Document L55NMNzpDQnnBbeLwXLY6qzq

awemOEMENTTALKUooRrAeTOrRoY 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 FFiinnaall RReeppoorrtt AAnnaallyyssiiss ooff MMiissssiissssiippppii RRiivveerr PPoorree WWaatteerr aanndd SSuurrffaaccee WWaatteerr SSaammpplleess nneeaarr tthhee 33MM CCoottttaaggee GGrroovvee FFaacicliiltityy-- SSeepptteemmbbeerr 22001166 SSaammpplilinngg Laabboorraattoorry RReeqquueesstt NNuummbbeerr:: 1ISSOO1111--0011--033--26 MMeetthhoodd RReeqquuiirreemmenetn:t: 33MM MMeetthhoodd EETTSS--88--004444..33 Repon Date: DaoftLaest Sar Report Date: Date of Last Signature Teessttiinngg Laabboorraattory Environmental Laboratory 33MM EEnnvviirroonnmmeenntt,, HHeeaaltlthh,, SSaaffeettyy aanndd SSuusstataininaabibliilittyy 33MMEnCCveenirntotenermr,, eBBnlldtdaggl 22L66a00b--o00r55a--toNNr--y1177 SSt.t. PPaauull,, MMNN 5555114444. RReeqquueesstteerr KKaarriiee BBlloommqquuiisstt 33MM EEHHSS&&SS 3M Building 224-5W-17 CCoorrppoorraattee EEnnvviirroonnmmeennttaall PPrrooggrraammss 3M Building 224-5W-17 SSaaiinntt PPaauull,, MMNN 5555114444--11000000 PPhhoonnee:: ((665511)) 773377--33447777 Z= SAl", e(ACCALTOTaIEG) flac in Testina Cert # 205201 Fr -- The testing reported herein meet the requirements of ANSI/ISO/IEC 17025:2005 "General Reaquraman fo th CompetenceofTosng nd Calbaton Laborato Requirements for the Competence of Testing and Calibration Laboratories", in SiwihaALEnS CeCRd FAUST AGORA. Be ors accordance with the A2LA Testing Certificate # 2052.01. Additionally, the laboratory's Rony pm usb such ndwas Sernats bm colawin ot EPA quality system has been audited and was determined to be in conformance with the EPA ri Ee b Toe ey ey GLPs (40 CFR 792) by an independent A2LA assessment. PAGE 1 OF 27 `CHCEOONNNNFFEIIDPDEIENNNTCTIAIOALU-LN- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTTT,EECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR-28EE8NN6TT2EERREEDD IINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00000011 Exhibit 2455 I3MM_MMNNO0#4B84444773333 ewROEmERNTOAL0Us1O0RA3T0OR0Y 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 33~M EEnnvviirroonnmmeennttaall LLaabboorraattoorryy 3S3MMMPEErninnvvciirioopnnamlmeAennniaatayllicLLaaalbboorIrnaavtteoosrrtyyigTTaeetccohrhinacincadalRl eDDpeirocetrcottorAr.u: tWWhioilrllialSmauKsnK.a.RnReoeaalggelenn,,PPhhD.D.. 3M Principal Analytical Investigator and Report Author: Susan Wolf AAnr~aaly~tyiticcaa~l RReeppoorrtt ~1SS0O1111--0011--0033--2266 AAn1naa1lly3yssMiissCooofftMMaiisgssseiiGsssrsiipoppviieRRFiaivvceeirrPlPoyor-reeSWeWaptateteermrbaaennrdd2SS0u1r6fuaScaemWrWpaaittnefegrr SSaaamylpcelessrneeeaarr the 3M Cottage Grove Facility- September 2016 Sampling RReeppoorrtt DDaatte:: DDtaeteooffLLaassttSSiiggnnaattuurree 11 SSuummmamrayr/yi/nInttrroodduuccttiioonn TTpohhreeso33nMMnelEEnnfivriooromnnmtmehneetnaMtaallsiLLsaasbboiorprapattooRrryyuepprreenppeaaarrreeddthaaennddSMaannCaalolyytzzoeegddessGaarmmoppvlleeessfacccooillyllee.cctteedSdabbmyyplIIenntsteeggwrroaalrl eCCoocnnoslsueulctlttiinsngdg S2Spo0eep1rpst6toeonmmnabbeneeldrrfr77oa.-m1n100a,l,tyh22ze00e11dM66..isfsSSoiasarmsm_ippppleplerei fssRuwwoivreeeorerebrunreteeattaunurrcmncteehddeato3cotMdthheeC(33PoFMtMtBaEAgEn)env.viGioroprnoenmvrmeeurecsnfraatocaloillcitLLiyaaa.bbnoodrSiraaoattmoorrapyyloeoodsnn wSS(eeePprpFettOeeRmcm)ob.bleleerrcat11en1,dd, p2e.rfucroocane sufona 2016 and analyzed for perfluorooctane sulfonate (PFOS), under SM perfluorobutanoic (PFOS), under 3M Environmental Laboratory project number acid (PFBA), perfluorooctanoic acid Environmental Laboratory project number ISO1101.03- (PFOA), and ISO11-01-03- 26. TTpohhreee S3wMMatEeErnnvvi(irrononnemmerenntstaallwLLaatabebroo,rraatWtoo)rryy lpporrecepapataroernde assnaadmmpptllheerecceoonnstutaarifinaneceresrfwfooarteefirftee(enSnWs)saammlpopclaliitnnigognslo.occaaitEiooanncssh:; wtewemelplvtveey Cacpooondnrtetaadiiwnniaeertretwvwraaoe(ssinsntemmearmaasrptriklkteieeasddletwwwsiaittvthheerr;aaeI""Wfiiilln)c1tolloucdhhaeeedtrritoee"on"bsileinnaueensdttehhaadthttraeccoeorrnrtoseooussdrpfepaodocn.neddeeSwddaam{tto0pelraaeb(SffoiintWntaall)l evvsloooeclltuasumtmicoeenosoo.ffn11Es00a00ciohmmfLsLa.e.meepAAdltnnyd saasaadmmdpiptldioleen,,oaifflivefliidvnetssoesaamammamplplplseelteaddusnupedpltailsirccadwatsteee,ra,enaadinnnddcsluuaardotteaagdrraggtteeoett baarenecauolsyvneteedrfyfaiieassldinamemnaedlatdatreiricdxs.ssSppSikRak.emS.p)lAAell[lb"ssoaaCttmm:lep1plslPeeeFsstsBbbAcooo,tttn[less"sisiCtnien}cdcPlluFuoddOfeeaAddfaittehnhledde cotecton. Sample bottes reserved fo targel anato fed mal spikes were fried wih an [a[1dP3dCCi.t4i}o]-PnPFFoOOfSSi,n,tewwrhhniiacclhhstwwaeenrrdeearaadddsddaeendddttosouttrhrhoeegSsaaatemmprpleleecoccvooennrtytaaisinntaeernrssdapprrrdiiosorr(SttooRbbSeesii)nngg[13ssCee3nn]t-tPttFooBttAhh,ee[1ffi3ieCelld4df]-foPorrFsOsaaAmmpaplnleed accaapoptplplerercoockptporiorniin.aa.ttee mat spke sluion containing Sample bottles reserved for matrix spike solution containing nc argot analy pri0booinrg sen 0 he field forsample target analyte field matrix spikes were fortified with an the target analytes prior to being sent to the field for sample collection. TTinwwtoohefdsieffaremerpenlntet sscaaemmspCplrliiinngggiommneeattnhhdoopddussswwheeprroeeunus.seeddetstoiogcnoacllteecodt talhheepppoiorrene twwhaaetteserarmsspaamlmpepldeleesss;c;rTTirrpiiiddoeennn.tt,,TddheeessiigpgunnsaahtteepddoiaanstsTT sSsinaaammtmhppepllliiisnnnagggmmmmpeeletetthhhdoooedddsacwwtraaipsstriouuensseeeoadfdntdbbhyyepWWunseehissntplooolnioncaata,nntdddieoAAsnsningcc(nh0haooctrerodmiinpantasherepepppaa0sinstt.tt.hhIIenitsTeeragoimradalpel nlCCetoodnmensseulclrdtiiipn,ntgiorrnhee.ippTcliihchcaehateopaddusstithhsispboeiennt sampling method at three of the nine locations to pursoevdidaediisnsietceiboenfo2r2e Abil descripon of he used at this site before. A brief description of the Trident and Push compare it to the Trident and Push point sampingmethods are Trident method, which hasn't point sampling methods are been provided in section 2.2. SmSeaatmmhppolldeessETwwSee.rr8ee.0pp4r4re.e3ppaaMrreedd aaenndd aatonnaafllAyynzhzeaeddysuuosssiifnnggrsdostolhvleveenDntettddeiiltmuiitioonnnataaoccncc0oorfrddPiinneggrtttoouo3IiMMnaEtEenndvviirCooonnmmmepenontutaanlldLLsaabibnoorWraaatttooerrryy method ETS-8-044.3 bsyamLpClMesSINS; Dict by LC/MS/MS; Direct jcton "Method Injection Aralyss. of Analysis Analysis". Intoml standards were for the Determination of Internal standards were used fo ad i Perfluorinated used to aid in he quantiaon Compounds in the quantitation of the Water of the samples TTquaaabbllileety11cssoruuimmrmmlarasiraizzmeepssletthsheepssraaemmppaprlleeedereassnuudlltssanuuassilinnyggzettdhheewiaannhaallytythtiieccaasllammmepetlthheoosddwiddieennbtteifieerddepaaobbrooivevede..anAAdlll fdreeisssuuclultssssffeoodrr aisennere i is report quality control samples elsewhere in this report. prepared and analyzed with the samples will be reported and discussed PAGE 2 OF 27 `CHCEOONNNNFFEIIDPDEIENNNTCTIAIOALU-LN- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTTT,EECNCTOTI.IVV2EE7-OOCRRV-DD1EE0RR-28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00000022 IM_MNO#B44724 3M MN04844734 eo3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-26 `TTaabbllee 11.. SSaammppllee RReessuullttss SSuummmmararyy.. (1) foe Jan 3M LIMSID SEEEemm. Surface Water Locations Sample Description ISO11-01-03-26-003 IW-14b-sw- Sample PFBA ET Concentration (ng/mL) PFOA PFOS Concentration Concentration (ng/mL) . (ng/mL) G=[5 z[=z|z <0.0250 0.0566 0.0260 ISO11-01-03-26-003-DUP IW-14b-sw- Sample Duplicate <0.0250 0.0500 <0.0232 ISO11-01-03-26-009 EmEm.m ISO11-01-03-26-009-DUP Average %RPD Sample/Sample Dup E rE s IW-19-sw - Sample =i] IW-19-sw- Sample Duplicate Average r EE eEE %RPD Sample/Sample Dup <0,0250 (2) NA <0.0250 <0.0250 <0,0250 (~1 NA 0,0533 12 <0.0240 <0.0240 <0.0240(z) NA 0,0260 NA <0.0232 <0.0232 <0,0232 (z) NA ISO11-01-03-26-015 ISO11-01-03-26-015-DUP E T Te r EEeea =E | 2E|Ee5r5| o]e ISO11-01-03-26-018 E ISO11-01-03-26-018-DUP IW-25f-sw - Sample IW-25f-sw - Sample Duplicate Average %RPD Sample/Sample Dup IW-19-sw-dup - Sample IW-19-sw-dup- Sample Duplicate <0.0250 <0.0250 <0.0250 NA <0.0250 <0.0250 <0.0240 <0.0240 <0,0240 NA <0.0240 <0.0240 <0.0232 <0.0232 <0,0232 (2) NA <0.0232 <0.0232 E rE e, .(Zlnls | Average %RPD Sample/Sample Dup Interstitial Water (Pore Water) ISO11-01-03-26-001 IW-14b-pw-T- Sample ISO11-01-03-26-001-DUP IW-14b-pw-T-Sample Duplicate <0.0250 NA 27.8 28.2 <0.0240 NA 99.7 98.9 <0.0232 NA 13.4 12.2 ISO11-01-03-26-002 EEE ISOll-01-03-26-004 e TEl ETEwg= ISO11-01-03-26-004-DUP Average %RPD Sample/Sample Dup IW-14b-pw-pp - Sample IW-14-pw-T - Sample IW-14-pw-T-Sample Duplicate Average %RPD Sample/Sample Dup 28,0 (3) 1.4 21,7(4) 32.7 33.9 33,3 (3) 3,6 99,3 (3) :0.81 94,0 (4) 660 64.6 65,3 (3) 2.1 12.8 (3) 9.4 20,0 (4) )9.46 7.93 8.70 (3) %318 ISO11-01-03-26-005 CE STTF] ISO11-01-03-26-005-DUP IW-14f-pw-T - Sample IW-14f-pw-T- Sample Duplicate Average %RPD Sample/Sample Dup 92.6 94.8 93.7 (3) 2.3 50.4 44.4 47,4 (3) 13 <0.0232 <0.0232 <0,0232 NA CFE EmeEErrre e mema NA=NotApplicable , (1) All samples associated with the reported sampling location were analyzed using solvent dilution with internal standard calibration unless noted otherwise. The analytical data uncertainties for the reported results are as follows: PFBA _+ 19%, PFOA _+ 11%, and PFOS _+ 13%. (2) The field matrix spike sample for the location did not meet acceptance criteria of 100 + 30%. The method uncertainty RE E EnE-- has been expanded, see section 4 of the report for additional information. RE (3) All samples associated with the reported sampling location were analyzed using solvent dilution with external standard calibration unless noted otherwise. The analytical data uncertainties for the reported results are as follows: PFBA _+ 34%, PFOA _+ 20%, and PFOS _+ 20%. (4) Due to insufficient sample volume, a field duplicate and field matrix spike sample were not collected. (5) Due to insufficient sample volume, a field duplicate was not collected; however a field matrix spike sample was FETT collected. (6) The RPD value did not meet method acceptance criteria of-<20%. PAGE 3 OF 27 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00000033 3M MN04844735 eo we 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 `TTaabblele1I ccoonnttiinnuueedd.. SSaammppllee RReessuullttss SSuummmmarayry.. (1) iggDesc A a mr|omy 3M LIMS ID Sample Description [merssstvieposton Interstitial Water (Pore Water) EEEeEe Te[2z3 5 ISO11-01-03-26-006 IW-19b-pw-T- Sample ISO11-01-03-26-006-DUP IW-19b-pw-T-Sample Duplicate EE 1S Average %RPD SamplelSample Dup ISO11-01-03-26-007 IW-19b-pw-pp - Sample ELEEEETEEaleo> ISO11-01-03-26-008 IW-19-pw-T - Sample ISO11-01-03-26-008-DUP IW-19-pw-T - Sample Duplicate Average a rr ter %RPD Sample/Sample Dup ISO11-01-03-26-010 IW-19f-pw-T - Sample rE,TT ISO11-01-03-26-010-DUP IW-19f-pw-T - Sample Duplicate mS TT Average %RPD Sample/Sample Dup ET. | 1515 | ISO11-01-03-26-011 IW-25b-pw-T - Sample rp a] ISO11-01-03-26-011-DUP IW-25b-pw-T- Sample Duplicate PFBA Concentration (ng/mL) PFOA Concentration (ng/mL) PFOS Concentration (ng/mL) 62.2 61.7 62.0 (3) 0,81 18.3 is) 89.3 91.3 90.3 is) 2.2 59.7 54.8 57,3 (3) 8,6 69.5 66.6 147 150 149 (3) 2,0 47.9 (2) 121 124 123 (3) 2.4 150 152 151 (3) 1.3 64.8 68.3 14.1 11.5 12,8 (3) 20 17.7 (2) 37.4 36.9 37.2 (3) 1,3 3.86 3.78 3,82 (3) 2,1 101 109 Average 68,1 t3) 66.6 (3) 105 (3) %RPD Sample/Sample Dup 4.3 5.3 7.6 ISO11-01-03-26-012 IW-25b-pw-pp- Sample 73.9 62.3 78.3 ISO11-01-03-26-012-DUP r EE EE T hT E ISO11-01-03-26-013 EEE EE eeRe |[1E5I[5FT| ISO11-01-03-26-013-DUP IW-25b-pw-pp - Sample Duplicate Average %RPD Sample/Sample Dup IW-25-pw-T- Sample IW-25-pw-T - Sample Duplicate Average %RPD Sample/Sample Dup 72.0 73.0 (3) 2.6 27.6 27.4 27,5 (3) 0.73 61.9 62.1 (3) 0,64 36.5 30.9 33.7 (3) 17 83.3 80.8 (3) 6,2 0.104 0.108 0,106 3,8 ISO11-01-03-26-014 oo mS Tr TY ISO11-01-03-26-014-DUP IW-25f-pw-T- Sample IW-25f-pw-T - Sample Duplicate Average %RPD Sample/Sample Dup -- FEEp EErr ee e , NA= NotApplicable 21.0 24.0 22.5 (3) 13 20.3 18.7 19.5 (3) 8.2 3.61 2.48 3,05 37 (~) (1) All samples associated with the reported sampling location were analyzed using solvent dilution with internal standard calibration unless noted otherwise. The analytical data uncertainties for the reported results are as follows: PFBA _+ 19%, PFOA + 11%, and PFOS + 13%. (2) The field matrix spike sample for the location did not meet acceptance criteria of 100 + 30%. The method uncertainty E has been expanded, see section 4 of the report for additional information. fSe E -- (3) All samples associated with the reported sampling location were analyzed using solvent dilution with external standard calibration unless noted otherwise. The analytical data uncertainties for the reported results are as follows: PFBA _+ 34%, PFOA + 20%, and PFOS + 20%. (4) Due to insufficient sample volume, a field duplicate and field matrix spike sample were not collected. P=(5) Due to insufficient sample volume, a field duplicate was not collected; however a field matrix spike sample was EEETEET collected. (6) The RPD value did not meet method acceptance criteria of-<20%. PAGE 4 OF 27 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00000044 3M MN04844736 aveRnRge aOR 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-26 `TTaabblel1eI ccoonnttiinnuueedd.. SSaammppllee RReessuullttss Suummmmarayry.. (1) PsE amp vsrgen 3M LIMS ID Sample Description Copeton| |Cor"e|en| Contain PFBA Concentration (rig/mE) PFOA Concentration (ng/mL) . PFOS Concentration (ng/mL) Interstitial Water (Pore Water) ISOll-01-03-26-016 IW-25b-pw-T-dup - Sample 68,9 ~ 67,2 ~ 105 ~ Field Blanks (Trip and Equipment) ISOll-01-03-26-017 i ey So ety Soo | ome | as ISO11-01-03-26-017-DUP [Soom [rmmsgmanoe sunpetanopeoees|||aowwmaw ||oan"mweae | ews| ISO11-01-03-26-021 [orroreszomm |exgmersn | wom | ome | aun] ISO11-01-03-26-022 EB-pw-pp - Sample EB-pw-pp- Sample Duplicate Average %RPD Sample/Sample Dup Travel Blank Equipment Blank <0.0250 <0.0250 <0,0250 NA <0.0250 <0.0250 <0.0240 <0.0240 <0,0240 NA <0.0240 <0.0240 <0.0232 <0.0232 <0,0232 NA <0.0232 <0.0232 Wwerctpessn NA = Not Applicable rt: tptsrinivas (1) All samples associated with the reported sampling location were analyzed using solvent dilution with internal standard foramina geek Ht Am et calibration unless noted otherwise. The analytical data uncertainties for the reported results are as follows: PFBA + 19%, rsa PFOA + 11%, and PFOS _+ 13%. 0 om pe snd 1 cpr sto 003304. Thad sry (2) The field matrix spike sample for the location did not meet acceptance criteria of 100 + 30%. The method uncertainty i has been expanded, see section 4 of the report for additional information. ee So pe Apahe tdri ai) (3) All samples associated with the reported sampling location were analyzed using solvent dilution with external standard naa es obese eeot n ho PONS calibration unless noted otherwise. The analytical data uncertainties for the reported results are as follows: PFBA + 34%, oro PFOA + 20%, and PFOS + 20%. Do ct one lie. i ted a at pe al ws lad (4) Due to insufficient sample volume, a field duplicate and field matrix spike sample were not collected. ee aoe aa a rl ws (5) Due to insufficient sample volume, a field duplicate was not collected; however a field matrix spike sample was So collected. J (6) The RPD value did not meet method acceptance criteria of-<20%. 22 MMeetthhoodd SSuummmmaarryy 21 Methods 2.1 Methods Ansys for PBA, PEOA, andPROSws complto flowing OM Envi Laboratory mth Analysis for PFBA, PFOA, and PFOS was completed following 3M Environmental Laboratory method EETTSS--88--004444..33 ""MMeetthhoodd ooff AAnnaallyyssiiss ffoorr tthhee DDeetteerrmmiinnaattiioonn ooff PPeerrfflluuocrriinnaatteedd CCoommppoouunnddss iinn WWaatteerr bbyy Chan: LC/MS/MS". Table 2 Target Antes. Table 2. Target Analytes. [rfe pms | sceoon |"mSan | Target Analytes [remor|soee r | PerTluorobutanoate (C4 Acid) etme Gora ron rwet PerTluorooctanoate (C8 Acid) pr ros | irre mes Penluorooctanesulfonate (C8 Sulfonate) Acronym PFBA PFOA PFOS Reference Material Structure Linear Linear + Branched Linear + Branched 2..22 Sammpplle CCoolllleccttiioonn PPoorree wwaatteerr ((iinntteerrssttiittiiaall wwaatteerr)) aanndd ssuurrffaaccee wwaatteerrssaammplpleesswweerree coolllleecctteedd iinn 125 mmLL NallggeneenTeMTM (hiigghh- Gory poor) bles eparod ho 1 Entonmene Labor Fo 67h comple a 5 density polyethylene) bottles prepared at the 3M Environmental Laboratory. For each sample set, a kta, Hk a upbeat conan wr ROG. A 6 GF bray field sample, field sample duplicate, and field matrix spike container were provided. A set of laboratory repre Tip Bark ang Ti Bark fod mae spe Sami wer Sot wi h colocion bes prepared Trip Blank and Trip Blank field matrix spike samples were sent with the collection bottles. Sioa tio vers received ty he abotoy 00 Seamer 11. 2016. Samgles wre sored Sample bottles were received by the laboratory on September 11, 2016. Samples were stored rreeffrriiggeerraatteedd aatt tthhee llaabboorraattoorryyafatfteerr rreecceeipipt.t. DDuueettoo tthhee lliimmiitteeddvvoolluummeeooff ssaammppllee ccoolllleecctteedd aatt llooccaattiioonnss Ti (SOT 075828008, NA100pu (SG10O828.T00) W10pw5 1801101 IW-14b-pw-T (ISOll-01-03-26-002), IW-19b-pw-T (ISOll-01-03-26-006), IW-19b-pw-pp (ISO1'1-01- PAGE 5 OF 27 CCHOEONNNNFFEIIDPDEIENNNTTCIIAOALU-LN- STSUUYBBDJJIEESCCTTTR ITTCO0T AACOPPURRROOTTT,EECNCTOTI.IVV2EE7-OOGRRV-DD1EE0RR-26EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00000055 aM_MNos844737 3M MN04844737 MENVRROENPMORETNITNGA,L5L0A7B7O0R1A0T3O2R5Y 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 0h0e33d:-2.266-.A000c07o7))p, yaaonnfd tIIhWNe--h22a55i0b-n-oppwwf--cTTu--sd<tuuoppdy((ISfSOoO1r11m-1i0-s01-1in0-0c3l3-u-22d6e6:d-00a116s6)a),,nnnaoottt aaalllcl tthhhmeessnaafmmtoprpleleepoccrootnnftotaariinnreeerfrsseriienncttheh.eesseettwweerree: filled. A copy of the chain of custody form is included as an attachment to report for reference. TTThwweoo ddpiuiffsfeehrreepnnottinsstaammspaplmliinpngginmmgeetmthheootddhssodwweewrraeesuussueesddedftoobccyoolWllleeecscttttohhnee ppaoonrrdee Awwnaacttheerorrssaaimmppltleheess;;paTTsrtri.iddeeInnnttteaagnnraddl PPCuuossnhhsupplooiiinn.tg. Twfreehhppiellcicchpaauhtteseadhdsnttpthroiisbsinetsseaasnmamumppsilpeinnldiggnagmme1metstehhtoohsddoideaatbtwettfahosrreeeu.eseooBfdfelttbhhoyewWninsiiennaseetbolleonofccaaadttnieiodsoncnsrAsinptfotcoihocconoormmoifpnphaatrehreeetiwiptoattososta.ttmhhIpeneltieTTngrrgriddaemelennCttthoommndesestut.hhltooinddg,, which hasn't been used at this site before. Below is a brief description of the two sampling methods. TTTrhriieddeeTnnrtit:d:ent probe i adirectpush, integrated temperature sensor, conducihy sensor, grain ize: TsdsieehsnnecsshoToarrrridgaaiennnnddgtpptpooorroraeebwwseauatirstefeararcssdeaairwmmeapctplte-leeprrrubdsdoheedv,vy.eeinllotDoepipgeferdedarttteeoodnssctcceerrsmeeeiepnnneorssbaiisttteueesrrsfevofeorsdreacanrorseneodaarus,scctwwoihhvneeidrrtueeycaggtinrrvodoituuytnnseddemwwnpaeastroteearr,rtugmmrraaaeyiynin-bbsdeeiizceate dTaarairseepcaaihsdsawywrhgcheionergnreeftgogirraoohuusennuddrpfwwraaecatseteeerwnrcaddeitisesocrcfhhbagaorrrdggoyeeu.niiDdsswioofafccetccreueurrnrcricionnenggss..tinTTihhvoeeebnsiitnenstrteveagegnrdradalcmppoaoonrrpdeeuwwtcahatteitveesirtruyssbeaasnmumdrppfetaleercmrcecpadaeninrsabbbtueeureiuussoieenndddoictfoate contaminants of concern rapidly confirm the presence contaminants of concern. of groundwater constituents and map the subsurface distribution of pTPhuuesshwhapptoieonrint-t:s:amping probe allows interstitial waters 0 be extracted fom the sedimenta selected Tdpoeehprpeiitshwtssaaltuuiecppr-pttsouoamamabpbpooleuiunxtttg9r9a00pcrtccoimbmoenbberaelolllooouwwwgstthhhiaenestesesredsmditaiiltmmikaeelnwnattmawewtaetatertsree,tronisnbftteearirafenaclxceeters.as. csPPteoeordrleefwwrpoaartmoteebrterhi.iessTccshooeelldleeipmccriteoeebnddet sbbayytcoslaneoslloewiwsc-tt-etfoldfooaww ltpleeuennbrggeisithtnhaelootaifcrf89.pt.55humemmtpmmperddxiitaeraammceetitisotee@nrrstsshaatarimoinpnulllgeeehsssspaossrsttteemeeclaol nlttls-uudibbsiiaitnnmiggnegfiittteoteer,fddswwthaiiottihnhlleaacssosslvoiselidtdre,o,edrelembpmoroyovabvaeast.mblTaleelhleppmoopnienrtsot.bhOOesnsnizcttohoheenssassiiiisddnteeoosoof fsfatthhee tss{uottebepeeerllonssveccirradeoereentanh..epTTrtihhep-eetihppeeoorrrrefeeowwristaahlateeesrrasssmaaampmmpplelplileepnrrogrccataancnnodnsatslosoisomtiibbnneegimccoioofznnaeffiigchgluouolrregeegddcionwwvgiieothhrfeatadhssebeeyccsaooamnnpsddlmaaerarryy.ll ssmTccrerrieesseehnnssewwicziioethhnsdaataasrsinayalnensdsdcspr-peaaeccnkk tipisosrieipnn-rsscottlavaeilldlaeeenddeadoovvspeearrernt-tdfhhileetoeMuorutufostlsiridtdeheeepoosrfaotmfbhheeepslppicnrragoonbbaeebn.,edaantunosddemttdhhinefimvvtooioiziddgeebbtceehloettwgrwgeeoieennngfuttothhfheetehrpperrioosnbbaceermeaapannsledder.stthhsuTerchfisrsaccerseeeeeacnrnoenaii,sds apperaanycchkskaecenrddeceewwinitthh Sampling rate, and minimize potential cogging. pre-cleaned sand. Multiple probes can be used sampling rate, and minimize potential clogging. to together to further increase surface area, enhance 22Al.33sampSSlaaemmspwpellreee iPPnrreeapplaaprrraaettpiiaoornne on 8/15/16 and analyzed on 8/16/16for all anaiytes by iting with Amtmelilethstnhaaangmonlpoi.tlle.wsiSStwhaamem4pr.ep5lleeminsisi.twiwaoeelflryrmeeeptddrehiilapuknaitoeerledd.d11o0D0n-fi0o9lKed/1db5by/y1sr6areemammpnolodvevisiannnagganaldyz00L.e.55dCmmoSLnLw9aae/llr1ikqe6uu/ofo1tot6orofffftoiterhhdaeelwlwwaeielnllal0lmmy.i0tie1xxseemddblyssaaodmmilfapuptlilsneeoglaauwnntddiitohn nominal concentration of 1 ngimL. The laboratory contol samples ere prepared and analyzed n the d`ccoilounntttianaiignniinitnggwisstuhurr4rroo.5ggaamtteeLrroeefccmoovveeetrhryyanssottaal.nnddDaarirldudte((SdSRRsSaSsm))p["l1e3CCs 31a]n-PPdFFBLBACA,S, s[[1"3wCCe4.re]--PPfoFFrOOtifAAieaadnnwddit[[h13CC0-.40]1P-PFmFOOLSSofssappiiskkoeelddutaaiottnaa Same manner as the sampies. Prepared samples nominal concentration of 1 ng/mL. The laboratory same manner as the samples. Prepared samples were analyzedbyextemal standard control samples were prepared and were analyzed by external standard caibaion analyzed in calibration. the p`SSraaemmppaplrleeessdttohhnaatt1ww0e/er4re/e1aa6ttbooyrrrbbeeemllooowwvittnhhgee ailimi0ti4t oomfflqa.uuaaainnqitiuataotttiiooofnntwwhhheeewnnelaalnnamalilyyxzzeeedddsuuassmiinpnglgetthhaeend1100d--ifo0tlddindigiluoittiwoninhwwe0e.rr4eemrreeL-- oaopffresmmpoepeatarthheraadantnooeolnli((n1dit0ilueu/m4ttai/oo1lnn6sffbaayacntcrcoeartmroofdoofv22rsi))np..igkDDiaunurg0rii.nn4sggolmttuhthLeiooappnlrirqweoupapoaastrraoaattfidootdhnneeoodfwftttehholeel tlmhlaaeibbxoeolrdaraabtostoorararmyytcopcorlonyenttacoronolndltssodaalimlmupstplianleemgssp,,iltaaewnnsitaha(llini0qqo.uu4mooitmtaooLlff cwacooensnrceecepensantprtrairaaktteteiiodoinnnwtieoofhrfn11aalnnnsggiti/nammtneLLdm))aarlppdrrsiiostorpanittkodoianidrgkdilufsmtioiinnluxggtaioiinnnatthwhneeaosmssiaaanmmadloedecmmdoanantconnenentehirreraaatl5saobtnthoheoroafstso1aarmmnypgpl/celmoesLns...trporlTTihhsoeeaomSspaablmmeepisplnlege(nsobbomeottnittnleetassol wtcthaheelerberffiaeistelpdodink.ffeoodrr sample with an sample collection. Prepared samples were analyzed internal standard mix at a nominal concentration collection. Prepared samples were analyzed onof on 10/1 1 ng/mL 10/5/16 by intemal standard prior to being sent to by internal standard calibration. 22Al.44samAAplnneasallayynssdiiqssual control samples were analyzed for PFBA, PFOA, PFO, SRSs, and IS using Ahihinilglgshhsiaumpmpeeeprnrlffetoosrprmaamranaandnmcceqeetuealrliliqsiat,uyuiidcdtohenccthhurroroiol mmdsaaatmctoohgpgorlremaasapphthwyoye!g/rrettaaaapnnnhddayeelymGmzerdmmeaafsonssr.sPpssFrppoBeegAcrci,atrrmPoo,FmmeOaefnAtrrd,yy tPh((FHeHOPPsSpLLe,COcSM/iMSRfIiSSM/smMS,a)Sas.)ns.dtIrSDDasenetstuaaoslinlienesdgd. adainennssaatclrlyruyzimzbeeeedddntaabrrpeeelaorddwa.eemssecctrreibirseb,dethiinne the raw data herd copies paced In the liquid chromatography gradient program, the raw data hard copies placed in the naland final daz packe, and the specific mass data packet, and are brie transitions are briefly described below. eDDnuuveeirt1oo0nmttehhneetannlaatotuucrrceeurooeffnttchheee ossfaammmpuplelle,,etthhieesowwmiieddrees orrafantnghgeee looafbfoccrooatnnoccreeyn'ntstrraaatntiiaoolnnyssteffsoououfnnddiniienns'tthh,eetsshaaemmsppollfeet,,aaraennddustthehdee environmental occurrence of multiple isomers of the laboratory's analytes of interest, the software used PAGE 6 OF 27 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTTT,EECNCTOTI.IVV2EE7-OOCRRV-DD1EE0RR-28EE8NN6TT2EERREEDD IINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00000066 I3MM_MMNND044884444773388 susmRowRETL UoTORY 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 ffoorr pprroocceessssiinngg tthhee aannaallyyttiiccaall rreessuullttss iiss nnoott aabbllee ttoo ccoonnssiisstteennttllyy iinntteeggrraattee tthhee aannaalylyttiiccaall ppeeaakk,, mmaannuuaall tepaion 0 he rat Pog 1s emessaty A maul eda to proms ong 0 integration of the analytical peak is necessary. All manual integrations are performed following the ORAS une ed ETS.12.01. Teconsseonfcnye aborson mapas ered procedures outlined in method ETS-12-010. The consistency of the laboratory's integration is ensured ri ing of Tract gost, bo Jes 1o0OV. Dcoss vated ot 8 mel through the training of laboratory personnel, the peer review process required for all manual agains eo of man raion ye AD, 3nd where ne h osofs marl integrations, the review of manual integrations by the QAU, and where necessary the review of manual raion oy bora mansgemen, integrations by laboratory management. Tables. Instrument Parameters. Table 3. Instrument Parameters. [emmmentone[eves [ewes | Instrument Name | |p| Cr Analysis Dates IT ---- re-- -- rc-- Analytical Method ETS Jonas 9/16/16 - External Calibration ETS-8-044.3 ETS DaVinci 10t5116 - Internal and External Calibration ETS-8-044.3 Liquid Chromatograph [omen |pam xsomm 52] mmxsorm se | Guard column [anspestcooms |semi |emc ir o mc rn m5:| Analytical column [opctonvonme| gm wa Injection Volume Ftc |sep|s sepi sis s | Mass Spectrometer Fontan my | asm Ion Source CS-- rr-- ---- Electrode ET -- i-- ---- Polarity FS-- TTS-- -- TT -- Software Agilent 1200 Prism RP (2.1 mm X 50 mm), 5 Betasil C18 (2.1 mm X 100 mm), 2 or 5 ;uL Applied Biosystems API 5000 Turbo Spray Turbo ion electrode Negative Analyst 1.6.3 Agilent 1260 Prism RP (2.1 mm X 50 mm), 5 ~_t Betasil C18 (2.1 mm X 100 ram), 5p 10 ~_tL Applied Biosystems API 6500 Turbo Spray Turbo ion electrode Negative Analyst 1.6.3 Table 4 Liquid Chromatography Condions. Table 4. Liquid Chromatography Conditions. erssons Step EAE-EE e a tins Number Co om[wo [wo Two | 0 ew [ow [wow| 1 Coen ow [ @ wo | 2 Is3 1 rm aw [se wo | 4 om [w |e wo | 5 : oo = 0 eo 6 Total Time (min) 0.00 0.50 so | 0.70 9.00 11.0 12.0 14.0 ETS-8-044,3 Flow Rate Percent A (l~L/min) (2 mM ammonium acetate) 300 90.0 300 90.0 300 m3000 | so 60.0 5.0 | 300 5.0 300 90.0 300 90.0 Percent B (Methanol) 10.0 10.0 eo 40.0 95.0 95.0 10.0 10.0 | PAGE 7 OF 27 CCHOEONNNNFFEIIDPDEIENNNTTCIIAOALU-LN- STSUUYBBDJJIEESCCTTTR ITTCO0T AA C OPPURRROOTTT,EECNCTOTI.IVV2EE7-OOGRRV-DD1EE0RR-26EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00000077 aM_MNos844739 3M MN04844739 MENVRROENPMORETNITNGA,L5L0A7B7O0R1A0T3O2R5Y 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 TTaabbllee 55.. MMaassss TTrraannssiittiioonnss.. Analyte oss TOm90n | parstandrg | Mass Transition Internal Standard (1) Noss Taran Mass Transition [oFrm[T2E 30 [eFee seron ] szo n PFBA QIlQ3 213/169 [13C4]-PFBA QI/Q3 217/172 PFOA 413/389 413/219 repro [13C8]-PFOA ams 421/378 pPrFoOsS 413/169 [ee 499/99 [won] 499/80 [cipros. [13Cs]-PFOS 507/80 [opera owe | pogerma |own | [13C3]-PFBA [ejeron | awa |popeoa | amen | [13C4]_PFOA [Pegeros | somo | cperos | som | [13C4]-PFOS 499tl 30 216/172 417/372 503/80 [13C4]-PFBA [13Cs]_PFOA [1308]-PFOS 217/172 421/376 507/80 Overwis 200 0 mc xochFaron.Th eek Taoswer unafo prac Haan Dwell time was 20 or 50 msec for each transition. The individual transitions were summed to produce a "total ion Granary TC)whch ves oe or umndeton chromatogram" (TIC), which was used for quantitation. 0) iatsarverrousedfor he aration slesane on 161 nd 016 (1) Internal standards were not used for the quan'~tation of samples analyzed on 9/16/16 and 10/5/16 for oon S011 E013 25) location ISO11-01-03-26-013 (IW-25-pw-T). 33 AAnnaallyyttiiccaall RReessuullttss 3I3n.41ternaCClaaSltliiabbnrrdaaattriidooAnnnalysis (10/5/16) - Samples were quariiated for all analytes against an inferal Isssnottaltaenuntrddinaaoarrnddls Siccatataloliinbb5drra0aattrimiodonLnAcconuufrarv5vley0e.s:. 5is0CC(ama1lel0ibtb/ha5raat/1ntii6oool)nn -sslSttaaabannomddraaaptrrleoddrsssywwwreeeerarregeeeqpnputrreeawppnaaatiirrtreae.dtdedbbTyyfhossrppcaiikallinlnabggnaaikklnyonotnoewwssnntaaaagnmamdiaonorusudtnnstasscnooonifnfttatseitoronncceakkdl sansantonnggali/umniimntdniLLtoaternerttdmsnooaaplinle11tssa00ottkaa5nnnna0ggddri/aamemmrraLdLdLcoomm((funinin5oxxotm0msaai:f5intnwa0@aaall)m)snnoeowwumtmesheireairnneednaaloltaalo:nccnaooilaaltnnlbyyctczzoeheenerenatddtrd.t.roaaartttyiiaAAoornnfeoqqoaouufrgafea0eda0d.rnc.ar5t5athwitinnaccagn,g,taie/lmmr11yL./tLx.xe.T.wwheTTTeeieehiggncnehhattdssleeiatbtddatar,,naandtdcicwoaaaaernrilrddiobesssrrtaaanrrtantoaiotondgnngafiironndccrggusucrerffcvvdrioeoeronmmtoooaffu0i0n.t.tgeh00hhde22e szh2te6ea1rrno0edsddauuurlrdrtiinanpggnetahthckeeaarftriteaitianniggoconppurrcooncuctseresvswses.a.csoCCnuaafsllceicudmulelatadottiinfanigtcgcthttuhhereeadcssayttatoaannfddfoeaararrdcdehaccccoohunnrccaveenennatiplryfaoteitii.oo.nnTssheuussdiinangtgatthwheeeprpeeeanakokatarforeeracareardatittiohosrsouaagnnddh the resultant calibration curve confirmed accuracy of each curve point. EaEgxxattieenrrsnntaalalSnStetaaxnntdedamararlddAsAntanalanydlysaisrsdisc((a93l/i11b66r/a/1t1i66onaanncuddrv11e0.0//55//C11a66lbffoorrratIISiSOOn11s11t-a-00n11d--a00r33d.-s226w6.e-00r11e33)p)r--eSSpaaarmmeppdlbleeyss wwsepeirrkeeinaagnnakallnyyozzweendd saaatmgmaoaoniundunasntrttssdasnoorfefaxnttthgheieernngasstltfoosocctkkamn0ssd.ooa0luru2dttiooncnngailibmiinnrLttaoottioo55n1000c0ummrnLvLeg.oomffLC99a(00ln-i:b11or00maitinmomeanetlhtsheataanrnonloed:la:arndllaasalbbywoozrreeaadrtet.oorrpyyAreMMpqaAuillariH-edQdrQTaTMMibcy,wwsap1atietkerirn.w.geiTTkgwwnhetoelewlvvdnee, cwscaateaflrinbberdraaanttoriidotosnnforccaruunorregvvdieenotgofhfrfrtotohhumeeghss0tzt.a0aennr2ddoaanurrgdrd/mippnLeegaatokktha1ar0refe0aainnccggoo/umupnnrLtotssc(enwwsosaam,ssinuuCassalee)ldcdwtuelotoaretfiiitangnhtthaehelyeddzsaeattdtaaa.nofdoArarrqeeduaaacccdhhornaaactnenicana,ltlyyr1tta/eetx..iwoTTnehhsieeguhddstaeaitndtaag, the pak were not the peak area counts and the forced through zero area counts and the resuliant calibration curve during the fitting process. resultant calibration curve confimed accuracyof cach curve pon Calculating the standard concentrations confirmed accuracy of each curve point. using TTbohhteehlrrieenffeeerarerenanccneedssbttraaannnddcaahrredddss oiosffomPPeFFrsOO.AA EaaanncddhPPcFFuOOrvSSe puuossieenddt wttoeo spprrqeeuppaanairreietahthteeedccuaaslliibbnrgaatthiooennossvtteaarnnaddlaacrrdadlssibccroolnnissoiinssttceeuddrvooeff aoabnnowdtdehsrrtleienvvceiiueaerwrwveaeeddnpdffoooibrnrrataa)cnccwccuehurreraaedccymyi:se.otmMMfeeoetrrtshha.ooddEaaccncaaahlliebbcsrruaa.rttviooennTphaaoeccincccutuorwrnaaaeccsayytqirrueeoaqqnnuucitiirorteaeemtfmeieedncnteutssnstioonf(gf1)11twh00ea00s+2o22vg5e5r%re%aalt(l(e1cr01a0lti0+bher3a0n0t%i02o.nf93foo9crr05tutrhohv%reee al analytes in esch lowest curve point) all analytes in each awanneaarlelyyssimisse.. t for all analytes. The correlation coefficient (r) was greater than 0.995 for 3A3..22calbSSrayytssottneem smtanSSduuairitdtaabwbiailsliittyaynalyzod four tmos at the begining of the anayical sequenco fo AdsGteeammcnoadonlanisbrsdirtaraadttieoteevniaootsvviteeaorrnnaadll(laRssrSdyyDss)ttweefamomsr sspauuetniaataabkiblylaizltriyteye.d.alfaoTTtuhhoreeatniaamdccecceesetppettanaatinnoccthneeetccirbeimteeergriiaiantoneofinrflgaleesfsossef sttthhhsaaennthaooanrnaeeolqyqftuuiecaaqallul atolse55fqo%%u2er%rneecllaReitSivvtDeoe weremet oral anabes in ach analysis. standard deviation (RSD) for peak area/ratio were met for all analytes in each analysis. and retention time criteria of less than or equal to 2% RSD PAGE 8 OF 27 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOTAACOPPURRROOTTT,EECNCTOTI.IVV2EE7-OOCRRV-DD1EE0RR-28EE8NN6TT2EERREEDD IINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00000088 I3MM_MMNNO044884444774400 MENVRROENPMORETNITNGA,L5L0A7B7O0R1A0T3O2R5Y 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 3T3h.33e LOLLQiim mfioirttaoocffhQQaunuaaanlytnsitiisttaatttiiohoennlo((wLLeOsOtGQn)o)n-zero calibration standard n the curve that me's inearty TaaapnnhpdderoLaapOcrciccQauutrrfeaaoccbrlyyeanarrkceeshq.quuaiiTnrrehaemlemyeesLninstOtssQis aatfhonnerddallolffowoarrneaswwlthyhinticcoehhsn-czttahehnereobaaecrraefeliaoaburnaccdtooiouuinnnniTtsssait/abraalntteidiooa6.rdaarrieen atthe at leastcurve least twice those of the that meets linearity twice those of the appropriate blanks. The LOQ for all analytes can be found in Table 6. TTaabbllee .6.LLiimmiitt ooff QQuuaanntitittaattiioonn ((LLOOGQ)).. wi ose owe 9/16/16 10/5/16 10/5/16 GoEtxbirambaonStnanadarsd CulnberomiaonSAtnasryas| GEalxwiamtaonStAanndaairds Analyte External Standard Calibration Analysis Internal Standard Calibration Analysis External Standard Calibration Analysis Loa.ngmt" Loo gmt" Lamm" [Terma 1 so 7 om | wm | PFBA [pron T om om |o wm | PFOA Coeos| oo 7 ome | oom | PFOS LOQ, ng/mL (i) 5.00 0.479 0.200 LOQ, ng/mL (2) 0.0250 0.0240 0.0232 LOQ, ng/mL (2) NA NA 0.0232 aNa Ape NA = Not Applicable 0) Auta oct 10was ppediotLh0Ge. (1) A dilution factor of 10 was applied to the LOQ. 2) Autentock 2wes spit(e00 (2) A dilution factor of 2 was applied to the LOQ. 3D3u..r44ingCCtohoennctotiiunnrsuueiinonfggeaCCcahallaiibbnrraaatltiioyonnsequence, continuing calibration verification samples (CCV) were raaDennupaaorlilrnyytgzzeeedtddhseattomocpocclouoenrnsfreifrmeiosfttuhehasaatwcehtthhreaeeniibnanrslsyattrtcriuckumaemleetsnneettdqbrrueeyessnppCcooCenn,Vsseecoaatnnnhtaddintmtuthheinetgiimncnietaaitallilbhrccoaaadtlliibobrnraattvteiieororannioficccfuuarrt1ivvo0een0w%wseearrmee2p5islte%iilsl.ni(nCccCoonVntstor)lo.lw. eAArelll reported sample results were bracketed by CCVs that met method criteria of 100% + 25%. 3F3o.5u5r tBByplleaasnnokkfssblanks were prepared and analyzed with the samples: solvent banks, method f((Fpeposrruuoolrccteetddywuuparresaasll)rbboellvfaainnebkkwlssae,,ndfekiesadldniw/dtrepipruesBbellapadnnrekktspso,,araeaenvndddaleeaaqqntuudeiippmmameneetannhltytozirdeinndsspeeeaawrttieeothmbballtanahncnekkess.sffaoomrr Pthphrleeeocswwe:adatusteerorralvlsseaanmDmpltplaenlbekslas..nrkeEEss,aauccsmhh ebbwtlaheanorndkek errreeeavsvciuihelewtawewenddaasaalcc.ccreoorvrddieiinwnggedftoo theand the method and used 0 used to evaluate method and used to evaluate method performance 1 determine the LOG or method performance. Procedural blank results were evaluate method performance to determine the LOQ for each analyte. L33o..6w6. miLLd,aabbandCCoohningthtrlroaolbl cSSopnptiiokkleessspik((eLLsCCwSSesrse))prepared and analyzed in plate. The LCS samples were pILparorbeewopp,raaamrrteeoidddr,ybbaMyyndsspphiQikkigiinhngglwakkabnntcoeoorwwnnnttoroaaplmmsoropuuoinkntedtsss wootfhfeettrhehseeipaarrenneapaldalyyrtecteeodniiacnnnettoodnt11aa00ntoammnlyL.LzeoodfTf hllianaebbtooLrirrpCaalittcSooarrtyywee.rrereTaeahggleeeunntLttCewwdSaattwseearirmhoorprmlee11tsmmhwaLLrecrooelff uilinannbcttohhreeaertoassraaiymmniMeeynilliS-mmQeaca7ntMninnoewenrra3t7aae.ssr the samples. to produce the the samples. Al LCS resus were used fo desired concentration. The LCSs All LCS results were used to determine overal meifod were diluted with methanol determine overall method uncertainty in Section 3.7. TT2h0he5em%m,eetwthhhooeddn aaecvcacelputacatneecdeicprcnirdtietteeprreiianaasdstetannatttleecysstathhetaaettattchhhee caaovvneecrreaanggteerarrteiecooncvleoervyavo.ofef LLrACClySSlLbbCeeSs1100m00e%t% a&+2c2c0e0p%%tawwniicttheh aacrRRtSSiDDa wilh the folowing exceptions <20%, when evaluated independently with the following exceptions: at each concentration level. All LCSs met acceptance criteria 99//1166//1166AAnnaaylyssii:s: TThheelloowwsseett oofLf LOCSSSsffoorr PPFFBBAAhhaadd aann aavveerraaggee rreceovceoryovoffe113r344%y%. TsTehhceetiobbnaattc3chh7 LLoCCfSSherreeccrooevpvoeerrrtyy. rreessTuuhlltess wwfoeelrrleeowirrneegvviiecewawkeeuddlawwtihhoeennns weevevaarlleuuaatutiisnneggd tthfhoee gaaennnaaellryyaitictcaeallcddaaattataa inuunnTcceaerbrtltaaeiinnt7tyyfioinnr Iaboratory conv) spikes. section 3.7 of the report. laboratory control spikes. The following calculations were used to generate data in Table 7 for Calin Commer; LCS Percent Recovery - Calculated Concentrat ion. 100% I I Spike Concentrat ion I i a [CS LCS% RSD = standard deviation LCS replicates . 100% I I I average LCS recovery PAGE 9 OF 27 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTTT,EECNCTOTI.IVV2EE7-OOCRRV-DD1EE0RR-28EE8NN6TT2EERREEDD IINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00000099 I3MM_MMNNO044884444774411 MEWRO`NREMPEONRTTIANGLKLOA1BO0R1A0T0O2R6Y 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 TTaabbllee 77.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReeccoovveerryy.. erssous ETS-8-044.3 EtemaiCattaton External Calibration |soyassaions prea PFOA Linear Branched)| Analyzed 9/16/16 PFBA PFOA (Linear + Branched) Labo ConclSeopnghtirona)dt| ion | CoCncaoecgnutirm)aotdio|n sReco ConocSgapnkierdato|n| CoiCncgeanterantion Reco Lab ID Spiked Concentration (n~llmL) Calculated Concentration (n~l/mL) % Recovery Spiked Concentration (nglmL) Calculated Concentration (ng/mL) % Recovery cstennist 090 as 090 LCS-160915-1 9.90 13.5 136 9.90 11.0 111 westemisz om rr 990 LCS-160915-2 9.90 12.7 128 9.90 11.0 111 es ramiss 000 1 000 LCS-160915-3 9.90 13.1 132 9.90 11.1 113 [avwogerwrso| weewases [TTCnmmenss | Average + %RSD 134% + 3,0% (1~ 112% + 1,8% Les temies wo Te ns 0 3 To LCS-160915-4 99.0 114 115 99.0 109 110 estes @0 no m %0 wo wo LCS-160915-5 99.0 110 111 99.0 109 110 rey @0 105 ws 20 06 ww LCS-160915-6 99.0 105 106 99.0 106 107 [memgeswrso| imran |Cemex | Average _+ %RSD CstemisT wn ED) wo LCS-160915-7 111% _+ 4,1% 498 477 95.9 109% _+ 1,6% 498 463 93.0 esieniss - 81 se LCS-160915-8 498 489 98.1 498 467 93.8 westenise so 1 [avemgecsmso | LCS-160915-9 498 Average _+ %RSD seresaaw | esawsasw 510 102 98,7% _+ 3,1% 498 494 95,3% _+ 3,5% | 99.1 ETS-8-044.3 EtemaiCattaton External Calibration 2 srazesorns -- cree Analyzed 9/16/16 te Conpcoanition ng) ' Lab ID cstennist 990 065 ra LCS-160915-1 Les teonts2 om ase 5s LCS-160915-2 Les remisa 09 aso 0 LCS-160915-3 [avengesmo | oreweam | Average + %RSD Cstemiss ET) wo LCS-160915-4 stems @0 LCS-160915-5 wesiemise 2 ns LCS-160915-6 [mvwogeswms | Coowsren | Average _+ %RSD =r - rl wr LCS-160915-7 Lostenntss - a oa LCS-160915-8 | esemrss - sr 2 LCS-160915-9 Average RSD sana Average _+ %RSD PFOS (Linear + Branched) Spiked Calculated Concentration Concentration (nglmL) . (ng/mL) % Recovery 9.90 9.65 97.4 9.90 9.46 95.5 9.90 9.90 100 97,6% _+ 2,3% 99.0 99.4 100 99.0 101 102 99.0 97.6 98.5 100% + 1.8% 498 468 94.1 498 485 97.3 498 5O7 102 97.8% + 4.1% (1) Ton rag recovery ctmaesceptnce cron 100+ 30% (1) The average recovery did not meet acceptance criteria of 100 + 30%. 2) LCSwas sph pstGuson, opr we hediz a pp. (2) LCS was spiked post dilution, but reported with the dilution factor applied. pace oF PAGE 10 OF 27 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOTAACOPPURRROOTTT,EECNCTOTI.IVV2EE7-OOCRRV-DD1EE0RR-26EE8NN6TT2EERREEDD IINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00001100 I3MM_MMNNO044884444774422 MEWRO`NREMPEONRTTIANGLKLOA1BO0R1A0T0O2R6Y 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 `TTaabbllee 77 ccoonnttiinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReeccoovveerryy.. Erse0ua ETS-8-044.3 ExwnaiCaton External Calibration sozesorne Analyzed 9tl 8/16 Lab ID Los temrst LCS-160915-1 westamisz LCS-160915-2 semis LCS-160915-3 [memgeewms Average 4- %RSD LCs teomiss LCS-160915-4 Lesteoniss LCS-160915-5 wesremise LCS-160915-6 [aegeewms Average 4- %RSD Spiked Concaniation Concentration ingimi) (n1/mL) osee0.988 osse0.988 | oss0.988 39.8 39.8 |39.8 [13C3].PFBA (2) Calculated Concentration pe(n1/mL) 1051.05 105. 1.05 osrz 0.972 osmeasn 104% _+ 4.5% az42.2 as43.3 as42.3 ormeren 107% + 1,6% reco Concinogneina)tion %Recovery I) ose 106 ose 107 ons ose 98.4 Spiked Concentration (n1/mL) 0.988 0.988 0.988 | To106 39.8 wo109 39.8 | wo106 39.8 Erseous ETS-8-044.3 tmaiCatnton External Calibration sezes016nE Analyzed 9/18/16 [13C4]-PFOS (~) Lab ID Cstemier LOS-160915-1 Lesemisz LCS-160915-2 testers LCS-160915-3 [awmgecunso Average _+ %RSD estemiss LCS-160915-4 [reser LCS-160915-5 Les temise LCS-160915-6 [mvemgerwmso Average _+ %RSD Spiked Concent| Concaniation Concentration loge) Togo) co (nglmL) 102 wo 0.947 wor ns 0.947 or o 0.947 | Cowwweozen wo | 38.1 "wr eo 38.1 1 vowaarzm m 38.1 Calculated Concentration (ng/mL) 1.02 1.07 1.01 109% _+ 2,9% 41.9 44.1 42.7 113% _+ 2,7% % Recovery 108 113 107 110 116 112 (1) Toawrangkmeataeccecptaoncreof1r003y0%. (1) The average recovery did not meet acceptance criteria of 100 + 30%. 2) LCSwos pkedpost kaon btrocred wih he donfcrss. (2) LCS was spiked post dilution, but reported with the dilution factor applied. ro [1304].PFOA (2) Calculated gm) Concentration (n1/mL) 1.05 1.05 0.972 reeeass 104% _+ 4,6% az42.2 a43.3 342.3 meres 107% _+ 1,6% % coRecovery 106 107 98.4 Tw | 106 0109 oe | 106 PAGE 11 OF27 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOTAACOPPURRROOTTT,EECNCTOTI.IVV2EE7-OOCRRV-DD1EE0RR-28EE8NN6TT2EERREEDD IINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00001111 I3MM_MMNNO044884444774433 MEWRO`NREMPEONRTTIANGLKLOA1BO0R1A0T0O2R6Y 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 `TTaabbllee 77 ccoonnttiinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReeccoovveerryy.. Erso0ut ETS-8-044.1 tenaCaran Internal Calibration soaized 10516 Analyzed 10/5/16 PFBA PFOA (Linea+r Branch) PFOA (Linear + Branched) Concianngiimai)tion Lab ID Los terunet ore LCS-161004-1 wstemz ore LCS-161004-2 estes ose LCS-161004-3 [memgeewnsp| Average 4- %RSD LCs tetnes LCS-161004-4 Lesteronis LCS-161004-5 westerns LCS- 161004-6 [mwngeewms | Average 4- %RSD LCs terner ws LCS-161004-7 wesieunts 0s LCS-161004-8 frssreny 2s LCS-161004-9 p----re Average 4- %RSD Spiked Concentration (n11mL) 0.198 0.198 0.198 1.98 1.98 1.98 39.6 39.6 39.6 Calculated Concentration pe(n1/mL) ore0.162 oe 0.146 ote0.160 eneraw 81,1% _+ 1,2% 202.03 01.99 202.02 demos 102% + 0,57% 3635.6 635.6 x835.8 01% 2030 90.1% -+ O.38% 2 Concinogneina)tion gm) %Recovery ae oro arse 81.6 ns oro om 73.5 =e om oso 80.6 | 0) [r) mewsozs 102 or 150 101 2 190 102 | we 20 srme4zss 89.9 o 10 ws 89.9 ns 10 asPuYs ran 90.5 Spiked Concentration (ng/mL) 0.190 0.190 0.190 1.90 1.90 1.90 38.0 38.0 38.0 Calculated Concentration (ng/mL) 0.159 0.170 0.159 83,8% _+ O,24% 1.73 1.80 1.81 93,7% _+ 2,3% 32.4 32.8 33.3 86.5% + 1.3% co % Recovery ws83.9 wr89.7 a1 | 83.7 91.2 94.6 95.3 we | 85.4 we86.4 ae87.6 ETS-8-044.1 EArE ad 10518 Internal Calibration Analyzed 10/5/16 | cree PFOS (Linear Branched) | Lab ID Los termner LCS-161004-1 Lesteionez LCS-161004-2 rer LCS-161004-3 [awogeswnss Average + %RSD (esters LCS-161004-4 Lesteiones LCS-161004-5 esters LCS-161004-6 Average 4RSD Average _+ %RSD Losteioner LCS-161004-7 stents LCS-161004-8 esieimio LCS-161004-9 [nvwmgeswms Average 4- %RSD Spiked Concentration Concentration ing) pe y (n1/mL) ores ws 0.184 ore os 0.184 oser wr 0.184 | wawsarm oss | 1.84 ws 1.84 =o 1.84 7 san2020m a2 36.7 %7 uz nz 36.7 | 7 wnFawYsam 0 | 36.7 Calculated Concentration (n1/mL) 0.155 0.160 0.167 87,3% + 3,7% 1.76 1.70 1.80 95,4% + 2,9% 32.0 34.2 33.4 90,4% _+ 3,3% %Recovery 84.3 86.8 90.7 95.8 92.5 98.0 87.2 93.2 90.9 (1) Toaragakemteaceecpiancoreraofr103+y30%. (1) The average recovery did not meet acceptance criteria of 100 _+ 30%. 2) LCSwasspdpost aon, ut100 whth honfcrapples (2) LCS was spiked post dilution, but reported with the dilution factor applied. PAGE 12 OF 27 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOTAACOPPURRROOTTT,EECNCTOTI.IVV2EE7-OOCRRV-DD1EE0RR-28EE8NN6TT2EERREEDD IINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00001122 I3MM_MMNNO044884444774444 MEWRO`NREMPEONRTTIANGLKLOA1BO0R1A0T0O2R6Y 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 `TTaabbllee 77 ccoonnttiinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReeccoovveerryy.. Erse0oua ETS-8-044.3 tenaCaran Internal Calibration soaized 10516 Analyzed 10/5/16 ro [13C3]-PFBA rey[13C4]-PFOA Concianngiimai)tion pe Lab ID Los terunet ores LCS-161004-1 wstemz ore LCS-161004-2 estes orm LCS-161004-3 [memgeewnsn| wmeerss Average + %RSD LCs tetnes LCS-161004-4 westerns LCS-161004-5 westerns LCS-161004-6 [aemgeewms | wsawsrm Average _+ %RSD Spiked Concentration (nglmL) 0.197 0.197 0.197 1.97 1.97 1.97 Calculated Concentration (ng/mL) 0.184 0.182 0.179 92,2% _+ 1,6% 1.87 1.90 1.86 96,2% + 1,1% reco Concinogneina)tion gm) %Recovery ne 1) ot 93.6 wz ore om 92.2 os ote om 90.8 | wr eeas18e0nsn 94.7 4 1 96.4 | a4 seweranr en 94.4 Spiked Concentration (ng/mL) 0.198 0.198 0.198 1.98 1.98 1.98 Calculated Concentration (ng/mL) 0.169 0.170 0.173 86,2% _+ 1,2% 1.84 1.81 1.87 92,9% _+ 1,6% erseous ETS-8-044.3 amsCateason Internal Calibration sessed 1016 Analyzed 10/5/16 vegeros. [I~C4]-PFOS Lab ID sterner LCS-161004-1 Lesteiniz LCS-161004-2 Lesterones LCS-161004-3 [awmgecunso Average _+ %RSD westerns LCS-161004-4 esters LCS-161004-5 testers LCS-161004-6 [memgernmso Average _+ %RSD Spiked Concent| Concaniation Concentration fog) gent) co (ng/mL) oreo ores 0.189 one oie 0.189 oxo ose 0.189 | mesnsn es ws | 1.89 168 1 1.89 1 wmewarasn as | 1.89 Calculated Concentration (ng/mL) 0.166 0.182 0.162 89,8% _+ 6,3% 1.71 1.68 1.74 90,5% _+ 1,5% % Recovery 87.6 96.2 85.5 90.6 89.1 91.8 (1) Toawrangkmeataeccecptaoncreof1r003y0%. (1) The average recovery did not meet acceptance criteria of 100 + 30%. 2) LCSwos pkedpost kaon btrocred wih he donfcrss. (2) LCS was spiked post dilution, but reported with the dilution factor applied. % coRecovery 85.3 85.9 87.3 | 92.7 91.6 94.5 | PAGE 13 OF 27 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOTAACOPPURRROOTTT,EECNCTOTI.IVV2EE7-OOCRRV-DD1EE0RR-28EE8NN6TT2EERREEDD IINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00001133 I3MM_MMNNO044884444774455 TTHE 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-26 `TTaabbllee 77 ccoonnttiinnuueedd.. LLaabboorraattoorryy CCoonnttrrooll SSppiikkee RReeccoovveerryy.. Cr ETS-8-044.1 natn External Calibration re ge o Analyzed 10/5/16 w=|m corey |wTrn | EE | se Lab ID oT ee om ar Tome LCS-161004-1 re va | we | om | am | om LCS-161004-2 a | mr |e am | oS LCS-161004-3 fommesams-- s | Average + %RSD rons = w LCS-161004-4 pram | = LCS-161004-5 a - | a. o LCS-161004-6 [omnes mann wma Average _+ %RSD rn CA LCS-161004-7 dint FEE LCS-161004-8 i =a LCS-161004-9 Fr wane Average _+ %RSD PFOS (Linear + Branched) Spiked Concentration (nglmL) Calculated Concentration (ng/mL) % Recovery 0.184 0.163 88.6 0.184 0.155 84.2 0.184 0.161 87.7 86.8% _+ 2.7% 1.84 1.83 99.6 1.84 1.87 102 1.84 1.83 99.7 100% _+ 1.4% 36.7 33.5 91.4 36.7 35.2 95.8 36.7 38.5 105 97.4% + 7.1% Spiked Concentration (ng/mL) 0.189 0.189 0.189 1.89 1.89 1.89 [13C4]-PFOS Calculated Concentration (ng/mL) 0.177 0.179 0.158 90.5% _+ 6.6% 1.84 1.92 1.82 98.7% _+ 3.0% % Recovery 93.4 94.5 83.7 97.5 102 96.5 ------ (1) The average recovery did not meet acceptance criteria of 100 _+ 30% et (2) LCS was spiked post dilution, but reported with the dilution factor applied. 33..77 AAnnaallyyttiiccaall DDaattaa UUnncceerrttaaiinnttyy AAnnaalylyttiiccaall uunncceerrttaaiinnttyy iiss bbaasseedd oonn hhiissttoorriiccaall QQCC ddaattaa tthhaatitiss ccoonnttrrooll cchhaar~tteedd aanndd uusseedd ttoo eevvaalluuaattee a he manos rec&chhtica STO ES. The method accuracy and precision. The method uncertainty is calculated following ETS-12-012.3. The iodo esa ea br sabe Pa sien Fo standard deviation is calculated for the set of accuracy results (in %) obtained for the QC samples. For mmeetthhoodd EETTSS--88--004444..33,, tthhee mmoosstt rreecceenntt ffiiffttyy QQCCssaammplpelesswweerree uusseedd.. TThhee aannaallyyttiiccaall mmeetthhoodd uunncceerrttaaiinnttyy he Sohn ac oA cos rs is calculated by multiplying the standard deviation by a factor of 2, which corresponds to a confidence EE scams na bacco oa ras ro noo Tae level of 95%. When determining the analytical data uncertainty assigned to the sample results in Table aah Pas oder oa LL8 Ss Pm es 1, in addition to the analytical method uncertainty, the batch LCS samples prepared with the projects mes rd SG Se pe TS sina oo Tae 3 samples and field QC data are also reviewed. The analytical data uncertainty is listed in Table 8 below. c Connea rs Shee rYoast erpcwosoa res go1Pit o + TThhee aannaalylyttiiccaall mmeetthhoodduuncnecretrataininttyywwhheenn ccaallccuullaatteedd bbyy EETTSS--1122--001122..33 ffoorr PPFFBBAA bbyy eexxtteermnaall standard calibration was + 16%; however, based on the average recovery for the low level LCSs analyzed on 9/16/16, the analytical data uncertainty was expanded to + 34%. `TTaabbllee 88.. AAnnaallyyttiiccaall MMeetthhoodd UUnncceerrttaaiinnttyy [Lore | ontram [ pir[Wetec| Analyte Calibration Coa| es em an] PFBA Internal [ros| ca ewan] PFOA Internal [Cros [ce | em [on | PFOS Internal Crm eae TwTon PFBA External a rr nr-- PFOA External Cros Tens TaeTom] PFOS External RS -- NA = Not Applicable Standard Deviation (%) 9.51 5.67 6.35 NA 10.2 9.90 Method Uncertainty (%) _+ 19 + 11 _+ 13 _+ 34 _+ 20 _+ 20 PAGE 14 OF 27 CHOENNNFEIPDIENNTCIOAU-LNTSUYBDIIESCTTRITCOTACOPURROTT.EC0T.I2V7E.O0R1O10E2R68E0N2TERED IN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00001144 noiseiris 3M MN04844746 oseems 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-26 3.8 Field Matrix Spikes (FMS) 3.8 Field Matrix Spikes (FMS) rE TTaarrggeett aannaallyyttee ffiieelldd mmaattirixx ssppiikkeess ((FFMMSS)) wweerree pprreeppaarreedd ffoorr eeaacchh llooccaattiioonn wwiitthh tthhee ssppiikkee lleevveell sseelleecctteedd a OESre pms tt based on the results from the last sampling of these locations in 2014. FMSs were generated by adding a measured volume of field sample to a container spiked by the laboratory with the target na analytes prior to shipping sample containers for sample collection. FMS recoveries within method acceptance criteria of 100+30% confirm that "unknown" components in the sample matrix do not aimee significantly interfere with the extraction and analysis of the analytes of interest. FMS concentrations Ten ie Peishh must be at least 50% of the sample concentration to be considered an appropriate spike level. The reference standards for PFOA and PFOS in the field matrix spiking solution consisted of linear and Tee branched isomers. Table 9 lists the locations and spiking levels for which a target analyte FMS was =prepared. re scotsi ry In addition, field matrix spikes for this project consisted of stable isotope surrogate recovery standard ssppiikkeess ((SSRRSSss)) ooff [[1P3CC.3]--PPFFBBAA., [[13'CC4J]--PPFFOOAA aanndd [[1"3CC4,]H-PPFFOOSS,, wwhhiicchh wweerree aaddddeedd aatt aa nnoommiinnaall orcntaonf 0.1 no. to salbts pr sacle To [iad 770A concentration of 0.1 ng/mL to all sample bottles prior to sample collection. The [13C3]-Iabeled PFBA BE En SIC was selected to represent PFBA the [ C4]-Iabeled PFOA was selected to represent PFOA, and the [[1C3aCH4a]-bIaebleeledd PPFFOOSS wwaass sseelleecctteedd ttoo rreepprreesseenntt PPFFOOSS.. FFoolllloowwiinngg ssaammppllee aannaallyyssiiss,, iitt wweass ssuussppeecctteedd [EE EE eySh that the surrogate recovery standards were not spiked as intended; therefore, no surrogate recovery ET standard results were used to assess sample recovery. ES The following calculation was used to generate the field matrix spike recovery in Section 4 of the report: FMS Recovery = (Sample Concentration of FMS - Averagespike ConcentrationCncentratin : Field Sample & Field Sample Dup.), 100% Table 9. Field Matrix Spike Levels. [om 2 2 2 Sampling location [w ivr e`vwn |w]e | IW-14b-sw, IW-19-sw, IW-25f-sw PFBA (ng/mL) 0.100 PFOA (ng/mL) 0.100 PFOS (ng/mL) 0.100 IW-14-pw 2.00 2.00 2.00 IW-14f-pw [mmm wo wo | wo | IW-25f-pw, Sets 1 - 5 ESCEE IW-25-pw [mm | mo | m mo | mo| IW-14b-pw, IW-19b-pw, IW-19-pw, IW-19f-pw 5.00 10.0 25.0 50.0 5.00 10.0 25.0 50.0 5.00 10.0 25.0 50.0 [meIW-25b-pw Trip Blank wo [me [| 200 200 200 50.0 50.0 50.0 FS ---------- IW-19b-pw {1) 379 379 379 (1) Due to the limited volume of sample collected, the field matrix spike concentration was adjusted for the final fill volume of 13.2 mL. PAGE 15 OF 27 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00001155 3M MN04844747 MENVRROENPMORETNITNGA,L5L0A7B7O0R1A0T3O2R5Y 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 44 DDaattaa SSuummmmaarryy aanndd DDiissccuussssiioonn T"sTahhmeeplttaiabnilgeesslobbceealltooiwownsssuuammsmmwaearlriizzaees ttthhheee ssTarampmpBelleanrrkee.ssuulRlttesssaaunnltddsttaaarnrggdeetvt aaalnnuaaelysltyearffeieiaelddvemmraaalgtreiixrssoppuiiknkedeerrdeeccfoofvvererreiieeess foorr hthee sissogaigsnmnfoipifilccilnaaignsntteliodfigcgnuaurttreiheosensaarccaaccswoowrdraddetiilanln.ggast1Fo0itheEEekPPdTAAmriaprroroBuuxnnladdsniipnkni.ggkerRruemelseese.sut.ltiBBsneegactcnaahduuessvmeealueoofefhsorouaunrndeadicaincnvgege,p,rtavvaaagnlelucueeerosstummneadareyyvadvactarofryyt+shsir3leig0geh%ht,tly ffroomm tdadhneeogmmseoeosnn.sliissrttrBeaadetteceianttuhhthsateettthohraefewrmmodeueantttdhhaioo.nddgF,siisevlaaadplppumpreroasoptpmrririxaiaaysttvepeaifkforoeryrtmthhegeoehggtitivnvgeefnntohmmemaamttrxeihxtohasaonenddsattthcehceedeiirpireteastsnphpoceecercitaciivrwvieteeGtqrqiaauu.aaonnftF+ittiaei3ltiz0dv%eem,ati ssmrappeniitkkgheeeosssd.aanniBsddeasscpuuaprrurroosogpegaiaotatefteerorrefeucconoordvvtienehrgrii,geeivssvammelunoeeemesitainmnigga.ytthhveeammryeetsthhligoohddtlaayccfccroeemppttatahnnoccseeeccrlriiistteteerrdiiaainooffth+e3300r%%a,w, dddeeammtaoo.nnsFstiterraladttemtthahaatrttixhthee method is appropriate for the given matrix. TTmhheeesmmetehttehhooeddxpiienncddiiicecaadtteaessnattlhhyaatttethhceeonttacarreggneetttaaainnoaanllyyntteehFFeMMsSSamsspaalmmep.plleeTsshesshhfooiuueldlddmbbaee sslppiSkepedidkaeattacapoppnrpcoreoxnxitimmaaiatotenellyywa00s.55--1100 tssliaeemsllteeecscstiaetemhddpelbbieaanxssgpeeoeddfcotohennedstthaheenealeeloyxxctppaeeetciccototneensddcieccnnoo2tnn0rac1c4teei.onnntrraaiAnttiSoothnneeoosfsfauPPmlFFpOOtleAAh.eaaTsnnhpddielk/oofeirreelPPdvFFemOO,SaS,at,trixbbtaiasmsspeeeiskdd,eooecnnxocttnhehceeeednrreetedrssauuttllithossenffrwrooamms tthhee rwlraeeasccstoosmramemmmpoeeprnnltidndegededdoafuuntpphppefeelsrareglligilmomeicdittaooatifsfo1n1a00sbottiniivmme2ee0ss110tt4hh.teeeaaAnsnsaaltalyyhttreeeessccuaoolmntnpctchleeeennttscrapoatnitokicoenen.nl.tervIIaenntl,itnhoaeentssteeimAliilennssss,tuiaeaonnxgccceaeessteetdthheeredeFFcthoMMevSSerrryeeccoovveerryy wseSxttaacasennpddrteaairprodcnosssr.teaadnnddafnfieddldflammgaagtterdiix Spe recoveriesmat method acceptance cena as above 10 times the sample concentration. All spike recoveries met method acceptance criteria wih he folosing surrogate recovery with the following exceptions. IsIWWa-m-1p14l4beb--cppowwn-t-TTa:i:nDDeruuseetwtoeorttehheenolmitmifiltteeedd.vvooTllnuumemeesuootffossgaaammtpeplrleeecccoovllleeercyitesd,t,ahtnhdeearffideoslld,d wddhuuippcllihccamateeetaamnneddtifhieokldd mmacaaclteriipxtssappniickkeee cea, sample criteria, were used containers were used 1 assess method accuracy. were not filled. The surrogate to assess method accuracy. recovery standards, which met method acceptance W4IW-3t-1%d4--fssowwr::PFTTBhhAee.FFMNSS rreeccoovevreyrffooyr PPFFBAA wwaass 114433%%.. TThhee mmeetthhoodd uunncceerrttaainitny hhaass bboeeenn eexxppaannddeedd ttoo +43% for PFBA. wIIWWa-s-11n99ob0--pfuiwl-e-dTT.:: TDDuuheefttiooelhtdheesalmmimpiilteeedavvnoodlluiummee oosffassaammmpppllceeupoclolclelaectcieteehd,a, dhthaee RffielPeldDd mmofaa2trti2x%sspfpixkkeePRssOaammSp.plleeTcchooennttaaiinneerr was not filled. The field sample and field sample duplicate had a RPD of 22% for PFOS. The SZcucourgaacty,e recovery standards, wich met method accepianc cre, were used 1 assess method surrogate recovery standards, which met method acceptance criteria, were used to assess method accuracy. InIWoWt--1l19o9dbb.--ppwwT-h-ppepp:f:ieDDlduumeateltooritthxheesplliiimmkiietteceoddnvvtooalliunumemreevooaffsssaaummnpdpleleerccofiollelleecdicaetednd,, ttthhhetffaiieregllddetdduunpplaliitccaaetteessspaaimmkepplcleeocnoccnoetnnattairinaneteirrwownaass Saandadojmjtuupfssillltteeeedddc.oaanTcccchcoeoernrdtdfirieniangltdgliylyom.n.afTTtorhhrixeePsFrrpeeEikssAeuulltaciinnonggdntssaPppiRniikOkeeSer,wccooabnnsuccteueninniddtrreaamrtiieofoielnnltewwdmaaeassntdhnnooottdht eaaapptcpapcrrreogoppeprltriaiaaantntceeael3ayrssteeccrsooepmm,ipkpeaarrTceeohddnecftoroeenhthstreeuastiohnave. been flagged accordingly. sample concentration for PFBA been flagged accordingly. and PFOS, but did meet method acceptance criteria. The results have IPIWWF-O-11S99:--pphwwo-w-TTe:v: eTTrhh,eehffeiieelalddvdecurupapiglicceaartteeecssoaavemmrppylleeorhhaatddheaasSSamRRpSSlerreescecotovfevorrey[ro1o'f3yfC11:33-55Po~%F/oBffAoorrabbnoodtthh|[1*31CC3JC:-3-P]-PPFFOFBBSAAmeaanntddm([e1"3tCCii4o]f-d acceptance cieria and no acjusiment was made {0 the daa PFOS; however, the average recovery for the sample set for acceptance criteria and no adjustment was made to the data [uunncCcee3rtr]-taaPiinFntBtyy.A. and [ C4]-PFOS met method mIIWWe-t-11h99o.d-s5wwun::ceTTrhhtaeeinFFtMIySSharrseecbcoeoveevnreyerfxfooyprraPPnFFdeBBdAAfwworaasPsF11B338A8%%,[0, ffoo3rr8PP%,FFOOfoAAr P1133F68%%O[aaA0nndd3ffoo6rr%PP,RFaOOnSSdf11o33r88P%%F.OSTThh0ee 136%. method uncertainty has been expanded for PFBA to +38%, for PFOA to +36%, and for PFOS to +38%. sIIWpWi:-k22e55s0ba--mpppww-l-TeT-c-ddounupap:i:nDDeuruseewtteoorttheheenilimomiitlteeeddd.vvoollTuumhmeesoofufsosagamamptplaleereclcoeolclveetcretyedsd,t,ahtnhdeearffidoeslldd, udwpuhplilccicahattmeoeaatnnmddefitiehdloddmmaartrixx acceptance citeria, wero sod to assess method accurcy. spike sample containers were not filled. The surrogate recovery acceptance criteria, were used to assess method accuracy. standards, which met method PAGE 16 OF 27 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTTT,EECNCTOTI.IVV2EE7-OOCRRV-DD1EE0RR-28EE8NN6TT2EERREEDD IINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00001166 M3M_MNMON40B448444774488 fr -- Table 10. IW-14b-pw-T 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 PFBA 3M LIMS ID Sonne wher ISO11-01-03-26-001 Sonar | Wie" Seskoses ISO11-01-03-26-001-DUP Description IW-14b-pw-T - Sample IW-14b-pw-T - Sample Duplicate CT ave commmsaszars ISO11-01-03-26-001-FMS IW-14b-pw-T - FMS Average Concentration (ng/mL) _+ %RPD NA = Not Applicable arstcsn. Samples were analyzed by external standard calibration. Table 11, Wetton Table 11. IW-14b-sw Concentration (ng/mL) %Recovery 27.8 NA 28.2 NA | mops 83.3 111 28.0 ng/mL _+ 1.4% PFOA PFOS Concentration (ng/rnL) %Recovery Concentration (ng/mL) %Recovery 99.7 NA 13.4 NA 98.9 NA 12.2 NA msi |nesses | 145 91.4 99.3 ng/mL _+ 0.81% 62.6 99.6 12.8 nglmL _+ 9.4% PFBA 3M LIMS ID Description Concentration (ng/mL) %Recovery ISO11-01-03-26-003 IW-14b-sw - Sample <0.0250 NA ISO11-01-03-26-003-DUP IW-14b-sw- Sample Duplicate ISOll-01-03-26-003-FMS IW-14b-aw- FMS Average Concentration (ng/mL) _+ %RPD <0.0250 NA 0.143 143m <0,0250 nglmL (2) oat getcon NA = Not Applicable Samples were analyzed by internal standard calibration. (1) The field matrix spike did not meet method acceptance criteria of 100 _+ 30%. (2) The method uncertainty has been expanded for PFBA to _+ 43%. PFOA Concenl]ation (ng/mL) %Recovery 0.0566 NA 0.0500 NA 0.173 120 0.0533 nglmL + 12% PFOS Concentration (ng/mL) %Recovery 0.0260 NA <0.0232 NA 0.144 118 0.0260 ng/mL TaeTable 1122.. Wet4pw IW-14-pw-T PAGE 17 OF 27 D`CICOSOTNNRFFIIIDCDETENCNOTTIUIARALTL-,SSUUNBBOJ.JEE2CC7TT-CTTVO-O1AA0:P2P8RR8OO6TT2EECCTTIIVVEE ORDER ORDER ENTERED ENTERED IN IN HENNEPIN HENNEPIN COUNTY COUNTY DISTRICT COURT, NO. 27-CV-10-28862 2085.0017 2455.0017 pr3M MN04844749 eeThe PFBA PFOA 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 [we] PFOS 3M LIMS ID sonora |WoeoeT samen ISO11-01-03-26-004 soins 0k0um sep SD ar n ISO11-01-03-26-004-DUP Description IW-14-pw-T - Sample IW-14-pw-T- Sample Duplicate Concentration (n~l/mL) 32.7 33.9 %Recovery NA NA Concentration (n~l/mL) 66.0 64.6 %Recovery NA NA Concentration (n~l/mL) 9.46 7.93 %Recovery NA NA CC vomcommmommizaro |ssmgnisn | esmein | smegma | ISO11-01-03-26-004-FMS IW-14-pw-T - FMS Average Concentration (ng/mL) _+ %RPD 33.4 NC 33,3 ng/mL _+ 3,6% 65.3 NC 65,3 nglmL _+ 2.1% 11.0 NC 8,70 ng/mL _+ 18% RS EINEI R,cnS emsm nc ec sn orn NA = Not Applicable NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concentration. Samples were analyzed by external standard calibration. Tae 13. WerpwtT Table 13. IW-14f-pw-T C mT T wer [wwe PFBA Ill PFOA (~1 PFOS 3M LIMS ID Sonera |eiweeT Soe ISO11-01-03-26-005 SonLRLS |MeikeeT.Supaoges ISO11-01-03-26-005-DUP Description IW-14f-pw-T - Sample IW-14f-pw-T - Sample Duplicate Concentration (ng/mL) =e92.6 | 01894.8 %Recovery =NA "NA ISOll-01-03-26-005-FMS IW-14f-pw-T - FMS 106 NC Average Concentration (ng/mL) _+ %RPD 93,7 ng/mL _+ 2.3% REE sa tn nrt NA = Not Applicable NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concentration. RE ate pense cen (1) Samples were analyzed by external standard calibration. (2) Samples were analyzed by internal standard calibration. (3) FMS spike concentration was greater than 10X the endogenous sample concentration. ConcentTation (ng/mL) ox50.4 us44.4 %Recovery | eam | we NA w | sem | ow NA Concentration (ng/mL) <0.0232 <0.0232 %Recovery NA NA 57.2 NC 5.86(31 117 47,4 nglmL _+ 13% <0,0232 nglmL Tobe Table 1414. W100. IW-19b-pw-pp PAGE 18 OF 27 D`CICOSOTNNRFFIIIDDCEETNNCTOTIIUAARLLT.-,SSUUNBBOJ.JEE2CC7TT-CTTVO-O1AA0:P2P8RR8OO6TT2EECCTTIIVVEE ORDER ORDER ENTERED ENTERED IIN HENNEPIN HENNEPIN COUNTY COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00001188 WeNoAsaa750 3M MN04844750 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 3M LIMS ID Description Concentration (ng/mL) % Recovery ISO11-01-03-26-007 IW-19b-pw-pp - Sample 18.3 NA ISOll-01-03-26-0007-FMS IW-19b-pw-pp- FMS 398 (~) 100 Concentration (ng/mL) 18.3 ng/mL NA = Not Applicable tycrcs t Samples were analyzed by external standard calibration. A SE pean cate. (1) FMS spike concentration was greater than 10X the endogenous sample concentration. Tate 15. WAS wT Table 15. IW-19-pw-T ee PFBA 3M MMS ID Cons | Wt town ISO11-01-03-26-008 soni mamor|i seveosm ISO11-01-03-26-008-DUP Description IW-19-pw-T - Sample IW-19-pw-T - Sample Duplicate AteConcnrtonpd 5550. ISO11-01-03-26-008-FMS IW-19-pw-T- FMS Average Concentration (ng/mL) _+ %RPD J NA = Not Applicable Samples were analyzed by external standard calibration. Concentration (ng/mL) 589.3 | a391.3 % Recovery NA NA I mamgmiam. 137 93.4 90,3 ng/mL + 2.2% Concent]-ation (ng/mL) %Recovery 47.9 NA 413 96.4 47.9 ng/mL Concentration (ng/mL) %Recovery 17.7 NA 374 (~) 94.1 17.7 ng/mL we PFOA [wePFOSs] Concentration (ng/mL) %Recovery 121 NA 124 NA gman 174 103 123 ng/mL + 2.4% Concentration (ng/mL) % Recovery 37.4 NA 36.9 NA Tangs in 88.1 102 37.2 ng/mL + 1,3% Tate 16. Wes Table 16. IW-19-sw PAGE 19 OF 27 D`CICOSOTNNRFFIIIDCDETENNCTTOIIAUALRLT-,SSUUNBBOJJEE2CC7TT.0TT1O-O1AA0.P2P8RR0OO6TT2EECCTTIIVVEE ORDER ORDER ENTERED ENTERED IN IN HENNEPIN HENNEPIN COUNTY COUNTY DISTRICT COURT, NO. 27-CV-10-28862 2085.0019 2455.0019 W_osaas7t 3M MN04844751 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 3M LIMS ID Description Concentration (ng/mL) % Recovery ConcenlTation (ng/mL) % Recovery ISO11-01-03-26-009 IW-19-sw - Sample <0.0250 NA <0.0240 NA ISO11-01-03-26-009-DUP IW-19-sw - Sample Duplicate <0.0250 NA <0.0240 NA ISO11-01-03-26-009-FMS IW-19-sw- FMS 0.138 138m 0.136 136 (1) Average Concentration (ng/mL) _+ %RPD <0,0500 nglmL (2) <0.0240 ng/mL (2) NA = Not Applicable assmarass sn. Samples were analyzed by internal standard calibration. (1) The field matrix spike did not meet method acceptance criteria of 100 _+ 30%. TETT an wasn. (2) The method uncertainty has been expanded for PFBA to _+ 38%, for PFOA to _+ 36%, and for PFOS to _+ 38%. Concentration (ng/mL) % Recovery <0.0232 NA <0.0232 NA 0.138 138 (1) <0.0232 ng/mL (2) Tae Table 1177.. WowT IW-19f-pw-T TrePFBA Te[we PFOA PFOS 3M LIMS ID Description Concentration (ng/mL) % Recovery ISO11-01-03-26-010 IW-19f-pw-T - Sample 59.7 NA ISO11-01-03-26-010-DUP IW-19f-pw-T - Sample Duplicate 54.8 NA ISO11-01-03-26-010-FMS IW-19f-pw-T - FMS 105 95.5 Average Concentration (ng/mL) _+ %RPD 57,3 ng/mL + 8,6% an NA = Not Applicable NENCitste etsso un rrsrg cnr. NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concentration. ty rae Samples were analyzed by external standard calibration. chemi so on 5i rh re (1) FMS spike concentration was greater than 10X the endogenous sample concentration Concentration (ng/mL) %Recovery 150 NA 152 NA 180 NC 151 ng/mL + 1,3% Concentration (ng/mL) %Recovery 3.86 NA 3.78 NA 52.8{1) 98.0 3,82 ng/mL + 2.1% atkTable 1188.. WasT IW-25b-pw-T PAGE 20 OF 27 D`CICOSOTNNRFFIIIDCDETENNCTTOIIUAARLLT.-,SSUUNBBOJ.JEE2CC7TT-CTTVO-O1AA0.P2P6RR6OO6TT2EECCTTIIVVEE ORDER ORDER ENTERED ENTERED IIN HENNEPIN HENNEPIN COUNTY COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00002200 WeNodsaa7s2 3M MN04844752 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 3M LIMS ID Sonora [iio n ISO11-01-03-26-011 sono1001IOP | Wipe" Stroker ISO11-01-03-26-011-DUP Description IW-25b-pw-T - Sample IW-25b-pw-T - Sample Duplicate Concentration (ng/mL) 69.5 66.6 % Recovery NA NA Concenl]-ation (ng/mL) 64.8 68.3 % Recovery NA NA Concentration (ng/mL) 101 109 % Recovery NA NA CT eeconmmsenpmressrs |mamma | sammain | wep ISO11-01-03-26-011-FMS IW-25b-pw-T - FMS Average Concentration (ng/mL) _+ %RPD 285 108 68.1 ng/mL_+ 4.3% 279 106 66.6 ng/mL _+ 5.3% 337 116 105 ng/mL _+ 7.6% S er E menses on, NA = Not Applicable Samples were analyzed by external standard calibration. athTable 1.19. W289 IW-25b-pw-pp 3M LIMS ID Description ISO11-01-03-26-012 IW-25b-pw-pp - Sample ISO11-01-03-26-012-DUP IW-25b-pw-pp - Sample Duplicate rr mnpg 3950. ISO11-01-03-26-012-FMS IW-25b-pw-pp - FMS Average Concentration (ng/mL) _+ %RPD i ------ NA = Not Applicable Samples were analyzed by external standard calibration. PFBA Concentration (ng/mL) % Recovery 73.9 NA 72.0 NA fre 282 105 73,0 ng/mL_+ 2.6% PFOA Concentration (n~l/mL) %Recovery 62.3 NA 61.9 NA iain 260 99.0 62.1 ng/mL _+ 0,64% PFOS Concentration (n~l/mL) %Recovery 78.3 NA 83.3 NA ares 272 95.6 80,8 ng/mL _+ 6,2% Table20.W25pT Table 20. IW-25-pw-T PAGE 21 OF 27 D`CICOSOTNNRFFIIIDCDETENCNTOTIUIARALT-L-,SSUUNBOB.JJEE2CC7TT-CTTVOO-1AA02PP8RR8OO6T2TEECCTTIIVVEE ORDER ORDER ENTERED ENTERED IN IN HENNEPIN HENNEPIN COUNTY COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00002211 WORT 3M MN04844753 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 3M LIMS ID Sonne We sn ISO11-01-03-26-013 sottanrsis | ice? seomOuken ISO11-01-03-26-013-DUP Description IW-25-pw-T - Sample IW-25-pw-T - Sample Duplicate ISO11-01-03-26-013-FMS IW-25-pw-T - FMS Average Concentration (ng/mL) _+ %RPD ER ay erraen NA = Not Applicable (1) Samples were analyzed by external standard calibration. (2) Samples were analyzed by internal standard calibration. Tate21, WastuT Table 21. IW-25f-pw-T Concentration (ng/mL) % Recovery 27.6 NA 27.4 NA 51.7 96.8 27.5 ng/mL_+ 0.73% me PFBA (1) 3M LIMS ID Description Concentration (ng/mL) %Recovery ISO11-01-03-26-014 IW-25f-pw-T - Sample 21.0 NA ISO11-01-03-26-014-DUP IW-25f-pw-T - Sample Duplicate 24.0 NA ISO11-01-03-26-014-FMS IW-25f-pw-T - FMS 32.3 98.0 Average Concentration (ng/mL) _+ %RPD 22.5 ng/mL_+ 13% NA = Not Applicable Ee ty sent srt. (1) Samples were analyzed by external standard calibration. mmm (2) Samples were analyzed by internal standard calibration. OT AS Crca ss ves s 2% (3) The sample / sample duplicate did not meet method acceptance criteria of-<20%. Concenl]'ation (ng/mL) % Recovery 36.5 NA 30.9 NA 60.4 107 33.7 ng/mL _+ 17% Concentration (ng/mL) % Recovery 0.104 NA 0.108 NA 25.2 100 0.106 nglmL _+ 3.8% wePFOA (i) [ween] PFOS (2) Concent]'ation (ng/mL) %Recovery 20.3 NA 18.7 NA 30.6 111 19,5 ng/mL _+ 8,2% Concentration (ng/mL) %Recovery 3.61 NA 2.48 NA 15.0 120 3,05 ng/mL + 37% (3~ Tab 22. Table 22. Wtow IW-25f-sw PAGE 22 OF 27 D`CICOSOTNNRFFIIIDCDETENCNTOTIUIARALTL-,SSUUNBBOJ.JEE2CC7TT-CTTVO-O1AA0:P2P8RR8OO6TT2EECCTTIIVVEE ORDER ORDER ENTERED ENTERED IN IN HENNEPIN HENNEPIN COUNTY COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22048555..00002222 Wosaaass 3M MN04844754 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 3M LIMS ID Sonar [Miter Ser ISO11-01-03-26-015 sono1sa00rso | wien sareics ISO11-01-03-26-015-DUP Description IW-25f-ew - Sample IW-25f-ew - Sample Duplicate Concentration (ng/mL) ow | meas <0.0250 ows | wm | <ae <0.0250 % Recovery NA NA Concenl]-ation (ng/mL) <0.0240 <0.0240 % Recovery NA NA Concentration (ng/mL) <0.0232 <0.0232 % Recovery NA NA [avomconmmsmmppmszirs |mame | omen | ISO11-01-03-26-015-FMS IW-25f-sw - FMS Average Concentration (ng/mL) _+ %RPD 0.108 108 <0,0250 ng/mL 0.120 120 <0.0240 ng/mL memes | 0.137 137 (1) <0.0232 ng/mL (2) NA = Not Applicable assmarass sn. Samples were analyzed by internal standard calibration. (1) The field matrix spike did not meet method acceptance criteria of 100 _+ 30%. mT I (2) The method uncertainty has been expanded for PFOS to - 37%. Tatl2. Table 23.EExxttraaBBoottttleeSSeett 11; E6 pp(EqvipmentBan EB-pw-pp (Equipment Blank foorrppuusshh pnt) point) mT we [wee] PFBA PFOA PFOS 3M LIMS ID Description Concentration (ng/mL) %Recovery ConcentTation (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO11-01-03-26-017 EB-pw-pp - Sample <0.0250 NA <0.0240 NA <0.0232 NA ISO11-01-03-26-017-DUP EB-pw-pp - Sample Duplicate EE [Ee[=[ZEEE] ISOll-01-03-26-017-FMS EB-pw-pp - FMS rr mnpg 960. atom amon ET Average Concentration (ng/mL) _+ %RPD <0.0250 NA 11.4m 114 <0,0250 ng/mL <0.0240 NA 10.8(1) 108 <0,0240 ng/mL <0.0232 NA 11.6(1) 116 <0,0232 nglmL Te Ee eo en amscen NA = Not Applicable Samples were analyzed by internal standard calibration. (1) FMS spike concentration was greater than 10X the endogenous sample concentration. Tal2, Table 24. EExxvtraaBBoottttlee SSeet2t2; 1S IW-19-sw-dup PAGE 23 OF 27 D`CICOSOTNNRFFIIIDCDETENCNTOTIUIARALT-L-,SSUUNBBOJ.JEE2CC7TT-CTTVOO-1AA02PP8RR8OO6T2TEECCTTIIVVEE ORDER ORDER ENTERED ENTERED IN IN HENNEPIN HENNEPIN COUNTY COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00002233 SW MNORA4TSS 3M MN04844755 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 3M LIMS ID Sonne ISO11-01-03-26-018 sonnssanon ISO11-01-03-26-018-DUP Description Wiseman Sn Sew IW-19-sw-dup - Sample |tbmes. seoeoskn | ozo IW-19-sw-dup - Sample Duplicate Concentration (ng/mL) <0.0250 <0.0250 % Recovery meme NA |W | owe NA Concenl]-ation (ng/mL) <0.0240 <0.0240 % Recovery NA NA Concentration (ng/mL) <0.0232 <0.0232 % Recovery NA NA ee ISO11-01-03-26-018-FMS IW-19-sw-dup - FMS Average Concentration (ng/mL) _+ %RPD TY 11.1 il) 111 <0,0250 ng/mL TT ----r-- 11.4 (1) 114 <0.0240 ng/mL 11.1 (1) 111 <0.0232 nglmL eas rnco ps an15m srg crs. NA = Not Applicable Samples were analyzed by internal standard calibration. (1) FMS spike concentration was greater than 10X the endogenous sample concentration. Table25.TavlBanc andEquipmentBlak" Table 25. Travel Blank and Equipment Blank PFBA 3M LIMS ID Description Concentration (ng/mL) ISO11-01-03-26-021 Travel Blank <0.0250 ISO11-01-03-26-021-FMS Travel Blank FMS 50.4 i2~ ISO11-01-03-26-022 Equipment Blank <0.0250 SJ e entren sianc is NA = Not Applicable (1) Samples were analyzed by internal standard calibration unless noted otherwise. (2) Samples were analyzed by external standard calibration. %Recovery NA 101 NA PFOA Concentration (ng/mL) <0.0240 53.3 (2) <0.0240 %Recovery NA 107 NA PFOS Concentration (ng/mL) <0.0232 50.9 (2) <0.0232 %Recovery NA 102 NA PAGE 24 OF 27 D`CICOSOTNNRFFIIIDCDETENNCTTOIIAUALRLT-,SSUUNBBOJJEE2CC7TT.0TT1O-O1AA0.P2P8RR0OO6TT2EECCTTIIVVEE ORDER ORDER ENTERED ENTERED IN IN HENNEPIN HENNEPIN COUNTY COUNTY DISTRICT COURT, NO. 27-CV-10-28862 2085.0024 2455.0024 Wosaaase 3M MN04844756 --e--s-- 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-26 `TTaabbllee 2266.. SSuurrrrooggaatteeRReeccoovveerryy (1/ trO e E [sororoszeoor 3M LIMS ID ISO11-01-03-26-001 ISO11-01-03-26-001-DUP EE es EE ISO11-01-03-26-001-FMS ISO11-01-03-26-002 LE L IRE ISO11-01-03-26-003 ee Lr ISO11-01-03-26-003-DU P [sonorosseonsius |wiasesw-ius | w=| wes| wed | ISO11-01-03-26-003-FMS rr ISO11-01-03-26-004 isort010ss500000F |wisouTsam|puwon u|pevme s| ISO11-01-03-26-004-DUP [Csonoroszeoosrus |witepwriws | we | we | wo | ISO11-01-03-26-004-FMS nre h TL ISO11-01-03-26-005 | witibonT-sompe Description IW-14b-pw-T - Sample IW-14b-pw-T - Sample Duplicate IW-14b-pw-T - FMS IW-14b-pw-pp - Sample IW-14b-sw - Sample IW-14b-sw- Sample Duplicate IW-14b-sw - FMS IW-14-pw-T - Sample IW-14-pw-T - Sample Duplicate IW-14-pw-T - FMS IW-14f-pw-T - Sample [13C3]-PFBA [13C4]-PFOA ['I3C4]-PFOS | wo | ws | ws | % Recovery 119 % Recovery 115 % Recovery 125 107 100 110 112 103 115 95.9 95. 102 97.6 (2) 101 (2) 96.8 i2) 111 (2) 102 (2) 97.9 101 (2) 106 (2) 106 (2) 107 107 113 111 106 115 112 108 110 109 104 99.0 (z) ISO11-01-03-26-005-DU P IW-14f-pw-T - Sample Duplicate [Csororoszscosens |wewpwtorus | we | we | wen] ISO11-01-03-26-005-FMS IW-14f-pw-T - FMS ISO11-01-03-26-006 IW-19b-pw-T - Sample Ee TE ISO11-01-03-26-006-DUP IW-19b-pw-T - Sample Duplicate ISO11-01-03-26-007 IW-19b-pw-pp - Sample Ep aneeSE= ISO11-01-03-26-0007-FMS IW-19b-pw-pp - FMS AEE ISO11-01-03-26-008 IW-19-pw-T - Sample [sotoros2e0080up |witopuT-SampieOupleste |ws| wae | uso | ISO11-01-03-26-008-DUP IW-19-pw-T - Sample Duplicate [sISoOr11o-0r1-o03s-2s6e-0o08o-FnMrS m| s mIWe -19-pr w-Tp - FMw S trms| [sonoroszeos |wirosw-sompe | wr | wes| ISO11-01-03-26-009 IW-19-sw - Sample 111 114 115 113 115 79.9 115 me 135 (3) 114 99.7 (21 109 108 (2) 109 118 (2) 111 102 (2) 109 102 (2) 108 114 78.9 81.7 110 116 wm] 124 135 (3) 107 117 102 (2) 99.0 ISO11-01-03-26-009-DU P [sororoszeocarns |wetoewrws ISO11-01-03-26-009-FMS [sonorsszeon |weopnrsampe ISO11-01-03-26-010 IW-19-sw - Sample Duplicate IW-19-sw - FMS IW-19f-pw-T - Sample 96.0 (21 | we| iE| wes | 102 (2) | ms | wee| we | 113 99.1 (2) 101 (2) 109 91.5 (2) 109 (2) 114 ISO11-01-03-26-010-DUP [Csonorosseonrus |weotpatiws ISO11-01-03-26-010-FMS [Csonoroszeon |wiaseonrsampe ISO11-01-03-26-011 IW-19f-pw-T - Sample Duplicate IW-19f-pw-T - FMS IW-25b-pw-T - Sample | me113 114 | we109 112 | wo116 120 | | wr117 | wo110 | wm121 | [Csonovaszeoreus ISO11-01-03-26-011-DUP ISO11-01-03-26-011-FMS |masmpnrorus IW-25b-pw-T - Sample IW-25b-pw-T - FMS Duplicate | wr117 107 | te111 104 | wo116 110 | ISO11-01-03-26-012 IW-25b-pw-pp - Sample 124 120 126 ISO11-01-03-26-012-DUP IW-25b-pw-pp - Sample Duplicate 118 112 120 [sonorosoeos ISO11-01-03-26-012-FMS ISO11-01-03-26-013 |wiospur-sampe IW-25b-pw-pp - FMS IW-25-pw-T- Sample | v6111 106 | we99.5 106 |w= | 113 99.1 ISO11-01-03-26-013-DUP IW-25-pw-T - Sample Duplicate [sonoromeonrus |waspuriws | ws | we | wer| ISO11-01-03-26-013-FMS IW-25-pw-T - FMS [Csonoroszmeon |wiastparsampe | wo | ees | we" | ISO11-01-03-26-014 IW-25f-pw-T - Sample Uisonorsamonrus |wiaspwrews ISO11-01-03-26-014-DUP ISO11-01-03-26-014-FMS IW-25f-pw-T - Sample Duplicate IW-25f-pw-T - FMS | 105 105 103 wo 98.0 113 | 100 108 98.5 we | 94.5 106 95.3 (2) 97.9 (2) 106 (2) we | 101 (2) 106 (2) m:E E -- EI E-- E ------ (1) Samples contained surrogate prior to additional surrogate being added during sample preparation and analyzed by external standard calibration, unless noted otherwise. EE r (2) Samples analyzed by internal standard calibration. (3) The SRS did not meet method acceptance criteria of 100 _+ 30%; however the average recovery of the SRS for the sample set was within method acceptance criteria. PAGE 25 OF 27 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00002255 3M MN04844757 aveTnEgTe aOR 3M ENVIRONMENTAL LABORA TORY REPORT NO. IS011-01-03-26 `TTaabbllee 2266 ccoonnttiinnuueedd.. SSuurrrrooggaattee RReeccoovveerryy (1) [= [~3C3]-PFBA [13C4]-PFOA [[1"3Cc4a]-ePrFoOsS 3M LIMS ID Description [CisISoOn11o-0r1c-0a3z-2e6-o01r5s |moIWs-2t5of-nsw--sSaammpplee % Recovery % Recovery % Recovery | et94e.9 | w9e9.6o| w10m2 - | ISO11-01-03-26-015-DUP [Csororcoosorsrus| wezsowpus ISO11-01-03-26-015-FMS [Csonorcosoe |wasoputap ISO11-01-03-26-016 IW-25f-sw - Sample Duplicate IW-25f-sw- FMS IW-25b-pw-T-dup 96.0 | we | oo| we | 93.8 (2) | ws | ms | wm | 113 98.3 101 113 100 (2) 93.8 (2) 111 ISO11-01-03-26-017 EB-pw-pp - Sample 85.8 89.5 87.7 [Csonorcazsorreus|eBpwpp-rus ISO11-01-03-26-017-DUP ISO11-01-03-26-017-FMS EB-pw-pp - Sample Duplicate EB-pw-pp - FMS 86.9 99.8 101 | w11m 3 | w1e0s5 | i1m09s | ISO11-01-03-26-018 IW-19-sw-dup- Sample 106 <2) 101 {2) 97.1 {2) ISO11-01-03-26-018-DUP IW-19-sw-dup- Sample Duplicate 102 94.2 (2) 104 (2) ISO11-01-03-26-018-FMS [sororcozsoer |Tuweimew ISO11-01-03-26-021 [Csororcoosterrus|Tmeipemews ISO11-01-03-26-021-FMS IW-19-sw-dup- FMS Travel Blank Travel Blank FMS 96.7 108 93.3 | w9e7.6"|e9r9.1 a{2) | e9s5.9e" | | w11s5 | m11o0 | m11o0 | ISO11-01-03-26-022 Equipment Blank 100 98.0 98.6 1 Sgcreatsrg rrr en a (1) Samples contained surrogate prior to additional surrogate being added during sample preparation and analyzed by external es standard calibration, unless noted otherwise. Ee, (2) Samples analyzed by internal standard calibration. OE repos ho 10+3 hve bo pry SHS srs (3) The SRS did not meet method acceptance criteria of 100 _+ 30%; however the average recovery of the SRS for the sample He ---- set was within method acceptance criteria. 55 CCoonncclluussiioonn J ------------ Laboratory control spikes were used to determine the analytical method accuracy and precision for all DT analytes. The accuracy and precision were then used to estimate the method uncertainty for the eur Fld ps at ie spheres (9 coat dun samp Heparin) results. Field matrix spike and lab matrix spike recoveries (SRS addition during sample preparation) Gomnsatedat hg Aas mah vas GDS oie Gn ST Ta APS wa demonstrated that the analytical method was appropriate for the given sample matrix. Analysis was Completing Emon Lasoo oben ETSS040 Monte o Wade 0 completed using 3M Environmental Laboratory method ETS-8-044.1 "Method of Analysis for the Somat porated Cotpounds Wa oyLOMSMS. ret ston Ach Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis". oto ar opores Ta an 10.30 op Analytical results are reported in Tables 1 and 10- 26 of this report. 66 DDaattaa//SSaammppllee RReetteennttiioonn AA i AAllll rreemmaaiinniinngg ssaammpplleess aanndd aassssoocciiaatteedd pprroojjeecctt ddaattaa ((hhaarrddccooppyy aanndd eelleeccttrroonniicc)) wwililll bbee aarrcchhiivveedd aaccccoorrddiinngg. to 3M Environmental Laboratory standard operating procedures. 77 AAttttaacchhmmeenntt Cranatcusody fom Chain of custody form PAGE 26 OF 27 CCHOEONNNNFFEIIDPDEIENNNTTGIIAOALU-LN- STSUUYBBDJJIEESCCTTTR ITTCO0T AAGOPPURRROOTTT,EECNCTOTI.IVV2EE7-OOGRRV-DD1EE0RR.08EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00002266 S_Nossaa7s8 3M MN04844758 88 SSiiggnnaattuurreess SMENVI`RROENPMOERTNITNAGLKLOA1BO0R1A0T0O2R6Y 3M ENVIRONMENTAL LABORATORY REPORT NO. IS011-01-03-26 `SSuussaann WWoloflf,, 33MM PPrriinncciippaall AAnnaalylyttiiccaall IInnvveessttiiggaattoorr Waka William KK_. RReeaaggeenn,, PPnh..0D..,, 33MM EEnnvvioronnmmenetnatall LLaabboorraattoorryy TTeecchhnniiccaall DDiireeccttoorr TThhee S3MM EEnnvviiroonnmmeennttaall LLaabboorraattoorryy''ss QQuualailittyy AAssssuurraannccee UUrniitt hhaass aauuddiitteedd tthhee ddaattaa aanndd rreeppoorrtt ffoorr tthhiiss pprroojjeecctt. QQuuaalltityy AAssssuurraannccee RReepprreesseenntatattiivvee Thistestroportshallnotbereproduced exceptinful, withoutwiitenapprooftvheaSlM. EnvironmentalLaboratory. This test report shall not be Environmental Laboratory. reproduced except in full, without written approval of the 3M PAGE 27 OF 27 CCHOEONNNFNFIEIDDPEEINNNTTCIIAAOLLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTTT,EECNCTOTI.IVV2EE7-OOCRRV-DD1EE0RR-28EE8NN6TT2EERREEDD IINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 22445555..00002277 I3MM_MMNNO044884444775509