to the LOQ. 33..44 CCoonnttiinnuuiinngg CCaalliibbrraattiioonn S RRRE A ene, During the course of the analytical sequence, several continuing calibration verification samples (CCVs) were analyzed to confirm that the instrument response and the initial calibration curve were still in control. All reported results were bracketed by CCVs that met method acceptance criteria of 100%_+25%. A mEmEm -- 33..55 BBllaannkkss Three types of blanks were prepared and analyzed with the samples: method/solvent blanks, field/trip blanks, and sampling equipment blanks. Each blank result was reviewed and used to evaluate method performance. The method/solvent blanks were used to determine the LOQ for each analyte. Oy n-- r -- 3.6 Lab Control Spikes (LCSs) Low, mid, and high lab control spikes were prepared for the target analytes and analyzed in triplicate. LCSs EE Er prepared for internal standard calibration analysis were prepared by spiking known amounts of the analytes into 10 mL of laboratory reagent water to produce the desired concentration. The LCSs were then diluted in the same I FL EE R SrrL a A manner as the samples. LeSs prepared for external standard calibration analysis were prepared by spiking known amounts of the analytes into 1.0 mL of laboratory reagent water and 9.0 mL of methanol to produce the desired e concentration. Method ETS-8-044.1 states that the average recovery of LCSs at each spiking level must be within 80%-120% with a RSD <20%. All LCS samples met criteria with the following exceptions: SS 1/24/14 internal standard analysis: The average recovery of the mid set of LCS for PFHS was 128%. * 113/300//1144 iinntteermnaall ssttaannddaarrdd aannaalylyssisis:: TThhee aavveerraaggee rreecocveorvyooefftrthhyee lloowwsseettooff LLCCSS ffoorr 1"3CC-3P-PFFBBAA wwaass 112288%%.. anPAGE 8 OF 39 33663300..00009900 3M MN01596039 REPORTING 1501101 50.13 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-13 AALCmmSsetathmhopdleddsaevvwiiaoatiriooonn usiissncewindcilunidtehed hdweittherttmhhieenarrtaaiwwonddoaafttaaheffoorrantnaholoyssteeicaLLlCCmSSesstththhoaadtt uddiniddcencrtotatimmneteyeetit mmseaetcthhtoooddn aa3.7cccceeopfptthaaonnccreeepccorerittrearia.. AAlll LCS samples were used in the determination of the analytical method uncertainty in section 3.7 of the report. TThheo ffoollloowwiinngg ccaallccuullaattiioonnss wweerree uusseedd ttoo ggeennoerraattee ddaattaa nin TTaabbllee 77.. 108Parc Reser -CSooledCoCncoannnosn.t. LCS Percent Recovery Calculated Concentration * 100% 8pike Concentration Loss antidovbtont crepes 1. LCS% RSD standard deviation LCS replicates. 100% average LCS recovery TTaabbllee 77.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuullttss.. Erseons ETS-8-044.1 ore suc Internal standard ar calibration hess 44 Analyzed 1t24114 PFBA Lab ID Spiked Concentration fn1lmL) Calculated Concentration (n1/mL) %Recover~ hea PFOA (Linear -~ Branched) Spies Casa Spiked Conconraion | Concammion Concentration Calculated Concentration (n~l/mL) (n1/mL) %Recover~ LCS-140122-1 LCS-140122-2 gam LCS-140122-3 [memgoewgso| Average 4- %RSD 0.198 <0.200 NA 0.190 0.211 111 0.198 <0.200 NA sm [smn] | ow |x 0.198 <0.200 NA wa | esserx | NA 0.190 0.190 0.181 O. 178 99.8% -+ 9.7% 95.1 93.4 LCS-140122-4 9.92 11.7 118 9.50 11.4 120 LCS-140122-5 9.92 10.9 110 [average evmso| LCS-140122-6 Average _+ %RSD 9.92 wrwesaw 12.1 117% + 5.2% 122 9.50 7 9.50 10.7 wewesw 11.8 119% + 5.1% 112 124 | LCS-140122-7 39.6 43.4 110 38.0 LCS-140122-8 39.6 40.5 102 wes ozo 0 LCS-140122-9 39.6 44.2 112 [awogeesmso| owweamn [7 Average %RSD 108% --. 4.9% 38.0 38.0 NA et picati NA = Not Applicable 1) LCS+ gece 8 tos ccc cr of 002204. (1) LCSs average recovery did not meet acceptance criteria of 100 + 20% 40.0 105 37.3 ws or 40.6 ewes] 103% -+ 4.4% 98.3 107 33663300..00009911 Prceaces PAGE 9 OF 39 3M_MNO1596040 3M MN01596040 REPORTING 1501101 50.13 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-13 TTaabbllee 77ccoonntitinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuultltss.. Erssont ETS-8-044.1 pis Intemal standard calibration Analyzed 1t24114 PFB8 Lab ID Spiked Concentration (nglmL) Calculated Concentration (ng/mL) %Recovery Spiked Concentration (ng/mL) PFHS Calculated Concentration (ng/m L) %Recovenj LCS-140122-1 LCS-140122-2 -- esos [Avempoewmso| LCS-140122-3 Average 4- %RSD wes oa LCS-140122-4 esos LCS-140122-5 Les ome [mvemgeswgso| LCS-140122-6 Average 4- %RSD 0.198 oi0.198 0.198 oe9.92 ose9.92 os-- 9.92 0.174 0.200 ow0.144 wawsen 87.2% -+ 16% 11.8 9.76 omeseme 10.5 107% -+ 9.2% 87.7 0.198 0.254 128 101 ns oi oms w 72.9 | 2 menwrs Ee) | 118 ox n2 = 98.4 | ry wswsrao1wn 2 | 106 0.198 0.237 120 0.198 0.205 103 117%_+11% 9.92 9.92 9.92 13.7 138 12.2 123 12.1 122 128% -+ 7.0%(1) LCS-140122-7 39.6 LCS-140122-8 39.6 [awmgoswmso| LCS-140122-9 Average 4- %RSD 39.6 44.6 39.3 woewesen 41.4 106% 4- 6.6% 113 39.6 42.3 107 99.2 39.6 46.3 117 | wewees. | 105 39.6 48.2 122 115% 4- 6.6% ETS-8-044.1 I ntemal standard rn calibration esa ava Analyzed 1124/14 Lab ID o PFOS (Linear + Branched) Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery LCS-140122-1 0.184 0.188 102 LCS-140122-2 0.184 0.212 115 cormsLE[=] LCS-140122-3 O. 184 0.208 113 [Average -uso| 0% 6% Average 4- %RSD 110% + 6.4% LCS-140122-4 = LCS-140122-5 LCS-140122-6 Average 4- %RSD 9.20 10.7 117 EEE 9.20 9.20 9.45 103 10.2 111 110% 4- 6.4% LCS-140122-7 36.7 40.9 111 wes ozs (= =e) LCS-140122-8 LCS-140122-9 36.7 36.7 39.0 106 39.3 107 Average _+ %RSD 108% _+ 2.4% N1A) tLCSspvtrgoaote moc ecspo nsrve oef 00y 2%. NA = Not Applicable (1) LCSs average recovery did not meet acceptance criteria of 100 _+ 20% 33663300..00009922 encer00r% PAGE 10 OF39 3M_MND1596041 3M MN01596041 REPORTING 1501101 50.13 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-13 TTaabbllee 77ccoonntitinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuultltss.. Erssont ETS-8-044.1 pis Intemal standard calibration Analyzed 1t24/14 ConSTcoeabrneairton||| CoCnlcoogancimaten Lab ID tsozr | own oz LCS-140122-1 some | ow oz LCS-140122-2 sums | ow oz LCS-140122-3 [Average eso| es2on Average 4- %RSD Spiked Concentration [ng/mL) 0.197 0.197 0.197 I~C3-PFBA Calculated Concentration (ng/mL) 0.231 0.221 0.231 115% 4. 2.5% co. %Recovery ww117 2112 a117 Sovos | Coeusoa Spiked Concansion| Concanaion Concentration ng) fin) < (nglmL) ore oz 0.198 ore oz 0.198 [ ose eoa z s 0.198 13C4-PFOA Calculated Concentration (ng/mL) 0.252 0.214 0.214 114% 4. 9.6% %Recovery 127 108 108 LCS-140122-4 1.97 2.34 119 1.98 2.29 116 wes ue 10s LCS-140122-5 1.97 2.11 107 1.98 2.43 123 LCS-140122-6 1.97 2.14 108 1.98 2.39 121 Average _+ %RSD 111% + 6.0% 120% + 3.0% ETS-8-044.1 Internal standard calibration Analyzed lJ24114 Lab ID Spiked Concentration (nglmL) ~3C4.PFOS Calculated Concentration (nglmL) %Recovery LCS-140122-1 0.189 0.222 117 LCS-140122-2 0.189 0.225 119 corms ==] LCS-140122-3 0.189 0.235 125 [Avw | agem: owsw amemso| Avera~le _+ %RSD 120% _+ 3.5% LCS-140122-4 1.90 2.27 120 we= s ue[2s]zns ] LCS-140122-5 1.90 2.13 112 LCS-140122-6 1.90 2.25 118 Average + %RSD 117% 4. 3.6% N1A) LCaSttempieat mgaotmrocceostcarsocrevaofe00 2y. HA = Not Applicable (1) LCSs average recovery did not meet acceptance criteria of 100 + 20% 33663300..00009933 excEn1or PAGE 11 OF 39 3M_MNO1596042 3M MN01596042 REPORTING 1501101 50.13 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-13 TTaabbllee 77ccoonntitinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuultltss.. Erssont ETS-8-044.1 nen External standard calibration Analyzed 1t28114 PFBA Lab ID Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery PFOA (Linear -~ Branched) Spiked Concentration (ng/mL) Calculated Concentration (ng/m L) %Recovenj LCS-140128-1 LCS-140128-2 -- rode [Avempoewmso| LCS-140128-3 Average 4- %RSD LCs oa LCS-140128-4 esos LCS-140128-5 Les ome [Average + ues | LCS-140128-6 Average _+ %RSD 1.00 io1.00 1.00 010.0 0010.0 10010.0 0.980 0.954 oar opwwewsn 0.837 92.4% 8.2% 0610.6 0310.3 om 03% 36% 9.87 103% -+ 3.6% 98.0 0.958 0.923 96.3 95.4 a oss om: ss 83.7 | 0 aowssIa] Ex | 106 0 oz a3 103 sor Le L wwmoniown s | 98.7 0.958 0.958 9.58 9.58 9.58 0.890 0.832 92.0% --. 5.2% 9.52 9.32 9.42 98.3% -+ 1.0% 92.9 86.9 99.3 97.3 98.3 LCS-140128-7 39.8 LCS-140128-8 39.8 [awngeswmso| LCS-140128-9 Average 4- %RSD 39.8 35.4 37.6 oasweasm 38.6 93.5% -+ 4.3% 89.1 38.2 33.4 87.4 94.5 38.2 33.9 88.8 | wena | 97.0 38.2 36.6 90.6% --. 4.9% 95.7 ETS-8-044.1 Emasti External standard Catenin calibration essa 124 Analyzed 1128114 Lab ID 5Spiked Concentration (ng/mL) PFBS nd Calculated Concentration (ng/mL) g %Recovery nd) Spiked Concentration (ng/mL) PFHS ng) Calculated Concentration (nglmL) = %Recovery LCS-140128-1 1.00 0.986 98.6 1.00 1.05 105 LCS-140128-2 Les o=ma[e 1 fous LCS-140128-3 [Avago -vmso| orsieams Average 4- %RSD LCs oa 0 LCS-140128-4 sos 00 LCS-140128-5 Les ome 00 LCS-140128-6 1.00 1.00 10.0 10.0 10.0 1.01 0.929 97.5% -+ 4.3% 10.1 10.1 10.2 101 s]2w ]2 oss a] 92.9 on | m Seo toarzn 101 0 00 01 lol 0 "00 100 102 1.00 1.00 10.0 10.0 10.0 0.905 0.925 96.0% --. 8.2% 10.7 10.1 10.0 90.5 92.5 107 101 100 Average 4- %RSD Cs oT ws LCS-140128-7 Lesoae wr LCS-140128-8 39.8 39.8 101% + 0.57% 34.9 36.9 8716 92.7 2 39.8 wo 39.8 103% + 3.7% 36.2 37.9 91.0 95.3 [Avengorsmso| LCS-140128-9 Average _+ %RSD 39.8 oawesson 39.2 92.9% 5.9% | eewaam | 98.5 39.8 38.7 97.1 94.50/o --. 3.3% N1A)=iLCtSt+piocragbaiecveny 8 otmoc eceprcs cre of 002%. NA = Not Applicable (1) LCSs average recovery did not meet acceptance criteria of 100 _+ 20% 33663300..00009944 encer20r PAGE 12 0F39 3M_MNO1596043 3M MN01596043 TTaabbllee 77ccoonntitinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuultltss.. Erssont ETS-8-044.1 nen External standard calibration Analyzed 1t28114 Lab ID rere LCS-140128-1 Les omz LCS-140128-2 Les ons LCS-140128-3 PFOS (Linear Branched) Spiked Concentration (ng/mL) ose7 0.927 ower0.927 oszr0.927 Calculated Concentration (ng/mL) om0.880 ose0.842 om0.808 %Recovery 94.9 90.9 87.1 Average 4- %RSD 91.0% _+ 4.3% LCS-140128-4 9.27 8.85 95.4 LCS-140128-5 9.27 8.84 95.4 eLesw ume |Eozlm[= ses LCS-140128-6 9.27 8.98 96.8 [Average -ums | ssa som Average _+ %RSD 95.9% + 0.84% Les rior = LCS-140128-7 36.9 32.8 88.8 esos 9 LCS-140128-8 36.9 34.0 92.1 esos = [avo | mpowowc iesr on mso| LCS-140128-9 Average + %RSD 36.9 92.9% -+ 5.0% 97.9 REPORTING 1501101 50.13 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-13 ETS-8-044.1 Intemal standard BE calibration Anal)'zed 1t30114 Lab ID Spiked Concentration (ng/mL) PFBA Calculated Concentration (ng/mL) | %Recovery en PFOA (Linear Branched) Couitea Spiked Concanmion Concentration Calculated Concentration | (ng/mL) (ng/mL) %Recovery LCS-140130-1 0.198 0.242 122 0.190 0.188 98.9 -- esos LCS-140130-2 LCS-140130-3 E ose ERIEosm IEozsRE 0.198 0.213 108 0.198 0.233 118 0.190 0.190 0.200 105 0.218 115 Average 4- %RSD 116% -- 6.2% LCs iowa 5 LCS-140130-4 esos os LCS-140130-5 9.92 9.92 11.8 119 11.1 112 106% 4- 7.6% 0 wo 9.50 aso om 9.50 11.0 115 9.87 104 LCS-140130-6 9.92 11.0 111 [vemgoswmso| waxes. | TmkEsTn Average 4- %RSD 114% -+ 3.8% LCs omr 2s 0 oo LCS-140130-7 39.6 42.9 108 Les ome we 20 0 LC8-140130-8 39.6 41.6 105 9.50 10.9 115 111%4-5,7% 38.0 41.0 108 38.0 39.0 103 [Average : uso| oes LL oesam LCS-140130-9 39.6 45.7 116 Average __ %RSD 110% --. &2% 38.0 38.9 102 104% 4- 3.1% NA Ht piste NA = Not Applicable 1) LCS+ ageacre 8 otmoc secon crn 00 20%. (1) LCSs average recovery did not meet acceptance criteria of 100 + 20% 33663300..00009955 excEnor PAGE 13 0F39 3M_MNO1596044 3M MN01596044 REPORTING 1501101 50.13 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-13 TTaabbllee 77'ccoonntitinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuultltss.. Erssont ETS-8-044.1 pis Intemal standard calibration Analyzed 1t30114 PFB8 Lab ID Spiked Concentration (nglmL) Calculated Concentration (ng/mL) %Recovery Spiked Concentration (ng/mL) PFHS Calculated Concentration (ng/m L) %Recovery LCS-140130-1 0.198 0.228 LCS-140130-2 -- esos [Avempoewmso| LCS-140130-3 Average 4- %RSD esos LCS-140130-4 esos LCS-140130-5 Les uo [vemgeswgso| LCS-140130-6 Average _+ %RSD 0.198 oi ous 0.198 o-- e owswarse 9.92 ose9.92 os vimesomn 9.92 0.182 0.176 98.5% -+ 1 ~/0 11.0 11.0 11.1 111%_+0.52% 115 0.198 0.182 92.2 91.7 0.198 0.261 132 er oi ome m 86.7 0.198 0.238 120 TT wexews | 115% -+ 18% 2 111 9.92 ox 0s 111 9.92 ry PS 112 9.92 11.3 114 10.4 105 10.5 106 | ose. | 108% _+ 4.6% LCS-140130-7 39.6 LCS-140130-8 39.6 [awngeswmso| LCS-140130-9 Average 4- %RSD 39.6 38.4 37.9 orowszen 40.0 97.9% _+ 2.8% 97.1 39.6 39.9 101 95.6 39.6 44.0 111 | essen | 101 39.6 40.7 103 105% -+ 5.0% ET8-8-044.1 Intemal standard E essaE 04] calibration Analyzed lJ30/14 re o | PFOS (Linear + Branched) Lab ID Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery LCS-140130-1 0.184 0.192 105 -- esos[oi= e = oz ] LCS-140130-2 O. 184 0.207 113 LCS-140130-3 0.184 0.211 115 Average 4- %RSD 111% -+ 4.8% LCs iowa I no ) LCS-140130-4 esos om 0s ve LCS-140130-5 9.20 9.20 11.0 120 10.9 118 LCS-140130-6 9.20 10.8 117 [ve|mg--ows exew rwmso| Average _+ %RSD 118% -+ 1.3% Csr = no LCS-140130-7 36.7 41.3 112 Les ome r wor LC8-140130-8 36.7 40.7 111 [Average : uso| 0% 19% LCS-140130-9 36.7 39.5 108 Average + %RSD 110% _+ 1.9% N1A) HLCtS+paisgteeacre 8 otmoc secon crn 00 20%. NA = Not Applicable (1) LCSs average recovery did not meet acceptance criteria of 100 + 20% 33663300..00009966 exer PAGE 14 OF 39 3M_MNO1596045 3M MN01596045 REPORTING 1501101 50.13 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-13 TTaabbllee 77ccoonntitinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuultltss.. Erssont ETS-8-044.1 pis Internal standard calibration Analyzed 1t30/14 ConSTcoeabrneairton||| CoCnlcoogancimaten Lab ID tstomr | own oz6 LCS-140130-1 some | ow 026 LCS-140130-2 sums | ow oz LCS-140130-3 [Average eso| Tas 17 Average 4- %RSD Spiked Concentration [ng/mL) 0.197 0.197 0.197 I~C3-PFBA Calculated Concentration (ng/mL) 0.236 0.246 0.274 128% 4. 7.7%1~) co ConSncoagvno)ssion|| CoCnofceiaunnsa)oiaon < %Recovery ore oz 120 ore om 125 [ voe se ee ox asn 139 Spiked Concentration (nglmL) 0.198 0.198 0.198 13C4-PFOA Calculated Concentration (ng/mL) 0.217 0.230 0.262 11 ~)% 4. 9.9% %Recovery 109 116 132 LCS-140130-4 1.97 2.36 120 1.98 2.22 112 Les ume 10s 2m LCS-140130-5 1.97 2.24 114 1.98 1.96 98.9 LCS-140130-6 1.97 2.20 112 1.98 2.33 118 Average _+ %RSD 115% + 3.6% 110% + 8.9% ETS-8-044.1 Internal standard calibration Analyzed lJ30114 Lab ID Spiked Concentration (nglmL) ~3C4.PFOS Calculated Concentretion (nglmL) %Recovery LCS-140130-1 0.189 0.221 117 LCS-140130-2 0.189 0.207 109 rms EEE LCS-140130-3 0.189 0.238 126 [Avw | agewrc wsrw me mso| Avera~le _+ %RSD 117% _+ 7.2% LCS-140130-4 Le= s ome LCS-140130-5 LCS-140130-6 1.90 2.02 106 EEE no 1.90 2.19 115 1.90 2.08 110 Average + %RSD 110% 4. 4.1% N1A) LCaSttempieat mgaotmrocceostcarsocrevaofe00 2y. HA = Not Applicable (1) LCSs averege recovery did not meet acceptance criteria of 100 + 20% 33663300..00009977 ence150F% PAGE 15 OF39 3M_MNO1596046 3M MN01596046 REPORTING 1501101 50.13 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-13 TTaabbllee 77ccoonntitinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuultltss.. Erssont ETS-8-044.1 nen Extemal standard calibration Analyzed 1t31/14 le| [| Lab ID (eso 00 10s LCS-140131-1 Lesonz 0 oss LCS-140131-2 esos i os LCS-140131-3 [Av|ag--ooe wewev nenmso Average 4- %RSD Spiked Concentration (ng/mL) 1.00 1.00 1.00 PFBA Calculated Concentration (ng/mL) 1.05 0.985 0.803 94.6% _+ 14% %Recovery 105 98.5 80.3 LCS-140131-4 10.0 9.94 99.4 LCS-140131-5 10.0 10.3 103 E esol s z 00 JB]%) LCS-140131-6 10.0 10.4 104 [Av|egeopmv eawnmso Average _+ %RSD 102% + 2.4% Les rior rn or LCS-140131-7 39.8 41.4 104 esos 2 se LCS-140131-8 39.8 39.2 98.6 Leste = ses [avo | mpowoc omew am mso| LCS-140131-9 Average + %RSD 39.8 39.2 100% -+ 3.1% 98.5 Nas et apisti NA = N~t Applicable 1) LCS sega covey otmoc aconpren creaof 00.27%. (1) LCSs average recovery did not meet acceptance criteria of 100 _+ 20% `33An..a77lyticAAanlnauanlclyeytrttiiacciaanltlyMMiseebttahhsoeodddonUUnhnicscetoerrritctaaaliinnOCttdyyata that control charted 11d used 10 evaluate method accuracy foAaarnnntddahlyrpetarsieccociatiilsoiuoonfnn.ca.cecrTTtuhhariaeanctmmyyeeirtstehhbsooauddslesiudn(nconenrc%tha)oiiosnbttortyraiistciscancalaealQdlccnfCuuolltradattateyetedadQfftohoClallotoswwiasiimnncpggolnEEetTrTsoSS.l-F1-c12oh2.ar-0r0m1te12ed2.t2.h2a.n.oddTTnuhEeseTsesStdtaa6tnon.dd0ea4avrr.add1lu,ddateetvhveieiaammttaiieoostnnhtoisdacccaaaocllncccutuulrsfaattceayydd f2QQ,oCCrwthhssieaacmmshpcepitleeossfoawwceecrrmueerauuscsee1yedd.r.eassTTuohhltraesfpee(dixxneppn%eaacnn)eddoeenbeddtvaeuuinlndnceocedferrtfs9toaa5riinn%tthtyye i caculted by mutplyng QC samples. For method is calculated by multiplying hestandard deviationby afactor ETS-8-044.1, the most recent fifty the standard deviation by a factor ocff 2, which corresponds to a confidence level of 95%. TT2hh4ee%aannaHaloylwytteiiccvaaellrmm.eehtthheoorddecuuonnvcceeerrrytaotiafnitynhateasysmcciaadllscceuutlaatotefeddLbCbySy EEaTTnSSa-l-11y22z.e-00d1o122n..221fo/o2rr4P/P1FF4HHwSaSsbbyy1i2inn8tt%eerfmnoaarll ssPttFaanHnddSaabrrddyccnaalleibrmraaattioosnntawvnaasds.ard SC_ca+aam2llip4btl%rraea.tstiHooaonnnwfafooelrrvytetzhhree,edtbsshaaeymmrpneplcleeeossmveaaarnnyaasolytyfa2ztne2hdddeaoromndnidc1tahsslisebtrddoaaatftteeoL,.nCTTSfrhoaeavrnPeeaFfrloyHsrzSe,e,dtttohoee4na2an18na/a%2yl4yl/t1cic4aallwmmaesesth1ho2o8dd%uunfocnrerPctaFiHnetSyrwwbayatssineaetxexprpinaaannlnddseettaddnfyfdooarrrd samples analyzed by internal standard calibration for PFHS to +28%. TTaabbllee 88.. AAnnaallyyttiiccaall MMeetthhoodd UUnncceertrtaaiinnttyy.. [ante|cumrotion |stndordDeistion0)|wethod ncersiory| [ema| wen | vis [www | Analyte P FBA Calibration Intemal Standard Deviation (%) 7.15 Method Uncertainty _+14% [roa 1 wens| vee |awe | PFOA Intemal 7.96 -+16% [ems 1wens eo | wee | PFBS Internal 8.90 +18% [ros 1 wens| we [ee | PFHS Intemal NA _+28% [eros 1 wewa T vw [wee | PFOS Intemal 7.97 _+16% [rma 1 owe | os [wwe| PFBA External 9.59 19% [ron TT owen| vee [awe| PFOA External 7.88 -+16% ES I 7S 7S | PFBS External 7.15 _+14% [ros Towa| a0 [www| [eros | emma [| PFHS PFOS Extemal Extemal Er NA = Not Applicable oe 8.10 9.99 | ae | _+16% 20% ence r80r PAGE 16 OF39 33663300..00009988 3M_MNO1596047 3M MN01596047 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-13 3.8 Field Matrix Spikes (FMS) E SRT E ESTSREene A target analyte field matrix spike sample was collected at each sampling point to verify that the analytical method is applicable for the collected matrix. Field matrix spikes are generated by adding a measured volume of field Le sample to a container spiked by the laboratory with the target analytes prior to shipping sample containers for TR sample collection. Field matrix spikes must be at least 50% of the analyte concentration to be considered an appropriate spike level. Field matrix spike recoveries within method acceptance criteria of 100_+30% confirm that E T ER E ee "unknown" components in the sample matrix do not significantly interfere with the preparation and analysis of the analytes of interest. The standards used for the preparation of the field matrix spiking solutions contained reference materials comprised of both linear and branched isomers for PFOS and only the linear isomer for PFOA. Field matrix spikes are presented in section 4 of this report. FMS Recovery = (Sample Concentration of FMS Average Concentration : Field Sample & Field Sample Dup.), 100% Spike Concentration Table 9. Field and Lab Matrix Spike Concentrations Final Concentration (nglmL) Location Spike Level PFBA PFOA PFBS PFHS PFOS [woMWr07,pPnW0o9,saandaPpWw10o | eFwMsS [wMWs13 TewFsMS [CMW1e6 TewFsMS [aaMrWo10n1, wMaWwi10o4n,wMwWi1c0s5,wMwWi1o08s,wMvWr1i1o0,aanndnMwWi1a4Rn| eFwMsS [wMW1e 2 TewFsMS Lewd Low Tdp Blank [voHnigh |o2.m00 | tw1.92 | 220.000 | 22.000 | 11m.85| |s5.w00 | er4.79 | s5o.0o0 |se5.0o0 | am4.64| | o2t4.o9 | as 24.8 |a250.0 | a250.0 | a2s5o.0 | | e99a.4 | s9e9.z2 | 1 0O0 | w1 Oo0 |w99s.8 | | ar 497 | we496 | so 500 | sw500 | am499 | bE2.00 oh 1.92 ba2.n00 ba2.00 La1.85 |e99a.4 | s99e.22| 110000| 01000 | 0909.88 | 52 SOMA opr cern 33..99 Lab MMaattrriix SSppiikes ((LLMMSS)) The field matrix spike level prepared for location MW14R was not sufficient for PFBA. Since this was the first ER SES sampling of this location, a laboratory matrix spike (LMS) sample was prepared for PFBA to verify that the analytical method is applicable to the collected matrix. The LMS sample was generated by adding a measured volume of E TERE LE RR Tn standard solution to an aliquot of the primary sample. Since the MW14R samples required dilution prior to sample analysis, the spike amount added was based on the on-column instrument concentration. The actual spike concentration for PFBA is presented in Table 10. J es pe. nre LMS recoveries within method acceptance criteria of 100_+30% confirm that "unknown" components in the sample matrix do not significantly interfere with the extraction and analysis of the analytes of interest. LMS concentrations EE must be 50% of the sample concentration to be considered an appropriate field spike. LMSs are presented in section 4 of this report. ESThe following calculation was used to calculate the lab matrix spike recovery in Section 4 of the report: e LMSRRecove~ -( Sample Concentration of LMS - A"vSeSprpaiigkkeeeCCoCnoocnneccneetnrntatrrtaaittooionnn : Field Sample & Field Sample Dup.). 1n00e% free [oe] Table 10. Lab Matrix Spike Levels. Sampling Location PFBA Final Concentration (ng/mL) Dw MaW1w4Rn r] 297 I PAGE 17 0F39 33663300..00009999 3M MN01596048 REPORTING 1501101 50.13 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-13 44 DDaattaa SSuummmmaarryy aanndd DDiissccuussssiioonn TTthhheoeTttaapbblleoBssinbbkel.loowwEasscuuhmmtmmaaabrerizzpeerotthvhieodsseaasmmtphplealeevrreeerssuaulglttssecaaonnnddceefnieltlrddammtaiatortnriixxansspdpiiktkeheerrereeclcoaovtiuevreeiperesirfofocosrernsstaadmmippflleiinrngegnllcooeccaa(ttiiRoonPnssD2a)5sowwfeetlllhl eaass tseshalaemamlpTpvlrlieeep daaBinnlafddnesskeaa.nmmcEpepla(leec%hcdRutuPappibDlcilc)eaavlpetae.rlo.uRveReidsseeussalurttlehtsseraaoannuvddnedraaeavvdgeeterroaacwggoeenocvvseaanlliuutreegasstinoaarnrfeeaicrnouaduunnrntdhdeeteesdd.rettloBoaetttihcvhraereeuepeseessriicggoenfniniofftiiucdcnaaidfnnfitetnrffiegigg,nuucrrveeeassl.(.u%ePPRsevePrarcDcree)ynnsottfgthel ffdrreteolomammtoivntthehsoordssaieeflfeeslirseettenhddcaei1tn(h%ttehhRmeerePrataDhww)ovddatalatua.ae.pspFFariiereoellpddrrmomiauaatnertdrfiioexxdsshpptoiekketewgssiovmmeseneigeenmttiinanfigcgia.ttnhhteefimmgeuetrtehhsoo.dd acceptance Because of acceptance crea of rounding, criteria of $30%, values +30%, vary slightly demonstrate that the method is appropriate for the given matrix. AfAollllfoeiewlikdngmmeaaxtcrtiexpstsippoiknkse:aanndd surrogate surrogate recovery recovery spikes spikes (ahereapplicable) (where applicable) metmethod met method acceptance crlera acceptance criteria wih with the the following exceptions: f`CoCGrGtMhMeNNtGGheWWrtMMarWWg3e1t3::anTTahhyeeteFFsMMaSSnlldeovsveuelTwwoaagssalnneootrteaacppoppvrreoorppireriisaattmeeefftoorrmPPeFtFOhOoAAd.. aTTchhceeepFFtaMAnSScessppcriiktkeeerimma.aettNmmoeetathhdooddtdiaaocncaccleeppOttaCanncsceeamccprrilitteeesrriiaa wore prepared for PFOA for the other target analytes were prepared for PFOA. and surrogate recoveries met method acceptance criteria. No additional QC samples ``CaCGcGcMMepNNtaGGncWWecMMrWWH1a66::foTTrhhteoheFFMMotSSrellreovtveaerlgwweataassnaonlotyttaaeppspparronoppdrriisaattueerffooorrgPPaFFrOOeAAcoaavnnerddiePPsFFmOOeSS.t. mTTerhtoehoFFdMMaSSsccspeppikoteamnmaceettcmmeoretaoh.odd No `addilonalQCsampesvere preparefodr PFOAanc PFOS. acceptance criteria for the other target analytes and surrogate additional QC samples were prepared for PFOA and PFOS. recoveries met method acceptance criteria. No ``CaCGcGcMMepNNtaGGncWWe cMMWWrH1Oe0110:a:TThthheeeFFtNMeSSrllteeavvreegllewwtaaasnsnalnoyottteaasp.ppprrNoooppriaraditdeaiiftooorerraPPlFFQBBACAsaaannmddplPPFeFHsHSwS.e.rTTehhpeerFFepMMaSSressdppioikkree PmmFeetBtAmmeaetnthhdooPddFHS. acceptance criteria for the other target analytes. No additional QC samples were prepared for PFBA and PFHS. e`CnCtGeGMrMNNfoGGrWWthMMe WWot1h1e01r0:t:aTTrhgheoetFaFnNMaSlSytoleevvsee.l wwNaaossanndodoit taaoppnpparlrooQpprCirasitaeamftooprerlPPeFFsOOwAeA.r. eTTphhreeepFFaMrSSedssfppoiirkkPeeFmmaOetAt mmeetthhoodd aacccceeppttaannccee criteria for the other target analytes. No additional QC samples were prepared for PFOA. f`CoCGrGtMMheNNtGGhWeWrtPPaWWrgS0e9t::aTTnhheaeeFFsMNSSanlledevvseelul TwwoaagssatnneoottraaepcpoppvrreoorppirreiiasatemeeofotrrPmPeFFtBhAAo.d. aTTcrhceeepFFtMMaSnScsesppriktieermmae,ett NmmeoettahhdooddditaaoccnccaeelppttQaanCncceseaccmrrpittleaeriiasa wore ropared or PFA. for the other target analytes were prepared for PFBA. and surrogate recoveries met method acceptance criteria. No additional QC samples f`CoCGrGtMhMeNNtGGhWeWrtPPaWWr1gI0e0:t:aTTnhhaeeytFFeMNsSSanlledevvseelul wwoagasastnneoottraaepcpoppvrreoorppirreiiasatemeeofotrrPmPeFFtBhAAo.d. aTTcrhceeepFFtMNanSScsesppriikteeerimmae,ett NmmeoettahhdooddditaaoccnccaeelppttQaanCncsceeamccpriitlaeerrisaa were prepared for PFA. for the other target analytes were prepared for PFBA. and surrogate recoveries met method acceptance criteria. No additional QC samples r`CtCGeGMMNNfoGGrWWheMMWWiHe1144rRRt::arTTghheeetaFFnaMMlSSytelleesvveeall nwwdaaassnnoaoldt daatpppoprnroaoplprribiaaotterefafootrrorPPFyFBBmAaA.t.riTTxhhseepiFFcMeMwSSsaspspiipkkreeempmaeerltedmmeaetnthhdooddmeaatccocmeeeppttthaaonndccee acceptancecreafor PFBA criteria for the other target analytes acceptance criteria for PFBA. and an additional laboratory matrix spike was prepared and met method 33663300..00110000 ence rnor PAGE 18 OF39 3M_MNO1596049 3M MN01596049 SE Table 11. CGMN GW MW07 140113 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. ISO'[ 1-01-03-'f3 FO 3M LIMS ID OO Description [o|m wa a] PFBA Concentration 1 1 (ng/mL) %Recovery PFOA Concentration (ng/mL) %Recovery ISO11-0,1-03-13-001 CGMI~-MW07-0-1401,13 ISO1,1-0"1-03-13-002 CGMI~-MW07-DB-"1401 "13 ISO1"1-0"1-03-13-003 CGMI~-MW07-FMS-1401,13 Average Concentration (n1lm L) -+ %RPD 30"1 NA 275 NA 504 108 2.88 n1/mL -+ 9.0% 0.407 NA 0.373 NA 2.35 102 0.390 n11mL -+ 8.7% mone lowse [[ pl [e EEem|s e| [T Eo wes| cre || 3M LIMS ID ISO11-01-03-13-001 ISOll-01-03-13-002 nT iZiaL ISOll-01-03-13-003 Description CGMN-MW07-0-140113 CGMN-MW07-DB-140113 CGMN-MW07-FMS-140113 PFBS Concentration (ng/mL) %Recovery <0.100 NA <0.100 NA 2.08 104 PFHS Concentration (ng/mL) %Recovery 0.0508 NA 0.0386 NA 2.09 102 PFOS Concentration (ng/mL) %Recovery 0.104 0.104 1.82 NA NA 92.6 Average Concentration (ng/mL) 4- %RPD <0.100 ng/mL 0,0447 ng/mL 4- 27%!1) 0.104 nglmL -+ 0.0% mune 3M LIMS ID ower Description | stems {ston |sms| 13C~-PFBA 130~-PFOA 13C~.PFOS %Recovery %Recovery %Recovery ny ISOll 01433 13 001 ISO11-014)3-13-002 ISO11-01-03-13-003 te[=[8]s] CGMN MW07 0 140113 CGMN-rvlW07-DB-140113 CGMN-MW07-FMS-140113 105 99.1 92.8 99.4 98.6 112 112 85.4 97.0 Average Recevery (%) 4- %RSD 98.8% 4- 6,0% 103% 4- 7.3% 98.2% "~ 14% Firman, NA - Not Applicable Samples were diluted 1:1 with methanol and analyzed by intemal standard calibration. (1) Sample/sample duplicate %RPD did not meet method acceptance cdteria of <20%. PAGE 19 OF 39 ners 3M_MN01596050 33663300..00110011 3M EHVIRONMENTAL LABORA TOR Y REPORTNO. IS011-01-03-!3 Table 12. CGMN GW MW12 140116 mone lower [e |Rmo a re "BEw ssa| te]] 3M LIMS ID ISO11-01-03-13-004 EEETIT ISO11-01-03-13-005 Description CGMN-MW12-0-140116 CGMN-MW12-DB-140116 PFBA Concentration (ng/mL) %Recovery 327 NA 297 NA PFOA Concentration (ng/mL) %Recovery 682 NA 653 NA ISOll 01~33 13 006 CGMN MW12 FMS 140116 866 111 1190 105 Average Concentration fng/mL) %RPD 312 n~/mL ~" 9,6% 668 nglmL ~" 4.3% a 3M LIMS ID o2sISO11-01-03-13-004 ISO11-01-03-13-005 ISQ11-01-03-13-006 Average NA = Not Applicable Joss Description CGMN-MW12-0-140116 CGMN-MW12-DB-140116 CGMN-MW12-FMS-140116 Cencentration (nglmL) _+ %RPD [om ms | ros. PFBS Concentration 15 Lave | EE tree]"0 | ates (ng~mL! %Recovery PFHS Concentration (ngtmL) %Recovery PFOS Concentration (ng/rnL) %Recovery ht 85.4 NA 78 8 NA 588 101 82.1 nglraL _+ 8.0% 14.1 NA 12 1 NA 505 98.4 13.1 nglmL_+ 15% 129 NA 113 NA 614 98.8 121 ng/mL _+ 13% Samples were diluted 1:50 and analyzed by external standard calibration. PAGE 20 OF 39 3M_MN01596051 33663300..00110022 es comonin Table 13. CGMN GW MW13 140114 -- he omaTwa] 3M LIMS ID ISOll-01-03-13-007 Et tallto ISOll-01-03-13-008 ISOll 01433 13 009 Description CGMN-MW13-0-140114 CGMN-rvlW13-DB-140114 CGMN MW13 FMS 140114 PFBA Concentration (ng/mL) %Recovery 969 NA 990 NA 13.8 80.1 PFOA Concentration (ng/mL) %Recovery 9.65 NA 9.90 NA 13.4 NC 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. ISO f 1-01-03-'13 Average Sie 3M LIMS ID ISOll-01-03-13-007 ISO11-0%03-13-008 ISO11-01-03-13-009 [eh ms 1 e ms]erT os Concentration fng/mL) 4- %RPD 9.80 ng/mL 4- 2.1% PFBS Concentration 9.78 ng/mL 4- 2.6% PFHS Concentration PFOS Concentration Description CGMN-MW13-0-140114 CGMN-IVfN13-DB-140114 CGMN-rvlW13-FMS-140114 (ng/mL! 1.12 1 27 6.54 %Recovery NA NA 107 (n~tmL) 0.857 1 08 6.03 %Recovery NA NA 101 (n~l/mL) 3.02 3 14 7.53 3%Recovery NA NA 96.0 ee Average Concentration (nglmL) _+ %RPD 3M LIMS ID Description T[cemrs f| ccerlon | "c]ron| 1.20 ng/mL _+ 13% 0.969 ng/mL + 23%m ~C~-PFBA ~C~-PFOA ~C.-PFOS %Recovery %Recovery %Recovery 3.08 ng/mL _~ 3.9% ISO11-01-03-13-007 CGMN-MW13-0-140114 103 108 89.9 ISO11-01-03-13-008 CGMN-MW13-DB-140114 ISO 11-01-03-13-009 CGMN-MW13-FMS-140114 Average Recovery (%) + %RSD 96.8 88.3 95.9%_+7.4% 118 98.3 108%+9.1% 97.7 94.3 94.0%+4.1% Co rm NA = Not Applicable fH reer m pe mr mi cia NC = Not Calculated; Spike level was less than 0.Sx the endogenous sample concen~ation. Samples were diluted 1:1 with methanol and analyzed by inten'~al standard calibra'een. (1) Sample/sample duplicate %RPD did not meet method acceptance cdleria of <20%. PAGE 21 OF 39 -- 3M_MN01596052 33663300..00110033 3M ENVIRONMENTAL LABORA TOR Y REPORTNO. ISOf 1-01-03-!3 Table 14. CGMN GW MW16 140114 moe 3M LIMS ID owe Description |oR orey|"BE steer] [ema PFBA Concentration (ng/raL) %Recovery wa] PFOA Concentration (ng/raL) %Recovery ISOll-01-03-13-0" 0 CGMI',J-MW16-0-140114 43.4 NA 93.1 NA ISO11-01-03-13-0" 1 ISOll 01~38 13012 CGMN-MW16-DB-140114 CGMN MWI&FMS 140114 42.3 63.2 NA 88.9 NA 81.9 >ULOQ NO Average Concentration fng/mL) 4. %RPD 42.9 n~/mL 4. 2.6% 91.0 ng/mL 4. 4.6% weome lows 3M LIMS ID ISOll-01-03-13-0" 0 ISO11-01-03-13-0" 1 Description CGMN-MW16-0-140114 CGMN-MW16-DB-140114 |ES TloveTs|"EEI|etreIe]"ai T| epee [ems PFBS | ms PFHS | rPoFOsS. Concentration (ng/mL! %Recovery Concentration (n~tmL) %Recovery Concentration (ng/rnL) %Recovery 41.1 NA 5.51 NA 51.0 NA 38 8 NA 5 52 NA 55 2 NA ISOll-01-03-13-012 CGMN-MW16-FMS-140114 65.3 101 32.8 109 78.0 NC Average Concentration (nglmL) _+ %RPD 40.0 ng/mL _+ &8% ~.~2 nglmL _+ 0.18% ~3.1 ng/mL ~" 7.9% ge oer 3M LIMS ID Description ISO11-01-03-13-0" 0 CGMN-rvIW16-0-140114 EeISO11-01-03-13-0" 1 CGMN-rvIW16-DB-140114 ISOll-01-03-13-012 CGMN-MW16-FMS-140114 =Average Recovery (%) + %RSD -- [corsa|coron|cores | I=C~-PFBA ~3C4-PFOA ~C4-PFOS LoweLoum [owe] %Re~;overy 92.7 TT 88.9 80.0 nel 87.2% -+ 7.5% %Recovery 91.0 95.3 101 95.8% -+ 5.2% %Re~overy 75.3 88.8 95.8 86.6% -+ 12% ir man rs wraap t s NA = Not Applicable NC = Not Calculated; Spike level was less lhan 0.Sx the endogenous sample concen~ation. Samples were diluted 1:1 with methanol and analyzed by inten'~al standard calibra'een. PAGE 22 OF 39 3M_MN01596053 33663300..00110044 Ta. comm GMmE Horts Table 15. CGMN GW MWl01 140115 3M ENVIRONMENTAL LABORA TOR Y REPORTNO. IS011-01-03-!3 mae 3M LIMS ID ooo|oma[ Tw mae ]| Description PFBA Concentration (ng/mL) %Recovery PFOA Concentration (ng/mL) %Recovery ISO11-01-03-13-0" 3 CGMN-MW101-0-140115 S-- a. ISO11-01-03-13-0" 4 CGMN-MW101-DB-140115 ISOll 01~93 13 0"5 CGMN MW101 FMS 140115 Average Concentration (ng/mL) ~" %RPD 1590 NA 80.0 NA [eminem] 1430 NA 1530 NO 1510 ng/mL ~- 11% 78.7 NA 164 85.3 79.4 ng/mL ~" 1.6% FS 3M LIMS ID FODescription [ems PFBS 1 Concentration Tens] ros PFHS YC 1I Concentration PFOS Concentration (ng/mL! %Recovery (ngtmL) %Recovery (ng/rnL) %Recovery ISO11-01-03-13-0" 3 CGMN-MW101-0-140115 25.7 NA ISO11-01-03-13-0" 4 CGMN-MW101-DB-140115 25 1 NA ISQll-01-03-13-0" 5 CGMN-MW101-FMS-140115 117 91.6 Average Concentration (nglmL) _+ %RPD 25.4 nglmL _+ 2.4% wn NA = Not Applicable NC = Not Calculated; Spike level was less lhan 0.5x the endogenous sample concentration. en5 yt ent ania Samples were diluted 1:50 and analyzed by external standard calibration. 383 NA 413 NA 477 NC 398 nglmL _+ 160 NA 158 NA 240 81.2 1~9 ng/mL _+ 1.3% PAGE 23 OF 39 awmorse 3M_MN01596054 33663300..00110055 Tot. COMMGWG rs Table 16. CGMN GW MWl04 140115 mae J| oo mT [me]| 3M LIMS ID ISOll-01-03-13-0" 6 PE thal lls ISQll-01-03-13-0" 7 ISOll 01433 13 0"8 Description CGMN-MW104-0-140115 CGMN-rvlW104-DB-140115 CGMN rvlwl04 FMS 140115 PFBA Concentr=ion (ng/mL) %Recove~ 194 NA 210 NA 285 83.5 PFOA Concentration (ng/mL) %Recovery 35.1 35.0 129 NA NA 94.7 3M ENVIRONMENTAL LABORA TOR Y REPORTNO. IS011-01-03-!3 Average Concentration (ng/mL) ~" %RPD FO 3M LIMS ID ISOll-01-03-13-0" 6 ISOll-01-03-13-0" 7 ISQll-01-03-13-0" 8 FODescription CGMN-MW104-0-140115 CGMN-IV~At104-DB-140115 CGMN-rvlW104-FMS-140115 202n~mL7,9% 35.1 n~/mL 0,29% [om Toe [we PFBS Concentration CC) FY CCI) CY (ng/mL! %Recovery 7.34 NA thAta 7 65 NA 111 104 PFHS Concentration (ngtmL) %Recovery 14.4 13 9 114 NA NA 99.9 PFOS Concentration (nglmL) %Recover~ 4.22 NA 4 27 NA 96.2 92.1 EoEo Y rp arm Average Concentration (nglmL) + %RPD NA = Not Applicable Samples were diluted 1:10 and analyzed by external standard calibration. 7.~0 nglmL _+ 4.1% 14.2 nglmL _+ 3.5% 4.2~ nglmL_+ 1.2% PAGE 24 OF 39 smerenss 3M_MN01596055 33663300..00110066 ro cme onle Table 17. CGMN GW MWl05 140114 omaTwa] PFBA PFOA Concentration Concentration 3M LIMS ID Description (ng/mL) %Recovery (ng/mL) %Recovery 3M ENVIRONMENTAL LABORA TOR Y REPORTNO. IS011-01-03-!3 ISOll-01-03-13-0" 9 CGMN-MW105-0-140114 56.0 NA 68.5 NA ISQll-01-03-13-020 CGMN-rvFA~105-DB-140114 55.1 NA 68.0 NA ISOll 01~33 13 021 CGMN MW105 FMS 140114 152 97.0 156 88.5 Average Concentration (ng/mL) 4- %RPD -- [eh ms 1 e ms]erT os 3M LIMS ID Description ISOll-01-03-13-0" 9 RE ENESEE NE ISOl1-61-03-13-020 CGMN-MW185-0-140114 CGMN-IV~N105-DB-140114 ISQll-01-03-13-021 CGMN-MW105-FMS-140114 Averago Concentration (nglmL) _+ %RPD ESEeE--errr EE NA=NotApplicable 55.6 ng/mL 4-1.6% 68.3 ng/mL 4- 0.73% PFBS Concentration (ng/mL! %Recovery 6.48 5 81 101 NA NA 94.9 6.1~ ng/mL + 11% PFHS Concentration (ngtmL) %Recovery 12.4 NA 12 8 NA 106 93.4 12.6 nglmL _+ 3.2% PFOS Concentration (ng/rnL) %Recovery 152 NA 152 NA 244 92.2 1~2 ng/mL _+ 0.0% Samples were diluted 1:10 and analyzed by ex[emal standard calibration. PAGE 25 OF 39 -- 3M_MN01596056 33663300..00110077 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. IS011-01-03-'f3 Table 18. CGMN GW MWl08 140114 moe 3M LIMS ID owe Description |Rore "BEyst| eer] [ema PFBA Concentration (ng/mL) %Recovery wa] PFOA Concentration (ng/mL) %Recovery ISOll-01-03-13-022 CGMN-MW108-0-140114 48.9 NA 171 NA ISQll-01-03-13-023 CGMN-MWl08-DB-" 40114 54.2 NA 166 NA ISOll 01433 13 024 CGMN MWl0&FMS 140114 Average Concentration (ng/mL) ~" %RPD [emse | mse | ros. 3M LIMS ID ISOll-01-03-13-022 EE TT TT ISOll-01-03-13-923 =a ISQll-01-03-13-024 Description CGMN-MW108-0-140114 CGMN-MW108-DBJ 48114 CGMN-MWl08-FMS-140114 141 90.0 51,6 ng/mL -~ 10% 264 96.3 169 nglmL -~ 3.0% PFBS Concentration (ng/mL! %Recovery 18.1 NA 159 NA 124 107 PFHS Concentration (ngtmL) %Recovery 4.19 NA 4 06 NA 106 102 PFOS Concentration (ng/mL) %Recovery 33.2 NA 33 7 NA 134 101 Average Concentration (nglmL) _+ %RPD 17.0 ng/mL + 13% 4.13 nglmL _+ 3.2% 33.5 ng/mL ~" 1.5% NA = Not Applicable Samples were diluted 1:10 and analyzed by external standard calibration. PAGE 26 OF 39 3M_MN01596057 33663300..00110088 Ta, comm GMIIrOte Table 19. CGMN GW MW110 140114 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. ISOf 1-01-03-'f3 mae 3M LIMS ID ogee Description omaTwa] PFBA Concentration Lommel| (ng/mL) %Recovery PFOA Concentration (ng/raL) %Recovery ISO11-01-03-13-025 CGMN-MWl 10-0-14{3114 S--- -- ISOl 1-01-03-13-026 CGMN-MW110-DB-" 40114 ISO11 014&3 13 027 CGMN MW110 FMS 140114 Average Concentration (ng/mL) 4- %RPD 177 NA min 181 NA 305 127 179 ng/mL 4- 2,2% 247 NA emi] 248 NA 340 NO 248 n~/raL 4- 0.40% El[e ei msLT eneein ars Lser] ee ar|os creer 31~1 LIMS ID Description PFBS Concentration (ng/mL! %Recovery PFHS Concentration (ngtmL) %Recovery PFOS Concentration (ng/mL) %Recovery ISO11-01-03-13-025 CGMN-MWl 10-0-143114 88.4 NA ISO11-01-03-13-026 CGMN-MW110-DB-" 40114 81 7 NA ISQ11-01-03-13-027 CGMN-MW110-FMS-140114 192 107 Average Concentration (nglmL) _+ %RPD 85.1 nglrnL 4- 7.9% wn NA = Not Applicable NC = Not Calculated; Spike level was less lhan 0.5x the endogenous sample concentration. ens yin ent aaa Samples were diluted 1:10 and analyzed by ex[emal standard calibration. 20.2 NA 18 6 NA 125 106 19.4 nglmL 4- 8.2% 12.0 NA 122 NA 106 94.1 12.1 ng/mL 4-1.7% PAGE 27 OF 39 awnctssose 3M_MN01596058 33663300..00110099 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. ISOf 1-01-03-'f3 Table 20. CGMN GW PW09 140115 EStEE3M LIMS ID ISOll-01-03-13-031 ISOll-01-03-13-032 H[e em Sh aLi y Shwa]cd Description CGMN-PW09-0-140115 TI CGMN-PW09-DB-140115 PFBA Concentration (ng/raL) %Recovery 500 NA 452 NA PFOA Concentration (ng/mL) %Recovery ,1.40 NA 1.26 NA ISOll 01~33 13 033 CGMN PW09 FMS 140115 730 NC 2.90 81.9 Average Concentration fng/mL) %RPD 4.76 ng/mL 10% 1,33 n~lmL4-11% FE 3M LIMS ID ISOll-01-03-13-031 ISOll-01-03-13-032 [om ms | Llros. Description CGMN-PW09-0-140115 MLIFEIEEE CGMN-PW09-DB-140115 PFBS Concentration (ng/mL) %Recovery 0.167 NA 0 178 NA PFHS Concentration (n~tmL) %Recovery 01,1"17 NA 0 ,10"1 NA PFOS Concentration (n~l/mL) %Recovery 2.29 NA 1 97 NA ISOll-01-03-13-033 CGMN-PW09-FMS-140115 2.23 103 2.27 108 4.08 105 Average Concentration (nglmL) _+ %RPD 0.173 nglmL ~" 6.4% 0.109 ng~m L _+ 15% 2.13 nglraL ~" 15% wane Joan 3M LIMS ID Description ISO11-01-03-13-031 CGMN-PW09-0-140115 EEEISO11-01-03-13-032 ISO 11-01-03-13-033 CGMN-PW09-DB-140115 CGMN-PW09-FMS-q 40115 55Average Recovery (%) + %RSD [corsa|cor | co oren s | I~C~.PFBA ~3C4.PFOA I~C4.PFOS | sn | nee |sme | %Recovery 84.0 TTI90.3 101 ats 91.6% + 9.1% %Re~overy 103 99.5 6.6 99.7% -+ 3.2% %Recovery 98.5 90.4 110 99.6% + 9.9% NA = Not Applicable reayia an NC = Not Calculated; Spike level was less lhan 0.Sx the endogenous sample concen~ation. Samples were diluted 1:1 with methanal and analyzed by inten'~al standard calibra'een. PAGE 28 OF 39 3M_MN01596059 33663300..00111100 Tato n.coweomvanrs Table 21. CGMN GW PWI0 140115 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. ISO f 1-01-03-'13 [oma PFBA Twa PFOA | 3M LIMS ID Description ISOll-01-03-13-034 CGMN-PW10-0-140122 EEE ISOll-01-03-13-035 CGMN-PW10-DB-140122 ISOll-01-03-13-036 CGMN-PW10-FMS-140122 Average Concentration (n11m L) -+ %RPD Concentration (n1/mL) %Recovery Concentration (n~/mL) %Recoveq/ 403 NA 0.223 NA FAERIE] 4 77 NA 679 NC 4.40 n~lmL -+ 17% 0 200 NA 223 105 0.212 n1Im L-+ 11% wise 3M LIMS ID Joss Description |G |sy|"BE ste |"5 | PFBS Concentration (ng/mL) %Recovery PFHS Concentration (ng/mL) %Recovery PFOS Concentration (ng/mL) %Recovery IS011-01-03-13-034 ISOll-01-03-13-035 ISOll-01-03-13-036 CGMN-PW10-0-140122 CGMN-PW10-DB-140122 CGMN-F~N10-FMS-140122 0.254 NA 0.D425 NA 0.12" NA 0.268 NA 0.0543 NA 0.126 NA 2.53 113 1.89 92.1 1.99 101 Average Concentration (ng/mL) -+ %RPD wise 3M LIMS ID Jom Description 0.261 nglmL -+ 5.4% 0.0485 nglmL -+ 24/=m [|e Soro |m mn| I~C~-PFBA ~C4-PFOA I~C~-PFOS | nee | teeny| stem| %Recovery %Recovery %Recover,j 0.124 nglmL -+ 4.0% IS011-01-03-13-034 ISOll-01-03-13-035 ISOll-01-03-13-036 CGMN-PW10-0-140122 CGMN-PW10-DB-140122 CGMN-F~N10-FMS-140122 99.6 102 99.6 116 89.1 5.0 83.4 73.7 103 Average Recovery (%) -+ %RSD er] NA = Not Applicable -" 100% --. 1.1% NC = Not Calculated; Spike level ',,,'as less than 0.Sx the endogenous sample concen'a'ation. Samples were diluted 1:1 with methanol and analyzed by intemal standard calibration. (1) Sample/sample duplicate %RPD did not meet method acceptance cdteria of <20%. 100%-+14% 86.6%--.17% PAGE 29 OF 39 wero 3M_MN01596060 33663300..00111111 SITable 22. CGMN GW MW14R 140113 ee l oo ef [oma PFBA Twa PFOA Concentration Concentration | 3M LIMS ID Description (ng/mL) %Recovery (ng/mL) %Recovery EAEISOll-01-08-13-037 ISOll-01-03-13-038 ISOll-01-03-13-039 ISOll-01-03-13-037 == CGMN-MW14R-0-140113 CGMN-IVIW 14 R-DB- 140113 CGMN-IVIW 14 R-FMS-140113 CGMN-MW14 R-0-140113 LMS |HHHE 300 NA 137 NA 289 NA 141 NA 361 NC 227 88.7 551 86.3 NA NA Average Concentration (nglmL) %RPD 295 ng/mL 3,7% 139 nglmL 2.9% 3M ENVIRONMENTAL LABORA TOR Y REPORTNO. IS011-01-03-!3 em PFBS [emPFHSs] rPoFOsS. 3M LIMS ID Description ISOll-01-03-13-037 CGMN-MW14R-0-140113 A ehdial Ed ISOll-01-03-13-038 CGMN-MW14R-DB-140113 total ISO11-01-03-13-039 CGMN-MW14R-FMS-140113 Average Concentration (ng/rnL) + %RPD Concentration (ng/mL) %Recovery 17.3 NA 17.7 NA 117 99.5 17,5 ng/mL + 2,3% Concentration (nglmL) %Recovery 12.1 NA 12.4 NA 114 102 12.3 ng/raL 2.4% EEETEerp Ee NA- NotApplicable NC = Not Calculated; Spike level was less lhan 0.5x the endogenous sample concentration. ConcentraBon (ng/mL) %Recovery 25.0 NA 24.8 NA 120 95.3 24.9 ng/mL 0.80% Samples were diluted 1 : 10 and analyzed by external standard calibration. PAGE 30 OF 39 -- 3M_MN01596061 33663300..00111122 Tal 3. COGHAMNHONL8 4015 and TR BLANKS Table 23. CGMN GW MWl04-RB 140115 and TRIP BLANKS mae J| oe e mm [[wmee]| 3M LIMS ID Description PFBA Concentration (ng/mL) %Recovery PFOA Concentration (ng/mL) %Recovery 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. ISOf 1-01-03-'f3 ISO11-01-03-13-043 ISOl 1-01-03-13-040 ISOll 01433 13041 ISO11-01-03-13-042 CGMN-GW-MWlO4-RB-" 40115 CGMN-TRIP-0-140113 CGMN TRIP LS 140113 CGMN-TRIP-HS-140113 move 3M LIMS ID oon Description <0200 NA 0.227 NA <0200 NA <0.0480 NA 223 112 1.90 99.2 99.7 100 95.0 95.8 [o 1 m me | am PFBS Concentration [im Loy [oe[Eir| ny (ng/mL! %Recovery PFHS Concentration (n~tmL) %Recovery PFOS Concentration (n~l/mL) %Recove~ ISO11-01-03-13-043 ISO11-01-03-13-040 ISO11-01-03-13-041 CGMN-GW-MWIO4-RB-" 40115 CGMN-TRIP-O-140113 CGMN-TRIP-LS-140113 <0.100 NA <0.0250 NA <0 100 NA <0 0250 NA 1.72 86.0 2.50 125 0.235 <0 0232 1.75 NA NA 94.4 ISQ11-01-03-13-042 CGMN-TRIP-HS-140113 106 106 102 102 102 102 mae 3M LIMS ID Jove Descdption Loven[vom | toe | %Recover]/ %Recovery %Recover7 ISO11-01-03-13-043 ISO11-01-03-13-049 ISO11-01-03-13-041 CGMN-GW-MW104-RB-'40115 CGMN-TRIP-O-140113 CGMN-TRIP-LS-140113 99.0 86.2 97.5 93.3 98.0 96.4 102 97.6 107 a02300 shy ed et crnvr rin TRS en 133 doy eecr, NA = Not Applicable Samples were diluted 1:1 and analyzed by internal standard calibration with the exception of the TRI P 14S, which was diluted 1:10 and analyzed by external standard calibratien. PAGE 31 OF 39 amworsoscsz 3M_MN01596062 33663300.00111133 REPORT KO 01013 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-13 55 CCoonncclluussiioonn LaaLbanobraoaertsao,troyryTcchoonetnratrocolclsusprpaiickeyessawnwedererpereuucssieesiddontoodwdeeerteetrtmeheincneuttshheeedaa0nnaaeylystttciciaamllatmmeeettthhheooddmaeactcchcuourdraauccnyycaearnntddanpptrryeeccfiiossriiootnnheffoorraallll arvreensesauulnltyltssts.ea.sm.FFpieTellhdodemmmaaatacritciiruixxxraesscxppyicikkoaeepntrrdewecchpooervevreecroirsiieienoossntddewdee.memoroenInnststhotrersaanttoeeuddsientthdshatataottntthecheoesstaiamwnnahaalotlyeyritiectchaatellhemmmefeeltttohhhdooodddmwauwalnascrseaarstpppapipirnkrootoypprrfrioeiaarcttteehoefovorer6rthhyee `gonwiolvatesmmnceeosemeatpmlmmpeeelttetehndmooddaustaariiccxnccgeee3xppcMttaeanpEnncct veewihCcrerroiirtneeemrreina,no,tttatehhldeeL. ammbIneeottrthhahootodsoeurunyincnmecserettatrtanhaicoinnedttsyyEhwhTaahSsse8r.bbe0ee4teeh4nne.aa1fiddejMjluduessmttteehaddotraadixcocccsfooprArdidkiniennagglrleylyy.c.osvAAioennrsraaylhlyydsosidiiss `wDDAeanetastloeyrcrtmomicimiannlpaaoltteisootennudoofuf saPPireneorgrffrlu3uecMoprroinrnEtaaneltvdeeiiddronCCnTomaobmmelpnpeotoasuuln1nLddaassnbdoiinnra1W W1tao-alr2yta3ermrofbbeyytthhLLoiCdCr!eMEMpToSSrSt/IM.-8;S-0; 4DD4ii.rr1eecc"ttMIInenjtehccottdionnofAAAnnnaaallyylysssissis"".for the Analytical results are reported in Tables 1 and 11-23 of this report. 66 DDaattaa// SSaammppllee RReetteennttiioonn AA1ll0lr3reeMmmaEaininvniiinnrggonssmaemntapalle maLaannbddoaprasasstsoolocrciyiaasettteeaddndpparrroodjjeeoctpteddraaatttaai(n(hghaaprrrddocccooepdpuyyaraensnd.d eelleecctrrooniicc)) wwiilll bbeeaarrcchhiivveeddaaccccoorrddiinngg to 3M Environmental Laboratory standard operating procedures. 77 AAttttaacchhmmeennttss `AMWpAEpp3ep,ndeiMxnA1Ad::5,TTaarArgg1oe0tt1AA,nnaallWyyt1et0HH4iiss,ttoorrMiicc1aal0l TT5rr,eonnAdd1DD0aat8taa,ffoorWrCC1ao1ttt0taa,ggeePGGOrroSovv,eeaMMnaodnntPioto1rri0inn.gg W Weelllss MMAWO077,, MMWW1122,, MW13, MW16, MW101, MW104, MW105, MW108, MW110, PW09, and PW10. 33663300..00111144 Face orm PAGE 32 OF 39 3M_MNO1596063 3M MN01596063 rv 51 anos 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-13 88 SSiiggnnaattuurreess > ety FERRE Digitally signed by Susan T. Wolf DN: c=US, st=MN, I=St. Paul, ou=3M Environmental Labo,ator~2 authenticated by LRA, email=stwolf@mmm.com, o=3M, cn=Susan T. Wolf Reason: ~ am the author of this document SanT WoT, 3HPrincipAnaalylcal vestgaior Date: 2014.02.18 11:50:28 Susan T. Wolf, 3M Principal Analytical Investigator Digitally signed by William K. Reagen DN: c=US, st=MN, I=St. Paui, FA Em, on=Laboratory Direc:or, ou=3M Environmental Laboratory authenticated by LP~ email=wkrea~en@mmm corn, o=3M, cn=William K, Reagen Wi K Ranger PRD. SEM nvronbomraenTetomla Reason: ~ am aporoving this document Date: 2014,02.18 13:t6:54-06'00' William K. Reagen, Ph.D., 3M Environmental Laboratory Technical Dioder Director 10 31 Environmental Laboratory QualyAssuranceUnthas auc th cataand pono is The 3M Environmental Laboratory's Quality Assurance Unit has audited the data and report for this poet project. Cray [ome] Digitally signed by Casey Howell DN: c=US st=MN I=St Paul. ou=Quality Smads Assurance Unit. rJu=SM Envir,)nrrental Laboratory authenticated by LRA, cn=Casey ~ lowell Reason: I agree to the terms ,defined by the Co Re Quality Assurance Representative ETnThvhiiissrtoteonstmtarrnoeapplooLrttasbshoharaaltlllonrnoyo.tbboerreepprroodduucceedd except in except in full, full, without writen approof tvheaSlH without written approval of the 3M Environmental Laboratory. 33663300..00111155 srcesnorn PAGE 33 OF 39 M_MNO1S56064 3M MN01596064 CotisgeGrove WWD? -unts re nn. AAppppeennddixiAAx:: TTaarrggeettAAnnaallyyttee HHiissttoorriiccaall TTrreennddDDaattaa Cottage Grove MW07 - units are ngfmL He REOOR11T015O.13 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-13 1] - {ora--eeg ERE worMW07 norPFBA PFOA nso 10/15/2012 am2.55 0.298 wen 1/29/2013 am2.09 0.259 on 4/22/2013 ow2.61 0.240 PFBS <0.0250 <0.0250 0.0268 Sos hiPS PFOS 0.0257 0.0439 0.0459 Samples were below the limit of quantitation for PFHS. GCoottitaaggeeGGrroovvee WIZ MW12 urs - units reare int. ngfmL ves 7/23/2013 om1.71 0.303 0.0396 0.241 wns 10/28/2013 om3.07 0.428 0.0291 0.104 vise 1/13/2014 om2.88 0.390 <0,100 0.104 200 150 5O : ci s,m bMS NN RN wenMW12 PFBA PFOA PFBS osPFHS PFO5 wn 10/19/2012 won 1/30/2013 975 484 1390 946 94.3 91.4 mw 20,9 122 13,7 143 saosin 4/25/2013 7/24/2013 622 1110 1020 2000 105 175 wm 16,4 145 23.9 204 won 10/31/2013 uneien 1/16/2014 408 312 954 668 87.7 82.1 mom 13,0 131 13,1 121 33663300..00111166 resicrs PAGE 54 OF 39 aW_no1so6065 3M MN01596065 CotageGrove MW13 nts are nn AAppppeennddixiAAx:: TTaarrggeettAAnnaallyyttee HHiissttoorriiccaall TTrreennddDDaattaa Cottage Grove MW13 - units are ngfmL ERKA ot orT aa.ts 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-13 1 E PT RT I Cot NN BR NN wisMW13 norPFBA PFOA owen 10/17/2012 wo7.10 3.33 ves 1/29/2013 ow5.60 2.56 sawn 4/24/2013 sans 7/23/2013 ww 9.34 5.46 8.30 6.17 PFBS 0.619 0.560 0.972 1.07 PFHS 0.487 0.396 0.931 1.05 PFOS 3.85 3.92 4.05 4.02 CottageGroveHIG--untsare gmt. Cottage Grove MW16 - units are ng/mL mans 10/30/2013 am6.48 4.01 0.571 0.366 1.40 vias 1/14/2014 am980 978 0.969 3.08 1 ea ppdy 3 =e + "NNN RN weMW16 PFBA PFOA PFB5 PFHS PI'OS wwe 10/18/2012 33.6 45.9 25.7 2.71 23.1 vs 1/29/2013 31.5 42.6 28.3 2.54 20.2 vives 4/24/2013 33,2 43.8 27.5 2.74 21.8 aw 7/24/2013 26.3 39.9 29.6 2.83 20.3_ ows 10/30/2013 45.0 73.9 42.1 395 38.2 1/14/2014 42.9 91.0 40.0 5.52 53.1 33663300..00111177 ressorn PAGE 35 OF 39 au_mnotsseoss 3M MN01596066 CottageGroveHWAD1 --unts are ng. AAppppeennddixiAAx:: TTaarrggeettAAnnaallyyttee HHiissttoorriiccaall TTrreennddDDaattaa Cottage Grove MW101 - units are ng/mL rv 51 anos 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-13 | rete ot NR RN won MW101 oaPFBA PFOA onsen 10/18/2012 uns 1/30/2013 wow 1860 147 1630 124 vives 4/23/2013 om1830 121 PFBS 23.9 25.2 19.5 PFHS 427 455 459 PFOS 154 206 188 CottageGrove W104--unts aronin. Cottage Grove MWl04 - units are ng/mL nen 7/25/2013 wm1680 112 24.0 464 189 wn 10/30/2013 om1020 86.7 25.5 314 158 20 -5 B | ee, \\/ u 0| -- e--A ---- t U-- \N "NN NR usa 1/15/2014 ome1510 79.4 25.4 398 159 MWI04 PFBA PFOA PFBS PFHS PFOS 10/18/2012 36.0 42.0 12.6 8.69 127 I 1/30/2013 4/25/2013 36.3 74.7 44.8 60.7 11.4 9.75 9.07 13.4 20~ 185 7/25/20~3 543 74.7 8.16 11,8 176 10/30/2013 53.6 72.5 7.95 10.1 165 re. 1/15/2014 202 35.1 7.50 14.2 4.25 33663300..00111188 orcencrs PAGE 36 OF 39 M_MNO1S56067 3M MN01596067 ERAT Kot oraa.ts 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-13 CottageGroveHWIOS unsarent AAppppeennddixiAAx:: TTaarrggeettAAnnaallyyttee HHiissttoorriiccaall TTrreennddDDaattaa Cottage Grove MW105 - units are ng/mL - A . /\ fo e [-- Ee n ed e/ ,. Cot RN BR NN ws MWI05 norPFBA PFOA --PFBS PFHS wen 10/19/20:12 eas 1/30/2013 wom 52.7 98.3 54.4 119 wm 9.46 18.9 8.03 2:1.1 amon 4/25/2013 wm57.0 104 we5.72 16.0 PFOS 120 129 95.0 CottageGroveHWIDS unsarent. Cottage Grove MWl08 - units are ng/mL san 7/25/20:13 om71.6 70.6 am6.49 6.35 923 om :10/30/2013 om38.9 87.2 em4.98 6.01 467 vies 1/:14/2014 ow55.6 68.3 me6.15 12.6 :152 3o~4 2004 Eee cM MANNS ws MWI08 PFBA PFOA PFBS PFHS PFOS onsen 10/18/2012 :155 550 30.5 20.7 55.2 en 1/30/2013 :10:1 348 26.5 :1:1.:1 45.5 vives 4/25/2013 42.5 201 16.:1 4.95 37.3 ws 7/24/2013 38.0 202 14.6 4.94 26.8 wenos 10/30/2013 5:1.7 218 2:1.6 4.47 33.2 :1/:14/2014 51.6 16 17.0 4.13 33.5 33663300..00111199 srcesrorn PAGE 37 OF 39 a_Motsesoss 3M MN01596068 CottageGroveHWH10 unsarent AAppppeennddixiAAx:: TTaarrggeettAAnnaallyyttee HHiissttoorriiccaall TTrreennddDDaattaa Cottage Grove MW110 - un its are ng/mL RS 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-13 |e wl ne Dib ae Cote nN NR NN win MW110 orPFBA PFOA owen 10/18/2012 es 1/30/2013 wom 144 171 193 141 vases 4/25/2013 ow183 160 PFBS 39.6 46.6 66.7 PFHS 17.6 10.3 11.8 CottageGrovePWO3 unt rerg. PFOS 21.6 28.6 26.4 Cottage Grove PW09 - units are ng/mL was 7/24/2013 wm304 144 43.8 9.41 17.8 i we weno 10/30/2013 vas 1/14/2014 ww 174 179 190 248 94.8 85.1 15.3 19.4 21.1 12. I 1 ere 1 ag | CNR RRR mwas P%V09 PFBA 4/25/2013 3.72 6/19/2013 NA 7/24/2013 2.95 aw 8/29/2013 NA 9/30/2013 NA PFOA 0,223 0.462 0.624 0.605 0.873 trs r nti po er. PFOS 0,324 0.376 0.622 0.818 NA = Not Applicable; analyte not requested for the sampling event. 1.3~ a 10/29/2013 ama 4.53 1/15/2014 4.76 1.02 1.33 1.52 2.13 33663300..00112200 srcesworn PAGE 38 OF 39 a_Motsesoss 3M MN01596069 CottageGrovePWAD unt re ng. AAppppeennddixiAAx:: TTaarrggeettAAnnaallyyttee HHiissttoorriiccaall TTrreennddDDaattaa Cottage Grove PWl0 - units are ng/mL He REOO1R10T15.O13 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-13 I AER a] | mio aso aon awn mn PWI0 4/25/2013 6/19/2013 7/24/2013 8/29/2013 ox om om emo om PFBA PFOA 4.25 0.428 NA 0.415 3.37 0.420 NA 0.471 PFBS 0.594 NA 0.540 NA PFHS O. 197 NA 0.185 NA Nat ati ag nrps et. PFOS 0.396 0.401 0.38 0.415 NA = Not Applicable; analyte not requested for the sampling event. sn 9/30/2013 emNA 0.528 NA NA 0.465 eon 10/29/2013 em6.09 0.524 0.703 O. 193 0.458 mr 1/22/2014 om4.40 0.212 0.261 0.0485 0.124 33663300..00112211 srcemorn PAGE 39 OF 39 m_Motsesoro 3M MN01596070 wien LL r@ed: [SO11-01-03-13 ~ 3M EEZNN ~V,rIIRROONNM MEENNTTAALL LLAABBOORRAAT]'OORRYY Chaiil-of-Custodv Shipping Address: TA Evesmmanar Laboratory 3M Environmental Laboratory 3M Center, Bdg 260-5N-17 Bena St, Pau MN 55144 [ip Phone: (651t 733-9873 Alt. Phor~e: (651) 736-6559 rms Fax: (651) 733-4687 Reqc~ester: Hohenstsh~, Gary Allan (MAPLEW(}( Der~arm~ent: 452090 Site Source: 0l!9C020 Prc~ect Nt~mber: 006983700] Dare Cremed: 1110/2014 Project Descrip~io~ 3M Cottage Grove Site: ts~ q umer 2014 samp] ng Corn <eti@: Date: Project Lead: Susan T. Wolf Phone Number 651-2330851 EmaH Address: stwolf@mmm.com Copy List~ Gaetz. ~'Iark An@onv {MAPLEWOOD.3MUS-MN 3M CENTER~ C omm e~ts: Date/Time Sarni!le4 Matrix Comment [[pSoonrean Toy [ocmoemmrs vars o[ry 3aCmlTsie[ o]|] | EEF oneS 43 7 0rAr [sonoraToomergic Tama]T1]I onoriror cT Coomrr moenvw o[4gyfosptm r| ] l 1 { ]SO l 1 0143-13-009 ral foorroos; Tocoommemsr TtupEpg tls J] Tj[ssEmTpluglA oT]] I [] A] items accom~ted for "iemrmamrc i)eg C [] Received on lee [] Other: fpr I Rdia,fliJished by: Date Time $hil:tl~ed Via Colle{tor's signature: Received by: "/ / Dat~ Time 33663300..0011222 Page l of 3 3M MN01596071 WM EAVIRONMENTAL LABORATORY Chain-of-Custody ~EN.~'IRONEMNT"AL~ LABORATORY Shoprg Addres Shipping Ad@ess: s 3M ~nviro~mantal Laboratory S 3 GenS ter FiRg 2605.17 3M Center idg 26Q-hN-1 "rect ISOLLAL48-13 cant) -'rnject: IS011-01-03-13 Resuees Hohe, GaryAlin OUAPLEWOX Requas{er: Hohep,stein_ Gary Allan (MAPLEWO{ Depuimen 4290 Si Sues 019020 Deparm~ent: 452090 Site Som'ce: 01Jgc02u Pct amber QOBESTO0N Pr@ect Nmnber: 0[769837001 One Cres 102014 Date Created: [: 10/2014 Prject Desrpio: 3M Cota GiveSi 1 sc 2014sapling Pr~;ject Descr ~tion: 3M Conage Grove S~te. 1st quarter 2014 sampling DiSiositunte Seon Desciin 3M Sample Number ri~}ti~m St. Paul, MN 55144 Phone 65123873 Phone: (651) 733-9873 A Prone: 03 73 288 Air. Phone: (651) 73e-6559 Fa oy dads Fax: (651) 733-4687 PCoonepteiLoerstDuSe sT. Walt Project Lead: Susan T. Wolf Pros Norte 691.733.9851 Pima~e Number: 651~733-985 El Ades smolgmmmeon Emai! Address: stwolf@mmm.com Dna Sompet Matcn Comms Date!Tidne Snmpled Matrix Comment [sonore oe TeommsWous -- Tisomjep] | 1 soos nos Tconwons ygpe soos | commie Huy Tus mufory||| oglu] TT oSor 0o15-r300_|| ccoormmmse:. 14g veagade] | 1 _ JsonaronanTeommins fgg) TI Lrwafise] TT7] wage] 1 [Sor oroiveas | commis. 1901y Sonoran cowie fap pips] | Woglew | Canam. Jy Tr A 1501 10L0313:077_| Contnmiions. [40] ww er|] osonnsnoenno TTT oowmneess yor[RT ApMlEiE]1 y] [souaronmeToommaens = T-- 17] 1 coer (ous Lisasfore] ow | Sump Cotton pen cipt C) acbe C1 tems scum or Sample Condition Up~3n Receip~ Te_m--pra bc "['empcr,~mre: Deg C 0 Reshetontee ~ Acceptable E~ Received en ke Cote [] All items accounted for [~ Other: Covey Grdin Tou Huron Cotectrs susie Zr D C~lleeted by (print): : ~#': :~ b :. : { 9~_ Collectur'~ signature: I~.elinq uiM~ed by: Dale Time Shipped Via Received by: ~./>7" D~te: Time TTT [nS Page 2of3 au_mnotsseor2 3M MN01596072 33663300..00112233 O~VERNOVINROCENhaNNiEnToNtATCAoLLnaLLdAsyBoOr~akrToOnRYy Siping Adress Shipping Address; Sf3M Environmen~[ Laboraloey 3SM CnatiSBngie2kr,17 3M Cenler, 8~dg 2~0-5~4d PPrroojjeecctt; IiSS0O1U10-I0-10-033--1133 ((ccoonntt.) Aoneho:re6:5G1 f752.60.05350 St. Paul MN 55~ 4~ Phone: (651} ?~3-9873 DFDRpeoe>eca~tmN:eonm[aH:~roo5:2h2b00sa9a%sstt0es,m5So3SiGG7aietar0eyr1ySSlo,Aulnrlcoaen:a(M<eA1pAPsPcLL:EEWWGOK~ AFFaairx.x::P(h(6o55n1Ie)): 77{633~55-4I4i0~788377~559 CrojmcpsLoenntDSutenT. Wott. Prqec~ Nt~mber: 006983700, FDueiCrDewes,sstoinIns Cogs Date C~ eatee: 1/10t20t4 ~ ]gCOzO roe ts It ur2e01 amping Priec~ Lead: Susan T. Wolf Prone Nuc, 631.7333850 Phone Number: 65. ~-733-985t Era Arn ninco Emai~ Addres.~: stwoI@mmr~om Smet Sana citer 0 05|c5 omrv5 onJ0 ary DuncansMun Cones Trandarml 5 1mm sede lesovoermonoon TJooomwernonnedHtooorss irsojore| 6d Trime | por Te [on on imu] u30110s.9715b25_] Joconmpnviiors w[yoorrzeg JoT iasnsaysgeell= CaoT [Jaks) evi] coi van |commie 1701, 1501101451303_| commanminos. [40/3 (visas Srey seca] 13 1ifistys. He Lis on _Viofei | & 5011000505 | commons 190113 [f0i1onaammisrooe[]ccnommmmrass Jypus gypr IN lrs|gT /mT eI e d fesoov0o0i0e9s0J[eomoe nBatcoonsan Forme | | / pntd- |pseltp2igeu[ |G] VTTT] 1900s cosmonm: Ton hudrol cmon Si Conon Upon espe Serre DCO CT cp remesontec --_--Te=;~er.'t~,are: !)eg C [] Re,eeive~ on lee owaes en ~ Other: Sect Rdi~q~ish~d Die Time eave Sean fe PE7 CE Dat~ Time 33663300..00112244 Pages aW_No1so6073 3M MN01596073 AAPPRRIILL 22001144 33663300.~001i2255 3M_MNO1596074 3M MN01596074 rv 51 ovosre 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 FFiinnaall RReeppoorrtt FFlluuoorroocchheemmiiccaall CChhaarraacctteerriizzaattiioonn ooff AAqquueeoouuss SSaammpplleess,, CCoottttaaggee GGrroovvee GGrroouunnddwwaatteerr SSaammpplliinngg --- 22n!d QQuuaarrtteerr 22001144 LLaabboorraattoorryy RReeqquueesstt NNuummbbeerr:: 1ISSOO1111--0011.-0033--1144 Rept Dat - Dotaof LastSgrature Report Date- Date of Last Signature TTeessttiinngg LLaabboorraattoorryy 3M EHS Operations. 3M EHS Operations 33MM EEnnvviirroonnmmeennttaall LLaabboorraattoorryy BBuuiillddiinngg 226600--55NN--1177 Maplewood, MN 55144-1000 Maplewood, MN 55144-1000 RReeqquueesstteerr Jim Kotsmith Jim Kotsmith 3M EHS Operations 3M EHS Operations 3M Building 224-5W-17 3M Building 224-5W-17 SSaaiinntt PPaauull,, MMNN 5555114444--11000000 PPhhoonnee:: ((665511)) 773377--33663355 Soow, in e TZeBERTI Th tevin porehr meet th recurs.of AVSHSONEC The testing reported herein meet the requirements of ANSI/ISO/IEC 7025.2005~Ganer Rocufo ithorComopetemnceaofnTestingsand 17025:2005 "General Requirements for the Competence of Testing and Calibration Laboratories", in accordance with the A2LA Testing Certificate et: mons nat ram osba id # 2052.01. Additionally, the laboratory's quality system has been audited a eintse. colon wi os EPAGL Uo CPR and was determined to be in conformance with the EPA GLPs (40 CFR Te pr ASAa es 792) by an independent A2.LA assessment. 33663300..00112266 orcerorn PAGE 1 OF 60 M_MNO1S5607S 3M MN01596075 ey 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 SM Environmental Laboratory 3r~ Environmental Laboratory 0EnesomentaLaboratory Techil Dec: WiamK. Reagen,Pn0 3M Environmental Laboratory Technical Director: William K. Reagen, Ph.D. 3Ponce aban Ever Sonor 3M Principal Analytical Investigator: Susan Wolf Rest:Solon Gochom Report Author: Chelsie Grochow Analytical Report 1S011.01.03.14 Ana~yt~caJ Rpo~ ~S011o01o03o14 Poshomicl Craton of AqioosSal, CotagsGrove Grounthstr Fluorochemical Characteriz`aSStaiaommnpploliifnnAggq--u22en"o~uQQsuuaSarartmteerpr l22e00s11, 44Cottage Grove Groundwater Report: DoftLost Snare Report Date: Date of Last Signature 11 IInnttrorodduuccttioino/nS/uSmummmaarryy 170 SM Ervormatl anarstry roared rd analzad grndvtr same colt y Weston The 3M Environmental Laboratory prepared and analyzed groundwater samples collected by Weston Sators param a ne 4 CHage Gov Foy. Sores war coecied cn om 2335, 204 Solutions personnel at the 3M Cottage Grove facility. Samples were collected on April 23-25, 2014. Sms vars adto Exel ab onAryy ,20a on asof Samples were returned to the 3M Environmental Laboratory on April 28, 2014 on ice for the analysis of a ame ami compounds io aar s amon ROY 01-014 twelve fluorochemical compounds under laboratory project number ISO11-01-03-14. Too 3 Eviormartl Last repr url cota futon sping cats. Each The 3M Environmental Laboratory prepared sample containers for fourteen sampling locations. Each Tami so cota of 3 od Same fos kets: 37d Told th 5 Ea Sty sample set consisted of a field sample, field sample duplicate, and field matrix spike. Each empty Comair wag makes wi a Tb Fre in oa careapcot a fol vane of 200 container was marked with a "fill to here" line that corresponded to a final volume of 200 mL. Corts ered1 ad Tod sks we ood wie OB ln SH so Containers reserved for field matrix spikes were fortified with an appropriate matrix spike solution Coming ol sha it 12 bor so 10 la Tor al clan, A sul soln we containing all analytes prior to being sent to the field for sample collection. All sample bottles were {ea tn ima Samra Samo ov Saris ir 1b so 0 To fortified with internal standards and surrogate recovery standards prior to being sent to the field for ec sample collection. Sawveroipreorodand nad or PEGA, PEPGA, PEHIA, PEA, PFOA PFI PFDA, SPPFaFUmUNnpAAle,,sPPwFFeDDroeoAAp,,rePPpFFaBBrSeS,d, PPaFnFHdHSSa,,nPaPFlyFOzOeSSdafanonrddPtthFheeBsAsu,urrrProoFggPaaetteAer,rePeccFooHvvexerAryy,sPsttaFanHnddpaaArrd,dsPs(F(SSORRASS,ssP))F"1N3CAC+,3P-PPFFFBDBAAA,,, 1"3CC.4-- PPFFOOAA,, ~"3'CC.2--PPFFUUNnAA,, aanndd "13'CC.4--PPFFOOSS,, uussiinngg mmeetthhoodd EETTSS--88.-004444..11 ""MMeetthhooddooffAAnnaalylsisyfofsorritthhsee. Daminof airrocinod ComWpotabyLsOVEsS. Dee cto Ae. Determination of Perfluorinated Compounds in Water by LCfMS/MS; Direct Injection Analysis". Fiomel nnds wesoo 1s30 dt cy coves Internal standards were used to aid in the data quality objectives. FT ---------------- Table 1 summarizes the sample results using the analytical method identified above. All results for Stycont et rot ad SPATS Sao ord a tind quality control samples prepared and analyzed with the samples will be reported and discussed Somberg elsewhere in this report. 21, TN cratoEen Tot ig bimete ets o IES De testing reported herein meet the requirements of .ANSI/ISO/IEC 17025:2005 "General Requirements for the Competence of Testing and a Calibration Laboratories", in accordance with the A2LA Testing Comes amor Sadr bo sss ay ram i Certificate # 2052.01. Additionally, the laboratory's quality system has center oe SA been audited and was determined to be in conformance with the EPA Tm GLPs (40 CFR 792) by an independent A2LAassessment. 33663300..00112277 ezcrio PAGE 2 OF 60 Su umorsseors 3M MN01596076 Tete. ts Table 1. Sample Results Summary 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA Concentration Concentration Concentration Concentration Concentration Concentration Concentration 3M LIMS ID IS011-01-03-14-001 [Eom|m 2 [l osa [onm [eme |om n am =[e om] ISOll-01-03-14-002 Lo swesaml Ww [ow [TL[L 0 ISOll-01-03-14-004 Eems [ol laas olmse als e] ISOll-01-03-14-005 Lo een[oo [Tw Tae|| ISOll-01-03-14-008 LE o ewoz wmm[m |ew ol [waa [ lalm F alm eL [oe NElW [s aN]] IS011-01-03-14-009 Sample Description CGM N-GW-MW07-0-140423 CGM N-GW-MW07-DB-140423 Average %RPD Sample/Sample Dup CGM N-GW-MW12-0-140425 CGM N-GW-MW12-DB-140425 Average %RPD Sample/Sample Dup CGM N-GW-MW13-0-140424 CGM N-GW-MW13-DB-140424 Average %RPD Sample/Sample Dup E mE EE = EE2 ISOll-01-03-14-0" 2 CGMN-GW-MW14R-DB-140423 (n~mL) 2.48 2z~ 2.48 0.0 218 222 220 1.8 745 683 7.14 8.7 :45 654 0.159 0.147 0.153 7.8 24.8 24.8 24,8 0.0 0.477 0.452 0.465 5.4 280 275 0.0806 0.0749 0.0778 7.3 26.4 27.1 26.8 2.6 0.265 0.249 0.257 6.2 195 199 <0.0250 <0.0250 <0.0250 NA "1.7 11.7 0.0 0.0893 0,8674 0.0779 271~1 25,4 26.7 (n~llmL) 0351 0.336 0.344 4.4 545 55O 548 (=1 0.91 8.87 8.39 8.63 5.6 542 543 (n~/mC) <0.0250 <0.0250 <0.0250 NA 1,77 1.75 1.76 1.1 0.0503 0.0387 0.044.5 26 1.70 1.74 <0.0250 <0.0250 <0.0250 NA 1.82 1.87 1.85 2.7 <0.0250 <0.0250 <0.0250 NA 2.11 2.08 ISO11-01-0.3-14-0" 5 FE ir I AI I I I ISOll 014)3 14 0"6 LT o mam]2[SWT [A] NA= Nat Applicable Average %RPD Sample/Sample Dup CGM N-GW-MW16-0-140424 CGMN GW MW16-DB 14-~424 Average %RPD Sample/Sample Dup 650 1.4 41 .I 40.3 40.7 2.0 278 1.8 6.91 6.52 6.72 5.8 197 2.0 6.57 6.42 6.50 2.3 26,1 5.0 3.15 3,30 8.8 543 (2) 0.18 89.1 82.3 85.7 7.9 1,72 2.3 0.546 0.523 0.535 4.3 2,10 1,4 9.329 0.339 0.334 3.0 (1) Samples wore analyzod using intomal standard c~libmtion unloss notod ot~orwiso. Tho analytical mothod uncertainties associatod with tho reportod results using intornal calibration are as follows: PFBA + 18%, PFPeA + 18%, PFHxA + 16%, PFHpA + 19%, PFOA + 12%, PFNA + 19%, PFDA 19%, PFUnA + 19%, PFDoA + 18%, PFBS + 10%, PFHS + 9.3%, PFOS + or De cemrmensmmeerevsmamrmit omsmetrs 1 (2) Sample set was analyzed using extemal standard calibraLion. The analytical method uncertainties associated with the reporLed samples using etemal calibration are as 1allows: PFBA 21%, PFPeA _+ 17%, PFOA 14%, PFBS _+ 18%, PFHS 11%, and PFOS 9.9%. 2 ER amr (3) Sample/sample duplicate RP~ did not meet accapt~nca criteria of <20%. (4) NR : Not reportable; sample area counts below flqe LOQ area counts and did not meet method blank criteria PAGE 3 OF 60 sworn 3M_MN01596077 33663300..00112288 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 T`Taabbllee 11 ccoonnttiinnuueedd.. SSaammppllee RReessuultltssSSuummmmaarryy 3M LIMS ID Sample De~cdption PFBA Concentration (n~/mL) PFPeA PFHxA Concentration Concentration PFHpA Concentration (n~l/mL) PFOA Concentration (n~llmL) PFNA Concentration (n~/mC) PFDA Concentration ISOll-01-03-14-0" 9 CGM N-GW-MW101-0-140425 1330 71.8 60.9 63.2 76.1 7.08 0.248 ISOll-01-03-14-020 E I I S I A ISO11-01-03-14-050 [ ree [w2[[ ae [wT w[[2n w]= w=e T=]] ISO11-01-03-14-051 CGM N-GW-MW161 -DB-140425 Average %RPD Sample/Sample Dup CGM N-GW-MW1O2-0-140425 CGM N-GW-MW162-DB-140425 Average %RPD Sample/Sample Dup 1330 1330 (2) 0.0 924 914 919 (2) 1.1 72.6 72,2 1.1 30.7 30.6 30.7 0.33 61.3 61.1 0.65 29.1 28.5 28.8 2.1 61.4 62.3 2.9 "6.1 "5.8 16.0 1.9 75.8 76.0 (~) 0.39 58.6 57.6 ~8.1 1.7 6.84 6.96 3.4 1.84 1 90 1.81 3.2 0.233 0.241 6.2 0.143 0.129 0.136 10 ISO11-01-03-14-054 CGM N-GW-MW1034)-140425 238 27.3 57.0 31.4 117 0.0487 <0.0250 ISOll-01-03-14-055 I EC I A ISOll-01-03-14-023 as I= 121 21121= 1 ISO11-01-03-14-024 I ISOll-01-03-14-027 [Sr [maaan|2 | aa | ua | aw| | cm |om| ISOll-01-03-14-028 CGM N-GW-MW103-DB-140425 Average %RPD Sample/Sample Dup CGM N-GW-MW104~)-140425 CGM N-GW-MW104-DB-140425 Average %RPD Sample/Sample Dup CGM N-GW-MW105-O-140425 CGM N-GW-MW105-DB-140425 243 241 (=~ 2.1 107 107 107 0.0 70.3 71.7 29.1 28.2 6.4 12.7 12.4 12.6 2.4 5.86 6.24 57.8 57.4 1.4 19.9 19.5 19.7 2.0 11.7 11.8 30.4 30.9 3.2 9.08 9.13 9.11 0.55 8.38 8.89 125 121 (=} 6.6 82.0 62.1 82.1 0.12 42.7 45.9 0.0566 0,0527 15 2.57 2.60 2.59 1.2 0.577 0.588 <0.0250 <0.0250 NA 3.20 3.32 3.26 3.7 0.328 0.339 Average %RPD Sample/Sample Dup 71.0 2.0 6.05 6.3 11.8 0.85 8.64 5.9 44.3 7.2 0.583 1.9 0.334 3.3 prewm-- NA = Not Applicable (1) Samples were analyzed using internal standard calibration unless noted o~erwise. The analytical method uncertainties associated with the repoded results using internal calibration are " Ph FRE FO FAS5FOS 5Fk is PRLS FEE as follows: PFBA _+ 18%, PFPeA _+ 18%, PFHxA _+ 16%, PFHpA _+ 1%, PFOA _+ 12'Y~, PFNA _+ 19%, PFDA 1%, PFUnA _+ 19%, PFDoA _+ 18%, PFBS _+ 10%, PFHS _+ 9.3%, PFOS _+ 1~/o. (2) Sample set was analyzed using extemal standard calibration. The analy~cal method ur~certainties associated wit~ the reported samples using external calibration are as follows: PFBA _+ LE To i ev eto ete ryt se ts 21%, PFPeA + 17%, PFOA _+ 14%, PFBS _+ 18%, PFHS _+ 11%, and PFOS 4- 9.9%. (3) Sample/sample duplicate RPD did nat meet acocptance criteda of-<20%. (4) NR = Not reportable; sample area counts below ~e LOQ area counts and did not meet method blank criteria. PAGE4OF60 smworsosars 3M_MN01596078 33663300..00112299 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 T`Taabbllee 11 ccoonnttiinnuueedd.. SSaam mppllee RReessuullttssSSuummmmaarryy 3M LIMS ID Sample Description PFBA Concentration (n~/raL) PFPeA PFHxA Concentration Concentration PFHpA Concentration (n~l/mL) PFOA Concentration (n~llmL) PFNA Concentration PFDA Concentration ISOll-01-03-14-031 CGM N-GW-MW108-0-140425 59.1 10.6 9.39 3.84 166 1.15 0.516 ISOll-01-03-14-032 I2C I I I ISO11-01-03-14-035 Fre PrevailI IE I I I I ISOll-01-03-14-036 [a Ww [Wm TwT [] ow [an] ISO11-0%03-14-039 Er -Tol TaloTe aleTl, amlTol m] IS11-01-~8-14-040 CGM N-GW-MW108-DB-140425 Average %RPD Sample/Sample Dup CGM N-GW-MW110-0-140424 CGM N-GW-MW110-DB-140424 Average %RPD Sample/sample Dup CGM N-GW-PW09-0-140425 C GM N-GW-PW09-DB-140A25 Average %RPD Sample/Sample Dup 71.6 65.4 19 186 191 189 2.6 418 410 4.14 1.9 12.3 11,5 15 24.6 23.4 24.0 5.0 0.268 0 275 0.272 2.6 11.0 10.2 16 34.0 31.7 32.9 7.0 0.127 014.3 0.135 12 4.45 4.15 15 12.7 2.4 0.0443 0 [3498 0.0471 12 162 164 (2} 2.4 310 316 310 {z! 0.0 1.03 1 07 1.05 3.8 1.36 1,26 17 0.191 0.197 0.194 3.1 0.0353 0 0377 0.0365 6.6 0.607 0.562 16 <0.0250 <0.0250 <0.0250 NA <0.0250 <0 0250 <0.0250 NA IS011-01.4)8-14-042 CGM N-GW-PW" 0-0-14PA25 4.99 0 250 0 [3420 0421 <0 0250 <0 0250 -- ISO11-01-03-14-043 CGM N-GW-PW" 0-DB-140425 Average %RPD Sample/Sample Dup 515 5.07 3.2 0.254 0.252 1,6 AI 0.167 0.151 22 (3~ 0.0517 0.0469 0 420 0.421 0,24 ll <0.0250 <0.0250 NA ll <0.0250 <0.0250 NA ISOll-01-03-14-045 CGM N-GW-MW105-RB-140425 <0.0500 <0.0250 <0.0250 <0.0250 <0 04~0 <0.0250 <0.0250 ISOll-01-03-14-046 CGMN-GW-TRIP-0-'40423 <0.0500 <0.0250 <0.0250 <0.0250 <00480 <0.0250 <0.0250 NA = Not Applicable Lirem aR e (1) Samples were analyzed using internal standard calibration unless noted o~er~se. The analy'acal method uncertain'~es associated w~th t~e reported results using internal calibration are s as follows: PFBA_+ 18%, PFPeA + 18%, PFHxA _+ 16%, PFHpA _+ lg%, PFOA + 12%, PFNA _+ 19%, PFDA 19%, PFUnA + 19%, PFDoA + 18%, F'FBS _+ 10%, PFHS + 9.3%, PFOS + 16%. on Be eri e att empti eetnentastsm Pe (2) Sample set was analyzed using external standard calibratJca. The analy~cal method uncertainties associated wit]l the reparLed samples using ex[emal calibration are as follows: PFBA _+ 21%, PFPeA _+ 17%, PFOA _+ 14%, PFBS _+ 18%, PFHS _+ 11%, and PFOS 9.9%. (3) Sample/sample duplicate RPD did not meet acceptance criteria of <20%. ERE (4) NR = Not reportable; sample area counts below t~e LOQ area counts and did not meet method blank cri[eria. PAGE 5 OF 60 worsens 3M_MN01596079 33663300..00113300 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 T`abTle1a1 ccobonntitlinnuueeedd..SSaammppllee RReessuullttss SSuummmmaarryy 3M LIMS ID Sample Description PFUnA Concen~aSon PFDoA Concentration PFBS Concentration PFHS Concentration PFOS Concentration ISOll-01-03-14-001 C GM N-GW-MW07-0-140423 <0.0250 0.0357 <0.0250 00495 IS011-01-03-14-002 Lo ma] a[ew]ww[en| un| ISOll-01-03-14-004 Eomsl[aoom[aomweTeo sn , ISOll -01.-03-14-005 I RS A 18011-01-03-14-008 [ L orl [a=e m a=a wm [[n oam |s oe| IS011-01-.03-14-009 CGM N-GW-MW07- DB-140A23 Average %RPD Sample/Sample Dup CGM N-GW-MW12-0-140425 CGM N-GW-MW12-DB-140425 Average %RPD Sample/sample Dup CGMN-GW-MW13-0-140424 CGM N-GW-MW13-DB-140424 Average %RPD Sample/sample Dup ISOll-01-03-14-0" 2 EEt El EE ISOl 1-01-03-14-0" 5 [m[ amaI[-- IomTIos-- [eorlTIu-- [ur | ISOll 014)3 14 0"6 OGM N-GW-MW14R-DB-140423 Average %RPD Sample/Sample Dup CGM N-GW-MW16-0-140424 CGMN GW MW16-DB 14~424 Average %RPD Sample/Sample Dup <0 0250 <0.0250 NA 0.433 0.415 0.424 4.2 <0.0250 <0.0250 <0.0250 NA <0.0250 <0.0250 <0.0250 NA <0.0250 <0.0250 <0.0250 NA <0 0250 <0.0250 NA 0.154 0.169 0.162 9.3 <0.0250 <0.0250 <0.0250 NA <0.0250 <0.0250 <0.0250 NA <0.0250 <0.0250 <0.0250 NA 0 0363 0.0360 1.7 67.5 70.3 4,1 0.791 0.712 0/752 11 18.2 18.2 18,2 0.0 37.7 38.1 37.9 (z) 1.1 <0 0250 <6.6256 9.97 9.67 9.82 3.1 0.594 0.517 0.5~6 14 19.7 20.3 20.0 3.0 4.43 4.55 4.49 2.7 0 ~3491 0.0493 0.81 115 118 117 a) 2.6 2.46 2.20 2.33 11 348 358 353 2.8 51.4 52.4 51.9 1.9 NA = Net Applicable EE ------ (1) Samples wore analyzed using internal standard calibration unless noted otherwise. The analytical method uncertainties associated with t~o reported msull~ using internal calibration are as follows: PFBA + 18%, PFPeA + 18%, PFHxA + 16%, PFHpA + 19%, PFOA + 12%, PFNA + 19%, PFDA 19%, PFUnA + 19%, PFDoA + 18%, PFBS + 10%, PFHS + 9.3%, PFOS + 16%. (2) Sample set was analyzed using extemal standard calibration. The analy~cal method unceriainties associated with the reported samples using etemal calibration are as follows: PFBA @ Stn, er or i mi 21%, PFPeA _+ 17%, PFOA _+ 14%, PFBS _+ 18%, PFHS _+ 11%, and PFOS 9.9%. (3) Sample/sample duplicate RPD did not meet acceptance criteria of <20%. aet coe em 4 eka odSh (4) NR : Not reportable; sample area counts below flqe LOQ area counts end did not meet method blank criteria PAGE 6 OF 60 [p-- 3M_MN01596080 33663300..00113311 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. IS011-01-03-14 T`Taabbllee 11 ccoonnttiinnuueedd.. SSaammppllee RReessuultltss SSuummmmaarryy 3M LIMS ID Sample Description PFUnA Concentration (n~l/mC) PFDoA Concentration {n~llmL) PFBS Concentration PFHS Concentration PFOS Concentration (n~l/mL) ISOll-0.1-03-14-019 3GM N-GW-MW101-0-140425 <0.0250 <0.0250 37.9 364 30 ISOll-01-03-14-020 Les a| t [rT] ISOll-01-03-14-050 eole| = |=]=] ISOll-01-03-14-051 LL wma wr [TO] or | ISO1%01-03-14-054 EA rIe e elEEl EE ISO1%0%03-14-055 lL wot]Se[|To | | ISOll-0%03-14-023 Bae |oe[=] 2[21=] ISO1%0%03-14-02~. I 2 ollEE A ISOll-01-03-14-027 Fl rr i I EE ISOll-01-03-14-028 3GM N-GW-MW101-DB-140425 Average %RPD Sample/Sample Pup ~GM N-GW-MW102-0-140425 ~.GM N-GW-iVIW 102-DB-140425 Average %RPD Sample/Sample Dup 3GM N-GW-MW103-0-140425 3GM N-GW-MW103-DB-14(H25 Average %RPD Sample/Sample Pup 3GM N-GW-MW 104-0-.140425 3GM N-GW-MW104-DB-14(H25 Average %RPD Sample/Sample Dup ~.GM N-GW-MW105-0-140425 ~.GM N-GW-MW 105-DB-140425 <0.0250 <0.0250 NA <0.0250 <0.0250 <0.0250 NA <0.0250 <0.0250 <0.0250 NA 0.0489 0.0625 0.0557 <0.0250 <0.0250 <0.0250 <0.0250 NA <0.0250 <0.0250 <0.0250 NA <0.0250 <0.0250 <0.0250 NA <0.0250 <0.0250 <0.0250 NA <0.0250 <0.0250 37.6 37.8 0.79 7.'0 7.'4 7.12 0.56 6.5"1 6.5.1 6.51 0.0 7.95 8.25 8.10 3.7 7.56 7.80 364 364 (21 0.0 146 147 147 0.68 21.0 22.5 21.8 6.9 128 123 12.6 4.0 8.z~ 8.70 "34 135 1.5 67.'1 67.6 67.4 0.74 7.99 7.64 7.82 4.5 238 229 234 3.8 56.6 60.7 Average <0.0250 <0.0250 7.68 8.59 58.7 %RPD Sample/Sample Dup NA NA 3.1 2.6 7.0 NA = Not Applicable BE s T ere persT ot ta Pre e Aeretse, (1) Samplas were analyzed using internal standard calibration unless noted o~erwise. The analytical method uncertainties associated with the repoded results using internal calibration are as follows: PFBA _+ 18%, PFPeA _+ 18%, PFHxA _+ 16%, PFHpA _+ 1%, PFOA _+ 12'Y~, PFNA _+ 19%, PFDA 1%, PFUnA _+ 19%, PFDoA _+ 18%, PFBS _+ 10%, PFHS _+ 9.3%, PFOS _+ 16%. (2) Sample set was analyzed using extemal standard calibration. The analy~cal method uncertainties associated wit~ the reported samples using external calibration are as follows: PFBA _+ a 21%, PFPeA + 17%, PFOA _+ 14%, PFBS _+ 18%, PFHS _+ 11%, and PFOS 4- 9.9%. (3) Sampla/samplo duplicato RPD did nat moot acceptanco critoda of-<20%. (4) NR = Not reportable; sample area counts below ~e LOQ area counts and did not meet method blank criteria. PAGE 7 OF 60 mors 3M_MN01596081 33663300..00113322 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. IS011-01-03-14 T`Taabbllee 11 ccoonnttiinnuueedd.. SSaam mppllee RReessuullttss SSuummmmaarryy 3M LIMS ID Sample Description PFUnA Concen~ation In,mE) PFDoA Concentration PFBS Concentration tn~/mL) PFHS Concentration (n~l/m L) PFOS Concentration ISOl1-01-03-14-031 3GM N-GW-MW108-0-140425 <0.0250 <0.0250 17.8 3.32 40.2 ISOll-01-03-14-032 I ol alA ISOll-01-03-14-035 ee ee =e =T= 1=1 ISO1~-0%03-14-036 -- ISO1~-0%03-14-039 I A re l Adl A Al EE E E IS(31~-0%03-14-040 3GM N-GW-MW108-DB-140425 Average %RPD Sample/Sample Pup 3GM N-GW-MWlI0-0-140424 ~.GM N-GW- MW 110-DB-14L~424 Average %RPD Sample/sample Dup ~.G M N-GW- PW09-0-140425 ~GM N-GW-FSNOg-DB-140425 Average %RPD Sample/Sample Dup <0.0250 <0.0250 NA <0.0250 <0.0250 <0.0250 NA <0.0250 <0 0250 <0.0250 NA <0.0250 <0.0250 NA <0.0250 <0.0250 <0.0250 NA <0.0250 <00250 <0.0250 NA 17.0 17.4 Iz) 4.6 87.1 85.1 86.1 Iz} 2.3 0.150 0 145 0.148 3.4 3.84 3.58 15 21.2 20.5 20.9 3.3 0.0823 0 0~52 0.0838 3.5 46.4 43.3 14 12.4 12.6 12.5 1.6 1.62 1.58 1.60 2.5 IS(31~-0%03-14-042 ~GM N-GW-FSN10-0-140425 <0 0259 <00250 0 45O 0 105 04.38 Lo ISOll-0%03-1~043 ssa 3GM N-GW-PW10-DB-140425 Average %RPD Sample/Sample Dup Ww [WS[0[0] <0.0250 <0.0250 NA <0.0250 <0.0250 NA 0.4~1 0.471 4.5 0.115 0.110 9.1 0.435 0.437 0.69 ISOll-01-03-14-045 3GM N-GW-MW105-RB-14(H25 <0.0250 <0.0250 <0.0250 <0.0250 <0.185 ISOll-0~-03-1~046 3GMN-GW-TRIP~-140423 <0.0250 <0.0250 <0.0250 <0.0250 <0.185 NA = Not Applicable LE S (1) Samples were analyzed using internal standard calibration unless noted otherwise. The analytical method uncertain'~es associated with t~e reported results using internal calibration are E as follows: PFBA_+ 18%, PFPeA + 18%, PFHxA _+ 16%, PFHpA _+ 1%, PFOA + 12%, PFNA _+ 19%, PFDA 19%, PFUnA + 19%, PFDoA + 18%, F'FBS _+ 10%, PFHS + 9.3%, PFOS + A ETAITAREE Fever wr vommi oe mt 16%. 8 FREI enn (2) Sample set was analyzed using external standard calibratJca. The analytical method u~certaintJes associated wiLh the reporLed samples using ex[emal calibration are as follows: PFBA _+ 21%, PFPeA _+ 17%, PFOA _+ 14%, PFBS _+ 18%, PFHS _+ 11%, and PFOS 9.9%. (3) Sample/sample duplicate RPD did not meet acceptance criteria of <20%. (4) NR = Not reportable; sample area counts below t~e LOQ area counts and did not meet method blank criteria. PAGE 8 OF 60 wanes 3M_MN01596082 33663300..00113333 Re Soros 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 22 MMeetthhooddss --AAnnaalylyttiiccaall aanndd PPrreeppaarraattoorryy y22.1s1 isMMeewttahhsoocddossmplete folowing 3M Envronmental Laborotory method ETS-804 1 iethod of Analysis was completed following 3M Environmental Laboratory method ETS-8-044.1 "Method of raayys". or he Deteminaton of Perforated Compounds n Wile by LGMSHS: Dred recon Analysis for lhe Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis". TTaabblel22e.. TTaarrggeett AAnnaallyytteess TT -- Target Analytes [Pacoumooc or rTae girmes| Perfluorobutanoic Acid (CA Acid) Errere-- a---- Perfluoropentanoic Acid (C5 Acid) [Putemmmcrosconse oman | teen | Perfluorohexanoic Acid (C6 Acid) Acronym PFBA PFPeA PFHxA Reference Material Structure Linear Linear Linear Perfluoroheptanoic Acid (C7 Acid) [Putarorimniscansn--Joron| Grewrbi | Perfluorooctanoic Acid (C8 Acid) [recmmcosraa| icovr ex en| Perfluorononanoic Acid (C9 Acid) [Prasromamoeorn asicrteom seg| Periluorodecanoic Acid (C10 Acid) [Puterontcumeriscrinss pra| toe | Perfluoroundecanoic Acid (C11 Acid) [Putoropuame cizrag pron| ue | Perfluorododecanoic Acid (C12 Acid) [Pur ores | ni toe a| Peffluorobutanesulfonate (C4 Sulfenate ) e PS T ------ Perfluorohexanesulfonate (C6 Sulfonat~) Couronnecostan) ros | row berms | Perfluerooctanesulfonate (C8 Sulfonate) PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHS PFOS Linear Linear Branched Linear Linear Linear Linear Linear Linear Linear Branched 22 Sample Collection 2.2 Sample Collection S`Saammpplleess wweerree ccoolllleecctteedd oonnAApprriil 2233--2255,, 22001144 iinn NNaallggeneenTeMTM ((hhiigghh--ddeennssiittyy ppoollyyeetthhyy/leenree)) bboottttlleess pprreeppaarreedd athe SH Envicrments Laboratory. Port samp calecton, bolle designatedforfeid mar at the 3M Environmental Laboratory. Prior to sample collection, bottles designated for field matrix pk wore Ske in Ie borat ih a Known youre of an propre mati Soi Soon spikes were spiked in the laboratory with a known volume of an appropriate matrix spiking solution Sonning Th anaof eeess All SampleDoes are Spike wiha me ofmassab0ed containing the analytes of interest. All sample bottles were spiked with a mixture of mass-labeled tema iadords at. nominal concertofo1 nin andwih surat recoverystandard internal standards at a nominal concentration of 1 ng/mL and with surrogate recovery standards (SRS) at nominal concentratfi0o1n ng. Calocied sample bolies were rsumed o ho (SRSs) at a nominal concentration of 0.1 ng/mL. Collected sample bottles were returned to the lecrstry onco61 At 28 204 laboratory on ice on April 28, 2014. A22l..3s3ompSSlaaemsmwppelrleeepPPrrerpeeappraeardrbaatytiirooennmoving 0.4mlaliquot fhe wolmedsampl and iuing with A0l4l smaLmpoflemsewthearneoplre(pBaureodnfbaycrteomrov2in.g a 0.4 mL aliquot of the well mixed sample and diluting it with 0,4 mL of methanol (dilution factor of 2). SSmeeambmpipealesnslrreeTqqhuueiirninsgganaap11i::n11g000cadctiuluiftooionnnswwtehearrlerpprereeeppaadrreedddbboyynGdiiluwntiengrg0e0.p.11rmemirLoeofdfbssayamamdpdlpeinliwgtiethhon99.u99momLLts ooofffa Smog methanol. surrogate standard slob arane concenetoofn1 GL The sampling locations that required dilution were prepared standard solution at a nominal concentration of I ng/mL. by adding an aliquot of a DpDuurhriinnngg thshoeelupptrireopenwaparaastrioaandotoofief otdhhe1netalahtboorraabtoorryaclcooornnyttorcolol ssnaacmvpeslsaem,sp, laaennsas(lihuqouomoit nooaffacosnescpeeaanrvatstaeetnoinnltemornaf1allgsstaalcnde)arrddThe spiking solution was added to the laboratory control samples (nominal concentration of 1 ng/mL). The SSaarmtpsebntiootwhafrleedS0pldsaemwpilheacollecakona. sTenanedaabrdcaitorayt connokmoilnsalacoenwecres rtetonfo1digedLipnr > sample bottles were spiked with an internal standard mix at a nominal concentration of 1 ng/mL prior to mbeeitnhgasnetnitntoththoseafiemldemfoarnsnama pale he samples. collection. The laboratory control samples were then diluted with methanol in the same manner as the samples. 33663300..00113344 orcesorm PAGE 9 OF 60 M_MNO1S56083 3M MN01596083 REPORT KO 01014 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 A22ll.44sAAonnaamlalyynsdspqiissulayoconstol samplos were aayzedfor wove target analytes using igh Apppaelelrrrsaffoamormemmlpaealrnensccs,eeatnilieqduuqqiiduiacclhhitrvycoohmcmroaaonttmtoroaoggllrroasagparphmanypyp/thtlaeyansngdwdreaeemdmrieemmnaatansspassrlyosszgpoereeadccmfrt,oroorammtenwetdetrrlhyyvee((HtsaPPpreLgcLCeift/CiMacnSSma/aMl)ystSes.)s. uaPPsreiesnrirgtttinnoheneisngn.thtaininnasslttryruzumemdeenntt ve doscribec ne tables bao. parameters, the liquid chromatography are described in the tables below. gradient program, and the specific mass transitiens analyzed DeDunuveeirotootnhtmheeenntanataluturareeocofcftthhueesrsaamormpfelpmelenu,, chttheeewwiiiddseoemrreaarnnsggoeefootffeccoolnnaccbeenontrrtaratatotiirooynnssafofnouaunnyddioiinonsftthhteeesrsaeamsmpt,lpelteh,,eaaSnnoddftttwhhaeere used ffeIoonnrtvoppigrrrroooancctmeieossenssoniintfnagtglhottehhceecanunaaranlrlayetylnyiicctcieacalalopl freamesisuuulltlltipsslneiesncinseoosotstmaaaerbiyrlse.e ottAofocltchoomenanslnsaiiubssaoteelrnantrttolyyorgyminr'astagealrgnoaraanltlseyeathethoseeoapafnnoianarytlfeyirotceicmasaolt,ldptphfeeeoaalkkso,,owfmimtnwaaganntruenaaelused preipnonrtocsecuegerdradeutudrioretenssooouofuugtththileinnheeaddneai1anlyitmmicneeanttlhhgpooeoddfaEEklTaTibsSSo.nr-1ae1t22co.-er00sy11s00pa.e.r11yr..s. oTTAnhnhlleeelmc,coaonhnnseusiaisspltteieenennrteccrygyoerofavtfitiheothewnesprllaaoarbceboeorpsraesatrortefrooqyrru'smsyireiinendttdeeffoggorlrlraaottwiaioloinnnmgiastnhueal eIIinnnnttteseoguggrrrraeaattdtiiioootnnhnssrs,bo, uyhthgeleharrbteheovveriiaetetrwwaoiroonyffinmmmgaaannonaufugalaaellbmoIiennrnttaetetg.ogrrraayttiipooennrssbsobynytnthehlee, QAU. and where necessaryte review the peer review process required for all QAU, and where necessary the review of manual manual of manual integrations by laboratory management. TTaabblleo 33.. IInnssttrruummeenntt PPaarraammteeterrss.. [Instrs umenm t Namm e | eoteErh TSsKiia rmk me| Liquid Chromatograph [Ans| tyssEsmsoomoa| Analysis Method [Anatyinvote |siasia,sarasaa | Analysis Date Agilent 1200 or 1260 ETS-8-044.1 5/6/14, 5/12/14, 5/13/14, 5/14/14 Guard column Betasil C18 (4.6 mm X 100 mm), 5 |AAnnaatltytcicnatl ccoolluummnn | BBoettsassil C01188 46x"COmm 84 (4.6 mm X 100 ram), 5 | [nfIoncjetcitoionn VVooltumree| s5aorr i10o~wL | [MaMsasssSSppecetcrtroommeteeterr | 4A8B SScciieexxTToripplee Quuaaad 8525000 | [onIosn oSowureceo TT mTuirbbooSsppramyy | [poPtolatryity TT MeNgeguantivee | [soma Software | wager Analyst 1.6.1 | TTaabbllee 44.. LLiiqquuiidd CChhrroommaattooggrraapphhyy GGrraaddiieenntt PPrrooggrraamm.. Step EEiTni} P me |g e ao Number Fo Tow Tm[ Emsam eT 60 1 0 ET ow To[ao Teo | 1 Total Time (min) 0100 0.50 Flow Rate (l.tL/min) Percent A (2 mM ammonium acetate) ETS-8-044.1 Analysis 750 90.0 750 90.0 Percent B (Methanol) 10.0 10.0 2 4.00 750 EsTew Tmo mo 1 wo 1 3 6.00 750 FoTmTw Tw o o | 4 11.0 750 Esme 1 wo a0 00] 5 13.0 750 70.0 70.0 20.0 20.0 30.0 30.0 80.0 80.0 ows me | wo | wo | 6 13.5 750 Er woTmo [veo 1 wo 7 16.0 750 eT es | veo [oo 1 00 1 8 16.5 750 10.0 10.0 90.0 90.0 90.0 10.0 CoTwoTmTwoTo] 9 19.0 750 90.0 10.0 33663300..00113355 Face 00rm PAGE 10 OF 60 3M_MNO1596084 3M MN01596084 Re Soros 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 Table 5. Mass Transitions Table 5. Mass Transitions [=[FoEva ] mer[om Analyte ES-- TTS------ PFBA Mass Transition Q 1 IQ3 2131169 Internal Standard (1) [13C4]PFBA Mass Transition QI IQ3 217/172 PFPeA IE Come1 PFHxA EE = PFHpA 263/219 313/119 3131269 3631319 363/119 on [I~CsIPFPeA [~SC2]PFHxA [I~C4]PFHpA 268/223 315/270 367/322 4131369 |e EE PFOA 4131219 4131169 [sn| 4631419 ro Cae| PFNA 4631219 [13C~]PFOA eee corm [13Cg]PFNA [ee 4211376 472/427 IT 463/169 5131469 PFDA saa] o- = = o asr a e|| PFUnA 513/219 5131269 5~31519 5631269 5631219 613/569 ror [13C6]PFDA [I~c7]PFUnA =519/474 570/525 o- PFDoA | 6131319 6131269 rere [lSc2]PFDoA 615/570 fePFBS [me PFHS 299/80 ---- 299199 I 399/99 Fmd 399/80 ---- 499/99 yrs come 303184 402/80 PFOS |e aw] 499/80 4~91130 rere 507/80 [oprossmae [I~C3]PFBA surrogate [13C4]PFOA surrogate | smn| 2161172 4171372 Tepron| [~3C4]PFBA [~3C~]PFOA woe] 217tl 72 421/376 [~3C4]PFOS surrogate 503/80 [~3C~]PFOS 507/80 [ofa | wom | opmm | ones | [lSC~]PFUnA surrogate 5651520 [13C7]PFUnA 570/525 rtsrrvs eka roecl rm 1274 0dS13 (1) Intemal standard was not used for the external calibration analysis on 5/12J14 and 5/13/14. Ad hb ias r cnSB.Obi ener 2050 osc sin A scheduled M RM was used for the initial analysis on 5/8/14. Otherwise, the dwell time was 20 or 50 msec for each transition. The individual transitions were summed to produce a "total ion chromatogram" (TIC), which was used for quantitation. 33663300..00113366 once nore PAGE 11 OF 60 M_MNO1S56085 3M MN01596085 Re Soros 3M ENWRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 33 DDaattaa AAnnaallyyssiiss 33.11 CCaalliibbrraattiioonn Intonat cattration analysis: Internal calibration analysis: Spwioreaenalsyz againa! mabixlched sie scope trl standard cabrio curve. Samples were analyzed against a matrix-matched stable isotope internal standard calibration curve. Colbratonstandardswere propyr$eprdg how aito ox e crsro SDcf 5L050 Calibration standards were prepared by spiking ~<nown amounts of stock solutions into 50 mL of 50:50 ieceatory reagentvelo: mith. Tho cltation standard contained 1 rel standard icta laboratory reagent water: methanol. The calibration standards contained an internal standard mix at a noinel sorcenrelo0n5 ng. Akao fourteen catratonslanderdsangng rom 00125 nominal concentration of 0.5 ng/mL. A total of fourteen calibration standards ranging from 0.0125 Pain i0 100rimL (nowemreainalnyzeadwliht)e repered same. Of hse fourteen alban ng/mL to 100 ng/mL (nominal) were analyzed with the prepared samples. Of these fourteen calibration Sardar, ton cotained he SuTaocgonceantreatiosn ergngfom D025 rg (0 10 mL standards, ten contained the surrogates at concentrations ranging from 0.0125 ng/mL to 10 ngfmL {nomina) Tho analyses of PEOS on 5/1411 consisted of caren siandardsrangingfom (nominal). The re-analysis of PFOS on 5/14/14 consisted of nine calibration standards ranging from 0CT25 n/m 10S nym. (rominal). Aut, 1 weighted, calbraoncurveof alo. tho 0.0125 ng/mL to 5 ng/mL (nominal). A quadratic, 1/x weighted, calibration curve of the ratio of the Saaspos roacousove Ih ina SardpeakareaCuswes Sed he dita or standard peak area counts over the internal standard peak area counts was used to fit the data for Sach anaes. Tecatswersno roadIDL 760 ing hen procs CAAT Th each analyte. The data were not forced through zero during the fitting process. Calculating the Canc concantatons us pereaa 1k0S vd 0 TESLA CAIabon Cu cored standard concentrations using the peak area ratios and the resultant calibration curve confirmed accuracyofeachcrv pont. Th erence sincards ofPEAand PEGS. fopepare ho accuracy of each curve point. The reference standards of PFOA and PFOS used to prepare the Calbraton standards consstad of bots near 3 branche Somers. calibration standards consisted of both linear and branched isomers. Extarmal catbration analysis: External calibration analysis: Sorweproloyzs againatn ctomal standard calbaton crv. Colbrton standards vere Samples wore analyzed against an external standard calibration curve. Calibration standards were veparedby sping kon amoaf fueslnook tsoulsan containing hearget anaes lo 10 prepared by spiking known amounts of the stock solution containing the target analytes into 90:10 Inebnanl LQ laboracy water Aioflon spked sora arg fom 002 ng 125 methanol: Milli-Q laboratory water. A total of ten spiked star~dards ranging from 0.02 ng/mL to 25 IL (Corwerie nnaas), TheSandards ao contained he utoatgconacenetratsors ng/mL (nominal) were analyzed. The standards also contained the surrogates at concentrations fanging om 0.n0g 2 1025 ng nominal. Aquacratc, x wood. calbralion cue of 00 ranging from 0.02 ng/mL to 25 ng/mL nominal. A quadratic, 1/x weighted, calibration curve of the Saridpo are counts as used 1 1 In data or each arate. Th datawer ot cedtrough standard peak area counts was used to fit the data for each analyte. The data were not forced through 201 tng re ng process. Calan he slandarsconoanatons 31hp) ka cons an zero during the fitting process. Calculating the standard concentrations using the peak area counts and Fe rest! cabraton cave come troaf eacchcyue pont. Th efovence andesof the resultant calibration curve confirmed accuracy of each curve point. The reference standards of POAand PROS se prepare he lation sasonn st ofd bonnesnd branched PFOA and PFOS used to prepare the calibration standards consisted of both linear and branched isomers. Eachcurv portwas cuantlated using ihe vera catraton ceand vivor aicourdcy. Each curve point was quantitated using the overall calibration curve and reviewed for accuracy. Metnod cabrio aceracy roquof 0r025e9 (m100a130n% orthe anest cur pot)were met Method calibration accuracy requirements of 100_+25% (100_+30% for the lowest curve point) were met oral anabtes. The corlaion coefcent 1) wes reertan 0.9fo0ra5l ana. for all analytes. The correlation coefficient (r) was greater than 0.995 for all analytes. 32 System Suitability 3.2 System Suitability Rcalteaton stanasdaanaryzde ot tesa hebegining of heanayicalsecence o A calibration standard was analyzed four times at the beginning of the analytical sequence to monster sysem SAN. Th Acceptance refotSrym Sut aie fess demonstrate overall system suitability. The acceptance criteria for system suitability samples of less iranor oqtuo 5a4 lav standard ceviaton (SfopDo )re rato and etek a cera of than or equal to 5% relative standard deviation (RSD) for peak area ratio and retention time criteria of Joahanor oq o 25 RSD,wor rot oa antes. less than or equal to 2% RSD, were met for all analytes. 33..33 LLiimmiitt ooff QQuuaanntitittaattiioonn ((LLOOQQ)) The OQas define methodETS-3.08.1 th lowest ncoalbratonstarcard nh cave The LOQ as defined in method ETS-8-044.1 is the lowest non-zero calibration standard in the curve Ira mats oar and curacy roueomannd otrwhich hea counts ao at eas Ws ose of that meets linearity and accuracy requirements and for which the area counts are at least twice those of Ire appropri banks. Tre LOLS associated wih 1h Sama nayssas isd he Tabl6e. the appropriate blanks. The LOQs associated with the sample analysis are listed in the Table 6. 33663300..00113377 once zor PAGE 12 OF 60 M_MNO1S56085 3M MN01596086 msn 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 _ Table 6. LOQ [oe ae[mLael[aime[| Analyte emaTowTso TwTm 1] PFBA oes Tomo[wa | 20 [wa | PFPeA eee Tom | wa ww PFHxA ror 1 ome | wa | ww| PFHpA roa 1 oom Tam [ww| PFOA emu Tom Twa | wa [wm | PFNA roa Tom Twa wa PFDA mm 1om TwaTwTw| PFUnA ra 1 om Twa ww| PFDoA [ems 1 ow | 20 [wa [wm | PFBS 518114 LOQ, ng/rnL (1) 0.0500 0.0250 0.0250 0.0250 0.0480 0.0250 0.0250 0.0250 0.0250 0.0250 5112/14 LOQ, ng/mL (=) 5.00 NA NA NA 4.79 NA NA NA NA 2.00 5/13/14 LOQ, nglrnL (=) NA 2.00 NA NA NA NA NA NA NA NA 5/14114 LOQ, ng/mL NA NA NA NA NA NA NA NA NA NA CmTe eEE esa PFHS 0.0250 2.00 NA NA PFOS En, NA = Not Applicable 0.185 1.85 NA 0.0232 (1) Dilution faclor of 2 was applied to lhe LOQ. A for m E e (2) Dilution factor of 100 was applied to lhe LOQ. 33..44 CCoonnttiinnuuiinngg CCaalliibbrraattiioonn `DDuurriinngg tthhee ccoouruseorofsftthheee aannaallyyttiiccaall sseeqquueennccee,, sseevveerraall ccoonnttiinnuuiinngg ccaalliibbrraattiioonn vveerriiffiiccaattiioonn ssaammplpeless. (CCVs) were analyzed to confirm that the instrument response and the initial calibration curve were still in control. All reported results were bracketed by CCVs that met method acceptance criteria of 100%+25%. 3.5 Blanks EEREre, Three types of blanks were prepared and analyzed with the samples: method/solvent blanks, field/trip blanks, and sampling equipment blanks. Each blank result was reviewed and used to evaluate method performance to determine the LOQ for each analyte. pr------ 3.6 Lab Control Spikes (LCSs) RB EEEEETeT g Low, mid, and high lab control spikes were prepared for the target analytes and analyzed in triplicate, while only low and high lab control s#ikes were prepared for the surrogates. LCSs were prepared by spiking known amounts of the analytes into 10 mL of laboratory reagent water containing calcium and B PpaA E n LE magnesium to produce the desired concentration. The LCSs were then diluted with methanol or in the same manner as the samples. Method ETS-8-044.1 states that the average recovery of LCSs at each Ls spiking level must be within 80%-120% with a RSD -<20%. All LCSs meet these criteria and were used to evaluate the analytical method uncertainty in section 3.7 of the report. eir--p-- The following calculations were used to generate data in Table 7. a -- Calculated Concentration LCS Percent Recovery = * 100% Spike Concentration Loswnso Simeon Ca"Sc. gy, LCS% RSD standard deviation LCS replicates. 100% average LCS recovery 33663300..00113388 PAGE 13 OF 60 3M MN01596087 REPORT KO 01014 3M ENWRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 TTaabbllee 77.. LLaabb CCoonnttrrooll SSppiikkee RReessuultltss.. ETS-8-044.1 Internal calibration Analyzed 5/8/14 Lab ID 5Spiked Concentration (ng/mL) PFBA potCalculated Concentration (ngtmL) " %Recovery oySpiked Concentration (ng/mL) PFPeA rg) Calculated Concentration (ng/mL) co %Recovery LCS-140507-1 O. 198 0.210 106 0.198 0.193 97.6 wE es weI ra EFIE ozsIEIEom IE oirEE wr LCS-140507-2 LCS-140507-3 0.198 0.198 0.210 0.2"15 106 0.198 108 0.198 0.199 0.197 101 99.7 Average _+ %RSD 107% _+ 1.1% 99.4% _+ 1.7% LCS-140507-4 wes wroere LCS-140507-5 LCS-140507-6 Average 4- %RSD sonra LCS-140507-7 wswoura LCS-140507-8 Los wore [avemgeswrso | LCS-140507-9 Average _+ %RSD 19.8 20.9 106 19.8 21.0 106 EHE 2s. HEos HEER22EER 19.8 20.6 104 19.8 20.7 105 19.8 21.5 108 19.8 21.2 107 05. 79.0 ans 79.0 vowsosms 79.0 106% 4-1.9% 80.5 81.5 82.3 103% _+ 0,97% 106% 4. 0.94% 0 0 2) 102 79.0 79.0 100 m0 mo 3 103 79.0 79.0 100 m0 nr for 104 79.0 79.7 101 | owsesw | 100% _+ 0.58% ETS-8-044.1 Eer sos. Internal calibration Analyzed 5/8/14 Spiked Concentration Lab ID (ng/mL) rr ota LCS-140507-1 ws wosrz oro LCS-140507-2 Los wosra ose [Avomgeswrso | LCS-140507-3 Average 4- %RSD 0.198 0.198 0.198 LCs ora LCS-140507-4 Los osrs LCS-140507-5 19.8 19.8 coCncaontmsion PFHxA Calculated Concentration (ngtmL) ore0.188 ore0.188 oso oswsoree 0.190 95.3% 4. 0.74% 0720.7 m220.2 %Recovery 295.2 ur94.7 196.1 I105 "102 PFHpA Spiked Calculated Concentration Concentration (ng/mL) or os 0.198 om ois 0.198 ose orm 0.198 | we com2s9zen wo | 19.8 a =a 05 19.8 (ng/mL) 0.185 0.175 0.179 90.7% 4. 2.6% 20.9 20.8 %Recovery 93.3 88.6 90.3 106 105 [Average +us| out 220% LOS-140507-6 Average 4- %RSD 19.8 21.1 106 104% _+ 2.0% 19.8 21.7 109 107% 4.1.9% LCS-140507-7 79.0 78.6 99.5 79.0 76.5 96.8 LOS-140507-8 re EERE AER LCS-140507-9 [amopewss| waweeem 1sme] Average 4- %RSD 79.0 79.0 78.0 72.9 96.8% 4- 4.1% 98.7 92.3 79.0 79.0 75.0 76.1 96.0% 4-1.0% 94.9 96.3 a1)=LCoSt4SAptdcaore hurof quanfcaton NA = Not Applicable (1) LCSs spiked above the upper limit of quantification. 33663300..00113399 Face orm PAGE 14 OF 60 3M_MNO1596085 3M MN01596088 REPORT KO 01014 3M ENWRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 TTaabbllee 77 ccoonnttiinnuueedd.. LLaabb CCoonnttrrooll SSppiikkee RReessuullttss.. ETS-8-044.1 Eesr as | Internal calibration Analyzed 5/8/14 p a| PFOA (Linear + Branched) om] PFNA Spiked Concentration Lab ID Los var LCS-140507-1 wswosrz LCS-140507-2 Los srs [Avemgeswrso | LCS-140507-3 Average _+ %RSD Cswonra LCS-140507-4 Los wosirs LCS-140507-5 (ng/mL) orto0.190 ors00.190 oro0.190 19.0 19.0 Calculated Concentration (ngtmL) arse0.196 om0.171 om esmwsesn 0.179 95.8% + 6.9% 18.6 18.2 %Recovery To103 2090.0 pers94.3 098.0 wo96.0 Spiked Calculated Concentration Concentration (nglmL) ore ror 0.198 ome ow 0.198 or om 0.198 | we essw2s1a5 en wo | 19.8 a 20 on 19.8 (ng/mL) 0.194 0.182 0.192 95.5% 4- 3.4% 21.5 20.0 %Recovery 97.9 91.8 96.9 108 101 LCS-140507-6 [Awogoevmso| "owosaee | Soe at Average 4- %RSD LCs osra nn we oo 72 LCS-140507-7 Loswosra ma oz mo nt LCS-140507-8 19.0 75.7 75.7 19.5 99.0% 4- 3.6% 73.1 71.3 103 96.6 94.2 19.8 79.0 79.0 21.7 106% ~- 4.1% 77.2 78.1 109 97.7 98.8 [awogeswmso | LCS-140507-9 Avera1e _+ %RSD 75.7 Teont ETS-8-044.1 onalcaten Internal calibration onswsasn 76.7 97.3% 4- 3.5% | eswezaw | 101 79.0 80.5 102 99.5% 4- 2.2% Anal~/zed 5/8/14 PFDA PFUnA Lab ID Spiked Concentration (ng/mL) Calculated Concentration (ngtmL) %Recovery Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery LCS-140507-1 Laes pwosnrs LCS-140507-2 LCS-140507-3 Average + %RSD 0.198 0.175 88.4 0.198 0.183 92.3 E oie HoE se I0 HoE s EoiRE 0.198 0.198 0.198 0.198 100 0.198 100 0.198 0.190 0.190 95.9 95.8 96.1% _+ 7.0% 94.7% _+ 2.2% LCS-140507-4 19.8 19.8 100 19.8 20.7 105 LCS-140507-5 Les wours LCS-140507-6 [Awogewmso| Averac~le 4- %RSD 19.8 19.8 19.2 10519.6 owmeiwe 98.7% 4- 1.5% 97.1 = | wem2eam | 98.9 19.8 20.0 101 19.8 21.3 108 105% 4- 3.3% LCS-140507-7 79.0 76.8 97.3 79.0 80.2 101 LCS-140507-8 LE es orsIERnsEI 0 E mo EoR r E @ LCS-140507-9 [Avwrage vrs | Ss 14% [Towson] Average 4- %RSD 79.0 79.0 77.8 79.3 98.6% 4- 1.4% NA= Not Alco NA = Not Applicable 1) L0545p are urbe of qsmtctin (1) LCSs spiked above the upper limit of quantification. 98.5 100 79.0 81.2 103 79.0 80.7 102 102% _+ 0.98% 33663300..00114400 Face sore PAGE 15 OF 60 3M_MNO1596089 3M MN01596089 REPORT KO 01014 3M ENWRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 TTaabbllee 77 ccoonnttiinnuueedd.. LLaabb CCoonnttrrooll SSppiikkee RReessuullttss.. ETS-8-044.1 Ee esas | Internal calibration Analyzed 5/8/14 0[a] PFDoA PFBS Spiked Concentration Lab ID (ng/mL) Los var ora LCS-140507-1 wswosrz ore LCS-140507-2 Los srs ote [Avemgeswrso | LCS-140507-3 Average _+ %RSD 0.198 O. 198 0.198 Cswonra LCS-140507-4 Los wsers LCS-140507-5 19.8 19.8 Calculated Concentration (ngtmL) I0.199 orsO. 194 oso sawwsasn 0.190 98.4% + 2.5% 0720.7 420.4 %Recovery To101 298.2 pe96.1 105 103 Spiked Calculated Concentration Concentration (ng/mL) ore ors 0.198 ome ois O.198 or oro 0.198 | we erowsasw | 19.8 a19.8 (ng/mL) 0.165 O. 175 0.180 87.5% 4- 4.2% 17.9 17.1 %Recovery 83.5 88.3 90.7 90.4 86.5 LCS-140507-6 [Auwrage + eso | Average 4- %RSD 19.8 rr LCS-140507-7 79.0 Les wosira LCS-140507-8 79.0 wos wore [awogeswmso | LCS-140507-9 Avera1e _+ %RSD 79.0 Tseont ETS-8-044.1 onalcaten Internal calibration 21.2 oss on 105% -+ 1.9% ws82.5 ws.80.5 ans Sowsosrs 81.4 103% 4- 0,97% 107 19.8 17.9 90.6 [emeaen 89.2% 4- 2.6% oo Suoa 104 79.0 >ULOQ NA mo suoa 102 79.0 >ULOQ NA mo suon 103 79.0 >ULOQ NA | wn | NA i1) Analyzed 5!8/14 PFHS PFOS (Linear + Branched) Lab ID Spiked Concentration (ng/mL) Calculated Concentration (ngtmL) %Recovery Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery LCS-140507-1 0.198 0.198 99.8 0.184 0.183 99.4 Laes pwosnrs E oie oE us mE 2 oie LCS-140507-2 0.198 0.183 92.6 0.184 0.210 114 LCS-140507-3 0.198 0.175 88.2 0.184 0.194 106 Average + %RSD 93.5% + 6.3% 106% --. 6.9% LCS-140507-4 Les wours LCS-140507-5 LCS-140507-6 Avera~le __. %RSD 19.8 19.8 19.8 19.5 19.6 19.4 98.4% 4- 0.58% 98.6 98.9 97.8 18.4 19.7 107 20 ww 18.4 18.8 102 18.4 20.0 109 106% 4- 3.4% LCS-140507-7 79.0 70.7 89.5 73.2 74.7 102 B Lese ors [plnlm py ls n ]x56 [=es] LOS-140507-8 79.0 71.9 91.0 73.2 76.5 105 LCS-140507-9 79.0 70.6 89.3 73.2 76.6 105 Average 4- %RSD 89,9% 4- 1,0% NA= Not Alco NA = Not Applicable 1) L0545p are urbe of qsmtctin (1) LCSs spiked above the upper limit of quantification. 104% ~- 1.7% 33663300..00114411 Face orm PAGE 16 OF 60 3M_MNO1596090 3M MN01596090 REPORT KO 01014 3M ENWRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 TTaabbllee 77 ccoonnttiinnuueedd..LLaabb CCoonnttrrooll SSppiikkee RReessuullttss.. ETS-8-044.1 Internal calibration Ee esas | o co=Cna,ccatnsrisee idon |CorScoohnessan|| Co"cnoecmoapunrtiemomeansen Analyzed 5/8/14 Spiked Concentration ~3C3-PFBA Calculated Concentration Spiked Concentration ~C4-PFOA Calculated Concentration Lab ID Los var LCS-140507-1 wswosrz LCS-140507-2 Los srs [Average +us| LCS-140507-3 Average _+ %RSD Cswonra LCS-140507-4 Los wsers LCS-140507-5 (ng/mL) or0.197 oir0.197 or0.197 1.97 1.97 (ngtmL) or0.192 oar0.207 ore or saTn 0.197 101% + 3.7% 202.02 i1.99 %Recovery nr97.7 05105 Py99.8 re103 on101 (nglmL) or ome 3 0.198 or ozo 0.198 orm ors 2 0.1 98 oweeren 1.98 7 1.98 (ng/mL) 0.208 0.210 0.183 101% _+ 7.4% 1.98 1.91 %Recovery 105 106 92.6 100 96.7 [Averagesuso LCS-140507-6 Average _+ %RSD Er ETS-8-044.1 enetcateo Internal calibration poses Analyzed 5/8/14 Lab ID rr LCS-140507-1 ws wosrz LCS-140507-2 | 1.97 enn 1.98 102% -+ 1.1% Sohos | "CCa.eouriusndn Spiked Conconiesion| Concanirsion Concentration I~C2-PFUnA Calculated Concentration (ng/mL) oro0.198 ote0.198 In~ltmL) ores0.185 oze0.208 101 %Recoven/ ws93.5 0s105 samen 1.98 1.97 98.7% -+ 1.8% Sobes | "Cocl.opursooss Spiked Conconiesion| Concanin Concentration I~C~-PFOS Calculated Concentration (ng/mL) or0.189 or0.189 (ng/mL) os0.188 on0.189 99.4 %Recovery 0499.4 we99.8 [awogersnso | LCS- 140507-3 Average %RSD O. 198 `onweerae O. 183 96.9% _+ 7.3% 92.2 1 eemeezen | O.189 O. 181 98.3% _+ 2.4% 95.6 LCS-140507-4 1198 2.05 104 1.89 1.99 106 we= s wsra [zle 200 l=0 lele i ]] LCS-140507-5 LCS-140507-6 1.98 1.98 1.97 2.06 99.7 104 1.89 1.89 1.86 1.92 98.4 102 Average %RSD 103% _+ 2.4% N1)A=LCoSt4dStpcareahausritof quantcaton NA = Not Applicable (1) LCSs spiked above the upper limit of quantification. 102% _+ 3.7% 33663300..00114422 ence orm PAGE 17 OF 60 3M_MND1596091 3M MN01596091 on 3M ENWRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 Table 7 continued. LasControl Spke Results. Table 7 continued. Lab Control Spike Results. Er cern ETS-8-044.1 External calibration Analyzed 5/12/14 PFBA . PFOA (Linear + Branched) [ me ol Je i SE [| Lab ID aa a LCS-140512-1 ivonez | ou | aw a LCS-140512-2 me | ow | om l= LCS-140512-3 rer Tr an Average _+ %RSD oma rn oo LCS-140512-4 vos = = LCS-140512-5 LCS-140512-6 [isa asa | Teiso Han Average 4- %RSD Tm Tat = LCS-140512-7 a | wm =] = - LCS-140512-8 LCS-140512-9 Camo Tra pg] Average _+ %RSD Spiked Concentration (ng/mL) 0.199 0.199 0.199 1.99 1.99 1.99 20.0 20.0 20.0 Calculated Concentration (ngtmL) 0.270 0.197 0.2"12 114% + 17% 2.30 2.30 2.33 116% 4- 0.86% 22.5 22.1 22.2 111% + 1.4% %Recovery 136 99.1 107 Spiked Concentration (nglmL) 0.191 0.191 0.191 116 1.91 115 1.91 117 1.91 113 19.1 110 19.1 11 "1 19.1 Calculated Concentration (ng/mL) 0.221 0.205 0.2"10 111% ~- 4.1% 2.17 2.21 2.25 116% ~- 1.7% 21.3 22.0 21.6 113% ~- 1.4% %Recovery 116 107 110 114 116 118 112 115 113 Tw ETS-8-044.1 frExternal calibration Analyzed 5!1 2/14 PFBS PFHS Lab ID Spiked Concentration (ng/mL) Calculated Concentration (ngtmL) %Recovery Spiked Concentration (nglmL) Calculated Concentration (ng/mL) %Recovery corms | ow | oe | LCS-140512-1 LCS-140512-2 frLeCeSr-140512-3 0.199 0.248 0.199 0.212 (m 0.199 l0.m 218 Average 4- %RSD 114% _+ 8.7% mw | ow| om 125 0.199 0.227 114 107 0.199 0.200 101 109 m0.19] 9 m 0.212 n] 106 107% ~- 6.1% reve] LCS-140512-4 LCS-140512-5 (oon LCS-140512-6 1.99 2.36 119 1.99 2.40 120 sla] 1.99 2.36 119 - | = 1.99 2.29 115 1.99 2.32 116 E 1.99 lE 2.37 x] 119 Averac~le 4- %RSD 119% 4- 0.49% mt ml Z| 2 LCS-140512-7 20.0 22.3 11 "1 LCS-140512-8 20.0 22.3 112 \eLCoSr-1o40n51n2s-9 (zal 20.0 22.7 113 noseYe opr io t mtn Average 4- %RSD 112% 4- 0.89% NA = Not Applicable (1) LCSs spiked above the upper limit of quantification. 117% ~- 1.8% RE 20.0 22.0 110 20.0 22.1 111 ls 20.0 l= 22.3 51] 11 111% 4- 0.52% 33663300..00114433 ee worm PAGE 16 OF 60 su_woreceos2 3M MN01596092 on 3M ENWRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 Table 7 continued. Las Control Spke Results. Table 7 continued. Lab Control Spike Results. Er cern ETS-8-044.1 External calibration Analyzed 5/12/14 fiePFOS (Linear + Branched) coro ~C4-PFOS == = Lab ID aT ae a eae LCS-140512-1 ivomaz | om | om | ww [ow | wm LCS-140512-2 mre | om | om | Worm] LCS-140512-3 amen | "page Fe gy Average _+ %RSD oma TT LCS-140512-4 vos mln] =| = LCS-140512-5 LCS-140512-6 [isa asa | a ro Average 4- %RSD Cerny TR LCS-140512-7 fread nl = LCS-140512-8 LCS-140512-9 CameosTso] Average _+ %RSD Spiked Concentration (ng/mL) 0.185 0.185 0.185 1.85 1.85 1.85 18.5 18.5 18.5 Calculated Concentration (ng/mL) 0.188 0.181 0.188 101%+2.5% 2.09 2.15 2.14 115%_+1.5% 21.0 21.3 21.5 115% + 0,87% %Recovery 102 97.6 102 113 118 116 114 115 116 Spiked Concentration (ng/mL) 0.190 0.190 0.190 1.90 1.90 1.90 Calculated Concentration (ng/mL) 0.214 0.211 0.216 112% ~- 0.89% 2.25 2.24 2.10 116% _+ 3.5% Te ETS-8-044.1 Er--a--n corm resron External calibration Analyzed 5/1 2/14 13C~-PFBA 13C4.PF0A Lab ID Spiked Concentration (ng/mL) Calculated Concentration (ngtmL) %Recovery Spiked Concentration (nglmL) Calculated Concentration (ng/mL) %Recovery 112 111 113 118 118 111 %Recovery coors LCS-140512-1 LOS-140512-2 LfCSr-1e40e512r-3 | Average + %RSD ow | 0.198 0.198 O. 198 om | 0.237 0.216 0.234 116% _+5.1% ve | ow | om | Ww 120 0.199 0.227 114 109 0.199 0.221 111 118 0.199 0.217 109 111% _+2.3% reve] LCS-140512-4 LCS-140512-5 (oon LCS-140512-6 1.98 2.44 123 1.99 1.98 2.40 121 1.99 EEE 1.98 2.30 116 1.99 |2.32 117 2.33 117 2.29 115 nuTtHesopechqtr cton Average 4- %RSD 120% -+ 3.0% HA = Not Applicable (1) LCSs spiked above the upper limit of quantification. 116% 4-1.0% 33663300..00114444 eenorm PAGE 19 OF 60 su_woreceoss 3M MN01596093 REPORT KO 01014 3M ENWRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 TTaabbllee 77 ccoonnttiinnuueedd.. LLaabb CCoonnttrrooll SSppiikkeeRReseuslutlsts.. ETS-8-044.1 Erpee| External calibration Analyzed 5!13/14 a PFPeA Spiked Calculated Concentration Concentration Lab ID (ng/mL) (ngtmL) %Recovery Los meat orto ozo oo LCS-140512-1 0.199 0.210 106 wswoszz ois0 oz0 00 LCS-140512-2 0.199 0.210 106 Lessa oto oze es [_Av|emge ioms estw en mso| LCS-140512-3 0.199 0.218 109 Average _+ %RSD 107% + 1,6% Tos wsza Ir = LCS-140512-4 Les wsizs py 2 LCS-140512-5 1.99 2.31 116 1.99 2.33 117 LCS-140512-6 [Auwrage + eso | some Average 4- %RSD Los osz7 0 a1 Ea LCS-140512-7 Lessee mo 2s ws LCS-140512-8 1.99 2.36 118 117% 4- 0.85% 20.0 23.1 115 20.0 22.9 115 [av| woge vsws soswwso| LCS-140512-9 Average _+ %RSD 20.0 22.9 115 115% + 0.0% Tseont ETS-8-044.1 onalcaten Internal calibration pe Analyzed 5!14114 . sq PFOS (Linear + Branched) Lab IB Spiked Concentration (ng/mL) Calculated Concentration (ngtmL) %Recovery Spiked Concentration (ng/mL) "c.or08 13C4-PFOS Calculated Concentration (ng/mL) %Recovery LCS-140513-1 0.0921 0D948 103 0.0949 0.0895 94.3 Lessa oo owes 0s om ours I LCS-140513-2 LCS-140513-3 0.0921 0.0921 0.0897 0.0966 97.3 105 0.0949 0.0949 0.0874 0.0973 92.1 103 Average + %RSD 102% _+ 3.9% 96.5% _+ 6.0% LCS-140513-4 E wesa wns LCS-140513-5 LCS-140513-6 0.921 0.985 107 0.949 m ost m 0 a0 ]ost 0.921 0.973 106 0.949 0.921 1.00 109 0.949 Avera~le -+ %RSD 107% 4-1.4% LCS-140513-7 Les osas LOS-140513-8 LCS-140513-9 3.67 3.88 106 sr a os 3.67 3.96 108 3.67 3.95 108 Average 4- %RSD 107% 4-1.1% NA= Not Alco NA = Not Applicable 1) L0545p are urbe of qsmtctin (1) LCSs spiked above the upper limit of quantification. 0.915 96.4 ww] 0.887 0.896 93.5 94.4 94.8% _+ 1.6% 33663300..00114455 Face mors PAGE 20 OF 60 3M_MNO1596094 3M MN01596094 REPORT KO 01014 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 A33v..a77iyicAAanlnaualnylcyetrtiticcaiaanltlyMMseebttahhseoodddonUUnhnicscteoerrirtctaaaliiQnnCttyydata thati controlcharted and used 0 ovaluate AmSmeneitathhlcyootiddacaaacldccuceunuvrcriaaenccryotyanaiannntdydCispparrbeescaciasisseliiodoenno.. onTTrhhhnieesatommresiectftahhloooQfddACuunncdccaeecrtarttauatihinnarttteyysisiusslctccosaanl(lctcnruo5ul6laa)tcteaehddabrfftoieolldleoowawsniinndgogurEEshTeT5deS-O-t11o2G2.e-s00va11am22lup2.al2.et.esTT.hheeFor scmmtaeaektntuhhdiooaaddrtdoEEdTdbTSeS.yv8-i-8am0-tu0i4o44ln.4l1.i,s1i,nct1aghlechummleasotessttdtarrfneeodccraeertnhndtetdfisiofetvyttalQoOyifCCoasncsacabmumypraapicleefysswarewesceruroooletfsu2rus(,sienewdd%h..i)TThohhbceetoareeinrxxeoppdsaapnnfeoddnreedtddsheuutonnQccaCeecrrosttanaafimniitdnpyetilneiyscsse.. For cleavlecluolafte9d5%b.y multiplying the standard deviation by a factor of 2, which corresponds to a confidence level of 95%. TTaabbllee 38.. AAnnaalylyttiiccaall MMoetthhoodd UUnncceertrtaaiinnttyy.. [ame| cwbonon |stamans ovson 0 | theauncanny | prea 1 Analyte PFBA wens | a0 [wen| Calibration Intemal Standard Deviation (%) 8.90 Method Uncertainty +18% [oma Toe [ow een | [eowPFPneA | [ora PF HxA PFHpA 1 [TerPoFOnA [emPFaNA T Internal enw Internal ems Internal weInternal em Internal 9.09 [7m | vex | 7.78 0sTee| 9.35 [sw wan | 5.83 Toes | won | 9.65 +18% _+ 16% _+19% ,+12% +19% [oon wo ow Tew | PFDA orn em 00 | een | PFUnA [ern| enw [ew |wew | PFDoA [erms | om |or | wow | PFBS [emms 1 em wes es | PFHS Internal Internal Internal Internal Internal 9.39 9.40 8.82 5.21 4.65 ,+19% _+19% ,+18% _+10% +9.3% [Toros Two [| 7 vex | [Terma 1 oto PFOS PFBA Internal External v0 | ew | 7.82 10.3 +16% _+21% [Como Tota [aw [om | PFPeA [Teron1 ote [ew | ean | PFOA [eres 1 emma[ow wen | PFBS [ems1 ota se | ew | PFHS Extemal Extemal Extemal Extemal 8.44 6.87 9.17 5.62 +17% +14% _+18% -+11% Cores 1 cts | aw | om | PFOS Extemal 4.93 _+9.9% A33f..8o8ldmFFaitieerilldxdspMMiakeatstrriaixxmSSeppiwikkaesescso((lFFeMcMtSSd))a e321sampingpoint 1 vey hal he analyical methosd Aaafippefkppiedliilscdcaaambmblplaelftrfeoioxrrttsot.hhpaeicckooecnlotsellaaecimctntpeeelrddespmwmiaaakstteri.dxc.obllFyFeiciettleseddmlmaaaatbotterriaixactsshopprsyikkaeewmssipaaltrirnheegggpeetnoanreiengrretaattttoeaednvdaebblryyiyfiyaaedtdshddapiintnrgtgihoeaatorammneSeaaialpsysputuiicrrnaeeglddmsvvaoeomtlluhpumolmdeeeisooff fcccieooolnndntctasaiaannimetnrapsetlfefrooonstrotssoaaabmmcopopcinloeetanccsinooileldllereeccsritpeiooidnkn.e.adnFFbaeieyplloddthrmemopaalraltarbistxoerssaspptoioikkrkeyeosswemmivtuheuslst.iht ebbFeetiaeaarllgtdeelemtaaaaslstnrtia00xly.55stepmtisimkepererssieocrtthhoteoavsaaehnnriaapsylpywltiineetghisnammoptlehod aacscociccnogecpfpetctnaatannrancctoteiconcnrrtoittooerrrbeaiaerooocffow1in1t00sh00id_t4e+h3r3ee00ed%%xtcarconaoncnaftifpiiropmnroattphnhradaiatt"at"euunsnnkpkninkaooewwollnnef"v"1ceyclo0.omamspFpoineonildonynesmtsnsatstoriiifnxtttshehproeiekcsseatam.rmepcplToloehvmeemarsiaetttsarinxwdddiatohornidnnsoomuttseethdofdor stnrhieegeanppirfrriaceepanpandartralabyttriiionaontnnecorohfffeettrdhheeeiwsffiioetehmlddetrhmmseaafetorxtrixtrPasscFpptiOkikoiAinnngagannssddooluPuatFtnioOoanSnlys.sscicsoFononettfaadtiihmnneeeaddatnrraeelsffyeetrerpeesnnecocefeiamnmrtaeaertlpeerrsaieta.srlseTncchtooeemmdpspsrtarieinsscdeetaddirodoofsfbnbouostteohhdf for isreport linear and branched this report. isomers for PFOA and PFOS. Field matrix spikes are presented in section 4 of 0rInecaaoddvdedirtoiyosnnpi{1kooeatasrorggfeett"aaCnn.aal-lyyPtLFeeBAffie.ilod"Cma.alPtrFrixOssApp,iike"essC,,PecFatUchRssAaa,mmpaplnleed bb"ooClttlPleeFccOooSnnte,aiinnweehddicsshtaabwbleleerSeisoaoldtoodppeeedssauulrrarrooggaates nrnCeoo.cmmo-iivnnPeaaFlrlyOccsAoopnnwickceaeernsntetoraatfstie1io3olCnneoc3otf-Pfed0F0..Bt11onAnr,gge13p/mCre4Ls-ePttonFotlOalpllAess,faa1lmm3uCyops2tlee-oPcbbFatoUrttntbleeAassx, yapplnraidecrri1tdt3ooCsis4saa-romPmopFmprlOleeCSA,cc-owoCllBhlee.icccthtoiTonwhn.e.ereTT"hhCaaeidad1"be3CedCsl3aPe-tPdFaFBPBAFAaUannDddA wwS13oaaClsse4-csstPeeellFdeeOcc0ttAeerddwet0eoprerrreeesppesrrleeeessncheetetnentdtCpp4toe,errrCfuel5uop,orrreoCosc8ceaanrprbteborpoxfexyuyrficlliuccraooariscoudicdfassrrfibfrocoomxmayciliCCdcs99.a.-cCCSi1du12sr2.r.frooTTgmhhaeetCe"~m43Ca-ClClr4a8i-1.bxaeTbslehpelieedkde1PP3rCFFe2OcO-o1SSvavebwraeialseesds.iPFiUnnA methodacceptancecrea of 100230% confimthatunknoan" companants in 1 samp mat do selected to represent the C4, C6, C8 perfluorosulfonic acids. Surrogate matrix spike recoveries within method acceptance criteria of 100_+30% confirm that "unknown" components in the sample matrix do 33663300..00114466 ecenorm PAGE 21 OF 60 3M_MNO1596095 3M MN01596095 ey 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 ot any troro ih ro rportn and analyseo haeof rest. Trurogae not significantly interfere with the preparation and analysis of the analytes of interest, The surrogate acorns es Socom 4 of wep spike recoveries are included in section 4 of this report. ay i CrP rn Goer Fl HO FMS Recovery = (Sample Concentration of FMS Average Concentration : Field Sample & Field Sample Dup.), 100% Se Spike Concentraton Tables. Fea at Spike Concenratons Table 9. Field Matrix Spike Concentrations I -- -- Final Spike Concentration (nglmL) sr [rea[ormn[me evg|von osero |runs|roca evs|ms cs| MW07, PW09, CS I POO PO PW10 [75 "so0| oo | wo |oo|ss| 0 | 0 | 00| 00|a0[00[zr| MW13 [urs JanTemTan enTan Tow FoonTeo ToTm anFan MW16 [ivi [[neoo[usee ouen[eomn[Loenna[ooon[Daowo[Toono[foomn[soae[onne[Tnaus]| MWl01, MWl03, SSS [or[| na[on eas[un oa | tn[wane[ono[ms| MW105, MW108 2.00 10.0 5.00 50.0 5.00 100 2.00 10.0 5.00 NA 5.00 NA 2.00 10.0 5.00 NA 5.00 NA 2.00 10.0 5.00 NA 5.00 NA 1.92 9.58 4.79 49.4 4.79 98.8 2.00 10.0 5.00 NA 5.00 NA 2.00 10.0 5.00 NA 5.00 NA 2.00 10.0 5.00 NA 5.00 NA 2.00 10.0 5.00 NA 5.00 NA 2.00 10.0 5.00 49.5 5.00 9.0 2.00 10.0 5.00 49.5 5.00 99.0 1.85 9.27 4.64 49.4 4.64 98.8 MW12, MW14R, MWl02, MWl04, BS oo[un[va[on sao[ua|oa| a|w|ano[so|ma| MW110 10.0 100 10.0 NA 10.0 NA 10.0 NA 9.58 98.8 10.0 NA 10.0 NA [[CCoioo|o0o0|o1w00||oroon{[sveiao[|o0w0|[ro0w0[|aoonn || 2m0o0|[s0o0o ||ooomn[|svaers|| Trip Bank 2.00 10.0 2.00 10.0 2.00 10.0 2.00 10.0 1.92 9.58 2.00 10.0 2.00 10.0 [renTue ue weLensLon [ow{ow[on oso [ono[oa] 100 NA NA NA 98.8 NA NA RTETo E Brn Ee NA = Not Applicable. The spiking solution did not contain all of the selected analytes. 10.0 NA 2.00 10.0 NA 10.0 NA 2.00 10.0 NA 10.0 9.0 2.00 10.0 9.0 10.0 99.0 2.00 10.0 99.0 9.27 98.8 1.85 9.27 98.8 44 DDaattaa SSuummmmaarryyaanndd DDiissccuussssiioonn Toston slows els ard Brac pk rato orbaton The tables below summarize the sample results and field matrix spike recoveries for the fourteen ators as wet 20 To Blk. Exch abe prove tho average coreariaion ad ho oats locations as well as the Trip Blank. Each table provides the average concentration and the relative rc erence (HRP) he soe 08 ase plete. Resse ndmarago aves ar percent difference (%RPD) of the sample and sample duplicate. Results and average values are eincadtobres sinfeant sure. Rao pacen dfrsnco (PD) vas ro founded os rounded to three significant figures. Relative percent difference (%RPD) values are rounded to two Seanres. Bocaun of on vous vary ty fot he sh radon, in significant figures. Because of rounding, values vary slightly from those listed in the raw data. Field phe mating ha mln acmance She oS deri Ve a eros matrix spikes meeting the method acceptance criteria of +30%, demonstrate that the method is ro a ua. appropriate for the given matrix. FFoorr tthhoosseeaannaalylytteesswwhheerreetthheeffiieelldd mmeatrtriixx ssppiikkeelleevveell wwaass nnoott aapppprroopprriiaattee aass ccoommpapreedtrtooetthhdee ssaammppllee Te i re ro Th concentration, the surrogate recovery standards were used to assess method accuracy. For all Sampinglocsios fed at Hee Wha pane)andor Tog recov Sands met sampling locations, field matrix spikes (where applicable) and/or surrogate recovery standards met poked tein method acceptance criteria except for the followirqg: MMWW101022:: TThheelolowwffiieekldd mmaatrtriixxssppiikkeessaammppllee hhaadd aa ssuurrrrooggaattee rreeccoovveerryy ooff 6699..00%% ffoorr 1"3'CC4--PPFFOOSS.. SSiinnccee To es va a etSp oe cn Sopa PE ol trrheeeccoomvveeorrsyyt for "C.PFOS was 73.3%, the methoduncertantywasnotexpanded. appropriate field matrix spike sample met acceptance criteria and the average for 13 C4-PFOS was 73.3 o~/0, the method uncertainty was not expanded. surrogate Tp Blak Th mid ove fod mae cs cowevro aepr rs50% of heexci ae, Trip Blank: The mid level field matrix spike recoveries were approximately 50% of the expected value. Saradon etn. AI api oh Coca of ho a vl By hamid Based on other FMS spike levels at half of the concentratiorq of the mid level, it is likely the mid field a pb wp Shor ge ofr tenes "OL A ter 0 shemset matrix spike was spiked at 5 ng/mL instead of the intended "10 ng/mL. All other field matrix spikes met pamnn acceptance criteria. zor PAGE 22 OF 60 Su uotsseoos 3M MN01596096 33663300..00114477 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Toe 15. COMMIT03 Table 10. CGMN-GW-MW07-140423 (1) mse 3M LIMS ID ome Description mms me] PFBA Concentration | 0cy [sey ty| (ng/mL) %Recovery PFPeA Concentration (nglmL) %Recovery PFHxA Concentration (ngtmL) %Recovery ISOll-01-03-14-001 CGMN-GW-MW07-0-140423 248 NA 0.159 NA 0.0806 NA ISOll-01-03-14-002 CGMN-GW-MW07-DB-140423 248 NA 0.147 NA 0.0749 NA ISOll-01-03-14-003 CGMN-GW-MW07-FMS-140423 458 105 2.06 95.4 1.99 95.6 Average Concentration tn1h~lL) 4- %RPD me Jo| rge owveyT || m on T gmm [| 3M LIMS ID ISO11 01433 14 001 SEN EY ISO11 01~ 14 002 Description CGMN GW MW07 0 140423 CGMN GW MW07 DB 140423 2.48 n~ltmL 4- 0.0% 0.153 n~ltmL 4- 7.8% 0.0778 n1/mL 4- 7.3% PFHpA Concentration (ng/mL) %Recevery <0.0250 NA <0.0250 NA PFOA Concentration (nglreL) %Recovery 0.351 NA 0.336 NA PFNA Concentration (ngtmL) %Recovery <00250 HA <00250 HA ISO11-0%03-14-003 CG MI'4-GW-MW07- FM S-140423 1 g0 95.0 2.06 89.4 1.90 95.0 Avarage Concentration (ng/mL) 4- %RPD ata omue]Eu E tee]E] eme| ga] 3M LIMS ID ISOll-01-03-14-001 ISOll-01-03-14-002 SAnT EIIE EIE ISOll-01433-14-003 Description CGMN-GW-MW07-0-140423 CGMN-GW-MW07-DB-140423 CGMN-GW-MW07-FMS-140423 <0,0250 ng/mL 0.344 ng/mL 4- 4.4% <0.0250 nglmL PFDA Concentration (n~/mL) %Recevery <0.0250 NA <0.0250 NA 1 86 93.0 PFUnA Concentration (n~lmL) %Recovery <0.0250 <0.0250 1.90 NA NA 95.0 PFDoA Concentration (ngtmL) %Recovery NR <00250 1.92 NA NA 96.0 Average Concentration (nglmL) + %RPD <0.0250 ng/mL <0.0250 ng/mL <0.0250 ng/mL a eh cars soLO tr Fe AA NA = Not Applicable NR = Not Reportable; sample area counts were below the LOQ area counts and did not meet method blank criteda (1) Samples were analyzed using internal standard calibration. PAGE 23 OF 60 sme 3M_MN01596097 33663300..00114488 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 10 continued. CGMN-GW-MW07-140423 (1) mse Jowsme | T sn | e ancee " ee|sy| 3M LIMS ID DescripLion PFBS Concentration (ng/mL) %Recovery PFHS Concentration (ng/mL) %Recovery PFOS Concentration (ng/mL) %Re~;overy ISOll-01-03-14-001 CGMI~-GW-MW07-0-140423 ISOll-01-03-14-002 CGMF4-GW-MW07-DB-140423 mar ISOll-01-03-14-003 CGMI~-GW-MW07-FMS-140423 Average Concentration (ng/mL) -+ %RPD 0.0357 NA 0.0363 NA 1 66 81.2 0.0360 ng/mL -+ 1.7% <0.0250 NA <0.0250 NA 1.77 88.5 <0.0250 ng/mL 0.0495 NA 0.0491 NA 1.87 98.4 0.0493 ng/mL -+ 0.81% simeleaena 3M LIMS ID ISOll-01-03-14-001 ISOll-01-03-14-002 I Description CGMN-GW-MW07-0-140423 CGMN-GW-MW07-DB-140423 EF EEE I~C~.PFBA %Recovery 98.6 93.6 ~C4-PFOA %Recovery 90.8 6.2 13C2-PFUnA %Recovery 95.6 98.2 13C4.PFOS %Recovery 99.6 100 ISOll-01-03-14-003 CGMN-GW-MW07-FMS-140423 106 87.9 9".0 Average Recovery (%) 4- %RSD 99.4% 4- 6.3% 91.P/g 4- 4.6% 94.9% 4- 3.8% prNA = Not Applicable NR = Not Reportable; sample area counts were below the LOQ area counts and did not meet method blank criteda Seemed ng oe ielp 8B ck cen (1) Samples were analyzed using internal standard calibration. 101 100% 4- 0.72% PAGE 24 OF 60 aw nctsoose 3M_MN01596098 33663300..00114499 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 11. CGMN-GW-MW12-140425 mse owe |meey| meey| m[ereey]| 3M LIMS ID ISOll-01-03-14-004 IS011-01-03-14-005 EEE EEE 2 ISOll-01-03-14-006 Description CGMN-GW-MW12-0-140425 CGMI'4-GW-MW12-DB-140425 CGMN-GW-MW12-LS-140425 PFBA I~ Concentration (ng/mL) %Recove~t 218 222 NA i~ NA NA NA ,~1 PFPeA Concentration (ng/mL) %Recovery 24 8 NA 24 ~ NA 35.0 NC PFHxA [a Concentration (ng/mL) %Recovery 26 4 NA 27 1 NA 35.9 NC ISOll-01-03-14-007 CGMN-GW-MW12-HS-140425 317 NC NA ~4) NA NA ~'~ NA~4~ Average Concentration (nglmL) + %RPD 220 ng/mL -+ 1.8% 24.8 ng/mL + 0.0% 26.8 nglmL -+ 2.6% PFHpA i~ PFOAI'l PF NA 12~ E=E==1HHHEH 3M LIMS ID ISOll-01-03-14-004 ISOll-01-03-14-005 ISOll-01-03-14-006 Description CGMN-GW-MW12-0-140425 CGMN-GW-MW12-DB-140425 CGMN-GW-MW12-LS-140425 Concentration (ng/mL) 11.7 11.7 22.8 %Recovery NA NA ~ Concentration (nglmL) 545 550 NA {3) %Recovery HA HA NA Concentration (ngtmL) 1.77 1.75 1 ~ .3 %Recovery HA HA 95.4 ISOll-01-03-14-007 CGMN-GW-MW12-HS-140425 NA ,4; NA Average Concentration (ng/mL) 4- %RPD 11.1 ng/mL 4- 0.0% Ee NA = Not Applicable BE ests NC = Not Calculated; Spike level was less than 0.Sx the endogenous sample concentration. (1) Samples were analyzed using external standard calibration. 13 Stn ev tsmtorgaicln. (2) Samples wure analyzed using internal sl~ndard calibra[Jon. (3) Ssmples were net re-analyzed f~r this analyte 0 Teresina ma (4) The spike level did not contain the target analyte. 652 NC 548 nglmL 4- 0.91% NA/:4; NA(4) 1.76 ng/mL 4-1.1% PAGE 25 OF 60 wero 3M_MN01596099 33663300..00115500 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 11 continued. CGMN-GW-MW12-140425 mse Jowsme |omsn,T | |ancm y" ew|sy| 3M LIMS ID Description PFDA I=~ Concentration (ngtmL) %Recovery PFUnAIzl Concentration (ng/mL) %Recovery PFDoA 12~ Concentration (ng/mL) %Reuovery ISOll-01-03-14-004 mn ISOll-01-03-14-005 ISOll-01-03-14-006 ISO11-01-03-14-007 CGMN-GW-MW12-0-140425 1 82 NA 0.433 NA 0.154 NA ESIHHHAHHA CGMN-GW-MW12-DB-140425 CGMN-GW-MW12-LS-140425 CGMN-GW-MW12-HS-140425 1 87 NA 0.415 NA 0.169 NA 11.5 96.5 10.7 103 10.2 100 NA t4) NA ~#) NA(4) NAu) Averae Concentration (ng/mL) -+ %RPD wise 3M LIMS ID omg Description 1,85 nglmL -+ 2,7% 0.42.4 ng/mL -+ 4.2% 8,162 ng/mL _+ 9,3% om [me we] PFBS In Concentration | "Gt| nen | "Ea |snc | "Ey | sty| (ngtmL) %Recovery PFHS ~m Concentration (ng/mL) %Recovery PFOS m Concentration (ng/mL) %Recovery ISQll-01-03-14-004 pe-- ISO11-01-03-14-005 ISOll-01-03-14-006 ISOll-01-03-14-007 CGMN-GW-MW12-0-140425 67 5 NA 9 97 HA 115 HA E1HHHHEH CGMN-GW-MW12-DB-140425 CG MI'4-GW-MW12- LS- 140425 CGMI'4-GW-MW12-HS-140425 70.3 NA ~s~ 164 NA NA 96.1 9.67 20.3 NA ~4) NA 105 NA 118 NA <~) 202 i',IA NA (s~ 86.0 Average Concentration (nglmL) + %RPD ma[oma [m[memaa | 68,9 ngtmL + 4.1% 9.82 ng/mL -+ 3.1% ~:~C:~-PFBA (~} ~C~.-PFOA le ~:~C~-PFUnA (~} ~=C~4~FOS (~) 117 ngtmL_+ 2.6% 3M LIMS ID ISOll-01-03-14-004 obvi ISOll-01-03-14-005 ISOll-01-03-14-006 ISOll-01-03-14-007 I Description CGMN-GW-MW12-0-140425 EEE CGMN-GW-MW12-DB-140425 CGMN-GW-MW12-LS-140425 CGMN-GW-MW12-HS-140425 %Recovery %Recovery %Recoveq/ %Recovery 109 105 88.0 110 HHHH 113 NA ~) 109 105 NA (:~I 106 963 114 92.1 108 NA ':~) 107 Average Recovery (%) _+ %RSD 110% -+ 2.1% 105% + 0.~% 97.6% + 12% 108% -+ 1.4% NA = Not Applicable Nee: so vb ne err rg cnr. NC = Not Calculated; Spike level "~as leas lhan 0.Sx the endogenous sample concentration. pp(1) Samples were analyzed using exlemal standard calibration. 3 Spm (2) Samples were analyzed using internal standard calibration. 38 m Smeet t (3) Samples were not re-analyzed for this analyte (4) The spike level did not contain the target enalyte. PAGE 26 OF 60 aw norssoon 3M_MN01596100 33663300..00115511 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 12. CGMN-GW-MW13-140424 (1) wove lower [w | m E00a|arene| s|"BRew|semery |"5 ee| ern|| 3M LIMS ID IS011-01-03-14-008 IS011-01-03-14-009 EEA INEIR ISOll-01-03-14-0"0 Description CG MI'4-GW-MW13-Q-140424 CGMN-GW-MW13-DB-140424 CGMN-GW-MW13-FMS-140424 PFBA Cencentration (ngtmL) %Recovery 74,5 NA 683 NA 1&1 110 PFPeA Concentration (nglmL) %Recovery 0 477 NA 0.452 NA 10.8 103 PFHxA Concentration (ngtmL) %Recovery 0 265 NA 0.249 NA 10.6 103 Average Concentration (ng/mL) 4- %RPD 7.14 ng/mL 4- 8.7% 0.465 ng/mL 4- 5,4% 0.257 ng/mL 4- 6,2% ne 3M LIMS ID Jo| m cnr | | | mer | "Ei |ster | Description PFHpA Concentration (ng/mL) %Recovery PFOA Concentration (nglmL) %Recove~ PFNA Concentration (ng/mL) %Recovery IS011-01-03-14-008 IS011-01-03-14-009 ISOll-01-03-14-0"0 CGMN-GW-MW13-0-140424 CGMN-GW-MW13-DB-140424 CGMII-GW-MW13-FMS-140424 0.0883 0.0674 947 NA NA 93.9 8.87 8.39 18.6 NA 0.0503 NA NA 0.0387 NA 104 9.81 97.7 Average Concentration (ng/mL) 4- %RPD 0.0779 ng/mL -~ 27% (2~ 8.63 ng/mL -+ 5.6% 0.0445 n/mL -+ 26% I~) agen 3M LIMS ID Jom Description [won Te7 wws ow] PFDA Concentration PE Lam LnI ne| (n~/mL) %Recevery PFUnA Concentration (nglmL) %Recovery PFDoA Concentration (ng/mL) %Recevery -- reve estgetin lsdotlrn. ISOll -01 -&3-14-008 CGMN-GW-MW13-0-140424 ISOll-01-03-14-009 CGMN-GW-MW13-DB-140424 ISOll-01-03-14-0" 0 CGMN-GW-MW13-FMS-140424 Average Concentration (ng/mL) 4- %RPD NA = Not Applicable <0.0250 <0.0250 966 <0.0250 NA NA 96.6 ng/mL <0.0250 NA <0.0250 NA 9.91 99.1 <0.0280 ng/mL <00250 NA <00250 NA 9.94 99.4 <0.0250 nglmL (1) Samples were analyzed using internal standard calibration. (2) Sample/sample duplicate RPD did not meet acceptance criteda of <20%. PAGE 27 OF 60 3M_MN01596101 33663300..00115522 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 12 continued. CGMN-GW-MW13-140424 (1) mse Jowsme | T sn | e ancee " ee|sy| 3M LIMS ID Description PFBS Concentration (ng/mL) %Recovery PFHS Concentration (ng/mL) %Recovery PFOS Concentration (ng/mL) %Re~;overy ISOll-01-03-14-008 CGMI~-GW-MW13-0-140424 0.781 NA cen [mnie | ISOll-01-03-14-009 CGMN-GW-MW13-DB-140424 ISOll-01-03-14-0" 0 CGMI~-GW-MW13-FMS-140424 Average Concentration (ng/mL) -+ %RPD 0.7"12 NA 912 83.7 0.752 ng/mL -+ 11% 0.594 NA comm 0.517 NA 9.76 92.0 0.55~ nglmL-+ 14% 2.46 NA IEsmIamEimY 2.20 NA 1"1.9 103 2.33 ng/mL -+ 11% Sms 3M LIMS ID Tome I Description Tos ome one [nny| I~C~.PFBA %Recovery '~C4-PFOA %Recovery 13C2.PFUnA %Recovery 13C4.PFOS %Recovery bmn ISO'~ "~ -0,1-03-14 -008 ISO1 "1-0"1-03-14-009 ISO,11-0,1-03-14-0" 0 iE[l=ls]%) CGMN-GW-MW13-0-'~40424 CGMN-GW-MW13-DB-'140424 CGMN-GW-MW13-FMS-140424 102 101 91.8 94.6 102 98.3 95.2 85.9 "109 97.6 94.8 101 Average Recovery (%) %RSD 98.3% 5.7% 98.3% 3.8% 96.7% 12% 97.8% 3.2% fog ------ NA = Not Applicable (1) Samples were analy~ed usin9 internal standard calibration. (2) Sample/sample duplicate RPD did not meet acceptance criteda of-<20%. PAGE 28 OF" 60 aw morse 3M_MN01596102 33663300..00115533 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 13. CGMN-GW-MW14R-140423 mune 3M LIMS ID | orm [omarvoy |Seewery |"|measreo || Description PFBA Concentration (ng~rnL) %Recovery PFPeA Concentration (nglmL) %Recovery PFHxA I~ Concentration (ng/mL) %Recovery IS011-01-0.3-14-0" 1 CG MI'4-GW-MW14R-0-140A 23 645 NA 280 NA 195 NA ISOll-01-03-14-0" 2 CGMN-GW-MW14R-DB-140423 654 NA 275 NA 199 NA ISOll-01-03-14-0" 3 CGMN-GW-MW14R-LS-140423 ISOll-01-03-14-0"4 CGMN-GW-MW14R-HS-140423 rnmeitoges |en | mame i, m, ame | Average Concentration (nglrnL) _+ %RPD me Joerg [eJnowmas[ [mw el e Tomeear [s || 3M LIMS ID ISOll-01-03-14-0" 1 ETT TT ISOll-01-03-14-0"2 Description CGMN-GW-MW14R-0-140423 CGMN-GW-MW14R-DB-140423 NA ~' NA ~:~ 751 NC 650 ng/mL _+ 1.4% NA (~) NA NA{'D NA 2"/8 ng/mL - 1.8/. 193 NC NA ('~) NA 197 ng/mL -+ 2.0% PFHpA ~ Concentration (ng/mL) %Recovery 25.4 NA 26.7 NA PFOA(~) Concentration (ng/mL) 542 543 %Recovery NA NA PF NA (2) Concentration (ng/mL) %Recovery 1.70 HA 1.74 HA ISOll-01-03-14-0" 3 CGMN-GW-MW14R-LS-140423 34.8 NC NA !3) NA 11.6 98.8 ISOll-01-03-14-0"4 CGMN-GW-MW14R-HS-140423 NA ~'D NA ~ Average Concentration (nglmL) -+ %RPD 26.1 ng/mL -+ 5.0% are NA = Not Applicable NC = Not Calculated; Spike level was less lhan 0.Sx the endogenous sample concent]*ation. 0 Sb mr arn (1) Samples were analyzed using external standard calibration. 1 E mre -- E " (2) Samples were analyzed using internal standard calibration. (3) Samples were not re-analyzed for this analyte (4) The spike level did not contain the target analyte. 646 NC 54-3 ng/mL + 0.18% NA ~4) NA 1.72 ng/mL -+ 2.3% PAGE 29 OF 60 aw morse 3M_MN01596103 33663300..00115544 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 13 continued. CGMN-GW-MW14R-140423 se owen |me|cy| we[sy| m[ere]y| 3M LIMS ID Description PFDA iz~ Concentration (ng/mL) %Recove~ PFUnA izl Concentration (ng/mL) %Recovery PFDoA (~) Concentration (ng/mL) %Recovery ISO,11-0,1-03-14-0" 1 C G MI'4 -GW-MW14R-0-'140423 2 11 NA <0.0250 NA <00250 NA ISO1"1-0"1-03-14-0" 2 CGMI'4-GW-MW14R-DB-'140423 208 NA <0.0250 NA <00250 NA ISO,11-0,1-03-14-0" 3 CGMI'4-GW-MW14R-LS-140423 ISO,11-0,1-03-14-0"4 CGMII-GW-MW14R-HS-140423 temas sammie | emma ema Average Concentration (nglmL) -+ %RPD FP POO CCe)rY T C m 7) 3M LIMS ID ISOll-01-03-14-0" 1 ISQll-01-03-14-0" 2 semi] FE] ISOll 01493 140"3 Description CGMN-GW-MW14R-0-140423 CGMN-GW-MW14R-DB-140423 CGMN GW MW14R LS 140423 11.4 93.0 NA 4, NA ~4~ 2.10 ng/mL -+ 1.4% 9.51 95.1 NA (4) NA (4! <0.0250 ng/mL 9.81 NA,:4) 98.1 NA(4, <0.0250 ngtmL PFBS (~) Concentration (n~l/mL) %Recove~ 18.2 NA 18.2 26.0 NA 78.0 PFHS Concentration (nglmL) %Recove~ 19.7 20.3 29.9 NA NA 99.0 Concentration (nglmL) 348 358 NA ,3) %Raeover~ NA NA NA ISOll-01-03-14-0"4 CGMN-GW-MW14R-HS-140423 NA ,3: NA i3) NA (3) NA 461 NC Average Concentration (ng/mL) -+ %RPD 3M LIMS ID Toe I Description l[oame [Lraoma[a mmora| 18.2 ng/mL -+0.0% 20.0 ng/mL --. 3.0% ~3C~.PFBA (1) %Recovery ~C~.PFOA(~) %Recovery l~C=.PFUnA(2) %Recovery ~ZC~.PFOS(~) %Recoven] 353 ng/mL-+ 2.8% ZL E IS011-01 -C).3-14-0" 1 CGMN-GW-MW14R-0-140423 ISOll-01-03-14-0" 2 CGMN-GW-MW14R-DB-140423 ISO11-01-03-14-0" 3 CGMN-GW-MW14R-LS-140423 ISO11-01-03-14-0" 4 CGMN-GW-MW14R-HS-140423 Average Recovery (%) _+ %RSD 107 112 NA (3) 111 110%2.4% 108 "09 NA (3) 106 108%-+1.4% 99.8 96.0 95.8 "102 98.4%-+3.1% 111 NA (3) 1,13 111%-+2.3% NA = Not Applicable NC = Not Calculated; Spike level "~as less than 0.Sx the endogenous sample concen'a'ation. 3 Stdatric (1) Samples were analyzed using external standard calibration. (2) Samples were analyzed using internal standard calibration. 1 Sona (3) Samples were not re-analyzed for this analyte EERE, (4) The spiko Iovel did not contain lho targot analyt~. PAGE 30 OF 60 sumerssros 3M_MN01596104 33663300..00115555 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 14. CGMN-GW-MW16-140424 mse owpe |me[sre |TE meey| mpey]| 3M LIMS ID ISO11-01-03-14-0" 5 IS011-01-0.3-14-0" 6 EEE EEEBE ISO11-01-03-14-0"7 Description CGMN-GW-MW16-0-140424 CGMN-GW-MW16-DB-140424 CGMN-GW-MW16-LS-140424 PFBA I~ Concentration (ng/mL) %Recove~ 41 1 NA ~.0 3 NA 457 NC PFPeA [11 Concentration (ng/mL) 691 6 52 11.7 %Recovery NA NA 99.6 PFHxA [1) Concentration (ng/mL) %Recovery 6 57 NA 6 42 NA 11.5 100 ISOll-01-03-14-0" 8 CGMN-GW-MW16-HS-140424 91 0 101 NA {~) NA I~) NA ~) NA Average Concentration (nglmL) + %RPD PO PO LCoePO T CC e poy 3M LIMS ID ISOll-01-03-14-0" 5 ISOll-01-03-14-0" 6 E EEE EE ISO11-01-03-14-0" 7 Description CGMN-GW-MW16-0-140424 CGMN-GW-MW16-DB-140424 CGMN-GW-MW16-LS-140424 48.7 ng/mL + 2.0% 6.72 ng/mL + 5.8% 6.58 nglmL --. 2.3% PFHpA (i) Concentration {n~llmL) %Recover~ 3.44 NA 3.15 NA 8.42 "02 PFOA (n Concentration n~llmL) %Recovers/ 89.1 NA 82.3 NA 94.3 NC Concentration (n~ltmL) 0.546 0.523 5.52 %Recover~ NA NA 99.7 ISOll-01-03-14-0" 8 CGMN-GW-MW16-HS-140424 NA ~2) NA ~2: 123 75.5 NA (2: NA (2) Average Concentration (nglmL) + %RPD 3.30 ng/mL -+ 8.8% 85.7 nglmL + 7.9% 0.535 ng/mL + 4.3% NA - Not Applicable NENA: ota ne cro sr comet. NO = Not Calculated; Spike level was less lhan 0.Sx the endogenous sample concentration. (1) Samples were analyzed using internal standard calibration. 1 Terpmomapie asmacm (2) The spike level did not contain Me target analyte. (3) Samples were analyzed using external standard calibration. Sma (4) Samples were not re-analyzed for this analyte PAGE 31 OF 60 wmerses 3M_MN01596105 33663300..00115566 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 14 continued. CGMN-GW-MW16-140424 mune | orm merey| [itmleey| im[eeo]n| 3M LIMS ID IS011-01-03-14-0" 5 ISOll-01-03-14-0" 6 =1HHERER ISO11-01-03-14-0" 7 Description CGMN-GW-MW16-O-140424 CGMN-GW-MW16-DB-140424 CGMI'4-GW-MW16-LS-140424 PFDA Concentration (ng~mL) %Recovery ~3 329 0.339 502 NA NA 93.7 PFUnA i, Concentration nglmL) <{3 0250 <0.0250 4.75 %Recovery NA NA 95.0 PFDoA Concentration (ng/mL) %Recovery <0 02,50 <00250 4.86 NA NA 97.2 ISOll-01-03-14-0" 8 CGMI'4-GW-MW16-HS-140424 NA ~z~ NA NA (z, NA izl NA (z) NA (a Average Concentration (ng/mL) + %RPD act 3M LIMS ID aur Description 0.334 nglmL + 3.0% <0.02~0 ng/rnL <0.0250 nglmL o or T ae] PFBS <3) Concentration | core Barge] SE cg] (ng/mL) %Recovery PFHS Concentration ng/mL) %Recovery Concentration (ngtmL) %Recovery ISOll-01-03-14-0" 5 ISO11-01-03-14-0" 6 ISO11-01-03-14-0" 7 ISOll-01-03-14-0" 8 CGMN-GW-MW16-0-140424 CGMN-GW-MW16-DB-140424 CGMI'4-GW-MW16-LS-140424 CGMN-GW-MW16-HS-140424 377 NA 51.4 NA 38 1 NA 4.55 NA 52.4 NA 9.30 96.2 59.2 NC 890 "03 48.6 89.1 108 114 Average Concentration Ingh~lL) + %RPD 37.9 ng/rnL -+ 1.1% 4.49 ng/mL + 2.7% 51.9 ng~rnL -+ 1.9% mmo 3M LIMS ID RA rerereeeES 0 SE) Description ~ZC~.PFBA(~) %Recover}/ ~C4.PFOAm %Recover~ ~C=.PFUnA<~! %Recovers/ ~ZC,~.PFOSIt) %Recover}/ IS011-01-03-14-0" 5 IS011-01-03-14-0" 6 CGMN-GW-MW16-0-140424 CGMN-GW-MW16-DB-140424 101 97.2 100 87.2 93.5 92.2 96.0 104 ISO11-01-03-14-0" 7 CGMIt-GW-MW16-LS-140424 100 108 ISOll-01-03-14-0" 8 CGMN-GW-MW16-HS-140424 100 92.7 TEE Average Recovery (%) + %RSD 99.6% + 1.6% 97.0% 9.3% NA = Not Applicable hl Cc:SotosPn ers srg ne. NC = Not Calculated; Spike level was less lhan 0.5x the endogenous sample concentration. BE(1) Samples were analyzed using internal standard calibration. (2) The spike level did not contain Me target analyie. 8 ES E ma (3) Samples were analyzed using external standard calibration. 98.5 107 97.8% -+ 6.9% 98.3 104 101% -+ 4.0% (4) Samples were not re-analyzed for this analyte PAGE 32 OF 60 awmerses 3M_MN01596106 33663300..00115577 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 15. CGMN-GW-MW101-140425 FR FO m FO CCmeIT mee] 3M LIMS ID ISO11-0fl-03-14-0" 9 ISO11-01-0,3-14-02~ =--"1HHHHHH ISO11-01-03-14-021 Description CGMN-GW-MW101-0-140425 CGMN-GW-MW1Q1-DB-140,425 CGMN-GW-MW101-LS-140425 PFBA !~1 Concentration (ng/mL) %Recovery 1330 1330 NA I~l NA NA NA ~! PFPeA (2! Concentration ng/mL) %Recovery 71 8 NA 72 6 NA 75.1 NC PFHxA (~) Concentration (ng/mL) %Recovery 60 9 NA 61 3 NA 68.4 NC ISO11-01-03-14-022 CGMN-GW-MW101-HS-140425 1410 NC NA/,*~ NA e) NA~ NA~ Average Concentration (nglmL) + %RPD PO PO LCoePO T CC e 2poy 3M LIMS ID ISOll-01-03-14-0" 9 ISOll-01-03-14-020 EE IHHHEHEH ISOll-01-03-14-021 Description CGMN-GW-MW101-0-140425 CGMiN-GW-MW101-DB-140425 CGMN-GW-MW101-LS-140425 1330 ngtmL + 6.0% 72.2 nglmL + 1.1% 61.1 ng/mL ~- 0.65% PFHpA (;~ Concentration {n~llmL) %Recover~ 63.2 NA 61.4 NA 67.7 NO PFOA (n Concentration n~llmL) 76.1 75.8 NA (:~ %Recover~ NA NA NA <~) Concentration (n~ltmL) 7.08 6.84 11.9 %Recover~ NA NA 98.8 ISOll-01-03-14-022 CGMN-GW-MWl01-HS-140425 NA <4) NA <4: 177 102 NA~4; NA(4) Average Concentration (nglrnL) + %RPD 62,3 ng/mL _+ 2,9% 76,0 ng/mL + 9,39% 6,96 aglmL 4- 3,4% NA - Not Applicable NENA: ota ne ror sr comet. NC = Not Calculated; Spike level was less than 0.Sx the endogenous sample concentration. (1) Samples were analyzed using exlemal standard calibration. 1 Stme masntcg tionn (2) Samples were analyzed using internal standard calibration. (3) Samples were not re-analyzed for this analyte 1 Terms mae (4) The spike level did not contain he target analyte. PAGE 33 OF 60 awmerseror 3M_MN01596107 33663300..00115588 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 15 continued. CGMN-GW-MW101-140425 ne 3M LIMS ID Jowgen Description ome |T werw] PFDA !zl Concentration |G [non [B00 anny| | re | {n~mL) %Recove~ PFUnA iz Concentration n~llmL) %Recove~ PFDoA Concentration ~n~llmL) %Reeover~ ISOll-01-03-14-0" 9 CGMN-GW-MW101-O-140425 0.248 HA <0.0250 NA '<00250 NA om ==1HHEHEHHA ISOll-01-03-14-020 ISOll-01-03-14-021 ISOll-01-03-14-022 CGMN-GW-MW101-DB-140425 CGMN-GW-MW101-LS-140425 CGMiN-GW-MW101-HS-1404.25 0.233 511 NA ~4) NA 97.4 NA (4) '<0.0250 4.78 NA (4i NA 95.6 NA (4) <00250 4.94 NA (4) NA 98.8 NA Average Concentration (ng/mL) + %RPD 0.241 nglmL + 6.2% <0.0250 ng/mL <0.0250 ngtmL swe 3M LIMS ID Logon Description | "Gt|amon [Erancy| "|ten | PFBS!~) Concentration (ng!mL) %Recovery PFHS (~) Concentration ng/mL) %Recovery PFOS (1) Concentration (ng/mL) %Reaovery ISO11-01-03-14-0" 9 CGMN-GW-MW101-0-140425 37.9 NA 364 NA ISO11-01.-03-14-020 CGMN-GW-MW101-DB-140425 37.6 NA 364 NA ISO11-01.-03-14-021 CGMN-GW-MW101-LS-140425 NA p~ NA NA (s~ NA <~) ISO11-01 .-03-14-022 CGMI'4-GW-MW101-HS-140425 142 135 4451 NC Average Concentration (ng/mL) 4- %RPD me 3M LIMS ID Toman I Description 37,8 ng/~L 4- 0,79% 364 ng/mL 4- 0.0% [mma [error[mea Scares ~C3-PFBA | suey| sion | sie| %Recovery I~C4-PFOA(~) %Recover~ ~Cz-PFUnA m) %Recovery ~C4-PFOS (1) %Recovery IS011-01-03-14-0" 9 CGMN-GW-MW101-0-140425 107 107 93.1 110 ISOll-01-03-14-020 CGMN-GW-MWl01-DB-140425 106 106 96.1 111 ISQll-01-03-14-021 CGMN-GW-MW101-LS-140425 ISQll-01-03-14-022 CGMN-GW-MW101-HS-140425 Sm == -- ZEEE Average Recovery (%) _+ %RSD NA (~ 106 106% -+ 0.54% NA ,~/ 104 106%4-1.4% 96.8 91.3 94.3%_+2.7% NA <~1 109 110%_+0.91% res NA = Not Applicable ETRE tsttre ceri, NO = Not Calculated; Spike level was less lhan O.Sx the endogenous sample concentration. E Ce m (1) Samples were analyzed using exlemal standard calibration. # Semis (2) Samples were analyzed using internal standard calibration. (3) Samples were not re-analyzed for this analyte (4) The spike level did not contain the target analyte. 136 HA 134 NA NA (3; NA (m 231 97.2 1~5 nglmL 4-1,5% PAGE 34 OF 60 smworsasios 3M_MN01596108 33663300..00115599 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 16. CGMN-GW-MW102-140425 wove Lowe [o | m "Ea 0r [soen| n[S0e0m]asre| re] "e|esover|| 3M LIMS ID ISOll-01-03-14-050 EeIS011-01-03-144)51 Description CGMlY-GW-MW102-O-140425 CGMlY-GW-MW1Q2-DB-14S425 PFBA !~1 Concentration (ng/mL) %Recovery 924 NA 914 NA PFPeA (2! Concentration ng/mL) %Recovery 30 7 NA 306 NA PFHxA I~ Concentration (ng/mL) %Recovery 29 1 NA 28 5 NA ISOll-01-03-14-052 ISOll-01-03-14-053 CGMtq-GW-MW102-LS-140425 CGMtq-GW-MW102-HS-140425 NA I~l NA ~! 40.3 NC 39.8 NC 995 NC NA NA~'~) NA ~-~ Average Concentration (nglmL) + %RPD 919 ng/mL + 1.1/. 30.7 ng/mL + 0.33% 28.8 nglmL -+ 2.1% wEie oEmmn T| "oan |T ovens[mrsT ovren| ee|sven | 3M LIMSID ISOll-01-03-14-050 ISOll-01-03-14-051 [meaPFHs pA (;n | wPoFOaA s(~ Description Concentration (n~llmL) %Recovers/ Concentration n~llmL) %Recovers/ CGMN-GW-MW102-0-140425 16.1 NA 58.6 NA CGMN-GW-MW102-DB-140425 15.6 NA 57.6 NA ean PFNA12) | Concentration (n~ltmL) %Recover~ 1.84 NA 1.90 NA ISOll-01-03-14-052 CGMN-GW-MW102-LS-140425 ISOll-01-03-14-053 CGMN-GW-MW102-HS-140425 Average Concentration (nglrnL) + %RPD 26.9 "09 NA ~4) NA ~4: 16.0 ng/rnL _+ 1.9% NA - Not Applicable ed i:Sectwa a1 oerps som. NC = Not Calculated; Spike level was less lhan 0.Sx the endogenous sample concentration. ieetm (1) Samples were analyzed using exlemal standard calibration. Cap tr (2) Samples were analyzed using internal standard calibration. 64.6 NC 140 82.9 ~8.1 nglmL + 1.7% 11.7 NA~4; 98.3 NA(4) 1.87 aglmL 4- 3.2% (3) Samples were not re-analyzed for this analyte rneoera--4--3--, (4) The spike level did not contain De target analyte. (5) Surrogate recovery did not meat acceptance cdteda of 100 + 30%. PAGE 35 OF 60 3M_MN01596109 33663300..00116600 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 =PP= PO Table 16 continued. CGMN-GW-MW102-140425 3M LIMS ID ISOll-01-03-14-050 ISO11-01-03-14-051 Description CGMN-GW-MW102-0-140425 CGMN-GW-MW102-DB-140425 TS ----C--] PFDA = a po (ng/mL) %Recovery PFUnA (~ Concentration nglmL) %Recovery PFDoA Concentration (ng/mL) %Recovery 0.143 0.129 NA <0.0250 NA <00250 NA NA <0.0250 NA <00250 NA ISOll 01433 14 052 ISO1%01-03-14-053 CGMN GW MW102 LS 140425 CGMN-GW-MW102-HS-140425 9.41 NA (4) 92.7 NA (4; 9.44 NA ( 94.4 NA (4) 9.74 NA(4; 97.4 NA(4) Average Concentration (ng/mL) %RPD into 3M LIMS ID oun Description 0.136 ng/mL 10% <0.0250 ng/rnL <0.0250 nglrnL mt Te wr] PFBS i~ Concentration | ol |sem | | ster, | stenee | (ng/mL) %Recovery PFHS (~) Concentration ng/mL) %Recovery PFOS I~) Concentration (ng/mL) %Recovery ISOll-01-03-14-050 CGMN-GW-MW102-0-140425 ISOll-01-03-14-051 CGMN-GW-MW102-DB-140425 ISOll-01-03-14-052 CGMN-GW-MW102-LS-140425 ISOll-01-03-14-053 CGMN-GW-MW102-HS-140425 Average Concentration (ngh~lL) %RPD 7.10 NA 7.14 NA 153 81.8 NA (:~) NA 7.12 ng/rnL 0.56% 146 NA 147 NA NA (~ NA !~) 244 98.0 147 ngtmL 4- 0,68% 67.1 NA 67.6 NA 71.5 NC 143 76.5 67.4 ng/mL 0.74% Sms 3M LIMS ID TomJ Description ateem,Teo |ah ~3C3.PFBA % Recover,,/ 13C4.PFOA (2) %Recove=~ ~3Cz-PFUnA (21 %Recover)t [on~3C4.PFOS (2) %Recovers/ ISOll-01-03-14-050 CG MI'4-GW-MW102-0-140425 110 133 ISOll-01-03-14-051 CGMN-GW-MW102-DB-140425 110 104 ISOll-01-03-14-052 CGMN-GW-MW102-LS-140425 95.3 ISOll-01-03-14-053 CGMN-GW-MW102-HS-140425 107 103 Average Recovery (%) -+ %RSD I O9% 1.6% 101% 4.0% NA - Not Applicable NC = Not Calculated; Spike level was less than 0.Sx the endogenous sample concentration. I (1) Samples ',,,,ere analyzed using external standard calibratien. 2 Emm (2) Samples were analyzed using internal standard calibration. (3) Samples were not re-analyzed for this analyte 18 Ser ov-- a (4) The spike level did not contain lhe target analyie. ne She4m 35. (5) Surrogate recovery did not meet acceptance cd'~na of 100 + 30% 92.2 93.3 95.1 97.0 94.4% -+ 2.2% 739 766 69.0 (~) 735 73.3% --. 4.3% PAGE 36 OF 60 aw netssnto 3M_M N01596110 33663300..00116611 3M ffNVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 17. CGMN-GW-MW103-140425 FR FO m FO CCmeIT mee] 3M LIMS ID ISOll-01-03-14-054 IS011-01-03-14-055 =--1HHHHHH ISOll-01-03-14-056 Description CGMN-GW-MW103-O-140425 CGMlY-GW-MW103-DB-14S425 CGMN-GW-MW103-LS-140425 PFBA !~1 Concentration (ng/mL) %Recovery 238 24,3 NA I~l NA NA NA ~! PFPeA (2! Concentration ng/mL) %Recovery 27 3 NA 2,9 1 NA 32.0 NC PFHxA (a Concentration (ng/mL) %Recovery 57 0 NA 57 8 NA 57.7 NC ISOll-01-03-14-057 CGMN-GW-MW103-HS-140425 331 NC NA/~, NA e/ NA~ NA~ Average Concentration (nglmL) + %RPD PO PO LCoePO T CC e 2poy 3M LIMS ID ISOll-01-03-14-054 ISOll-01-03-14-055 EEEfiefEE ISOll-01-03-14-056 Description CGMN-GW-MW103-0-140425 CGMN-GW-MW103-DB-140425 CGMN-GW-MW103-LS-140425 24"1 ng/mL + 2.'1% 28.2 nglmL + 6.4% 57.4 nglmL -+ 1.4% PFHpA (;n Concentration {n~llmL) %Recovers/ 31.4 NA 30.4 NA 36.0 "02 PFOA (n Concentration n~llmL) %Recovers/ 117 125 NA (a NA NA NA PFNA12) Concentration {n~ltmL) %Recover~ 0.0487 NA 0.0566 NA 4.76 94.1 ISOll-01-03-14-057 CGMN-GW-MW103-HS-140425 NA <4) NA <4; 227 107 NA(4: NA(4) Average Concentration (nglrnL) + %RPD 30,9 ng/mL _+ 3,2% 121 ng/mL _+ 6,6% 0.0527 ng/mL ~- 15"/0 NA - Not Applicable NENA: ota ne ror sr comet. NC = Not Calculated; Spike level was less lhan 0.Sx the endogenous sample concentration. (1) Samples were analyzed using exlemal standard calibration. 1 Sime marycts ion (2) Samples were analyzed using internal standard calibration. (3) Samples were not re-analyzed for this analyte 1 Terms mae (4) The spike level did not contain De target analyte. PAGE 37 OF 60 sumer 3M_M N01596111 33663300..00116622 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 17 continued. CGMN-GW-MW103-140425 ws [ome [|o"Hm E e [men| e| o[s sme [ | "o EE w [ane c || 3M LIMS ID ISOll-01-03-14-054 ISOll-01-03-14-055 =E=HHEHBEHRA ISOll-01-03-14-056 Description CGMN-GW-MW103-0-140425 CGMI'4-GW-MW103-DB-140425 CGMN-GW-MW103-LS-140425 PFDA Concentration (ng/mL) %Recovery <0.0250 <0.0250 4.75 NA NA 95.0 PFUnA(=) Concentration (ng/mL) %Recovery <0.0250 <0.0250 4.90 NA NA 98.0 PFDoA (=) Concentration (ng/rnL) %Recovery <0.0250 <0.0250 4.85 NA NA 97.0 ISOll-01-03-14-057 CGMII-GW-MW103-HS-140425 NA (41 NA {4; NA 14) NA 4; NA ~4) NA {4) Average Concentration (nglmL) + %RPD <0.0250 ng/mL <g.g2~0 nglmL <0.0250 ng~mL PFBS ~ PFHS i~l PFOS 3M LIM$ ID Description ISO'11-0'1-03-14-054 ISO11-0'1-03-14-055 CGMN-GW-MW103-O-140425 CGMI'q-GW-MW103-DB-140425 = ==1HHEHHHH ISO11-0'1-03-14-056 ISO1'1-0'1-03-14-057 CGMN-GW-MW103-LS-140425 CGMN-GW-MW103-HS-'140425 ee Average Concentration (nglmL) + %RPD Concentration (ng/mL) %Recovery 6.51 HA 6.51 NA 103 75.8 NA (3) NA 6.51 ng/mL -+ 9.0% Concentration (ng/mL) %Recovery 21.0 NA 22.5 NA NA (3) 124 NA :3: 103 21.8 nglmL + 6.9% Concentration (nglmL) %Recovery 7.99 NA 7.64 NA 11.9 87.9 108 101 7.82 nglmL -+ 4.5% aso Towrgion 3M LIMS ID I Description ISOll 0143.3 14 054 CGMN GW MW103 C~140425 ISOll 0143.3 14 055 CGMN GW MW103 DB 140425 BEESE ISOll-01-03-14-056 CGMN-GW-MW103-LS-140425 ISOll-01-03-14-057 CGMN-GW-MW103-HS-140425 | seco |Soacomny| Sitocony|sotcorey| ~C~-PFBA (~ %Recovery ~C4-PFOA (~) %Recovery ~C=-PFUnA !~ %Recovery ~C~-PFOS (~ %Recovery HEEE 108 110 NA (3~ 107 109 109 NA (~) 1"10 92.9 97.6 990 95.4 92.0 98.1 89.6 97.0 Average Recovery (%) 4- %RSD 108% 1.4% 109% 4- 0.~3% NA = Not Applicable ek: ptt nO res en NC - Nat Calculated; Spike level ',,,'as less lhan O.5x the endogenous sample cancon'a'atien. (1) Samples were analyzed using external standard calibration. [ iEmsse (2) Samples were analyzed using internal standard calibration. (3) Samples were not re-analyzed for this analyte (4) The spike level did not centain the target analyte. 96.2% 2.8% 94,2% 4.2% PAGE 38 OF 60 3M_MN01596112 33663300..00116633 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 18. CGMN-GW-MW104-140425 wwe L| ower [omar [me| | "EeEm|aames| "Fi nea|sme| 3M LIMS ID ISOll-01-03-14-023 EEL IS011-01-03-14-024 Description CGMN-GW-MW104-0-140425 CG M N -GW-MW1OA- DB-140,425 PFBA !~1 Concentration (ng/mL) %Recovery 107 NA 107 NA PFPeA Concentration (ng/mL) %Recovery 12 7 NA 12 4 NA Co~central~on (ng/mL) 19 9 19 5 %Recovery NA NA ISOll-01-03-14-025 CG MII -GW-MW104-LS- 140425 114 NC 22.6 100 28.8 91.0 ISOll-01-03-14-026 CGMII-GW-MW104-HS-140425 197 90.0 NA Average Concentration (nglmL) + %RPD 107 ng/mL + 0.0% 12.6 nglmL + 2.4% 19.7 ngtmL -+ 2.0% w= ie 3M LIMS ID ISOll-01-03-14-023 ISOll-01-03-14-024 omen Description | "oe | ver]"eae |semen] "eae |sere [meas PFHpA(11 | wor|ear] PFOA (~} PFNA (~1 Concentration {n~llmL) %Recover~ Concentration (n~/mL) %Recover~ Concentration (ngfmL) %Recovers/ CGMN-GW-MW104-0-140425 908 NA 82.0 NA 2.57 NA CG Mi'1 -GW-MW104- DB-140425 9.13 NA 82.1 NA 2.60 NA ISOll-01-03-14-025 CG MII -GW-MW104-LS- 140425 ISOll-01-03-14-026 CGMN-GW-MWl04-HS-140425 Average Concentration (nglrnL) + %RPD 18.4 92.9 NA ~2) NA ~2; 9,11 ng/mL + 0,5~% NA - Not Applicable ed i:Sectwa os a1 oerps som. NC = Not Calculated; Spike level was less lhan 0.Sx the endogenous sample concentration. F De ------m (1) Samples were analyzed using internal standard calibration. ---- (2) The spike level did not contain Me target analyte. (3) Sample/sample duplicate RPD did not meet acceptance criteda of ~20%. EEE (4) Samples were not re-analyzed for this analyte (5) Samples were analyzed using exlemal standard calibration. 92.1 NC 158 79.2 82,1 nglmL -+ 0,12% 12.3 97.1 NA ~2) NA ~2) 2,59 nglmL -+ 1,2% PAGE 39 OF 60 3M_M N01596113 33663300..00116644 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 18 continued. CGMN-GW-MW104-140425 re 3M LIMS ID Toe Description [ [e mm raLo 1 [oo eaLso [ [oora]| PFDA!n Concentration (n~l/mL) %Recoven/ PFUnA ill Concentration (n~/mL) %Recovers/ PFDoA Concentration (n~lfmL! %Recover~ ISOll-01-03-14-023 CGMN-GW-MW104-O-140425 3.20 NA 0.0489 NA <0.0250 NA a)F=IHHHHAEHH ISOll-01-03-14-024 ISOll-01-03-14-025 ISOll-01-03-14-026 CGMN-GW-MW104-DB-140425 CGMN-GW-MW104-LS-140425 CGMN-GW-MW104-HS-140425 3.32 133 NA (2] NA "00 NA (2' 0.0625 10.0 NA iz) NA 99.4 NA :2' <0.0250 9.83 NA ~z) NA 98.3 NA (2) Average Concentration (ng/mL) + %RPD 3.26 ng/rnL __ 3.7% 0.0557 ng/mL ~- 24% la <0.0250 ng/n~L PT 3M LIMS ID PODescription [o1 mer 1 Ls emePrO TT w1eFsy] PFBS Concentration (ng/mL) %Recovery PFHS !~) Concentration (ng/mL) %Recovery PFOS Concentral~ion (ng/mL) %Recovery ISOll-01-03-14-023 CGMN-GW-MW104-0-140425 7.95 NA 12.8 NA ISOll-01-03-14-024 CGMN-GW-MW10d-DB-140425 8.25 NA 12.3 NA ISOll-01-03-14-025 CGMN-GW-MW104-LS-140~25 156 75.0 21.9 93.0 ISOll -01 .-03-14-626 CGMN-GW-MW104-HS-1404.25 NA (4) NA (4) NA ~4) NA :4) Average Concentration (ng/mL) 4- %RPD 8.10 ng/mL 4- 3.7% 12.6 ng/mL 4- 4.0% miso 3M LIMS ID Jowapin Description [cera [cr [cor mmao|n ServoTM s | | secon |swcomey | stacomey |steconey| ~C3-PFBA n) %Recovery l~C4.PFOA n) %Recovery ~C2-PFUnA d) %Recovery ~C~-PFOS (~ %Recovery 238 NA 229 NA NA ~4) NA (4) 332 I-4 C 234 ng/mL 4-3.8% ISOll-01-03-14-023 CGMN-GW-MW104-0-140425 99.2 86.7 ISOll-01-03-14-024 CGMN-GW-MW104-DB-140425 100 96.9 ISQll-01-03-14-025 CG MI'4-GW-MW104.-LS- 140425 99.1 96.1 a === HH ISQll-01-03-14-026 CGMN-GW-MW104-HS-140425 96.1 98.7 Average Recovery (%) 4- %RSD 98.6% -+ 1.7% 94.6%_+5.7% E LL--R ---- NA = Not Applicable NC = Not Calculated; Spike level was less than 0.Sx the endogenous sample concen~ation. (1) Samples were analyzed using internal standard calibration. PE(2) The spike level did not contain Me target anal~@. 101 111 HEH 102 113 98.6 111 HA e) 101 104%_+6.1% 108%_+5.3% artes ste. (3) Sample/sample duplicate RPD did not meet acceptance criteda of g20%. (4) Samplas were not re-analyzed for this analyte (5) Samples were analyzed using external standard calibration. PAGE 40 OF 60 snes 3M_MN01596114 33663300..00116655 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 19. CGMN-GW-MW105-140425 (1} mse Jowpe | m[orT e | TE [T ste | i e [one | 3M LIMS ID ISOll-01-03-14-027 IS011-01-08-14-028 se|e EEm E]s E ISOll-01-03-14-029 Description CGMlY-GW-MW105-O-140425 CGMlY-GW-MW1Q5-DB-l,~S425 CGMtq-GW-MW105-LS-140425 PFBA Concentration (ng/mL) %Recovery 70 3 NA 71 7 NA 741 NO PFPeA ConaentratJon (ng/mL) %Recovery 5 86 624 10.5 NA NA 89.0 PFHxA Cor~central~ion (ng/mL) %Recovery 11 7 NA 11 8 NA 16.6 110 ISOll-01-03-14-030 CGMtq-GW-MW105-HS-140425 164 93.0 NA ~2~ NA 2i NA ~'~ NA Average Concentration (nglmL) + %RPD PON PO LoYe eYeP Tm py 3M LIMS ID IS011-01-03-14-027 ISOll-01-03-14-028 =E=SHHEIHHA ISOll-01-03-14-029 Description CGMII-GW-MW105-0-140425 CGMiN-GW-MW105-DB-140425 CGMIN-GW-MW105-LS-140425 71.0 ng/rnL _+ 2.0% 6.05 nglmL + 6.3% 11.8 ng/mL + 0.85% PFHpA Concentration (n~llmL) %Recover~ 8.38 NA 8.89 NA 13.5 97.2 PFOA Concentration (n~/mL) %Recover~ 42.7 NA 45.9 NA 47.2 NO PFNA Concentration (nglmL) %Recovers/ 0.577 NA 0.588 NA 5.51 98.5 ISOll-01-03-14-030 CGMIt-GW-MW105-HS-140425 NA ~2) NA ~2: 122 78.6 NA ~2) NA ~) Average Concentration (nglrnL) + %RPD 8.64 ng/rnL _+ 5.9% 44.3 nglrnL + 7.2% 0.~83 ng/mL ~- 1.9% NA - Not Applicable NENA: ota ne cro sr comet. NC = Not Calculated; Spike level was less lhan 0.5x the endogenous sample concentration. (1) Samples were analyzed using internal standard calibration. 1 Teppe es (2) The spike level did not contain Me target analyte. | EERE (3) Samples were not re-analyzed for this analyte PAGE 41 OF" 60 sumer 3M_M N01596115 33663300..00116666 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 19 continued. CGMN-GW-MW105-140425 (1) mune ore |m " oe imeweT [on T [ome e [oo| 3M LIMS ID IS011-01-08-14-027 ISOll-01-03-14-028 sem [EEE] ISOll-01-03-14-029 Description CGMN-GW-MW165-O-140425 CGMII-GW-MW105-DB-140425 CGMII-GW-MW105-LS-140425 PFDA Concentration (ng/mL) %Recovery {3 328 0.339 5.10 NA NA 95.3 PFUnA Concentration (ng/mL) %Recovery <0 025{3 <0.0250 4.91 NA NA 98.2 PFDoA Concentration (nglmL) %Recovery <{3 0250 <0.0250 4.83 NA NA 96.6 ISOll-01-03-14-030 CGMIt-GW-MW105-HS-140425 NA (z) NA <z) NA iz) NA :z) NA ~z) NA ) Average Concentration (ng/mL) + %RPD atau 3M LIMS ID Description 0.334 nglmL + 3.3% <0.0250 nglmL <0.0250 ng/mL omeT Tax PFB8 Concentration cree}IE |cra}EE[srg] (ng/mL) %Recovery PFHS Concentration (ng/mL) %Recovery PFOS Concentration (ng/mL) %Recovery ISOll-01-03-14-027 CGMN-GW-MW105-0-140425 7.56 NA 8.48 NA 56.6 NA ISO11-01-03-14-028 CGMN-GW-MW105-DB-140425 7.80 NA 8.70 NA 60.7 NA ISOll-01-03-14-029 CG MI'4-GW-MW105-LS- 140425 120 86.4 12.9 86.2 66.1 NC ISOll -01-03-14-030 CGMN-GW-MW105-HS-140425 NA I'~) NA {3) 97.0 89.3 169 112 Average Concentration In1h~lL) + %RPD 7.68 n1/mL 4. 3.1% 8.59 n1h~lL + 2.6% 58.7 ng/mL 4- 7.0% mmo 3M LIMS ID Tompson Description | inecovy|stcomny| sotacoey|sotwcommy| 13C3-PFBA %Recover~ ~C4-PFOA %Recoverer 130~-PFUnA %Recovers/ ~C~-PFOS %Recovers/ IS011-01-03-14-027 CGMN-GW-MW105-0-140425 96.4 95.6 92.9 88.0 ISOll-01-03-14-028 CGMN-GW-MW105-DB-140425 102 99.3 98.4 95.5 ISOll -01-0.3-14-029 CGMIt-GW-MW105-LS-140425 100 101 94.4 90.6 ISOll-01-03-14-030 CGMN-GW-MW105-HS-140425 99.5 104 Average Recovery 1/0) 4- %RSD 99.5/0 + 2.3% 100% -+ 3.5% ran NA = Not Applicable LE mugs NC - Not Calcula[ed; Spike level ',*,'as loss than 0.Sx the endogenous sarnplo concon'~]'atien. (1) Samples were analyzed using internal standard calibration. Ee (2) The spike level did not centain ~e target analyte. Hs(3) Samples were not re-analyzed for this analyte 95.8 95.4-% + 2.5/0 96.9 92.8% -+ 4.5% PAGE 42 OF 60 sumer 3M_MN01596116 33663300..00116677 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 20. CGMN-GW-MW108-140425 FREREE3M LIMS ID ISOll-01-03-14-031 IS011-01-0.3-14-~)32 ISOll-01-03-14-033 FODescription CGMN-GW-MW108-0-140425 CGMN-GW-MW1QS-DB-140A25 CGMII-GW-MW108-LS-140425 mTeT me PFBA !~1 Concentration Cc)FC) FU 0) (ng/mL) %Recovery 59 1 NA 71 6 NA EE EEE 743 NC PFPeA Concentration (ng/mL) %Recovery 10 6 NA 123 NA 17.0 NC Co~central~on (ng/mL) 9 39 11 {3 16.3 %Recovery NA NA NC ISOll-01-03-14-034 CGMII-GW-MW108-HS-140425 156 90.6 NA Average Concentration (nglmL) + %RPD mEe JEom E| 3M LIMS ID ISOll-01-03-14-031 ISOll-01-03-14-032 ISOll-01-03-14-033 Description CGMN-GW-MW108-0-140425 CG Mi'1 -GW-MW108- DB-140425 CGMII-GW-MW108-LS-140425 65.4 ngtmL -+ 19% 11.5 ng/mL -+ 15% 10.2 ng/mL + 16% oe Te Te PFHpA (11 Concentration | oem]i |e] ai [| {n~llmL) 3.84 4.45 SEER] 10.1 %Recover~ NA NA "19 PFOA (~} Concentration (n~/mL) %Recover~ 166 162 NA ~4) NA NA NA :4~ PFNA (~1 Concentration (ngfmL) %Recovers/ 1.15 NA 1.36 NA 6A3 103 ISOll-01-03-14-034 CGMN-GW-MWl08-HS-140425 NA ~2) NA ~2; 265 102 NA ~2) NA ~2) Average Concentration (nglrnL) + %RPD 4.15 nglmL + 15% 164 nglmL -+ 2.4% 1.26 ng/mL + 17% NA - Not Applicable NENA: ota ne cro sr comet. NC = Not Calculated; Spike level was less lhan 0.Sx the endogenous sample concentration. (1) Samples were analyzed using internal standard calibration. 1 Terpmomapie asmacm (2) The spike level did not contain Me target analyte. (3) Samples were analyzed using external standard calibration. Sma (4) Samples were not re-analyzed for this analyte PAGE 43 OF 60 sumer 3M_M N01596117 33663300..00116688 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 20 continued. CGMN-GW-MW108-140425 wise owen |m|e eng|T " | mere|e "ie [ono | 3M LIMS ID ISOll-01-03-14-031 ===ETL ISOll-01-03-14-032 Description CG MI'4-GW-MW108-O-140425 CGMN-GW-MW108-DB-140425 PFDA Concentration (n~rnL) %Recove~ 0.516 NA 0.607 NA PFUnA(11 Concentration tn~lJrnL/ %Recovers/ <0.0250 NA <0.0250 NA PFDoA(11 Concentration (n~lfmL! %Recover~ <0.0250 NA <0.0250 NA ISOll-01-03-14-033 CGMN-GW-MW108-LS-140425 534 95.6 4.95 99.0 4.98 99.6 ISOll-01-03-14-034 CGMN-GW-MW108-HS-140425 NA (21 NA (2) NA (2i HA (2 NA ~z) NA (2) Average Concentration (ng/mL) + %RPD 0.~62 ng/mL -+ 16% <0.0250 ng/mL <0.0250 ng/rnL sie Jour | "i|smn| "Ei | smerny|"En [smn| 3M LIMS ID Description IS011-01-03-14-031 CGMN-GW-MW108-0-140425 ISOll-01-03-14-032 CGMN-GW-MW108-DB-140425 sem Ela EEE] ISOll-01-03-14-033 CGMN-GW-MW108-LS-140425 ISOll-01-03-14-034 CGMN-GW-MW108-HS-140425 tmnt |imin | sre i] Average Concentration (ng/mL) + %RPD mmso Tomerpsen | suecomey | swcovey|stecomey| scone | 3M LIMS ID I Description IS011-01-03-14-031 = ISO11-01-03-14-032 CGMN-GW-MW108-O-140425 CGMN-GW-MWl08-DB-140425 PFBS ~3~ Concentration (ngtrnL) %Recovery 17.8 NA 17.0 NA NA ~) NA ~) 124 108 17,4 ng/mL _+ 4,6% PFHS (~) Concentration (ngimL) %Recovery 3.32 NA 3.84 NA 8.85 105 93.0 90.3 3.58 ng/mL -+ 15% PFOS (~} Concentration (nglmL) %Recovery 40.2 NA 46.4 NA 52.2 NC 153 111 43.3 ng/mL + 14% ~C3.PFBA(~} %Recovery 97.6 96.6 ~3C4.PFOA(~} %Recevery 98.8 97.4 ~Cz.PFUnAI~) %Recovery 101 99.2 ~C4.PFOS (~) %Receve~ 98.6 89.5 ISOll-01-03-14-033 CGMN-GW-MW108-LS-140425 99.3 NA ~4~ ISO11-01-03-14-034 CGMN-GW-MWl08-HS-140425 mrss mls Average Recovery (%) _+ %RSD 98.8 98.1%-+1.2% 9.4 98.5% -+ 1.0% ST NA = Not Applicable NC = Not Calculated; Spike level was less than 0.Sx the endogenous sample concentration. (1) Samples were analyzed using internal standard calibration. SS (2) The spike level did not contain lhe target analyte. JE(3) Samples were analyzed using external standard calibration. (4) Samples wcrc not rc analyzed for this analyta 102 a 94.6 99.2%-+3.3% 103 .94.1 96.3%-+6.0% PAGE 44 OF 60 sumer 3M_M N01596118 33663300..00116699 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 21. CGM N-GW-MW110-140424 FRR FO Cm c)FT Ce )FUT=)me 3M LIMS ID ISO11-01-03-14-035 IS011-01-03-14-036 Ems EEE]E ISOll-01-03-14-037 Description CGMN-GW-MW110-0-140424 CGMlY-GW-MW110-DB-14S424 CGMN-GW-MW110-LS-140424 PFBA Concentration (ng/mL) %Recovery 186 191 NA (31 NA NA NA {~! Concentration (ng/mL) 24 6 234 38.4 %Recovery NA NA 90.6 Cormentra~on (ng/mL) 34 0 31 7 47.6 %Recovery NA NA NC ISOll-01-03-14-038 CGMN-GW-MW110-HS-140424 306 "17 NA Average Concentration (nglmL) + %RPD me Jom | oe| oeT r]ie |rT ] ate [| 3M LIMS ID ISO1.1-0"1-03-14-035 ISO.1 "1-0.1-03-14-036 E EEE] ISO.1 "1-0.1-03-14-037 Description CGMN-GW-MW110-0-140424 CGMN-GW-MWll 0-DB-'140424 CGMN-GW-MWl10-LS-140424 189 ng/mL + 2.6% 24.0 nglmL + 5.0% 32.9 ngtmL -+ 7.0% PFHpA (z~ Concentration {n~llmL) 12.5 12.8 28.6 %Recover)/ NA NA "00 PFOA (~} Concentration (n~/mL) %Recover~ 310 310 NA/:~ NA NA NA ::~) PFNA (7 Concentration (ngfmL) %Recovers/ 0.19.1 0.197 15.8 NA NA 98.2 ISO.1 "1-0.1-03-14-038 CGMN-GW-MWll 0-HS-'140424 NA <4) NA <4; 410 NC NA ~4) NA <4) Average Concentration (nglrnL) + %RPD 12.7 ng/rnL _+ 2.4% 310 ng/mL -+ 0.0% 0.194 ng/mL ~- 3.1% NA - Not Applicable NENA: ota ne ror sr comet. NC = Not Calculated; Spike level was less lhan 0.Sx the endogenous sample concentration. (1) Samples were analyzed using exlemal standard calibration. 1 Sime marycts ion (2) Samples were analyzed using internal standard calibration. (3) Samples were not re-analyzed for this analyte 1 Terms mae (4) The spike level did not contain De target analyte. PAGE 45 OF 60 sumer 3M_M N01596119 33663300..00117700 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 21 continued. CGMN-GW-MW110-140424 se 3M LIMS ID lowe Description ome [mar [we] PFDA!zl Concentration | FE [nen |"Loney|Eamon | (n~l/mL) %Recoven/ PFUnA i=l Concentration (n~/mL) %Recover,,/ PFDoA 1 Concentration (n~lfmL! %Recovered/ ISO11-01-03-14-035 CGMI'4-GW-MW110-0-140424 <0.0250 NA <0.0250 NA <0.0250 NA omEEE(rE[E ISO11-01-03-14-036 ISO11-01-03-14-037 ISO11-01-03-14-038 CGMN-GW-MW110-DB-140424 CGMN-GW-MW110-LS-140424 CGMN-GW-MW110-HS-140424 <0.0250 153 NA (4) NA 96.2 NA (4 <0.0250 15.5 NA ~4) EEE] NA 97.5 NA :4 <0.0250 15.3 NA ~4) NA 96.2 NA (4) Average Concentration (ng/mL) + %RPD <0.02S0 ng/mL <0.0250 ng/mL <O.O2S0 ng/mL swe 3M LIMS ID Jogen Description | Ri |smn|"To [ney| "El[smn| PFBS(~) Concentration (ng/mL) %Recovery PFHS (zl Concentration (ng/mL) %Recovery PFOS (~} Concentra~on (ng/mL) %Recovery ISOll-01-03-14-035 CGMN-GW-MW110-O-140424 871 HA 21.2 NA ISO11-01 .-03-14-036 CGMN-GW-MW110-DB-140424 85 1 NA 20.5 NA ISO11-01 .-03-14-037 CGMN-GW-MW110-LS-140424 NA (~) NA (3; 33.7 80.5 ISOll -01 .-03-14-038 CGMI'4-GW-MW110-HS-140424 185 9.9 NA NA Average Concentration (ng/mL) 4. %RPD me 3M LIMS ID Toman I Description 86.1 ng/mL 4. 2.3% 20.9 ng/mL 4- 3.3% [mma oron [min erat| ~C3-PFBAg) | nee [smo | sty|sng| %Recovery I~C4-PFOA g) %Recover~ ~C2-PFUnA i~) %Recovery I~C4.PFOS ~) %Recevery ISO11-01-03-14-035 CGMN-GW-MW110-0-140424 101 102 100 93.6 mm ISO11-01-03-14-036 ISQll-01-03-14-037 ISQll-01-03-14-038 === CGMN-GW-MW110-DB-140424 CGMN-GW-MW110-LS-140424 CGMN-GW-MW110-HS-140424 HHHE 96.6 NA ~' 104 97.3 NA '~ 99.6 95.3 106 99.8 91.7 92.8 96.4 Average Recovery (%) 4- %RSD 101%4.3.7% 99.7% 4.2A% nes NA = Not Applicable ETRE tsttre, NO = Not Calculated; Spike level was less lhan O.Sx the endogenous sample concentration. E Ce m (1) Samples were analyzed using exlemal standard calibration. # Semis (2) Samples were analyzed using internal standard calibration. (3) Samplas were not re-analyzed ler this analyte (4) The spike level did not contain the target analyte. 100%4.4.4% 93.6%4.2.1% 12.4 NA 12.6 NA 26.3 93.9 114 103 12.5 ng/mL 4- 1.6% PAGE 46 OF 60 sw_morsasizo 3M_MN01596120 33663300..00117711 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 22. CGMN-GW-PW09-140425 ~) somsoJomsmn [w |"w0e srT |"0e [sty[m |e"eea [tc | 3M LIMS ID ISQ11-01-0.3-14-039 EE HHEA RE ISOll-01-03-14-040 ISOll-01-03-14-041 Description CGMN-GW-PW09-0-140425 CGMN-GW-PW09-DB-140425 C G MI'4 -GW-PW09-FMS-140425 PFBA Cencentration (ngtmL) %Recovery 4 18 NA 410 NA 614 NC PFPeA Concentration (ngJmL) %Recovery 0 268 0.275 2.17 NA NA 94.9 PFHxA Concentration (nglmL) %Recovery Q 127 0.143 2.08 NA NA 97.3 Average Concentration (ng/mL) 4- %RPD 4.14 ngknL 4- 1.9o/= 0.272 ng/mL 4- 2.6% 0.135 ng/mL 4- 12% sone Loman 3M LIMS ID Description | |crc [0 tre | EE src PFHpA Concentration (ng/mL) %Recovery PFOA Concentration (n1JmL) %Recovery PFNA Concentration (nglmL) %Recovery IS011-01-03-14-039 CG MI'4 -GW-F~W09-0-140425 En . ISO11-01-03-14-040 ISO11-01-03-14-041 CG MI'4 -GW-F~W09-DB- 140425 CG MI~ -GW-F~W09-FMS-140425 Average Concentration (ng/mL) 4- %RPD 0.0443 NA me 0.0498 NA 214 105 0.0471 ng/mL -+ 12% 1.03 NA me 1.07 NA 2.69 85.4 1.05 ng/mL -+ 3.8% 0.0353 NA ms 0.0377 NA 1.89 92.7 0.0365 nglmL 4- 6.6% mane lowme [|wGo]enen| ,[om mnw y[[w oo m w Lon]| 3M LIMS ID ISOll -01-0.3-14-039 aEIRIEIEIE IEE ISO11-01-03-14-040 Description CG M N -GW-PW09-0-140425 CGMN-GW-PW09-DB-140425 PFDA Concentration (n~mL) %Recover' <0.0250 NA <0.0250 NA PFUnA Concentration (n1JmL) %Recovery <0.0250 NA <0.0250 NA PFDoA Concentration (ng/mL) %Recovery <0.0250 NA <0.0250 NA ISOll-01-03-14-041 CGMN-GW-PW09-FMS-140425 1 82 91.0 1.90 95.0 1.99 99.5 Average Concentration (n1/mL) 4- %RPD <0.0250 ng/mL <0.02~0 ng/mL <0.0250 ng/mL I Na: ov ta nde errsr coment. NA = Not Applicable NC = Not Calculated; Spike level was loss than 0.Sx the endogenous sample concen~ation. (1) Samples were analyzed using internal standard calibration. PAGE 47 OF 60 awmorssran 3M_MN01596121 33663300.00117722 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 22 continued. CGMN-GW-PW09-140425 (1} mse Jo| wsme e stony| |"EawneT eTs|e TEa[an] ce | 3M LIMS ID DeecripLion PFBS Concentration (ng/mL) %Recovery PFHS Concentration (ngJrnL) %Recovery PFOS Co~centraaon (ng/mL) %Recovery ISOll-01-03-14-039 CG MI~ -GW-PW09-0-140425 ISO11-01-03-14-040 CGMN-GW-PW09-DB-140425 enemas ISOll-01-03-14-041 CG MI~ -GW-PW09-FMS-140425 Average Concentration (ng/mL) -+ %RPD 0.150 NA 0.0823 NA 1.62 NA 0.145 NA 0.0852 NA 1.58 NA | osargeizai, | esr|main] 1 79 82.1 0.148 nglmL -+ 3.4% 1.87 89.3 0.0838 ng/mL -+ 3.5% 3/!4 99.5 1.60 ng/mL -+ 2.5% Sms 3M LIMS ID Tome I Description eee,Teng one Toner | I~C~.PFBA %Recovery ~C=-PFOA %Recovery I~C2-PFUnA %Recovery ~C4-PFOS %Recovery Fmt ISO11-01-03-14-039 ISO11-01-03-14-040 ISOll-01-03-14-041 ol EERE CGMN-GW-PW09-0-140425 C G MI'4 -GW-PW09-DB- 140425 CGMN-GW-PW09-FMS-140425 9&0 102 99.9 95.4 99.4 87.5 96.2 90.9 91.6 Average Recovery (%) 4- %RSD 100% 4- 2.0% 94.1% 4- 6A% ---- NA = Not Applicable E STE te m be evn NC = Not Calculated; Spike level was less than 0.Sx the endogenous sample concentration. 92.9%4-3.1% (1) Samples were analyzed using internal standard calibration. ~6.6 97.9 99.7 98,1% 4-1.6% PAGE 48 OF 60 aw morsetzz 3M_MN01596122 33663300..00117733 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 23. CGMN-GW-PW10-140425 (11 sane 3M LIMS ID Jourem Description JB] cour [0 | renee| "5 {ener [ema PFBA | ema PFPeA Concentration (ng~mL) %Recovery Concentration (ngJmL) %Recovery ees] PFHxA Concentration (nglmL) %Recovery IS011-01-03-14-{342 CG MlY -GW-PW 19-0-149425 ISOll-01-03-14-043 CGMN-GW-PW10-DB-140425 ISOll-01-03-14-044 CGMII-GW-PW10-FMS-140425 Average Concentration (ng/mL) -+ %RPD 4.99 NA 515 NA 716 NC 5.07 ngknL _+ 3.2/= 0 250 NA 0.254 NA 2.22 98.4 0.252 ng/mL-+ 1.6% 0 134 NA 0.167 NA 2.13 99.0 0,151 n~/mL _+ 22% ~ muse l1 owme [meeren[] oiwena y| [omem Loan]] 3M LIMS ID ISOll -01-03-14-042 ETL ISOll-01-03-14-043 Description CGMN-GW-PW 10-0-140425 CGMN-GW-PW10-DB-140425 PFH )A Concentration (ng/mL) %Recovery 0.0420 NA 0.0517 NA PFOA Concentration (ngJmL) %Recovery 0.421 NA 0.420 NA PFNA Concentration (ngfmL) %Recovery <0.0250 NA <0.0250 NA ISOll-01-03-14-044 CGMII-GW-PWl0-FMS-140425 1 92 93.7 2.32 98.~ 1.88 94.0 Average Concentration Ing/mL) %RPD 0.0469 ng~mL 21% (2) 0.421 ng/mL -+ 0.24% <0.0250 ng/mL [won [ews [wow] 3M LIMS ID Description ISOll-01-03-14-042 Ee TIT ISOll-01-03-14-043 ISOll-01-03-14-044 CGMN-GW-PW10-0-140425 CGMII-GW-PW10-DB-140425 CGMlY-GW-PW10-FMS-140425 =ee Average Concentration (ng/mL) -+ %RPD PFDA Concentration (ngtmL) %Recovew <0.0250 NA <0.0250 NA 1 83 91.5 <0.0250 ng/mL PFUnA Concentration (ng~mL) %Recovery <0.0250 NA <0.0250 NA 1.93 96.5 <0.0250 ng/mL PFDoA Concentration (ng/mL) %Recovery <0.0250 IdA <0.0250 IdA 1.97 98.5 <0.0250 ng/mL NA = Not Applicable Petree ar ri NC = Not Calculated; Spike level was less lhan 0.Sx the endogenous sample concentration. (1) Samples were analyzed using internal standard calibration (2) Sample/~ample duplica[u RPD did no[ mee[ accepLance cri[eria of <20%. PAGE 49 OF" 60 3M_MN01596123 33663300..00117744 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 23 continued. CGMN-GW-PW10-140425 (1} mse Jowsme | e |stony|"EawneT eTs|e TEa[an] ce | 3M LIMS ID DescripLion PFBS Concentration (ng/mL) %Recovery PFHS Concentration (ngJmL) %Recovery PFOS Cor~centration (ng/mL) %Recovery ISOll-01-33-14-042 CGMN-GW-PW10-0-140425 ISOll-01-03-14-043 CGMF4-GW-PW10-DB-140425 eetoemnenara | ISOll-01-03-14-044 CGMI~-GW-PW10-FMS-140425 Average Concentration (ng/mL) -+ %RPD 9.450 NA 0.481 NA osmrgnizen, | 211 82.0 0.471 nglmL -+ 4.5,/o 0.105 NA 0.115 NA avian 1.92 90.5 0.110 ng/mL -+ 9.1% 0.438 NA 0.435 NA |serie] 2.31 101 ti.437 ng/mL -+ 0.69% Sms 3M LIMS ID Tome I Description eee,Teng one Toner | I~C~.PFBA %Recovery ~C=-PFOA %Recovery I~C2-PFUnA %Recovery ~C4-PFOS %Recovery Fmt ISOll-01433-14-042 ISOll-01433-14-043 ISOll-01-03-14-044 el[sz]&] = CGMN-GW-PW10-0-140425 CGMN-GW-PW10-DB-140425 CGMN-GW-PW10-FMS-140425 99.2 97.7 98.5 87.6 ~0~ 95.5 95.9 99.8 97.6 94.1 88.4 93.4 Average Recovery (%) _+ %RSD 98.5% 4- 0.76% 94.7% 4- 7.1% wee NA = Not Applicable Sr mea NC = Not Calculated; Spike level was less than 0.Sx the endogenous sample concen~ation. (1) Samples were analyzed using internal standard calibration. es mtet aes en 20. (2) Sample/sample duplicate RPD did nat meet acceptance criteda of-<20%. 97.8% 4- 2.0% 92,0% 4- 3.4% PAGE 50 OF 60 aw morsetae 3M_MN01596124 33663300..00117755 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 24. CGMN-GW-TRIP-140423 (1) FRR 3M LIMS ID FODescription mT Te PFBA Concentration Cc) FU =) FU 0) po (ng/mL) %Recovery PFPeA Concentration (ng/mL) %Recovery PFHxA Concentration (ng/mL) %Recovery ISOll-01-03-14-046 IS011-01-0,3-14-PA7 ISOll-01-03-14-048 ISOll-01-03-14-049 CGMN-GW-TRIP-0-140423 CGMN-GW-TRIP-LS-14(]423 CGMN-GW-TRIP-MS-140423 CGMN-GW-TRIP-HS-140423 FP3M LIMS ID PODescription <0 05~30 NA <0 0250 NA <0 0250 IdA 200 "00 1 86 930 1 82 91 0 5.19 51.9 '~ 4.96 49.6 '~! 4.79 47.9 990 99.0 NA I:~l NA :~) NA I,~l NA ~:~) om | we | PFHpA Concentration LC PL (ng/mL) %Recevery PFOA Concentration (ng/mL) %Recovery PFNA Concentration (ng/mL) %Recovery ISOll-01-03-14-046 ISOll-01-03-14-047 ISOll-01-03-14-048 ISOll-01-03-14-049 CGMN-GW-TRIP-0-140423 CGMN-GW-TRIP-LS-140423 CGMN-GW-TRIP-MS-140423 CGMN-GW-TRIP-HS-140423 FR 3M LIMS ID FODescription <00250 NA <0.0480 NA <0.0250 NA 1.94 97.0 1.79 93.2 1.81 90.5 4.88 48.8 ~2: 4.91 51.3 ~2: 4.69 46.9 i2) NA (3) NA (3) 85.4 86.4 NA ~3) NA (3) Tr PFDA Concentration =) FO ==) FO =) (ng/mL) %Recovery PFUnA Concentration (ng/mL) %Recovery PFDoA Concentration (ng/mL) %Recovery ISOll-01-03-14-046 CGMN-GW-TRIP-0-140423 <0.0250 ISOll-01-03-14-047 CGMN-GW-TRIP-LS-140423 1.82 ISOll-01-03-14-048 CGMN-GW-TRIP-MS-140423 4.74 ISOll-01-03-14-049 CGMN-GW-TRIP-HS-140423 NA (3] NA = Not Applicable _ (1) Samples were analyzed using internal standard calibration. (2) Field matdx spike recovery did not meel acceptance criteda of 100 + 30%. 8 Tenatiwnp aiann (3) The spike level did not contain lhe target analy[e. HA 91.0 47.4 ~:~ NA (3: <0.0250 1.83 4.9g NA (3) NA 94.0 49.9 (2: NA :3: <0.0250 1.89 4.93 NA ~3) NA 94.5 49.3 i2) NA (3) PAGE 51 OF" 80 awmersers 3M_MN01596125 33663300..00117766 3M ENVIRONM~-NTAL LABORA TOR Y REPORT NO. IS011-01-03-14 Table 24 continued. CGMN-GW-TRIP-140423 (1) mune 3M LIMS ID Jone Description [ws | me PFBS Concentration | | | | (ng/mL) %Recovery PFHS Concentration (ng/mL) %Recovery we] PFOS Concentration "EE[ate (ng/mL) %Recovery ISOll-01-03-14-046 ISOll-01-03-14-047 ISOll-01-03-14-048 IS011-01-03-14-O49 CG MII -GW-TRI P-0-140423 CGMII-GW-TRIP-LS-140423 CGMII-GW-TRIP-MS-140423 CGMN-GW-TRIP-HS-140423 <0.0250 1.67 4.19 71 8 NA 83.5 41.9 ':~ 72.5 <0.0250 1.78 4.63 83.9 NA 89.0 46.3 ,:2) 84.7 <0.185 1.77 4.50 102 NA 95.7 48.5 i2) 103 3M so LIMS ID Tomarpien I Description | Snecovey |Secomy| stocomy|sutwcomery | I~C~-PFBA %Recovery ~C,~-PFOA %Recove[y I~C2-PFUnA %Recovery ~C4-PFOS %Recovery ISOll-01-03-14-046 CGMN-GW-TRIP-0-14O423 100 104 97.2 99.1 ISO11-01-03-14-047 CGMII-GW-TRIP-LS-140423 97.3 90.5 95.2 99.7 ISO11-01-03-14-048 CGMII-GW-TRIP-MS-140423 104 109 100 99.0 ISOll -01-03-14-049 CG MI'4 -GW-TRI P-H S-140423 98.3 103 97.0 89.2 T Emm e NA = Not Applicable (1) Samples were analy~ed using internal standard calibration. (2) Field matrix spike recovery did not meet acceptance criteda of 100 + 30%. (3) The spike level did not contain Me target analyte PAGE 52 OF 60 ners 3M_MN01596126 33663300..00117777 TERT, 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 55 CCoonncclluussiioonn nostra wre tdi forts sdsci rr Laboratory control spikes were used to determine the analytical method accuracy and precision for all Fctgoplvamisackpmsoapihissirsr sep sr analytes. The accuracy and precision were then used to estimate the method uncertainty for the reas pd Pos pa8 results. Field matrix spike recoveries demonstrated that the analytical method was appropriate for the rember par apt given sample matrix. Analysis was completed using 3M Environmental Laboratory method ETS-8a oFe B Compr neNn: 044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Ss ean ra i oo 0 rg Direct Injection Analysis". Analytical results are reported in Table 1 and 10-24 of this report. Eremmoanadvcattarratsa comrsdy dc rds 66 DDaattaa// SSaammppllee RReetteennttiioonn All remaining sample and associated project data (hardcopy and electronic) will be archived according to 3M Environmental Laboratory standard operating procedures. mr: Soto tor tr sc Cole rs 77 AAttttaacchhmmeennttss Attachment A: Select target analyte historical trend data for select Cottage Grove locations. 88 SSiiggnnaattuurreess Digitally signed by Susan T Wolf DN: c=US, st=~,4N, I=St Paul, ou=3M Environmental Laboratory, - authenticated hen > Moly EERE Reason: I have reviewed 1his dooun1~nt Date: 2014.0527 12:1723 -05'00' SETTER -- Susan T. Wolf, 3M Principal Analytical Investigator Digi[ally slgrl~d by Willarn K DN: c=US, st=\4N, I=St Paul, Environmental Laboratory - authenticatec byl RA email=wkreagen@mmm corn EE o=3M, on=William K. Reagan Reason: I am apprcvlng this document Date: 2014.0527 12:57:44 William K. Reagen, Ph.D., 3M Environmental Laboratory Technical Director pTi on EelQty erencinto dftsi The 3M Environmental Laboratory's Quality Assurance Unit has audited the data and report for this project. E-- EQuality Assurance Representative Dtiest rmtihal,l ot be reprodicd xcpt nl, ct itn ppl of th This test report shall not be reproduced except in full, without written approval of the 3M Environmental Laboratory. 33663300..00117788 PAGE 53 OF 60 3M MN01596127 ERAT Kotoraats 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 tachmenAt: Slot TargetAnaHistoriTrcenad Dataurcfnsl. Attachment A: Select Target Analyte Historical Trend Data; units of ng/mL wor MW07 | Tree * Ta tyTe Ny :PFBA ~ PFO$ -- @ -- PFOA wer onsnon MW07 10/15/2012 PFBA 2.55 PFOA 0.298 PFBS <0.0250 wzPFOS MW12 0.0257 @ :PFBS men 1/29/2013 2.09 0.259 <0.0250 0.0439 wen 4/22/2013 2.61 0.240 0.0268 0.0459 pn 7/23/2013 1.71 0.303 0.0396 0.241 non 10/28/2013 3.07 0.428 0.0291 0.104 vino 1/13/2014 2.88 0.390 <0.100 0.104 smo 4/23/2014 2.48 0.344 0.0360 0.0493 | --t--t--t--p----} Te Te Ny eS, :PFBA @ :PFH:S ------ ~ ----- PFOA @ F'FO$ -- ~1 -- :RFES werMW12 wan 10/19/2012 von 1/30/2013 O en 4/25/2013 wes 7/24/2013 PFBA 975 484 622 1110 PFOA 1390 946 1020 2000 PFBS 94.3 91.4 105 175 PFHS 20.9 13.7 16.4 23.9 PFOS 122 143 145 204 waves 10/31/2013 4O8 954 87.7 13 131 sas 1/16/2014 312 668 82.1 13.1 121 ae 4/25/2014 22O 548 68.9 9.82 117 33663300..00117799 srcesorm PAGE 54 OF 60 _Motses1z 3M MN01596128 ERAT Kotoraats 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 AtachAmcoonntat: Soc Target Anata Historical Ten Dat: riof rgs Attachment A continued: Select Target Analyte Historical Trend Data; units of ng/mL wis MW13 o [=e---. aN ~ L ty Bt ee Te t= mmo re wer wen sms wmies MW13 10/17/2012 1/29/2013 4/24/2013 wes wees 7/23/2013 10/30/2013 PFBA 7.10 5.60 9.34 8.30 6.48 PFOA 3.33 2.56 5.46 6.17 4.01 PFBS PFHS nsPFOS wie MW16 0.619 we0.487 3.85 0.560 am0.396 3.92 0.972 am0.931 4.05 1.07 0.571 awe 1.05 0.366 4.02 1.40 wwion sie 1/14/2014 4/24/2014 9,80 7.14 9.78 8.63 1.20 0.752 mm 0.969 3.08 0.556 2.33 dre es oe Som N%. %N_ R% RNY wonMW16 PFBA PFOA PFBS PFHS PFOS ww 10/1812012 33.6 45.9 25.7 2.71 23.1 en 1/29/2013 31.5 42.6 28.3 2.54 20.2 won 4/2412013 33.2 43.8 27.5 2.74 21.8 em 7/24/2013 26.3 39.9 29.6 2.83 20.1 wp 10/30/2013 1/14/2014 45.0 42.9 73.9 91.0 42.1 40.0 3.95 5.52 38.2 53.1 awe 4/24/2014 40,7 85.7 37.9 4.49 513 33663300..00118800 ressor PAGE 55 OF 60 aumnotss12s0 3M MN01596129 ERAT Kotoraats 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 AlachAmconetinnuetd: SelectTargetAnata Historical TrendDat:usof inl. Attachment A continued: Select Target Analyte Historical Trend Data; units of ng/mL wir MW101 we - = - Etter aot mg eee Ca wh RN FOA @ :P:F~SS @ win MW101 onsen 10/18/2012 uns 1/30/2013 vis 4/23/2013 nw 7/25/2013 PFBA 1860 1630 1830 1680 PFOA 147 124 121 112 PFBS PFHS osPFOS wiz MWI02 23.9 25.2 19,5 24.0 wom om ow 427 154 455 206 459 188 464 189 nes 10/30/2013 1020 86.7 25.5 om314 158 wisp 1/15/2014 avi 4/25/2014 1510 1330 79.4 76.0 25.4 37,8 mm 398 159 364 135 - PFHS ~ ee tt ENwh3 ~. PFOS MWI02 PFBA PFOA PFBS PFHS PFOS 10/18/2012 648 42.2 5.52 129 107 4/25/2013 621 62.0 4.57 401 250 4/25/2014 919 58.1 7,12 147 67.4 33663300..00118811 srceseorm PAGE 56 OF 60 W_Mo1se6130 3M MN01596130 SS 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 AMachAmcoenntdt: Sct Target AnataHiscl Tend Dat: riof rgs Attachment A continued: Select Target Analyte Historical Trend Data; units of ng/mL ios MWI03 . a ~ a, , *, t= mmo re wes MWI03 en 10/18/2012 nso 4/25/2013 sso 4/25/2014 PFBA 226 241 241 PFOA 115 126 121 PFBS PFHS -PFOS ioe MWI04 7.16 7.01 6.51 - wm 26.2 4.02 24.7 1.55 21.8 7.82 a 7 of v TN as -- =r= PRINA \L / BN NT PFOA @ wee MWI04 _PFBA won 10/18/2012 ee36.0 eas 1/30/2013 me36.3 von 4/25/2013 we74.7 sans womens 7/25/2013 wee 54.3 10/30/2013 53.6 PFOA 42.0 44.8 60.7 74.7 72.5 PFBS 12.6 11.4 9.75 8.16 7.95 PFHS PFOS 8.69 127 9.07 201 13.4 lg5 11.8 176 i0.i 165 ss sie i/is/2oi4 mm 202 4/25/2014 107 35.1 82.1 7.50 8.10 14.2 12.6 4.25 234 33663300..00118822 [r-- PAGE 57 OF 60 aw_Notsse3t 3M MN01596131 ERKA ot orT aats 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 AtachAmcoonntat: Soc Target Anata Historical Ten Dat: riof rgs Attachment A continued: Select Target Analyte Historical Trend Data; units of ng/mL ios MWI05 MN" " //AA\\ /\ a. ot mmMotNsM RNR F~FOA @ :p:F~SS @ J MWI05 10/19/2012 1/30/2013 4/25/2013 | 7/25/2013 PFBA 52.7 54.4 57.0 71.6 PFOA 98.3 119 104 70.6 PFBS PFHS nsPFOS ios MWI08 9.46 8.03 5.72 6.49 w wm wm wm 18.9 21.1 16.0 6.35 120 129 95.0 92.3 ------ 10/30/2013 1/14!2014 4/25/2014 38.9 55.6 71.0 87.2 68,3 44.3 4.98 6.15 7.68 ow mw 6.01 467 12.6 152 8.59 58.7 ie,i, Som NN NN won MW108 PFBA PFOA PFBS PFHS PFOS er 10/18/2012 155 550 30.5 20.7 55.2 a 1/30/2013 101 348 26.5 11.1 45.5 va4/25/2013 42.5 201 16.1 4.95 37,3 a 7/24/2013 38.0 202 14.6 4.94 26.8 10/30/2013 51.7 218 21.6 4.47 33.2 1/14/2014 51.6 169 17.0 4.13 33.5 4/25/2014 65.4 164 17.4 3.58 43.3 33663300..00118833 resecr PAGE 58 OF 60 au_mnots1s3s2 3M MN01596132 Re Soros 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 tAttaachcmehntAmAccoeonnttininnuuetedd:: SSeelleeccttTTaarrggeettAAnnaalytte HHiissttoorriiccaall TTrreenndd at;Data; atof isnl units of ng/mL wo MW110 . . Teed Hae [= E Me Nd N RR :PFBA ~ PFOA @ :P:F~SS @ RN, wo MW110 avon 10/18/2012 on 1/30/2013 use 4/25/2013 nm 7/24/2013 PFBA 144 171 183 304 PFOA 193 141 160 144 PFBS 39.6 46.6 66,7 43.8 esPFHS PFOS Pus PW09 me me me wa 17.6 21.6 10.3 28.6 11,8 26,4 9.41 17.8 wes 10/30/2013 174 190 94.8 om~5.3 21.1 vis 1/14/2014 179 248 85.1 om19.4 12.1 avs 4/24/2014 189 310 86,1 ous20,9 12.5 |a Bs NR NN ron asin cnet va wa ws PW09 4/25/2013 6/19/2013 7/24/2013 8/29/2013 9/30/2013 PFBA 3.72 NA 2.95 NA NA PFOA 0.223 0.462 0.624 0.605 0.873 Nts tow relrs slvit PFOS 0,324 0.376 0.622 0.818 1.38 HA=Not applicable; analyte was not requested for this sampling event. nos 10/29/2013 4.53 1.02 1.52 yi 1/15/2014 4.76 1.33 2.13 AA 4/25/2014 4.14 1.05 1.60 33663300..00118844 oncescren PAGE 59 OF 60 _MNO1S56133 3M MN01596133 ERKA ot orT aats 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-14 AtachAmcoonntat: Soc Target Anata Historical Ten Dat: rofs rg Attachment A continued: Select Target Analyte Historical Trend Data; units of ng/mL puto PW10 ee Te RN, RN, PW10 A 4/25/2013 6/19/2013 7/24/2013 8/29/2013 9/30/2013 10/29/2013 1/22/2014 4/25/2014 PFBA 4.25 NA 3.37 NA NA 6.09 4.40 5.07 PFOA 0.428 0.415 0.420 0.471 0.528 0.524 0.212 0.421 PFBS 0.594 NA 0.540 NA NA 0.703 0.261 0.471 PFHS 0.197 NA 0.185 NA NA 0.193 0.0485 0.110 [PE ------------ PFOS 0.396 0.401 0.38 0.415 NA=Not applicable; analyte was not requested for this sampling event. 0.465 0.458 0.124 0.437 33663300..00118855 [ro PAGE 60 OF 60 auotss1s34 3M MN01596134 ovnowsTtoLny oes Chin-afCoty ENVIRONIVl ENTAL LABORATORY ,Shipping Address: 3M Environmental Labora:crY SaCnoma SBpEo 15 3M Cen~,e~, Bid# 260~5N~I 7 Prec 5011010314 St. Paul, MN 55144 Phone: 851 rsser Phoae: (65!) 733-9873 AFan Pr1o6n5e) 7(50390)018976.0886 All. Phone: (651) 736-6559 DREepsaeItR: o4u52i09,0 nSsie SRoounracel:d Project Number 007338015 Departme>~: 432C.90 S~{e Source: (0M1A1P90L2E0 0 l J9C020 Fax: {65!) 7334687 PCroomjpeclteLtieoand:DaSsu:san T. Wolf PDPrruoot,soCtcrt eDNemtcaemepbte~4io1n40:0370C311a43g80e~ 5 Grove OW Sapling 2nd Quer 2014 FPPPiharaqooiin:~eleectANNdLudeurmaedsois:e.rS: uv66so55al1nJ i7-7T33.G33.W,m-9-a9o88l5mf51cen MSsmpieNentes Sanne ein DimeSmad Matix Comma sons von | Comovowanis 1 gay Sota oe Jomoverimmwos EE Tih pg | | J] sonar JoonvavevrssmnTulssi wil TT ree ce T [ronan ioon Toowovman wot --e Tir] psoioriseoy Tcomonamnos oun ionJoonevwing og ison ovar roo: comovamrien Forors|rcoiwovrmommn i t,;('}'..-014)3-~44.q4 ~" ..... ', - [iff aT Tw TT] TYP I FjZaPsReYA 6 Some ComtitonUpon -- Recipe Dc C1 Accept Oreeoncaontee CJ Alton conned for Ors coa nan -- iy T70-- 41 HUN-- TER. -- PR -- Keita bs Due Time Supp Va Recut ve lime Shipl}ed Via l{~ce~v~d Date IB tie [ - NN -- Page ots Page 1 of 4 _3MMNMON10S155696113355 33663300..00118866 Project: |.~011~1-03- t 4 (con L) ENVIRONMENTAL LaRORATORY Chaln-of-Custody G Shipuing AddreS: p 333MMM CCEeennnwttereorrnmBBieidgng$la22l66-00a.5b5NoM.r..a11[7o7r7 St, PaU!, MN 55144 Ay Phone: (651} 7~-9873 bigAft, Phone (51) ,,~6-6s59 Fax: {651) 733~4687 Corn pletien Dare: Projed Lead: Susai~ T Wolf Pt:,oa ~ N tim ~er: ~5 ] ,,?33 ~985 ~)nail Addrc.~s: ~r,voll~mm ntcom uggs Toomwoagns mer ToT ] pfe onenTTomoeormnuesJpsedT ToTe T T ] re Eee er a ono e [emer T T wT] Ee Ta ea ] 1501010510] commas Mw ~ "l'mpera~ure: Constr Deg C 700 ~ Received o~ lee Or ~ Other: curse by: - Fl JX Date l-i~r e 3363300..001187 I Page 2 054 3M MN01596136 ENVIROCNhMuiEnNaTt-ACLustLaAdByORATORY SmCeorgteiBisgg:Seoy SPC S514 Prsject roJect: ItSSOO1l11L-.0011-0036--1144 (cont AFAPParIhtox.onPPneheh:6o:on5ne((1e6:6:55(11()66)255377114)33)03377.5-3g3576868.7-76833555590 Deegpuaensnee:n:K4o5t20i9,0 JSamieSsoRurocnea: (1MIIACPOL2E0WG Pojct Number 0073138015 Fax. ,65I; ~33-4687 CPormeplcetLieoadn:DaStuesaTn. Wolf DPureicCerDieesdcrp4i1o4n20C1a4nage Grove GW Sampling: 2nd Quarer 2014 EPPPmhh,"aoooinnileeectANNLudumemebasedbr::e:tS: tu6655o~1t.f-7T7_33G33W.m-99om88l55fc1on Email k d~less: stv,'o4:~mum.com Semple Nonber Gpronosieon Same Desrien DatcTime Somaled Mats Comment Toom wgovTwomoeTn Tg emery Fe T4 -- ororeoe |emo el] pronsiengy JeonammmyToT ] 501010110301100004] JecoommoawnemvtesosZn| T] hi owme [ T TT T ] 150110, 0014017 JsmovmneTT Isoirormaon pronwevion Tesmon 2 un . TT Jenoowenr ov{sjamrn] rF onson Jomo wisS T7u 27207TU] sO10L03150 | comvonranvs. 4 0923 PERT Semple Condition poo Recent 3 ceptable -- pac Oeste CJ lems acount for ome "l'eml~eraturt~r Deg (2 Colaavy rin: Relsquinhdby: |'{dinquis~ed b~: [ TopL 11/0o i17 me DaeDat~ me Swpivie !'ime Reet Shipped Via Rece~ed by: T gfe gE : bie Te Dat~ gime -- PaPaggee s3 ort of '~ S3MW_MMNNO011S59966113377 33663300..00118888 WW EENSVVIIRROOCNNiMMnEENNaTTCAAuLLnoLLnAAyBBOORRAAT1XOR)RYy S Shipping Address: e 3M Envlronrnenta L~i:eratcl~, S Sonara en abt 3M Cemer, Bid<~ 260-5N-" T Frist 50101814 coy AFPSroto.nPPeaar:uol,enMaNS1n 5153s+37453a88753520 ORPoeepertntee:n:nKo5o2t50i00.,75amoSeiesvSRoonsess (1MA0PLmEWO PCornepstetiaon:DSuoTe wit PDoareesCoDmeetsi:iaCtote rns GW Sampling, ad Qa 201. EFoaneANdaebsesS5ohlrGmammentsom Sunken Sung bein DusSotma iMancs Comes ison avon vary[onomis digs froin Teomormine jens [ly ee[27] Tye oonones |TocmmoowvommviammmsmsT ] = [ ] TT sonore eos ours JToewonnoovivnmgmeyy| T= T [ES Sonor |[eCoonmoroermansn TATE TTp ale ws 7[W ] ] emptor cova C~qlected b~ tprint): Cambs Relinquished by: r oc Ol heonctontee Doin 770 Zovzie coterie ok ree nemSEEJN .+;(,+ Date Time Sh pped Via Received by: 7'~ Date Time 33663300..0011889 Pasion Page 4 of 4 Su umorsseiss 3M MN01596138 JJUULLYY 22001144 33663300.~001i9900 3M_MNO1596139 3M MN01596139 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-16 FFiinnaall RReeppoorrtt AAnnaallyyssiissooff PPFFBBAA,, PPFFOOAA,, PPFFBBSS,, PPFFHHSS,, aanndd PPFFOOSS iinn AAqquueeoouuss SSaammpplleess,, CCoottttaaggee GGrroovvee GGrroouunnddwwaatteerr SSaammpplliinngg 33r"d QQuuaarrtteerr 22001144 Laboratory Rogues Number 15011010316 Laboratory Request Number: ISO11-01-03-16 otterLa Sr Report Date - Date of Last Signature TTeessttiinngg LLaabboorraattoorryy a sas poraions 3M EHS&S Operations 33MM EEnnvviirroonnmmeennttaall LLaabboorraattoorryy Buono Building 260-5N-17 Moplonser NN. 351441060 Maplewood, MN 55144-1000 Requestor Requester SSnM SbootinWgN255451144015000 GGaarryy HHoohheennsstteeiinn 33MM EEHHSS&&SS OOppeerraattiioonnss 3M Building 224-5W-03 Saint Paul, MN 55144-1000 PPhhoonnee:: ((685511)) 773377--33557700 fe B>oeurWwoRm The testing reported herein meet the requirements of ANSI/ISO/IEC 17025:2005 TE eeete ots Tye "General Requirements for the Competence of Testing and Calibration SEITRIRIREIILS Bonn Laboratories", in accordance with A2LA Certificate # 2052.01. Additionally, the iSaias s E ar l,TShesEh laboratory's quality system has been audited and was determined to be in conformance with the EPA GLPs (40 CFR 792) by an independent A2LA assessmenL 33663300..00119911 J. PAGE 1 OF 37 -- 3M MN01596140 REPORTING1501 0118 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-16 3H3r~ EEnnvviirroonnmmeennttaall LLaabboorraattoorryy 333MMM PEErnnivnvicirrioopnanlmmeAennntataabll LtLacababoorvraaottsoortryytTTeoecrch:hnniScicuaaslaDDneirWecocttlo:r: Wika K William K. Reagen, Reagen, PhD. Ph.D. Report Author:Chelsie 3M Principal Analytical Report Author: Chelsie Grochow Investigator: Grochow Susan Wolf AAnnaal~yytt~iccaalJ RReppoor~t ~ISSO01111-o0011-o0033-o116~ ``AACnnoaatllayysgs'oissGoorffoPPvFFeBAGA,r,oPPunFFdOOwAAa,,tePPrFFBSSSa,,mPPpFFiHHnSS-,g,3aannddQuPPaFFrOOteSSrii2nn0AA1qq4uueoouss SSaammppleless,, Cottage Grove Groundwater Sampling - 3rd Quarter 2014 RReeppoorrtt aDtaete:: DDaateeooff LLaasstt Satie Signature 11 _IInnttrroodduuccttiioonn/S/Suummmmaarryy TTShhcoelu33oMMnsEEnnpvveiirrrosononmnmeeenlntataatlltLLaahbboIoerMraatCtooarrtyyippargreeepGpararoreevddeaafnnaddcaalnnya.allyySzzaeemddpgglrreoosuunnwddewwaeattecerorslsaeacmmtpepldoleesns ccJouollllyeecc1tee6-dd1b7by,yW2W0e1esdst.toonn SSP`Seoaarlmumfptpuiloloeenosssbuwwpleeearrrneoscorrineclntuuearlmncaeedtddt(httPoeoFBtt3hhAMee),33CMMPoettEEranngfvveoiirrrGooonnroommcveeetnntaftaanalcloiLlLiataaybcb.oeorSra(aatPtmooFrrOpyyAleo)os,nnwPJJeuelrrlyeu11oc88r,o,oll22eb00cu1t1te44adnoooennsniJlceufolofyororar1i5tteh-r1eo(7Paa,Fnn2Baa0Sly1y)s.4si.ss ooff Perfluorobutanoic acid (PFBA), Perfluorooctanoic acid (PFOA), Perfluorobutane sulfonate (PFBS), nPourmfbuecrro5h0e1x1an.o0s1u.f0o3ns.ts(PFS)and Por oroocano sonal (PROS)undorlaboratory pojct Perfluorohexane sulfonate (PFHS) and Perfluorooctane sulfonate (PFOS) under laboratory project number ISO11-01-03-16. TTshahomep33lMMe sEEannvvciirrooonnnmmseeinndttaaollfLLaaabb0oordraattsoorrayyplprreeeppaaorrekeddsssaaammrpeeleduccpoolncntaatlineae,risanfnfoosdrr atwweaervlvgeelssanammpaplliyinnggolcodccaatmtoionanss.l. EsEpaakccehh. sEmEaalamcchhpCeleeommnpsttpeayttiycncceooornrsnsttirsaaetniensedeerrrwovwfeadaassffoimermaldfarreskkdaeemddmwpwalierit,hhxfaiaeslp"fdfiklllsea0tsomeheperrleree"d" ufilipnnrloeicetahadtaelt,wccaioonhrdrraesanspptoaaopnrnpgdrdeoeetpddarin0taoat4layetenmfinaafailetllidvvoosmluupaimmtkroeeioxsofsfpo22ik0o0e00n. cbCmoooLtnn.itaetCisanoiwinnnegtarthihneefeorttsraatrrrfgegeeesdttewraavinnehadalynfetotesersmfippaerlrldiiosormtrtaoiantbdbrieaexirinsndgpgsiksaseeensnndttwstooeuerrteho.efgof1aritetifliderfdfeoocwrmoisvthaeprmaynplsleatapccnpodorlaolnerpccdrtisniaotp,neo. mrSSaee0tllreiexbccetsnspsagaikmmesppeslloteeluottiohne fot for samplocolocton bottles were fortified with internal standards and surrogate recovery standards prior to being sent to the field for sample collection. S5`S.aa0mm4pp4ll1eessMwaweierhreoodpprroeefppanarreadeyaasnndd aoarnnaalhlyeyzzeDeddtefoorrrmPiPFnFBaBAtA,o,nPPoEFfOOPAAo,,rPuPcFFrBSrS,a,tPPoEFdHHCSS,o,maapnnoddunPPdFFsOOSSn uuWssaiinntggammbeeyithhoodd ETS- ETS- 8-044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water by LadGjMecStIiMveSs;foDircetanbajloycsteonofAsenleactssamptleosm, awesrteanadpapridcawbloere sod ta ad the co ually LC/MS/MS; Direct Injection Analysis". Internal standards were used to aid in the data quality objectives for the analysis of select samples, were applicable. TTuaaablbllleey 11cossnuumnrmaasirazizmeepssletthsheprsseaapmmapprlleeedrraeenssduultassnuuassyiiznnoggdtthhweeiaahnntaahhlyettciscaaalml pmmleeettshhooviddldibdeeeinpftiiofieerddteaasdboovavene.d. dAAilllsrcreuesssusteltssdffoorr Ssntare n his roprt quality control samples prepared elsewhere in this report. and analyzed with the samples will be reported and discussed RIA SToIwN (R RcoafE omis) se gpa rt rte HS TREE ]he testing reported herein meet the requirements of ANSIIISO/IFG 17025:2005 "General Requirements for the Competence of Testing and Calibration rvssian fhASACae WEY, Ashbm Laboratories", in accordance with A2LA Certificate # 2052.01. Additionally, the bebe cust tershisban soca 30d wsdrometobo laboratory's quality system has been audited and was determined to be in ee ELT i by cn conformance with the EPA GLPs (40 CFR 792) by an independent A2LA assessment. 33663300..00119922 encezoesr PAGE 2 OF 37 SU_MNO18%6141 3M MN01596141 TTaabbllee 11.. SSaammppllee RReessuullttss SSuummmmaarryy wes 3M ENVIRONMENT.A L LAB ORA TORY REPORT NO. IS011-01-03-16 a REA ISOll-01-03-16-001 ISOll-01-03-16-002 e EE-- E S Ee TETEn STE ISOll-01-03-16-004 ISOll-01-03-16-005 e-- e ETETR[ETE ISOll-01-93-16-007 EE a ISOll-01-93-16-008 E---- a A -- ISOll-01-03-16-010 e p a Ey llla T A[EAEE E[EA 15;] ISOll-01-03-16-011 CGMN-MW07-0-140716 CGMN-MW07-DB-140716 Average %RPD Sample/Sample Dup CGMN-MW12-0-140717 CGMN-MW12-DB-140717 Average %RPD Sample/Sample Dup CGMN-MW13-0-140716 CGMN-MW13-DB-140716 Average %RPD Sample/Sample Dup CGMN-MW14R-0-140716 CGMN-MW14R-DB-140716 Average %RPD SamplelSample Dup 3.16 2.93 3.05 7.6 157 150 154 (z~ 4.6 7.86 8.29 8.08 5.3 685 657 671 (2) 4.2 Concentration (n~llmL) 0.606 0.598 0.602 1.3 395 409 402 (z~ 3.5 13.9 14.8 14.4 6.3 430 421 426 (2~ 2,1 0.0759 0.0765 0.0762 0.79 49.3 51.4 50.4 (z/ 4.2 0.970 0.975 0.973 0.51 29.8 29.3 29.6 (2/ 1,7 0.0434 0.0398 0.0416 8.7 7.87 8.34 8.11 (z~ 5.8 0.700 0.726 0.713 3.6 20.7(2; 19.4(2~ 20.1 (2) 6,5 0.237 0.236 0.237 0.42 94.2 99.5 96.9 (2) 5.5 4.37 4.58 4.48 4.7 156(2) 159(2) 158 (2/ 1.9 ISOll-01-03-16-013 ISOll-01-03-16-014 ---- EAaL:A-- A ISOll-01-03-16-016 EmEEee [Ell alals] ISOll-01-03-16-017 e El EEe TETFHA[T2ATE] ISOll-01-03-16-019 ISO11-01-03-16-020 e EEeEl ES ATFEATEE[AEEE] ISOll-01-03-16-022 CGMN-MW16-0-140716 CGMN-MW16-DB-140716 Average %RPD Sample/Sample Dup CGMN-MW101-0-140717 CGMN-MW101-DB-140717 Average %RPD Sample/Sample Dup CGMN-MW104-0-140717 CGMN-MW104-DB-140717 Average %RPD Sample/Sample Dup CGMN-MW105-0-140717 46.7 44.7 45.7 4.4 1460 1450 1460 (2) 0.69 47.4 48.4 47.9 12) 2,1 40.9 99.1 97.4 98.3 1,7 83.5 84.2 83.9 (2) 0.83 74.4 78.5 76.5 (2) 5,4 27.3 37.4 38.3 37.9 2,4 29.5 29.0 29.3 (2) 1.7 8.62 8.74 8.68 (2) 1,4 4.87 5.39 5.52 5.46 2,4 483 477 480 (2) 1.3 8.90 8.99 8.95 (2) 1,0 6.34 57.8 56.1 57.0 3.0 191 194 193 (2) 1.6 228 238 233 (2) 4.3 37.5 ISOll-01-03-16-023 EEEEEE ISOll-01-03-16-025 ISOll-01-03-16-026 CGMN-MW105-DB-140717 Average %RPD SamplelSample Dup CGMN-MW108-0-140717 CGMN-MW108-DB-140717 Average %RPD Sample/Sample Dup 37.4 39.2 I=) 8.9 224 219 222 (2) 2.3 28.0 27.7 I~) 2.5 526 518 522 (2) 1.5 4.91 4.89 (=/ 0.82 60 5 60.9 60.7 (2) 0.66 6.96 6.65 (=~ 9.3 11 4 11.1 11.3 (2) 2.7 34.9 36.2 (=) 7.2 58 2 57.7 58.0 (2) 0.86 S CEozE rcrr eRTT E rCGRR LSRR5E] NA=NotApplicable (1) Sample set was analyzed by internal standard calibration, except where noted. The analytical method uncertainties associated with the reported results by internal standard calibration are as follows: PFBA + 17%, PFOA + 15%, PFBS + 18%, PFHS + 17%, and PFOS + feA 20%. (2) Sample set was analyzed by exlemal standard calibration. The analytical method uncertainties associated with the reported results by external standard calibration are as follows: PFBA _+ 18%, PFOA _+ 13%, PFBS _+ 15%, PFHS + 13%, and PFOS _+ 11%. (3) The sample/sample duplicate RPD did not meet acceptance criteria of-<20%. aPAGE 3 OF 37 33663300..00119933 3M MN01596142 Table 1 continued. Sample Results Summary (1) ws 3M ENWRONMENTA L LAB ORA TORY REPORT NO. IS011-01-03-16 3M LIMS ID ET ISO11-01-03-16-028 (r mag r Le 3 ISO11-01-03-16-029 Sample Description CG M N-MW 110-0-140716 CGMN-MW110-DB-140716 Average %RPD SamplelSample Dup 187 183 185 (2) 2.2 Concentration (n~llmL) 344 435 390 (2) 23 (3) 81.1 83.4 82.3 (2) 2.8 21.4 26.7 24.1 (2) 22 (~) 16.4 14.4 15.4 (2) 13 ISO11-01-03-16-031 I SO 11-01-03-16-032 Ceo mr engy rm rt hIaR s ISO11-01-03-16-034 eET TE EE ISO11-01-03-16-035 CG M N-PW09-0-140717 CGMN-PW09-DB-140717 Average %RPD SamplelSample Dup CGMN-PW10-0-140717 CGMN-PW10-DB-140717 Average %RPD Sample/Sample Dup 4.32 4.32 4.32 0.0 4179 5.01 4.90 4.5 1.17 1.15 1.16 1.7 01479 0.489 0.484 2.1 0.152 0.158 0.155 3.9 01522 0.558 0.540 6.7 0.0810 0.0806 0.0808 0.50 01101 0.106 O. 104 4.8 1.79 1.78 1.79 0.56 0.498 0.507 0.503 1.8 cTE EE ZEepree eRrTEE TRE NA=NotApplicable E Sample set was analyzed by internal standard calibration, except where noted. The analytical method uncertainties associated with the reported results by internal standard calibration are as follows: PFBA + 17%, PFOA + 15%, PFBS + 18%, PFHS + 17%, and PFOS + E SmTn 20%. a T (2) Sample set was analyzed by exdemal standard calibration. The analytical method uncertainties associated with the reported results by extemal standard calibration are as follows: PFBA + 18%, PI-OA _+ 13%, PFBS -+ 15%, PFHS + 13%, and PFOS -+ 11%. (3) The samplefsample duplicate RPD did not meet acceptance criteria of -<20%. B re m 22 MMeetthhooddss --AAnnaallyyttiiccaall aanndd PPrreeppaarraattoorryy 2.1 Methods Analysis was completed following 3M Environmental Laboratory method ETS-8-044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis". Table 2. Target Analytes `EL SampleEswerecoR leoncJutly1e5-d17n,2014 ineNageneTM (high-density poyetbohttyesplrepearnedaett)he Target.~3alytes [Pumoutum|merogac|soouecewirn| [Petco soacarsy Perfluorobutanoic Acid (C4 Acid) Perfluorooctanoic Add (C8 Acid) |Potomtuanesstonsio 4Sunste) | pres| umew | Perf]uorobutanesulfonate (C4 Sulfonate ) [Putoshomesstoran Cosme) |pevs | uw | Penluorohexanesulfonate (C6 Sulfonate) [PutonomensotoCosutoratey | pros| mewr+Boches | Perfluorooctanesulfonate (C8 Sulfonate) Acrony~ | pro | PFBA PFOA PFBS PFHS PFOS Reference Material Structure tmewrBmched | Linear Linear + Branched Linear Linear Linear + Branched 22.22 SSaammpplleeCColollleeccttiioonn Samples were collected on July 15-17, 2014 in NalgeneTM (high-density polyethylene) bottles prepared at the 3M Environmental Laboratory. Prior to sample collection, bottles designated for field matrix spikes were spiked in the laboratory with a known volume of an appropriate matrix spiking solution containing the analytes of interest. Collected sample bottles were returned to the laboratory on ice on July 18, 2014. 33663300..00119944 iPAGE 4 OF 37 3M MN01596143 fc 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-16 23 Sample Proparation 2.3 Sample Preparation Simpl oncanatons wae expected 0 ang fom <0.023 rn 101008 gL Samping catshat were Sample concentrations were expected to range from <0.025 ng/mL to >1000 ng/mL. Sampling locations that were expected o nave concanvatan 100 hy. wero analyzed mal siardardcsbrtn anaes. Samping expected to have concentration <100 ngfmL were analyzed by internal standard calibration analysis. Sampling Eaton Tat wero poco 0 havo ancora 100mGweryoee by rie svar cooation locations that were expected to have concentration >100 ng/mL were analyzed by external standard calibration ana, Th folowing samp separation procedures were hous 1Sac by of nas. analysis. The following sample preparation procedures were followed for each type of analysis. Le ------------------ Internal standard calibration analysis: Samples analyzed by internal standard calibration were prepared by mang 804 luo 0nwel mcd 3m 0 tn wi 4 of ms (ton ator2) removing a 0.4 mL aliquot of the well mixed sample and diluting it with 0.4 mL of methanol (dilution factor of 2). During th preparation of th borstarycon same, an sauofl separate tera sander sing scksion During the preparation of the laboratory control samples, an aliquot of a separate internal standard spiking solution a 300 0 ha abrBI0 Coro SA 65 (hoinlcononTtn | LY Tho Sami bolle wre sed was added to the laboratory control samples (nominal concentration of 1 ng/mL). The sample bottles were spiked Vihar Moral Standard os a a nominal concanaionf 1 ML rr 5 bain sotlon 0 or Salo with an internal standard mix at a nominal concentration of 1 ng/mL prior to being sent to the field for sample Calocton: Th aboatory core samples wer hon tod wih thal og am mnr as hesais. collection. The laboratory control samples were then diluted with methanol in the same manner as the samples. Exams standardcataton analysis:Samples anazad by extemal aad craton roqured don pro External standard calibration analysis: Samples analyzed by external standard calibration required dilution prior to anys. Sawmero oprassad o ing 01 ofa waked sample wih 06 mLof tna (dition aco analysis. Samples were prepared by diluting 0.1 mL of a well-mixed sample with 9.8 mL of methanol (dilution factor SHI00) An aut ofsagt 9H SOLNG" wasaddedtoh Gkted armas at a mina concaatona 1 of 100). An aliquot of surrogate spiking solution was added to the diluted samples at a nominal concentration of 1 on ng/mL. 22..44 AAnnaallyyssiiss FE -- All samples and quality control samples were analyzed for five target analytes using high performance liquid Cromatogapyandon mass spacvaety HPLOMSMO). Paint itamon parameter, bo ud chromatography/tandem mass spectrometry (HPLC/MS/MS). Pertinent instrument parameters, the liquid ramatogayygaden ogame pach Ss arstans anayaed ae desired nh abs blo. chromatography gradient program, and the specific mass transitions analyzed are described in the tables below. Dustothenar th sample, he idsrang of conoantatns found n th sample, a he eirmetal Due to the nature (~f the sample, the wide range of concentrations found in the sample, and the environmental accofrgeesnomercs ofehe abrs anaes of ret, h sore us or proses he occurrence of multiple isomers of the laboratory's analytes of interest, the software used for processing the cl oul notai Gan lay Sth arate. mantelof rap pk analytical results is not able to consistently integrate the analytical peak, manual integration of the analytical peak is ocak Al mania motatons ae arora lowing ho pecoGies utined i mead ETS 13.010. The necessary. All manual integrations are performed following the procedures outlined in method ETS-12-010. The Conny of Batya ing arr MOU asf bron, parse, hepet eve consistency of the laboratory's integration is ensured through the training of laboratory personnel, the peer review rocess eae ra anal Aton hwof al AGSAGTSby1a GIA. aNn S Peco process required for all manual integrations, the review of manual integrations by the QAU, and where necessary arrowof mans tatatons by abr management the review of manual integrations by laboratory management. Table 3. Instrument Parameters. Table 3. Instrument Parameters. [h| omenm a e Instrument Name ETS Kirk Liquid Chromatograph Lorapuanaros| crseous | Analysis Method [orsmaone | mum | Analysis Date [ues |amcuscoomms x| Guard column [ora cnmn--| oamcisusomxconmsu | Analytical column [otontotne |u| Injection Volume Agilent 1260 ETS-8-044.1 7122114, 7/23/14, 7/28/14 Betasil C13 (4.6 mm X 100 mm), 5 ~ Betasil C13 (4.6 mm X 100 mm), 5 ~.L 5 ~L [o| otmren tuto | Mass Spectrometer AB Sciex TripleQuad 5500 Ion Source [pT owoy T vege | Polarity CT sotwae auren| Sottware Turbo Spray Negative Analyst 1.6.1 33663300..00119955 srcesoesr PAGE 5 OF 37 _Motseses 3M MN01596144 nan no 5011 are 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-16 Table 4. Liquid Chromatography Gradient Program. Table 4. Liquid Chromatography Gradient Program. 7 -- ETS-8-044.1 Analysis Step Total Time Flow Rate Percent A Percent B Number CoTaw TmTwo Two -- 0 CowTmTwoTwo| 1 CwTmTmTwo| 2 CemTwTmoTwo| 3 ome TmTmoTwo| 4 CeTmo TwTmo wo | 5 omeTmTooTwo| 6 me me oo wo | 7 Co ee[me Two | woo | 8 CoTwTmTwoTw| 9 (min) 0.00 0.50 4.00 6.00 11.0 130 13.5 16.0 16.5 19.0 (#L/min) 750 75O 75O 75O 750 75O 750 750 750 75O (2 mM ammonium acetate) 90.0 90.0 70.0 70.0 20.0 2O 0 10.0 10.0 90.0 90.0 (Methanol) 10.0 10.0 30.0 30.0 80.0 80O 90.0 90.0 10.0 10.0 Tables. Mass Transitions. Table 5. Mass Transitions [ron[om [eo| n ogi s| Analyte om ew | Tome | wm] PFBA [ee -- am-- ] reperon PFOA Mass Transition Q11Q3 213/169 4131369 413/219 Internal Standard I13C4] PFBA [13Cs]-PFOA Mass Transition Q11Q3 2171172 421/376 [ame| PFBS [[ormeP Po m2 2e 2 2 m e ] ocgormese PFHS 413/169 299/80 299/99 399/99 399/80 499/99 303/84 402/80 |= PFOS ==499/80 499/130 rere 507/80 [13C3]-PFBA 2161172 [13C4]-P FBA 2171172 [lowron| amen | Towson| snom | [13C4]-PFOA 417/372 I~SC~]-PFOA 421/376 [Toirros T wow |Jogoros 1 somo | [13C4]-PFOS 503/80 I13C~]-PFOS 507/80 Du20nraesr Totbron A 3 Dwell time was 20 msec for each transition. The individual transitions were summed to produce a "total ra TC)wg snoa carn ion chromatogram" (TIC), which was used for quantitation. cn sino od sinao hon tn sre srt (1) Internal standard was not used for the samples analyzed by solvent dilution external standard calibration 33663300..00119966 Prcescesr PAGE 6 OF 37 _MNO1S56145 3M MN01596145 nan no 5011 are 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-16 33 DDaattaa AAnnaallyyssiiss 31 Calibration 3.1 Calibration Solvent dt ana' using lem! standard cabal: Sageswere anayzedoralanaes agaist Solvent dilution analysis using internal standard calibration: Samples were analyzed for all analytes against a mar vache itl 500pt toma nord calbraton Ge. CATIONSandsWarspreparedby pHing matrix-matched stable isotope internal standard calibration curve. Calibration standards were prepared by spiking Kumamour of sackslaons no SDLof 5950methancaborsoy reagentvate.Thecaloraton known amounts of stock solutions into 50 m L of 50:50 methanol:laboratory reagent water. The calibration Sars contains an tema standard mix a ral concenta03toginlf. Calbaton sanaards standards contained an internal standard mix at a nominal concentration of 0.5 ng/mL. Calibration standards Tangng om 00125 nin.Io 100 gm (nominalwareanahed (0.0125 ng 1 10 gm.(nominal for he ranging from 0.0125 ng/mL to 100 ng/mL (nominal) were analyzed (0.0125 ng/mL to 10 ng/mL (nominal) for the SRE) arate, 1 weight, carsonciv of hrl th standard poak area cous overre smal SRSs). A quadratic, 1/x weighted, calibration curve of the ratio of the standard peak area counts over the internal andarpack 103 counwa us 1 dota or 0ach ana. Thodatanr not cedIY 2610 ur standard peak area counts was used to fit the data for each analyte. The data were not forced through zero during nefing rocess. Galanth standard concenbakans ith pel ar akc and ho estan elraton the fitting process. Calculating the standard concentrations using the peak area ratios and the resultant calibration creconf accuracy of coch curvepont curve confirmed accuracy of each curve point. Solvent dition analy' usingextemal sandard caoraton: Sayles wer analyzedagainstan xtral stacard Solvent dilution analysis using external standard calibration: Samples were analyzed against an external standard calraon curve. Calbraton slanwderaerepdersby Spica ron amouof 1n%tlosckSoon 0 80 calibration curve. Calibration standards were prepared by spiking known amounts of the stock solution into 50 mL 190-10 mano: laborer MILGTM vate Carat sandadsrangin fom 002 rom10 25nont. of 90:10 methanol: laboratory Milli-QTM water. Calibration standards ranging from 0.02 ng/mL to 25 ng/mL {romveirsannaalzelc. Aquat, 1Wega, GaRDRICN Ge fh Sana peck rea cs aS used (nominal) were analyzed. A quadratic, 1/x weighted, calibration curve of the standard peak area counts was used {do atafon achae nata. Low ohigh polswera saied 1 el meio cra, Th daawrenot reed to fit the data for each analyte. Low or high points were disabled to meet method criteria. The data were not forced rough zour ring he(ingproces. Cacs2ig ne Sanda Concanratons 3 ha peak roa cous ani ha through zero during the fitting process. Calculating the standard concentrations using the peak area counts and the estan cabvatoncurve coredaccuracyof ch cure pont resultant calibration curve confirmed accuracy of each curve point. Forbobmethodsof nays, each curvepotwas quantated stihe ovgsralcaltraton cuanrdrvviwesd for For both methods of analysis, each curve point was quantitated using the overall calibration curve and reviewed for Sctracy, Method caisaton scaracyoqutements of 100425% (1004300 aie weet ut sont wer ml accuracy. Method calibration accuracy requirements of 100_+25% (100_+30% for the lowest curve point) were met {ora anaes, Thacomiatcn cooficen es aro than0.995 for all arcs. for all analytes. The correlation coefficient (r) was greater than 0.995 for all analytes. 33..22 SSyysstteemm SSuuiittaabbiilliittyy AXcalbratonstandard was analyzed our mes at he begin ofthe analytesequence to demcrsirts overall A calibration standard was analyzed four times at the beginning of the analytical sequence to demonstrate overall Sysam sutabify. Ta aocepane ciarafor sar Suraoty sampolfes ano alto 5%reais system suitability. The acceptance criteria for system suitability samples of less than or equal to 5% relative Standard deiabon(RSD) orpk recount ofpkare aoand leno Lerrof 0 hnor equal standard deviation (RSD) for peak are counts or peak area ratio and retention time criteria of less than or equal to 2S weremetloralantes. 2% RSD were met for all analytes. 33 Limit of Quantitation (LOG) 3.3 Limit ofQuantitation (LOQ) TheLOG as defined n meth ETS-5.04.1 i the lowestnov7e10caltatohnescuarvne dha amreedss The LOQ as defined in method ETS-8-044.1 is the lowest non-zero calibration standard in the curve that meets ineaty vt 20a unsA fo WhCh 1h 5 court's2,1 221Wn 06 fe PION linearity and accuracy requirements and for which the area counts are at least twice those of the appropriate Banks. The LOGS assowcihahatsaempdle analyar std n 1 Takbloew. blanks. The LOQs associated with the sample analysis are listed in the Table 6 below. Tables. 10a Table 6. LOQ Analyte args | are LOQ, ng/mL ~1) Td | TESTI 7122/14 Analysis LOQ, ng/mL 7/23/14, 7/2811 Analysis [ees 1 oowo| sw | PFBA Fr-- --r-------- PFOA [res Tomao 0 | PFBS [ere ommo T2001] PFHS loos 1 oom | as | PFOS 0.0500 0.0240 0.0250 0.0250 0 0232 5.00 1.92 2.00 2.00 1 85 PT -- (1) A dilution factor of 2 was applied to the LOQ. pipette (2) A dilution factor of 100 was applied to the LOQ. 33663300..00119977 orceroesr PAGE 7 OF 37 _MNO1S56145 3M MN01596146 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-16 3.4 Continuing Calibration LERE eee During the course of the analytical sequence, several continuing calibration verification samples (CCVs) were analyzed to confirm that the instrument response and the initial calibration curve were still in control. All reported results were bracketed by CCVs that met method acceptance criteria of 100%+25%. BE E CE nSrT eeRos 3.5 Blanks Three types of blanks were prepared and analyzed with the samples: method/solvent blanks, field/trip blanks, and sampling equipment blanks. Each blank result was reviewed and used to evaluate method performance. The method/solvent blanks were used to determine the LOQ for each analyte. 8 OSS rn 33..66 LLaabb CCoonnttrrooll SSppiikkeess ((LLCCSSss)) Low, mid, and high lab control spikes were prepared for the target analytes and analyzed in triplicate. LCSs S S S mT eeE prepared for internal standard calibration analysis were prepared by spiking known amounts of the analytes into 10 mL of laboratory reagent water to produce the desired concentration. The LCSs were then diluted in the same Ee manner as the samples. LCSs prepared for external standard calibration analysis were prepared by spiking known SE HER e amounts of the analytes into 1.0 mL of laboratory reagent water and 9.0 mL of methanol to produce the desired concentration. Method ETS-8-044.1 states that the average recovery of LCSs at each spiking level must be within 80%-120% with a RSD <20%. All LCS samples met criteria. ps All LCS samples were used in the determination of the analytical method uncertainty in section 3.7 of the report. em The following calculations were used to generate data in Table 7. -- L CS Percent Recovery= C~ IsC~;Ika~ecdoCnc~t~ttrioa~n * 100% [LCS% RSD - standard deviaLtOinS LreCcSovreprylicates * 100%laverage Table 7. Laboratory Control Spike Results. EE=l S |ao e=s=z | ETS-8-044.1 Internal standard calibration Analyzed 7/22/14 Spiked PFBA Calculated Spiked PFOA (Linear + Branched) Calculated Lab ID LCS-140722-1 LCS-140722-2 be SlEllelEZ [a] LCS-140722--3 [avemposwmso| somesarsx 1 eeawsaen | Average + %RSD Concentration (ng/mL) 0.198 0.198 0.198 Concentration (ng/mL) 0.158 0.160 0.159 80.2% + 0.75% %Recovery 79.6 80.8 80.2 Concentration (ng/mL) 0.190 0.190 0.190 Concentration (ng/rnL) 0.198 0.180 0.188 99.2% 4. 4,6% %Recovenj 104 94.8 98.9 LCS-140722-4 19.8 19.1 96.7 19.0 17.6 92.9 LCS-140722-5 [meogersmso| LCS-140722-6 Avera~le _+ %RSD 19.8 --19.8 19.4 osowssow 20.6 99.6% + 3.9% 98.0 19.0 18.4 98.7 | esmesaw | 104 19.0 18.2 95.6 95.1% 4- 2.1% LCS-140722-7 160 LCS-1407224 160 [aemgesswso| LCS-140722-9 160 Average + %RSD 163 162 ssmwesow 154 99.8% + 3.0% I O2 153 149 97.2 101 153 144 94.4 | eseweren | 96.4 153 145 95.4% -+ 1.6% 94.6 erPAGE 8 OF 37 33663300..00119988 3M MN01596147 TTaabbllee 77 ccoonnttiinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuultltss.. Erseont ETS-8-044.1 ar Internal standard calibration Analyzed 7/22/14 PFB~ Lab ID igSpiked Concentration (nglmL) Calculated Concentration (nglmL) < %Recovery ing) Spiked Concentration (ng/mL) REPORTING 15011015218 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-16 PFHS ogni) Calculated Concentration (ng/mL) %Recovery LCS-140722-1 0.198 0.178 89.7 0.198 0.193 97.6 LCS-140722-2 L= ess[oE ie m ou ela ois ] ow 5@] LC8-140722-3 [Avemgoswmso| woxsasx | Soar Average 4- %RSD cs ora wo LCS-140722-4 esas a LCS- 140722-5 wes ure 20 LCS-140722~6 [mvemgoswmso| -- seowesww | eererern | Average _+ %RSD 0.198 0.196 19.8 19.8 19.8 0.171 0.180 89.0% -+ 2.6% 17.1 17.5 18.2 89.0% -+ 3.1% 86.4 90.9 86.6 88.4 92.0 0.198 0.198 19.8 19.8 19.8 0.199 0.197 99.0% -+ 1.3% 18.6 19.5 20.2 98.2% -+ 4.1% 100 99.4 94.0 98.5 102 LCS-140722-7 160 138 86.0 160 142 88.9 LCS- 140722-8 Erm Ea[m]=] 8[x] LCS-140722-9 [aeagosswso| wenasw | emseew | Average 4- %RSD 160 129 160 129 82.4% 4- 3.8% 80.4 80.8 160 141 160 140 88.2% 4. 0.69% 88.1 87.7 ETS-8-044.1 Internal standard En calibration " Analyzed 7/22/14 Lab ID o PFOS (Linear + Branched) Coote Spiked Concanmion Concentration Calculated Concentration (nglmL) (nglmL) %Recovery LCS-140722-1 LCS-140722-2 cars LCS-140722-3 [veogeswmso| Average + %RSD 0.184 0.184 0.184 0.180 0.171 esowezew 0.179 95.9% + 2.8% 97.8 92.8 97.2 | LCS-140722-4 18.4 mm LCS-140722-5 LCS-1407224~ ln18.4 18.4 Average _ %RSD 17.2 93.3 mw) 18.0 17.9 97.6 97.2 96.0% 4. 2.5% LCS-140722-7 148 142 96.2 Les ar[ s 21s] LCS-1407224} 148 LCS-140722-9 148 137 92.3 136 91.6 Average 4- %RSD 93.4% 4. 2.7% 33663300..00119999 Prceacear PAGE 9 OF 37 3M_MNO15%6148 3M MN01596148 TTaabbllee 77ccoonntitinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuultltss.. Erseont ETS-8-044.1 ar Internal standard calibration Analyzed 7/22/14 coSnocaanemdion|| CoCncoantimeion Spiked Concentration 13C3-PFBA Calculated Concentration Lab ID cs. aorzz: LCS-140722-1 wsuorma | LCS-140722-2 suns | LC8-140722-3 (ng/mL) or0.197 ow0.197 ow0.197 (ng/mL) ors0.195 ot0.188 ous0.185 %Recovery ao98.9 295.2 su94.1 ConScaenvreaian Spiked Concentration (ng/mL) ore0.198 ore0.198 ois0.198 Average :1: %RSD 96.1% _+ 2.6% LCS-140722-4 1.97 2.03 103 1.98 wes uorze 20 a LCS-140722-5 LCS-140722-6 1.97 1.97 1.91 2.04 96.9 103 1.98 1.98 Average _+ %RSD 101% + 3.5% REPORTING 15011015218 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-16 13C4-PFOA Calculated Concentration (ng/mL) I0.212 om0.193 ozs0.208 103% _+ 4.8% 2.13 2.01 2.20 107% + 4.2% %Recovery or107 oe97.6 0s105 107 102 11" ETS-8-044.1 Internal standard calibration Analyzed 7/22/14 Lab ID Spiked Concentration (ng/mL) 13C4.PFOS Calculated Concentration (ng/mL) %Recovery LCS-140722-1 01189 01182 96.6 LCS-140722-2 cera LCS-140722G [mw|oges samrw aenrso| Avera~le _+ %RSD 0.189 0.189 0. f185 0.195 99.1% -+ 3.4% 97.8 103 LCS- 140722-4 1.89 1.89 1 O0 = wes uz wo ot a LCS-140722-5 LCS- 1407224} 1.89 1.89 1.80 1.94 95.1 103 Average + %RSD 99.4% -+ 4.0% 33663300..00220000 encer00F PAGE 10 OF37 3M_MNO15%6149 3M MN01596149 TTaabbllee 77ccoonntitinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuultltss.. Erseont ETS-8-044.1 in External standard calibration Analyzed 7/23/14 PFBA Lab ID igSpiked Concentration (nglmL) Calculated Concentration (nglmL) < %Recovery REPORTING 15011015218 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-16 PFOA (Linear Branched) ing) Spiked Concentration (ng/mL) ogni) Calculated Concentration (ng/mL) %Recovery LCS-140723-1 0.199 0.196 98.7 0.191 0.204 107 LCS-140723-2 0.199 0.201 101 0.191 0.201 105 = esos(m oi eormlse r a]l = pe) z] 0 LCS-140723-3 0.199 0.179 89.7 0.191 0.197 103 [vooswmsol-- -- oemeseax | esse | Average 4- %RSD 96.~/o -+ 6.2% 105% -+ 1.9% Les ars 2 LCS-140723-4 1.99 222 112 Less 2m LCS-140723-5 1.99 218 110 wes ume 216 LCS-140723~6 1.99 220 111 |Avgeswmsol -- vwmesosow | vweaen | Average _+ %RSD 111%_+0.90% 1.91 2.17 114 1.91 2.09 109 1.91 2.18 114 112%_+2.6% LCS-140723-7 20.0 22.0 LCS- 140723-8 20.0 21.9 [aemgosswso| weweosw LCS-140723-9 Average 4- %RSD 20.0 22.2 110%_+0.52% 110 19.1 21.9 115 110 19.1 22.0 115 | wees | 111 19.1 21.6 113 114% -+ 1.0% ETS-8-044.1 Exenasoies External standard Cann calibration " Analyzed 7/23/14 Lab ID ogSpiked Concentration (ng/mL) PFBS Calculated Concentration (nglmL) %Recevery rpm) Spiked Concentration (ng/mL) PFHS ogni) Calculated Concentration (ng/mL) %Recovery LCS-140723-1 0.199 0.225 113 0.199 0.220 110 LCS-140723-2 0.199 0.221 111 = wes o=na[oiElen mw a os]s oz r] 1 LCS-1407234 0.199 0.226 113 [avwge:vmsol-- --vpwesow | as Average + %RSD 112% _+ 1.0% rer) I) Ea LCS-140723-4 1.99 232 117 sans = m LCS-140723-5 1.99 221 111 Les ze io ws LCS-1407234~ 1.99 228 115 [average:uso] naar wea Average + %RSD 114% _+ 2.7% reer =o ER a LCS-140723-7 Lesa @0 mo 20 LCS-140723-8 20.0 20.0 22.6 113 22.4 112 0.199 0.199 0.229 115 0.227 114 113%_+2.3% 1.99 1.99 1.99 2.28 115 2.19 11o 2.29 115 113% -+ 2.5% 20.0 20.0 22.4 112 21.8 109 [Avengossmso| wamsosm | onion LCS-140723-9 20.0 22.4 112 Average + %RSD 112%_+0.51% 20.0 21.7 109 110% _+ 1.6% 33663300..00220011 ence nors PAGE 11 OF 37 3M_MNO1596150 3M MN01596150 TTaabbllee 77 ccoonnttiinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuultltss.. Erseont ETS-8-044.1 in External standard calibration Analyzed 7/23/14 Lab ID Les aoa LCS-140723-1 wes omz LCS-140723-2 wes aos LC8-140723-3 PFOS (Linear Branched) Spiked Concentration (ng/mL) ons0.185 ons0.185 os0.185 Calculated Concentration (nglmL) ore0.199 ox0.202 om0.197 %Recovery or107 wo109 or107 Average 4- %RSD 108% _+ 1.1% LCS-140723-4 1.85 2 09 113 ELesm anemele 21 l) LCS-140723.-5 LCS-140723-6 1.85 1.85 2 05 111 2 12 114 Avera~le _+ %RSD 113% _+ 1.4% Test a LCS-140723-7 18.5 21.3 115 wes ara = LCS-140723.-8 18.5 20.8 112 wes orze 21 LCS-140723-9 18.5 20.7 112 [vo|mgoe swas ns mso| Average + %RSD 113% _+ 1.5% REPORTING 15011015218 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-16 ET8-8-044.1 == ---] -- Internal standard calibration Analyzed 7/23/14 oe 2 la "eprom] 13C3.PFBA 13C4-PFOA Lab ID Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery LCS-140723-1 0.198 0.216 Ex lela LCS-140723-2 LCS-140723-3 0.198 0.198 0.214 0.195 Average + %RSD 105% _+ 5.5% 109 0.199 0.215 108 =lels) 108 0.199 0.212 107 98.6 0.199 0.209 105 107% _+ 1.4% LCS-140723-4 1.98 2.22 112 1.99 2.23 112 LCS-140723~5 1.98 2.21 111 EAHA LCS-140723-6 1.98 2.21 112 [esgoromso| vmmsosms | wees | Average _+ %RSD 112% _+ 0.52% 1.99 2.17 109 1.99 2.20 110 110% _+ 1.4% 33663300..00220022 ence r20r PAGE 12 OF37 IM_MND1596151 3M MN01596151 TTaabbllee 77ccoonntitinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuultltss.. Erseont ETS-8-044.1 ar Internal standard calibration Analyzed 7/23/14 ConScoabnanon|| CoCncoancimoion Spiked Concentration 13C4-PFO8 Calculated Concentration Lab ID Les aoa oto ome LCS-140723-1 wsuoma | om om LCS-140723-2 sams | om ozs LCS-140723-3 [aw|goe "roms eerem e so| Average 4- %RSD (ng/mL) 0.190 0.190 0.190 (ng/mL) 0.208 0.202 0.205 108% _+ 1.4% %Recovery 110 107 108 LCS-140723-4 LE es am me LCS-140723.-5 LCS-140723~6 1.90 2.11 111 Ele 20 ] 0 1.90 2.10 110 1.90 2.08 110 Average 4- %RSD 110% _+ 0.52% REPORTING 15011015218 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-16 ETS-8-044.1 External standard El calibration Analyzed 7/28/14 Lab ID ogSpiked Concentration (nglmL) PFBA Calculated Concentration (ng/mL) | < %Recovery en | PFOA (Linear + Branched) Colona Spiked cancanraton Concentration npn) ogni) (ng/mL) Calculated Concentration (ng/mL) %Recovery LCS-140728-1 0.199 0.204 LCS-140728-2 La es urs oi oan LCS-140728~ [awogeevmsol-- -- wimessow Average + %RSD 0.199 0.199 0.176 0.201 97.~'/o + 8.0% 103 0.191 0.197 103 88.6 0.191 0.196 103 o pe ozs. wo 101 0.191 0.205 107 | eeeam | 104% -+ 2.2% LCS-140728-4 1.99 223 112 1.91 2.01 105 wes EERE LCS-140728-5 1.99 223 112 1.91 LCS-140728-6 1.99 220 111 1.91 2.05 107 2.04 107 Average 4- %RSD 112%--.0.52% pres wo Tw LCS-140728-7 wes uoras 0 0s LCS-140728~ 2010 2010 21.5 108 21.1 105 106% --. 1.1% Ex as ) 19.1 20.9 109 1 20 0s 19.1 20.0 105 [avemgossmso| LCS-140728-9 Average 4- %RSD 2010 women 21.8 107% -+ 1.9% | esweaee | 109 19.1 21.0 110 108% -+ 2,4% 33663300..00220033 ence nors PAGE 13 0F37 3M_MNO15%6152 3M MN01596152 TTaabbllee 77ccoonntitinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuultltss.. Erseont ETS-8-044.1 in External standard calibration Analyzed 7/28/14 PFB8 Lab ID igSpiked Concentration (nglmL) Calculated Concentration (nglmL) < %Recovery ing) Spiked Concentration (ng/mL) REPORTING 15011015218 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-16 PFHS ogni) Calculated Concentration (ng/mL) %Recovery LCS-140728-1 0.199 0.212 107 LCS-140728-2 0.199 0.223 112 = Les ons(oi EozE 6 LCS-140728-3 0.199 0.219 110 [vomoswmsol-- -- wowsam Average 4- %RSD 110% -+ 2.3% Los aorana LCS-140728-4 1.99 217 109 Less LCS- 140728-5 1.99 221 111 Los urns LCS-140728-6 1.99 215 108 |Avgeswmsol -- oweerew Average _+ %RSD 109% -+ 1.4% 0.199 0.208 105 0.199 0.222 111 a pee ]E ozs r] 0.199 0.219 110 TT ewsas 109% -+ 3.0% ) 1.99 PY 1.99 8 1.99 2.16 109 2.17 109 2.14 108 | ewwsosw | 109% -+ 0.53% LCS-140728-7 20.0 21.6 LCS- 140728.-8 EEE LCS-140728-9 [aemgosswso| oewease Average 4- %RSD 20.0 20.0 20.7 21.4 106% -+ 2.5% 108 20.0 21.9 110 103 20.0 21.2 106 EERE 107 20.0 21.6 108 | ese | 108% - 1.9% ETS-8-044.1 External standard calibration Ema r ras]CondSeonhseadtiPoEn||S Cnn oCnuecoa+dmBesaraaens nceh | Analyzed 7/28/14 PFOS (Linear + Branched) Spiked Concentration Calculated Concentration Lab ID (ng/mL) (nglmL) %Recovery LCS-140728-1 0.185 0.191 103 = esos oes osm 05 LCS-140728-2 0.185 O. 195 105 LCS-140728-3 0.185 0.197 106 Average 4- %RSD 105% _+ 1.5% Tos ara I To LC8-140728-4 Les ams 200 LCS-140728-5 1185 1.85 1 98 107 2 O0 108 LCS-140728-6 1.85 2 O0 108 |mvogosowsm o sol| Average 4- %RSD 108% _+ 0.54% re LCS-140728-7 18.5 19.9 108 Les omna LCS-140728-8 18.5 19.6 106 [ave | mgeoos meas sn mso| LCS-140728-9 18.5 20.7 112 Average + %RSD 109% _+ 2.8% 33663300..00220044 ence or PAGE 14 OF 37 3M_MNO15%6153 3M MN01596153 TTaabbllee 77ccoonntitinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuultltss.. Erseont ETS-8-044.1 ar Internal standard calibration Analyzed 7/28/14 coSnocaanemdion|| CoCncoantimeion Spiked Concentration 13C3-PFBA Calculated Concentration ConScaenvreaian Spiked Concentration Lab ID Les.LCS-140728-1 wsuoma | LCS-140728-2 soma | LC8-140728-3 [awogoesmso| Average 4- %RSD (ng/mL) ore0.198 om0.198 om0.198 (ng/mL) ome0.208 0160.196 ois0.190 "osoweame gg.g% 4. 4.7% %Recovery ws 010 105 a0 oro 98.9 sn TToi 95.8 (ng/mL) 0.199 0.199 0.199 LCS-140728-4 1.98 2.02 102 1.99 wes 2u a ww LCS-140728.-5 1.98 2.11 1 (37 1.99 LCS- 140728-6 1.98 2.14 108 1.99 Average _+ %RSD 106% + 3.0% REPORTING 15011015218 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-16 13C4-PFOA Calculated Concentration (ng/mL) ozn0.208 oan0.211 oz0.201 eesese 104% 4. 2.4% 1.99 2.14 2.11 104% + 3.7% %Recovery 104 106 10" | 99.8 107 106 ETS-8-044.1 Internal standard calibration Analyzed 7/28/14 Lab ID Spiked Concentration (ng/mL) 13C4.PFOS Calculated Concentration (ng/mL) %Recovery LCS-140728-1 0.190 0.203 107 LCS-140728-2 O. 190 O. 195 103 reid ==]: LCS-140728G O. 190 O. 194 102 [me|ogeroms esamw e so| Avera~le _+ %RSD 104% + 2.5% LCS-140728-..4 1.90 1.88 99.1 Ir=[ze]%] LCS- 140728-5 1.90 2.05 108 LCS- 140728-6 1.90 2.02 106 Average + %RSD 104% 4. 4.5% 33663300..00220055 encersor PAGE 15 OF37 3M_MNO15%6154 3M MN01596154 a 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-16 37 Analytical Method Uncertainty 3.7 Analytical Method Uncertainty Rot ants bas nite! OCdt t's con cated dud to veto mera scrcy Analytical uncertainty is based on historical QC data that is control charted and used to evaluate method accuracy and reisan: Tha etna nce scalcaated Iowa 16.12.0122. Th sara dvaton s aousad and precision. The method uncertainty is calculated following ETS-12-012.2. The standard deviation is calculated forthe sof scarry esl (50)Oban or GC sr Fo MetRadETS 6.0441 no meshrcsnfy for the set of accuracy results (in %) obtained for the QC samples. For method ETS-8-044.1, the most recent fifty GC samples ve Ta rpandob rer is closed 1 kph Sanda ovation oy a arf QC samples were used. The expanded uncertainty is calculated by multiplying the standard deviation by a factor of Smee 5a rnin ovof 3. 2, which corresponds to a confidence level of 95%. Tabl.e Anaytcl Method Uncertainty. Table 8. Analytical Method Uncertainty. [ome | coi |svt Tweet) er | Analyte Com oe Tee Tom PFBA Coron | oes[70 uo PFOA Comes | owe [en we | PFBS os|oma | ew wm | PFHS IEr -------- PFOS ro caer ow PFBA ron Caen oo PFOA ores |[ owe r [w ew PFBS II -- -- ---- PFHS oresToT me s oe] PFOS Calibration Intemal Intemal Intemal Intemal Internal Extemal External External Extemal Extemal Standard Deviation (%) 8.56 7.42 9.14 8.69 9.93 8.93 6.59 7.67 6.37 5.33 Method Uncertainty -+17% +15% -+18% _+17% -+20% _+18% _+13% -+15% -+13% -+ 11% 33..88 FFiieelldd MMaattrriixx SSppiikkeess ((FFMMSS)) Ria cry Fol ae see cmp ves colia ach samping pro very at he anata methd A target analyte field matrix spike sample was collected at each sampling point to verify that the analytical method 1opgiaflreclocied ati, Led mat spkes regated oy a0403 a amr vole of 1 is applicable for the collected matrix. Field matrix spikes are generated by adding a measured volume of field Sr containsapa yo aeraeg wh Ae ras DT 65 it corer 5 sample to a container spiked by the laboratory with the target analytes prior to shipping sample containers for cote thSphes mak aS050 is cee ty come sample collection. Field matrix spikes must be at least 50% of the analyte concentration to be considered an omeoret ve vl Fold ma Spe econ wih moh cept ct TAS0% cot nt appropriate spike level. Field matrix spike recoveries within method acceptance criteria of 100_+30% confirm that tnecomponent 15 salemdant Sy hanly mars wih oo proprioand cro "unknown" components in the sample matrix do not significantly interfere with the preparation and analysis of the rataof esto nae os oe rasan of So mat Sn tons conan analytes of interest. The standards used for the preparation of the field matrix spiking solutions contained reference escompra ofso ner and rh amenx PROS a oy ne e3r PEON. Pa materials comprised of both linear and branched isomers for PFOS and only the linear isomer for PFOA. Field spas a reseed soem 40 eon matrix spikes are presented in section 4 of this report. 106d to ret nat fed mati ses, eachsample covind sal sco sroqporecor ks of C1In3CPa3dF-dPBiFtioABnA,,to"13tCCa4Prg-PFeFtOOaAnA,a, layatnneddfi"1e3'lCdC4.m--PaPFFtrOOixSS,s,pwwihkhieiccshh, ewwaeecrrheesaaaddmddeepddleaacltoaantnnaooinmmieindnaaslltaccobonlnecceeinsntotrtroaatptiieoonnsouofrfr0o0.g.11atnnegg/r/memLcL.ovttooerssyeelsleepccitkt es of Sen bas ie Same colecion yt oie cocoetan of1 ng GoM Spa lacion. The sC13a.Cm-3pP-PleFFBbBAoAatatlnensdd p1C3rCi.o4-r-tPoPFFsOaOmAAwpweleerrceeolssleeelcleeticcottneeddor(to0atrreeappnrreeossmeeinnnttappl eecrorffnlluucocerrnoolccraaartribbooonxxyoyilfiicc1 aanccgiiddfsms..L TTfohhlleeow"13inCCg4.-l1saaabbmeelpleeldde PPcoFFlOlOeSSctiwwonaa.ss The sonar proses St. Soa mov sp ovwei od mest selected to represent the perfluorosulfonic acids. Surrogate matrix spike recoveries within method acceptance toraol TO0L30 CoN Ta ToWcOneO Sa tcBo Scat nero 0 criteria of 100+30% confirm that "unknown" components in the sample matrix do not significantly interfere with the Tr ees preparation and analysis of the analytes of interest. The surrogate spike recoveries are included in section 4 of this rreeppoortr.t. [ FMS Recovery (Sample Concentration of" FMS oie Average Spike Comenratin Concentration Concenlration : FieldSample & FieldSample Dup.), 100%] 33663300..00220066 oxo PAGE 16 OF37 Su umorseiss 3M MN01596155 TTaabbllee 99.. FFiieelldd MMaattrriixx SSppiikkee CCoonncecnetnrtaratitioonnss. REPORTING 15011015218 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-0!-93-16 Location [PMwWo07r, PeWm09o, amndoPeWal0o [oMwW1e3 [oMW1w10 e [owe MW16 [Camo mio wos mamwics MW101, MW104, MW105, and MW108 [ome MW12 and MW14R owe Trip Blank Final Concentration (nglmL) Spike Level PFBA PFOA PFBS PFHS PFO8 | eFwMsS |o2o.0o0 | v1s.98e [| r1o.9s8 | w1 o98e| v1o.9n8 | TomFsMS |s5o.0o0 | a4o.94e|440.955 | 440.965 |a4s.9s5 | TewFsMS | 2200.00 | w19e.8s | w19s.8 | v19e.s8 | te19s.8 | 1 oFuMSs [0050.0 | soa 49.4 | aos49.5 | sos49.5 |a4s9.5 | | oFwMSs | w10o0 | w9e8.8e|oo99o.0 | seo99.0 | m099.0 | | oFuMSs [o5n00 |a4m94 | a4o9s5 |as49s5 | a4e9s5 | LemLow damsLaoLo 2.00 1.98 1.98 1.98 1.98 [ThHoigrh To1o00 Toe98.s8 [ow990.0 |o9o9.o0 |w9o9.0| 44 DDaattaa SSuummmmaarryy aanndd DDiissccuussssiioonn TTthhheoetTatrabpblleeBssabnbkee.lloowwEasscuuhmmmtmaaabreriizzpeerotthvh iedsseasamtmhpepalevrreeerssuaulglttssecaaonnnvdceefnieltlrddatmmiaoatnrtriixxansspdpiiktkeherereercecolovaevtrievireoipesesrffcorer nsstaadmmippflleiinrngegnllcooeccaa(ttiKiooRnnPss Daa)ssweowfletlllhaaess tssehaalemmaplTplvrlieeep daaBinnlfaddfnesskraa.emnmcEppelalee(ch5cdRutuapPpibDlcilce)aalvpetae.rlo.uRveReidsseeussalurttlehtsseraaoannuvddnedraaeavvdgeeterroaacgtgoeewnocvvseaalnliuutreegasstinoaarnrfeeairrnooaduuunrnrthddeteeesdd.rettloBoaetttihcvhraereeuepeseessriicggoenfniniofftiiucdcnaaidfnnfitetnrffgiegi.nrucerveesas.l(.u%ePPRsevePrarcDcree)ynnsottif gthhet ffdrreeoolmammtoivntthehsooidssrieefafeeslirseehtenaddctei1hn(e%thhemReerPrtaaDnww)ovGddaaatltuaae.a.spFpFairiereoellpddrrimomauatanertdrfitxoexdhssppteoikkteewgssoemmsneeigeenmttiiannfirgcgxat.tnhhteefimmgeuetrtehhsoo.ddaBacecccceaepuptstaaennoccfee creaof 230%. rounding, values criteria of_+30%, vary slightly demonstrate that the method is appropriate for the given matrix. TTdehhmeeossneesssiaarmmatppnilignnggatllootcchaatteiioomnnessthhhaaovvdeeibbeeaeepnnpiaacnnaaatlllyyezzeeotddh rreeppeseaaattmeepddllyye aamnnaddintth.hee Wllahabiboloreraatttooirreyymhheaatsshhhoiidssttnoordriicccaaalltffeiieselddthmmaatathtriexstspapirikkgeeedtdaattaa dS`aaaenmnmapalyolltneey,sFtFtraMLhotSSintgassraatghmmoaplptlalteehnssaelssmthhoooesutufhloddordbcbeeaiscssaphppikkpseelaiddcamaapbtileaanppgtpoprlrtoohoxxceiiammstaaoatmnteelwplyyoler00o.m.55ea--1x1tr0p0ixett.cimteWeesdshtitleotehhcxetohpeveexepmrcete@ctethweodidddaoainnncaadolliynyctctaeeotenccsioorntnahcctaeeotnnnttthrreaaattnitooagnnregiiennt tthhee sTPThaFhemOerSrepe.flfeoor,rAeeth,d,efaiietadrldrogsmmeat,aaatrtrnixharlssypoptieikakseerfooccrroosnnetccaaeecnnnhtctrrseaaasttiwmoorhrp~eslsiwrnweegterlrheoecoasssteeipollekenccottweeelddorebvbaeaessxoeepxddeccoootnoneddhtahotdeoheecxxeoppveereccerttcaeeoddwmccimdooeenncnccedeonentndrtcraaepttniiootornnartooioffinPPrFFmaoOOngAAea1a.n0ndtdlm/ooerrs tstPhhaFeomOpaaSnlnae.allyyActotseencacceoonrntnecrsceauenttlnitr,otarntat.hiteioornen..arIIenn these instances, instances where these instances, thethe the FISspike FMS recovery was epartedandflagged level exceeded the recommended recovery was reported and flagged as above 10 upper limit of as above 10 times the 10 times times the sample concentration. hFFooerrstthuhorosrseeogaaannlaalrlyyettceeossvwwehrhyeesrrteeantthdheearffideislsdwemmaralertruiixxsessppdi1ikk0ee laeesvvseeelwswasasmsenntoohttopadrpaopcrpcorupirraaiacttyee. a3sAslccoosmmuprpaatrroeegddattorethhceoevssearaymmspteleacncodonancrcednesainrtnraaditoionn,, id matrix spk recoveries met metrod acceptance cron (whoro appicablo) the surrogate recovery standards were used to assess method accuracy. All surrogate field matrix spike recoveries met method acceptance criteria (where applicable). recovery standards and 33663300..00220077 ence rors PAGE 17 OF37 3M_MNO15%6156 3M MN01596156 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. ISO'Z 1-01-03-'f6 Table 10. CGMN GW MW07 140716 EEee 3M LIMS ID ISOll-01-03-16-001 ISO11-01-03-16-002 8m [ CEo tage| } ]m IwLa aee]] Description CGMN-MW07-0-140716 TFET CGMN-MW07-DB-140716 PFBA Concentration (ng/mL) %Recovery 316 NA 293 NA PFOA Concentration (ng/mL) %Recovery 0.606 NA 0.598 NA ISO11-01-03-16-003 CGMN-MW07-FMS-140716 516 106 2.69 106 Average Concentration (nglmL) -+ %RPD 3.05 n~l/mL -+ 7.6% 0.602 n~llmL -+ 1.3% FERE3M LIMS ID ISOl 1-01-03-16-001 ISO11-01-03-16-002 FO [e Ccw )P| NCemP s | C=wes | Description CGMN-MW07-0-140716 TE CGMN-MW07-DB-140716 PFBS Concentration (ng/mL) %Recovery 0.0759 NA 0.0765 NA PFHS Concentration (ng/mL) %Recovery 0.0434 NA 0.0398 NA PFOS Concentration (ng/mL) %Recovery 0.237 NA 0.236 NA ISO11-01-03-16-003 CGMN-MW07-FMS-140716 2.09 102 2.14 106 2.44 111 Average Concentration (ng/mL) -+ %RPD 0.0762 ng/mL 0.79% 0.0416 ng/n~L _+ 8.7% 0.237 ng/raL -+ 0.42% Bmuner3M LIMS ID ISOll 01~33 16 001 ISO11-01-03-16-002 ISO11-01-03-16-003 oEwer e|TstemsT{stonTes|s]ms| Description CGMN MW07 0 140716 CGMN-MW07-DB-140716 13C~-PFBA 130~-PFOA 13C~.PFOS %Recovery 123 123 %Recovery 120 112 %Recovery 110 127 CGMN-MWO7-FMS-140716 105 115 111 Average Recevery (%) %RSD 117%8.0% 116% 3.5% 116%~ 8.1% Sn nra nr y cn. NA - Not Applical~lo Samples were diluted 1:1 and analy~d by internal standard calibration. PAGE 18 OF 37 3M_MN01596157 33663300..00220088 Toa. com rT Table 11. CGMN GW MW12 140717 mae | oe mT [me]| 3M LIMS ID ISO11-01-03-16-004 SEER ISO11-01-03-16-005 ISOll 01433 16 006 Description CGMN-MW12-0-140717 CGMN-MW12-DB-140717 CGMN MW12 FMS 140717 PFBA Concentration (ng/mL) %Recovery 157 NA 150 NA 669 103 PFOA Concentration (ng/mL) %Recovery 395 NA 409 NA 1010 123 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. ISO f 1-01-03-'16 Average Concentration fng/mL) 4- %RPD mmr omer omoeeensTT ea weve| re]"Siet Laee]r] 3M LIMS ID IS011-01-03-16-004 Bhae h tha] ISO11-01-03-16-005 Description CGMN-MW12-0-140717 CGMN-MW12-DB-140717 154 ng/mL 4- 4,6% 402 nglmL 4- 3.5% PFBS Concentration (n~l/mL! %Recovery 49.3 NA 51 4 NA PFHS Concentration (n~tmL) %Recovery 7.87 NA 8 34 NA PFOS Concentration (n~l/mL) %Recovery 94.2 NA 99 5 NA ISO11-01-03-16-006 CGMN-MW12-FMS-140717 583 108 549 109 {~) 700 122 Average Concentration (nglmL) _+ %RPD ae [|octournte[|satro[reoers)| 3M LIMS ID Description 55.4 ng/raL _+ 4.2% 8.11 nglmL _+ 5.8% %Recovery %Recovery %Recovery 96.9 nglmL _+ 5.5% ISO11-01-03-16-004 CGMN-MW12-0-140717 101 99.7 101 ISO11-01-03-16-005 CGMN-MW12-DB-140717 ISO11-01-03-16-006 CGMN-MW12-FMS-140717 se Average Recovery (%) + %RSD NA = Not Applicable Samples were diluted 1:100 and analyzed by ex'temal standard calibration. (1) FMS concentration greater than 10 times the sample concentration. 105 105 103%2.2% 107 103 103% 3.6% 106 103 103% 2.2% PAGE 19 OF 37 awe 3M_MN01596158 33663300..00220099 Toe 12. COMMSrts Table 12. CGMN GW MW13 140716 mae | oe mT [om] e | 3M LIMS ID ISO11-01-03-16-007 Ph EETtal fo ISO11-01-03-16-008 ISOll 0143,3 16 009 Description CGMN-MW13-0-140716 CGMN-MW13-DB-140716 CGMN MW13 FMS 140716 PFBA Concentration (ng/raL) %Recovery 786 NA 829 NA 14.0 119 PFOA Concentration (ng/mL) %Recovery 13.9 NA 14.8 NA 19.1 NO 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. ISO f 1-01-03-'16 Average Concentration fng/mL) 4- %RPD mmr omer omoeceT n ea ve| re e]"SieeLaee]r] 3M LIMS ID ISO11-01-03-16-007 EER SESEITE NEY ISO11-01-03-16-008 Description CGMN-MW13-0-140716 CGMN-MW13-DB-140716 5.08 ng/mL 4- 5.3% 14.4 ng/mL 4- 6.3% PFBS Concentration (ng/mL) %Recovery 0.970 NA 0 975 NA PFHS Concentration (ntmL) %Recovery 0.700 NA 0 726 NA PFOS Concentration (ng/mL) %Recovery 4.37 NA 4 58 NA ISO11-01-03-16-009 CGMN-MW13-FMS-140716 6.06 103 6.26 112 9.62 104 Average Concentration (nglmL) + /~PD a |T ctu w|rtouma es]| ts reee|] 3M LIMS ID Description 0.g73 nglraL _+ 0.51% 0.713 nglmL _+ 3.6% %Recovery %Recovery %Recovcry 4.48 nglmL _+ 4.7% leO11-01-03-16-007 CGMN-MW13-0-140716 117 ISO11-01-03-16-008 CGMN-MW13-DB-140716 116 ISO11-01-03-16-009 CGMN-MW13-FMS-140716 115 Average Recovery (%) + %RSD 116%~0.87% wn NA = Not Applicable SEE NC = Not Calculated; Spike level was less than O.5x the endogenous sample concen~ation. Samples were diluted 1:1 and analyzed by internal standard calibration. 115 117 106 113%5.2% 104 111 105 107%3.5% PAGE 20 OF 37 awe 3M_MN01596159 33663300..00221100 ------ Table 13. CGMN GW MW14R 140716 mae L ooo om m mT e] l| 3M LIMS ID ISO11-01-03-16-0" 0 SEER EY ISO11-01-03-16-0" 1 ISOll 01433 16 0"2 Description CGMN-MW14R-0-140716 CGMN-MW14R-DB-140716 CGMN MW14R FMS 140716 PFBA Concentration (ng/mL) %Recovery 685 NA 657 NA 1190 104 PFOA Concentration (ng/mL) %Recovery 430 NA 421 NA 962 109 3M ENVIRONMENTAL LABORA TOR Y REPORTNO. IS011-01-03-!6 Average Concentration fng/mL) 4- %RPD mee ower | [om|eT ame| e | ea[se]n] 3M LIMS ID IS011-01-03-16-0"0 IS011-01-03-16-0"1 etAa Sel Rein] IS011-01-03-16-0"2 Description CGMN-MW14R-0-1407fl 6 CGMN-MW14R-DB-140716 CGMN-MW14R-FMS-140716 671 ng/raL 4- 4,2% 426 nglmL 4- 2.1% PFBS Concentration (ng/mL! %Recovery 29.8 NA 29 3 NA 549 105 PFHS Concentration (n~tmL) %Recovery 20.7 194 535 NA NA 104 ~) PFOS ConcentratiOn(n1/mL) 156 159 866 %Recovery NA NA 103 Average Concentration (nglmL) _+ %RPD a 3M LIMS ID Description 29.6 nglraL _+ 1.7% 20.1 nglmL _+ 6.5% [a | womm en| ws orm | I=C~-PFBA ~3C4-PFOA ~C4-PFOS | tee| gre Fate %Recovery %Recovery %Recovery 1~8 ng/mL _+ 1.9% fetid ISO11-01-03-16-0" 0 ISO11-01-03-16-0" 1 ISO11-01-03-16-0" 2 EhE c [=]IE CGMN-MW14R-0-140716 CGMN-MWl 4R-DB-140716 CGMN-MW 14R-FMS-140716 109 105 102 103 104 101 se Average Recovery (%) + %RSD NA = Not Applicable 105% -~ 3.5% 103% -+ 1.9% Samples were diluted 1:100 and analyzed by internal standard calibration. (1) FMS concentration greater than 10 times the sample concentration. El 106 103% -~ 2.7% PAGE 21 OF 37 awmerserso 3M_MN01596160 33663300..00221111 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. ISO f 1-01-03-'16 Table 14. CGMN GW MW16 140716 ET i [e i m Sa a Lat 2 wa]cd 3M LIMS ID ISO11-01-03-16-0" 3 SEETD ISO11-01-03-16-0" 4 Description CGMN-MW16-0-140716 CGMN-MW16-DB-140716 PFBA Concentration (ng/mL) %Recovery 46.7 NA 44.7 NA PFOA Concentration (ng/mL) %Recovery 99.1 NA 97.4 NA ISOll 01433 16 015 CGMN MW16 FMS 140716 103 115 161 127 Averase Concentration fng/mL) 4- %RPD 45.7 n~/mL 4- 4.4% 98.3 n~lmL 4-17% a 3M LIMS ID IS011-01-03-16-0" 3 ISO11-01-93-16-0" 4 [ems 0T| C ons | ees | Description CGMN-MW16-0-140716 WEEE CGMN-MW16-DB-140716 PFBS Concentration (n1/mL! %Recovery 37.4 NA 38 3 NA PFHS Concentration (n~tmL) %Recovery 5.39 NA 5 52 NA PFOS Concentration %Recovery 57.8 NA 56 1 NA ISO11-01-03-16-015 CGMN-MW16-FMS-140716 92.8 111 63.2 117 119 125 Average Concentration (nglmL) _+ %RPD 37.9 nglraL _+ 2.4% 5.46 nglmL _+ 2.4% 57.0 nglmL _+ 3.0% wane omer | sn | shee |sn | 3M LIMS ID Description ISOll-01-03-16-0" 3 CGMN-MW16-0-140716 Er EE TI ISO11-01-03-16-0"4 CGMN-MW16-DB-140716 ISO11-01-03-16-015 CGMN-MW16-FMS-140716 == miata Average Recovery (%) + %RSD [corsa|coron|cores | I=C~-PFBA ~3C4-PFOA ~C4-PFOS %Recovery 106 94.8 123 108% -+ 13% %Recovery 110 116 120 115% -+ 4.4% %Recovery 115 98.3 107% -~ 7.9% NA = Not Applicable maaa 7 NC = Not Calculated; Spike level was less than 0.Sx the endogenous sample concen~ation. Samples were diluted 1:1 and analyzed by external standard calibration. PAGE 22 OF 37 3M_MN01596161 33663300..00221122 Toe t5 Com WIG tr Table 15. CGMN GW MWl01 140717 mae L ooo om m mT e] l| 3M LIMS ID ISO11-01-03-16-0" 6 Bh I edhdllls ISO11-01-03-16-0"7 ISOll 01493 16 0"8 Description CGMN-MW101-0-140717 CGMN-MW101-DB-140717 CGMN MW101 FMS 140717 PFBA Concentr=ion (ng/mL) %Recove~ 1460 NA 1450 NA 1610 NO PFOA Concentration (ng/mL) %Recovery 83.5 84.2 177 NA NA 94.3 3M ENVIRONMENTAL LABORA TOR Y REPORTNO. ISOf 1-01-03-!6 Average Concentration (ng/mL) 4- %RPD Tre SeRr EeetsTer ]ToE eLee ta[wR] eaLetsst] 3M LIMS ID IS011-01-03-16-0"6 ba aie] IS011-01-03-16-0"7 IS011-01-03-16-0"8 Description CGMN-MW101-0-140717 CGMN-MW101-DB-140717 CGMN-MW101-FMS-140717 1469 n~L 4-0,69% 83.9 n~/mL 4. 0.83% PFBS Concentration (ng/mL! %Recovery 29.5 NA 29 0 NA 128 99.7 PFHS Concentration (n~tmL) %Recovery 483 NA 477 NA 574 NC PFOS Concentration (nglmL) %Recovery f191 NA 194 NA 281 89.4 Average Concentration (nglmL) _+ %RPD a [o|coturnee[[staupra][teoures)| 3M LIMS ID Description 29.3 nglraL _+ 1.7% 480 nglraL _+ 1.3% %Recovery %Recovery %Recovery 193 ng/mL _+ 1.6% ISOll-01-03-16-0" 6 CGMN-MW101-0-140717 105 104 ISO11-01-03-16-0" 7 CGMN-MW101-DB-140717 106 103 ISOll-01-03-16-0" 8 CGMN-MW101-FMS-140717 109 Average Recovery (%) + %RSD 106%2.0% wn NA = Not Applicable rm NC = Not Calculated; Spike level was less than 0.Sx the endogenous sample concen~ation. Samples were diluted 1:100 and analyzed by external standard calibration. 105 104% 0.96% 106 105 108 106% 1.5% PAGE 23 OF 37 awe: 3M_MN01596162 33663300..00221133 Tot. CoM WIG tr Table 16. CGMN GW MWl04 140717 mae | ooo mT [me]| 3M LIMS ID ISO11-01-03-16-0" 9 Phe Er [21:15] ISO11-01-03-16-020 ISOll 01433 16 021 Description CGMN-MW104-0-140717 CGMN-MW104-DB-140717 CGMN MW104-FMS 140717 PFBA Concentr=ion (ng/mL) %Recove~ 47.4 NA 48.4 NA 143 95.1 PFOA Concentration (ng/mL) %Recovery 74.4 NA 78.5 NA 176 101 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. ISO f 1-01-03-'16 Average Concentration (n~/mL) 4- o/oRpD mmr omer [eomm eeT ns ea ve| re e]"Siet Laeve]r] 3M LIMSID ISOll-01-03-16-0"9 Sae tolEal ISO1%01-03-16-020 Description CGMN-MW104-0-140717 CGMN-MW104-DB-140717 47.gn~mL4-2.1% 76.5 ng/mL 4- 5.4% PFBS Concentration (n1/mL! %Recovery 8.62 NA 8 74 NA PFHS Concentration (n~tmL) %Recovery 8.90 NA 8 99 NA PFOS Concentration %Recovery 228 NA 238 NA ISOll-01-03-16-021 CGMN-MW104-FMS-140717 106 98.3 i~) 105 97.0 il) 328 NC Average Concentration (nglmL) + %RPD ae [o|coturnte[[staupra][teoers)| 3M LIMS ID Description 8.68 nglmL _+ 1.4% 8.95 nglmL _+ 1.0% %Recovery %Recovery %Recovery 233 ng/mL _+ 4.3% leO11-01-03-16-0" 9 CGMN-MW10#-0-140717 104 ISO11-01-03-16-020 CGMN-MW104--DB-140717 107 ISOll-01-03-16-021 CGMN-MW 104-FMS-140717 105 Average Recovery (%) + %RSD 105%1.5% wn NA = Not Applicable re a NC = Not Calculated; Spike level was less than 0.Sx the endogenous sample concen~ation. Samples were diluted 1:100 and analyzed by external standard calibration. (1) FMS concentration greater than 10 times the sample concentration. 101 104 106 104%2.4% 104 104 104 104% 0.35% PAGE 24 OF 37 awe 3M_MN01596163 33663300..00221144 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. ISO f 1-01-03-'16 p------ Table 17. CGMN GW MWl05 140717 mae 3M LIMS ID 1 owe [w|m G we[a aon]| Description PFBA Concentration In~l/mL) %Recover~ PFOA Concentration In~/mL) %Recovers/ ISO11-01-03-16-022 CGMN-MW105-0-140717 40.9 NA 27.3 NA -- gf ISO11-01-03-16-023 CGMN-MW105-DB-140717 ISO11-01-03-16-024 CGMN-MW105-FMS-140717 Average Concentration (ng/mL) 4- %RPD [la ls 2] 37.4 NA 141 102 39.2 ng/mL 4- 8.9% 28.0 NA 128 102 27.7 ng/mL -+ 2.5% FO EO[ems1POTeme I ] ros. 3M LIMS ID ISO11-01-03-16-022 El H BEo REE ISO11-01-03-16-023 Description CGMN-MW105-0-140717 CGMN-MW105-DB-140717 PFBS Concentration (nglmL) %Recovery 4.87 NA 4.91 NA PFHS Concentration (ng/mL) %Recovery 6.34 NA 6.96 NA PFOS Concentration (ng/mL) %Recovery 37.5 NA 34.9 NA ISO11-01-03-16-024 CGMN-MW105-FMS-140717 106 102 (1) 103 97.3 137 102 Average Concentration (ng/mL) 4- %RPD 4.89 ng/mL 4- 0.82% 6.65 ng/mL 4- 9.3% 36.2 ng/mL 4- 7.2% ane 3M LIMS ID JomDescription | ctuger [stupee] ge [ ccoran | coro | veers| %Recovery %Recovery %Recovery Simpes IS011 014)3 16 022 IS011 014)3 16 023 IS011 01493 16 024 i EEE CGMN MW10,~0 140717 CGMN MW10,~DB 140717 CGMN MW10~FMS 140717 103 101 103 106 105 104 108 107 108 SE rT Avera~le Reeove~ (%) + %RSD NA - Not Applicable Samples were diluted 1:100 and analyzed by external standard calibration. (1) FMS concentration greater than 10 times the sample concentration. 105% 2.4% 105% 4- 2.9% 105%4- 2.3% PAGE 25 OF 37 sumerssiss 3M_MN01596164 33663300..00221155 SO Table 18. CGMN GW MWl08 140717 --3M LIMS ID ISO11-01-03-16-025 Phe ISO11-01-03-16-026 ISOll 01433 16 027 hoe maTwa] Description CGMN-MW108-0-140717 Ere [E12]: 1c] CGMN-MW108-DB-140717 CGMN MW10&FMS 140717 PFBA Concentration (ng/mL) %Recovery 224 NA 219 NA 320 NC PFOA Concentration (ng/mL) %Recovery 526 NA 5"18 NA 631 NC 3M ENVIRONMENTAL LABORA TOR Y REPORTNO. ISOf 1-01-03-!6 h [ems T e ens] ros Average Concentration fng/mL) 4- %RPD 222 n~/mL 4- 2,3% PFBS Concentration 522 n11mL 4-1,5% PFHS Concentration PFOS Concentration eT 3M LIMS ID Description (ng/mL) %Recovery (ngtmL) %Recovery (n1/mL) %Recovery ISO11-01-03-16-025 CGMN-MW108-0-140717 60.5 NA 11.4 NA ISO11-01-93-16-026 CGMN-MW108-DB-140717 60 9 NA 11 1 NA ISO11-01-03-16-027 CGMN-MW108-FMS-140717 159 99.3 107 96.7 lT e l| Scf eoraa | cero] n |cores | Average Concentration (nglmL) _+ %RPD 3M LIMS ID Description 60.7 nglraL _+ 0.66% 11.3 nglmL _+ 2.7% ~C~-PFBA ~C~-PFOA '~C~-PFOS %Recovery %Recovery %Recovery 58.2 NA 57 7 NA 155 98.0 ~8.0 nglmL _+ 0.86% ISO11-01-03-16-025 CGMN-MW108-0-140717 112 107 105 ISO11-01-03-16-026 CGMN-MW108-DB-140717 ISO11-01-03-16-027 CGMN-MW 108-FMS-140717 Average Recovery (%) + %RSD 104 106 107%3.9% 103 107 106%2.2% 103 104 104% 0.90% Co i NA = Not Applicable NC = Not Calculated; Spike level was less than 0.Sx the endogenous sample concen~ation. ae Aa Samples were diluted 1:100 and analyzed by external standard calibration. PAGE 26 OF 37 -- 3M_MN01596165 33663300..00221166 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. ISO f 1-01-03-'f6 Table 19. CGMN GW MW110 140716 mone lower [e | Rmaorey|"BE wsate]] 3M LIMS ID ISO11-01-03-16-028 EET ISO11-01-03-16-029 Description CGMN-MW110-0-140716 CGMN-MW110-DB-140716 PFBA Concentration (ng/mL) %Recovery 187 NA 183 NA PFOA Concentration (ng/mL) %Recovery 344 NA 435 NA ISOll 01~33 16 030 CGMN MW11(~FMS 140716 206 NO 390 NC Average Concentration fng/mL) %RPD 185 n/mL 4- 2,2% 390 n~lmL 4. 23% (1) -- sls3M LIMS ID ISO11-01-03-16-028 ISO11-01-03-16-029 Joss [1o 5mLave | Eemstree|]"5r|os. ates Description CGMN-MW110-0-140716 EEE EE CGMN-MW110-DB-140716 PFBS Concentration (ng/mL! %Recovery 81.1 NA 83 4 NA PFHS Concentration (n~tmL) %Recovery 21.4 NA 26 7 NA PFOS Concentration (n1/mL) %Recovery 16.4 NA 144 NA ISO11-01-03-16-030 CGMN-MW110-FMS-140716 99.9 NC 43.4 97.7 32.9 88.4 Average Concentration (nglmL) _+ %RPD 82.3 nglraL _+ 2.8% 24..1 ng/raL + 22% 15.4 nglraL ~" 13% [corsa|cor | co oren s | I~C~.PFBA ~3C4.PFOA I~C4.PFOS ge lee Low LoomLeones] 3M LIM8 ID Description leO11-01-03-16-028 CGMN-MW110-0-140716 EE TET leO11-01-03-16-029 CGMN-MW110-DB-140716 ISO11-01-03-16-030 CGMN-MW110-FMS-140716 Average Recovery (%) + %RSD %Recovery 102 105 103 103% -~ 1.5% %Recovery 94.0 95.3 98.2 95.8% -+ 2.2% %Recovery 100 98.8 99.8 99.7% ~" 0.79% =NA = Not Applicable NC = Not Calculated; Spike level was less lhan 0.Sx the endogenous sample concen~ation. S enh eapi oa m aa, Samples were diluted 1:100 and analyzed by external standard calibration. (1) Samplelsample duplicate RPD did not meet acceptance cdteda of-<20%. PAGE 27 OF 37 3M_MN01596166 33663300..00221177 ae comoweonr Table 20. CGMN GW PW09 140717 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. ISO f 1-01-03-'f6 we 3M LIMS ID IS011-01-03-16-032 Zim ISOll 014)3 16 033 ISOll 014)516 034 o| we omLaaT|wa] Description CGMN-PW09-0-140717 mms [Elo CGMN PW09 DB 140717 PFBA Concentration (ng/mL) %Recovery 432 NA 432 NA PFOA Concentration (ng/mL) %Recovery 1.17 NA 1.15 NA CGMN PW09 FMS 140717 669 NC 3.28 107 Average Concentration (ng/mL) 4- %RPD 4.32 ng/mL 4- 0.0% 1.16 ng/mL 4-1.7% mane 3M LIMS ID ISOll-01-03-16-032 andl ISOl 1-01-03-16-033 ISO11-01-03-16-034 Joogme | [ome[omy7 |"EE mesn T|T"EEw[e ote] Description CGMN-PW09-0-140717 S EAE LEEREY CGMN-PW09-DB-140717 PFBS Concentration (n~l/mL! %Recovery 0.152 NA 0 158 NA PFHS Concentration (n~tmL) %Recovery 0.0810 NA 0 0806 NA PFOS Concentration (n~l/mL) %Recovery 1.79 NA 1 78 NA CGMN-PW09-FMS-140717 2.06 96.2 i~) 2.26 110 ~) 3.84 104 Average Concentration (nglmL) _+ %RPD 0.155 nglmL ~" 3.9% 0.0808 nglmL _+ 0.~0% 1.79 nglmL _+ 0.~6% [eras |eovos |eres| 3M LIMS ID Description %Recove~ %Recovery %Recover/ ISOl 1-01-03-16-032 CGMN-PW09-0-140717 ISO11-01-03-16-033 CGMN-PW09-DB-140717 oa i HEE ISO11-01-03-16-034 CGMN-PW09-FMS-140717 Average Recovery (%) _+ %RSD 90.6 108 112 103% -+ 11% 115 112 119 115% -+ 3.0% a NA = Not Applicable men ee NC - Not Calculated; Spike level was lees lhan 0.5x the endogenous sample concentration. EERE Samples were diluted 1:1 and analyzed hy internal standard calibration. 108 115 108 110% -~ 3.8% (1) FMS concentration greater than 10 times the sample concentration. PAGE 28 OF 37 swmorsesr 3M_MN01596167 33663300..00221188 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. ISO f 1-01-03-'f6 Table 21. CGMN GW PW10 140717 mEeE3M LIMS ID ISO11-0'1-03-16-034 ISO1 '1-0'1-03-16-035 88e [r o| s m Iw] La aee]] Description CGMN-PW10-0-'140717 TFT CGMN-PW'10-DB-140717 PFBA Concentration (ng/mL) %Recovery 479 NA 501 NA PFOA Concentration (ng/mL) %Recovery 0.479 NA 0.489 NA ISO1 '1-0'1-03-16-036 CGMN-PW10-FMS-'140717 744 NC 2.61 108 Average Concentration (nglmL) -+ %RPD 4.90 ng/mL -+ 4.5% 0.484 ng/mL -+ 2.1% CC Tews [ens] ros. 3M LIMS ID ISOll-01~)3-16-034 EEE TLD ISO11-014)3-16-035 Description CGMN-PW10-0-140717 CGMN-PW10-DB-140717 PFBS Concentration (nglmL) %Recovery 0.522 NA 0.558 NA PFHS Concentration (nglmL) %Recovery 0.101 NA 0.106 NA PFOS Concentration (ng/mL) %Recovery 0.498 HA 0.507 NA 18011-014)3-16-036 CGMN-PW10-FMS-140717 253 101 2.32 112<~i 2.81 117 Average Concentration (ng/rnL) + %RPD 0.540 ng/mL -+ 6.7% 0.104 ng~mL -+ 4.8% 0.503 nglmL_+ 1.8% Bmuner3M LIMS ID ISOll 01<)3 16 034 ISO11-01-03-16-035 loE wer T Lorem|stT eers|some| Description CGMN PW10-0 140717 CGMN-PW10-DB-140717 I~C~-PFBA ~3C4-PFOA ~C,~-PFOS %Recovery 106 112 %Recovery "114 120 %Recovery 117 109 ISO11-01-03-16-036 CGMN-PW10-FMS-140717 92.0 "108 112 Average Recevery (%) %RSD 103% 0.7% NA - Not Applicable EEE cama cme erm NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concent~'ation. Samples were diluted 1:1 and analyzed by internal standard calibration. TR rn otho Rn. (1) FMS concentration greater than 10 times the sample concentration. 114% 5.3% 3% ~- 3.8% PAGE 29 OF" 37 3M_MN01596168 33663300..00221199 Tal 2.COMM GANS. 14an8d TR7IPB1LAN8KS Table 22. CGMN GW MW13-RB 140716 and TRIP BLANKS mae J| oe e mm [[wmee]| 3M LIMS ID Description PFBA Concentration (ng/mL) %Recovery PFOA Concentration (ng/mL) %Recovery 3M ENVIRONMENTAL LABORA TOR Y REPORTNO. ISOf 1-01-03-!6 ISO11-01-03-16-037 CGMN-GW-MW13-RB-140716 <0.0500 NA <0.0240 NA ISOl 1-01-03-16-038 ISOll 01493 16039 ISO11-01-03-16-040 CGMN-GW-TRIP-0-140715 CGMN GW TRIP LS 140715 CG MN-GW-TRI P-HS- 140715 move 3M LIMS ID oon Description <0.0500 NA <0.0240 NA 1 91 95.5 2.14 108 97.7 97.7 96.8 98.0 [o 1 m me | am PFBS Concentration [im Loy[Em oer [Ei | oy (ng/mL! %Recovery PFHS Concentration (n~tmL) %Recovery PFOS Concentration (n~l/mL) %Recovery IS011-01 .-03-16-037 IS011-01-03-16-038 CGMN-GW-MW13-RB-140716 CGM N-GW-TRI P-O-140715 <0.0250 NA <0.0250 NA 0.0388 NA <0 0250 NA <0 [3250 NA <0 0232 NA ISO11-01-03-16-039 CGMN-GW-TRIP-LS-140715 1 98 100 2.22 112 2.10 106 ISO11-01-03-16-040 CGMN-GW-TRIP-HS-140715 101 102 97.7 98.7 98.7 99.7 mae 3M LIMS ID owe De~cdption Lovee [om | te | %Recover]/ %Recovery %Recove~ ISO11-01-03-16-037 CGMN-GW-MW13-RB-140716 96.4 116 116 ISO11-01433-16-038 CG MN-GW-TRI P-0-140715 90.9 115 114 ISO11-01-03-16-039 CG MN-GW-TRI P-LS-140715 92.3 112 102 E en t saahpaaoty ettsiev"e R813hh tty sesn ISQ11-01-03-16-040 CGMN-GW-TRIP-HS-140715 107 101 104 NA = Not Applicable Samples were diluted 1:1 and analyzed by internal standard calibration with the exception of the TRI P 14S, which was diluted 1:100 and analyzed by external standard calibration. PAGE 30 OF 37 awmorsaetes 3M_MN01596169 33663300.00222200 RY 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-16 55 CCoonncclluussiioonn VT ---- Laboratory control spikes were used to determine the analytical method accuracy and precision for all ny analytes. The accuracy and precision were then used to estimate the method uncertainty for the Dn results. Field matrix spike recoveries demonstrated that the analytical method was appropriate for the ml a cos A Soro TEES given sample matrix except where noted. Analysis was completed using 3M Environmental Laboratory Lt? method ETS-8-044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water A ww a a A a Ho by LC/MS/MS; Direct Injection Analysis". Analytical results are reported in Tables 1 and 10-22 of this report. 66 DDaattaa// SSaammppllee RReetteennttiioonn Pitkinpo Ub AAllll rreemmaaiinniinngg ssama pleam annddp aassssol occiiaae tteeddpprorojjeecctt ddaattaa ((hahrdcaopryaadnnddceeleleoccttrproonniyicc)) wwililll bbeeaarrcchhiivveeddaaccccoorrddiinngg to 3M Environmental Laboratory standard operating procedures. 77 AAttttaacchhmmeennttss s[Leipnao Trt a Any g tre a TadoGrogtohCoonog droaMeantrWels VAGE, WV, Appendix A: Target Analyte Historical Trend Data for Cottage Grove Monitoring Wells MW07, MW12, MW13, MW16, MW101, MW104, MW105, MW108, MW110, PW09, and PW10. 88 SSiiggnnaattuurreess ( NY, py Ei et N Enviromnental LaboratoB,'- authenticated by LRA. Ban 0. WA EEEEESERT ~v'olf SET R---- _.1'~{ ~'>} .... ..... # emai'=s~'v3'f~IRehaasovne..r.e.v.ie.w..e.d.t.h.is. 3%4documentcn=S..... Susan T. Wolf, 3M Principal Analytical Investigator DN: c-US, st-MN, l-St. Paul, oh- Labe~tory Director, TR RamenFD. EroThey Tees Date: 2014.08 11 !D:37:!8 -05'00' William K. Reagen, Ph.D., 3M Environmental Laboratory Technical Director TE sR RT The 3M Environmental Laboratory's Quality Assurance Unit has audited the data and report for this project project. olof Gtr EEE Quality Assurance Representative Bihontorepntnhsalanstboreproduce oxcsp inFl withoutwriten approval of ho This test report shall not be reproduced except in full, without written approval of the 3M Environmental Laboratory. psn PAGE 31 OF 37 sw_osso170 3M MN01596170 33663300..00222211 CottageGroveHWE?--untsaro ng. AAppppeennddixiAAx:: TTaarrggeettAAnnaallyyttee HHiissttoorriiccaall TTrreennddDDaattaa Cottage Grove MW07 - units are ngfmL ERKA otarT ash 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-16 4 Tht | CORARRRANN PFOS--@-- [oawor1 so:sons|umraons [ asaons| psnons [somwmons[sone|amavis| sngoons | MW07 fonT os sol sal wn] sol ow] sw sa PFBA [roa| om ool oso] om om ome] ome] owe] PFOA [ores | como| como] oe| _aome| coms | oon | ooseo| sores PFBS Coes| omw| wom| oom oan om] om] oom| om] PFOS 10/15/2012 2.55 0.298 <0.0250 0.0257 1/29/2013 2.09 0.259 <0.0250 0.0439 4/22/2013 2.61 0.240 0.0268 0.0459 Sates eb fr hr PS Samples were below the limit of quantitation for PFHS. 7/23/2013 1.71 0.303 0.0396 0.241 10/28/2013 3.07 0.428 0.0291 0.104 1/13/2014 2.88 0.390 <0.100 0.104 4/23/2014 2.48 0.344 0.0360 0.0493 7/16/2014 3.05 0.602 0.0762 0.237 CotsgeGrove WW12 units re ng. Cottage Grove MW12 - units are ng/mL 100 | mmr RR RNR RN Foz] somo|smo|arms|sans[sown|sno|ese| ome| MW12 [oe| om| wl en] nl ea ow] ml wm PFBA fron Tim se] som wo] wu] ww su] wr] PFOA [osTol wel awl awl ws] wal wo] od] PFBS [ons | wool wl seal aol wel wal ww] wal PFHS loo 1 wl sol wl ml nl wl wl msl PFOS 10/1912012 975 1390 94.3 20.9 122 1/30/2013 484 946 91.4 13.7 143 4/25/2013 622 1020 105 16.4 145 7124/2013 iii0 2000 175 23.9 204 10/31/2013 408 954 87.7 13.0 131 1/16/2014 31Z 668 82.1 13.1 121 4/25/2014 2Z0 548 68.9 9.82 117 7/17/2014 154 402 50.4 8.11 96.9 [r-- PAGE 32 OF 37 _Motsee71 3M MN01596171 33663300..00222222 AgpandicA:TargetAnal HlorcaTrendData Appendix A: Target Analyte Historical Trend Data CottageGroveHWH3 intsaro ng. Cottage Grove MW13 - units are ngfmL ERAT Kotarash 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-16 . a ILe RE N tet fy t ot SMR NNR [omaIsommmons| smosons Tamers| arson soonons |snes| apanons [anemone| [v/W13 [reToso] seo] ose] esol awl aml onl aw] PFBA [ron Tool asl sal ew] sal aml wml uw PFOA [ros | eas] ase] om] sw] om| aml om] osm] PFBS [ons | owl omel om ses] ose oom] omsl om] PFHS loos[ssl sw[ so] sol sol sal on] ul PFOS 10117/2012 7.10 3.33 0.619 0.487 3.85 1/29/2013 5.60 2.56 0.56 0.396 3.92 4/24/2013 9.34 5.46 0.972 0.931 4.05 CottageGroveHWIG --untsaro ng. Cottage Grove MW16 - units are ng/mL 7/23/2013 8.30 6.17 1.07 1.05 4.02 10/30/2013 6.48 4.01 0.571 0.366 1.40 1/14/2014 9.80 9.78 1.20 0.969 3.08 4/24/2014 7.14 8.63 0.752 0.556 2.33 7/16/2014 8.08 14.4 0.973 0.713 4.48 4".aye et et Wo tir CRRA [ame T sonsnons|sono |srsimss| suena| wrsima|"sosnons [_snecne| MW16 [re1 wel wsT wal ses] sol wo] wo al PFBA [roa | wo] wel we seal mel mol wal ams) PFOA [ows [aol asl os] see] wal wol wel ol PFBS fos Tam as] aul an] sw] sol an] sul PFHS bros Toul soo] el si] wa] sul wo[ wo PFOS 10/18/2012 33.6 45.9 25.7 2.71 23.1 1/29/2013 31.5 42.6 28.3 2.54 20.2 4/24/2013 33.2 43.8 27.5 2.74 21.8 7/24/2013 26.3 39.9 29.6 2.83 20.1 10/30/2013 45.0 73.9 42.1 3.95 38.2 1/14/2014 42.9 91.0 40.0 5.52 53.1 4/24/2014 40.7 85.7 37.9 4.49 51.9 7/16/2014 45.7 98.3 37.9 5.46 57.0 33663300.00222233 srcesnors PAGE 33 OF 37 _otses172 3M MN01596172 CottageGroveHWIDA unsarent AAppppeennddixiAAx:: TTaarrggeettAAnnaallyyttee HHiissttoorriiccaall TTrreennddDDaattaa Cottage Grove MW101 - units are ng/mL ERKA otarT ash 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-16 LEE RRR [oawsorIsoswors | ssomons| apamns |srsponsTsrsomons|sssona|"asrone |sporns MWI01 [rn T sol sow[ sol so] so] we] wo] sao PFBA fron Tol wal al wel so] mal wo wl PFOA [ros | aol wal wes] aso] ass] mal wal as PFBS [os | wo] ww nl we we] we] wa aw PFHS los| wl owl ml wl wl wl ws ml PFOS 10/18/2012 1860 147 23.9 427 154 1/30/2013 1630 124 25.2 455 206 4/23/2013 1830 121 19.5 459 188 7/25/2013 1680 112 24.0 464 189 10/30/2013 1020 86.7 25.5 314 158 1/15/2014 1510 79.4 25.4 398 159 4/25/2014 1330 76,0 37,8 364 135 7/17/2014 1460 83.9 29.3 480 193 CatiagoGroveNWIDA uns arog. Cottage Grove MWl04 units are ng/mL = =o v/ Aaa. --~--\/ AJ -d f= aeheam"A 1A A TS Te hh RN [aes[sone | samons | sosons|srsons [orsaoons | nsions |amsoos|smoone| MWI04 [ow| sol sol wl sol sel wml wl as PFBA [ro | wo] ws] wor] sual ms] esi] mi] es] PFOA [oe | wel wel on]wl ml iw] ww] ea PFBS [ous I wol sol wal wel wil sal we] um] PFHS boTol ol wl wl wl an] ul ou] PFOS i0/18/2012 36.0 42.0 12,6 8.69 ]27 1/30/2013 36.3 44.8 11.4 9.07 201 4/25/2013 74.7 60.7 9.75 13.4 ~85 7/25/2013 54.3 74.7 8.16 11,8 176 a0/30/2013 53.6 72.5 7.95 10.1 ]65 a/15/2014 202 35.1 7.50 14.2 4.25 4/25/2014 107 82.1 8.10 12,6 234 7/~7/2014 47.9 76.5 8.68 8.95 233 33663300..00222244 srcesiors PAGE 94 OF 37 _Motses17s 3M MN01596173 rv 51 avon 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-16 CottageGroveHWI05 --unts are ng. AAppppeennddixiAAx:: TTaarrggeettAAnnaallyyttee HHiissttoorriiccaall TTrreennddDDaattaa Cottage Grove MWl05 - units are ng/mL - = = 7\ r Le ES~T ~. SRNR Bo mm [omc T sonanors|sysnons |amsons|srspons[ropanons| snasens|amsons | one| k4WiO5 [rnTool sel ool mel sol sel mol sal PFBA fron I wsl wel wm] wel wal wal wal am] PFOA [ros | ol ww] snl owl awl es] sal am] PFBS [ows | wo an] wool awl wml mel ssl eel PFHS [ros 1 sol wo] wo] ws] ww sw] wil sel PFOS 10/19/2012 52.7 98.3 9.46 18.9 120 1/30/2013 54.4 119 8.03 21. I 129 4/25/2013 57.0 104 5.72 16.0 95.0 7/25/2013 71.6 70.6 6.49 6.35 923 10/30/2013 38.9 87.2 4.98 6.01 467 I/i4/2614 55.6 68.3 6.15 12.6 152 4/25/2014 71.0 44.3 7.68 8.59 58.7 7/17/2014 39.2 27.7 4.89 6.65 36.2 CottageGroveMWA08 unairontins. Cottage Grove MWl08 units are ng/mL JE? tom RRR [sacs soswnons| ssomons| sosions [sacsTsssomns[sens |_amsimna|smanns MW~O8 [oonTl ol ws] sol wal sie] wal aml PFBA [roa | sol sal sal | an] | | a PFOA [ows | sosl oes sal see] ane] wel wal ail PFBS us Trl wal awl ws] ww] awl aw] ual PFHS broTol ws] wel al wl was] wl PFOS J0/~8/20~2 ~55 550 30.5 20.7 55.2 ~/30/20~3 ~01 348 26.5 i~.i 45.5 4/25/20~3 42.5 20~ ~6.~ 4.95 373 7/24/2013 38.0 202 ~4.6 4.94 26.8 ~0/30/2013 5].7 218 2~.6 4.47 33.2 ~/~4/2034 5~.6 169 ~7.~ 4.13 33.5 4/2S/2034 65.4 164 ~7,4 3.58 43.3 7/17/20~4 222 522 60.7 11.3 58.0 33663300..00222255 pice sors PAGE 35 OF 37 _MNO1SS617s 3M MN01596174 AopendiAx: TargaAnas Hora Trond ata Appendix A: Target Analyte Historical Trend Data CotsgeGrove WWH10 ut re ng. Cottage Grove MW110 - un its are ng/mL ERAT Kotarash 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-16 TY Dae Eee a SRN RRR % % . [oawsoTsoswors | ssomons| apsns [snapsTsrsomons |sone|"srarone |smnarns MW110 "10/18/2012 "1/30/2013 4/25/20"13 7/24/2013 "10/30/2013 1/14/2014 4/24/20"14 7/16/2014 fr T= al" nl wel sw] we] wl wl wl PFBA 144 171 183 304 174 179 189 185 fron I wl wl sol wae] ww[ aul wo] sol PFOA 193 141 160 144 190 248 3"10 390 [ros | wel wel wor] wal sa] wal wa] wal PFBS [ons| mel PFHS Loos Toe] PFOS 39.6 17.6 21.6 46.6 wos] wel 10.3 ose] seal 28.6 66.7 11.8 26.4 43.8 om] 9.41 wal 17.8 94.8 sss] "15.3 sal 21.1 85.1 seal 19.4 oa] 12.1 86,1 00] 20.9 ses] 12.5 82.3 aul 24.1 usd]15.4 CotageGrove PWo9 unisaeng. Cottage Grove PW09 - units are ng/mL Lpe em RNR NY [owen Tssinons [aaons [oars[nemo Tassos[ramon[nse| asons [one] PW09 [oon1 sn] wl oo] wal wel asl wl ass] an] PFBA [roa | om] ow] cos] we|om] se] am] ae] uel PFOA [mos | oml owl cw] oswl awl sol aul sl inl PFOS 412512013 3.72 0.223 0.324 61"1912013 NA 0.462 0.376 712412013 2.95 0.624 0.622 8129120"13 NA 0.605 0.818 9/30/20"13 NA 0.873 1.38 10/29/20"13 4.53 1.02 1.52 1/15120"14 4.76 1.33 2.13 4/25/2014 4,14 1,05 1.6 7/17/20"14 4.32 1.16 1.79 [------ NA = Not Applicable; analyte not requested for the sampling event. 33663300..00222266 sesecry PAGE 36 OF 37 auotsse 17s 3M MN01596175 CotageGrovePWD ntsasrg. AAppppeennddixiAAx:: TTaarrggeettAAnnaallyyttee HHiissttoorriiccaall TTrreenndd DDaattaa Cottage Grove PWl0 - units are ng/mL He REOR011T015O.18 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-16 Lorepe t WN RNR NN 7= [woTamspons| nopons [rons["ssmnons| amos[somomons [spore|amsione|sors] PW10 fonTwo] wel sol wl wl] ol sw| sol uso] PFBA [mon | wos] ous] owl om] ous] ows] om| om] om] PI:OA [ros | osm] me] oso wa] wl] om] om] om] esol PFBS [ows | ow] wel ows wl wl om] oow| om| om] PFHS [ros1 osmel om] om[ ous] oms[ om] om] om[ om] PFOS 4/25/2013 4.25 0.428 0.594 0.197 0.396 6/19/2013 NA 0.415 NA NA 0.401 7/24/2013 3.37 0.420 0.540 0.185 0.38 8/29/2013 NA 0.471 NA NA 0.415 9/'30/2013 NA 0.528 NA NA 0.465 10/29/2013 6.09 0.524 0.703 0.193 0.458 1/22/2014 4.40 0.212 0.261 0,0485 0.124 4/25/2014 5.07 0.421 0.471 0.110 0.437 7/17/2014 4.90 0.484 0.540 0.104 0.503 EE ---- NA = Not Applicable; analyte not requested for the sampling event. 33663300..00222277 [r-- PAGE 37 OF 37 auotsss 17s 3M MN01596176 OOCCTTOOBBEERR 22001144 33663300~.00222288 3M_MNO1596177 3M MN01596177 rT Kotarash 3M ENWRONMENTAL LABORATORY REPORT NO. IS011-01-03-18 FFiinnaall RReeppoorrtt AAnnaallyyssiiss ooff PPFFBBAA,, PPFFOOAA,, PPFFBBSS,, PPFFHNSS,, aanndd PPFFOOSS iinn CCoottttaaggee GGrroovvee GGrroouunnddwwaatteerr 44tthh QQuuaarrtteerr 22001144 SSaammpplliinngg LLaabboorraattoorryy RReeqquueesstt NNuummbebre:r: 1ISSO01111.-0011.-0033--1188 RDeot-p Det ot fLast Satire Report Date - Date of Last Signature TTeessttiinngg LLaabboorraattoorryy 33MM EEHHSS OOppeerraattiioonnss 3M Environmental Laboratory 3M Environmental Laboratory Building 260-5N-17 Building 260-5N-17 MMaapplleewwoooodd,, MMNN 5555114444--11000000 RReeqquueesstteerr 3MGGaaErryyHSHHooOhhpeeennrsasttteeiiionnns 3M EHS Operations SSaa33iPinnMhMtot nPPBBeuaau:iuuill,dld(,ii8nMMn5gg1NN)22552275544311--75445-W443W.-5---11700000330000 Phone: (651) 737-3570 S&, acs 7 DV (EAcaEfBgEs) Th eating ported arn oth rocuirofeAmNSeHSnOtIEsC 70252005 The testing reported herein meet the requirements of NI$1/ISO,'IEO 17025:2005 "General Requirements for the Competence of Testing and Calibratio~l res secre nhAS Cates8 10920, Astao.a Laboratories", in accordance with A2.LA Certificate # 2052.01. Additionally, the labors quilky system has been audied and was defemined to bo in laboratory's quality system has been audited and was determined to be in mn TE Sal i men A conformance with the EPA GLPs (4~ CFR 792) by an independent A2LA 33663300..00222299 . PAGE 1 OF 34 _MNO1Ss6178 3M MN01596178 3M `REPORTNO. 1SO011.01-03-18. ENWRONMENTAL LABORATORY REPORT NO. IS011-01-03-18 Environmental Laboratory 3M Environmental Laboratory Eri abort o Tashi n Otect. WimSoonP10. 3M Environmental Laboratory Technical Director: William K. Reagen, Ph.D. as 3M Principal Analytical Investigator: Susan Wolf tis Report Author: Kevin Eich Analytical Report 1S011.01.03.18 Analytical RepoA ~SO11o01 o03ol 8 AveBA, PFOA PBS FS, PEGS in Cte Grove Grama Analysis of PFBA, PFOA, PFBS, PFHS, and PFOS in Cottage Grove Groundwater LAAN AR 4th Quarter 2014 Sampling Sette peton Report Date: Date of Last Signature 1 Introduction/Summary 1 Introduction/Summary A -- The 3M Environmental Laboratory prepared and analyzed groundwater samples collected byWeston io So Sa oh. Solutions personnel at the 3M Cottage Grove facility. Samples were collected on October 28-30, 2014. Be So re em pee Samples were returned to the 3M Environmental Laboratory' on October 30, 2014 on ice for the a ae te oe 2% analysis of Perfluorobutanoic acid (PFBA), Perfluorooctanoic acid (PFOA), Perfluorobutane suifonate PE eae ro Coe sams (PFBS), Perfluorohexane sulfonate (PFHS) and Perfluorooctane sulfonate (PFOS) under laboratory rers project number ISO11-01-03-18. ToSM Eon arnt rd aio corr ov sarin ocstors. Ech The 3M Environmental Laboratory prepared sample containers for twelve sampling locations. Each s`saammppllee sseett ccoonnssiisstteeddooffaaffiieelldd ssaammplpele,, ffiieellddssaammppllee dduupplliiccaattee,, a andan attaard rggeett aannaallyyttee ffiieelldd mmaatrtriixx ssppiikkee.. i as ot mriCoa rke Each empty container was marked with a "fill to ~ere" line that corresponded to a final volume of 200 Feige EE iDredd min to mE Containers reserved for field matrix spikes were fortified with an appropriate matrix spike solution a a containing the target analytes prior to being sent to the field for sample collection. Select sample ave bottles were fortified with internal standards and surrogate recovery standards prior to being sent to the an field for sample collection. Sapovend read br FEA SFO PEGS, PES and PEGS sing mah ETS. Samples were prepared and analyzed for PFBA, PFOA, PFBS, PFHS, and PFOS using method ETSSe om 8-044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water by Bs mast) LC/MS/MS; Direct Injection Analysis". Internal standards were used to aid in the data quality eam objectives for the analysis of select samples, were applicable. a -------- Table 1 summarizes the sample results using the analytical method identified above. All results for Ee eo quality control samples prepared and analyzed with the samples will be reported and discussed --; elsewhere in this report. = SN wa| ToRY GESTS Thetesingreper her mtth ruinsofANSUISOEG 170252005 [he testing reported herein meet the requirements of ANSI/ISOflEO 17025;2005 "General Requirements for the Competence of Testing and Calibration Trey laboratory's qualitysystershasbeen aucitedandwasdeterminedtoboin Laboratories", in accordance with A2LA CerfJficate # 2052,01, ~ditionally, the laborato~'s quality system has been audited a~d was determ~aed to be in MesSel en bebe eeesad seitbe confo~an~ ~ the EPA GLPs (40 CFR 792) by an independent ~LA ~$ess~en~ 33663300..00223300 -- PAGE 2 OF 34 3M MN01596179 Table 1. Sample Results Summary 3M ENWRONMENTAL LABORATORY REPORT NO tS011-0!-03-18 ISOli-01-03-18-001 A emit] ISQI 1-01-03-18-002 E aA WL AA LLL ISO! 1-01-03-18-004 I E EES a E Ne AL LAS3A ISO11-01-03-18-005 CGMN-GW-MW07-0-141028 CGMN-GW-MW07-DB-141028 Average %RPD Sample/Sample Dup CGMN-GW-MW12-0-141030 CGMN-GW-MW12-DB-141030 Average %RPD Sample/Sample Dup 3.15 2.87 3.01 9.3 !26 128 127 ~2) 1,6 Concentration (ngtmL) 0.615 &547 0.581 12 345 350 34812~ 1.4 00762 00639 0.0781 18 45.8 46=4 46.1 ~21 1.3 0.0511 0.0495 0.0503 3.2 7.79 7.76 7.78 ~2~ 0.39 0.I94 0.187 {).191 3.7 92,0 93.0 92.5 1,1 eSe TRTATEE] ISO11-01-03=18-007 ISO11-01-03-18-008 CGMN=GW-MW13-0=141028 CGMN-GW-MW13-DB-141028 Average %RPD Sample/Sample Pup 9.52 9.76 9.64 2,5 9,76 10.3 10,{) 5.4 1,07 1.10 1.0~) 2.8 0,712 0.727 0,720 2.1 483 494 ~$,89 ISO11-01-03-18-010 CGMN-GW-MW14 R-0-14 t 029 570 355 38.7 16.5 85,2 ISO11-01-03-18-011 CGMN-GW-MW14R-DB-141029 569 351 37.4 16.7 80.0 ISO11-01-03=18-013 ISO11-01-03-18-014 Average rn> %RPD Sample/Sample Dup CGMN=GW-MW 16-0=141028 CGMN-GW-MW16-DB-141028 Average 570 (2) 0.18 38.2 39.6 38,9 353 t2~ 1.1 73.7 77.8 75,8 38.1 (21 3.4 32.8 35=0 33,9 16,6 (2) 1.2 4.45 4.71 4.58 82,6 41.7 43.4 42,6 ISO11-01-03-18-016 ISOll-01-03-18-017 r Ei E r TeTETETE Te ISO11-01-03-18-019 ISO11-01-03-18-020 fE oE EEE E aE T STE ISO11-01-03-18-022 [E5rik: ISOll-01-03-18-023 %RPD Sample/Sample Dup CGMN-GW-MW101-0-141029 CGMN-GW-MW101-DB-141029 Average %RPD Sample/Sample Dup CGMN-GW-MWI04-0-141029 CGMN-GW-MW 104-DB-141029 Average %RPD Sample/Sample Dup CGMN-GW-MW105-0-141029 CGMN-GW-MW105-DB-141029 3.6 1410 1400 1410{~ 0.71 3"1.0 30,8 30.9 (2} 0.6~; 45.6 47.0 5.4 75.2 74,4 74.8(~1 1.1 50.3 49,7 50,0 (=1 1.2 93.8 91.8 6.5 29.6 29.6 29,6{~ 0.0 7.73 7,71 7.72 {z~ 6.26 3.88 4.13 5.7 460 443 452~) 3,8 5.81 6.67 6.24 {2} 14 1&7 19.0 165 174 170 5,3 176 177 177 0.57 73.9 73.0 EEE IS(')11-01-03-18-025 reo ISOll-01-03-18-026 Average %RPD Sample/Sample Dup CGMN-GW-MW108-0-141029 CGMN-GW-MW108-DB-141029 Average %RPD Sample/Sample Dup 46.3 iz~ 3,0 88 1 85,9 87.0 2.5 92.8 (~1 2.2 268 267 4.01 ~1 6.2 23 0 22.4 18,9 ~z~ 1,6 8 20 8.79 73.5 1,2 42 3 41,6 e E Ri E Ie ER ARR (~) Sample set was analyzed by internal standard calibration, except where noted. The analytical method uncertainties associated with the reported results by internal standard calibration are as follows: PFBA _+ 14%, PFOA _ 22%, PFBS 16%, PFHS _+ 12%, and PFOS _+ Em e 16%. RR (2) Sample set was analyzed by exlemal standard calibration --he analytical method uncertainties associatad with the reported ~sult. by external standard calibration are as follows: PFBA + 24%, PFOA 14%, PFBS 8.6%, PFHS 11%, and PFOS 15%. 33663300..00223311 aPAGE 3 OF 34 3M MN01596180 3M ENWRONMENTAL LABORATORY REPORT NO tS011=0!=03=18 Table 1 continued, Sample Results Summary (1) [mse swguoucsgton |oron |pron| eres | pews | pros| 3191 LIMB ID Sn i EE T ET T ISO11-01-03-18-028 ISOI 1-01-03-18-029 E eE ma aaEs ISO11-01-03-18-031 ISO! 1-01-03-18-032 Sample Description CGMN-GW-MW110-0-14i028 CGMN-GW-MW110-DB-141028 Average %RPD Sample/Sample Dup CGMN=GW=PW09=0=141030 CGMN-GW-PW09-DB-141030 290 297 294 (~) 2,4 3.84 3=90 Concentration (ngtmL) 415 4I 9 417 Im 0.06 0.721 0=681 57=9 57.3 57.6 (:) 1.0 0.101 0=I 10 2&4 23.6 23,5 ~2} 0.85 0.0560 0,0522 12.9 12.8 12.9 (~) 0.78 0,919 0.757 J tn EAEATAT ISO11-01-03-18-0,14 [rmsHTB ISO11-01-03-18-035 Average %RPD Sample/Sample Dup CGMN-GW-PW10-0-141030 CGMN-GW-PW10-DB-141030 Average %RPD SampledSamp~e Dup 3.87 1.6 4.48 4.38 4.43 2.3 0.701 5.7 0.379 0.372 0.376 1.9 0,106 8.5 0.412 0.387 0.400 6.3 0.0541 7.0 0.0795 Q0759 0.0777 4.6 0.838 19 0.345 0.329 0.337 4.7 r R -- g ---- AE E A T (!) Sample set was analyzed by intemal standard calibration, except where noted. The analytical method uncertainties associated with the reported results by internal standard calibration are as follows: PFBA 14%, PFOA 22%, PFBS 16%, PFHS 12%, and PFOS + Emr RR = 16%. (2) Sample set was analyzed by exlemal standard calibration. "-he analytical method uncertainties associated with the reported results by extamal standard calibration are as follows: PFBA _+ 24%, PFOA _+ 14%, PFBS _+ 8.6%, PFNB _+ 11%, and PFOS _+ 15%. E c gr r eT e r -- 22 M Metehotds-h-AAnnoaalyldyttiiccsaall aanndd PPrreeppaarraattoorryy 2.1 Methods Analysis was completed following 3M Env ronmental Laboratory method ETS-8-044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC!MSiMS; Direct Injection Analysis". Tabie 2. Target Analytes I B ES r E re Te r TargetAnalytes Acronyre Reference Materia~ Structure [Pobomtmo| chprsea| oiciumressg| Perfluorobutanoic Acid (C4 Acid) PFBA Linear [Pemoscamo | cprh on| ooinc ew+Baancnhesss| ........P_.~..d._!~_~._.~_a...~.A...A_.~.~..L.C_~.._.A...~!.g.)_............................................................................._P_.E~.......................................................L_.!_.n..~.L_+....~.r_~b_~.................................... |PetontutmonsorusCasumonote) | rss| ume | Perfluorobutanesulfonate (C4 Sulfonata ) PFBS Linear [Pemorsrermensorste Cosutonay |pews| uma | Pedluorohexanesulfonate (C6 Sulfonate) PFHS Linear [Pemoncamensono osuonsty | pros| unew:Bohes | PerfluorooctanesuFonate (C8 Sulfonata) PFOS Linear 4- Branched 2.2 Sample Collection `SSaammpplleesswweerreeccoolllleecctteeddoonnOOctcotobbeerr2288--3300,, 22001144iinn NNaailggeenneeTTMM(h(hiigghh-=ddeennsstityyppoolylyeetthhyylleennee))bobtottitloesspprreeppaarreeddaatt the 3M Environmental Laboratory. Prior to sample collection, bottles designated for field matrix spikes were spiked in the laboratory with a known volume of an appropriate matrix spiking solution containing the analytes of interest. Collected sample bottles were returned to the laboratory on ice on October 30, 2014. 33663300..00223322 _--PAGE 4 OF 34 3M MN01596181 REPORTRO 501 0150.15 3M ENVIRONMENTAL LABORA TORY REPORT NO IS01I-0f-,,03-18 2`2S.3a3mpleSScaaommncpeplnlieeraPPtrornoesppawaerrraaetteiioxopnnected 0 ange fom <0.025 ng. 101000 ng. Sampinglocationstavers. leSeoxxacppmaeetcpcitolteeendsdctotthoonaclnheaawnvveteerraocctioooennxnccpseeewnrcttiereaaredttioofennoxph<<ea11cv00te0e0dcnnotggnoifcmm,eaLLnniwwgaeeterirfeeoronaamn1naa0<lly0y0z.z0nee2dd5gbbyn.ygii/nnimtterLermnotaoalal>nssItai0aya0nnz0daearndrddgb/mccyaaLelli.xbbtrrSaeatamtioamilnnpsaalitnnnaagalnlydylosasicrissad..ticoSSanaalsmmrtphapiatlintnogwgnere analysis. locations analysis. Thefolowingsampe that were expected to The following sample preperation procedures were alowedfor ach have concentration >100 ngimL were analyzed preparation procedures were followed for each typeof analysis. by external standard type of analysis. calibration rtIneotmeorrnvaailngssttaaann0dd.aa4rrdmd ccLaall_ibtvraaattilooonnfqaathunneayolwyssoti:ls: mSSiaaxmmepdpllseeassmaapnnlaaollyyazzneeddddbbiyuytinnngteerawnalil shsttaa0nn.dd4aamrrddLcocafallmitbreraattthiooannnwweee(rrdeeiptpirreoonppaafrreeaddcbbtyyofo2r) removing a 0.4 mL aliquot of the well mixed sample and diluting it with 0.4 mL of methanol (dilution factor of 2). DwDuautsriinnaggdttehhede pp0rreehppeaarralatatbiiooonrnaootfofrtthyheecaloabnbtorororalaltaorrmyyccaoonsntt(roonlosmsaaimmnpalplelescs,o, naacnneanaitliqrquauooolntoofof af|sseneppLaar)raa,ttee einTrthemarnasallassmttaaenndbdaaortrddlesssppwkikeiinnrggesssooollusktieioodnn wwowliiatlhhsocaaatndnodnti.neetderTrntnohaaeltlhlsseattbaaloannrbddaotaaorrrarddytommcryxioxcoaaottnlaatrosnnloaosmmmaipinmlnaeaplsl!eccwsooenn(rocnaeeonnmtithrriaenatnatiilodocnlnouoontffocd1e1 nwnntirggah/mmtiomLLneptporhrifiaooInrraotnolgbi!bmeeitLinnh)gge. essTaeahnnmettost0oamtmfthhapellenfiedbalndostffetotloerhrrsesswaamsmeparplemelpe.slpsik.ed collection. The laboratory control samples were then diluted with methanol in the same manner as the samples. aEEnxxattleoyrsmniasal.l ssSttaaamnnpddlaaerrddsccowalelbirbraeratitpioornnepaaannraaelydlysbsiysis::dSSuatamimpnlpgeles0s.a1annmaallyoyzzeeaddwbbeyyleex-xtmteexmrenadalsl assmttapnaldneardwditcchaall8ibb.r9raatmtiioLonnorrfeemqqouutiirrheeaddrcdlliulu(ttidooinnupptrnrioifroattcorotor analysis. Samples were prepared by diluting 0.1 mL of a well=mixed sample with 9.9 mL of methanol (dilution factor n0g1i1n0L0.). Analiquotofsumogate spiking sotionwasadded tote diutedsamples ta nominal concentration of of I00). An aliquot of surrogate spiking solution was added to the diluted samples at a nominal concentration of 1 ng!mL 22ll.44sampAAlnnoasallayynssdiiqssuay coil samploswera analyzedfor fe target analytes using high porfomanco iui cAcchhhlrlrvosoomammamaatptloolgoegrgsraarappanhhpdyyh/qygtauranaanddldiieteyemnmctommpnaratrsosogsslrsssaappmm,eeccpattlrnerodsommtweehetetrryyesp((aeHHncPPfaLiLlycCCzmieMMadSSsMf/soSMr)vSfa.iv)n.esttPPaoreegnrresttitnnaaeennnanatlliiyynnztsesettsrdruuuammsreeiennngGttephpsaiagcrrhraabmmpeeeetdrteefironrsrst,m,h0tahnetcalelbiqallueiuqsiddubidelow. chromatography gradient program, and the specific mass transitions analyzed are described in the tables below. DoDuueecttoottchhee onunafatmtuurrrueetodefetthhnieesssoaacmmmeprlpeesle,,ftthhheeewwaiidbdceerrraaalnnoggreeyo'offaccnooanniccteeennsttrroafatteioornnesssffo,ouunntddheinnsttohheelssaaarmmppulsleee,,daafnnoddrtphthreeoceeennsvvsiiirronongnmmieheen.nttaall oaPanencaccaleulyysrtstricaecaranlylc.erreesoAsuuflllmttmssuaiilnstiuppnalooelttaiasnbboellmgeeaetttoroiscocoononfsnitshsiaestrtoeelannbpttolyeyrarninttomtoereyrg'arsdattaeefnotatlhhloyeewteiaansnnagaloyltfythtiieincctaapelrlreoppsceetae,akdkt,uh,remmeassandnoutuuwaatlail rniiennettdeueggsirnreaadmttiieofootnnrhooopffdrothEncoeTeaSsan-san1ilna2ygl.yt0itti1hcc0aea.ll ppTeeahakek iiss pccnoroenoncscesieisssssttsaeernrnycc.oyyqAoofulfl ttrmhheefeaodnllauababaololrrimaanatttoenorgruyyra'as'ltiiioninntntesteggearrgaraerttioaipntoeinrissofotneersmnne,sseuurdrreeefoddvlilrtohewoorowfuinuggmgahhtnhttuehhaeeplrttoriaacniienendiignnugggraetoosfof roolasubrbtaolyintrtaeohtdoreryiyQn AppmeeUrer,ssthaooonnndnndeewEllh,TethShre-ee1p2po-en0eee1cr0rer.eesvsvTiaieherwewy hproocesrs roeoqfuvmiraeednufwoarlaillntmegarnautiaolnisntbeygrlaatbioonrast,otrhyeMraenviaegweomfemntanual integrations by the QAU, and where necessary the review of manual integrations by laboratory management. TTaabbllee 33., IInnssttrruummeenntt PPaarraammeteeterrss., [msitnsvtrmuemrenttMNaammee----T eErTsSoBuussteerr | Liquid Chromato~lraph [anotysisnotnoa | evssoms | Analysis Method [Anotysisome TT insemanaons | A~aiysis Date Agilent 1100 ETS=8-044.1 11/18/14 and 11t20/14 [uracoumn | pensicio@smm commis | Guard column Betasil C18 (4,6 mm X 100 mrq), [aniybeniconmn |owsicin 6mm tommyse | Analytical column Betasil C18 (4.6 mm X 100 mm), [InoctonvonmeTowa| ~njectien Volume 10 p.L, 30 p~L Mass Spectrometer [o1 nsowee vuosomy | ~on Source [Posy TT egw Pola~ty L| oomwas depier So,ware AB Sciex '[dple Quad 4000 Turbo Spray Negative Analyst 1.6.2 33663300..00223333 Prcesceas PAGE 5 OF 34 3M_MNO15%6182 3M MN01596182 ay 3M ENWRONMENTAL LABORA TORY REPORT NO IS01I-0!-,93-18 Table 3. Liquid Chromatography Grados Program. Table 4o Liquid Chromatography Gradient Program. ----r-- Step [e lTlIom m | Tpt=e , [or me] Number Pe Teeny) 0 r TmT e s] 1 Hea 2 oe meme] 3 F To mTe e ] 4 he me Two he 5 TTTa 5] 6 7 1 Foe mw] 8 eee TmTT] 9 ETS.,8-044ol ~nal~sis Tofal Time Flow Rate (FLlmin) Percent A (Methanol) Percent 8 (2 mM ammonium acetate) 0.00 750 &0 97.0 0.50 750 3.0 97.0 4.00 750 30=0 70.0 6.00 750 30.0 70.0 11.0 750 80.0 20.0 130 750 80.0 20.0 wo | me| eo| 00 | 13.5 750 160 750 90.0 90.0 10.0 10.0 18,5 750 3.0 97.0 19.0 75O 3.0 97.0 Tae 5. Mass Transits Table 5. Mass Transitions Ce [ po e[o = | Analyte FT--we--TT we PFBA Mass Transition Q 1/Q3 213/169 413/369 internal Standard [13C4]-PFIBA Mass Transition Q1/Q3 217/172 PFOA 413/219 [13Cs]-PFOA 421f376 |~ = roe 413/!69 [re -- 2 -- come PFBS 299/80 299/99 [I~O2]-PFBS 303/84 [=P-- 22--] oe PFHS 399/99 399/80 [ sC@PFHS 402/80 em 499/99 | ropes PFOS 499/80 507/80 as 499/! 30 Em TT [lSc~]-PFBA 216/172 217/172 [res[IsCp4]r-PFoOnA | awa 417/372 |rogeron| awe 421/376 | ChooTum--Tfeime Tm--1 [I~C4]-PFOS 503t80 507/80 rT . Dwell time was 50 to 100 msec for each transition. The individual transitions were summed to produce Aas a "total ion chromatogram" (TIC), which was used for quantitation. Ee i--------------r-------------------- (1) Intemal standard was not used for the samples analyzed by solvent dilution extemal standard calibration. 33 DDaattaa AAnnaallyyssiiss 33..11 CCaalliibbrraattiioonn Savor oars ing eal sandr alban: Samples ware ay or af ras agra Solvent dilution analysis using internal standard calibration: Samples were analyzed for all analytes against a ans matrix-matched stable isotope internal standard calibration curve. Calibration standards were prepared by spiking Dd known amounts of stock solutions into 50 mL of 50:50 methanol:laboratory reagent water, The calibration In standards contained an internal standard mix at a nominal concentration of 0.5 rig/mE Calibration standards gra OTS 100 rom ema eohond DTS 110 gL pen ranging from 0.0125 ng/mL to 100 ng/mL (nominal) were analyzed (0.0125 ng/mL to 10 ng/mL (nominal) for the Rein wei coboncas ho rt th datpan roo over on lon SRSs). A quadratic, 1/x weighted, calibration curve of the ratio of the standard peak area counts over the internal Sando tesco soo dra aT de ot rd oo loSr standard peak area counts was used to fit the data for each analyte. The data were not forced through zero during ais the fitting process. Calculating the standard concentrations using the peak area ratios and the resultant calibration rors, curve confirmed accuracy of each curve point. Poser PAGE 6 OF 34 sworso153 3M MN01596183 33663300..00223344 "REPORTNO 15011019315 3M ENVIRONMENTAL LABORA TORY REPORT NO IS01I-0f-,,93-18 c`SaSololiwvreeanntttidodniiluctouiornvne.aannCaaallylysbsirssatuuissoiinnnggseetxaxtnteedramnraadllssswtteaarnnoddpaarrrddepccaaalrliibeorrdaattbiiooynn:s: pSSiaanmmgpplkleenssowwwneerraeemoaanunanaltlyyszzeeodfdatgahageiasnintsostctakannsoeeuxxttteoernrnnanalfssotta5ann0ddmaaLrrd.d o(ocfaf l99nib00r::ao11t00iommnmweecirttuhhernaavaennn.ooaa:il:Cylilaazalbebi)boodrr.raaatttioooArrnyyqusMMatiadilllrni-a-dQtQaiT"rcMdTM,sfww/awaxtewteeerrer.i.gphCCrtaeaelpdliiabb,rrreaactdtaiiolobnbnyrsasstttpaiainoknndidnaacgrrudcrkssvneorroawafnnngtgiihannmggsoffrturoanomnmtdsa00or..0df0p2t2henenaggs/k/tmmoaLcLrtketoaos5o5cl0u0otuinnorggnsi!mmiwnLLtaos5u0smedL tto(onhforifiotmtuttihghnheeazdld)eoawrttoaaedrffueoorrriacnengaaacclythhzheeaadnnia.atiyliAytntoegq..upLLraooodcwwreaostorsic.r,hh1iiCgg/axhhlcwppuoeoliiiangnttthisstnegwwdtoeh,rreceosatddliaibisnsraaadbbtailloerenddd cttcouoornmmvcoeeeoneotttfrtmmahoteetitoshhntooasddnudccsraritirtnoedgrtraipah.e.eaTTpkhheoeaadrkdeaaatataraceowwauoencrrtooesunwnnotoatstsffaoournrsccdeeodtddhe: resutant calbaton through zero during resultant calibration curve confimed accuracy of eachcurve point the fitting process. Calculating the standard concentrations curve confirmed accuracy d each curve point. using the peak area counts and the F`Faoocrrcubbrooatcthhy.mmeMetethhtoohddossdoocffaanaianblrayalsytisisois,na, ceecaauccrhhacccuuyrrrvveeepqopuiiorninettmwweeanstssqquuoafannt1ti0itta0att:ee2dd5uu%ssii(nn1gg0tt0hh:ee3oo0vv%eerrfaaolrlll tcchaaelliiblborraawtteiioso!nncccuuurrrvvveeepaaonniddn)rreewvveiiereweweemddetffoorr oral analytes. Thecomeiaton coefficient r)wasgreater than 0.995forallanalytes. accuracy. Method calibration accuracy requirements of 100+25% (100+30% for the lowest for all analytes. The correlation coefficient (r) was greater than 0.995 for all analytes. curve point) were met 3A3c,22aibrSSatyyossnttesetmamndSSauruidwittaaabsbialiliittnyy aifouyrfmzeseattdhe begining oftheanalytical sequencteo demnsirate overall Asssytycassanttedleimabmrradsstuuidotietnaavibbsaiitltiaytiy.no.dnaTT(rnhRdeeSwDaaa)ccsccfeeoarppntptaaaelnynazcckeeeadccrrfreioitteucerrroiiatauimfonorertsosssyyasstpttteeehamrek bssaeuurgiettiaanabrndiilainityygoassonaaf mdmthppelrleeeatssneonaoftlfyieltoeincssastslmttsheheaaqncnurooeerrnreceaqequuotafaollldtteoeosms57%to%hnraesrneltraloaatrttiieveveqeouvaelratlol 2% RSD standard 2% RSD weremet deviation were met or all (RSD) for all aafnonarallypyteteeassk.. are counts or peak area ratio and retention time criteria of less than or equal to 3T3h.33e LLLiiammO sidittefooG iffneQQduuainanmtneittitthaaotdtiioEoTnnS-((6L-L0OO4QQ4.))1 is the lowest non-zero calbraion standard inthecurve that mea's TiblilnnhaeeenaakrsLrti.OtyyQaTannhaddes aaLdcceOccfGiiunrSreaadccayysinsrroeemcqqieuautithrreeoedmdmweeEintnThtstsSah-a8nen-d0ds4fafo4orm.r1pwwhihsiiactchnhhealtthlyhoesewiaaserrsaeetraaenccosoontuu-enzntdetssraoianrcreteahleaaibttTrlaaleebtaailossentt 6ttswwtbaiicecneeotdwhath.orodsseienoofthfehtheceuaarpvpperporthopapritriaamtteeeets blanks. The LOQs associated with the sample analysis are listed in the Table 6 below. TTaabbllee 66.. LLOOQQ LoangnL' | LoGnomLe LO~, ng/mL (1) LOQ, ng/rnL Ana~yte [oreaTomas T2001] PFBA [eros 1 om | ee | PFOA [oT res om | s 2m | PFBS [T oes om |os m | PFHS 11/18/14 Analysis 0.0250 0.0240 0.0250 0.0250 11t2[fl14 Analysis 2~00 1.92 2.00 2.00 PFOS 0.0232 I =85 () Adivcof2vnestppioedicohheLOrO. (i) A dilution factor of 2 was applied to the LOQ. 2) Aditonoct cf 100scpl a heLOG. (2) A dilution factor ef 100 was applied l:o the LOQ. D33u..r44ing CCthooennctotiuinrnsuueiinonfggthCCeaaalnlaiilbbytrriaacattliiosoennquence, several continuing caloraton verification samples (CCS)were rea`DsanuunaraiillnytygzszewetdehdtertooecccoobournnrasffcierikmmeotfttehthdhaabettyttahhnCeeianVliynstssitctrrauutlhmmsaeleemnqnteutrerteenssmcppeeoot,nnhsssoeeedvaeanarnacddcl ectthphoetenatiiinnnnciuttieailcnlrcgcatalecblrairbiliaarbtaoritafiootnin1oc0ncu0uvr%re2vvr2eeif5wicw'ea%ert.iroeenssttsiillal miinnpccleoonsnttr(roCollC. VAAlslll) rrweeepprooerrtteedd results were bracketed by CCVs that met method acceptance criteria of 100%_+25%. 3T3h.55reetyBBplleaasnonfkkssbienkswere preparedandanalyzed wih the samples: methodisalvent barks, ediip banks, and Ts``ashmamremeppelitintnyhggpoeeesqqduuoiiifppsbmbmlleoaeannnlntktksvbsblwlweaaenennkrrksetse..purEEesaapeccadhhrbetlobdaldaanennktkderrreaemsnsiuaunlllettyzwtwehaaedssLwrrOeietvhvQifieteohwwreeeeddsaaacamnhndpaleuunsssa:eelddmyt.toeotheeovvdaal/lsuuoaalttveeenmmteetbtlrhaoonddkspp,eefrireffooldrrm/mtraaipnnccbee.la.nTkThshe,e,and method!solvent blanks were used to determine the LOQ for each analyte. 33663300..00223355 Pace TCE PAGE 7 OF 34 33MM_MMNNO011559966118844 3M ENVIRONMENTAL LABORA TORY REPORT NO IS01I-0f-,.03-18 826 SLDavCOcMoImSToIsSpetoessn nyrricn co 3.6 Lab Control Spikes (LCSs} Low, mid, and high lab control spikes were prepared for the target analytes and analyzed in triplicate. LCSs bE Rt gen prepared for internal standard calibration analysis were prepared by spiking known amounts of the analytes into 10 B EE E E era T mL of laboratory reagent water to produce the desired concentration. The LCSs were then diluted in the same manner as the samples. LCSs prepared for externa standard calibration analysis were prepared by spiking known C ER n amounts of the analytes into 1.0 mL of 18boratory reagent water and 9.0 mL of methanol to produce the desired concentration. Method ETS-8-044.1 states that the average recovery of LCSs at each spiking level must be within EET 80%=120% with a RSD _<20%. All LCS samples met criteria. eee een eth er All LCS samples were used in the determination of the analytical method uncertainty in section 3,7 of the report. a The following calculations were used to generate data in Table 7. I == LCS Percent Reco',~-ry Calculated Concentrat ion, 100% SpiNe Concentrat ion I LCS% RSD standard de~,4ation LCS re~icates . 100% average LCG recovery Table 7, Laboratory Control Spike Results, ETS-8-044.1 hl[e~nal s[a~dard calibration Z| l| Analyzed 11/18f14 I = E E E LabID LCS-141118-I LCS-141118-2 Erosamries ES or orT s ow E | 5ow ] [2w1 LCS-141118-3 [Avongeesmso| -- -- ovoweaww 1 ews Averase + %RSD Spiked ing Concentration (ngtmL) 0.198 0.198 0.198 PFBA Calculated Concentration (ng/mL) 0.18I 0.172 0.187 91.0% 4.3% y %Recovery 91.6 86.8 94.5 PFOA (Linear + Branched) Spiked | Concentration (nglmL) Calculated ingen) Concentration (nglrnL) 0.190 0.190 0190 0.189 0.184 0.191 98.6% 1.8% %Reeove~ 99.2 100 LCS-141118-4 9.91 9.72 98,1 9.50 8.90 93,6 [Avesgerwmso| Lc a11188 LC8-141118-5 LCS-141118-6 Average + %RSD -- ssowsossw ao 06 9.91 9.81 9.91 9.63 98.0% _+ 0.92% 98.9 o9r7s.1 1 wmeseesw | 9.50 8.97 94.4 99,8500 l 883.855 9933.22 93.7% _+0.65% LCS-141118-7 157 149 94.9 150 126 83.8 LCS=141118-8 157 144 91.7 150 127 84.5 Cemgesnasn| mmiaam | emer LCS-141118-9 Average _+ %RSD 157 142 92.~% 4- 2.3% 90,8 i 50 124 83.7% 4-0.96% 82,9 33663300..00223366 reese PAGE 8 OF 34 3M MN01596185 REPORTRO 501 0150.15 3M ENWRONMENTAL LABORA TORY REPORT NO IS01I-0f-,,03-18 TTaabbllee 77ccoonntitinnuusedd., LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuultltss.. EE ETS-8-044.1 Internal standard min calibration Pe Analyzed 11/18/14 PFB8 Lab ID sama LCS-141118-1 weno LCS--141118.-2 Spiked Concentration og(ngtmL) ore0.198 ore0.198 Calct~lated Concentration pr(ng/rnL) Darr0.211 oz0,220 o %F~ecovery 107 111 [Average +uso | Hons2in LCS-141118-3 0,198 0,220 111 Average _+ %RS~3 110% 4. 2.1% Les iiet we wz LCS=141118-4 9.92 10.2 102 wsres sx 03 LCS-141118-5 9.92 10=3 104 pretyines om 02 [Avosgoswmso| ---- oweesme LCS=141118=6 9.92 10.2 102 Average _+ %RSD 103% _+ 1.1% Sphed | Spiked Concmnrston | Concentration ing) (ng/mL) ows | 0.I98 ose | 0.198 PFHS Coles Calc~llated Canconesion Concentration pe(nglmL) azn0.21"1 ome0,208 co %Recovery or107 "105 ema 0.198 0,207 104 t05% 4- 1o5% wm] ez ws 9.92 9.21 92.8 wm | we ss 9,92 9.48 95=5 om 01 a6 1 eeernts | 9.92 9.18 93.6% _ 1.7/8 92.6 LCS-141118-7 157 155 99.0 LCS=141118-8 157 148 94.3 [aversgo+ wrso | LCS-141118-9 Average _+ %RSD 157 sens147 95.6% 3o1% 93.4 Ee ETS-8-044.1 Internal standard min calibration x rans Analyzed 1 II18/14 PFS(Linear+ Branched PFOS (Linear + Branched) Spe Spiked Consanenion Concentration Calculated Concentration Lab ID ~ 57 153 97=6 157 147 93.6 oaona2en 157 147 94.9% 2.4% 93.6 LCS=141118-1 0184 0.176 95.8 LCS-141118-2 E ses uies EE sito = LCS-141118-3 [Ave | --sgsooms erewn mso| Average :J: %RSD 0.184 0.184 0,176 0.180 96.5% 1.4% 95,6 98.1 LCS-141118-4 9.20 8.40 91.3 LCS-141118-5 Eweosnuines |= sm m]x=e LCS-1411 ! 8-6 [Awo--g-- oeovev wcam wn so|| Average _+ %RSD 9.20 9.20 8.64 8.18 91.4% + 2.8% 94.0 88.9 LCS=141118-7 145 133 92.0 E frotiA ives EAEE = LCS-141118-8 145 LCS=141118=9 145 124 85,3 126 86,6 .. ~_~_~....-+_.~.~.................................... ~._~_..~..~~(~_................................. 33663300..00223377 Prceacess PAGE 9 OF 34 3M_MNO15%6185 3M MN01596186 TTaabbllee 77 ccoonnttiinnuusedd., LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuultltss.. EE ETS-8-044.1 Internal standard min calibration Pe Analyzed 11/18f14 I=C3-PFBA Lab ID same LCS-141118-1 wens LCS-141118-2 roti LCS-141118-3 0] Spiked Concentration (ng/mL) Q 197 0.197 0.197 Calculated Concentration pind (ng/mL) ozs0.208 ozs0=215 ozs0=218 < %Recovery os105 wo109 10110 Spikad Concentration (ng/raL) ors0.198 orm0,198 ous0,198 Average _+ %RSD 11)8% _+ 2.t% LCS=141118-4 1,97 LCS-141118-5 wees io LCS-141118-6 [avesgoswmso| Average _+ %R~D 1.97 1.97 i .94 1.90 sooner ~ .94 98,0% _~ 1,2% 98, 7 1.98 96.6 sae | 98.6 1.98 1.98 REPORTRO 501 0150.15 3M ENVIRONMENTAL LABORA TORY REPORT NO IS01I-0f-,.03-18 "cceron 13C4-PFOA Calculated Concentration pre(ngtmL) oz0.207 ozo0=210 0220=212 I66% _+ &94% 1.96 1.90 ssn aime 1.92 97,3% _+ 1,7% co %Recovery 05105 wr106 107 99.1 96.0 96.7 ETS-8-044,1 B=rane Internal standard calibration Analyzed 11/18/14 Lab ID Spiked Concentration (nglmL) "coors ~SC4-PFOS Calculated Concentration (ng/mL) %Recovery LCS-141118-1 0.189 0.188 99.5 LCS-141118-2 0,189 0.196 104 [Awo | sgetos meraw ow mso| LCS-141118-3 0,189 0.212 112 Average + %RSD 11}5% + 6,1}% LCS-1411184 ~ .90 1,89 99.6 E wes Hse LCS-141118-5 LCS-141118-6 I 90 ~ .90 i .89 i .85 9 7 97.2 Average _+ %RSD 98.8% _ 1.4% 33663300..00223388 Face ocr PAGE 1 O OF 34 3M_MNO15%6187 3M MN01596187 REPORTRO 501 0150.15 3M ENVIRONMENTAL LABORA TORY REPORT NO IS01I-0f-,,03-18 TTaabbllee 77 ccoonnttiinnuusedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuulJttss.. Tsao ETS-8-044.1 External standard fries calibration is Analyzed 11/20f14 PFBA Lab ID sara LCS-141120-1 wen02 LCS--141120.-2 Spiked Concentration og(nglnqL) ER20,2 m220.2 prCalct~lated Concentration (ng/rnL) 21.6 21.0 : %F~ecovery "or107 or104 a PFOA (Linear Branched) Sphed | Coes Spiked Comentaton | Comonbaion Concentration ing) pe (nglmL) Calc~Jlated Concentration (ngimL) we | ms 19.9 w | wo 19.9 19,3 19.0 . %Recovery ans97.1 os95.3 [average+ uso] LCS-14"1120-3 Average _+ %RSD Test LCS=141120-4 wsar0s LCS-141120-5 wears | mvemgoswesol LCS-141120-6 Average _+ %RSD Tos anor LCS-141120-7 20.2 w@502 @502 wo --502 wo4040 LCS-141120-8 wsraron poy LCS-141120-9 [awesgoevmso| Average _+ %RSD 4040 4040 Tsao ETS-8-044= 1 eon External standard calibration ota19=9 103% + 4.1% 488 487 io saenzzww 505 98.4% + 2.3% 4I 60 4080 ao4090 wwpweswn 102% 4. 1.1% wea 98.6 19=9 18.7 9&8% 4. 1o8% 94= I wr ww] 97.1 496 480 96.8 wo wo | aw 97.0 496 481 96.9 on we | aw | emesis | 101 496 493 99.4 97.7% + 1.5/8 wo | eo Sas, 103 3980 3620 90=8 101 3980 3460 86.9 sw | ss 101 3980 3600 90.4 wanes] 89.4% _ 2.4% Analyzed 11/20/14 PFBS PFHS Lab ID Spiked Concentration {nBlrnL) Calculated Concentration (ng/rnL) /~eoove~ Spiked Concentration {n~ImL) Calculated Concentration {n11m L) %Recove~ LCS-141120-I wsrra0z 22 or a | me LCS-141120-2 Bre esomn [wn 20 ]x6.) = mo |=ms 5 [ mversgoswesol LCS-141120-3 Average + %RSD Ts ariaot = ws 0 wm LCS-141120-4 freee - - = wo | os LCS-141120-5 wees pe @ wo | eu [Avegoswmsol LCS-141120-6 Average _+ %RSD Tsar on so To ww | wo = LCS-141120-7 weirs m0 a0 3 ww | eo 0 LCS-141120-8 19.8 19.8 --19.8 494 4.94 494 3970 3970 21.3 21.2 erwsoswe 21.0 107% _+ 093% 495 492 owes503 101% 4- 1.3% 4090 3940 108 20.0 22.0 110 107 2&0 20.6 103 1 esweasw 106 20.0 20.6 103 105% -+ 3.8% 100 498 99.6 498 498 99.9 512 103 1 essen 102 498 513 103 102% _+ 1.8% 103 4000 4480 112 99.3 4000 4400 110 [Average+umso | LCS-14"1120-9 Average + %RSD 3970 ors20n 3960 101% 4. 2.0% 997 Ts ton 4000 4470 tt 1% 4- 1.0% "112 33663300..00223399 Facer PAGE 11 OF 34 3M_MNO15%6185 3M MN01596188 TTaabbllee 77 ccoonnttiinnuusedd., LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReessuultltss.. Tsao ETS-8-044.1 External standard fries calibration Sry 12018 Analyzed 11/20f14 . PFOS (Linear Branched) oe |e [EE |ap | Lab ID esa 09 "06. wr LCS-141120-1 wsnmz 1 2 oz LCS-141120-2 fratiteeey 99 5 mo LCS-141120-3 Spiked Concentration (ng~'raL) 19.9 19.9 19.9 Calculated Concentration (ng/rnL) 18.6 18=2 15=5 %F~ecovery 83.7 81.2 78.0 Average _+ %RSD 8t LCS=1411204 496 442 89,1 LCS-141120-5 496 wees pes - se LCS-141120-6 496 443 88.7 469 94.6 [Ave-- og --osromv zaem n sol| Average _+ %RSD 90.8% + 3.6% Wenuiaor 00 wo LCS-141120-7 toss 000 0 we LCS=141120-8 3980 3980 3990 3930 100 98.6 wenn 00 0 a [Avo | oge eimsses rnmso| LCS-141120-9 Average _+ %RSD 3980 3940 99.1% 0.76% 98.8 REPORTRO 501 0150.15 3M ENWRONMENTAL LABORA TORY REPORT NO IS01I-0f-,,03-18 ETS-8-944.1 B= vias External standard calibration Analyzed 11/20/14 Lab ID fol Spiked Concentration ln~/mL) ol 13C~-PFBA Calculated Concentration (ng~r~Ll co %Recove~ Spiked Concentration "coro 13C~=PFOA ognt) Calculated Concentration %Recever~ LCS-141120-1 19.9 22.8 115 19.9 23.2 117 Ells] LCS=141120-2 19,9 23.2 117 19,9 23,4 117 LCS-141120=3 19.9 22.6 1!3 19.9 22.9 115 Average _+ %RSD 115% 1.7% 116% 1 LCS-141120-4 199 216 109 LCS-141120-5 199 215 108 LCS-141120-6 199 215 108 Average 4- %RSD 108% + 0.53% "199 22 1 111 199 213 107 199 209 105 108% 2.8% 33663300..00224400 Face rece PAGE 12 OF 34 3M_MNO15%6189 3M MN01596189 Tabla 7 continued. Laboratory Control Spike Results. Table 7 continued, Laboratory Control Spike Results. Ese ETS-8-044.1 External standard en calibration neyo 2004 Analyzed 11/20/14 IZC4=PFO8 Spiked Calculated Concentration Concentration Lab ID tes arm ar LCS-141120-1 wowma | or LCS-141120-2 Lesions 0 LCS-141120-3 [aeo--g-- os "wiv ieamresol| Average _+ %RSD (nglmL) 19.1 ~9=1 i 9= 1 (ng/mL) 22=6 21.0 22.5 11 ~% _+ 4..0% %Recovery 118 140 118 LCS=141120-4 191 205 107 LCS-141120-5 191 201 105 E icsrerne EE wo LCS-141120-6 191 204 107 Caveo --g--o"osmev ervme sol| Average _+ %RSD 106% + 1,1% REPORTING 8017003018 3M ENWRONMENTAL LABORA TORY REPORT NO IS01I=0f-,,03-18 An33a.l77yticAAalnnuanalclyeytrttiiacciaantllyMMfseebttahhsoeodddonUUninctceoerrcrttaaaliinnOCttydyata thal is coil charted and used to evaluate method accuracy Aaafnnnoddarlpypertrioecsccaeiitlssiuooonfnn.ca.ecrTTctuhahrieenatmcmyyeeiisrthheboosaddusteuusdn(connenr%tcha)iisnotetoybiriiascrsaicclaatnQllccefCuuoadllrdaaatttieetnaddefnftGohollaCltoot wwsisiaiynmncgpgolnEeEtsTrTo.SSl--c11Fh2o2a:r-r00tme11ed22t..a2h2n.oddTTunhEseeTeSsds-t0aato-nn0ded4av4rard.lu,ddaeeitveveiiaammttoiieoostnnhtoiirssdecccaaaecllncccutuufraaattyceeydd 2,fGQowCCrhtihssceaahmmspcepiotleerossfeawwscepecrroueenrauduscsseyedd0.r..esTTuchhloteesrefe(xidnxppea%anncn)dedoeeblddetavueuinlnnecocedferrt9fotaa5rii%nnthttyyeiissQCacacslcuaulmlatpteeledds.bbyyFmmoruumlltiepitlyhlonnygdg he standard deviation ETS-8-044.1, the most the standard deviation by afactorof recent fifty by a factor of 2, which corresponds to a confidence level of 95%. TTaabbllee 88.. AAnnaallyyttiiccaall MMeetthhoodd UUnncceertrtaaiinnttyy.. [ema| wens [6 |m wwe | PFBA Calibration In[ernal Standard Deviation (%) 6.78 Method Uncertainty _+14% [ern1 owns Tv [ume | PFOA Internal 10.8 _+22% [ems|wen | ver wen | PFBS Internal 7.91 _+16% [ems | wma[e [an me | PFHS Internal 6.13 +12% [eros| www| sa | see | PFOS Internal 824 +16% [ema | oon | wer [aw | PFBA External 12.1 +24% [eraTown rm awe | PFOA External 7.23 _+14% [ores 1 owen | as | seex | PFBS External 4,31 _+8.6% [ems 1 emma | oa [ame | PFHS External 5.39 -+11% CeresTT own vss | awe] PFOS External 7,55 15% 3`3t..8a8rgetFFiaienealllddyteMMafatetrdriixmxaSStppsiipkkieesssa((mFFpMMlSSo))was oli at each samping pinto very that te analytical meth! ASiissaatpamappprlgplieelcicta0ababln:elaelcyffootrerntfabhieneeldeccoomstllaeeptccretitxeedddsbpmmyikaaetthrasoixa..mabFFpoieleerlddawlmmacasyattcrwioixillhsespcp1tihke0eedssGaaatrlreeoaggcaeehnnnseearyrmaatspelldeinrbbgyypraacd0d4ddnitiSnnthoggFvaaIeNmmriegfeyaaSstshuauarrtmeetdhdeevvcoaoolnkunaumtlmyaeetoincofrafslffifmeoeleddthod ssSapaaapmmrmopppelleeritccaoootlelaleesccctotpoinonent.a.ilneFFevieerellsddpFimmikeasadltrirmbxyasstprphiiiekkeelsksabmmoesurarstettocbbroyeevaweatrittihlleeetsashswse!t i55ta00nr%g%emootfefat(tnhrhaeeolydaatennasaaclcyypetreeipotcrcaootonnncccseeehnnripttrptaaintteigoonnsoattfoom1bbp0el0eccoco3ron0sns%itidadceeinrroeeerddnsaaffonnrthat a"a"unpUnapknlrnoykoptwrueiantot"feccesoorpmmoikpspeotonl.neeevnneTttlh.ssoinFnsieatbhlndeeasmsraadammtsrpipxluleesspemaidkaleftorrrrixetcdhdoaoovnenporroiteetpsssairwgcanittaihifiinocnnatmnoytelyhthienortdelerafdrecercemewpwatiahtxhnctnshepeeickppriirtneergrpiSaaeroaupftino1an0s0aar_nn+cdd3ao0aar%ninaaalcnoloyyensdnfiisremforftehtFhanoetce mmamanataaetleriyirtieaaslslspsoiccfeoisanmtaepmrrreoipssept.rrdooTossfhefbaerboiotsdoththdanilninndeseaaoarrdcrastanonunddse4bbdrroaaffonnircchtshheeeddreppisosrreootpmm.aaerrarsstioffonorr PFOS and of the field PFOS and only1a Inoa soomr ePFOrA. matrix spiking solutions contained only the linear isomer for PFOA. Fieldreference Field matrix spikes are presented in section 4 of this report. 33663300..00224411 censors PAGE 13 OF 34 3M_MNO15%6190 3M MN01596190 REPORTRO 501 0150.15 3M ENWRONMENTAL LABORA TORY REPORT NO IS01I-0%,,03-18 S1InCaa,dPddFitiiBonAtttoSotCotaaPrrggnFeetOt aaAnn,aallyyattneedffi"leelCddemmPaFaltOrieSx,ssppwiikkheecss,h, 0ewaaoccrhhe ssaaadmmdpepldleeacctoonnntaonimneiedndaasltacboblrlecosisncotltrooappteeonSsuourfrgo0.ga1atnerreeccgoovtvoeerrsyyo lspopiciktkeess of of s`5lsasCma>CpmPloeFPBbbAooFtt,tflleSessBC"gppCr-rAiPi.ooFrr.OAtoPoAF,ssNaOaammnApdplWl~eeearccCeoo4lls-llPeeeccFlttOiieooScnn,toowrerh0daaicrttheaapwrnneeoosmrmeeiinrnataadplldocceroodunncaccrteeonacn~antaroatbimtooinixnoyaofnllfcc11onanngcgcis/emm.nLLtrfaTflothiololaonwwCioiennfggd0s.a1sabamnmepgepl/mdleeLPccotoFollllOeescScettiliewooncan.t.s TThhee. sse~oearllCteo3occ-tirPeoiFdodafB0tAo1a0rreno0pdp3rr~ee0assC%oe4nn-tctPotthFnheefOiAppmoetwrrhflealuurtoec"rruosonsesukluelnffcoootnewridncc"taaocccirioddesmsp..preoSSsnueuranrrrntoospggeaailrntfeeltuhMmooaraotstciraiaxmxrpbsslpopoixkyimelarictrerecaicoxcoviddevrseoi.rneieosTsthwwiestigt~hh3fiinCnc4amm-1aneattbthhyeooleddidnaaPcfcFoceOoeropSttawawnniacchseethe prreepooratraton andanalysis of criteria of 1004-30% confirm preparation and analysis of the analytesof that "unknown" the analytes of intrest. Thesurogatespikerecoreries are incuded components in the sample matrix do not significantly interest. The surrogate spike recoveries are included insection 4ofths interfere with the in section 4 of this report. I FASReoorry CSI Concent of FNS Aver Coreetrtion Fill Spl & Fed Spi Dip) oo] FM SRecovery = (Sanple Coacentratio~ of FMS- Averege Concentraion : Field Smnple & Field Sample Dt:p.), 100%i Spike Connon Spike Concentration TTaabbllee 99., FFiieelldd MMaattrriixx SSppiikkee CCoonncecnetnrtaratitioonnss. le Location [woMWr07,pPWw0o9 sanad ePViV1o0 fos MW13 Pawo MW110 [omvemowroe MW16 and MW105 [ovo wviotaosiwios MW101, MW104, and MW108 [EoEmvgmowran MWl 2 and MW14R Tr~p Blank Final Concentration (ngfmL) eT] Spike Level PFBA PFOA PFBS PFHS PFOS 1 eFwMsS |o2.w02 | ve1.99 | ve1 98 | o2o.00o| se1.99 | Tews [vor|ooo[ow| 00]oom | FMS 10.1 9.96 9.92 10.0 9.96 Tous [200| woo | es|ano |v0| FMS 20.2 19.9 19.8 20.0 19.9 [ous | sos| uss | aon|so|aon| FMS 50.5 49.8 49.6 50.0 49.8 | ws |cor|wo | 2| wo|ees | FMS 101 99.6 99.2 100 99.6 | ows |e| wo |ow | ow | aw | FMS 252 249 248 251 249 [Thon TorTos[wa| wo | wos| Low High 2.02 101 1.99 99.6 1.98 99.2 2.00 100 1.99 99.6 44 DDaattaa SSuummmmaarryy aanndd DDiissccuussssiioonn TtThhhoeoTttraapbblleBosisnbbke.lloowwEasscuuhmmfmmsabaroriizpzerotthvhiedsseaasmmtphpleleeavrreeessruuallgttssoacrnovdnclfeiendtldrammtaiatortnriixxansspdpiikrkeeorrerecacoovauetreiperosirfofocosrornsstaammdpiplaliirnnoggnllcoooccaa(ttiKiooRnnPssDaa)ss owwfeeltlllhaeass tsrsheaaelmmapTtplrvlieeep daaBinnlfaddfnesskraa.emnmcEppela(leoc%hpdRtuiPapbDclilc)eaavpt.aerlo.uveRRideseesssuaulrtltehtsseraaoanruvddnedraaeavvdgeeterroaacwggoeenocvvseaalniluutgreeansstiaoaarnnreetarrnogoduuunntrhddeeeedd.rettolBoaetttihcvhraereeuepeseessriicggoenfninirfftioicdcuaaninfndftteinfrfieggin,rucerveesas.l(.u%ePPRsevePrarccDree)ynnsottif gthhet relative difference (%RPD) values are rounded to two significant figures. Because of rounding, values fdoemmtoosnesitshread 1htehemertahwoadtaa.pFoireolpdrmiaaerfxo spheiegsmeenetmnagit.hemethodacceptancecreaof 230%, from those listed in the raw data. Field matrix spikes meeting the method acceptance criteria of_+30%, vary slightly demonstrate that the method is appropriate for the given matrix. hFFooerrtSthhuoossreegaanenaalflyyettceeossvwwehrhyeeSrreeAtthhEee ffsieilsdwemmraalatrrixxsssepptiikk0ee l2eev5ve5el8l 5ww5aasMs nneootNaappp=prcroorpprrariicaayttee. aassAlccooSmmIppTaaOrreeGddAftoretthchoeevssearaymmSptlieanccdooannorcetenniatrnrada.ttioonn,, id main spike recoveries met metrod acceptance criteria (where appicabl). the surrogate recovery standards were used to assess method accuracy. All surrogate field matrix spike recoveries met method acceptance criteria (where appiicaNe). recovery standards and 33663300..00224422 Face worn PAGE 14 OF 34 IM_MND1596191 3M MN01596191 3M EHVIRONMENTAL I...4BORA TORY REPORT NO, tS011-01-03-!8 e E EEE TT Twe] ISO11-01-03-18-001 ISO11=01-03-18-002 CGM N-GW-MW07-0-141028 CGM N-GW-MW87-DB-141028 PFBA 3.15 NA 2.87 NA PFOA 0.615 NA 0547 NA ISO! 1-01-03-18-003 CGMN-GW-MW07-FMS-141028 4.95 96.0 2.50 98.3 Average Concentration (n[jlmL) %RPD 3.1}1 m~J;mL -+ 9.3% 1~.581 n~mL 12% EEELee TT ee we] 3M LIMS ID ISQI 1-01-93-18-001 ISO11-01-03-18-002 Description CGIV N-GW-MW07-0-141028 CGMN-GW-MW07-DB-141028 PFIB~ Concentration (ng/mL) %Recovery Concentratio=~ (ngimL) %Recevery Concentration lngtmL) 0.0762 NA 0.051 " NA 0194 NA 0.0638 NA 0.0495 NA 0.187 NA ISOi 1-01-03-18-003 CGM N-GW-MW07-FMS-14! 028 ~.98 96.3 2.00 97.5 ~ .99 90.3 Average Co~ce~[r~on (eghr~L) ~ %RPD 0.0701 ng/mL ~ 18% 0.0503 ng~'n~L 3,2% 0.191 ~#nL ~ 3.7% [aEme Eower T|ToreIm [sTnr |stony| 3M LIMSID ISOq 1 01-03-'18 001 ISO! 1-01-03-18-002 Description CGMN GW MW0~0 141028 CGM N.GW-MW07- DB. 141028 | o ~C~-PFOS %Reeevery 120 103 %Recovery 116 97.3 %Recovery 115 108 I SOI 1-01-03-18-003 CGIV N-GW-MW07-FMS-141028 103 103 102 Average Receve~'y (%) ~ %RSD 108% = 9.1% 105% 4- 9.1% 108% Sim en 0ky a clk. NA = Not Applicablo. Samples were diluted 1:1 and analyzed by internal standard calibratioll= PAGE t 5 OF 2,4 3M_MN01596192 33663300..00224433 Tat 1. comman41a50 oJ e eera] 3M LIMSID ISOd 1-01-03-18-094 hla ISOI 1-01 ~&18-005 I~! 1 01 ~18 006 Description CGIV N-GW-MW 12-0-i 41030 CGMN-GW-MW12-DB-141030 CGMN GW MWI~FMS 141030 PFBA 126 NA 128 NA 367 95.4 PFOA 345 NA 350 NA 576 91.8 3M EHVIRONMENTAL 1_4BORA TORY REPORT NO, tS011-01-03-!8 CeT m Tee [ew] 127 ng#mL 4-1,PI~ PFBS 348 ngJmL 4-1,4% PFHS PFOS Thbt gdtt 113 ISO11-01-03-18-004 ~),~184)05 ~18-006 Description CGM N-GW-MW12-0-141030 CG~i) N-GW-MW12-DB-'14! 030 CGMN-GW-MW12-FMS-141030 Conoentration !ng/mL! 45.8 46 4 292 %Recovery NA NA 99.2 Concentration 7.79 7 76 250 NA NA 96.5 Concentration (l'~J/i~LJ 92.0 93 0 322 %Recovery NA NA 92.2 Tem[wea] ew] 46.1 nglmL .+_ '1.3% 7~78 ng]mL .+_ 8.39% ~'~C~-PFBA ~C.:PFOA "C4-PFOS 92..~ r~j/~L _+ 1.1% 3M LIMS ID Desoription %Reoovery %Recovery %Reoo~ery ci IS!! 1-01-03-1 ISO11-01-03-18-005 ISO1 "1-01-0[~18-006 loroCGM N-GW-f~W12-0-! 41030 CGMN-GW-MW12-DB-141030 CGMN-GW-MW12-FMS-14" 030 eotz118 113 !13 111 109 115 101 97.7 97.4 ..............................................A_z~_ra.~_e....~,_~z~_~z._(~/~)_-+. ._~/~B_s..u_.............................................. ......!..!_01~_-+...7_:~"_{~.........J.fT~(~_-+...&4~....... re it 10 yt ce mc ken, NA = Not Applicable Samples were diluted 1 :I~X) and analyzed by externa~ sb3ndai,d calibration. PAGE t 6 OF 2,4 sw morsstsa 3M_MN01596193 33663300..00224444 Toe2. COR ws Table 12. CGMN GW MW13 141028 ee3M LIMS ID ISOd 1-C1-03-18-007 tS ISOI 1-01 ~&18-008 I~! 1 01 ~18 009 tt Description CGIV N-GW-MW 13-0-i 41028 CGMN-GW-MW13-DB-141028 CGMN GW MWI~FMS 141028 9.52 9.76 !94 PFBA PFOA lt NA NA 96.6 9.76 10,3 190 rlNA NA 90.1 3M EHVIRONMENTAL LABORATORY REPORT NO, tS011-01-03-16 CC Tm 9.64 n~rnL _ 2.5% PFBS mT] l&0 ng/rnL _~ 5.4% PFHS PFOS Th i 31Vl LiMS ID ISO11-01-03-18-007 IS()d 1-014"),~ 18-6~')8 I~I 1-01~&18-009 Description CGM N-GW-MW13-0-141028 CGI~iI N-GW-MW13-DB-14! 028 CGMN-GW-MW13-FMS-141028 totaTal Con.entration !ng/mL! .07 10 "~0.9 %Recevery NA NA 98.9 Concentration 0.712 0 727 1010 NA NA 92.8 Concentration 4.83 4 ~:~ ~4.0 NA NA 91 .~ CC Tm[oom oem] !.09 nglmL .+._ 2.8% ~C~-PFBA ~C.-PFOA 0.720 ~g~mL 2.1% "'C.-PFOS &8~ r'~j/,~nL _+ 2.3% 3M UMS ID Description IS!! 1-01-03-18-007 ISO11 =01-03-18-008 ISOI "1-01-03-18-009 CGIV'N-GW-~W13-0-!41028 CGM N-GW-MW1 3-DB-141028 CGM N-GW-MW13-FMS-14" 028 .............................................. ~ ~...~_~. 1_ ~/&~.t4B~ O_ .............................................. re nt 1 rsstyme css. NA = Not ~pli~ble Samples were diluted 1:1 and analyzed by internal s~ndard calibration. %Recovery 104 99.0 101 %Recovery 99.8 103 102 %Recovery 103 99,9 198 3.~ItL-+..~..... PAGE'_ t 7 OF 2,,4 awmerseros 3M_MN01596194 33663300..00224455 A -------- Table 13. CGItItN GW MW14R 141029 ee oe 3M LIMS II) ISO! 1-01-03~18-010 SHEERS ISOI 1-0143~18-011 ISO!l 01 @~_~18 012 Description CGIV N-GW-MW 14R-0- !41029 CGM N-GW-MW14q:-DB-141029 CGMN GW MW14~: FMS 141029 PFBA 570 NA 569 NA 823 NC PFOA 355 NA 351 NA 597 98.0 3M EHVIRONMENTAL 1_4BORA TORY REPORT NO, tS011-01-03-!8 CC Tm Average Co=l~entration (nl~IraL) ~ %RPD 570 n~mL - 0.18% PFBS mT] 353 nglraL _ 1.1% PFHS PFOS BTi aboSlt 3M LiMSID ISO11-01-03-18-010 I~]! 1-014"],~ 18-0! 1 ISO11-01433-18-012 Description CGM N-GW-MW14R-0-141029 CGI~iI N-GW- MW 14R-DB-141029 CGM N-GW-MW14R-FMS-141029 Con.entration !ng/mL! %Recovery Concentration 38.7 NA 16.5 NA 37 4 NA 16 7 NA 282 98.4 273 102 Concentration (rig/i~LJ 85.2 80 O 318 %Recovery NA NA 94.5 CCeee]trTe Sm t [e orme,d octm] 3M MMS ID Description 38.1 ngimL .+_ 3.4% 16.6 ng/mL _+ t.2% ~sC4-PFOA %Recovery %Recovery i %Recovery 82.6 rl~j/,mL _+ 6.3% IS!! 1-01-03-18-0!0 CGMN-GW-MW14 R-0-141029 111 112 ! 09 ISO11=01-03-18-011 CGM N-GW-MW14R-DB-141029 109 108 i 108 ISO1 "1-01 ~03-18-012 CGM N-GW-~4W14 %FMS-141029 120 117 j ..............................................A_,~_ra~_e....P,_~z~_r~_(Y&-+...Y~ES.E.............................................. ..._!.!.~_/~_-+..5_,7B...... _...!1.:~"_t~.._+_ ,~._~ _.~...._1...!.0~!~__+...&.~.... ra NA = Not Applicable mn NC = Not Calculated; Spike level was less lhan 0.5x the endogenous sample Samples were diluted '1:1{X) and analyzed by external ~andard calibration PAGE t 8 OF 2*4 awmerses 3M_MN01596195 33663300..00224466 Toe. CoRR ws Table 14. CGMN GW MW16 141028 ee3M LIMS ID ISOd 1-[~1-03,-18-013 tS ISOI 1-0143&18-014 ISO! 1 01 ~_~18 015 tl Description CGIV N-GW-~,4W 16-0-i 41028 CGMN-GW-MW16-DB-141028 CGMN GW MW16FMS 141028 .'~2 39,6 842 PFBA PFOA le NA NA 89.7 737 77,9 11! DdNA NA 70.8 3M EHWRONMENTAL I...4BORA TORY REPORT NO, tS011-01-03-!8 CC Tw 38.9 ngtmL _~ 3.~% PFBS me] 75.8 nglraL _~ 5.4% PFHS PFOS i i 113 ISO11-01-03-18-013 4"],~ 18-0! 4 ~&18-015 Description CGM N-GW-MW16-0-141028 CGI~iI N-GW-MW1 ~[]B-'I 4f! 028 CGMN-GW-MWl@FMS-141028 lotht a Conoentretion !ng/mL! 32.8 35 0 78.4 %Recovery NA NA 89.7 Concentration 4.45 4 71 50.5 NA NA 91.8 Concentration (rig.,/~'nL) 41.7 43 4 83.1 %Recovery NA NA 81.4 Average Concentration (ngtmL) %RPD CCere]ter TSm tm[oe grme,id om] 3M LIMS ID Desoriptio~ 33.9 ng/mL ~ 6.5% #,.~8 ng/mL _+ &7% ~:~C4-PFOA %Reoovery %Reoovery i %Reoovery 4,2.6 r~j/~L _+ IS!! 1-01-03-18-0! 3 CG M N-GW-~W16-0-! 41028 102 103 ! 00 ISO11=01-03-18-014 CGM N-GW-MW16-DB-141028 102 101 i 101 ISO1 "1-01-0C~18-015 CGM N-GW-MW16-FMS-14" 028 104 100 i 103 ..............................................A_~_re.~_e....P,_~,~_r~._(?/~)_-+.._~/~B_s.O_.............................................. ...J.~.2_/~.!=:!.~...... _...!_0.!.~_4....-+_~._~(~_.,....J..~_!~_-+...~_.~.... re nt 1 rssty csr. NA = Not Applicable Samples were diluted 1:1 and analyzed by internal standard calibration. PAGE t 9 OF 2,4 awe 3M_MN01596196 33663300..00224477 CE 3M LIMS ID EET TL ISO~ 1-(:1-03-18-016 Description CGIV N-GW-MW101-0-141029 PFBA 4410 NA PFOA 252 NA ISOI 1-01-0~18-017 CGMN-GW-MW101-DB-141029 1400 NA 74,4 NA ISO!1 01 ~_~18 018 CGMN GW MW10! FMS 141029 4480 NC 172 97.6 Average Conaentration (n~lraL) -~ %RPD 1410 ng~mL 0.71% 74.8 nglmL -~ 1.1% 3M ENWRONMENTAL 1_4BORA TORY REPORT NO, tS011-01-03-!8 Ee 3~1 LIMS ID ISO11-01-03-18-016 I ~]d 1 -[~14"].~ 18-[] ! /' Description CGM N-GW-MW101-0-I 41029 CGI~iIN-GW-MW 101-DB- 141029 emsTews [es | PFBS PFHS Concentration !ng/mL! %Recovery Concentration 29.6 NA 460 NA Tir il 296 NA 443 NA PFOS Concentration Ing/mL} %Necove~ 165 NA 174 NA ISO11-01-03-18-018 CGMN-GW-MW101-FMS-141029 129 100 558 NO 259 89.9 Average Concentration (ngiraL) _+ %RPD 29.6 nglmL ~ 0.0% 4,~2 nglmL .+._ 3.8% 170 ~g~mL 5.3% EE TY EY | ~'~C~-PFBA ~C,-PFOA "C4-PFOS 3M LIM8 ID Description ISO! 1-01-03-18-0! 6 CGM N-GW-MW101-0-! 41029 EE rEEl E Tl IT I~I1-01-0~18-017 CGM N-GW-MW101-DB-141029 ~SO1 "1-01-0:~18-018 CGMN-GW-MW101-FMS-141029 SELES ia .............................................. ~...~_~~_ ~.!?/~k~..~/~B~D_.............................................. %Recovery 106 110 I{38 %Recovery 107 110 1{38 %Recovery !05 112 111 J.~f~_-+..~=~. . . . mime ean 7 NA = Not #~pli~ble NC = Not Cnlcu~L~d; Spike level was loss ~han 0.Sx the endogenous sample conce~7~atie~. Samples were dilut~ 1:109 and anai~ed by e~mal ~andard calibration PAGE 20 OF 2,4 3M_MN01596197 33663300..00224488 Tat te. com con 0 Table 16. CGMN GW MWI04 141D2g Joe leer] 3M LIltS ID ISO1 "1-01-03-18-019 cab EEE ISO! 1 01433 18 020 EY I~11 01-0~18 021 I)escripfJon CGM N-GW-MW104-0-141029 CGMN-GW-MWl~--DB-141029 CGMN GW MWI~ FMS 141029 PFBA 31 0 30,8 125 NA NA 93.2 PFOA 503 49,7 145 NA NA 95.4 3M ENWRONMENTAL LABORATORY REPORT NO, tS011-01-03-!8 CeT m Tee [ew] 38.9 ng/mL 4. 0.G5% 5G.0 n~lrnL -~ 1.2% PFHS PFOS IE 31Vl LiMS 113 I S!! 1 ..01 ..03.18.0! 9 LO11-01-03-'18-020 I SOI 1-01-03-18-021 Description CGM N-GW-MW104-0-I 41029 CGI~i)N-GW-MW 104-DB- 141029 CGIV N-GW-MW104-FMS-141029 sat Concentratiorl !ng/mL! 7. 73 7 7! 102 %Recovery NA NA 95.0 ld Concentration 5.81 6 67 03 NA NA 96.8 tesa Concentration (i'~JlJIIL) 176 ,i 77 271 %Recovery NA NA 94.9 Average Concentration (ngtraL) 4" %RPD Tem[wea] 7.72 ng~'raL 0.26% ew] 6.24 ng/~*t'~L _+ 14% 177 ng,~raL _+.. 0.~7% 3M LIMS ID Description %Recovery %Recovery %Recovery ie I SOq 1-01-03-18-0! 9 I SO11-01-03-18-020 I SOI 1-01-03-18-021 LanCGIV N-GW-MWI(YF0-! 41029 CGM N-GW-MW104-DB=141029 CGMN-GW-~4W104-FMS-141029 112 112 !11 117 119 114 115 115 113 ..............................................A_z~_ra.~_e....P,_~z~_~z._(~/~)_-+..._"/~B_s..u_.............................................. ......!..!A&~.&~t{~.........J..!.~f~_-+...~~.... re mt 0 tymce ken NA = Not Applicable Samples were diluted 1 : I~X) and analyzed by external st~3nda#d calibration. PAGE 2! OF 2,4 sw morsstsn 3M_MN01596198 33663300..00224499 3M ENVIRONMENTAL L4BORA TORY REPORTNO, tSOf l-Of-O3-f8 [------ Table 17, CGMN GW MWI05 141029 [T mCCe Tow [m ole [ee] 3M LIMS ID Description PFBA {ns/mL) %Reco,,-er~ PFOA (n~lr~L) %Recover~ I SQI 1-01-03-18-022 CGM N-GW-MW105-0-I 41029 466 NA 938 NA ISOI 1-01-03-18-023 CGIViN-GW-MW10b-DB-141829 ISO! 1-01-03-18-024 CGIV N-GW. MW105..F MS-141029 em EeT ][w 5E]LT 13m 2]1: Average Cou~centration (ng/mL) %RPD 47.0 NA ,94.3 46.3 ngtr~lL 4- 3.0% PFBS 91.8 NA 140 94.8 92.8 ngiraL 4- 2.2% wm] PFOS an 3M LIMS ID IS011-01-03-18-022 ISOI 1-01-03-18-023 ISO11-01-03-18-024 CGM N-GW-MW105-0-I 41029 CGM N-GW-MW105-DB-141029 CGM N-GW-MW105-FMS-141029 EEEEEE &88 4.13 53.2 NA NA 99.2 18.7 19.0 66.8 NA NA 95.9 73.9 73.0 117 NA NA 87.4 -- rr Average Co~central3on (n1lrnL) %RPD 4,01 ngtmL 1 &9 nglmL 4- 1 ~3C:~=PFBA IzC.-PFOA ~4~FOS 73.5 ngh~L 4-1.2% Ep EEoE serm [2m | 3~ LIMS ID ISO! 1-01-03-18-022 1O11=01-03-18-023 ISO11-01-0~18-024 Description CGMN GW MW105 0 141029 CGIVN GW MWI05 DB 141029 CGMN GW MWI~ FMS 141029 %Recover~ 111 115 112 %Recovery t08 112 112 %Recovery !10 111 ~11 Avenge Recev~ (%) ~ %RSD 112%_+1,9% t11%4-2.1% 111% 4- 0.~5% Sa0 10 weary cont vc cr NA - Not ~pli~ble Samples were dilut~ 1:1~ and ana~ by e~ernal standa~ calib~tion. PAGE 22 OF 2,4 I3MM__MMNNO10510569169199.9 33663300..00225500 Te5. Com ti Table 18. CGMN GW MWI08 141029 oe3M LIltS ID ISOI "1-01-03-18-025 Sone ~SO! 1 01 ~3 18 026 I~11 0~)~18 027 Description CGM N-GW-MWI~-0-141029 CGMN-GW-MWl~--DB-141029 CGMN GW MWI~ FMS 141029 PFBA 88 ! NA 85.9 NA 18! 93.1 PFOA 268 NA 267 NA 352 NC 3M EHVIRONMENTAL LABORATORY REPORTNO, tS0f1-01-03-~8 CC Tm 87.0 ngtmL 4- 2.5% PFBS me] 268 n~/mL - 0,37% PFHS PFOS IE 31Vl LiMS 113 I S!! 1-01-03.18.025 ISO11-014"~3-'18-026 I SOI 1-014:)3-18-027 RA R r rie drh t tt Description CGM N-GW-MW108-0-141029 CGI~iI N-GW-~v~W 108- DB- i 41029 CGIV N-GW-MW108--FMS-141029 Concentration !ng/mL! 23.0 22 4 115 %Recovery NA NA 93.0 Concentration 8.20 8 79 "07 NA NA 98.5 Concentration (ng,,/mL) 42.3 41 6 129 %Recovery NA NA 87.4 CC Average Concentration (ngtraL) _+ %RPD Tm[oom 22.7 ng/mL ~ 2.6% ~'~C~-PFBA ~C,-PFOA 8.~0 ng/mL _+ 6.9% "C4-PFOS 42.0 ng/mL _+. ~.7% 3M MMS ID Descriptio~ %Recovery %Recovery %Recovery Es| EEEaRde ISO1 1-01-03-~ 8-025 ISO11-01-03-18-026 ISOI 1-014~3-18-02f CGM N-GW-MW10~-0-! 41029 CGIV N-GW-MW108-DB-141029 CGIV N-GW-MW108-FMS-141029 ERE[=] 116 114 !16 112 110 138 110 110 11"1 .............................................. A_z~_ra.~_e....~,_~_o.z~_ ~z._(~/~)_ -+. ._~/~B_s..u_.............................................. a NA = Not Applicable a NC = Not Calculated; Spike level was less lhan 0.Sx th~ endogenous sample conce, ntration. J..!._z'f~_-+..~=~. . . . Samples were diluted 1:10{) and analyzed by extema~ standard calibration PAGE 23 OF ,',4 were 3M_MN01596200 33663300..00225511 [pe ------ Table 19. CGMN GW MW11[~ 141028 Joe leer] 3M LIltS IB ISOI "1-01-03-18-028 cia ISO! 1 01433 18 029 Description CGM N-GW-MW 110-0-141028 CGMN-GW-MW110-DB-141028 PFBA 290 NA 297 NA PFOA 415 NA 419 NA I~11 01-0~18 030 CGMN GW MW110 FMS 141028 314 NC 426 NC 3M ENVIRONMENTAL I...4BORA TORY REPORTNO, tSOf l-Of-O3-f8 CemT Tee Tem 294 ng,~mL - 2.4% PFBS 417 n~/mL - 0,96% PFHS PFOS nSESET 3M LiMS ID ISO! 1-01-03.18028 LOl 1-01-03-'18-029 ISO11-01-03-18-030 Description CGIVN-GW-MW110-0-141028 CGI~i)N-GW-MW 110-DB-141028 CGMN-GW-MW110-FMS-141028 Concentration !ng/mL! 57.9 75.5 %Recovery NA NC Concentration 23.4 23 6 43.0 NA NA 97.5 EE Concentration (ng/~'nL) 12.g ~28 29.8 %Recovery NA NA 85.1 ET ET Average Concentration (ngiraL) _+ %RPD ,~7.6 nglmL .+_ '1.0% ~C~-PFBA ~:~C4-PFOA 23.5 ng]raL .+_ 129 ng!mL _+ 038% ESaEin Elo ee [TE: ] x 3M LIMSID ISOq 1-01-03-18-028 ISO11-01-03-18-029 I ~I 1-01-03-18-030 Description CGMN-GW-MW110-0-! 41028 CGMN-GW-MW110-DB-141028 CGMN-GW-~4W110-FMS-141028 %Recovery 109 113 111 %Recovery 107 109 106 %Recovery !38 111 138 ..............................................A_z~_ra.~_e....P,_~z~_r~._(~/~)_-+.._~/~B_s..u_.............................................. ...J.!.~_/~_-+..!_.~3...... _ ...!_0.~"_/~....-+_~,.4_1~ _ .. J.~~f~_-+...~_.Z~.... anes NA = Not Applicable ETI TA NC = Not Calculated; Spike level wan less ~han 0.Sx th~ endogenous sample concemt~atian. Samples were diluted 1:1(]() and analyzed by extema~ standard calibration PAGE 24 OF 2,4 swmorssznn 3M_MN01596201 33663300..00225522 S-- Table 20. CGMN GW PW09 141030 eo 3M LIltS ID ISOI "1-01-03-18-031 Bi ttl ISO! 1 01 ~3 18 032 LT I~I 1 01-0~18 033 OescripfJon CGM N-GW-PW094%141030 CGMN-GW-~709DB-IA1030 CGMN GW ~t709 FMS 141030 PFBA 3.84 3.90 5.85 NA NA 98.0 PFOA 0.721 0.681 2.57 NA NA 93.8 3M ENVIRONMENTAL I...4BORA TORY REPORT NO. tS011-01-03-!6 CT Avenge Concentration {~I~L) ~ %RPD 3.87 ngtrnL _~ 1.~% PFBS Ta) 0,701 n~tmL ~ 5.7% PFHS PFOS IAntold d Bete 3M LiMS113 ISO! 1-01-03.18.031 I SO 11-01-03-'18-032 ISOI 1-01-03-18-033 Description CGIV N-GW- PW09-0-141030 CGIV N-GW- ~H09-DB-! ~ 10,'~') CGMN-GW-PW09-FMS-141030 Conoentration !ng/mL! 0.101 0~10 2.07 %Recovery NA NA 99.0 Conoentration 0.0560 0 0522 1.96 NA NA 95.3 Concentration (i'~JlJ'nL) 0.919 0 75? 2.68 %Recovery NA NA 92.5 CC Average Concentration (ngtmL) _+ %RPD Tew{maw 5.1 ~6 ng~mL &5% ~'C~=PFBA ~3C~-PFOA 0.5~141 ng/rnL .+_ 7.0% ~:~C~=PFOS 0.82,8 ngtmL 19% 3~1 LiMS 113 Description %Recovery %Recover~ Ei | ISO! 1-01 ..0&. 18.031 I SO I 1-01-0~'I 8-032 lSOI 1-01 ~18-033 te|E]IE CGM N-GW-PW09-0-141030 CG M N-GW- ~H0g-DB-f! ~ 10:~1 CGM N-GW-#709-FMS-141030 107 110 105 I03 102 102 pE ro rer pA oprssneonn Ave~e Recove~ (%) ~ %RSD NA = Not A#pli~ble Samples were dilu[ed 1:1 and analyzed by internal s~ndard calibration. 104% ~ 2.4%, 105%~4.22/~ %Necovery =] !03 !12 102 PAGE 25 OF 2,4 morse 3M_MN01596202 33663300..00225533 [ C p------ T Table 21. CGII~N GW PWI0 141036 PFBA PFOA 3M ENVIRONMENTAL I..=4BORA TORY REPORTNO, tSOf l-Of-O3-f8 EEEe = dt = Ee ISO11-01433-18-034 I SQq "1-01-03-18-035 ISO11 ..01 ..03.18.036 CGM N-GW-PW 10-0-141030 CGM N-GW-PW 10-FMS-141030 4.48 4.38 6.66 NA 0.379 NA NA 03~'2 NA NC 2.21 92.1 CTmw Avera~e Concentration (n[jlmL) - %RPD 4"43 nfJ;mL - 2.3% PFBS 0.376 n,~lm L -+ 1.9% 1 PFOS sanoEEIEE EEAE 31~ LIMIB 180! 1-0i-03-!8-034 1801%01*03-18-035 ISO11-0!-03-! 8-036 Description CG M N-GW- F~/ 10-0-1410,'~3 CGM N-GW-P~!v'10-DB-141030 CGM N-GW-~f~10-FMS-! 41030 Coacentration {ng]rnL) 0412 0,387 2.34 %Recovery NA NA 97.8 Concentration 00795 0.0759 1.99 NA NA 95.6 Concentration (ng/r~L} 0.345 0.329 2.i6 %Recovery NA NA 91.5 Ave[age Cor~en~ation (nga~JL) -+ %RPD 0.400 ngJraL + 6.3% 0.0777 n~rl~L 4.6% 0,337 ng~=nL + 4,7% CC cma [even|e~aC~vPFeOS|s E i EE THaEToHmTaEm 3M LIMS IB Description ISO11-01433-18-034 ISO! 1-01-03-18-035 I SOI 1-01-03-18-036 CGMN GW PW104) 141030 CGIV N.GW-F~710..DB.I 41030 CGM N-GW-~'V 10-FMS-"41030 Average Receve~ (%) =~ %RSD %Recovery 106 106 109 107% A 1.6% %Recovery 100 107 103 103% =~ 3,4% %Recovery 102 92.1 111 102% 9.3% NA = Not Applicablo, NC = Not CalculaLed; Spike level was less lhan 0.Sx [he endogenous saq~ple concen'a'ation, Samples were diluted 1:1 and analyzed by internal standard calibration. PAGE 26 OF 2,4 aw notseans 3M_MN01596203 33663300..00225544 [A ---------------- Table 22. CGMN GW MWI08-RB 141029 and TR~P BLANKS Te ee PFBA PFOA 31~1 LIltS D ISO1141-03-18-037 ISO! 1 01433 18 038 ISOI 1 01-0,~18 039 ISO! 1-01-03-18-040 CG M N-GW- RB-IVlW 108-04 41029 CG M N-GW--TRP-0--141028 CGMN GW TR~P LS 141028 CGMN-GW--TR~P-HS-141028 0.0385 <0.0250 2.00 89.7 NA NA 99.0 88.8 0.0319 <00240 1.84 94.0 NA NA 92.4 94.4 3M Eft~VIRONMENTAL L4BORA TORY REPORTNO, tSOf l-Of-O3J8 31Vl LIMS 113 IS!! 1-01-03.18037 LO11-01-03-18-0,8 ISOI 1-01-03-18-039 I S!! 1-014)3-18-040 CGMt,I-GW-RB-MW108-0-14102~ C(~1~,4 N- ~WJ RI p-0-141028 CG M N-GW--TRI P-LS--14 I028 CGMN-GW-TRIP-HS-141028 PFBS Concentration Ing/mL) %Recovery <0.0250 NA <0 0250 NA 1.91 96.3 92.4 93 1 PFHS Concentration [ngtmL) %Recoveq <0.0250 NA <0 0250 NA 1.82 98.4 91.0 98.4 PFOS Concentration (rig,,/~L) %Recovery 0.020 NA <0 0232 NA 1.69 84.8 91.8 922 lie 3M LIMS ID Jose IX~cription Loney [once| %Recovers/ I SO11-01-03-18-037 CGMN-GVV*RB-MW 108-0q 4 I029 106 EE ISO11-01-03-'18-038 I SO q 1-01-03-18-039 ISO11-01-03-18-040 si CGMN-GV'# 1 RIP-O-141028 CGMN-GW- 1RiP-LS-141028 CG M N-GW--TRI P-H S--14i028 NA = Not Applicable Samples were diluted 1:1 and analyzed by internal standard calibration 105 106 HHH 116 -- "~th lhe exception of lhe TRI P HS, which was diluted 1:100 and analyzed by external standard calibration PAGE 27 OF 2;4 I3MM__MMNNO011559966220044 33663300..00225555 pa 3M ENWRONMENTAL LABORATORY REPORT NO. IS011-01-03-18 55 CCoonncclluussiioonn Libor orksph are stad otic oss mtacasoyand gacioror Laboratory control spikes were used to determine the analytical method accuracy and precision for all es Tr ry onener ar dis Set Behn cee analytes. The accuracy and precision were then used to estimate the method uncertainty for the Tet a ova Grated ok ral mee stl or results. Field matrix spike recoveries demonstrated that the analytical method was appropriate for the in Bl i CaP Wer, RS TW Enea given sample matrix except where noted. Analysis was completed using 3M Environmental Laboratory Te 02 eofAra as Selof Peobsre Compt se method ETS--8-044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water LSI, Dre cin rayon Ana ets ar Tae ond 02310 by LC/MS/MS; Direct Injection Analysis". Analytical results are reported in Tables 1 and 10-22 of this enreport. 66 DDaatta !/ Sammpplle RReetteennttiioonn Mogieat: s gisi aleb asss t retpdotatbardby aongdoer) whoreing All remaining sample and associated project data (hardcopy and electronic) will be archived according to 3M Environmental Laboratory standard operating procedures. 77 AAttttaacchhmmeennttss F A TS, INE TTCH VAO135. W108 M115, PGEondPT--. ---- Appendix A: Target Analyte Historical Trend Data for Cottage Grove Monitoring Wells MW07, MW12, MW13, MW14R, MW16, MWl01, MWl04, MWI05, MW108, MW110, PW09, and PW10. 88 SSiignnaatturrees Diet!tally si#ned by Susan T. Wet on >. MIZE DN: c=US st=MN, I=S[ Patti, i~u=3~v TW WE Susan T. Wolf, 3M Principal Analytical Investigator Digi:ally signed by William K Reagan SC S-- DN: c=US st=MN, I=St Pat, I, ou=LaJoraior/ Director. ou=3M En~ir0nmerltal Laboratory - Wa FanPRD. SMEmrormaraTabaiey Tees order William K. Reagan, Ph.D., 3M Environmental Laboratory Technical Director ToSErvionmonal Labora QuayAssurance Une has ahee da ndrep ons Tpprrhooejjeec3ctMt.. Environmental Laboratory's Quality Assurance Unit has audited the data and report for this E langueE ) r EER-- Quality Assurance Representative hfuirbosottriopnattsihiaaltnitobo produce oxcept bn ui, withoutwriten approoftvhoaIl This test repot1 shall not be reproduced except in full, without wri#en approval of the 3M Environmental Laboratory. moar PAGE 28 OF 34 Su uotssez0s 3M MN01596205 33663300..00225566 GatiageGroveMWD? -- ntsaro ng. AAppppeennddixiAAx:: TTaarrggeettAAnnaallyyttee HHiissttoorriiccaallTTrreennddDDaattaa Cottage Grove MW07 - units are ng!mL 3M rKT otarash ENWRONMENTAL LABORATORY REPORT NO. IS011-01-03-18 | | a a ee a] MAREERR PFOS- @ -- MW07 Pra IT ool sal wn sol owl aul sul sal PFBA [ros| osm oso ows oms| owl osul owe] osm PFOA [oes | comms| some] oom] oom| om| oom| owa| oom] PFBS Coes | oom| wom| onal ome] ome] oom| ow] om] PFOS 1/29/2013 2,09 0259 <0.0250 0.0439 4/22/2013 2,61 0.240 0.0268 0.0459 7/29/2013 1,71 0303 0.0396 0.241 10/28/2013 3,07 0,428 0.0291 0.104 Suro ertb rineS Samples were below the limit of quantitation for PFHS. 1/13/2014 2.88 0,390 <0.100 0.104 4/23/2014 2.48 0.344 0,0360 0.0493 7/16/2014 3,05 0,602 0.0762 0.237 10/28/2014 3.01 0,581 0.0701 0.i91 Cotiage GroveHWI2 uresro ng. Cottage Grove MWt2 - units are ng!mL J SySS mRNA FussToons |amwose| vousons |sorssnons| sacra|wsoons [snoreTrou MW12 fo 1 wl wl wel al wl wl of uw] PFBA [ro I se] sol wow sul ww] sl we] ua] P~OA Po oa] wl wl wl wa] wel me] we PFBS Pos Trl eel wal mol wal owl an] on PFHS Gos 1 wl awl al ml ol wl wal ws) PFO5 1/30/2013 484 946 91.4 13.7 143 4/25/2013 622 1020 i05 16.4 145 7/24/2013 iii0 2000 175 23.9 204 10/31/2013 408 954 87,7 13.0 131 1/16/2014 312 668 82.1 13.1 121 4/25/2014 220 548 68.9 9.82 117 7/17/2014 154 402 50.4 g.ll 96,9 10/30/2014 127 348 46.1 7.78 92,5 srcemorss PAGE 29 OF 34 _Motses205 3M MN01596206 33663300..00225577 rT Kotarash 3M ENWRONMENTAL LABORATORY REPORT NO. IS011-01-03-18 GatiageGroveHWH3 ntsaro ng. AApppenpdiex AAnccoodnnttiiinnuuexedd::TTaarrggeett AAnnaallyytteeHHiistosritcaolTTrrreeinnddcDDaaatltaa Cottage Grove B/IW13 - units are ng!mL f Co. * L-- ey on HES eer ea EL SY PF:HS -- @ -- PFgS -- @ -- MW13 Pra sol ssl eo] eal smo] sa] sm] su] PFBA roo| asl sul ew] col aml sel al oo] PFOA [ous Toso om swr[ om sco] om] om] sof PFB5 Pos Towel oom] wos] ome] oo] ase] om] om] PFHS Lo Tso eo] sol sol sal oul ssl un] PFOS 1/29/2013 5.60 2.56 0.560 0.396 3.92 4/24/2013 9.34 5,46 0,972 0.93"- 4.05 7/23/20:13 8.30 5.2_7 1.07 1.05 4.02 10/30/20t3 6.48 4,01 0.571 0.366 1.40 1/14/20:14 9.80 9,78 1.20 0.969 3.08 4/24/20:14 7. :14 8.63 0.752 0.556 2.33 7/16/20:14 8.08 14,4 0.973 0.7:13 4.48 :10/28/20:14 9,64 1.09 0,720 4.89 CotiagoGroveHWHAR -urts arorginl. Cottage Grove MWI4R units are ng/mL A ee * moh N [oamaa["arnsTonss|nvesosre [orapoaonne | MW:I4R [ow T wel l en] snl PI'BA [rosTo sul l wae] ase] PFOA fos [wwws ] mel] al PFBS fos Te ooo wl or wee] PFH5 loT os oso ul [l we] PFOS 1113/20:14 295 139 ~.7~5 12~3 24,9 4!23120:14 650 543 18~2 20,0 353 7116t20:14 671 426 29.6 20.1 ~58 ~0t29120~4 570 353 38.1 3.6.6 82.6 33663300..00225588 sresoos PAGE 30 OF 34 _Motsee207 3M MN01596207 CotiageGrove WWIB units re ng. AApppenpdiex AAnccoodnnttiiinnuuexedd::TTaarrggeettAAnnaallyytteeHHiistosritcaolTTrrreeinnddcDDaaatltaa Cottage Grove MW16 - units are ng!mL 3M EE ORTNO 101015318 ENWRONMENTAL LABORATORY REPORT NO. IS011-01-03-18 eE e g pre 9 SNR MW16 froT=ssl sol seal sol wa] ws] wo] wo PFBA fron wel ws ona al io] wr] ws] a PFOA fousTass] os] mel wal wl ssl wal ml PFBS Los os] an] onl sos] snl col sal aul PFHS bro Tool ms] wa] wal sul wil wol wel PFOS 1/29/2013 31.5 42.6 28.3 2.54 202 412412019 33.2 43.8 27.5 2.74 21.8 712412019 26.3 39.9 29.6 2.83 20.1 1013012013 45.0 73.9 42.1 3.95 38.2 1/14t2014 42,9 91,0 40,0 5,52 53.1 412412014 40,7 85,7 37,9 4,49 51.9 7/16/20:~4 45,7 98,3 37,9 5.46 57.0 10/28/2014 38,9 75.8 33~9 4.58 42.6 CotageGrove WWIDA units rong. Cottage Grove MWI01 units are ng!mL =e tN NN Faron I vssons Tamviors [sspears snsons |arson | on sopons| MW10:I founTwo] wl wel swol wo] sso] wo] el PFBA [roa1 uel al wel worl reel seo] wo] mal PFOA foes 1 sal was sael wl wal wa] mal me) PFBS foe Tol wl wl me] on] we] wo] PFHS Loo IT el [wel wa] wl wn] wl vo PFOS :1!30/2013 1630 124 25.2 455 206 4t23/207 B 1830 121 19.5 459 188 7t25/201~ 1680 112 24.0 464 18 :10!301207 3 1020 86.7 25.5 314 158 ~/:15t2014 1510 79,4 25,4 398 159 412512014 1330 76,0 37,8 364 135 7!~ 7/20:14 1460 83,9 29,3 480 193 ~0t29/2014 1410 748 296 452 1/0 33663300..00225599 nestor PAGE 31 OF 34 aW_No1s06208 3M MN01596208 rT Kotarash 3M ENWRONMENTAL LABORATORY REPORT NO. IS011-01-03-18 CotiageGrove W104 unis re nn. AApppenpdiex AAnccoodnnttiiinnuuexedd::TTaarrggeettAAnnaallyytteeHHiistosritcaolTTrrreeinnddcDDaaatltaa Cottage Grove I~iWI04- units are ng/mL Te AT +/ Ca [ee eee Ved RRRRRRARA PF:HS -- @ -- PFOS -- @ -- MWI04 [ow | sol wl slsl ml wl ws] PFBA fron| wal earl ur] mal ona ani] es] smo PFOA [rs| ial aml a] om| so] sw] ea] sm PFBS foe| sol mel wal won| wel ne] em] ea PFH5 Coo Tl wl onl sel aml oul ml wl PFOS 1/30/2013 36.3 44.8 11.4 9,07 201 4/25/2013 74.7 60.7 9,75 13.4 185 7/25/2013 54.3 74,7 8.16 11.8 176 10/30/2013 53.6 72,5 7,95 10.1 165 1t15/2014 202 35,1 7.50 14.2 4.25 4/25/2014 107 82,1 8.10 12.6 234 7/17/2014 47.9 76,5 8,68 8,95 233 10/29/2014 30.9 50.00 7.72 6.24 177 CotisgeGroveMWIBS units ro nin. =Cottage Grove mm MWI05 units are ng!mL //\\ --/ Ee Mp tTSo te | SN RR RRS, ~/30t20:13 [ol sol 54.4 [onl el 119 Cool snl 8,03 Col wel 21.1 Con] mol 129 4/25/2013 57.0 104 5,72 16.0 95.0 7125/2013 mel wal wel mol oil wa] sa 71.6 we] wl ws] wa] wr] wa] 70.6 wn onl ul sal un sn] wal 6.49 onl ol wel wal wal wl nl 6.35 ol wl wl wi] wl ws] ml 92.3 :]0/30/2013 38.9 87.2 4,98 6,01 467 1/14/20:14 55.6 68,3 6.15 12.6 152 4/25/2014 71.0 44.3 7.68 8.59 58,7 7/17/2014 39.2 27.7 4,89 6,65 36.2 10/29/2(]:14 46.3 92.8 4,01 18.9 73.5 :l/30/2013 54.4 119 8.03 21.1 129 33663300..00226600 [ro PAGE 32 OF 34 au_Notsse200 3M MN01596209 CotiageGrove W108 unit re ngnt. AApppenpdiexAAnccoodnnttiiinnuuexedd::TTaarrggeettAAnnaallyytteeHHiistosritcaolTTrrreeinnddcDDaaatltaa Cottage Grove MWI08 - units are ng/mL 3M EE ORTNO 101015318 ENWRONMENTAL LABORATORY REPORT NO. IS011-01-03-18 : ratetd OR RNARRNRY FanosT vsoors | sosoons| pspmns | somos |"svamons|"sosone[soo ronson | MWl08 Pr Tol ws] wel wl wel wl ml mo PFBA ProeI ul ol ol aul ww wl wl el P~OA [ro | esl ww] wel ae] we] we] ws] ms PFBS Loe|i] en eal awl en] alae] ee PFHS Loo IT asl ol wel al wel al wel mol PFOS 1/30/2013 ~.0:I 348 26.5 11.1 45.5 4/'25/2013 42.5 201 16.1 4.95 37.3 7/24/2013 38.0 202 14.6 4.94 26.8 10/30/2013 51.7 218 21.6 4.47 33.2 1/14/2014 51.6 169 17,0 4.13 33.5 4/25/2014 65.4 164 17,4 3.58 43.3 7/17/2014 222 522 60,7 11,3 58,0 10/29/2014 87.0 268 22.7 8.50 42.0 CotisgeGrove WHO ut ro nin. Cottage Grove MW110 units are ng!mL 7I Jl eae SREB, [ann | vsaors | smsoons[opens | sosapons |"svaone[name[sewsTromamma| MWll0 Pw Tol wl wl wl wl wm wl wl PI-BA Pros| sol we] sul wl aw] ae sel a] PFOA Lows 1 wel wr] asl sal wal wal wa] we] PFBS Pos Tol uel sal al od oan an] PFHS bo Tel wal wn oil iT ws wel wa] PFOS :1!30/2013 i/i 141 46,6 10.3 28.6 4t25/2073 183 160 66,7 11.8 26.4 7t24/2013 304 144 43,8 9,4~ ~7,8 :10!3012073 174 190 94,8 15.3 21.1 ~/:14t2014 179 248 85.1 19,4 12.1 412412014 189 310 86.~ 20,9 12.5 7!16/20:14 185 390 82,3 24,1 ~5,4 ~0t28/20i4 254 417 576 23.5 129 33663300..00226611 sressorse PAGE 33 OF 34 au_mnotssez10 3M MN01596210 CottageGrovePWO9 - nts areng. AApppenpdiex AAnccoodnnttiiinnuuexedd::TTaarrggeett AAnnaallyytteeHHiistosritcaolTTrrreeinnddcDDaaatltaa Cottage Grove PWO9 - units are ng/mL 3M rv soi roan ENWRONMENTAL LABORATORY REPORT NO. IS011-01-03-18 ] a ER * RRRRRN RAS PW09 Pro T snl wl onl wl PFBA [ros |om owe]oan] oms| PFOA [roe1ome] ome] owe] ome] PFOS 4/25/:13 3.72 0.223 0.324 6/~.9/~.3 NA 0.462 0.376 7/24/:13 2,95 0.624 0.622 8/29/:13 NA 0.605 0.8:18 J ------ NA = Not Applicable; analyte not requested for the sampling event. 9/30/:13 wl snl eae] wel NA ows sel sn so] 0.873 se] sm]aml sel J..38 :10/29/:13 4.53 1.02 1.52 :1/:15/14 4.76 1.33 2.13 4/25/:14 4,:14 1.05 1.60 7/17/:14 sof sol 4,32 el el 1.16 sm[ oss] 1.79 :10/30/:14 3,87 0,701 0.838 CottageGrovePWIO - natro gsmt. Cottage Grove PWI D ....- units are ngimL teed ty " WEABARARN PWl0 fonT wonl wl sul wl wl wl wl sol aol a] PI'BA [ronToms] ans]aol om] om]wwm|ome] om|oes]ose] PFOA [oes |osm] wlool wl wlwel wal om| esol om PFBS [ome 1om] wlom wl wel os] oous[ono] oso]oom] PFHS [ros1ome]owl om[ om] om]owal om]ow] osm]om] PFOS 4/25t~3 4.25 0~428 &594 0,:197 0,396 6119113 NA 0.415 NA NA 0.401 7124113 3.37 0.420 0.540 0.185 0.380 ~129t~ NA 0,471 NA NA 0~415 Na tspseyo sindro in vt NA = Not Applicable; analyte not requested for the sampling event. 9!~01~ NA 0.528 NA NA 0.465 ~0129113 6.09 0.524 0,703 0.~.93 0.458 :~i~5I~4 4,40 0.212 0.26:1 0.0485 0.'[24 4175114 5.07 0,421 0,471 0,:110 0,437 71171~4 4,90 0.484 0.540 0.:104 0.503 ~0/30/~4 4.43 0.375 0.400 0,0777 0.337 orcesscen PAGE 34 OF 34 M_MNo1ss6211 3M MN01596211 33663300..00226622 -- dl sample bottles include the addition of ~ternat standards and surrogates, not pre-rinse the bottles. not pour out the contents of the bottle. Project: ISO1 I-0!-03-!8 ENVIRONMENT ~L LABORATORY Cha n-of- 2ustody } Shipping Address: 3M Environmental Laboratory pee gan 3M Center, Bldg 260-5N-17 St. Paul, MN 55144 Phone: (851) 733-9873 AIt. Phone: (651) 736-6559 Fax: (651) 733-4687 Requester: Kotsmith, James Ronald (MAPLEWO Department: 452090 Site Source: 01J9C020 Project Number: 00731380t5 Date Created: 10/24/2014 Project Description: Cottage Orove 4th Quarter 2014 Sampling Comments: Completion Date: Project Lead: Susan T. Wolf Phone Number: 651-733-985 I Email Address: stwolf@mmm.com 35'1 S,qmple Number ~ample Description Ser mw a l SO 11-01-03-18-001 oraswr Toomer tag Tul wa]1] 1SOl 1-01-03-18-002 ores urToomer rn Tela polJ ISOI 1-0t-03-18-003 Ieovorsewoe Tesoro Jaze | Bae co 11 I$O11-01-03-18-004 Iooorseos Toomer gyros | JarJos [1 15011-01-03-18-005 oo Toowovmme jviose |lou pe] | 1SOl 1-01-03-18-006 omawnTomo Tait Tah pe TT ISO11-01-03-18-007 oaroeos Teowovwer |ae wel| [ood] ISOI 1-01-03-18-008 [roaroreon Teowovwmmefol TopppelTT ISO11-01-03-18-009 ae TeTr Tee ar e TT a i ISOI 1-01-03-t8-010 loner Toomeryor]Toros we TTT] ISO11.01-03-t8-011 IrosarareotJeomermans un | VoiponTT1] 1SOl 1-01-03-18-012 ona TeowormeemtTTge ee]V1 ISO11-01-03-18-013 Date/Time Samp!gd. Mntrix Comment ISO11-01-03-18-014 Sample Condition Upon Receipt: [] Acceptable [] A II items accounted for Temperature: DegC [] Received on Ice Cottyeesinen Husted Collected by (print): ~ ~3 ~' 14 cuncorvspsre._ .0 JA [] C thor: Collector's signature: e CrTT T T T Relinquished by: Date Time Shipped Vi Received by: // Date Time FFT rs Page l of 3 33663300..00226633 3M MN01596212 Cuinof 3M film ENVIRONMENFAL ENVIRONMEN Chain-o Prec: 1SOMLOLA3-1 (cont) Project: ISO! 1-01-03-18 (cont.) Regueser Kors, James Rens (APLEWO, Requester: Kotsrnith, James Ronald (MAPLEWO Dearne 452050 Sic Sure, 115CC20 Department: 452090 Site Soarce: 01J9C020 Pree Number 0073138015 Project Number: 0073138015 Dat Cres: 0242014 Date Created: 10/24/2014 Proc Descripia: Cotage Grtohuvree2014Sampling Project Description: Cottage Grove 4th Quarter 20!4 Sampling AMSpl Note Seater 3M Samgle NumbeL" Snmole Deseriptiq Cotody 7LALALBAOBROARATTOORRYY -Custody ee ron Shipping Address: 3M Environmental Laboratory SV Cor Beg2850017 3M Center, Bldg 260-5N-17 SR Bid St. Paul, [,/IN 55144 Prone: 051 Tse8r3 Phone: (651) 733-9873 Ai Prone (83)738 50 Alt. Phone: (85!)736-6559 Fac (680 1304007 Fax: (651) 733-4687 CCPoromompjlepteletteiiooanntDDSaautese:an T. Wott PPEPhhroooljnneeectANNLduuememadbse:er:rS:us66s55at1n1w.-T7o733.l33Wl.-99@o89ml58fm11mom Email Address: stwolf@mmm.com [ Date/Time Sampled Matrix -- Comment [oro [ISOI won Teomonmiens wet [iISoO orev 1-0!-03-18-016 Teomovmiewet |Tofu | Lown mse[od|] geo][1] [porous won ISOI 1-01-03-18-017 Jcomonmmanwn Jun pw]TT] psonanrvos ISOt 1-01-03-18-018 Teomaovswionston 1 Tojwu [rorvoros wan Tcomewmme iiov1Tom iol11] ges]TT] [St') 11-0 t -03-18-019 [[osnoarna wiownan I5011-01-03-18-020 Temmowsmmoe Teomovsoionns tv]Tipu Too |Tiowi gs] 11 wwee] [1 ) ISO 11-01-03-18-021 [s1SoOv11o-0v1a-0s3-i18s-0o22nToomowmmiore yim | Tiiufngg] 11 [rISonI 1a4n)1-03-!w8-a02n3 Teomovimmmn ot]Tom js] 11) [sISoOu1o1-v01e-0y3-w18-0n24 Teomommmnewns |Tu pe] |1] ova ISO 11-01-03-18-025 Teonovswore wey |Jas wg]J] ] ronan ISO11-01-03-18-026 Jeonowmooewai |Lfyw we]TT] [onavoswanTeoma t SOl 1-0 t-03-18-027 eTJon wl]11) [overswan ISOl 1-01-03-t8-028 Teomovsmne wit 1Tonswe]T1) [oISOoI 1r-01-03-w18-0s29 Teomommosewed 1JoulewuTT] [sonore woo tSO11-01-03-18-030 Tcomovwwions wil |Twp wg] V] [ISOI s1-01-0o3-w18o-r03n1 o|cormoowrwnme p57 hp es TT Sammie CoUnp oRenc: C0acepatie Sample Coadltion Upon Receipt: Tempers gc 0Reetontee Temperature: Deg C [] Acceptable [] Received on Ice C1 Aems acum for [] All terns accounted for our [] Ott eomeisyorinr__ Collected by (print): [vee Relinquished by: ---- -- Tih Hfosbic cucurssgme 7) J] Due Time Sipave| Reewams 7 we mn Date Time Shipped Via Colleclor's signature: Received by: ;;~" / Date Time r r[ r r r T r r Tr T r r 1 T TPag] e2013 Page 2 of" 3 _MNotss6213 3M MN01596213 33663300..00226644 HomoNCIonLf CsonoeUToy Jigs ENVIRONME~ TAL LABORATORY y S 0 Coerrsa y 3 Chain-, f-Custody Shipping Address: 3M Environmental Laboratory 3M Center, Bldg 260-5N-17 St. Paut, MN 55144 Projet 1501101935 cant) e ere: ee s7339e 073 Project: ISO11-01-03-18 (cont,) Regus Kati, fms Rosi UAPLEWO Fo ae Requester: Kotsmith, James Ronald (MAPLEWO Depart 5200 Se Sone 15020 Campion Die Department: 452090 Site Source: 0IJgC020 Jaton Ni Pres Lse: Son Twit Project Number: 0073138015 FDaoc Crue 034adis PErone Naber 65173 861 Date Created: 10/24/2014 e Desripion: Cte Grove th Qu 2014 Sling ri Adi: swoon Project Description: Cottage Grove 4th Quarter 2014 Sampling Sang unter Seep erinion Dot Som Mocs 3M Sample Number Sa mple_l)_es c r i ~tio~_9.n [ronnie Jcomo Common 1501 1-01-03-18-032 Phone: (651) 733-9873 AIt. Phone: (651) 73S-6559 Fax: (651) 733-4887 Completion Date: Project Lead: Susan T. Wolf Phone Number: 651-733:9851 Email Address: stwolf@mmm.com Date/T me Sampled Lylatrix .Comment frovorsresn comcovmwon sgimge |Teg Jere ww TT ISOI I-0!-03-18-033 [poston Teomo rwor pose | Tidy gor fT] ISOI 1-01-03-18-03'4 [sonora Tomonrmmoe jgugse TT me]TT] [SO11-01-03-18-035 [sono now Tcomo moon gz 1Toy gee TT] 'tSO[ t-01-03-18-036 rmune jose | mfrseid TT] 1 SO I 1-01-03- l 8-037 psouorovisen Jeomonmrew IS() 114)1-03-18-038 [ sonaroiwsoor nnTecooo nwaevtrmeersass muiennst27s 1C|TJ2ohwa7n geensel|T A w T]7] 1SO11-01-03-18-039 romper o2C Ol Resmetantce `SSaammppllee CCoonnddiittiioonn UUppoonn RReecceeipipt:t: Temperature: Des C [0] AAcccceeppttaabbllee [] Received on Ice 00[3] [] one AAlll tteermnss Orb aaccccoouunntteedd ffoorr prossere re Time Sven| Rees ee Cotebcy rpreimd: Tobia [lyn bere CoClolellcetcotor'r'ssssiiggnnaattuurree:: ~A/~~t /Z7D Relinquished by: Date Time Shipped Via Received by: *I Date Time 33663300..0022665 Pae3ors l Page 3 of 3 Sw umorssezis 3M MN01596214 T PFBA, P_ FOAAATATtNTADACcPHeFMOmSEeNTnTRtEEeND G_ RAPHS PFBA, PFOA AND PFOS TREND GRAPHS 33663300~.00226668 u_mnotsse21s 3M MN01596215 BBAACCKKGGRROOUUNNDD LLOOCCAATTIIOONN 33663300..00226677 33MM_MMNNO011559966221166 --2a i-- Monitoring Well MW-07 (Background) H, 10/2012 - 10/2014 Cottage Grove, MN Site 3,5 | z| 3 i te | ------ Wim 10/15/2012 vomos sen 1/23/2013 5/3/2013 wonwasvon ow 8/11/2013 11/19/2013 2/27/2014 sow 6/7/2014 ssw wwe 9/15/2014 12/24/2014 ess CGMFI All FC data Cros~ta5 thru 2014 C7 17(150 14) xlsx; ~W07 3M_MN01596217 33663300..00226688 DDI11//DD22 AARREEAA 33663300..00226699 33MM_MMNNO011559966221188 Wriwtelin1g01 Monitoring Well MW-101 em, (D1/D2 Area) a:as 1012012- 1012014 cr. Cottage Grove, MN Site 2OOO 1800 I.1600 1400 gm1200 a = 1000 we] 800 600 T eT ee TTT 10/15/2012 1/23/2013 5/3/2013 8/11/2013 11/19/2013 2/27/2014 6/7/2014 9/15/2014 12/24/2014 Pp-- 3M_MN01596219 33663300..00227700 MonitoringWell MW-102 Monitoring Well MW-102 oi/o3 ra) (D1/D2 Area) ir 10/2012 - 4/2014 Camas Grove0, Cottage Grove, MN Site 2000 1800 1600 1400 gm ee 1200 TM FE i000 Fe 800 600 400 son I011512012 as 112312013 ns 51312013 ws 811112013 ws 111"I 912013 a2127/2014 wns 61712014 wmorssezzn 3M_MNO1596220 33663300..00227711 rnp Monitoring Well MW-103 raa (D1/D2 Area) EE 10/2012 - 4/2014 Cottage Grove, MN Site 2OOO 1800 SE 1600 1400 -- 1200 EE 1000 -- ow] 800 600 40O e 2000 Se ew ]aes 1o/15/2o12 1/23/2013 5/3/2013 8/11/2013 11/19/2013 2/27/2014 6/7/2014 wane 3M_MN01596221 33663300..00227722 I: Monitoring Well MW-104 roe (D1/D2 Area) c WEm , 10/2012- 1D/2014 Cottage Grove, MN Site 2OOO 1800 -- 1600 1400 Ee ---- 1200 1000 800 600 40O 200 J a ----- 0 Some mn ss wns wn in lO/15/2o12 1/23/2013 5/3/2013 8/11/2013 11/19/2013 2/27/2014 Sioe n sy mn 6/712014 9/15/2014 12/24/2014 samere 3M_MN01596222 33663300..00227733 DD99 AARREEAA 33663300..00227744 33MM_MMNNO011559966222233 ---- Monitoring Well MW-105 mrovEe(D9 Area) Ee 10/2012- 10/2014 Cottage Grove, MN Site 500 45O 40O "a. ~ 3o0 I ._~ ~ 250 o 200 .150 ---- i00 SAT 550O <<. 10/1.5/2012 wm 1/23/201:3 wn 5/3/2013 NOTE: Expanded Y scale compared to other D9 area wells. wees 8/11/2013 whem 11/19/201:3 wm 2/2712014 we 6/7/2014 ew 9/1512014 12/24/2014 I 3M_MN01596224 33663300..00227755 | sos Monitoring Well MW-13 (D9 Area) 10/2012- 10/2014 Cottage Grove, MN Site I, 16 14 12 I NS INS wi 0 10/15/2012 vn 1/23/201~ wm 5/3/2013 wen 811112013 waves 1111912013 sms 212712014 aioe 6/7/2014 ws 9t15/2014 won 12/24/2014 ms 3M_MN01596225 33663300..00227766 ProductionWell Pw:09 Production Well PW-09 ose (D9 Area) asin safmie 04/2013- 10/2014 Cana Grav,0 Cottage Grove, MN Site 10 I -- _ -- = ---- 0 sao wens wm wes unves ss anew sian wae 10/15/2012 1/2312013 5/3/2013 8111/2013 11/19/2013 2/27/2014 6/7/2014 9/15/2014 1212412014 awmorsaezzs 3M_MN01596226 33663300..00227777 W WWWTTPP AARREEAA 33663300..00227788 33MM_MMNNO011559966222277 Monitoring Well MW-108 Monitoring Well MW-108 aw are (WWTP Area) joni aie 10/2012-10/2014 CoGotv as0 Cottage Grove, MN Site 600 5O0 4O0 300 200 ioo ison o 10/15/2012 wens 1/23/2013 wn 5/3/2013 wm 8/11/2013 wens 11/19/2013 gms 2/27/2014 f wnsAwen 6/7/2014 9/15/2014 wave 12/24/2014 awmorsaezzs 3M_MNO1596228 33663300..00227799 DD55 AARREEAA 33663300..00228800 33MM_MMNNO011559966222299 enera Monitoring Well MW-110 ree(DS Area) rn 10/2012- 10/2014 ms Cottage Grove, MN Site w5OO 450 400 350 ~,~ 300 ir /\ 1 ._. ~ 250 I" NS ~200 o> --L A| 150 i00 TT --a r ] a 10/15/2012 1/23/2013 5/3/2013 8/11/2013 11/19/2013 2/27/2014 6/7/2014 9/15/2014 12/24/2014 33MM__MMNNO011550966223300 33663300..00228811 enone van Monitoring Well MW-12 op (DS Area) J.Th 10/2012- 10/2014 -25OO Cottage Grove, MN Site 2000 f3 o |i. \ ZN - -- 5OO TT 10/15/2012 1/23/2013 5/3/2013 8/11/2013 NOTE: Expanded Y-scale compared to other D5 area wells. eh 11/19/2013 2/27/2014 6/712014 ~/15/2014 12/24/2014 srs 3M_MN01596231 33663300..00228822 entries Monitoring Well MW-16 fie (DS Area) L arSm e 10/2012- 10/2014 Cottage Grove, MN Site 4OO 35O ~ 25o 3I- EE .I~ 200 M 150 ioo 50 en o 10/15/2012 1/23/2013 5/3/2013 8/11/2013 11/19/2013 ewe 2/27/2014 6/7/2014 911512014 12/24/2014 33MM__MMNNO011559966223322 33663300..00228833 DD88 AARREEAA 33663300..00228844 33MM_MMNNO011559966223333 i Monitoring Well MW-14R Ea vi(D8 Area) n. 7/2013 - 10/2014 Cottage Grove, MN Site .800 "I 70O 600 ~ 5oo ._~ ~ 400 : TN] 300 200 lOO --] o wi umn wn wm wn sms wow san mao 10/15/2012 1/23/2013 5/3/2013 8/11/2013 11/19/2013 2/27/2014 6/7/2014 9/15/2014 12/24/2014 I3MM__MMNNO011550966223344 33663300..00228855 EEAASSTT CCOOVVEE AARREEAA 33663300..00228866 33MM_MMNNO011559966223355 ---------- Production Well PW-10 ps (East Cove Area) Ty 04/2013 - 7/2014 ETE, Cottage Grove, MN Site .io 9 ~~ -- a a-- 10/15t2012 1/23/2013 51312013 8/11/2013 1111912013 2t2712014 61712014 ] 9t15t2014 12/24/20:14 wanes 3M_MN01596236 33663300..00228877 AATTTTAACCHHMMEENNTT FF ANDLLAASBBUOORRRFAAATTCOOERRWYYAAATNNEAARLLYYSTTAIIMCCPAALLLINPPGAACC-KKSAAEGGPEETSSEMFFBOOERRRPP/OOORRCEETOWWBAAETTREE2RR014 AND SURFACE WATER SAMPLING - SEPTEMBERIOCTOBER 2014 33663300~.00228888 3M_MNO1596237 3M MN01596237 EmmenmSoOtOtT 3M Environmental Laboratory Report No. IS011-01-03-17 FFiinnaall RReeppoorrtt AAnnaallyyssiissthooeff M3MiMisssCsioisstsstiiappgppeii GRRirivvoeevrrePPFooarrceeilWWitayatt-eerrSeaapnntddeSSmuubrreffraacc2ee01WW4aatSteearrmpSSlaaimmnppglleess NNeeaarr the 3M Cottage Grove Facility - September 2014 Sampling LLaabboorraattoorryy RReeqquueesstt NNuummbebre:r: 1ISSO01111--0011--0033--1177 MMeetthhoodd RReeqquuirireemmenetn:t: 33MM MMeetthhoodd EETTSS--88--004444..11 Repor Ost Deof ast Snare Report Date: Date of Last Signature TTeessttiinngg LLaabboorraattoorryy 33MM EEnnvviirroonnmmeennttaall HHeeaalltthh aanndd SSaaffeettyy OOppeerraattiioonnss 3MEEnnCvveiinrrtooennrmm,eenBntltadalgl L2La6ab0bo-or0ra5at-tooNrr-yy17 3M St. Paul, MN 55144 Center, Bldg 260-05-N-17 St. Paul, MN 55144 RReeqquueesstteerr 3M JJEiimHmSKKoOotptssemmriaittthhions 33MM3MBBuuEiillHddSiinnggO22p22e4r4a--t55ioWWn--s1177 SSaaiPinnhtot nPPeaa:uull,(, 6MM51NN) 55755311744-443-6-1130050000 Phone: (651) 737-3635 7, To sing pod hr rt crofISt USOIEC 1315.20 Gora The testing reported herein meet the requirements of ANSI/ISO/IEC 17025:2005 "General fick Rocyirsmantsfo hoCampatenceof Tosbg rd CakbeaionLaborstores"in Requirements for the Competence of Testing and Calibration Laboratories", in accordance with the A2LA Testing Certificate # 2052.01. Additionally, the laboratory's ZF (RCCATOIFED) lym asbersha basdemir Cranacbo EhPA quality system has been audited and was determined to be in conformance with the EPA Tn GCSB Baa eben sted ee GLPs (40 CFR 792) by an independent A2LA assessment. 33663300..00228899 orcerorn PAGE 1 OF 36 M_MNO1ss6238 3M MN01596238 eFonstmBiOtTyT17 3M Environmental Laboratory Report No. IS011-01-03-17 33MM EEnnvviirroonnmmeennttaall LLaabboorraattoorryy 333MM0 EPEnrnvnvioirrpooannlmmeAennntataatllLcLaaablboorIarnattvooreryysTtTeocerhcn:hinScicuaaslaDDneirWecocttlo:r: WWiiklliaamKK.,RReaegaegenn,, PD.Ph.D. Report Author: Celso 3M Principal Analytical Report Author: Chelsie Grochow Investigator: Grochow Susan Wolf AAnnaalylyttiiccaall RReeppoorAt I~SSOO1111-o0011--0033-o1l 77 AA4nanly3asMisloCoofftyMMisaissigsseissiGsiriposoppvieRRiFivvaeerrcPPtoo-ryreeWSWaetpaetteerrmaabnneddr S2Su0ur1rff4aaccSeeaWW mapalitenerrgSSaammplpeless NNeeaarr the 3M Cottage Grove Facility- September 2014 Sampling RReeppoorrtt DDoatte:: Daoe Date of LLaasstt SSiiggnnaattuurree: 11 _SuSmummamryafriyn/Itnrtroodduuccttiioonn TT1hh0eem 33rMMe MEEnnivvisirrsoonnimm:eenntRtaialvlerLLaanbbaooarrraatftooerryy3pprreeCppoaalrrleeaddgeaaGnnrddovaaennaafllayyczzieeydd. ssSaaammmpppllleeesss wccooellrleeeccttceooddlebbcyyleWWdeesSsletoopnntppeeemrrssboo2ennrnn9eell fOaGronccmtalozobthebeerde22rM,,fi22so0r0s1i1s4p4s,o.iprpfSSiuaaoRmmrpiovplebleerusstnaewwneaeorrrieethaerrece3ttudMurnm(CeePddoFtfttAoao)ght.heeeGp33reMoMrvfeEuEnonfrvavoicioriolocintniymma.enencSniiatcaamllapLLcleaadsbcoow(rreaPartFoelOrAoyc)oroo.lynnlecaOOtncecdtdtoobSbpeeeorrrpft33ei,,mc22r00bo11eod4rct2aaa9nnndd-e Suonate analyzed sulfonate (PFS), under 3M Envronmerta Lobalary project number for perfluorobutanoic acid (PFBA), perfluorooctanoic acid (PFOS), under 3M Environmental Laboratory project number 1S011-01-03-17 (PFOA), and perfluorooctane ISO11-01-03-17. TsTihhxeeoe33nMMpoEErnnevviiwrocanrommreenn(ttralolrtLLtaabibolorraawttaootrroyyr:pprrIeeWpp)aarrleeoddcatssiaaommnsppilaeendccoosnniitaaoiinoeenrrsscoffomcrrosItphoinrntydy-itwnogo sssuaafmmappciloinnggwelltoorccaati(iooSnnWss):; slvlooioxccktaaeatteimoonrenss.op.foEr1eE0aa9cwchmhaLt.eaermmpS(plinyatytemcrcsopotnintiatbaanlainteweerarwtsewara;sskfIWomma)aersrilkkogeechdadtwtoiwofinithhsheaa21nTdt"ifyills-ittxoowteohehseenarrmeocp"olIrliirnneneesgplthohoanacladtctinicoogonrsrrsecuseorpfnoassncsedpieewdodatn0tooefarda a (feSfneinWaldald)l fvssoaadmmlupmlpselee,a,mopflifeld1led00assnaamdmmLppa.lleefSadddumupppsililcaceaamtbtpeo,l,tetaalencndsuepaatisattfalaorrerggeeeottniglaayh.nntaaollfyyAtttleheesffiaethdmldiprtlymme-taaswtrotbixastpsaipemkiskepe.lii.nngcAAlllluoldcooeadtvhtitoerhnresllooacccdoaadnttiiistooiinsnostsnednioncfcoilnfuutaddaeefmddieallada wfssieetaalrndneddasaaarrdmddssdpslaaennddoanssdtuuhroearoggsfaieaatlmtdeeplsrreeeaccmcooopvvneeleraryyidnssuettparalnsincddaraatrreiddrsson0((lSySR.bRSeEAsn)l)gl[[s*1sa3CeCm.n}stpP]-loPeFsFBBtAbhA,oe,tt[fl1e3esCC}~infP]c-oPFrluFOdsOeaAAmdapantlnhedde c[[a1o*d3ldeCCci.4tii]oPo-PnnF.FOoOSfS,Si,nawwtmehhprinilccahehl wBSboeootrtlteleoesandrrdceeoessnedetrravvtioeendditnhffgeotohrrsetlaaatmrragpgrelgeteeaatcnnaoaalnnlyytaatteeienefsfirieselpddpmrmioitaarotrbxtioxerbnsspepgiiinkksgeeessnstwweneetrrehtoeffotoherfteiiifideefiddefoldrwwsiiaftohhmrpaaslnnaemaacpppoplplerreoocpcprtoriolilaaenttc.eetiommnaa. rtrixSxassmpppikliee solution containing the target analytes prior to being sent to the field for sample collection. S`MSaeamtmphploleedssowwfeAernreealppyrresepepaaorrerderaaennddDeaatnneaarllmyyizzneeaddtiaaoccnccooofrrdiPinnegrgftouocr33iMMnaEEtnendrvoiCrononmmmepneotnuatnaldl sLLaanbboorWraaatttooerrryy bmmyeetLthhOooddMEEATTSS8--;85-00D44i44.c.11t "IiInMrrjejeecctihttnioootdnnemoAaAflnnAasanltyaasslniys"ds"a.isrdfFFosoorlalltoohnwwediinDnsgguettsseoaargmmmapirpnlelaeestioaawnnneaarolleyyfssPirisseotrbbflyuyspoilirniknteeeadrtnemaadlsCssetaoannmndddpaeaorrduddn,dccaasslifiibnrncraaW ettiohoanntee.,rititbnvywtaeaLmssCal/ssMuusSsstppa/MenedccSatt;ereddDd irtanhenaacdttt tsschuuoermnrofoingigtamaetetrenedalrrweesicctnoaovvnetedhrrayeyrd(rrsenepssappnSoodannsnsseekurrwwmoaagasastteiaaspppspwrpreookxrxeeiimmnasatoatetemllpsyylpeiooknneweedicahheshalllfinhotoaeffdndtthreheeedc,oeevsxxeinpprecieeeccsttetehdodef rraienepssteppprroonnonasxsleme.sa.tlaenlTTdyhhaiirss2d0wwa0ana%sds cSS10uournartrfsoiorsgmgoaasettsdesrsrweeacicmtohopvvieeotrhryyersestcttraaoipnvndedrabayrlraddanssnkdaaddmhddaoeetddrSixttaoosmttphoiheksessawasmeamrmpoelepqleccuooanwrnktahaiiiicannhlerordsshabppdyroiorarrxtettcoooomssvaaealmrimespstpleanoccdfooallraleedpccpcttiraooolnnxbiwwmreaeartrteeerl.ynnooTt2ta0uur0ssg%eeeddt. to assess sample recovery and aannaal floalbdomraallryomastiki. spks analyte laboratory matrix spikes wero preparefor the samples were were prepared for hose samping quantitated by those sampling locatiohnas didrot includea target external standard calibration. Target locations that did not include a target analyte field matrix spike. TTuaaabltlleey 1 1 csosunutmmommlaarsriiazzmeepssletthshee pssraaemmppaplrleeed rreeassnudultssanuusasilinnyggzettdhheeiatannhaallytythtiieccaalsl ammmpetltheodsd wiiiddleenntbtiieffiieerddepaaosbrootvveeed.. a nAAdlll rdreeisssuculutsssfsfoeodrr Esebere n his report. quality control samples elsewhere in this report. prepared and analyzed with the samples will be reported and discussed 33663300..00229900 exce2cen PAGE 2 OF 36 3M_MNO15%6239 3M MN01596239 sreerme 3M Environmental Laboratory Report No. IS011-01-03-17 TTaabbllee 11.. SSaammppllee RReessuullttss SSuummmmararyy.. (1) 3M LIMS ID Sample Description Surface Water Locations T eg r IS011-01-03-17-001 IS011-01-03-17-002 CGMN-SW-M RIW09b-0-141001 CGMN-SW-MRIW09b-DB-141001 Average EEiEE %RPD Sample/Sample Dup PFBA PFOA PFOS Concentration Concentration Concentration (ng/mL) ETE <0.0500 <0.0500 oT2 <0.0500 (ng/mL) 0.0332 0.0274 0.0303 (ng/mL) <0.0232 <0.0232 <0.0232 NA 10 NA ISO11-01-03-17-003 CGM N-SW-M RIW09-0-141001 <0.0500 <0.0240 <0.0232 ISO11-01-03-17-004 CGMN-SW-M RIW09-DB-141001 <0.0500 <0.0240 <0.0232 E EEa E ETE ISO11-01-03-17-005 ISO11-01-03-17-006 [oerr ISO11-01-03-17-008 ay ISO11-01-03-17-009 Ave rag e %RPD Sample/Sample Dup CGMN-SW-MRIW09d-0-141001 CGMN-SW-M RIW09d-DB-141001 Ave rag e %RPD Sample/Sample Dup CGMN-SW-M RIW09f-0-141001 CGMN-SW-MRIW09f-DB-141001 <0.0500 NA <0.0500 <0.0500 <0.0500 NA <0.0500 <0.0500 <0.0240 NA <0.0240 <0.0240 <0.0240 NA <0.0240 <0.0240 <0.0232 NA <0.0232 <0.0232 <0.0232 NA <0.0232 <0.0232 E TEEESEE ISO11-01-03-17-010 ISO11-01-03-17-011 Ave rag e %RPD Sample/Sample Dup CGMN-SW-MRIW14b-0-140930 CGMN-SW-MRIW14b-DB-140930 Ee <0.0500 NA <0.0500 <0.0500 <0.0240 NA 0.0789 0.0711 <0.0232 NA <0.0232 <0.0232 ISO11-01-03-17-012 ISO11-01-03-17-013 ii Average %RPD Sample/Sample Dup CGMN-SW-M RIW14-0-140930 CGMN-SW-M RIW14-DB-140930 <0.0500 NA <0.0500 <0.0500 0.0750 10 <0.0240 <0.0240 <0.0232 NA <0.0232 <0.0232 EEE ISO11-01-03-17-015 [S | ehT5 ISO11-01-03-17-016 Ave rag e %RPD Sample/Sample Dup CGMN-SW-MRIW14d-0-130813 CGMN-SW-M RIW14d-DB-130813 Average <0.0500 NA <0.0500 <0.0500 <0.0500 <0.0240 NA <0.0240 <0.0240 <0.0240 <0.0232 NA <0.0232 <0.0232 <0.0232 %RPD Sample/Sample Dup NA NA NA ISO11-01-03-17-017 CGMN-SW-M RIW14f-0-140930 <0.0500 <0.0240 <0.0232 ISO11-01-03-17-018 CGM N-SW-M RIW14f-D B-140930 Ave rag e %RPD Sample/Sample Dup <0.0500 <0.0500 NA <0.0240 <0.0240 NA <0.0232 <0.0232 NA eE EH EeEmee mpeg neeeoe NA = Not Applicable (1) Samples were analyzed by solvent dilution with extemal standard calibration. The analytical method uncertainties associated with the reported results are as follows: PFBA _+ 25%, PFOA _+ 13%o, and PFOS _+ 17%. EEE (2) The RPD value did not meet method acceptance cntena of-<20%. (3) The field matrix spike sample for location CGMN-IW-MRIW14d did not meet acceptance criteria of 100 _.t 30%. The method uncertainty has been expanded to _.t 48% for PFBA. 33663300..00229911 --PAGE 3 OF 36 3M MN01596240 sreerme 3M Environmental Laboratory Report No. IS011-01-03-17 ome Jom [EEE| Table 1 continued. Sample Results Summary. (1) PFBA Concentration PFOA Concentration PFOS Concentration 3M LIMS ID Sample Description (ng/mL) (ng/mL) (ng/mL) Surface Water Locations IS011-01-03-17-019 ISQ11-01-03-17-020 C EES E E TETET1ET] ISOl 1-01-03-17-022 ISOl 1-01-03-17-023 fo150110105-17-024|TCOMN-SWVSRIN1930.1408%0 IS011-01-03-17-024 IS011-01-03-17-025 [ E EEE T E oehT e IS011-01-03-17-026 CG M N-SW-M RIW19b-0-140930 CGMN-SW-MRIW19b-DB-140930 Average %RPD Sample/Sample Dup CGMN-SW-MRIW19-0-140930 CGMN-SW-MRIW19-DB-140930 Average %RPD Sample/Sample Dup CGM N-SW-M RIW 19d-0-140930 CGMN-SW-M RIW19d-DB-140930 Average %RPD Sample/Sample Dup CGM N-SW-M RIW 19f-0-140930 0.0808 0.0549 0.0679 38 <0.0500 <0.0500 <0.0500 NA <0.0500 <0.0500 <0.0500 NA <0.0500 0.200 0.205 0.203 2.5 0.0922 0.0898 0.0910 2.6 <0.0240 <0.0240 <0.0240 NA <0.0240 0.139 0.135 0.137 2.9 <0.0232 <0.0232 <0.0232 NA <0.0232 <0.0232 <0.0232 NA <0.0232 IS011-01-03-17-027 E EEE E IS011-01-03-17-028 [ETEREERa Te ISI1-01-03-17-029 CGMN-SW-MRIW19f-DB-140930 Average %RPD Sample/Sample Dup CGMN-SW-MRIW25b-0-140930 CGMN-SW-MRIW25b-DB-140930 Average %RPD Sample/Sample Dup <0.0500 <0.0500 NA 0.575 0.530 0.553 8.1 <0.0240 <0.0240 NA 0.171 0.174 0.173 1.7 <0.0232 <0.0232 NA 0.150 0.145 0.148 3.4 IS011-01-03-17-030 CGM N-SW-M RIW25-0-140930 0.659 0.181 0.128 ISQ11-01-03-17-031 CGMN-SW-MRIW25-DB-140930 0.687 0.181 0.126 Average 0.673 0,181 0.127 %RPD Sample/Sample Dup 4.2 1.6 IS011-01-03-17-032 ISQ11-01-03-17-033 CGMN-SW-MRIW25d-0-140930 CGMN-SW-MRIW25d-DB-140930 <0.0500 <0.0500 0.0396 0.0509 <0.0232 <0.0232 IS011-01-03-17-034 w EEg IS011-01-03-17-035 Average %RPD Sample/Sample CGM N-SW-M RIW25f-0-140929 CGM N-SW-M RIW25f-D B-140929 Average %RPD Sample/Sample Dup <0.0500 NA <0.0500 <0.0500 <0.0500 NA 0.0453 25 (a <0.0240 <0.0240 <0.0240 NA <0.0232 NA <0.0232 <0.0232 <0.0232 NA -- ;EEEE NA = Not Applicable EEmfemreeSnd (1) Samples were analyzed by solvent dilution with extemal standard calibration. The analytical method uncertainties associated SEEEEERED with the reported results are as follows: PFBA + 25%, PFOA + 13%, and PFOS -+ 17%. (2) The RPD value did not meet method acceptance criteria of -<20%. (3) The field matrix spike sample for location CGMN-IW-MRIW14d did not meet acceptance criteria of 100 + 30%. The method uncertainty has been expanded to _+ 48% for PFBA. 33663300..00229922 anPAGE 4 OF 36 3M MN01596241 vresm 3M Environmental Laboratory Report No. IS011-01-03-17 ome Lr [EEE Table 1 continued. Sample Results Summary. (1) PFBA Concentration PFOA Concentration PFOS Concentration 3M LIMS ID Sample Description (ng/mL) (ng/mL) (ng/mL) Interstitial Water (Pore Water) ISO11-01-03-17-037 CGMN-IW-MRIW09b-0-141002 47.6 8.31 3.00 ISO11-01-03-17-038 E EEE IS011-01-03-17-039 S SEE a W TEAT ISOl 1-01-03-17-040 CGM N-IW-M RIW09b-DB-141002 Average %RPD Sample/Sample Dup CGM N-IW-M RIW09-0-141002 CGMN-IW-M RIW09-DB-141002 Average %RPD Sample/Sample Dup 44.3 46.0 7.2 6.77 6.65 6.71 1.8 7.88 8.10 &3 1.39 1.39 1.39 0.0 2.90 2.95 3.4 0.392 0.374 0.383 4.7 ISO11-01-03-17-042 CGMN-IW-M RIW09d-0-141001 2.93 0.781 <0.0232 ISOl 1-01-03-17-043 CGM N-IW-M RIW09d-DB-141001 EE ISO11-01-03-17-044 ISO11-01-03-17-045 Average %RPD Sample/Sample Dup CGM N-IW-M RIW09f-0-141002 CGM N-IW-M RIW09f-DB-141002 2.94 0.797 0.0269 IEE 2.94 0.34 15.6 15.1 0.789 2.0 0.523 0.524 0.0269 NA 0.0236 <0.0232 Average 15.4 0.524 0.0236 TSOT10105-17-04| COMNAW-MRN 1450-14102 [ | = 5 |= 25a] ISO11-01-03-17-046 ISO11-01-03-17-047 %RPD Sample/Sample Dup CGM N-IW-M RIW 14b-0-141002 CGM N-IW-M RIW 14b-DB-141002 Average 3.3 24.4 24.4 24.4 0.19 101 102 102 NA 37.1 37.0 37.1 %RPD Sample/Sample Dup 0.0 0.99 0.27 ISO11-01-03-17-048 ISO11-01-03-17-049 [ TSOT1.0105-17:050| COMN-WAMRR NY146.0.141001 [oo | e om | em] ISO11-01-03-17-050 ISO11-01-03-17-051 fS 150o1101-08-17-083|CGMIN-W-MRNY1410-41002 [ E 2l| oae[om] ISO11-01-03-17-053 aE ISO11-01-03-17-054 CGMN-IW-M RIW14-0-141001 CGMN-IW-M RIW14-DB-141001 Average %RPD Sample/Sample Dup CGMN-IW-M RIW14d-0-141001 CGMN-IW-MRIW14d-DB-141001 Average %RPD Sample/Sample Dup CGM N-IW-M RIW 14f-0-141002 CGMN-IW-M RIW14f-DB-141002 Average %RPD Sample/Sample Dup 2.29 2.03 2.16 12 0.307 1.40 0.854 (2) 128 ~z) 72.0 80.2 76,1 11 4.49 3.99 4.24 12 0.0780 0.354 0.216 128 (~) 3.96 4.42 4,19 11 0.284 0.218 0.251 26 i2~ <0.0232 0.0952 0.0952 NA 0.0477 <0.0232 0.0477 NA E = ES E mremmpe eeeen NA=NotApplicable (1) Samples were analyzed by solvent dilution with external standard calibration. The analytical method uncedainties associated with the reported results are as follows: PFBA _+ 25%, PFOA _+ 13%, and PFOS _+ 17%. (2) The RPD value did not meet method acceptance criteria of -<20%. EE (3) The field matrix spike sample for location CGMN-IW-MRIW14d did not meet acceptance criteria of 100 + 30%. The method uncertainty has been expanded to + 48% for PFBA. 33663300..00229933 --PAGE 5 OF 36 3M MN01596242 sreerme 3M Environmental Laboratory Report No. IS011-01-03-17 ome Lr EEE EEE Table 1 continued. Sample Results Summary. (1) PFBA PFOA Concentration Concentration PFOS Concentration 3M LIMS ID Sample Description (ng/m L) (ng/mL) (ng/m L) Interstitial Water (Pore Water) IS011-01-03-17-055 CGMN-IW-M RIW19b-0-141001 69.0 149 33.1 ISI 1-01-03-17-056 EE ERNEAeE IS011-01-03-17-057 T ISOl 1-01-03-17-058 EEE ISO11-01-03-17-059 ISOl 1-01-03-17-060 ATE ISOl 1-01-03-17-062 EE IS011-01-03-17-063 EA em 5 51% | ISO11-01-03-17-064 --on i: ISO11-01-03-17-065 CGM N-IW-M RIW 19b-DB-141001 Average %RPD SamplalSample Dup CGM N-IW-M RIW 19-0-141001 CGMN-IW-MRIW19-DB-141001 Average %RPD Sample/Sample Dup CGMN-IW-M RIW19d-0-141001 CGM N-IW-M RIW 19d-DB-141001 Average %RPD Sample/Sample Dup CGM N-IW-M RIW 19f-0-141002 CGMN-IW-M RIW19f-DB-141002 Average %RPD SamplalSample Dup CGM N-IW-M RIW25b-0-140930 CGMN-IW-MRIW25b-DB-140930 69.4 69.2 0.58 62.6 62.5 62.6 0.16 13.3 13.5 13.4 1.5 50.0 53.0 51.5 5.8 54.6 53.2 144 147 3.4 9.20 9.10 9.15 1.1 0.112 0.116 0.114 3.5 223 239 231 6.9 38O 368 29.2 31.2 13 91.9 92.7 92.3 0.87 <0.0232 <0.0232 <0.0232 NA 0.896 0.930 0.913 3.7 1300 1290 Average 53.9 374 1300 %RPD Sample/Sample Dup 2.6 3.2 0.77 IS011-01-03-17-066 CGM N-IW-M RIW25-0-140930 59.1 23.8 16.3 1E 501101.03-17-068|COMNE -W-MRN25.0-141001 [2{= IS011-01-03-17-067 ISO11-01-03-17-068 ISO11-01-03-17-069 CGMN-IW-M RIW25-DB-140930 Average %RPD Sample/Sample Dup CGMN-IW-M RIW25d-0-141001 CGMN-IW-M RIW25d-DB-141001 58.6 58.9 0.85 11.0 10.5 23.3 23.6 2.1 37.4 35.9 = =16.1 16.2 1,2 0.0962 0.0920 Average 10.8 36.7 0.0941 fo ERP %RPD Sample/Sample Dup I1S5001111-0011--0083--1177.-007700|CCGGMMINN--IWW--MMRRNIYW2255f-0O--14411000011 IS011-01-03-17-071 CGMN-IW-M RIW25f-DB-141001 Average %RPD SamplelSample Dup [=] a] 4.7 4.1 4.5 16.5 10.2 7.21 15.9 9.83 6.09 16,2 10.0 6.65 3.7 3.7 17 IS011-01-03-17-073 ISOl 1-01-03-17-074 IS011-01-03-17-075 CGMN-SW-MRIW09-RB01-141001 CGMN-IW-M RIW09-RB02-141001 CGM N-IW-TRI P-0-140929 <0.0500 <0.0500 <0.0500 <0.0240 <0.0240 <0.0240 <0.0232 <0.0232 <0.0232 C E EE EE e HA = NotApplicable mm n (1) Samples were analyzed by solvent dilution with extemal standard calibration. The analytical method uncertainties associated with the reported results are as follows: PFBA _+ 25%, PFOA + 13%, and PFOS _+ 17%. SEE (2) The RPD value did not meet method acceptance cdteria of-<20%. (3) The field matrix spike sample for location CGMN-IW-MRIW14d did not meet acceptance criteria of 100 + 30%. The method uncertainty has been expanded to + 48% for PFBA. --PAGE 6 OF 36 33663300..00229944 3M MN01596243 eFonstmBiOtTyT17 3M Environmental Laboratory Report Rio. IS011-01-03-17 22 MMeetthhoodd SSuummmmaarryy A22.n11aisMMefeottrhhPooFddAss, PFOA, and PFOS was complete falling 3M Environmental Laboratory method Analysis for PFBA, PFOA, and PFOS ELTSa8m044s.1 `Mebodof Anas for ETS-8-044.1 "Method of Analysis for thewas the Determination of Perfuorratod Compounds in Walar oy completed following 3M Environmental Laboratory method Determination of Perfluorinated Compounds in Water by LC/MS/MS". Table2. Targot Analyte. Table 2. Target Analytes. Target Anal~es [Potoommat Gras Perrluorobutanoate (C4 Acid) [Pooomormnaste carci Perfluorooctanoate (C8 Acid) [Posomocmmesstoost CoSwonse) Pe[fluorooctanesulfonate (C8 Sulfonate) Reference Material | pron| tow | Acmnym PFBA | pros PFOA | POS PFOS Structure |unew+ Backed| Linear Linear + Branched | tiLnineeaarr++ BBaranncchheedd| 22Po.22re aSStoaarmmp(pvlelreestCCtoaolllllveeaccttteii)oonannd surfacewatersamples were olected i 125 ml. NaigeneTM (vg ddpPoreoennrpessaiitrwyyeadptpeaoTryliye(epihnthytBeiylrlesaentnnitckeia))lanwbbdoaatttteTleerrss)pappnBrrdieoppnsaakurrreeffaddcieaattwmttahahteoeir33sMMsapmiEEpennlsevvisirowowvennremeereernstcetaaonllltleLLcwaatiedbhdoorrtaianhoteor1ryys2.e.5t moAAfL scsNooeatltlgeooecffnieoalTnabMboborar(lahtotiegorhsryy- prepared Trip Blank and Trip Blank field matrix spikes were sent Satatmhpelaedboroattosryawefresrrreecceaivte.d by th laboratoorny October 3.2014. Sample bottles were received by the laboratory on October 3, 2014. Sampies were sioed refigered with the set of collection bottles. Samples were stored refrigerated at the laboratory after receipt. `22Sa.33mpleSSsaawmmitphpllaeediPPurreeoppnaarfraaactttoiirooonfn 2werepreparedbyremoving a 0.4 mi. audof the welmixed sSsraaaammtmppprlleleeeqsaaunniwddeidtidhiflunuattinhgdegilruittidowwiniitdhhfoa00nc-.t44owrmmerLoLefoo2iffnmmwteaeettrthhyeaapnnpraorelelppaaaannrrddeeddaannubaasylilyynzrzgeeemdadoGbbvyyinoeegxxnttaeermnf0aaal.c4ltssomtraanLnodfdaaalr1irq0ddubccoaaytsltiorbrferaatmtithioooenvn.iw. geSSllaaammmp1 pilxmleeeLdss ta3ihilqiaqqutuuo0orttetqoooufffirttehhhdoee further dilution were initially prepared 1w1el0 uvteeddssampalemwaandspdduiintgeeaigaiihn well mixed sample and diluting it with w99uishmminiL0g.oo4affiidlaLbilbuoootrfiroaamnotorefrayyacrrtneoeara!ggoeafnn11tw0waatdabetdyeri.rr.ne,mTTohhgveeeinnngt3a aa00..n414 ymmmlsLL. alllaaalbibbqoumrmoaatatototrrfiiyxthmsseappii1tkk:iee10sssdpaaimkmlupeptlelleedessvsealwwsmeearrpreeleeppdwrrieaesppscaaudrrseiesluddetdeffdooirnrassgseaaammicnpoplwnleeitss3h.9tt0hh.oa4aft mh6deLiddorennfpoomoltretccthooannnttaoainln. field mairx In addition, field matrix spies. The target analyte spikes. The laboratory matrix spike levels are discussed in section 3.9 of the report. SaSaaammmpppliileinnsggwelloroccoaatptiioronnossprCCeOGMMbyNNr--IeWWmoI-MvRiRnWgIW 1O109F-f1 aamnnLdd. aCCiOqGuMMoNtNo--fNIW-tA-hMRwRIIZe2S5bmbixrreeedqquusiirreaeddmpffuurtathhneedrr dddiiidluiotninog.n. wiTTthhhee0ss5ee sm`malLdmoopeffleamdmseetwht2haeannrneoolom.pil.rneaTTplaoocreeeodaancccbahnynooirfrfeahtmhteeoonvidinoitlgfuete1addn0.ss1gaamm.mplpLel(esads,l,iiqaauoon00t.f.11oacfmmttohLLreaoawllfiieqqluu1l oo0mt0t)ioo.xffeadaThssseoaolmusotapiomlnenplaccenoosdnrwttdaeaiilnrnuietnninggagnSSaitRRlwySSzisstehdww9aao.s8sy aexdtdeemdalatstaanndoamridnacal lcbornatcoenn.tration of 1 ng/mL (dilution factor of 100). The samples were analyzed by external standard calibration. DsDuurpriinnngg ttshheoe opprrneepgwaarraaastiiooannddooeffdtth1he0e tllhaaebboolrrbaaottoorrrayylrccyoonncttroooll nssaammspalpemlesps.l,esaann(naaoblmigqiuunaoatlt oocffoaanssceeppeaarrraalntee oiifnnte1ermgnaailllss)tt.aannddTaahrrded sssbpaoaiimmknpipgnilgeesesobnootluttotloeiosnwtwehfwereaerfessltspadpidfikdkoeeeedddsvswtaoiimtlhtphleaaennlacirbnoolteerractnttaoolrnye.stcaonmTndhtareoraldlmsamaiblmioxxrapaatlstetaosaryan(nnoocomomminnintninaoalladlclcosconaocanmnecpnceltenrrentasrttaraiwdtiotoeinonrneooofftfh11n1enpngnggd/m/rimLeLip)d.riowTrrihttoheo melanin thesamemarer 3s the samples being sent to the field for sample collection. methanol in the same manner as the samples. The laboratory control samples were then diluted with A22l.44samAApnlneaasllyyassnidissquay convo! samoles were anahzed for PFBA. PFOA, and PFOS using high Apppaelelrrrafstomaoremmmtaeaprnnlesccs,eetailihqnuddildqshcudhraroliotcmymharalcotooomnggatrrrloaaolppghrnsyaay!pmntaapynnledgdsreeamrdwieemmrnaeatsspsasrnossagpolyreezaccemttr.droomafmoneedrttryyPthF((eHBHPsAPLp,LCeOP/cSMFIiOSVA/mSM,a)Ssa.)sn. dtDDaePentFtasaiOlilloeSedndsuiinsnasisnnttrgarulumymhzeeigenndhtt parameters, the liquid chromatography gradient program, vbeeloewscribed ntherawdatahardcones placed In the are described in the raw data hard copies placed in the fradata packel, and the specific final data packet, andarebry mass transitions and are briefly Cescroed analyzed described below. 33663300..00229955 encerorn PAGE 7 OF 36 IM_MNOtSS6244 3M MN01596244 swme: 3M Environmental Laboratory Report No. IS011-01-03-17 E A BE Due to the nature of the sample, the wide range of concentrations found in the sample, and the CE FS E EE E EE C i SR environmental occurrence of multiple isomers of the laboratory's analytes of interest, the software used HREReE TSE nh for processing the analytical results is not able to consistently integrate the analytical peak, manual aL Ea, integration of the analytical peak is necessary. All manual integrations are performed following the procedures outlined in method ETS-12-010. The consistency of the laboratory's integration is ensured through the training of laboratory personnel, the peer review process required for all manual integrations, the review of manual integrations by the QAU, and where necessary the review of manual integrations by laboratory management. Table 3. Instrument Parameters. [o|i nn e| [Insti rumen nt Nas me trTTm " enerETst SiKiimro k me| Analysis Dates [Basbcimonos| erssoms | Analytical Method [wisCroomatograph | agers r200 | Liquid Chromato1raph [usacotamn | guteCro mmx100mm51 | Guard column 10/7/14, 10/13/14, 10/15/14, 10120!14, 10/23/14, 10/24/14 ETS-8-044.1 Agilent 1260 Betasil C18 (4.6 mm X 100 ram), 5 Analytical column [nctonvonume | 25004 | Injection Volume [aseSpectrometer |scpiegBossesaPiss00 | Mass Spectrometer [onsowse TT umospw, | Ion Source Betasil C18 (4.6 mm X 100 ram), 5~ 2, 5, or 10 l.tL Applied Biosystems API 5500 Turbo Spray Electrode [poy TT egw Polarity [o7 twae herez | Software Turbo ion electrode Negative Analyst 1.6.2 [oe i=r[a La eni| 0n| Table 4. Liquid Chromatography Conditions. Total Time Flow Rate Percent A Percent B Step Number eT omTm TemeITs-- wo Two |] Eo 01 FewTT 00 1 wo] 2 Fo Tem Tm 0Two | 3 e Tm e 0 1 a0 | 4 e Tm m 0o 1 wo | 5 Fe 1 wsTm LT oo 1 wo |] 6 7 EE TE 8 CoTee Tm1 wo 1 0 9 (min) om 0.00 0.50 4.00 6.00 11.0 13.0 13.5 16.0 16.5 19.0 (FL/min) (2mM ammonium acetate) (Methanol) ETS-8-044.1 ise Teo 750 90.0 750 90.0 1 100 | 10.0 10.0 750 70.0 30.0 750 70.0 30.0 750 20.0 80.0 750 20.0 80.0 750 10.0 90.0 750 10.0 90.0 750 90.0 10.0 750 90.0 10.0 33663300..00229966 aPAGE 8 OF 36 3M MN01596245 swme: 3M Environmental Laboratory Report No. IS011-01-03-17 Table 5. Mass Transitions. [em [ = me= Analyte [rma owe |roema | aw | PFBA Mass Transition Q1/Q3 [oso 213/169 413/369 Internal Standard [~3C4]-PFBA Mass Transition QI/Q3 217/172 PFOA [ I oT we| |= 413/219 a. 413/169 499/99 [13Cs]-PFOA rem 421/376 on PFOS [wero] | 499180 = 499/130 [13Cs]-PFOS fem 507f80 [1303]-PFBA 216/172 [~3C4]-PFBA 217/172 Cowen wuen | Cogeron | sears | [13C4]-PFOA 417/372 [~3Cs]-PFOA 421/376 [foE r pei roE s |Rcm | d eeros | sow | [13C,,,]-PFOS 503180 [lSCs]-PFOS 507f80 Dwell time was 20 or 50 msec for each transition. The individual transitions were summed to produce a 'total ion chromatogram" (TIC), which was used for quantitation. ra (1) Internal standard was included in lhe acquisition method on 10t7/14 and 10/13/14; however, internal standard calibration was not used for the quantitation of the analyzed samples. 3 Analytical Results 3.1 Calibration FE TRaS rr 10/7/13, 10/13/14, 10/20/14, 10/23/14, & 10/24/14 Analysis - Sam pies were q uantitated for all analytes fE eL o Se L T Deme against an external standard calibration curve. Calibration standards were prepared by spiking known Ee Tae t amounts of stock solutions into 50 mL of 50:50 methanol: laboratory reagent water. Between nine and fourteen standards ranging from 0.02 ng/mL to 5 ng/mL, 10 ng/mL, or 100 ng/mL (nominal) were nSL analyzed. A quadratic, 1ix weighted, calibration curve of the standard peak area counts was used to fit the data for each analyte. The data were not forced through zero during the fitting process. Calculating the standard concentrations using the peak area ratios and the resultant calibration curve confirmed accuracy of each curve point. C EE Aea ree SA 10/15/14 Analysis - Samples were analyzed against an external standard calibration curve. Calibration E SEE eR e ER standards were prepared by spiking known amounts of the stock solution into 50 mL of 90:10 methanol: laboratory Milli-QTM water. Nine standards ranging from 0.02 ng/mL to 10 ng/mL (nominal) were analyzed. A quadratic, 1Ix weighted, calibration curve of the standard peak area counts was used SR SR to fit the data for each analyte. The data were not forced through zero during the fitting process. Calculating the standard concentrations using the peak area counts and the resultant calibration curve confirmed accuracy of each curve point. ECE RREEAT er For both analyses, each curve point was quantitated using the overall calibration curve and reviewed ER BEER for accuracy. Method calibration accuracy requirements of 100+25% (100+30% for the lowest curve point) were met for all analytes. The correlation coefficient (r) was greater than 0.995 for all analytes in each analysis. ES 32 LSyIstemSuitability 3.2 System Suitability TR RE rO m A calibration standard was analyzed four times at the beginning of the analytical sequence to demonstrate overall system suitability. The acceptance criteria of less than or equal to 5% relative standard deviation (RSD) for peak area/ratio and retention time criteria of less than or equal to 2% RSD were met for all analytes. enPAGE 9 OF 36 33663300..00229977 3M MN01596246 eFonstmBiOtTyT17 3M Environmental Laboratory Report AIo. IS011-01-03-17 33Th.33o LOLLGiimfmoiittcooacffhQQaunuaaalnyntsiitisttaiattihioeonnlo((wLLeOsOtQQn)o)n-zero calbraton standard the curve tal moots nary ATaaonpnhrddeopLaarOcciocaQuutrrfaaobccrayyenakrrcesehq.cuuaiTinrerahmelyemLesein0sttGssisfaatohnnreddllloffoowarrneaswwlthyhtinieccoshhnc-aztthenhereboaaacrraefeloiaabu racctooi1ouunnnttTsssait/abrralnateldiooa6rdaarreien aithe at least tice hose of the curve that meets linearity least twice those of the appropriate blanks. The LOQ for all analytes can be found in Table 6. Table Table 6. 6. Limit ofQuantitation Limit of Quantitation ((LLOOGQ).). EE Loa A mgmt E 00ngA mi |E 160 agin |E 106nR g | 00 gem Analyte 1017/14 Analysis LOQ, nglmL 10/13/14 Analysis LOCI, nglmL i1~ [Tra ow | om | wa |ow| wa | wm | PFBA 0.0500 0.0250 [TeronTomo|ooo|oowe |oo | wm |oma | PFOA 0.0240 0.0240 [pros |ome | ome | oows |owe | owe| wm | PFOS 0.0232 0.0232 Tr Tatregae NA = Not Applicable (0 Aut acor of23 ans p10 (1) A dilution faotor of 2 was applied to the LOQ. 2 Aan cr wot OLS (2) A dilution factor was not applied to the LOQ. 10115/14 Analysis LOQ, ng/mL (2) NA 0.0192 0.0185 10/20114 Analysis LOQ, ng/mL (1) 0.0500 0.0480 0.0232 10f23114 Analysis LOQ, ng/mL (1~ NA NA 0.0232 10/24/14 Analysis LOCI, nglmL NA 0.0240 NA 33DaDun..ura44rilinnyggzeCCtdhootenoncctcootioiuunnnrrssfuueeiiimnoonffggtaehacCCcaahhayltelaaiinnbbnaalrsrylayatttituticcimioaaeollnnnssteeqqruueeesnnpccoeen,,seccooannnttidinnutuiiennggncctaaillibtrcaaattlioobnnravvteeorrnifficccuaarttivooennwsseaarmmepplsleebss ((CCcOOcVVnErs)l)w,weerArele aopnoarlyizeeddstoacmoenrfiremstuhsatwtehreeinbsrtraucmkeetnetdrbeyspCoCnsVe hanadt met method crea the initial calibration of 100% = 25% curve were still in control. All reported sample results were bracketed by CCVs that met method criteria of 100% -- 25%. 33Th.55ree BtByllpaaesnnkkossf banks wero prepared and analyzed wih the samples: Sobent blanks (procedural Trbbealhavrrneikkesesw))e.t,ydffpieieaelsdnd/ditornifppubsbblealaardnnkkks1ss,0, waaeennvrddaeleeuapqqturueeiipppmammreeeentndtht osardinnedsapeelaartnsecarllbymalzeanennkdckses.wffooitrhr DtPhterheowecwaesladaetuemrrrapssllaaemmsnp:lpkeslesos.l.vreEEneatsaccubhhslabbnwllkaaesnnrkke(rpreerrsoseucuvleltitdwewuwaraeasdsl aaareccnvccaiooyerrewdd.eiinndgg fo the method and used to to the method and used 1 evaliate method perfomance & determin the LOG evaluate method performance. Procedural blank results were and used to evaluate method performance to determine the LOQ for cach reviewed for each analyte. 33Lo.66w, miLL,aabbandCCohonnhttrlroaollcoSSpnpitikkoeessspi((eLLsCCwSSesrs)e) prepared and analyzed i lcate. The LCSsampleswere pILperorbeewcpp,raaamrrteeoidddr,ybbaMyyndisspphQiikigiTMnnhgglwakkabnnlcooeowrwnnnftoroaaplmmrsooopduuikunnecttsse wtoofhfeertthedeepeaarsennpaaiailyrtetceeodnficanentonodtr11aa00tniamomlnyLL.zeoodTffhllianeabbtoroLirprCaalSittcoosarrtyyew.errereTaaoghgdeeeinnutLttCwweSadattwseeairrmhoorprmlee11tsrmmwiaLlnecrooelff uilinannbcttohehreearttossaraaynmmtiMeeynilliS-mmQeaTacnMninnoewenrra3.t4ae7.ssr he sampes, to produce the the samples. All LCS resus were used (0 desired concentration. The LCSs All LCS results were used tu determine overall metiod were diluted with methanol determine overall method uncertainty in Section 3.7. TT2hh0ee%m,metewhthhooednaaceccvcaeelpputtaaatnneccdeeicncdreieteprreiansdseatntatetlesysaethhaaaltcthhheeaacvoveenrrcaaeggneetarrteeocconovvelereryvyoeolff LLACClSlSbLbCeeSs11m00e00%%l a++c22c0e0%p%twawniicthhe aacReRSrSDaD wit hefoloving exceptions: <20%, when evaluated independently with the following exceptions: at each concentration level. All LCSs met acceptance criteria 1i100n7/c71u/11d44dAAwnnaialhylystsihsise::rTTawnheecoolto,ww seset ooff LLCCSSss ffoorr PPFFBBAA hhaadd aa RRSSDD vvaalluuee ooff 4411%%.. AA mmeetthhoodd ddeevviiaattiioonn iiss included with the raw data. TThheeffoolllolwwiinngg ccaalccuulaattioonnss wweerree uusseeddttooggeenneerraatte dcaattaa iinn TTaabbllee 77 ffoorr llaabboorraattoorryy ccoonnttrrooll ssppiikkeess.. : ETT LCS Percent Recovery = CalculatedspiCkeoncentrationCncentratin. 100% kPS LCS% RSD vragoLCSreovry standardaveragedeviatiOnLcs LreCplSicateSrecovery * 100% 33663300..00229988 orce ror PAGE 10 OF 36 3M_MNO15%6247 3M MN01596247 si utnd ory 3M Environmental Laboratory Report No. IS011-01-03-17 THR Labatt be Reson Table 7. Laboratory Control Spike Recovery. oT ETS-8-044.1 I Cn Extemal Calibration Analyzed 10/7/14 co=in Lab ID S am LCS-141007-1 fe =| = LCS-141007-2 pr" vn | re LCS-141007-3 Average 4- %RSD fromeLn LCS-141007-4 ns LCS-141007-5 a LCS 14100T6 Average 4- %RSD i LCS-141007-7 jrLCS-141007-8 LCS-141007-9 Ee En Average _+ %RSD PFBA Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) 0.198 0.198 0.198 19.8 19.8 19.8 157 157 157 0.178 0.331 0.166 113% _+ 41% (1) 19.4 19.4 20.0 99.1% -+ 1.7% 173 170 164 108% 4- 2.3% %RecoveQ/ 89.8 167 83.6 98.1 98.2 101 110 108 105 on PFOA (Linear + Branched) Spiked Calculated Concentration (nglmL) Ae0.190 Jie0.190 oe0.190 en 19.0 w 19.0 wn = 19.0 7 150 > 150 a 150 Concentration {ng/mL) 0.184 0.202 0.193 101% _+ 4.5% 19.2 19.4 19.8 102% -+ 1.5% 158 152 150 102% 4- 2.6% %Recovery 96.8 106 101 101 102 104 105 101 100 E pretir ven ETS-8-044.1 Extemal Calibration Analyzed 1017/14 PFOS (Linear + Branched) Lab ID rmLCS-141007-1 prLCS-141007-2 es LCS-141007-3 f --m Average 4- %RSD LCS-141007-4 LCS-141007-5 Spiked Concentration (ng/mL) 0.184 0.184 0.184 18.4 18.4 Calculated Concentration (ng/mL) a0.153 a0.158 jo0.158 me 0 8&0% _+ 2.1% 16.8 17.2 %Recovery 82.9 86.1 85.9 91.4 93.2 LCS-141007-6 Average 4- %RSD Ss LCS-141007-7 ae LCS-141007-8 --" LCS-141007-9 or Average _+ %RSD 18.4 145 145 145 17.8 93.7% _+ 2.8% 164 152 150 107% _+ 4.9% 1 Sm -------- (1) RSD value did not meet acceptance criteda of -<20%. 96.6 113 105 103 33663300..00229999 ners PAGE 11 OF 36 swmorssazes 3M MN01596248 SFuEanriotmiRL0z1o1o2m16t5o1r7y 3M Environmental Laboratory Report No. IS011-01-03-17 `TTaabbllee 77 ccoonnttiinnuueedd.. Erseont ETS-8-044.1 Soma Cartan Extemal Calibration ppion Analyzed 10/13/14 Lab ID Cs ara LCS-141013-1 ws worsz LCS-141013-2 Les woaa LCS-14101 3-3 LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReeccoovveerryy.. ConScpoinremsion Spiked Concentration (ng/mL) 01080.198 osO. 198 ois0.198 PFBA Calculated Concentration (n~l/mL) om0.176 on0.170 om0.177 %Recove~ mo89.0 wr85.7 m289.2 Average _+ %RSD wsoraa LCS-141013-4 Lesonas LCS-141013-5 Les oa LCS 141013-6 " 1.98 2m 1.98 200 1.98 88.0% _+ 2.2% 1.91 2.06 2.01 96.6 104 101 Average + %RSD ree LCS-14101 3-7 wes oae LCS-141013-8 15.9 15.9 101% -+ 3.7% 15.8 17.2 99.3 108 [Amognevnso LCS-14101 3-9 Average _+ %RSD 00% 154% 15.9 17.4 110 106% _+ 5.4% a PFOA (Linear + Branched) Spiked Concentration (nglmL) I)0.190 ow0.190 ois0.190 To1 90 1%1 90 pry1 90 Calculated Concentration {ng/mL) om0.182 om0.178 oi0.190 96.5% _+ 3.3% 1.81 1.92 1.88 %Recovery 95.6 93.9 100 95.4 101 98.8 98.a,% _+ 2.9% 15.2 16.5 108 15.2 17.1 113 [wea 15.2 16.9 111 111% _+ 2.3% ETS-8-044.1 soni gs 01e 304 | Extemal Calibration Analyzed 10113/14 PFOS (Linear + Branched) | Lab ID esas LCS-14101 3-1 wsonz LCS-14101 3-2 rane LCS-141013-3 Spiked Concentration (ng/mL) 0.184 0.184 0.184 Calculated Concentration (ng/mL) oro0.150 ose. 0.146 oso0.150 %Recovery ws81.6 mr79.1 aa81.4 Average %RSD Lessa LCS-141013-4 Lesonas LCS-14101 3-5 Leswoss LCS-14101 3-6 Average _+ %RSD resLCS-14101 3-7 sons LCS-14101 3-8 wes wae LCS-14101 3-9 80.7% _+ 1.7% 1.84 1.53 83.2 1.84 1.58 85.9 1.84 1.56 84.9 wr 50 14.7 wr oa 14.7 ur oz 14.7 84.7% + 1.6% 14.0 14.3 14.3 95.0 97.3 97.2 Average _+ %RSD 96.5% _+ 1.3% 0) ASDvelo dd netrctcoprc <a2. (1) RSD value did not meet acceptance criteda of -<20%. 33663300..00330000 Face zor PAGE 12 OF 36 3M_MNO1596249 3M MN01596249 SFuEanriotmiRL0z1o1o2m16t5o1r7y 3M Environmental Laboratory Report No. IS011-01-03-17 `TTaabbllee 77 ccoonnttiinnuueedd.. Erseont ETS-8-044.1 Soma Cartan Extemal Calibration pepo Analyzed 10/15/14 Lab ID LCs awe LCS-141015-1 ws wosz LCS-141015-2 Looms LCS-141015-3 LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReeccoovveerryy.. he PFOA (Linear + Branched) Spies Spiked Conconrmion Concentration Calculated Concentration (ng/mL) om0.191 owO. 191 om0.191 (ng/mL) ors0.175 oi0.175 om0.181 %RecoveQ/ 91.6 91.5 94.6 PFOS (Linear + Branched) Spiked Concentration (n11mL) Calculated Concentration {n1/mL) %Recovery 0.185 0.185 0.185 0.179 0.183 0.181 97.0 98.8 98.0 Average 4-%RSD wsores LCS-141015-4 Les-anorss LCS-141015-5 Les worse LCS 141015-6 92.6% _+ 1.9% Tor 1.91 1.98 104 @s 1.91 1.91 99.9 sor 1.91 1.92 101 97.9% _+ 0.92% Ir Ee) 1 85 1.90 103 18s PY 1 85 1.88 102 tos on 1 85 1.87 101 Average 4- %RSD reer LCS-14101 5-7 Lesorse LCS-14101 5-8 102% -+ 2.1% 7.60 7.89 104 7.60 7.92 104 102% -+ 0.98% 50 736 7.50 102 ar 736 7.47 101 [hwogewmso| LCS-14101 5-9 Average _+ %RSD 7.60 voswrnan| vomeersw 8.05 106 103% _+ 1.1% 736 7.65 102% + 1 104 | ETS-8-044.1 E songe s 01504 | Extemal Calibration Analyzed 10115/14 ae | [13C41-PFOA os [13C4-PFOS Lab ID esas LCS-14101 5-1 wesorsz LCS-14101 5-2 Loswnss LCS-141015-3 Spiked Concentration (ng/mL) 01%0.199 01%0.199 010.199 Calculated Concentration (ng/mL) oar0.201 oan0.201 ois0.198 %Recovery 0101 "101 os99.5 Spiked Concentration (ng/mL) 0100.190 0100.190 oi0.190 Calculated Concentration (ng/mL) om0.192 om0.192 om0.191 Average 4- %RSD Los-anorsa LCS-141015-4 Lesorss LCS-141015-5 Less LCS-141015-6 [awogoenmso Average 4- %RSD 1.99 1.99 11.99 101% _+ 0.86% 20 o 0 2.10 106 20 @ 1% 2.03 102 201 sor 150 2.01 101 wwrzen | 103% _+ 2.6% 1 90 1 90 1 90 1) RSDvole dd ekkdci5205. (1) RSD value did not meet acceptance criteria of -<20%. 101% _+ 0.37% 1.99 1.94 wwe1.94 103% + 1.7% %Recovery on101 "101 oo100 os105 0102 0 | 102 33663300..00330011 Facer PAGE 13 OF 36 3M_MNO1596250 3M MN01596250 si utnd ory 3M Environmental Laboratory Report No. IS011-01-03-17 Talo 7continued. Table 7 continued. oT ETS-8-044.1 oern Extemal Calibration Analyzed 10/20/14 Lab ID -- LCS-141020-1 frLCS-141020-2 ----" LCS-141020-3 Frere s-- Average + %RSD i. LCS-141020-4 Es LCS-141020-5 a LCS 141020~6 Average + %RSD -- LCS-141020-7 on LCS-141020-8 LCS-141020-9 ---- Average _+ %RSD Laboratory Gonrl Sik Racovry. Laboratory Control Spike Recovery. =Spiked coin Concentration (ng/mL) rr 0.199 |0.199 vn | em 0.199 mo wiz 19.9 n19.9 wn19.9 PFBA Calculated Concentration (ng/mL) 0.164 0.199 0.169 89.1% + 11% 22.0 21.6 21.3 109% -+ 1.4% 157 177 FT 157 173 157 172 111% _+ 1.6% %RecoveQ/ 82.3 100 85.1 110 109 107 113 110 110 i PFOA (Linear + Branched) Spiked Concentration (nglmL) Calculated Concentration {ng/mL) %Recovery 0.191 0.189 98.7 0.191 0.191 100 0.191 0.195 102 proves 100% + 1,7% Fra 19.1 20.9 109 Fl 19.1 20.3 106 nou 19.1 20.2 106 107% -+ 1.6% z151 165 110 >151 162 107 151 160 106 te 108% + 1.9% Efre eien ETS-8-044.1 Extemal Calibration Analyzed 10/20/14 [| PFOS (Linear + Branched) | rpre---- Lab ID LCS-141020-1 LCS-141020-2 Spiked Calculated rvoe | Twaw | Toam Concentration (ng/mL) 0.185 0.185 Concentration (ng/mL) 0.157 0.165 %Recovery 84.7 89.2 LCS-141020-3 Average 4- %RSD i LCS-141020-4 -- LCS-141020-5 fe LCS-141020-6 Average _+ %RSD a LCS-141020-7 re LCS-141020-8 -- LCS-141020-9 0.185 18.5 18.5 18.5 146 146 146 0.162 87.6 87.2% -t- 2.6% ran18.5 nol ow 17.9 ol. 18.1 100 96.7 97.9 98.2% + 1.7% 159 109 152 104 150 103 1 Sm -------- Average _+ %RSD 105% _+ 3.1% (1) RSD value did not meet acceptance criteda of -<20%. 33663300..00330022 nner PAGE 14 OF 36 swmorssezs1 3M MN01596251 Talo 7continued. Table 7 continued. oT ETS-8-044.1 rSe ee Extemal Calibration Analyzed 10/23/14 Lab ID RSLCS-141023-1 frLCS-141023-2 prLCS-141023-3 [-- Average 4- %RSD i. LCS-141023-4 as LCS-141023-5 a LCS 141023-6 Average 4- %RSD i LCS-141023-7 jrLCS-141023-8 Laboratory Gonrl Sik Racovry. Laboratory Control Spike Recovery. d PFOS (Linear + Branched) =Spiked eon Concentration (ng/mL) Calculated Concentration (ng/mL) %RecoveQ/ am 0.185 | om | om 0.185 ve | ew | om 0.185 miTia x 1.85 | 1.85 bl 1.85 or 7.36 ou 7.36 0.143 0.155 0.155 81,7% _+ 4.4% 1.74 1.74 1.70 93.4% -+ 1.5% 6.97 6.97 77.5 83.9 83.6 94.3 94.0 91.8 94.7 94.7 LCS-141023-9 7.36 6.86 93.2 Average _+ %RSD 94.2% _+ 0.92% E preiren E, ETS-8-044.1 Extemal Calibration Analyzed 10/24/14 PFOA (Linear + Branched) Lab ID reLCS-141020-1 pr---- LCS-141020-2 fs LCS-141020-3 imma] Average 4- %RSD i LCS-141020-4 -- LCS-141020-5 fe LCS-141020-6 Average 4- %RSD fom LCS-141020-7 re LCS-141020-8 -- LCS-141020-9 Spiked Calculated Concentration (ng/mL) Ta 0.191 | oe 0.191 | am 0.191 amnn 19.1 a 19.1 o 19.1 em 151 Concentration (ng/mL) 0.213 0.216 0.236 116% _+ &7% 21.0 20.7 20.6 109% _+ 0.92% 169 151 164 151 161 %Recovery 112 113 124 110 109 108 112 109 106 1 Sm ---------- Average _+ %RSD 109% _+ 2.8% (1) RSD value did not meet acceptance criteda of -<20%. -- i-- d 3M Environmental Laboratory Report No. IS011-01-03-17 33663300..00330033 J. PAGE 15 OF 36 swmorssazs2 3M MN01596252 eFonstmBiOtTyT17 3M Environmental Laboratory Report Rio. IS011-01-03-17 A33n..a77ytcAAanlnaualnylcyetrtiticcaiaanltlyMMeeattshheoodddonUUnincscoerercrtataaliiQnnCttyydaa hts contol chatod and used to evalua ASmmeneatathhlryootiddrcaaacliccucuknurcraaoeccrtynyaiaannntyddcispprrobeecacicsisseiioodonno.. 0nTThhhIieesntommreSiectltahhloooQfddACuucnncdccuaeerrtaarttacatiyhinnaotttyyisiissscccoaanl(lcticrnuoul5laat)cteehbddarfftoeeolldloocwawniinndgfgourEEshTeTSdeS--Ot11o2C2.e-00va11am22lu..ia22t.ee.TThheeFor smcmteaeinlthndoaedrdEETodTSeS.vb-8i8ay--t00iom44ns44t.is11,p,cithahnleecgmumloatostnestdtsrrtfeeoaccrneetdnhnatetrifdsitfetydyteOQovCfCiastcascanmumpbryalpclaeeysswarewesercureletusous1(siene2d,d%..AT)cThohbheetaaacinnnoaearydlyaiftcoiscarpaltlehmmenedeiQ6tsnhCooaddsucanumocnnpecfrleeterstana.icinnFetoyr lisevceallcoful8a5te%d. by multiplying the standard deviation by a factor of 2, which corresponds to a confidence level of 95%. TTaabblel88e.. AAnnaallyyttiiccaall MMeetthhoodd UUnncceerrttaaiinnttyy [oe[oliiny, [Heotigimsm] Analyte [oma | ws Two| PFBA [Teron Tow [+ | PFOA Ceres Tass [wv | PFOS Standard Deviation (%) 12.5 6.56 8.55 Method Uncertainty (%) _+ 25 + 13 _.t 17 33Ta..r88get FFaiieenllddaMMfaatdtrrimixxaSStppisikkpieeksses(((FFFMMSSS)))were preparedfo set locals. Fotssamping oven, TFaFpaMUprSSigceatsstaaaimmncpaptllyoleetressefwiweceeldorrleemecccaoootrldlilxeemccsitapeeiddxke.aasftF(FeeAMig'gShst)wwsseaaermmroeppgilpionnrngegepraallorioececdadattifobooynrrssasdettdoloeicnvvtgeelarorifcyymaetittaohhsnaaustr. tethhdFeeovroaatlnnhuaaismliyestcoiacafamllfpilemmilnedegtsthhaeoomvddepnl'ites,s at1sopa0mpaaplicccloaoenbntltceaaoiinltnoleecrrtihssoeppni.ickkoeellddeFcbbtMyeydStthhmeeralelatacrbobixovo.reraraFtitoeoMrsrySyswiwitwtithhheirnttehhemegeetttanahrreggoreeadttteaaadnncaabcllyeyypttaetedssadnirpcnregicoracotrmoicessiahhaisippupporiiefnndgg1v0ssoa0laummm3p0eple%occfoocfninoettnlaadfiinniseemarrmssbpfoeolerlr s"a"uaUnnmnakkypnnslooeswwnnc"o"ofllccetoocammtioppnoao.nnneeranFietsMssSiinnorfttehhceeeorvsseoaramisemspleewFimmthMaainiStirixxmcoeddntoochaonnndototatalcssiciogcennpsaiftiacnmnautcnsetytlycDrinnieteteerrarieafferrleeoafswwt1iit0hh05_0tt+h%h3ee0%oeefxxctttroaaenccfitiirocsmnnaaam[hnnapddt accPoonRnnaOccleySensntisitrrnaatohtiifoeonnthfetooodabbnoemaalccytootneensssiisddpoeeifrrkeieidnndgteaasrnneosuaat.tpppoprnroFopcpMroriSiaanttseeciosssnpptciieekcoenefdtrllIaeentvvioeecllna. saTTnmhhdueesatrrreefbfceeehrreeeanndtcceeliesssaottsamatennrdd5saa0.rr%ddssToffaoof rrothPPeFFOOssAaAtmaaptnnhledde lPoFcOatSionins athned fsieplidkimngaterivxesspfikrinwghsiocluahtioanrgceotnsainsateldy oFf MlinSewaar sanpdrebpraarnecdhed isomers. Table 9 lists the locations and spiking levels for which a target analyte FMS was prepared. IsInnpkaadedksdtitoi(onnR,,Sfisioe)lldd ommfaat[rti(xCssIppPikkFeeBssAfo,orr [rthi"issCppPrrooFjjeeOcctAt ccoaonnsdnisst[e"dioCosfLfPtlsFteaOabSdll,e siswcohltioocppheo sswuueTrrrooeggaaattdeedrreeedccooavvteerryya ssnttaoanmndidanaarrdld wscCpoaoinnskcoeesesennlttr(eaaScttRtiooeSnndsfo)ooff or00.fe.11p[r1non3sCge/3gmn]t-LPPFtBoAFaa,ll t[sAsh1a3aCmm4p[]el-ePCF.bbOHooaAttbtleesaslneppddriioPr[r1F31tCOo4As]s-aaPwmmFapOpsllSees,eoclowoellchleeticccethtdoionno.w. errTTeephhreeaesd([e1dCn3et.CdJ3Pa]F-abIaOtebAlea,eleddannoPPdmFFitnBEhaAAel trw{[laSaCCsighfs]l-eeIaalbebseceiutleeotdddatPPtoFOoOreSSrpercewwosaavessenrtssyeePlsleFetccBattnAeedddatthrtoedsrr[~ewe3ppoCrrree4ess]-eeoIanntbttePlPseRFdoOOkPSeS,Fd. OaAFFsoolwfllloaeowswniidnnsgegedlesscaattmmehpdeplrleeetofoaarrnneeaa,pllyrynsesoisisse,S,nutitTwPwGaFgasOsaeAss,uufssaoppnceedoccvittehrsdeyd standardrsulswee used 0assesssamplerecovery. that the surrogate recovery standards were not spiked standard results were used to assess sample recovery. as intended; therefore, no surrogate recovery Thofolowingcacaton asused1 generateth fadmati spk recovery inSectan 4 of ho apart: The following calculation was used to generate the field matrix spike recovery in Section 4 of the report: FMS Recovery = (Samplc Conccntration of FMS - AvcragCSpike ConcentrationCnccntratin : Ficld Samplc & Ficld Samplc Dup.), 100% Table 9 Feld Matrix Spike Lovel. Table 9. Field Matrix Spike Levels. f[ reee mma gmt)| G] uy)| git) Sampling location Surface Water (SW) locations: [a nnas | wo [om [ome| MR.IW09d, MRIW14, MRIW19b, MRI25f Vo 0 sors Interstitial Water (IW) locations: [Erem[m re [e em [e em] MRIW14d and Trip Blank Low Interstitial Water (IW) locations: MRIW09, MRIWlgd. MRIW25f, and FpEr Ei EE~ [eee] Trip Blank High PFBA (ng/mL) 1.01 1.01 PFOA (ng/mL) 0.996 0.996 PFOS (ng/mL) 0.996 0.996 5 05 4 98 4 98 ore rsorn PAGE 16 OF 36 33663300..00330044 SW_MNo1S56253 3M MN01596253 sepimes 3M Environmental Laboratory Report I~1o. IS011-01-03-17 SRSA se 33..99 LLaabb MMaattrriixx SSppiikkeess ((LLMMSS)) BR SoE necse Due to noncompliant surrogate recovery standards using external standard calibration, laboratory RR Se Sn matrix spike (LMS) samples were prepared for all sample locations that did not contain a field matrix Ee OE EE T nS spike sample. The LMSs were used to verify ~at the analytical method is applicable to the collected matrix. LMSs were generated by adding a measured volume of standard solution to an aliquot of the primary sample. The spike concentrations are presented in Table 10. e ee e et rn r LMS recoveries within method acceptance criteria of 100+30% confirm that "unknown" components in EL the sample matrix do not significantly interfere with the extraction and analysis of the analytes of interest. LMS concentrations must be 50% of the sample concentration to be considered an Eee appropriate spike level. LMSs are presented in section 4 of this report. A The following calculation was used to calculate the lab matrix spike recovery in Section 4 of the report: LMS Recovelw~ = (Sample Concentration of LMS - A,~reragespike ConcentrationCncentradn : Field Sample & Field Sample Dup.), 100% Table 10. Lab Matrix Spike Levels. [ssmpgtomsors | eran[ron [ros| Sampling Locations r e err-- m Surface Water (SW) locations: MRIW09b, MRIW09, MRIW09f, MRIW14b, MRIW14d, MRIW14f, BEER MRIW19, MRIW19d, MRIW19f, MRIW25b, MRIW25, and MRIW25d Final Concentration (nglmL) PFBA PFOA PFOS 0.998 0.957 0.926 Interstilial Water (IW) locations: MRIW09f and MRIW25d E Smm I InterstilJal Water (IW) locations: m Toe ole] MRIW09d, MRIW14, MRIW14f, and MRIW19f [=Interstilial Water (IW) location: Emm To To oa MRIW09b nEth r. [or |= Interstilial Water (IW) locations: MRIW19, MRIW25b, and MRIW25 Interstilial Water (IW) locations: E ees mm Tw[e ww] MRIW14b and MRIW19b 4.97 9.98 49.7 98.9 4.77 9.57 47.7 94.9 4.61 9.26 46.1 91.8 33663300..00330055 en PAGE 17 OF 36 3M MN01596254 SFuEanriotmiRL0z1o1o2m16t5o1r7y 3M Environmental Laboratory Report No. IS011-01-03-17 44 DDaattaa SSuummmmaarryy aanndd DDiissccuussssiioonn TTmhhaetxatabblslpeeisskbebeerllooewwcssouumnmmeamrfaoirrzizteehetthsheamsspaalmmipnplgleelrroeecssautulilttossnsaannadds twtaaerrlggleeattsaatnnhaaelylTtyerpffieeBildadnmmk.aatRrtiexsssuppilkkse aoonfrdllavababoolrruaaettsooarryyre aVamavvakeetirrreaiaxsggmseeprariokoyueuvnnarddersecyddosvoteortithehhrsreeffeeorysrositmihggnentfifihsicocaasamnentptilffisinggtguuorrleoiescsaahacticecoconoarsrddwaiisnndggwalteto.oll EEaFPPsiAAetlhdrreoomTuuannrliddpriiinnxBgglsarrpnuuklklee.ess..RanBBedeseucclbaatsouurssaaeenldooofrfvyrramooluuaunentddsriiinangxgre., vss`aapppiliukpkreeeosprrreemiccaooatvvyeeerfvriaieeorssyhremsmelieGegiethvtitienlnynggfrmtothahmteer immthxeeotatshnheododdlihsaaeteccdcceeeinppsittpahaneencccreeiawrceiriqdeterauritiaaaa. oonfFfti_+e+il33d00rm%%an,a,gtddreieexsmm.soponinsktsertraaalnteed tat the method is laboratory matrix that the method is appropriate for the given matrix and their respective quantitative ranges. rFFoolellowociwngiowhntheevgereiienntitgiiaarrlel aaaitnneaarleltyyhssiasissnuu1ssi5inn0gg%,ninftieonrmcnalaluldssinttagatnnhddeaaUrrddpccbaalllibtrarattoiosnna,m,pmalleomss.osttTahlleooFff thNhoSe FFreMNcSSovsseraaimmepspllaeeppear brrbeeiaacsssopeevoddenrsihie.iggshhwTddheueurreeesfotgootrretheha,eetehtirnetethsemaarnanmalp1ll5sset0tsaa%nned,daairnrrdcedlurrqdeeuissnappgnootntnihssaeeetatrbbdiepeuiinsbngiglaanangppkpaprsreaoomxxripmaaleatsstete.lalyyTnodhonaenereFdhhMacalSallfloobrfecfcatrhoteeovneee,rxixewppsheeiccacttpheepddreeasruled IIrinenocsssapuutorrorrnnoossgg.eaa.tteBeTarhraseececrooedvvfeooerrnreyyst, tstohtaaenindnsdtaaaerrmrdndaspsllewwssitittawhhnedaarapperppdqrrrouexoaisnxmptiiaotamtnetaselyetda55eun00lsd%%iyntgrhreeeccxooftvveeeerlnrryaymwlwisaitttahhtnttdhshaeepredexkxcccearepelpitcbtoirivoaoentniroioonfef,stt,wwothowicssahaasmmreppsllueelted wccloeoocrnnacectliloupunddrseee.ddptBthhaaaarsltfetetohdhdreeossnsuautmtrhopreogingaignal.tteeesrsnTaaahlennrsddetafninontredeearm,nrdaaalllrssesttasaapmnnpoddlnaaesrrseddwssaenwwderererteehqessuppfaiiienkkletdedidmaiienandctcroioaxrrrresrpceritckleyteaplaotyrtretthcheeoedvuetsmimirieneegs,tehhxietetwbbeaoamsttatleless PwsFstteaOarnendAaapsnrrudderpccoaaagrlebiabdrtraaefootriornen.ss.aumlNNspoolfinssorguuT.rsroaoTgmghapaetltereeerfrloeeorccceooa,tvviaeeolrlrnyysWass-tmtaaAnpnRdldeIaasrYrddw9err1eer.essuuqilttussaawanhriteictarhreteephpdooerraetsnedudd,r,rwrwoeigpithahotretthheeredeeecuoxsxvcineecgrpeyteiopsxnattenooridnffataothrhlnedes `wereadded a the me ofsamplepreparanadtdliuoonn. PFOA surrogate results for sample location IW-MRIW'I 9f, in were added at the time of sample preparation and dilution. which the surrogate recovery standards cUUssriinenggaaewxxitteohrmntaarllessfttoaalnnldodwaairrnddgcceaaxblicbrraeatptoitonno,, aa1ll ffiieeldd mmaattriix ssppiikeess aannddllaabboorraattoorryymmaartriex ssppiikkeoss mmeelt aacccoeappitaannccee criteria with the following exception: I5IW2W1H-M%M.RRIIW WS1i14n4gcd:a: tTThhhoeossasaammmpylspoelello/sscaaamtmippoinlee hddauudppvilieccaralyteehRiRPgPhDDRffPoorDr SPPfEFoBBraAAlwwaaanssal11y22t88e%%,..thTTehhseeaFFmMNplSSereroectcouovveesrryywow-aass e5pprp2reeo.1ppr%aatrre.eedddSuaasinnnicddnegrreotthh-aaeennnasalaalyymlzzepeadldn.e.alloTTycshhaieetsir.oroen-aTahnhnaeadllyvymseesisrtyhccohooidngnfhfuirinmRcmePeerddDtasttihhnfeeotyrtinahitlaaliasal nbcraeeulseylutnleltssse,xaatpnnhaddenttsdhhaaeomdsspataolremo4pls8elet%wssoeafttosrrharaePss-bFboAeo.enn reported using the initial analysis. The method L~ncertainty has been expanded to _+48% for PFBA. 33663300..00330066 Facer PAGE 18 OF 36 3M_MNO15%6255 3M MN01596255 SRST 3M Environmental Laborato~ R epo# No IS 0~i1-0"i-03-17 Table 11. CGMN SW MRIW09b 141001 woe lew | [emaLon|gweLao | [omweLo]| 31~1 LIMS ID ISOl 1-01-03-17-001 EETTE ISO11-01-03-17-002 Description CGMN-SW-M RIW09b-0-" 41001 CGMN-SW-M RIW09b-DB-14100" PFBA Concentration (nEI/mL) <0.0500 <0.0500 %Recovery NA NA PFOA Concentration (ng/mL) 0.0332 0.0274 %Recover), NA NA PFOS Concentration (nEItmL) <0.0232 <0.0232 %Recovery NA NA ISOll -01-03-17-001 ; LMS CGMN-SW-M RIW09b-LMS (lppb) 1.15 115 1.09 11" 0.904 97.6 Average Concentration (ng/mL) 4- %RPD <0.0500 ng/mL 0.0303 ng/mL 4- 19% <0.0232 ng/mL rncom mon NA = Not Applicable Table 12. CGMN SW MRIW09 141001 wets 3M LIMS ID lamer Description 170 eure) SG Lene PFBA Concentration (nEIImL) %Recove~ PFOA Concentration (n~lmL) %Recover~ ISO11-01-03-17-003 CGMN-SW-MRIW09-0-141001 ISO11-01-03-17-004 CGMN-SW-M RIW09-DB-141001 ISOll-01-03-17-003; LMS CGMN-SW-MRIW09-LMS (lppb) Average Concentration (ng/mL) + %RPD <0.0500 NA <0.0500 NA 1.10 110 <0.0500 ng/mL <0.0240 NA <0.0240 NA 1.04 109 <0.0240 ng/mL EE er PFOS Concentration {n~/mL) %Recover~ <0.0232 NA <0.0232 NA 0.888 95.9 <0.0232 ng/mL NA = Not Applicable PAGE t9 OF 36 3M_MN01596256 33663300..00330077 red 3M Environmental Laborato~ Repo# No IS0~i1-01-03-17 Table 13. CGMN SW MRIW09d 141001 [omPe FBA wen PFOA we PFOS | 3M LIMS ID Description Concentration (ng/mL) %Recevery Concentration (ng/mL) %Recovery Concentration (nglmL) %Recovery ISO11-01-03-17-005 CGMN-SW-MRIW09d-0-141001 ISO11-01-03-17-006 CGMN-SW-MRIW09d-DB-141001 ISQ11-01-03-17-007 CGMN-SW-MRIW09d-FMS-141001 CS Average Concentration (ng/mL) 4- %RPD ets NA = Not Applicable Table 14. COMN SW MRIW1O41900!1 Table 14. CGMN SW MRIW09f 141001 <0.0500 NA <0.0240 NA <0.0232 NA <0.0500 NA <0.0240 NA <0.0232 NA = TTT Si =| 0994 98.4 <0.0500 ng/mL 0.916 92.0 <0.0240 ng/mL 0.840 84.3 <0.0232 ng/mL | ema PFBA Ten[wes PFOA PFOS | 3M LIMS ID Description ISO11-01-03-17-008 CGMN-SW-M RIW09f-0-141001 ISO11-01-03-17-009 CGMN-SW-M RIW09f-DB-141001 ISO11-01-03-17-008; LMS CGMN-SW-M RIW09f-LMS (1 ppb) Ceampizave | Average Concentration (ng/mL) 4- %RPD rents NA = Not Applicable Concentration (nglmL) %Recevery Concentration (nglmL) %Receveq/ Concentration (ng/mL) %Recovery <0.0500 HA <0.0240 NA <0.0232 NA <0.0500 NA <0.0240 NA <0.0232 NA amon| mmr | wma] 1.12 112 <0.0500 ng/mL 1.06 11 " <0.0240 ng/mL 0.906 97.8 <0.0232 ng/mL PAGE 20 OF 36 M_norsoe2s7 3M_MN01596257 33663300..00330088 SSE 3M Environmental Laborato~ R epo# No IS 0~i1-0"i-03-17 Table 15. CGMN SW MRIW14b 140930 [omPFBA 1 wea PFOA [we PFOS ] 3M LIMS ID Description Concentration (ng/mL) %Recevery Concentration (ng/mL) %Recovery Concentration (nglmL) %Recovery ISO11-01-03-17-0" 0 CGMN-SW-M RIW14b-0-" 4030 ISO11-01-03-17-0" 1 CGMN-SW-M RlW14b-DB-140930 ISOll-01-&3-17-0"0; LMS CGMN-SW-MRIW14b-LMS (1ppb) Conswtomnym 5000 | Average Concentration (ng/mL) 4- %RPD aero NA = Not Applicable Tala 1. CGNSW MRIWHA 14099 Table 16. CGMN SW MRIW14 140930 <0.0500 NA <0.0500 NA tsoget 1.13 113 <0.0500 ng/mL 0.0789 NA <0.0232 NA 0.0711 NA <0.0232 NA |_owmm|etawimgwm e 1.08 105 0.0750 ng/mL 4-10% 0.882 95.2 <0.0232 ng/mL mweT wm] PFBA PFOA PFOS 3M LIMS ID Description Concentration (nglmL) %Recevery Concentration (nglmL) %Recovery Concentration (ng/mL) %Recovery ISO11-01-03-17-0" 2 CGMN-SW-M RIW14-0-140930 <0.0500 HA <0.0240 NA <0.0232 NA ISO11-01-03-17-0" 3 CGMN-SW-M RIW14-DB-140930 ISO11-01-03-17-0" 4 CGMN-SW-M RIW14-FMS-140930 Crmmpmisomre |ssn | abe |sem] Average Concentration (ng/mL) 4- %RPD erate NA = Not Applicable <0.0500 NA 0991 98.1 <0.0500 ng/mL <0.0240 NA 0.922 92.6 <0.0240 ng/mL <0.0232 NA 0.827 83.0 <0.0232 ng/mL PAGE 2t OF 36 aw_notsss2s8 3M_MN01596258 33663300..00330099 red 3M Environmental Laborato~ Repo# No IS0~i1-01-03-17 Table 17. CGMN SW MRIW14d 140930 [omPFBA 1 wea PFOA [we PFOS ] 3M LIMS ID Description Concentration (ng/mL) %Recevery Concentration (ng/mL) %Recovery Concentration (nglmL) %Recovery ISO11-01-03-17-0" 5 CGMN-SW-M RIW14d-0-" 4030 ISO11-01-03-17-0" 6 CGMN-SW-M RlW14d-DB-140930 ISOll-01-&3-17-0"5; LMS CGMN-SW-MRIW14d-LMS (1ppb) Consemym $5000 | Average Concentration (ng/mL) 4- %RPD aero NA = Not Applicable Tala 1. COMNSW MRIWIAI 140930 Table 18. CGMN SW MRIW14f 140930 <0.0500 NA <0.0240 NA <0.0232 NA <0.0500 NA <0.0240 NA <0.0232 NA age |coral| aww 1.11 111 <0.0500 ng/mL 1.11 116 <0.0240 ng/mL 0.91 fl 98.4 <0.0232 ng/mL mweT wm] PFBA PFOA PFOS 3M LIMS ID Description ISO11-01-03-17-0" 7 CGMN-SW-M RIW14f-0-140930 ISO11-01-03-17-0" 8 CGMN-SW-M RIW14f-DB-140930 ISO11-01-03-17-0" 7; LMS CGMN-SW-MRIW14f-LMS (1 ppb) osm pmisomre | Average Concentration (ng/mL) 4- %RPD eat NA = Not Applicable Concentration (nglmL) %Recevery Concentration (nglmL) %Receveq/ Concentration (ng/mL) %Recovery <0.0500 HA <0.0240 NA <0.0232 NA <0.0500 NA <0.0240 NA <0.0232 NA ssabn r | s] eme] "I.08 "108 <0.0500 ng/mL 1.07 "1 "12 <0.0240 ng/mL 0.892 6.3 <0.0232 ng/mL PAGE 22 OF 36 aw_No1s96259 3M_MN01596259 33663300..00331100 red 3M Environmental Laborato~ Repo# No IS0~i1-01-03-17 Table 19. CGMN SW MRIW19b 140930 me J [orm l1lwea [ lwre)] 3M LIMS ID ISO11-01-03-17-0" 9 PE a A 5[FFLhet ISO11-01-03-17-020 Description CGMN-SW-M RIW19b-0-" 4030 CGMN-SW-M RlW19b-DB-140930 PFBA Concentration (ng/mL) 0.0808 0.0549 %Recevery NA NA PFOA Concentration (ng/mL) 0.200 0.200 %Recovery NA NA PFOS Concentration (nglmL) 0.139 0.135 %Recovery NA HA ISO11-01-03-17-021 CGMN-SW-M RIW19b-FMS-140930 1.08 100 1.14 4.1 1.01 87.7 Average Concentration (ng/mL) 4- %RPD 0.0679 ng/m14- 38% (~) 0.203 ngtmL 4- 2.5% 0.137 ng/mL 4- 2.9% eeEnncoackm17m08oentsac 4535. NA= NotApplicable Sample/sample duplicate RPD did not meet acceptance criteria of ~20%. Table 20. CGMN SW MRIW19 140930 me J l[ eem r wen lT rwe )] 3M LIMS ID Description ISO11-01-03-17-022 Cai EERE EE RY ISO11-01-03-17-023 CGMN-SW-MRIW19-0-140930 CGMN-SW-M RIW19-DB-140930 ISO11-01-03-17-022; LMS CGMN-SW-MRIW19-LMS (1 ppb) E--Average Concentration (ng/mL) + %RPD PFBA Concentration (ng/mL) %Recevery <0.0500 HA <0.0500 NA 1.12 112 <0.0500 ng/mL PFOA Concentration (ng/mL) %Recovew 0.0922 NA 0.0898 NA 1.09 104 0.0910 ng/mL + 2.6% PFOS Concentration (ng/mL) %Recovery <0.0232 NA <0.0232 NA 0.929 100 <0.0232 ng/mL NA = Not Applicable PAGE 23 OF 36 3M_MN01596260 33663300..00331111 red 3M Environmental Laborato~ Repot[ No IS0~i1-01-03-17 Table 21. CGMN SW MRIW19d 140930 J l [om l 1 wleaee [ lwle)] 3M LIMS ID Description ISO11-01-03-17-024 CGMN-SW-M RIW19d-0-" 4030 el 5CLL i] ISO11-01-03-17-025 CGMN-SW-M RlW19d-DB-140930 ISOll-01-03-17-024; LMS CGMN-SW-MRIW19d-LMS (1ppb) Average Concentration (ng/mL) 4- %RPD as NA = Not Applicable PFBA Concentration (ng/mL) %Recevery <0.0500 NA <0.0500 NA 1.15 115 <0.0~;00 ng/mL PFOA Concentration (ng/mL) %Recovery <0.0240 NA <0.0240 NA 1.12 117 <0.0240 ng/mL PFOS Concentration (nglmL) %Recovery <0.0232 NA <0.0232 NA 0.966 104 <0.0232 ng/mL ree on Table 22. CGMN SW MRIW19f 140930 le [ lo erm T eeelnl[w le )] 31~1 LIMS ID ISOl 1-01-03-17-026 am a Pa ilei] ISO11-01-03-17-027 ISOll-01-03-17-026; LMS Description CGMN-SW-MRIW19f-0-140930 CGMN-SW-MRIW19f-DB-140930 CGMN-SW-MRIW19f-LMS (lppb) PFBA Concentration (n~l/mL) <0.0500 <0.0500 1.10 %Recovery NA NA 110 PFOA Concentration (n~/mL) <0.0240 <0.0240 1.03 %Recover}" NA NA 108 PFOS Concentration (n1tmL) <0.0232 <0.0232 0.884 %Recoveq/ NA NA 5.5 Average Concentration (ng/mL) 4. %RPD <9.0500 ng/mL <0.0240 ng/mL <0.0232 ng/mL NA = Not Applicable PAGE 24 OF 36 3M_MN01596261 33663300..00331122 red 3M Environmental Laborato~ Repo# No IS0~i1-01-03-17 Table 23. CGMN SW MRIW25b 140930 J [orm l1lwea [ lwre)] 3M LIMS ID Description ISO11-01-03-17-028 CGMN-SW-M RIW25b-0J 4030 aa 4 iL it ISO11-01-03-17-029 CGMN-SW-M RIW25b-DB-140930 ISOll-01-03-17-028; LMS CGMN-SW-MRIW25b-LMS (1ppb) Average Concentration (ng/mL) %RPD as NA = Not Applicable nin Table 24. CGMN SW MRIW25 140930 PFBA Concentration (ng/mL) %Recevery 0575 NA 0to30 NA 1.68 113 0.553 ng/mL 8.1% PFOA Concentration (ng/mL) %Recovery 0.171 NA 0.174 NA 1.16 103 0.173 ngtmL 1.7% PFOS Concentration (nglmL) %Recovery 0.150 NA 0.145 NA 0.984 90.3 0.148 ng/mL 3.4% me Jo mleemaewea r | ww | 3M LIMS ID Description ISO11-01-03-17-030 CGMN-SW-M RIW25-0-140930 EE di aL Ltad ISO11-01-03-17-031 CGMN-SW-M RIW25-DB-140930 IS011-01-03-17-030; LMS CGMN-SW-MRIW25-LMS (1 ppb) -- ne Average Concentration (ng/mL) -+ %RPD PFBA Concentration (ng/mL) %Recevery 0659 NA 0687 NA 1.80 113 0.673 n~/mL-+ 4.2% PFOA Concentration (ng/mL) %Recovery 0.181 NA 0.181 NA 1.16 102 0.181 n~tmL -+ 0.0% PFOS Concentration (ng/mL) %Recovery 0.128 NA 0.126 NA 1.09 104 0.127 ng/mL -+ 1.6% NA = Not Applicable PAGE 25 OF 36 3M_MN01596262 33663300..00331133 red 3M Environmental Laborate~ R epo# No IS 0~i1-0"i-03-17 Table 25. CGMN SW MRIW25d 140930 J3M LIMS ID ISO11-01-03-17-032 ISO11-01-03-17-033 l [om l 1 wleaee [wre l] ) Description CG MN -SW-M RIW25d-0-" 4030 EI EEEIY CGMN-SW-MRIW25d-DB-140930 PFBA Concentration (ng/mL) <0.0500 <0.0500 %Recovery NA NA PFOA Concentration (ng/mL) 0.0396 0.0509 %Recovery NA NA PFOS Concentration (nglmL) <0.0232 <0.0232 %Recovery NA NA ISOll-01-&3-17-032; LMS CGMN-SW-MRIW25d-LMS (1ppb) 1.08 108 1.08 108 0.869 93.8 enEcnoacmk 1m708oentsac 4535. Average Concentration (ng/mL) 4- %RPD <0.0500 ng/mL NA = Not Applicable (1) Sample/sample duplicate RPD did not meet acceptance criteria of~20%. Table 26. CGMN SW MRIW25f 140929 0.0453 ng/mL -~ 25% I1! <0.0232 ng/mL le [ lo erml Teel n[w ) e] 31~1 LIMS ID ISOl 1-01-03-17-034 R Li LL PL hl ISO11-01-03-17-035 ISO11-01-03-17-036 Description CGMN-SW-M RIW25f-0-140929 CGMN-SW-MRIW25f-DB-140929 CGMN-SW-MRIW25f-FMS-140929 PFBA Concentration (n~l/mL) <0.0500 <0.0500 0976 %Recovery NA NA 6.6 PFOA Concentration (n~/mL) <0.0240 <0.0240 0.977 %Recover), NA NA 98.1 PFOS Concentration ~n1tmL) <0.0232 <0.0232 0.869 %Recoveq/ NA NA 87.2 Average Concentration (ng/mL) 4. %RPD <0.0500 ng/mL <0.0240 ng/mL <0.0232 ng/mL NA = Not Applicable PAGE 26 OF 36 3M_MN01596263 33663300..00331144 Sr OWA 3M Environmental Laborato~ R epo# No IS G~i1-0"i-03-17 Table 27. CGMN IW MRIW09b 141002 mame 3M LIMS ID omen Description [ema [w| ewa s | PFBA Concentration |i [cn [5 [|550[ene (ng/mL) %Recevery PFOA Concentration (ng/mL) %Recovery PFOS Concentration (nglmL) %Recovery ISO11-01-03-17-037 CGMN-IW-MRIW09b-0-141002 ISO11-01-03-17-038 CGMN-IW-MRIW09b-DB-141002 ISOll-01-03-17-037; LMS CGMN-IW-MRIW09b-LMS (10ppb) Average Concentration (ng/mL) %RPD 476 NA 443 NA 60.2 NC 46.0 ng/mL 7.2/= 8.31 NA 7.88 NA 19.6 120 8.10 ng/mL 3.00 HA 2.90 NA 13.7 116 2.95 nglmL 3.4% NENA tm fm: prs in NA = Not Applicable NC = Not Calculated; Spike level was less lhan 0.5x the endogenous sample concentration. Table 28. CGMN IW MRIW09 141002 meme omer [ |ei ma[ove[ [iw Le| ew[a eene| 3M LIMS ID Description ISO11-01-03-17-039 CGMN-IW-MRIW09-0-141002 EE TT TT ISO11-01-03-17-040 CGMN-IW-M RIW09-DB-141002 ISO11-01-03-17-041 CGMN-IW-MRIW09-FMS-141002 oeAverage Concentration (ng/mL) + %RPD PFBA Concentration (ng/mL) %Recevery 6.77 HA 6.65 NA "11 7 98.8 6.71 ngtmL -+ 1.8% PFOA Concentration (ng/mL) %Recovew 1.39 NA 1.39 NA 6.66 106 1.39 ngtmL + 0.0% PFOS Concentration (ng/mL) %Recovery 0.392 HA 0.374 NA 5.12 95.1 0.383 ngtmL -+ 4.7% NA = Not Applicable PAGE 27 OF 36 3M_MN01596264 33663300..00331155 red 3M Environmental Laborato~ Repo# No IS0~i1-01-03-17 Table 29. CGMN IW MRIW09d 141001 J [orm l1lwea [ lwre)] 3M LIMS ID Description ISO11-01-03-17-042 CGMN-IW-M RIW09d-0-141001 aeLh 2 SL i] ISO11-01-03-17-043 CGMN-IW-M RIW09d-DB-141001 ISOll-01-03-17-042; LMS CGMN-IW-MRIW09d-LMS (5ppb) Average Concentration (ng/mL) %RPD as NA = Not Applicable SR Table 30. CGMN IW MRIW09f 141002 PFBA Concentration (ng/mL) %Recovery 2.93 NA 2.94 NA 8.43 111 2.94 ng/mL 0.34% PFOA Concentration (ng/mL) %Recovery 0.781 NA 0.797 NA 5.70 103 0.789 nglmL 2.0% PFOS Concentration (nglmL) %Recovery <0.0232 NA 0.0209 NA 4.42 5.3 0.0269 ng/mL me Jo mleemaewea r | ww | 3M LIMS ID ISO11-01-03-17-044 EA EEAHHEIHEIN ISO11-01-03-17-045 Description CGMN-IW-M RIW09f-0-141002 CGMN-IW-M RIW09f-DB-141002 PFBA Concentration (ng/mL) 15.6 15.1 %Recovery NA NA PFOA Concentration (ng/mL) 0.523 0.524 %Recovery NA NA PFOS Concentration (ng/mL) 0.0236 <0.0232 %Recovery NA NA IS011-01-03-17-044; LMS CGMN-IW-MRIW09f-LMS (lppb) 16.4 NC 1.50 102 0.959 101 Average Concentration (ng/mL) _+ %RPD 15.4 ng/mL -+ 3.3% 0.524 ng/mL -+ 0.19% 0.0236 ng/mL TARR tm 05 ges ese NA = Not Applicable NC = Not Calculated; Spike level was less lhan 0 5 the endogenous sample concentration PAGE 28 OF 36 3M_MN01596265 33663300..00331166 red 3M Environmental Laborato~ Repo# No IS0~i1-01-03-17 Table 31. CGMN IW MRIW14b 141002 me Jr [om l 1 weal [wre l] ) 3M LIMS ID Description ISO11-01-03-17-046 CGMN-IW-'VlRIW14b-0-141002 aa 5LIn AL i] ISO11-01-03-17-047 CGMN-IW-'Vl RIW14b-DB-141002 ISQll-01-03-17-046; LMS CGMN-IW-MR.IW14b-LMS (100ppb) asAverae Concentration (ng/mL) 4- %RPD PFBA Concentration (ng/mL) %Recevary 24.4 NA 24.4 NA 131 108 24.4 ng/mL 4- 0.0% PFOA Concentration (ng/mL) %Recovery 101 NA 102 NA 207 11" 102 ngtmL 4- 0.99% PFOS Concentration (nglmL) %Recovery 37/1 NA 37.(3 NA 122 92.5 37.1 ng/rnL 4- 0.27% NA = Not Applicable Table 32. CGMN IW MRIW14 141001 me Jo mleemaewea r | ww | 3M LIMB ID ISO11-01-03-17-048 a IEEEEIE ISO11-01-03-17-049 Description CGMN-IW-M F{IW14-0-14100~ CGMN-IW-M RIW14-DB-141001 PFBA Concentration (ng/mL) 2.29 2.03 %Recevery NA NA PFOA Concentration (n/mL) 4.49 3.99 %Recovery NA NA PFOS Concentration (ng/mL) 0.284 0.218 %Recovery NA NA ISOll-01-03-17-048; LMS CGMN-IW-k4P,IW14-LMS(Sppb) 7.39 105 9.06 10" 4.39 89.8 Average Concentration (ng/mL) 4- %RPD 2.16 nglmL 4-12% 4.24 n~/mL -+ 12% 0.251 n~lrnL 4- 26% (~ Saindk 17. ot cencen 45 NA = Not Applicable (1) Sample/sample duplicate RPD did not mee[ acceptance criteria of~20% PAGE 29 OF 36 3M_MN01596266 33663300..00331177 Sr OWA 3M Environmental Laborato~ Repo# No ISG~i1-01-03-17 Table 33. CGMN IW MRIW14d 141001 woe oe [e |m Ga|e[ [ogw [ome| e | wa [ses| 3M LIMS ID Description ISO11-01-03-17-050 CGMN-IW-M RIW14d-0-141001 ETT ISO11-01-03-17-051 CGMN-IW-M RIW14d-DB-141001 ISO11-01-03-17-052 CGMN-IW-M RIW14d-FMS-141001 oiAverage Concentration (ng/mL) %RPD PFBA Concentration (ng/mL) %Recevery 0307 NA 1.40 NA 1.38 52.1 ni 9.854 ngirnL 128% 12~ PFOA Concentration (ng/mL) %Recovery 0.0780 NA 0. r354 NA 1.07 85.7 0.216 ng/mL 128% is PFOS Concentration (nglmL) %Recovery <0.0232 NA 0.0952 NA 0.926 83.4 0.0952 ng/mL TRIE roves NA = Not Applicable (1) FMS recovery did not meet acceptance criteria of 100 + 30%. The megqod uncertainty has been expanded to +48% for PFBA. (2) Sample/sample duplicate RPD did not meet acceptance cdteda of~20%. Table 34. CGMN IW MRIW14f 141002 oe 3M LIMS ID E [eEme Eater 2 wenl e| re w{wee| Description PFBA Concentration (nglmL) %Recevery PFOA Concentration (nglmL) %Recoven] PFOS Concentration (ng/mL) %Recovery ISO11-01-03-17-053 CGMN-IW-MRIW14f-0-141002 72.0 HA ISO11-01-03-17-054 CGMN-IW-M RIW14f-DB-141002 80.2 NA ISOll-01-03-17-053; LMS CGMN-IW-MRIW14f-LMS (5ppb) 77.6 NC Average Concentration (ng/mL) -+ %RPD 76.1 nglmL -+ 11% NETRA ntset fm errssein NA = Not Applicable NC = Not Calculated; Spike level was less than 0.Sx the endogenous sample concentration. 3.96 NA 4.42 NA 8.70 4.5 4.19 ng/mL -+ 11% 0.0477 HA <0.0232 NA 4.14 88.8 0.0477 ng/mL PAGE 30 OF 36 3M_MN01596267 33663300..00331188 Sr OWA 3M Environmental Laborato~ R epo# No IS 0~i1-0"i-03-17 Table 35. CGMN IW MRIW19b 141001 mame omer [|eima[c[ n [5w [| e |550wa [sene | 3M LIMS ID ISO11-01-03-17-055 EET TTT ISO11-01-03-17-056 aISOll-01-03-17-055; LMS Description CGMN-IW-M RIW19b-0-141001 CGMN-IW-MRIW19b-DB-141001 CGMN-IW-MRIW19b-LMS PFBA Concentration (ng/mL) 69.0 69.4 171 %Recovery NA NA "103 PFOA Concentration (ng/mL) 149 144 240 %Recovery NA NA 98.5 PFOS Concentration (nglmL) 33/1 29.2 109 %Recovery NA NA 84.8 Average Concentration (ng/mL) %RPD 69.2 ng/mL 0.58% 147 ng/mL 3.4% 31.2 ng/mL 13% NA = Not Applicable Table 36. CGMN IW MRIW19 141001 wre oom [o 17m 00a|vere| 0oa | ee" ee[sie]| 3M LIMS ID ISO11-01-03-17-057 ET I ISO11-01-03-17-058 BeIS011-01-03-17-057; LMS Description CGMN-IW-MRIW19-0-14100~ CGMN-IW-MRIW19-DB-141001 CGMN-IW-MRIW19-LMS(50ppb) PFBA Concentration (ng/mL) 626 625 116 %Recevery NA NA 108 PFOA Concentration (ng/mL) 9.20 9.10 56.8 %Recevery NA NA 99.9 PFOS Concentration (ng/mL) 91.9 92.7 125 %Recevery NA NA 70.9 Average Concentration (ng/mL) _+ %RPD 62.6 ng/mL -+ 0.16% 9.15 ng/mL -+ 1.1% 92.3 ng/mL -+ 0.87% NA = Not Applicable PAGE 3t OF 36 3M_MN01596268 33663300..00331199 red 3M Environmental Laborato~ Rope# No IS 0~i1-0"i-03-17 Table 37. CGMN IW MRIW19d 141001 [omPFBA 1 wea PFOA [we PFOS ] 3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery Concentration (nglmL) %Recovary ISO11-01-03-17-059 CGMN-IW-M RIW19d-0-141001 13.3 NA ISO11-01-03-17-060 CGMN-IW-MRIW19d-DB-141001 13.5 NA ISOll-01-03-17-061 CGMN-IW-M RIW19d-FMS-141001 rempnisatre | main Average Concentration (ng/mL) 4- %RPD 17.8 NC 13.4 ng/mL 4- 1.5% ergs NA = Not Applicable FETE ont vr rncori. NC = Not Calculated; Spike level was less lhan 0.5x the endogenous sample concentration. | 0.112 NA <0.0232 NA 0.116 NA <0.0232 NA anes | 4.94 96.9 0.114 ngtmL 4- 3.5% sw | 4.29 86.1 <0.0232 ng/mL Tala 3. COMNIW HRW! 14002 Table 38. CGMN IW MRIW19f 141002 3M LIMS ID foe Description [mr eee i [ste [i[me se | PFBA Concentration (nglmL) %Recovery PFOA Concentration (nglmL) %Recovery PFOS Concentration (ng/mL) %Recovery 13C4 PFOA'2} %Recove=~t ISO11-01-03-17-062 CGMN-IW-MRIW19f-0-141002 50.0 NA 223 NA 0.896 NA ISO11-01-03-17-063 CGMN-IW-MRIW19f-DB-141002 cromempomizwes | ISOll-01-03-17-062; LMS CGMN-IW-MRIW19f-LMS (5ppb) Average Concentration (ng/mL) -+ %RPD 53.0 NA 239 NA 0.930 NA summiie |meson |_ewsmmoan 54.8 NC 51.5 ng/rnL -+ 5.8% NA (~) NA <~) 231 ng/mL-+ 6.9% 4.96 87.8 9.913 ng/mL -+ &7% NA = Nat Applicable ATC. svtna os han rg acoso. NC = Not Calculated; Spike level was loss than 0.Sx the endogenous sample cancan~atiorl. frm (1) The LMS sample was not included in the re-analysis of the sample set for PFOA. FR EV, (2) The ~C4-PFOA surrogate recovery standard was added to the sample dilutions dudng sample preparation 96 950 wan) NA 95.5% -+ 1.2% PAGE 32 OF 36 Sw_unore96269 3M_MN01596269 33663300..00332200 red 3M Environmental Laborato~ Repo# No ISG~i1-01-03-17 Table 39. CGMN IW MRIW25b 140930 me J [orm l1lwea [ lwre)] 3M LIMS ID ISO11-01-03-17-064 EEENEEAY ISO11-01-03-17-065 Description CGMN-IW-M RIW25b-0-140930 CGMN-IW-M RIW25b-DB-140930 PFBA Concentration (ng/mL) 54.6 53.2 %Recovery NA NA PFOA Concentration (ng/mL) 380 368 %Recovery NA NA PFOS Concentration (nglmL) 1300 1290 %Recovery NA NA ISOll-01-03-17-064; LMS CGMN-IW-MRIW25b-LMS (50ppb) 108 109 410 NC 1220 NC Average Concentration (ng/mL) 4- %RPD 53.9 ng/mL 4- 2.6% 374 ng/mL4- 3.2% 1300 nglmL 4- 0.77% NeEvNeAc:coomatmsontc er src. NA= NotApplicable NC = Not Calculated; Spike level was less lhan 0.5x the endogenous sample concentration. Table 40. CGMN IW MRIW25 140930 me Jol e [ l m welner lT rwe )] 3M LIMSID Description ISO11-01-03-17-066 E Liie fli Lt ISO11-01-03-17-067 CGMN-IW-MRIW25-0-140930 CGMN-IW-MRIW25-DB-140930 ISO11-01-03-17-066; LMS CGMN-IW-MRIW25-LMS (50ppb) E--Average Concentration (ng/mL) + %RPD PFBA Concentration (ng/mL) %Recevery 59 1 HA 586 NA 111 105 58.9 ng/mL -+ 0.85% PFOA Concentration (ng/mL) %Recevenj 23.8 NA 23.3 NA 70.9 99.3 23.6 ng/mL_+ 2.1% PFOS Concentration (ng/mL) %Recovery 16.3 HA 16.1 NA 52.0 77.7 16.2 nglmL + 1.2% NA = Not Applicable PAGE 33 OF 36 3M_MN01596270 33663300..00332211 Sr OWA 3M Environmental Laborato~ R epo# No IS 0~i1-0"i-03-17 Table 41. CGMN IW MRIW25d 141001 mame 3M LIMS ID omer Description [ema [w| ewa s | PFBA Concentration |i [cn [00 [|550 [ene (ng/mL) %Recevery PFOA Concentration (ng/mL) %Recovery PFOS Concentration (nglmL) %Recovery ISO11-01-03-17-068 CGMN-IW-M RIW25d-0-141001 ISO11-01-03-17-069 CGMN-IW-M RIW25d-DB-141001 ISOll-01-03-17-068; LMS CGMN-IW-MRIW25d-LMS (1ppb) Average Concentration (ng/mL) 4- %RPD 11.0 NA 10.5 NA 11.9 NC 10.8 ng/mL 4- 4.7% 37.4 NA 35.9 NA 36.5 NC 36.7 ng/mL 4- 4.1% 0.0962 NA 0.0920 NA 0.939 91.2 0.0941 ng/rnL 4- 4.5% NENA tm fm: prs in NA = Not Applicable NC = Not Calcula[ed; Spike level was less lhan 0.5x the endogenous sample conce~qt~ation. Table 42. CGMN IW MRIW25f 141001 meme o| men [emaLov,[ [iw Le| e 0wa [eene| 3M LIMS ID Description ISO11-01-03-17-070 CGMN-IW-MRIW25f-0-141001 eTIT TT ISO11-01-03-17-071 CGMN-IW-MRIW25f-DB-141001 ISO11-01-03-17-072 CGMN-IW-MRIW25f-FMS-141001 oLe ee Average Concentration (ng/mL) + %RPD PFBA Concentration (ng/mL) %Recevery 165 HA 159 NA 215 NC 16.2 ngtmL -+ 3.7% PFOA Concentration (ng/mL) %Recevenj 10.2 NA 9.83 NA 15.1 NC 10.0 ngtmL + 3.7% PFOS Concentration (ng/mL) %Recovery 7.21 HA 6.09 NA 11.7 101 6.65 ng/mL + 17% NA = Not Applicable NC = Not Calculated; Spike level "~as less lhan 0.Sx the endogenous sample concentration. PAGE 34 OF 36 3M_MN01596271 33663300..00332222 red 3M Environmental Laborato~ Repo# No ISG~i1-01-03-17 Table 43. CGMN IW rRIP 140929 same 3M LIMS ID o| nes [esat[ r e 0tr n| "e ETees s | Description PFBA PFOA PFOS ConcentratiOn(ng/mL) %Recovery Concentration (ng/mL) Concentration %Recovery (ng/mL} %Recovery IS011-01-03-17-075 ISO11-01-03-17-076 ISO11-01-03-17-077 CG MN -IW-TRI P-0-140929 CGMN-IW-TRIP-LS-140929 CGMN-IW-TRIP-HS-140929 <0.0500 0.958 4.77 NA 4.9 4.5 <0.0240 0.952 4.73 NA 95.6 95.0 <0.0232 0.937 4.74 NA 4.1 95.2 NA = Not Applicable PAGE 35 OF 36 w_morsoearz 3M_MN01596272 33663300..00332233 -- nd 3M Environmental Laboratory Report AIo. IS011-01-03-17 55 CCoonncclluussiioonn \aboror areas so dio dolar rt med cy rd rein or Laboratory control spikes were used to determine the analytical method accuracy and precision for all Ee pe ett ts betaa analytes. The accuracy and precision were then used to estimate the method uncertainty for the a ras Sorosaoe Samrat vas results. Field matrix spike and lab matrix spike recoveries demonstrated that the analytical method was ee a evioas ae WE hoy appropriate for the given sample matrix. Analysis was completed using 3M Environmental Laboratory a Saco Ponta ones ee method ETS-8-044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water bsNERS ee haanSen oa ets coed oe To to by LC/MS/MS; Direct Injection Analysis". Analytical results are reported in Tables 1 and 11- 43 of this report. lE amanEgsaps si tsscaatid rs otngaorpnsr cnc sR 66 DDatataa//SSaammpplleeRReteetennttiioonn All remaining samples and associated project data (hardcopy and electronic) will be archived according to 3M Environmental Laboratory standard operating procedures. 7_ signatures 7 Signatures S Yop iE Sn. Nebpir--ree -- ET---------------- Susan Wolf, 3M Principal Analytical Investigator D gilally signed 3yWilliam K. Reagen DN: c=US, s[=MN I=St Paul, ou=Laborat0ry D rec~0r ou=3M Environrqan:al Laboral0ry - BT William K. Reagen, Ph.D., 3M Environmental Laboratory Technical Director Te 3 Emormen Lato' Quy Asan Usk has std din ad tbr Tpprrhooejjeecc3ttM.. Environmental Laboratory's Quality Assurance Unit has audited the data and report for this E % E EE ------ Quality Assurance Representative D Tetestn o sh:nt prc cep lout ton spr fh This test report shall not be reproduced except in full, without written approval of the 3M Environmental Laboratory. 33663300..00332244 sen PAGE 36 OF 36 suorssezrs 3M MN01596273 a -- All sample bottles include the addition of aenn internal standards and surrogates, cone een tie Do not pre-rinse the bottles. one pot okt af ene Do not pour out the contents of the bottle, Projet 15011010317 Project: ISOI 1-01-03-17 4 EENNVVIIRROOCNhNMaMiEnENoNfGT'ACArLLtLLoAdAyBBOORRAATTOORRYY Chain-of .Custody SiSppiinvgiAcarrsas:nasorl Shipping Address: St Cogt2005,y 3M Environmental Laboratory 817 3M Center, Bldg 260-5N-17 Spain shies St. Paul, MN 55144 Phan: (6507203873 Phone: (651) 733-9873 AFo ratry aGnadn7asr cn AIt. Phone: (651) 736-6559 Fax: (651) 733-4687 Reausi: Kosaid, anes Renld MAPLEWO Requester: Kots,nith James Ronald (MAPLEWO Depart: 42090 SiSows: OLSCARD Department: 452090 Site Source: 01J9C020 Pet Number 073138015 P,'oject Number: 0073138015 Due Crs: 392014 Date Created: 9/9/2014 jek Derpion: Missi Kier Susie and Pore War Sein Project Description: Mississippi River Surface and Pore Water San piingSerena 014 September 2014 Commer Comments: Conpleion Due Cmnpletion Date: Poet Leu: Stan T Wo Project Lead: Susan T. Wolf Eran Numbir 6511339851 Phone Number: 651-733-9851 Eri Ades sonoGmmcon Email Address: stwolf@mmm_com [somos ror [commweons pugs || 507 ir] Stent Sinn Durnion Dacia Suna Mts Coma 3M Sample Number Sample Descr_iption Date/Time Sampled Matrix Comment [isonovosvan ISOI 1-01-03-17-001 Jcomswnnonsfg) |Torialpso[ST sirais | [sororavrron|comovmamonce pge) |Lior]po]T Tsipirwots | [s[ IISSoOOn1I1o1--00r11--s0033ia --11n77--e0000s32 |[cn coonssuo mmeogv ppei a || L|ierbaifo iwse] oT | | Sitois | 1 Tonar wis ISOI 1-01-03-17-004 [sonora Jccomosvnmmsoreo iipool ISOI 1-01-03-17-005 ||LTip ppew r|T/ |TT1 p 7T e] r ISOI 1-01-03-17-006 ISO11-01-03-17-007 [ssooranorrona iSO11-01-03-17-008 [cooom mmejayponny~ ||LLeetoem r||1]|Logvrienfensrs ISOl 1-01-03-17-009 connie (igo |Tgwmjse] || [sonora ISOI 1-01-03-17-010 consvammmon pro | | gwejes] | 1 | ISO11-01-03-17-011 [[ssoonnoovnriaan ISO11-01-03-17-012 [[cocmsovmammmseaepjiyooiz o ||ome/o]| 1 | Lommel TT1 [sonoma ISO11-01-03-17-013 Teonsvmmunsjp | Tonle ET 7] ISO11-01-03-17-014 -- ' beoac SSaammppllee CCoonnddiittiioonnUUppoonnRReecceeiipplt:. Temperature: Deg C OReetontes [0] AAcccceeppttaabbllee [] Received on Ice Oper [0] AAbI iitteemmssaaccccoouunntteedd ffoorr [] O JT coRteesteaeby ring: Collected by (print): Relinquished by: Daze Due (gros Date Te Spd f Nix 10 Time Shipped Vi~ cotwirssigmnee Collector's signature: Reed Received by: CE LA LX Date Time 33663300..00332255 Fue os Page i of 5 auotssezrs 3M MN01596274 Profs 5011.15.17 con) SM ENVIROCNoMiEfNTACLotLAyBORATORY pA rSA SoHraeC.aotneeoenBs7ys 3a3d3n0s7s5iy Project: IS011-01-03-17 (cont,) ~ ENVIRONMEN "AL LABORATORY Chain-o~ .Custody Shipping Address: 3M Environmental Laboratory 3M Center, Bldg 260-5N-17 St. Paul, MN 55144 Phone: (651) 733-9873 AIt. Phone: (65!) 736-6559 Fax: (651) 733-4687 Requester: Kosi, mes Rena(MAPLEWG Conplion ut: Requester: Kotsmith, James Ronald (MAPLEWC3 Deparment 42050 Si ewe: OLSCC2) FrotLeu: Susan T Wolf Department: 452090 Site Source: 01J9C020 Pct umber 007138015 Tron Number 6517359851 Project Number: 0073138015 Dus Cras 192014 Eat Ades. soGmammcon Date Created: 919/2014 prjrc iesvrptnMissi Riser Soe and Fre Wtr Sli Project Description: Mississippi River Surface and Pert Water Sam ~ling- Completion Date: Project Lead: Susan T. Wolf Phone Number: 651-733-9851 Email Address: stwolf@mmm.com September 2014 3M Sample Number Sample Description D~te/Time Sampled Matrix Commea.t [isortoros asTeomowmavies[oase [souaisirae Toomer dogzo | Jgsordfsoe[50| | |[serglyrae] | |] [sonore ISO[ 1-01-03-17-016 Tconsmmvie[goo |[@su/pos | 1 | [sora0mnon Teomswmmicegogo |[games || | | [[ssoonooroaT Tconesmuomwnmos swswo m | |lv Tagosm pofnpfe piumeet||||g| | or| | so [sonora ISO 11-01-03-17-020 Teonswamwmnspogo | Topp| 1 1 [sonaoren|con ISO l 1-01-03-l7-022 smvanss Wotso | lgsoujpss| |[| [sonaronnon [SO11-01-03-17-023 [common Woas0 | Jpoen/pss| 1[| [sooo ron ISO 11-01-03-17-024 Tcomovamvieo 140930 | Tgsomjios| | | [sonore ISO 11-01-03-17-025 Teonswmvon (49430 |Tgaemfpos | || [sonora ISO11-01-03-17-026 Teomowsmmse Moj30 |T9s0m/us| | | [soovonionTeomswwmonon piogse [sone nonJoomswvamne 190930 |{qggufurs || || | lommfipss [1|] [sonore ionT 1SO l 1-01-03-17-028 ISO11-01-03-17-029 con svmv enc e p oi g0 |losemfps|| | | [sonore ronToms ISOI 1-01-03-17-030 gogo |lommfom[| | | Tope ___ dc 0 feenctanice Done ~ Sample Condition Upon Receipt Temperature: Deg C [] Acceptable [] Received on Ice [] All terns accounted for [] Oth comaenvyimy Collected by (print): Divi Lue ~ ' !~': Fr itr L" cotesurs seme Collector's signature: 411 O57 Relinquished by: Date Time Shipped Via Received by: Date Time -- [rrr 7171 rrr -- CC rrr TT m TT ge 201 Page 2 of 5 Sw umorssez7s 3M MN01596275 33663300..00332266 ENVIROWINIAL LuboaTORY i~1 ENVIRONMEN' 'AL LABORATORY Chsivof Custody Chain-ol-Custody Spa Shipping Address: s 3M Environmental Laboratory Ssi Conne yaas 3M Center, Bldg 260-5N-17 Pcs 15011816517 con) Project: ISOll-01-03-1"7 (cont.) St, Paul, MN 55144 prone: est 733.873 Phone: (651) 733-9873 AFole Sat Alt. Phone: (651) 736-6559 Fax: (651) 733-4687 Fe ------ Campion Requester: Kotsmith, Jmnes Ronald (MAPLEWO P[reiN -- Pic LessDiSeun Department: 452090 Site Source: 01J9C020 Due cranatme92003138015 Pros Namie 65 . Wolf Project Number: 0073138015 rest ex 14 Ene Adie, r1o733m9351 Date Created: 9/9/2014 Sveicepntion: Missi Rive Sree Wr Spin eo ProJect Description: Mississippi River Surface and Pore Water Sam )ling- September 2014 Completion Date: Project Lead: Susan T. Wolf Phone Number: 651-733-9851 Email Address: stwolf@mmn~com Swine Sane pci Dain omts an Commas 3M Sample Number ~am l~le Description Date/Time Samaled Matrix Comment fionavssiron TomswmvvoeHote || gsp ISOI 1-01-03-17-032 CGMN-SW-MRtW25d-0- [sonorasironTcomomvimtogse | |gpmpjgotoaes[|o|w | |] | [ronan von Toommwmvins pigs ISOI 1-01-03-! %033 I SO 11-01-03-17-034 CGMN-SW-MRIW25d-DB- cG N- w-MR w . r-0- tqoqzq [sotvoros ns |comovsamesrss joppng |1 ISO11-01-03-17-035 [sora |con season png | | gpampe)gran] || 1SO11-01-03-17-036 CGbtN-S W-MRIW25 f-FMS- [ionavasiran Toonmms fog |V ujgap]|] ISO11-01-03-17-037 [onarcs ran |comm|i Vpp2-sofoper| po] ISOI 1-01-03-17-038 [ovo vas Jcomenvsmnss Foor | Vporosgen lros]g 2]| ISOI 1-01-03-17-039 [ovo rou comms gor | afspor |11] ISOI 1-01-03-17-040 CGMN-IW-MRtW09b-DB- lq/~~ Iq/oo [oro van Teommmmors goo | LLpozsuigor]11] !1SO11-01-03-17-041 [sooonee Toommmwossjor | | prrforer]11] ISOI i-01-03-1%042 [son inonTom |Tom nygaros||i T|| Stigt purer | tSO 11-01-03-17-(343 CGMN-IW-MRIW09d-DB- [oor vow Foommwommo er | |jpa TT *e ISO [ l-01-03-! 7-044 [ovo vos Tcommmmmorcs yon | Tj ssigjjgpar |JT] ISOI 1-0t-03-l%045 [otvorcsvow | commspoe | | jp apse|JT] ISOt 1-01-03-17-046 [soto now Jeon pgm | Tp sajguw][1] ISO 11-01-03-17-047 | | pos gra] J 1] lsowaisvronTeomammmee igo) |Tiosmpjorgo] [1 ISO11-01-03-17-048 SomeConspoieRoeni 0 ppite a emcnt o]=] Sample Condition Upon Receipt Tempero big 0 heeetantce Dou Co Temperature: Deg C Acceptable Received on Ice [] All terns accounted for [] Oth Cotetbriyms cotmrsigmaore [LUX Collected by (print): Seid: Die Time Spa| ent tee Relinquished by: Date Time Shipped Via Collector's signature: Received by: Date Time ------T1 r T r T r T r r T [ 1 T T 1 [-- ] - Page 3 of5 sw umorssezrs 3M MN01596276 33663300..003327 Project: ISOll-01-03-17 (cont.) WW ENVIRONMENTAL LABORATORY ~ ENVIRONMEN'I'AL LABORATORY Chain-ol-Custody O Shipping Address: ns i 3M Environmental Laboratory 3M Center, Bldg 260-5N-17 ERSt. Paul, MN 55144 JiPhone: (651) 733-9873 Air. Phone: (651) 736-6559 Fax: (651) 733-4687 Requester: Kotsmith, James Ronald (MAPLEWO Department: 452090 Site Source: 01J9C020 Project Number: 0073138015 Date Created: 9/9/2014 Project Description: Mississippi River Surface and Pore Water San" ~ling September 2014 Completion Date: Project Lead: Susan T. Wolf Phone Number: 651-733-9851 Email Address: stwolf@mmn~com 3M Sample Number Sample Description_ fron ro0 Toonwarees it lSOI 1-01-03-17-049 t 1IS5O01111-00110-033--1177-005500 | covvawaminases-pgp [eons |commsJs ISOI 1-01-03-17-051 [sovtrorro Toomer og ISI 1-01-03-17-052 [sonore Joon gigs lSO11-01-03-17-053 CGMN-tW-MR1WI4d-DB- ISO 11-01-03-17-054 leonora ISO11-01-03-17-055 ISO11-01-03-17-056 commons CGMN-IW-MRIW19b-DB- lpq el I5;O11-01-03-17-057 Te FO ISO11-01-03-17-058 [ovomar Joomrmsavrer igo ISOI 1-01-03-17-1359 [pono rinJomresmvress jupe] ISO11-01-03-17-1360 CGMN-IW-MRIW[9-0- Date/Time Sampled IVIatrix Comment |||TTTeorpompaoeargfggemgg|T T|]T|T Fgka] y] [Tire ooo | psp prog TT] TpYiEoegr7e2eTNTN F EoT] Tp refgreyTT] ISOt 1-01-03-17-1361 feJo om s ISOI 1-01-03-17-062 I$O 11-01-03-17-063 ISO 11-01-03-i 7-064 11005] Sample Condition Upon Receipt Temperature: Deg C [] Acceptable [] Received on Ice [] AI items accounted for [] Otl~ Collected by (print): Relinquished by: Date Time Shipped Via Collector's signature: Received by: Date Time 33663300..003328 vrs Page 4 of 5 3M MN01596277 Project: ISO11-01-03-17 (cont.) ww envion aL Laorrony ~ ENVIRONMEN'?AL LABORATORY Chain-ot-Custody Spas Shipping Address: 3M Environmental Laboratory 3M Center, Bldg 260-5N-17 STR St. Paul, MN 55144 PhRoneo: (5p1733e087,3 ||| Phone: (651) 733-9873 AIt. Phone: (651) 736-6559 Fax: (651) 733-4687 Requester: Kotsmith, James Ronald (MAPLEWO Department: 452090 Site Source: 01J9C020 Project Number: 0073138015 Date Created: 9/9/2014 Project Description: Mississippi River Surface and Pore Water Star 9ling September 2014 Completion Date: Project Lead: Susan T. Wolf Phone Number: 651-733-9851 Email Address: stwolf@mmmcom 3M Sample Number [Teonseomomogmnem|e Tovar [Jo| oor 7] ISOI 1-01-03-17-065 [sores Jeommumnse Fogo 1Topofge TIT] ISO11-01-03-17-066 sors von Jconevsmnases tio aseas po TTT] ISO11-01-03-17-067 rE 77777 ISO11-01-03-i7-068 [ro mron Jeroemneners sper 1 Liordabo TTT] IS11-01-03-17-069 ET 7| ISO 11-01-03-17-070 Samlole Description [[ssoonvaerrrroonn{Jwscerrmomeso jppon Lgrrooejgggaiso]T|T]T ISO11-01-03-17-072 oye EE e B 7177775 Fe ISO11-01-03-!7-073 sepor Vora To To] ISOI 1-01-03-17-074 [sors Jowmorrrs gn rigeefa |] 1] ISO11-01-03-17-075 fora Jcomowrmres tTTruro TTT] ISOI 1-01-03-17-076 boTs oonsne f s Tran/g =1] ISOt 1-01-03-17-077 Date/Time Sampled Matrix Comment t Sample Condition Upon Receipt: [] Acceptable TeTmepmepreartauturree:: cCooellaeectdevdybiypr(piroinnt:): Dus (o J7H id DDeeggCC [[J]ReRceecieivveeddoonncIcee /] [] All tems accounted for e Cotectorssgmuret {LA 47 ] [[J]OOtettr~:r: Collector's signature: { IY /; V / i u,.~C_~C_./" iJ Relinquished by: Date Time Shipped Via Received by: Date Time 33663300..00332299 PPaaggee5sooffs5 | 3M MN01596278