Document 85w6D5J9qMNd0qpg9kJXZD65e

TTOOXXIICCIITTYY TTEESSTT FFIINNAALL RREEPPOORRTT EEVVEENNTT 22 EE0044--00112266 FFeebbrruuaarryy 2255,, 22000044 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 1939.0001 3M MN01539152 _Ft braamL--NabotSrat btoDrieLs, In0c. 107 Marc9h,2004 MMsi.nnSeussoatna BMeiancihng and Manufacturing EME9n3nvi5~niBnroueosn~somhne~~nAntrv~taae'Iliin~TTei~ee,gcehhaBnnnucoiddll~odMiig~nymyg~a2nu9d~5aS-~a0fi9entgy St Paul, MN $5106 Cex 3MsM. CToitntaagGealGlroowvaey B1u0i7l4d6inIgnn1o4v5ation Road Cotage Grove, Minnesota 35016 Me. Beach, N4~ .................................................................................. Thcohened3utcMabtleCedostabtseaolguoetwlGirsnouedvmemianfratichizelei3ty3t1hseGacmPhoOelmeidscaatreledcaeFniedvbertduoaxbriyycoEl,roag2i0coa0nl4Fraeenbsdurluttahsryfor2I6t,NhSe20tn0eu4s.mtsbecTrohne5d0u4sc.et3se1sd26ww,eirteh sBarmipelle,, eTaecnh 1s5amdpalyeolwdasshteswteedreatex1po0s0e%d cpoenrcerneptlriactaitoenanwidtthestt otemrpeeprlaictautree ewsats cmhaainmtbaeirnsedpear: h3a5dCbe+en1Cs.toreSdoliuntidoanrsknweesrsearte1n4ewCe.d aTetshte d4u8rahtoiuorn tweastsi9n6terhvoaless,ianngdhpeerorsgoiunralgusidaamnpclee,tthhre tess wereconduincdatrkneesds. eifmoieon ||SaDieens| Siwien|g|} a Dae || dTmooevl |A|r(TaSol|[aAenlms|| aTRtE E : ier1E 2 |2052006] love 222000] 102| 03 |; 0s | wo ] Foria tc~]uen~ ] '2 ans 2/25/20(?4 useI0:46 |22/a26e/m20n0e/| wea| !0:- 2 os0.5 | os,L6 | we <002 | RE I2/25/2004 i RE !0:56 I 2/26/2004 10:i2 a | row Taman] ries Tages = 05 | os | 00 E rnseome ni vas |2zewed| ontom|| 0s |Leoss|lewm CombinedEffuent_2252008| 1137 | 2062008| 10:12 | 05 | os | om Con~ined Eff]uem 2/25/2004 i 1 ::37 2/26/20{)4 dNNoootnneeecioooffnttlhhieemisstaanom'_pfpllee0ss.02ccmoonnLttaa.iinneeddAmttomottoaalnlirraee~sciddouunaacllenccihhalltooirriionnnees {(fTTorRRCtCh))e ccsooannmcpcelenmetsrraarttaiionognnsesdaafbbrooovvmee 0t.t5~hee mmmeeLtthhootddo ad00.c8gk~smmcc:Lgio/t.Lno.KthrTneTihh~feeioshmfmeOaea,naOssd2uurtrreehadedirLeaaf.mmomrmAeoomntnhimeiaaotccnaootiansnccceseonnwtntrceracatmtniiooortnanstspiowHwneesarrdeefubsnrntotoe~hde.aanmsatiAlncc>rippAiiNactseelddratttne~hgmepccdeaaruufassrteeoumraaecc0uuf.tto5eermaaaddgcvv.heLerrosstoeef the samples was 05C. effects to ff~e fis[~ a~qd ~hereJi~re the sur:~plcs ~,a~ 0.5~'C. the tests were no~ pI{ adjuqed. ArrRa] temperature {i~r each of `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTTT.EECNCTOT,IIVV2EE7:OOCRRV-DD1EE0RR-2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00000022 m_morsaorss 3M MN01539153 eWsE Resultsfo the tosieiy exposureeres shown in the table below. T ZAow| 4How [DORow | elon| pl aT TeaSneimfipclaeton PeMrteenotage| RerMceeatsay| e|perMceemm:ag| e|perMceerwag|e| RoP3Hge | RDanOgS|e RaConngdei :VoEwRY || 0 urvival|[Suwr]v{i}voaol | Survp[iwveal||Sorwvieval|i([CreUa0| e n90 essG|oo stesa)s I T[nnfl]luuecnmt 11/22 OGeel 0 an [on [ow ,, PPoorrt t1As | 995 Port 4A papPoiort 1stB ai| a 90 95 re 99~s ET pel CoCmombibinneedd TnFEE os Cason Ef?]uent 9~ | wan lw os 5 05} wm 0 7980 | 5270| H1w27a @ |J7a785p|o617n3| nim2 sai[5dswa[77n8s | erar [eons | m[amnaniex 5 |7ossleT rer]| nm. oITnfafeltuhmceontdteesr1t7a2tiesnldayimcphaaltreidnwgraestc.hoenosbftsiisethruvtaeendddwtaofteesctrau(mseeMtHchooRmdWpsl)ewtseeurpe(po1ar0ct0ce%edp)t1af0bi0slhe%mffooirrsahlassiustreyvsisvwiainltghfioLnroxt2ih4ceiyhd.ouurratsTihooefn Otteefsstt80iinn%ii,ttiiaaattniioodnn.t.h T~hseeamsspaalmmepplildeeeniitddieefnmiteiidf~ieaesdd PaasostPPoo4r~t3t 1]wAAaswwaoahsssfeortv~zeddd tttooo sssuuuppppppooorrrttt m mmeeeaa~nn 99956d hhhooauumrr fiiissshh ssuurrvviivvaall roefsp6e0c%t.ivelPyo.rt T1hBeanCdomPboirtne4d Esfafmipelnets ssaumpppolretesdupmpeoartned96mheaonu 9fi6shhosuurrvifviaslh osfur9vi0v%alanodf 9755%%., respectb-cI~. T|~e C{}mbined Effhmm sampe sup~<~ed meas 96 hour fis]~ survival of 75%. IInntteerrmmeeddiiaattee tteess~t filn~tteerrvvaallmmeeaannfifisshh SsumrwviivvaalI wvadl~u,aeess aarree sshhoowwnn iinn ~t-h~ec ttaabbllee aabboovvee.. Noa of the outine chemistry parameters (pH, dissolve oxygen, conductivity) measured daring the testwere abnormal for this ty ofp stue dy. Please call or mail me ifyou have any questions Sincerely, Era Laboratories, Inc. GiAo Joe Dierkes, Project Manager, Eco-Toxicology CR oe C 1Fr `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITOCOT AACOPPURRROOTTT.EECNCTOT,IIVV2EE7:OOCRRV-DD1EE0RR-2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00000033 SW_NO1E59154 3M MN01539154 5 Lavcroteries inc. EErraa LLaabboorraatotorriieess,, IInncc.. Client: _3M__( dv-bize) EraProject#: 17983 TTeesstt:: FFaatthheeaadd M Miinnnnooww AAccuuttee TTooxxiicciittyy TTeessttss TTeesstt iI~niittiiaattiioonn DDaartee:: 5 /2 / oly ] TTeesstt TTeerrmmiinnaat~ii~omn DDaattee:: 3/1 fo p Page 106 `CHGEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- TSSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTTT.EECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00000044 SW_MNo1S39155 3M MN01539155 Cots ENVIRONMENTAL SAMPLE TEST INFORMATION ENVIRONMENTAL SAMPLE TEST INFOR!~,IATION oCheer.i ~2a/iMz7G 00,~0 = I DFCilnielxiP~rot:onj5WeMactter:#5X1o79A8p3pTEable MFRW Control Dilution Ware.r: FToeosdt:Chtamebmers ['es~ Chamber: 00pNr.88ioorLLtiAfittoeeprr4pB%Bleiechsaaokkbueelrrer,reMneIwlRalW Control -- - | Food: A~em~a prior to 48 hour r~ewal Temperature: 25"C Tost Organise Age Fathead NmowI 1 Test Organism(s)/Age: Fathead Mmno v. ~ [Commens: Commeats: EE -- lest solntiom renewed -~ 8 ho~s ~mg stored/re~igerated samples fi~ra aa~ ple reeei[?u _ [/N3 ! | - -- PPaaggee 22. ooff66 CCHEOONNNNFEIDFPEIINNTDCIAOELU-NN- TSSTUYUIBBDJJIAEESCCLTTTRTITOCOT AAGPOPRUROROTTT.EECNCTOTIIVV2EE7 -OO0RR1-DD1EE0RR.0E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00000055 1 1 Swumorsssiss 3M MN01539156 eo tabootois TOOXXIICCIITTY TFEESSTT RP~ENNEEWWAALL FFOORRMM aun ROANS ahow TESTAmeToc Eb TEST: ~cute Toxic]p," E~,Iuatio_B AROECT: 13483 TESTNTUATONDAIE _2/26/0% mestMTONDATE_3/1 0% TST TE~MINATR}N DATE TEST DAk | {1 =] }A TE I | | moore | 3 | 242 11616 [1300 | 23s | | T~ME OF FBEDD,~G "o CONTRO. WATER || mas ]NIT]ALS ~RW MHRW MHRW Awl | || Ae Az fo N s~zZ PPaaggee33 ooff66 CHEONNNEFPIINDCOEU-NNTSTYUIBDJIAESCLTTRITCOTACPORUORTT.ECNTG.IV2E7-O0R1D1E0R.8E8N6T2ERED IN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00000066 su_wmoresors 3M MN01539157  p= T T = | | EE md 2Q CT, Ire | g EE + ----T be J LB [olslepele ||] |] a EEE fz az NN Nn | | Er 4 E18) 9 {3 =m "He EERE | | || | I ERIE LL : z, T F R3eiCN o:SiE lay;RC| 1|i Zgz lds = = ESn EE ISEelEe F ET |EH |! 2 T mJS sy 5 mie gTaof o=f| ol $|n|s) FEES | iCli Y | 1 2>2 Ede: Bobo Ll EZa9zZz b Fil faess. TT]NE]E F EENEF EELEGECCEETETEGEE Hl ie: [EL Sa LL || 2[: Eat vo gin | Sn BER ERE IN | | ESnEeR SSNS NING } | 14 oy " | | El pagnt s ~gofe 3 No T i [| fi PN ENN PS TN fl | 1 | | Fe 1 1] | BF ff4if2g fi LEap 3 F | 2 _odER[EBH aaoao zi]g . || F_|dt} CCHEOONNNNFEIDFPEIINNTDCIAOELU-NN- TSSTUYUIBBDJJIAEESCCLTTTRTITOCOT AAGPOPRUROROTTT.EECNCTOTIIVV2EE7-OO0RR1-DD1EE0RR.0E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 Swumorsssiss 3M MN01539158 11993399..00000077 i |JE BeREeEC[ E sE Y|aafEsnlEddSaEReEEEEEEEER||| g: PELEEA FEFBEE LLi] 33 sas ea TEE gs | EERE el AEE REE E | EE EIEEEER 1 WR acl EE SR I EN RY ES bl ae S<Sl =Rs=|.3 1! |Z Lo I| | NC[E 2 PSgRoF8SEt)EqEnEE gEale Ee] l |] s| ] . 2 EEE EEE 2a |. filiIenEe&E A 23353B 9B97= 4E | |~ E ERR IER B iRRI R E peR ppE y SN TETN | z Zn aS 2 22l 2 5) % =29s EPEgLie Eda S = 2S3 EslR2E2]2 |||| - = zE g E Jzz R [30 E 13|QIE= aBlle e2aa 1| MEER 0 ENEEEE I 1 Sif BmsNEIECE EEErEr EhEsEt INrEoReT 7 ls Saas IRE ESEegRnEee EEEwRE EENE7] R | |= =a w wl gw Wal w | I| pes 3 | disPAR h| igr 9aSaT P2E Ll1 1[1 i igIEJ?3EEa ausoe rl {ill ok CHEONNNEFPIINDCOEU-NNTSTYUIBDJIAESCLTTRTIOCTAGPORUORTT.ECNTOIV2E7-O0R1-D1E0R.0E88N6T2ERED IN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00000088 Swumorsssis 3M MN01539159 g Ee - :g o 202 r [ e i "qr | a of rh | eh | | | | |||] EDT || | EIN PRC || 1|EEE [| s| h ER 20e 29s] 83 s 3 NAFh | Elf 7 [1 eEYi ezf(zEel EL | |F |r | SFE:RERiEffid oR a,E|IS fri pi | EE|RLEL. TTT | I LTTTE<5 al | |' | | | T171H4l EH a ARN 41 dF HE iE Res] nin | JIih f. pSeadse tpi? FRgaNSS CONFOENTIAL SUBJECTT0 A PROTECTIVE ORDER EVTEREDIN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 || | |a | ih] |] | worse 3M MN01539160 11993399..00000099 Laboratory Report -instgrworty M`SISUNuSNAsENNSBBOEETAAACCMHHINING AND MANUFACTURING 9EM E3NRI5NVVtNIBRERUOSOSNNOH['JWT~AEAEVNENM,TTIANABLLIUNITTGLDEEIACCNNGHHDNN2OOM :LL3AO6ON.GGU0YY9FAAACNNTDDUSSRAAINF~GEET~YY S9T3.5 PBAUUSLH MNAV~ 55105 BUiLDiNG 2-3E-09 ST. PAUL MN 5~136 GPPrOrooGjieeccNttuNtmiubumemsrseerr TCTOeeOnmmeGppeRerNera:ac~tetmuuvrbreeeedr::((~'C|C)}: Report Dae Date Received Report Date: 017083 017983 Eo]3M os6_5 2262004 7,'26/2004 "aos S! 81204 Sites PIaNrNaFFmLLeUUtEEeNrN:TTPPHPA:ASSEE 112 1/2 SAPNeacatouraegtere.~neFF,taaeathrh:meemaaoddnMiiniannn:o~nw Resaual N~trosen. Res dua~ ior Ammonia 3hJodne DDaattee:;R01e22s/22t65/2s200:0044 Results: droynedone ane0.86 aerie TTiimmee:U: ni1"s00:446 Units: momgiL [re -- Matrix: Wastewater DateAnahzed: GC Comments: Date AnaJ~zed: QC Comments: 37772008 3/7/2004 202672004 2/26/2004 y7acos 3/7/2C04 Site: UNIT 1PORTALEAD Site: SNtT I PCRTA LEAD AANPcicariurceetge,re~neFF,taaatAthrhr:eemaaoddnMMiaiinnoonw Residual Nitrogen. Residua~ Chore AmmoNa Chlorine Date: 02252004 Date: 02/25/2004 Resu its Gone aose ass0.48 anea Time: 1055 Time: 10:56 U n its: mot. mg,'L Matis: Wastewster ~at~ix: Wastewater 3772008 3/7/2004 pr 2/26/2004 72004 3/W2004 QO Comments: Site: UNIT4 PORTALEAD Site: RPPaaUarerNaa.mmITeeFt4taeetrPrh.:OeaRdTwAiLnEnAoDw Acute. Fa:head Mi~mow NRietsriodguean,l CArhmoorneia NitrBlen Ammonia Residue ChJor:~e Date: 02252004 Resourites: Date: 02/25/2004 Resutts: 00do55n00e dor:e Time: 11:11 Unis: Uaits: mt mgiL tri: Wastewater Matrix: Wastewate~" DateAnshzes QCComments: Date Analyzed: QC Comments: 37772008 3/7/2004 2282000 2/26/2004 7001 3/7/2004 SSiittee::PaUUrNNaImITTe 1 PORT t; ePrO.RT BLEAD B LEAD AANPcicatiurreatoe,mgeenFFt,aaetAtrhh:meemaaoddnMMiiiannnnooww RNeitsriocgueanl, Chon Ammonia Residual Chiorine DDaattee::R0Ce22s/2u255l2;t200s00;44 Results: G0o5n2edone d0o.5ne2. do~e TTiimmeeU:: n11i11s.:0033 Units: mmog/rL [ep -- taa~rix: Wsst~swster DaeAnalzed QC Comments: Date Anal' zeal: QC Comments: 31772008 3/7/2004 2252008 2/76/2004 372004 3/7/20:34 SSiittee`::PUaUrNaNImITTe4t4ePPrOO:RRTT8BLLEEAADD `ANPAicacturirateoemg,,eeFnFt,eaarAth~hemeaamddoMMnisJpnnooww Residual Nitroflen, Residual Chicrne Ammon:a Chlor ne DDaattee::B00e22/s22u55t/22s000:044 ResuIts: 0o5n0edose done0.59 done TTiimmee:U:ni11t1s1::2255 U~its; mo mgiL Matrix: Wastenater ~atri: Waste# afar DateAnalyzed: QCComments; Date Ana|yzed: QC Comr~er~ts: 272008 3/7/2004 2s00s 2/26/2004 372004 3/7/2004 Sito: COMBINED EFFPHALSE/UDstEe: (N2262T004 SiteP: aBPriCaatrOmaeMem ,tBeFetaerNtr,Eh: eadEFMFiLnUoEwN r PHASE ii2Date: ReGsourlats: C12/25/2004 Results: Acute, Fatnead 'v1~now NReisriodgueanl, CArhmoorneia Nitrogen, Ammonia do~e 0ao7e 0.76 Residue ChIori~~e ao;~e Time: 11.37 Unis: Time: 1l 37 Units: mo. mg/L tatix; Wastewater ~atri: Wastewater DateAmized: QCComments: Date Analyzed: QC Comments: 3172000 3/7/2004 2262004 2/26/2004 72008 3/7/2094 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITOCOT AACPOPRUROROTTT.EECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00001100 SU_MNo1839161 3M MN01539161  Sonn RE mE 83 CHEE ed EY Lie fo} BE Q [Til oli < EZ = | iS TEN 2 | [Tome LEER TTT ol E| [EE 5 3 || ly A El lTa TaaaaAn yVeJs bi i Ep ffal [MTR I [ew 107 i I le mT 28 2 El HEH 3 2 I hie shall i =e al gEe lllzeed| 5 i [BEE Sfunopsdaa Spiny fifemal] A= LTeLI ! nn gn does||| Blk 28 lLi THTAE ||| 2g KER I 5 lize |] AR i} | 1 e)n || EdTNT| 5 | Bean NIN) & [FCIELTmaeeriy| rte ee = conibentL surscer oAprorcce oRFosFR EvTERED CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN A HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 morse 3M MN01539162 11993399..00001111 CCoonnvveennttiioonnaall PPoolllluuttaannttss FFIINNAALL RREEPPOORRTT EEVVEENNTT 22 EE0044--00112266 FFeebbrruuaarryy 2255,, 22000044 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 1939.0012 3M MN01539163 JOBE 9suEnpvipsorsmeenstel Laboratory Gran CunoMagus or Ls ahi er Im 2& p HIE he HLL llpress aE mee rime EE ye FE Comran PeEh e ed YA Le LTT RARER EE Eee EE = AH ET Ea a LH i E E e E ! 0 7 rh ste S FFEE -------- CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 p-- 3M_MN01539164 11993399..00001133 INTERREGIONAL WORK ORDER #| (Z-- TeomTmo ri ee] [sere] -- TT Ail questionsshouldbe addressed to sending projectmanager (Fawn] Lo wt pain Goning Oo bt] CE c= I | Fd1 -------- I[ SE 5% a3] I 1 me Sec gon -- | I | om | pie ove Svc To - CranotCooyotes ves Me Sapo Same amseroSumies___ oo novo Ove Ee Yes co Wate Cer rt) -- I rego ten -- ire concerns Bol and 3 Recei'd~mg ReO on comenuats Pa~ ~: Sen@ng Region mason `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00001144 i5 _MNO1S39165 3M MN01539165 Po coo rece SNPLE Lo SHEET lw RP - A. rT h ae-- i -- = (e(rroossieornswrEaRLeRS [Seavroiaeoveoreve Groves I Cotsarst Te[on otrot |i 1Afen EBER pareom | T pe LAB# Cooler ACID/ '3ASF LOT# Rowan | REMARKS: CONDITION O~: SAMPLE SHIPMENT, E~C TI oa n rm[or sf rr a Ere, intact/Broken cmonsms nan ase sor | CUSTODY SEALS NOS.: 105362768 = pre ............................................ I0536277E wp we em erm -- 105382784 [ C|| Eear ,E mes rsmr e [Ecl SC| T mil ei L7 R | ]=-- i Pr~perly F~lled Out EE | [anos swan | ON T 4 AIR,ILL ~rB~# | camps | 5 A AIRB~LL NO; 4S3891945140 AVE 1 [--mma N-- T 6 COOLER ind w= I E-- [ | pEotEas? Ty~ of PaokiRg? LA Se TT -- +sawme os 7 ~PLE TAGS imme ns a A~sent [Eu ---- 8, ~MPLE CON~31T~ON IN IN ------ + | 1 N -- t 1------ frees Separa'.e P|as~ic Bags? eEReIsE won Correct Conta~ne~ Used :sr Te~t~ ~nd~ca~? DEE wm Cermet ~e~e~'afive7 c ssomm Labels Complete [LD. Dale, Y~s~ NO I Y~ No [ Yes/No ff|fePrP emere ommoraT crsR e sT R al2sw-eeswn oe GEMS YORCOE 1 TN A -- 7! ~ ~ 1 1 I- I: TT i 1 Na -- --] Pte ec,OD A, FC,Cn, WR, RRA 17 CNONFEIDNENTICAOLUNSTUYBIJESCTTTHOACPORUORTTEC18T.3I7 VE ORDER ENesTERED CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00001155 sumersores 3M MN01539166 } / "_FaceAnalwyertminctaeln PaE idSepE r iy ~ax: 9~~.25!.2~g9 Maron 8, 2004 March 8. 2004 Roxanne Paterson Reanne Patterson o176g0 Ewin Snweet 1700 Elm Street SSuuiittee 220000 Minneapolis, UN 55414 Minneapolis, MN 55414 Project: interLabi 1085104 Project: |nter Labt 1085104 Soe sees SDG: 5;3988 Dear is. Patterson Dear Ms. Patterson: toned plan ino aA TR AAS Ny S00 Encloseu p~ease find our standard [abu ar repo~ for samples received by our llaabboorraattoorryy oonn MMaarrcchh 55,. 22000044., PPlleeaassee sseeee tthhee eenncclko)sseedd SSDDGG NNaarrrraattiivveess ffoorr aaddddiittiioonnaall Tr so information regarding analysis of these samples, 1, in yout review. you should have any questions or recuie adeional inert, ~f. in your review, you should have any questions or require additiona'~ information, pioase do not nesuate To aah otease do not hesitate to call. Sicerel, Sincerely, RaannccyysSatgagseosncelabs com Propet Manager rancy,staggs~acetabs Proiect Manager Enclosures I ---------- "We cer~if-i that the ~i~lIowing report mee~s all required NELAC reportm~ s~andards as peed inNIAC S13 hs 1 Te 2 dato ote .specified in NE~.AC 5.13_ _lal~ 1. 1999. ~:, dcviati:)n or vari~ce ~s notea m the case Come Stone gs nr~arsr~aatti:~ve,c((ss)~., EEssttiimmaatteedd ukn~cnecrct~aianimtijews r~e~g:gaarrddibn~g4 tthheessee annaallyyses aarree preegseeznltted iinn tlhhe QOuaaal~iit~yy Controj Section c~f this ~eport.' 1 FEANERI COUNTY DISTRICT COURT NG. 27Gunio26303 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00001166 3M MN01539167 FJaceAnaelaymtieocsaoeln [ SDG NNAARRRRAATTI%VVE ce i BepnrsTioosneov8mey a CLIENT: PACEMN CPRLOIEJNECTT: :PIANCTEEoRMLNAB PROJEC'i : iNTER-LAB DATE: March 8, 2004 EDPAITSEO: DMEaNrcOh :g~ 523090848 EPISODE NO~: 53988 INORGANIC FRACTION: INORGANIC FRACTION: dSSieec:v,i'eenrngl wwtahaetteearnasslaaymmspiplsleeossfwwtheeereseessnsuabbmmmpilittetsee.ddfTfoohr ddsiissassmoopllvlve'edds o~aronataall!yoosrreggsmawn~ieiccreccaacrrobbmoopnnleaantnaeal]dyyssaiicss.c~oNNrdo~inmsgao(j0orrthpperroofbbolllelemomwssinoogccccu~rreedd during ~}~e analysis of these samples. T~e sample's anatyaes were completed according to ~he iiol[owing: SsWwLLIsNoSIp0# SWI AN-310 Mset\hond Reference TPoatralamOorgtaonric Carbon Total Organic Carbon Please Please feefer ttoo CCoooolIeerr RRe~ceeei~pit~/t/SSaummp~l]e LLoogg-JInn SShhe#ee~t ~fobrr ddeetaalilss ooff ssaammppllee ccoonnddiittiioonnss aatt rreecceeiippt.t. TThheerree wweerree nnoo ~hoolldd ttiimmee vviioollaattiioonnss nnootteedd,. SSaammpplleess wweerree Fired filtered uus~iin%gaa tteetflloonn ilefiI{er pprriioor 1to0 sannaallyyssisis.. PLPrareebppaCaroraantitiooennlBBSlipaainnkkek:s::NNooALttaarrlggaeebttoraaxant~sodyr;t.y~eecssowwneerrrlee ddspeeitektcettseedweiirnetthhweeihpprireenppaQarrCaattiilooinnmibbtsal.~nkk aaNboovvee t~hee PPQQLL.. DMMLuaapatbltririCicxxaotnSSeptspri:iokkelesAS:s:lpliNNkLeooCs:SmmaAsatntrtrdiixxlmassbpptoiirkkraee~ssodwwuuepelcrrioeecnasstturuoebblmrmseiip~tsieekuddesswwwwieiirehheredhw~iviis&stheeNippninissOooQCddCee..llii:mti.~s. Duplicates: AI! LCS arid maaix duplicate res~ilts were within QC limits. No No father tL~dm~ dats data usability usability ~liimmiti~atdioo~nss eexxiiss~t ffco~rr tthiiss Iinnoorrggaanniicc AAnnaallyyssiss DaData PPaacckkaaggee.; Explanationsofthe E~@anatio~.s of the fIbor~mss raree t~hhee ffaolllloowwiinngg: FFFooourrmnm 3I| SSBlaaammnppkllsee-rrePesrauollvtssided by the LB Quality Control Dita Shests FomFo~m Form 73 7 Laboratory Control Sample - BIanks - Provided by ~e LB Laboratory ConFol Sample - Provided by the Qt~ality Control Provided by dac LCSILCSD Data Sheets LCS/LCSD Quay Quality CCotnmttrrooll DDaattaa SShheeee~tss. cicoucnertrrtiafcytthhfiaon. ttt'hahiiessrddata~haaaniisshe~eeccchhonnnlidccia~taiIlyonaascccdcue~rtaaat,ieel,,edccooambmoppvlelee.tte,,Reaalrnieddasii~neccooofmmtphpleliidsaanatccaeecwwcinit~thittnhhgeedtteiernrmmhssisaannhddarccdoocnnoddpiitytiioodnnasstsoofft~hhee pSpcooae~ccmkvharaaiaggcneete,hhfo~sr benother been authorized by the Laboratory Manage, or his'er designeea.s verified by the folowing tt~aIa t~e conditions detailed above Release ofthe data contained in this hardcopy data authoi;ized by tim Laboratou Manager, or his.&er designee, as verified by the foI1owing a = WWe~etstaCnChhSee.mmiTsiutsrtrnry)erSSuuppeerrvviissoorr RhEoPTnOhRs TneOanFloLfAotBfeORFrAitTooOnRYaASNAtLYSIS `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- TSSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTTT.EECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00001177 2 au_mnorsases 3M MN01539168 "Pace f Analytic_ al owpcat com Sample Results an reScien Tososn,osO,aE P,~one: a 9t&Z51o2858 RvEPTTOthniRs TerepopoO~o1nFrsisaaLl! AnesBttbeOsrrReFrsA~cioTdeuOcredaRd.Yc~xctAeseNtiviAne,~Lsul~Y.SrIcS nehc: `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTTT.EECNCTOT,IIVV2EE7:OOCRRV-DD1EE0RR-2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00001188 3 SW_NO1859169 3M MN01539169 I. "Pace Analyeteainschoaslom RFbaeeind: |sBwopeciace-ersos i TOTAL ORSAN!C 2AR~ON ru s PLe L cErS a a2 5s Phone. g~.25L2858 SSseeearmtoesna || aGa/ssjraor2si0u0en8s YY Pips pe Conpcuny + resuLTs scpoRTED as RECEIVED COMPOUND* - RESULTS REPORTED AS RECEIVED HS - NOff DETEC~E~ ABOVE QUANTIIATIOH LIXIT EC sotire necorery Sosiot oF ac ths SURROGATE RECOVERY OUTSIDE OF QC LIMITS ErReanntidTe rsa3, wane 1508 NiA - NOU APPLISASLE HETH2DOLOG~: SH = STANDARD KETffODSo ERA = ~EPA6CCi4-79-020, MARSH 1985 SW = SW 8~6 Revo 4 %996 I~7H OI'!:ON,19~;/19TH EDZTZCN, 199~ ArTHornian-- a oa n REPORT OF LABORATORY ANALYSIS This r~port shal notb~ CCHOEONNNFNFIEIDDPEEINNNTTCIIAAOLLUN-- TSSUYUBBDJJIEECSCTTTRTITCOOT AAGPOPRUROROTTT.EECNCTOTIIVV2EE7-OO0RR1D-D1EE0RR.0E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00001199 1 su_wmoresoro 3M MN01539170 Pace Analytical wwwpacsiabs.com rsnsy ~ 700 W~ saminnTiim PFhoonre:991188.,225511.22855089 ~x. 918.25t 2599 mSeelme:|sifoern-nniede-ee0 SHEhenTeese Sseeromnes +| cc3/i08a/2r00a RZPORTE3 SAHFLED : 03/08,200z~ : 02/20/'2006 SUZ~ "liT:) : EPOR'K NG Ye ...........~ ; _ ~ FOTAL ORGANIC CARBf)N _.0 mT/i ~ :.;..L_ :: 58'.0 DATE~ ~ i HE KKTH ,.93 VY %NALY ZED 03/4/04 EP....... ~ REFERENCE 20:38 }~,L SW9OF0 N8 = NOT NETECTED A~O\~: QUAN~ITAT~ON SURROGATE EECOVKR win Nor Heviichsis N/A NO? APPL! EABLE METHODOLOGY: SH ST/4h~bAR~ HETHOES, ES on = Ra EAR 1-79-030, WAH 138% EPA = ~HPAF0 ~4~29-020, HARCH I@85 oto gos pipAL REPORT OF LABORATORY ANALYSIS Whout the wrtienconst of Pace Analrical Services, Inc. `neh: CCHOEONNNFNIFEIDDPEEINNNTTICIAAOLLUN-- TSSUYUBBDJJIEECSCTTTRTITCOOT AACPOPRUROROTTT.EECNCTOT.IIVV2EE7-OOCRRVD-D1EE0RR.2E0E0NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00002200 5 aw_morsaon1 3M MN01539171 a. Pace Anwaelyatviecsalon L3wBAeeKteP.k1,:E |s| EBf503eer49-8ec80s.ii0236i-s67e61n1 ~3988 EY ewin PossAatisftosniuAifsa ne a saoa2898 SsSR3heAEaisHPeovPOirLRiicE?oenDE.sEa :||+: 0o59}23z33///"0200280380/////2a522000000000088444 SUBMiFT[ : 93/03/2004 TOTAL ORGANIC CARION To men sa 03/04/04 20:53 KaL 545050 SOKSOUND* = RESULTS RERORTEE AS ~ECEYED NOT DETECTED ABCVE }UANTITATION iZHZ7 [ S Hb]EET?HHOOLDO#OLELe e OOTGGATY6:;00/SSWH4e -7=9St-STe0EA2eAN0NsG~AARSM)}ARCMHHEET'EN1OO9DD8SSs,, 1374EDITION, 1992/1TH l~?H KDI~I<:N~992 'Ig~H EOITICS, Er~IT_Cl~ 1995 199S ReEPTOooRTroOtF LSoAtBobeOoRnAbTaoORsYeArSNAoLvYSIS "neh CCHOEONNNFNIFEIDDPEEINNNTTICIAAOLLUN-- TSSUYUBBDJJIEESCCTTTRTITOCOTAACPOPRUROROTTET.CENTCGIT.VIVE2E7O-OGRRuD-D1EE0RR.2E8E8NN6TT2EERREEDDIINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00002211 ;5 suumorsssi2 3M MN01539172 PaceAnaelyetitcaoln wn: sisee.oe 53988 Sei? | Bectizee ~tS4-P 126-67612 BLE~,3988 w rezone rezontes + 0310912008 REPORTED : 83 'P BSoEme|A 830372008 SUB~I~TEB : 03/03/200~ nr syi 700 We~ Albany bromii ~roken Arrow6 OK 74012 Phone: 9~ 8 2ff I 2858 Ei Fax: 9~ &251,2599 were vers VT comron: = ESULTS seroRces as secervey COHPOEND~ = RE]U~TS REPORTED s.S RECETVSD ND = HOT OiT~CTS ABOV 0UAHTIT~,TKON %TH!T = HU~H{}(-;T~' RSCCVERY OUTSIDE O~ @C L!HITS Va RLicaeie NiL - NOT APPLICABLE ETHOIGIOGt: Si = STAND KETICIS, 167K OITION, 1992/197K EOCTION, 1535 HETH3,COEOSY: SH = ST~NDARD HE~HSDS~ !8~H E~ETiON, 1992il~TH RDYTON, 3995 Ba ae Ren.n 1 Sane SW ~ SH ~46 Rev ~ R996 RETPOhRoT OtFtLt ABORc ATORYxAN1ALYSIS hou hewriten corse cfPace ANayIcal Services, Inc. `nelac: HCEONNFNIEDPEINNTICAOLUNTSYUBDJIESCTTRITC0TACPORUORTT,ECNTG.IV2E7-OCvR-D1E0R26E3N6T2ERED IN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00002222 7 swmorszoirs 3M MN01539173 .Pace Analytic]alo exciteson re So t1mtese i517n2td%5H08] Phone: 9f~,25 <2858 wero ~AB IS SSEule MATRIX SERITE |s; am53ep9c8.8isos0s~eersn oesaee : w : IOSSIC6 sane ~ARAMETER Cora cre cen TOTAL ORGANIC CARBON s[earcrurniWems LaLEHI? mar UNITS 1.3 mG'] SSRSsAEhePMriOPTRLeaZTn.S~me |T+:: GaC00aTa23/aj//o0r2osz~0ur////2zi2a00D00o0n00n44k8 SUBHITTED : 03/03/2004 sans RESULTS ss%8.~ canes aio DATE~TIHE HETO2 win mcrs serene ANALYZED ANALYST REEEREHCE ava aie wa swe 93/04/04 2]:18 [~L SW9C69 COHPOUNE~ = RESULTS REFORTEE AS RECEIVE9 NOT DETECTED ABOVE OUANTITAT!ON LIH!7 SURROGATE ~ECCVERY OUTSIDZ OK OC h~ ~ TER aEERROO/4-79-020, NARCH 1355 NCT ~PPLICASLE ~ETHO~LOSY: SH : .<..T.~..D..~R~ HEUHOD~.~ #E_~0~, -,9-~0, }~ARCH 1995 ]8TH EDITION~ 1992'!9TH EDITION, 1995 SW ~46 Rev~ ~ 1996 ReEPTOehRTmnOtFdLrAmBtaOsRa oATnOsRSYpoAe, NtALYSIS CCHOEONNNFNIFEIDDPEEINNNTTICIAAOLLUN-- TSSUYUBBDJJIEECSCTTTRTITCOOT AACPOPRUROROTTT.EECNCTOT.IIVV2EE7 -OOCRRVD-D1EE0RR.2E0E0NN6TT2EERREEDD IN N HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00002233 2 awmorsao7n4 3M MN01539174 ~_Pace Analyeteicealon e MsieS is]s Phone: 918.25!.2858 i Fax: 9t 8.251.~99 FGuieaizto: | Bsaamteitneeees waRh hese seroma: 03/0/2008 RBSORT'EP : 03/08/2C0a Sams | 0 SAHPLED 92/23/2004 Shwirren| Sov/3008 .... : /03/2@04 se PAFS@dETER Torn orate en TOTAL ORGANIC ~ARBON : EPOP, T I NG TT Wr LI[,:[!T N'~-~~_,_~~, Lo awa 1.O m~/i ven _RESULTS Bs5@,2 !}87E '~TIME [4 [TNOD an wast sis ANALYS? REFERENCE oars hi Kal swaeen 03/04/04 21:34 K~i 8X9060 CN$c1DOo0Hw1CPp2O-oUmNSNWoLiCr:*SRad==DDtEEasTRTrzEEEesCSCUuTTLEuEs?DnDeSsAAc~BRsoOOEeVVPrnEECcRaGGQTreUEeUnADsAsMNis&Tos5iTtTARsAToEs~IfCcOOEaNNIraVcvELeLDLDiiHiIvaIrs ETioo3i00te Sh STAIRD Wetions SURROGATZ {ECOVERY OUTSZ~E OF N/A NCT AF~LICABLE OC L~HITS 143 EOTEON,1552/1678 Barr, 1656 HETHODDLOGY: SH - STAN~R~ METHODS. I~TH EDITZOH. 1992i19TH E~ITION, 1995 EP~ #EPA60~,d-/9-620~ MARCH lD~b 8H = SW ~46 Revo 4 ]996 Ts at oe siscpt REPORT OF LABORATORY ANALYSIS who the writen consofePnacte Analytical Services, inc `nebe- CHCEOONNNFNFIEIDDPEEINNNTTCIIAAOLLUN-- TSSUYUBBDJJIEESCCTTTRTITC0OT AACPOPRUROROTTTE.ECNCTOTI.IVV2EE7.OO0RRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00002244 3 > awmorson7s 3M MN01539175 / iis `ace Analytical te GSueustroy: hs| utosevecise-ercaz Se a ~A[t~ET E R T~COTT~A.LL OORRGGAANNIZCC C<;AARKbBOO~N4 RESULTS~ I1~.00 v[] sSSoeraiosswt.ees r0300/333700330r/7s32000000a46 PetGttr os, mar na k1oe 2BE X5425s2 UNITS nmg~//Ll wr oa DATE DATE PREPARED ANALYZED -- REFEREKCE HET~[OD 0033//0044//0044 2211::4422 S8WW9I(C]E6D0 - COMPDUND* = RESULTS REPO~TSD AS RECEIVED REPOTRhTaOtFlLAtBoottORspyAokTtORYpAeNAoLrY,S1IS `nelac: `CHCEOONNNFNFIEIDDPEEINNNTTICIAAOLLU-N- TSSUYUBBDJJIEESCCTTTRITTCOOTAACOPPURRROOTTT.EECNCTGTI.IVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDDIINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00002255 aunotsssiTs 3M MN01539176 PaceAnalytiacn al - wow paces com QQCC RReessuullttss Pceartnr08oS, m4hs0,a7n5y roFeo 391188.325517.22589560 RuEPtTOR1oTwoOiFtsacLriAeBrOoRofAptToO,RnYxcASNaA0nL,eYSII. S nebe `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- TSSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTTT,EECNCTOT.IIVV27EE-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00002266 it. _MNOtS391TT 3M MN01539177 /"_Pace Analytic'alo /- vce PcsSosrTaseSt:OoEy ome raestaxe i QAtaQeoc n eEmetmanecen s : .-~23~:4(74b! HAERIX : % ,~:,.~,IET~. TOTAL CESANIC CARBON a sions :IEPOR NN.S LIHIT UN!~S 1.0 mgil AHsSNeiAoziLoYtniZmteEesDn | " 01a03a3///300484///222000000488 20:50 ]77,11770@ .~ o sureDATE / TIKE vezwcp ME?HOD ..... LYZED ANALYST RZPERENCE ND 03/04 ~8'4 14 ;34 KAL S;990~ SEER CeTECTED Amore QUavEITHiion LouiT COMPOUND* : RESULTS REPORTED AS RECE[VEE N~ = NOT DETECTED ABOVE QUANTITATiON LIMIT S[]~R()GA~E ~HCOVERY OUTSIDE OF ot LiMitS N/A - ~ST APPLICABLE HETHO0OL35E: Si STAUDARD WETACDS, 15TH ZOLTION, 1392/19T8 SDITION 1995 HETHODOLOGY: SH : STANDARD HETHOES, 19SH EDITiON, 19g2/19TH EDITION, 1995 Ton Senarto 0oa), aac 196s EPA = }E~A600i4-79-020, MARCH 1985 Soe ree. 1 5995 SW - SW 846 Rev~ 4 i996 REPTOhRt T OFaLrABtOgRAtTORY ANALYSIS Th~s re,or1 shall ,sot be reproduced ANALYSIS ro a a de ii:hgut t~e ~en cc~sent o~ Pace A~al~ical Services `nelac: CHCEOONNNFNFIEIDDPEEINNNTTCIIAAOLLUN-- TSSUYUBBDJJIEESCCTTTRTITC0OT AACPOPRUROROTTTE.ECNCTOTI.IVV2EE7.OO0RRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00002277 12 awmorson7e 3M MN01539178 Py ace AnalytiCcael excite on asoiri oan BsErriSrs Phone: 918251.2858 a ~ax: 918,25t.2599 -- SShceiooci:nt Lb~C~O3C60~ mes LABORATORY CON?ROL s SP:HE/SRIKSesonaED }UPE!CACE 0R3E/C0O8/TE2R0Y98 bSraosmoioonst ARTNooAiLrrYooZeEirDoor 1t0i:e5s0 wn WwNm sSmNe semre oSweN oheee me wWsD Leocuse RiEPaOTmRhTorOFrtrLAinhBeOTRATocOeR"YtAgSNAvLYSIS "nebe CHCEOONNNFNFIEIDDPEEINNNTTCIIAAOLLU N-- TSSUYUBBDJJIEESCCTTTRTITC0OT AACPOPRUROROTTTE.ECNCTOTI.IVV2EE7.OO0RRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00002288 125 awmorson7e 3M MN01539179 '_PacecAenAanlayticaalt~' wo acatts sem { Chain ooff CCuussttooddyy I/ CCoooolleerr RReecceeiipptt cic em, eneBE Phone: ~18.25 t.2~58 Tok $8 51 2588 @x: ~ ~,251.2599 RETPOnRs T OFsolLr rAtBORAeTgOoRYcAtNALYSIS io er ren ofFires `nehc- `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTTT.EECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00002299 i m_Morsaote0 3M MN01539180 (TE TE | HibsFEE ClwdFECTiLBE | E feEeEs ara |CIE | Iin|| HeI e IE RToph TL HB rae) le ee He : fBigleeeE sl HaylE2 E BBae eE l1k2 see) Cf ii i 581 Re || RITES S10 PEEI:TH glue Sl | ONE EE | iWdiN te C = H bef E [Tg < Ni AES a L|T Te N R TERRdE SPLE! Eer lBmied =Sis Ji E2\el PRE zl 8H 5 = 15 FERNEPINCOUNTY DISTRICTCOURT NO 27 Sv 20862 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00003300 smote 3M MN01539181 A INTER-REG(I1O0NbeAcLonWpOivRobKys sOoRnDdEaRge# | UZ [Sommpogent [[ mev ereegeno |T s T Jswomgpmenra] Ei ae [Semargr] ary A questionsshouldbediessed 0 ndingProjectmana vi | seat remiy ___cenasos --_overtiwir TT ---- E -- e --_-- Cm ---- Teg ur TT TT TTT i HSA CHE ef one come comme TOTAL Tor T~t~l ities FaeneiCusoryhkens Des Mo mm. Reino rpc aaa - Zo a. 2.205Faces gen spent sense i Pasta a-- swore Boo [p-- Ge ie -- -- `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTYUBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00003311 oe 3M MN01539182 HL, ad el RecsxssivowaerURDEy 2 'RECENVED BY (PRINTNAME) JASONSPRIGGS. RECEh/ED BY (SIGNATURE): LLOOGGGGEEDD NPY(SIGNATL [more2 | aeee[mee PROJEG~I INTERoLA.B [ER EPISODE: 53988 CTT TT TTT wee aaa ee ww Toco 20000303 1281 --E-- cores [IS00 TE Lie Bd BEaR 22 RReemmaarrkkss BN _-- Se mg fe ~ CUSTODY S~L(S); gress.Pre | dd] Loe fmm -- | 2CUSTODYSEALS N 2 CUSTODY SEALS NtA a [EEE [a CT am A! ew ww id ] [ E m| a mC mm cre sr wapye EN o [|| pe Tm p fvwae -- f--|| | aE man e aos [NC T I1 i -- =nCoN ] Ciba: A[RB~LL 483891945140 Nl 7 1 c20me -----] ----_ TT] l er, Enough ice? eis pe INT t ype o~ t@? toeWet Yes/No IN I Ce ||ssaawvmeecaocnsomon. aan 1 1 ! 1 I || espmp . -- ---- | Cvara toom n yeina] I. 1 SN]| 11 farrcu Som? -- [IN [ [waoRampm m--ee--sl I T X TN -- ~D SCREEN W~TH foes TT COUNTER? | Jean I 1 |110.Coan A -- wm wome-- n eee =Note ampleswihDitties derroma section. I T r Ry. 17 EE CBA hey SER vo 5oer CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00003322 3M MN01539183 aceAAnnaallyyttiiccaall ee ton Pace Analytical Services, Inc. 1700 Elm Slreet, Sm'te 200 FreIne: 612T607170 Minneapolis, MN 55414 Phone: 612.607,1700 Fax: 612.507.6444 March 11, 2004 Mr. Brian Mader 3M Environmental Laboratory 935 Bush Avenue Bldg. 2-3E-09 [EBIE St. Paul, ~ 55144 Lab Project N~mbar: Client Project ID: ccm sem 1085104 E04-0126 Cg Carbon System Test ont eO siois a st t The rg S or 5.e Dear Mr. Mader: Enclossd are the analytical results for sample(s) received by the laboratory on February 25, 2004. Results reported herein conform to the most current NELAC standards, where applicable, unless otherwise narrated in the body st the report. If you have any questions concerning this report please feel free to contact me. Sincerely, RpanniPettiam Roxanne Patterson pRPoerxooajgneenccett. YMPaaasntaatggeeerrrson@pacelahs.} c~m Minnesota Certification @: 027 053 137 Wisconsin Certification ~: 9999407970 Enclosures ionhelAtaec,: momen RREEPPOORRTT OOFF LLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'Thi~ r'eps~ shall n~t I~ r~pro~uce~, ~ept i. f~ll, without th~ written consent ~f Pac~ ,~naly'dcal Servi~e~, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00003333 pr 3M MN01539184 iceAAnnaallyyttiiccaall ee ton Pace Analldical Services, Inc. 1700 Elm Slreet, Sm'te 200 Minneapolis, MIV 55414 fri Id T Phone: 612.60Z 1700 Fax: 612.607.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test NT) es i SOO cs Lab Sample No: 105362743 SY vn il RE Client Sample ID: E04-0126-67609 Influent Phase 1/2 Project Sample Number: 1085104-001 Matrix: Water Date Collected: 02/25/04 10:46 Date Received: 02/25/04 18:00 Oe, Parameters Microbiology Results _ Uni_ ts Report Limit Analyzed By CAS No. mm 4 epi Lattin Biochemical Oxygen Demand, 5 d Prep/Method: / SM 5210B i EEE cpdis s ostinSamto . BOD, 5 day 14 mg/l 6 03/02/04 JPHI Qual RegLmt 1 Date Prepared -- Wet Chemistry SL, re Phenolies Total. in Water enPhenol SI GC/MS Semivolatiles OL 625 wastewater GC/MS SVOA eyPhenol Pre bis(2-Chloroethyl) ether So 2-Chlorophenol rm 1,3-Diehlorohenzene mee 1,4-Diehlorobenzene Filo 1,2-Dichlorobenzene mr bls(2-Chloroisopropyl) ether fide N-Nitroso-di-n-propylamine Le Nitrobenzene ps Isophorone fe2-Nitrophenol 3 ite 2,4-Dimethylphenol 02/26/04 10:30 02/26/04 10:30 wigs mingmit, Method: EPA 420.4 ND ug/l re mens wi 25.0 03/05/04 08:41 VAF 108-95-2 ima tin Prep/Method: EPA 625 / EPA 625 Dimitar| tie ws ND ug/l ii. 3 ob Lm ~D ug/l ii. PZ amma ND ug/l ~. 2 2 Imm ND ug/l ii. Doom on pemaim ens ND ug/l ii. PE ZL Hanae ND ug/l ii. BL RL ae ~D ug/l ii. 2 2 OF Uhen ~D ug/l ii. Doom on ema a ND ug/l 11. EEL Eo ND ug/l ii. FEEREE ND ug/l n. 22 23b tgumsaeaniiuene ND ug/l ii. 03/03/04 19:12 KSK 03/03/04 19:12 KSK o~/o~/o4 19:12 KSK 03/03/04 19:12 KSK 03/03/04 19:12 KSK o3/o3/o4 19:12 KSK 03/03/04 19:12 KSK 03/03/04 19:12 KSK 03/03/04 19:12 KSK 03/03/04 19:12 KSK 03/03/04 19:12 KSK 03/03/04 19:12 KSK 108-95-2 111-44-4 95-57-S 541-73-1 106-46-7 95-50-1 39638-32-9 621-64-7 98-95-3 78-59-1 88-75-5 105-67-9 bis(2-Chloroethoxy)methane 2,4-Dichlorophenol jar. 1,2,4-Trichlorobenzene EANaphthalene Hexachloro-l,3-butadiene Dhogmde 4-Chloro-3-methylphenol me 2,4,6-Trichlorophenol a 2-Chloronaphthalene LoDimethylphthalate nim Acenaphthylene 2,6-Dinitrotoluene boAcenaphthene Et 2,4-Dinitrophenol Ty 4-Nitrophenol EL, 2,4-Dinitrotoluene an Diethylphthalate ND ug/l ND ug/l I 3b mana ND ug/l EZ iE NB ug/l NB ug/l 3 3b mime ND ug/l Doom on amu ~D ug/l 2 Zp baba ND ug/l Doom semammoe ~D ug/l EE ~D ug/l ~D ug/l 2 2 Rie ND ug/l FEE ~D ug/l EIND ug/l 2 ZL Smee ~D ug/l 2 ZL dene ~D ug/l ii. 03/03/04 19:12 KSK 111-91-1 ii. 03/03/04 19:12 KSK 120-83-2 11. 03/03/04 19:12 KSK 120-82-1 ii. 03/03/04 19:12 KSK 91-20-3 ii. 03/03/04 19:12 KSK 87-68-3 11. 03/03/04 19:12 KSK 59-50-7 11. 03/03/04 19:12 KSK 88-06-2 ii. 03/03/04 19:12 KSK 91-58-7 iio 03/03/04 19:12 KSK 131-11-3 ii. 03/03/04 19:12 KSK 208-96-8 ii. 03/03/04 19:12 KSK 606-20-2 ii. 03/03/04 19:12 KSK 83-32-9 55. 03/03/04 19:12 KSK 51-28-5 55. 03/03/04 19:12 KSK 100-02-7 ii. 03/03/04 19:12 KSK 121-14-2 ii. 03/03/04 19~12 KSK 84-66-2 Date: 03/11/04 Page: i of 33 ionhelHaec: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00003344 [pr 3M MN01539185 iceAAnnaallyyttiiccaall eto Pace Analytical Services, Inc. en 1700 Elm Slreet, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.607,1700 Fax: 612.507.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test NT) es i SOO cs Lab Sample No: 105362743 SY vn il RE Client Sample ID: E04-0126-67609 Influent Phase 1/2 Project Sample Number: 1085104-001 Matrix: Water Date Collected: 02/25/04 10:46 Date Received: 02/25/04 18:00 Hto ear eerie con E818 ieie EE Parameters rg i 4 Chlorophenyiphenyl ether oe 5 LD a= Fluorene CEE gs & Th mmm nD 4,6-Dinitro-2-methylphenol ims 3 2 EF Honea 4-Bromophenylphenyl ether Lar Doom on semana Hexachlorobenzene bd ? 2 tmasy Pentachlorophenol [oe 2 ZL sami Phenanthrene fea, = 0 ommmmgin Anthracene Di-n-butylphthalate fr 2 Zo imam Fluoranthene bo Doom on amma Pyrene En --_-- EE Butylbenzylphthalate Gpmewess EA naan nen 3,3'-Dichlorobenzidine Da P 2 mmnih Benzo(a)anthraeene i 2 2 LD ImmErs Chrysene is BTA Di meas bls(2-Ethylhexyl)phthalate se PZ Hanae Di-n-octylphthalate [a Doom on aman na Benzo(h)fluoranthene re 2: ZL Hamma Benzo(k)fluoranthene es Doom on ema we Benzo(a)pyrene Solow Lf ob mae Indeno(l,2,3-cd)pyrene bi EN ET i Dibenz(a,h)anthracene a 2 2 meas Benzo(g,h,i)perylene feres IEo LaEnEai Hexachloroethane Results ND ND ~D ~D ~D ND ND ~D ffD ffD ffD ND ffD ffD ND ~D ~D ~D ~D ~D ~D ~D ND ~D Units ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l Report Limit Analyzed By ii. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK 55. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK 25. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK 22. 03/03/04 19:12 KSK ii. 03/03/04 19:~2 KSE ii. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK ii. 03/03/04 19:12 KSK CAS No. 7005 72 3 86 73 7 534-52-1 101-55-3 118-74-1 87-86-5 85-01-8 120-12-7 84-74-2 206-44-0 129-00-0 85-68-7 91-94-1 56-55-3 218-01-9 117-81-7 117-84-0 205-99-2 207-08-9 50-32-8 193-39-5 53-70-3 191-24-2 67-72-1 Qual RegLmt Nitrobenzene-d5 (S) 85 % 03/03/04 19:12 KSK 4165-60-0 2-Fluorobiphenyl (S) 91 % 03/03/04 19:12 KSK 321-60-8 ~erphenyl-dl4 (S) Phenol-d6 (S) amet 2-Fluorophenol (S) 2,4,6-Tribromophenol (S) a Date Extracted A GC/MS Volatiles EI Volatile GC/MS by 624 rs Chloromethane ShVinyl chloride on es Bromomethane Sre e Chloroethane 92 % 1 % FI0 % 7 % Cots 03/01/04 03/03/04 19:12 KSK 1718-51-0 03/03/04 19:12 KSK 13127-88-3 2 Gem pm 03/03/04 19:12 KSK 367-12-4 2 03/03/04 19:12 KSK 2 we 03/01/04 wap Method: EPA ae WE I0. TE 3 umnmnrm ND Sn ats 7.8 22 23B4 Hamdmaanna ~D 624 ug/l ug/l ug/l ug/l 1.0 02/27/04 03:08 RJS 74-87-3 1.0 02/27/04 03:08 RJS 75-01-4 1.0 02/27/04 03:08 RJS 74-83-9 1.0 02/27/04 03:08 RJS 75-00-3 Trichlorofluoromethane ~D ug/l 1.0 02/27/04 03~08 RJS 75-69-4 Date: 03/11/~4 Page: 2 of 33 iS nelE ac: momen RREEPPOORRTT OOFF LLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'Thi~ r'ep(:,~ shall n~t I~ r~pro~u~. ~ept i. f~ll, without th~ written consent ~f Pac~ ,~naly'dcal Servi~e~, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00003355 aw rsores 3M MN01539186 iceAAnnaallyyttiiccaall eto Pace Analytical Services, Inc. en 1700 Elm Slreet, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.607,1700 Fax: 612.507.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test NT) es i SOO cs Lab Sample No: 105362743 SY vn il RE Client Sample ID: E04-0126-67609 Influent Phase 1/2 Project Sample Number: 1085104-001 Matrix: Water Date Collected: 02/25/04 10:46 Date Received: 02/25/04 18:00 Sai con S081 g erile fm EE Parameters Co , EE a Methylene chloride re P55 are I,i Dichloroethene Dame E Zu mmmmoen n trans-l,2-Dichloroethene Sn 2 OZ Laan l,l-Dichloroethane Le Doom ammnam on Chloroform ri : 2 I anew l,l,l-Trichloroethane Fn 2 Zi fsiabie Carbon tetrachloride = 2 a a1 Benzene 1,2-Diehloroethane fn FZ i amma Trichloroethene Fer Doom amma ne 1,2-Dichloropropane s meete EDI mNN NEmC mmnaaw a on Bromodichloromethane Results ND ND ND ND ND ND ~D 2.0 II. ND ~D ~D Units ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l Report Limit Analyzed By 1.0 02/27/04 03:08 RJS 1.0 02/27/04 03:08 RJS 1.0 02/27/04 03~08 RJS 1.0 02/27/04 03:08 RJS 1.0 02/27/04 03:08 RJS 1.0 02/27/04 03:08 RJS 1.0 02/27/04 03:08 RJS 1.0 02/27/04 03:08 RJS 1.0 02/27/04 03:08 RJS 1.0 02/27/04 03:08 RJS 1.0 02/27/04 03:08 RJS 1.0 02/27/04 03:08 RJS CAS No. 75 09 2 75 35 4 156-60-5 75-34-3 67-66-3 71-55-6 56-23-5 71-43-2 107-06-2 79-01-6 78-87-5 75-27-4 Qual RegLmt trans-l,3-Dichloropropene ~D ug/l 1.0 02/27/04 03:08 RJS 10061-02-6 Toluene cls-l,3-Diehloropropene Sra 1,1,2-Trlchloroethane Tetraehloroethene fe Dibromochloromethane in Chlorohenzene a EthylSenzene SaXylene (Total) neBromoform m Lpes l,l,2,2-Tetrachloroethane 4.2 ug/l 1.0 ND ug/l 1.0 oom ND ug/l 1.0 ND ug/l 1.0 Doom ND ug/l 1.0 2 Zi ~D ug/l 1.0 oom ND ug/l 1.0 PE ND ug/l 3.0 Doom ~D ug/l 1.0 3I B 2 OBH ~D ug/l 1.0 02/27/04 0~:08 RJS 02/27/04 03:08 RJS amma wen 02/27/04 03:08 RJS 02/27/04 03:08 RJS mamma 02/27/04 03:08 RJS aman 02/27/04 03:08 RJS mame 02/27/04 03:08 RJS ne 02/27/04 03:08 RJS maa ne 02/27/04 03:08 RJS mgmaaan 02/27/04 03:08 RJS i08-8g-3 10061-01-5 79-00-5 127-18-4 124-48-I 108-90-7 100-41-4 1330-20-7 75-25-2 79-34-5 1,3-Dichlorobenzene 1,4-Dichlorobenzene ho1,2-Dichlorobenzene are 2-chloroethylvinyl ether Soar Dibromofluoromethane (S) Toluene-d8 (S) We en 4-Bromofluorobenzene (S) mE 1,2-Dichloroethane-d4 (S! ~D ug/l 1.0 ~D ug/l 1.0 2 Zi ~D ug/l 1.0 2 2B ND ug/l 5.0 2 3 129 % AE 104 % 105 % 120 % 02/27/04 03:08 RJS 02/27/04 03:08 RJS imananm gn 02/27/04 03:08 RJS EanmEi 02/27/04 03:08 RJS Srna 02/27/04 03:08 RJS 02/27/04 03:08 RJS ae 02/27/04 03:08 RJS TARTAR va, 02/27/04 03:08 RJS 541-73-I 106-46-7 95-50-1 110-75-8 1868-53-7 2037-26-5 460-00-4 17060-07-0 Date: 03/11/~4 ionhelHaec: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'Thi~ r'epn~ shall n~t I~ r~pro~u~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00003366 Page: 3 of 33 aw mrsarer 3M MN01539187 iceAAnnaallyyttiiccaall ee ton Pace Analldical Services, Inc. 1700 Elm Slreet, Sm'te 200 Minneapolis, MIV 55414 fri Id T Phone: 612.60Z 1700 Fax: 612.607.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test oe es i SO i cs Lab Sample No: 105362750 0 cvs on il RE Client Sample ID: E04-0126-67610 Sample Port Lead IA Project Sample Number: 1085104-002 Matrix: Water Date Collected: 02/25/04 10:56 Date Received: 02/25/04 18:00 iamnowSeiifm iE Parameters Microbiology Results _ Uni_ ts Report Limit Analyzed By CAS No. Tm ome 14 ergs Ltn Biochemical Oxygen Demand, 5 d Prep/Method: / SM 5210B EEveiEn a rss Sm en . BOD, 5 day 6 mg/l 6 03/02/04 JPHI Qual RegLmt 1 Date Prepared -- Wet Chemistry SL, re Phenolies Total. in Water enPhenol SI GC/MS Semivolatiles OL 625 wastewater GC/MS SVOA eyPhenol Pre bis(2-Chloroethyl) ether So 2-Chlorophenol rm 1,3-Diehlorohenzene mee 1,4-Diehlorobenzene Filo 1,2-Dichlorobenzene mr bls(2-Chloroisopropyl) ether fide N-Nitroso-di-n-propylamine Le Nitrobenzene ps Isophorone fe2-Nitrophenol i 3 le 2,4-Dimethylphenol 02/26/04 10:30 02/26/04 10:30 wigs mingmit, Method: EPA 420.4 ND ug/l re mens wi 25.0 03/05/04 08:41 VAF 108-95-2 ima tin Prep/Method: EPA 625 / EPA 625 Din at Ae ws ND ug/l ii. 3 ob Liem ~D ug/l ii. P 2 mmngl ND ug/l ~. 2 2 0 mmm ND ug/l ii. Doom on aemuem ens ND ug/l ii. PE ZL Diane ND ug/l ii. BL RL Se ~D ug/l ii. 2 2 OF Unnan ~D ug/l ii. Doom on aamnenm a ND ug/l 11. CIND ug/l ii. ER Ei ND ug/l n. 22 23b Lgumsuaamiiuens ND ug/l ii. 03/03/04 20:05 KSK 03/03/04 20:05 KSK o~/o~/o4 20:05 KSK 03/03/04 KSK 03/03/04 20:05 KSK o3/o3/o4 20:05 KSK 03/03/04 20:05 KSK 03/03/04 20:05 KSK 03/03/04 20:05 KSK 03/03/04 20:05 KSK 03/03/04 20:05 KSK 03/03/04 20:05 KSK 108-95-2 111-44-4 95-57-S 541-73-I 106-46-7 95-50-1 39638-32-9 621-64-7 98-95-3 78-59-1 88-75-5 105-67-9 bis(2-Chloroethoxy)methane 2,4-Dichlorophenol jar. 1,2,4-Trichlorobenzene EANaphthalene Hexachloro-l,3-butadiene Dhogmde 4-Chloro-3-methylphenol 2,4,6-Trichlorophenol a 2-Chloronaphthalene Lno im Dimethylphthalate ND ug/l ND ug/l I 3b maaan ND ug/l EZ iain NB ug/l NB ug/l 3 3 Lanes ND ug/l ~D ug/l 2: Zp tama ND ug/l E Doom un a samnemoe ~D ug/l ii. 03/03/04 20:05 KSK 111-91-1 ii. 03/03/04 20:05 KSK 120-83-2 11. 03/03/04 20:05 KSK 120-82-1 ii. 03/03/04 20:05 KSK 91-20-3 ii. 03/03/04 20:05 KSK 87-68-3 11. 03/03/04 20:05 KSK 59-50-7 11. 03/03/04 20:05 KSK 88-06-2 ii. 03/03/04 20:05 KSK 91-58-7 iio 03/03/04 20:05 KSK 131-11-3 Acenaphthylene 2,6-Dinitrotoluene boAcenaphthene Et 2,4-Dinitrophenol Ty 4-Nitrophenol EL, 2,4-Dinitrotoluene an Diethylphthalate ~D ug/l ~D ug/l 2 2 Snide ND ug/l 2 7 LL imiemid ~D ug/l EI El ND ug/l 2 2 Smmamies ~D ug/l 2 ZL dmnen i ~D ug/l ii. 03/03/04 20:05 KSK 208-96-8 ii. 03/03/04 20:05 KSK 606-20-2 ii. 03/03/04 20:05 KSK 83-32-9 54. 03/03/04 20:05 KSK 51-28-5 54. 03/03/04 20:05 KSK 100-02-7 ii. 03/03/04 20:05 KSK 121-14-2 ii. 03/03/04 20~05 KSK 84-66-2 Date: 03111/04 Page: 4 of 33 ionhelHaec: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00003377 aw rsoren 3M MN01539188 iceAAnnaallyyttiiccaall eto Pace Analytical Services, Inc. en 1700 Elm Slreet, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.607,1700 Fax: 612.507.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test oe es i SO i cs Lab Sample No: 105362750 0 cvs on il RE Client Sample ID: E04-0126-67610 Sample Port Lead IA Preject Sample Number: 1085104-002 Matrix: Water Date Collected: 02/25/04 10:56 Date Received: 02/25/04 18:00 Rto ear merit fn E0818 erie ie EE Parameters rag i 4 Chlorophenyiphenyl ether oe 5 LD anErs Fluorene CEE gs & Th mmmnemn 4,6-Dinitro-2-methylphenol primo song SE RE RE od 4-Bromophenylphenyl ether Lar Doom on semua an Hexachlorobenzene bd 2 2 masse Pentachlorophenol [oe 2 ZL fuiesia Phenanthrene fea, =D magn Anthracene Di-n-butylphthalate fr 2 Zo immsemud Fluoranthene bo Doom on ammuem ou Pyrene En --_-- Doom on mambo me Butylbenzylphthalate Srnec EA pane wen 3,3'-Dichlorobenzidine Da : 2 mmmnih Benzo(a)anthraeene i 2 2 0 FmmEis Chrysene is BTA Dmne nes bis(2-Ethylhexyl)phthalate se PZ Lb fnew Di-n-octylphthalate [a Doom on pamuem na Benzo(h)fluoranthene re 2: ZL Hamma Benzo(k)fluoranthene es Doom on aamnenm owe Benzo(a)pyrene Solow Lf SL mem Indeno(l,2,3-cd)pyrene bi EN JET i Dibenz(a,h)anthracene a 2 2 Lmaamel Benzo(g,h,i)perylene feres IEo 2 Lb ananienniga Hexachloroethane Results HD HD ND ND HD ND ND ~D ffD ffD ffD ND ffD ffD ~D ~D ~D ND ~D ~D ~D ~D ND ~D Units ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l Report Limit Analyzed By ii. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK 54. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK 25. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK 22. 03/03/04 20:05 KSK 11. 03/03/04 20:05 KgK ii. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK ii. 03/03/04 20:05 KSK CAS No. 7005 72 3 86 73 7 534-52-1 101-55-3 118-74-1 87-86-5 85-01-8 120-12-7 84-74-2 206-44-0 129-00-0 85-68-7 91-94-1 56-55-3 218-01-9 117-81-7 117-84-0 205-99-2 207-08-9 50-32-8 193-39-5 53-70-3 191-24-2 67-72-1 Qual RegLmt Nitrobenzene-d5 (S) 88 % 03/03/04 20:05 KSK 4165-60-0 2-Fluorobiphenyl (S) 89 % 03/03/04 20:05 KSK 321-60-8 ~erphenyl-dl4 (S) Phenol-d6 (S) amet 2-Fluorophenol (S) 2,4,6-Tribromophenol (S) a Date Extracted A GC/MS Volatiles EIS Volatile GC/MS by 624 rs Chloromethane ShVinyl chloride on es Bromomethane Sae e Chloroethane 89 % 0 % co0 % 36 % "A 03/01/04 wage Method: EPA 624 15% ur 8.4 ug/l 1.0 > 3 ~D ug/l 1.0 I 8.5 ug/l 1.0 22 2TB4 ~D ug/l 1.0 03/03/04 20:05 KSK 1718-51-0 03/03/04 20:05 KSK 13127-88-3 2 seme a 03/03/04 20:05 KSK 367-12-4 2 03/03/04 20:05 KSK 2 we 03/01/04 mm we 02/27/04 03:35 RJS UmmEr 02/27/04 03:35 RJS mats 02/27/04 03:35 RJS Hamdaannn a 02/27/04 03:35 RJS 74-87-3 75-01-4 74-83-9 75-00-3 Trichlorofluoromethane ~D ug/l 1.0 02/27/04 03~35 RJS 75-69-4 Date: 03/11/~4 Page: 5 of 33 iS nelE ac: momen RREEPPOORRTT OOFF LLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'Thi~ r'ep(:,~ shall n~t I~ r~pro~u~. ~ept i. f~ll, without th~ written consent ~f Pac~ ,~naly'dcal Servi~e~, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00003388 [pT 3M MN01539189 iceAAnnaallyyttiiccaall ee tn o Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.607,1700 Fax: 612.507.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test oe es i SO i cs Lab Sample No: 105362750 0 cvs on il RE Client Sample ID: E04-0126-67610 Sample Port Lead IA Project Sample Number: 1085104-002 Matrix: Water Date Collected: 02/25/04 10:56 Date Received: 02/25/04 18:00 Sapg on SOR e urilm fm Parameters Methylene chloride re STE arerE I,i Dichloroethene Dame EZ ummm trans-l,2-Dichloroethene Sn 2 Zane l,l-Dichloroethane Le oom amma nn Chloroform ri PZ aianam l,l,l-Trichloroethane Fn EZ i fpsiabie Carbon tetrachloride = Doom amma Benzene 1,2-Diehloroethane fn $Z Nh imminee Trichloroethene Fer Doom aman ne 1,2-Dichloropropane s meete EDI mI H ny mme mnae nn Bromodichloromethane Results 2.1 ND ND ND ND ND ~D ~D 5.3 ND ~D ~D Units ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l Report Limit Analyzed By 1.0 02/27/04 09:35 RJS 1.0 02/27/04 09:35 RJS 1.0 02/27/04 03~35 RJS 1.0 02/27/04 03:35 RJS 1.0 02/27/04 03:35 RJS 1.0 02/27/04 03:35 RJS 1.0 02/27/04 09:35 RJS 1.0 02/27/04 09:35 RJS 1.0 02/27/04 09:35 RJS 1.0 02/27/04 03:35 RJS 1.0 02/27/04 03:35 RJS 1.0 02/27/04 03:35 RJS CAS No. 75 09 2 75 35 4 156-60-5 75-34-3 67-66-3 71-55-6 56-23-5 71-43-2 107-06-2 79-01-6 78-87-5 75-27-4 Qual RegLmt trans-l,3-Dichloropropene ~D ug/l 1.0 02/27/04 03:35 RJS 10061-02-6 Toluene els-l,3-Diehloropropene Sra 1,1,2-Trlchloroethane Tetraehloroethene fe Dibromochloromethane in Chlorohenzene a Ethylbenzene SaXylene (Total) neBromoform mes l,l,2,2-Tetrachloroethane Lp 1,3-Dichlorobenzene 1,4-Dichlorobenzene ho1,2-Dichlorobenzene are 2-chloroethylvinyl ether mid Dibromofluoromethane (S) Toluene-d8 (S) We en 4-Bromofluorobenzene (S) mE 1,2-Dichloroethane-d4 (S! ND ug/l 1.0 ND ug/l 1.0 Doom ND ug/l 1.0 ~D ug/l 1.0 Doom ~D ug/l 1.0 2 Zi ~D ug/l 1.0 Doom ND ug/l 1.0 Pe ND ug/l 3.0 Doom ~D ug/l 1.0 3 BO ~D ug/l 1.0 I 2 BH ~D ug/l 1.0 ~D ug/l 1.0 22 i ND ug/l 1.0 2 2B ~D ug/l 5.0 114 % 104 % 106 % ii0 % 02/27/04 0~:35 ~JS 02/27/04 03:35 ~JS ama wen 02/27/04 09:35 RJS 02/27/04 03:35 RJS mma man 02/27/04 03:35 RJS abana 02/27/04 03:35 RJS mma 02/27/04 03:35 RJS Tn 02/27/04 03:35 RJS aman ne 02/27/04 03:35 RJS mane 02/27/04 03:35 RJS mania 02/27/04 03:35 RJS 02/27/04 03:35 RJS manag 02/27/04 03:35 RJS EAE 02/27/04 03:35 RJS Srna 02/27/04 03:35 RJS 02/27/04 03:35 RJS a 02/27/04 03:35 RJS TaAnak va, 02/27/04 03:35 RJS 10S-SS-3 i0061-01-5 79-00-5 127-18-4 124-48-1 108-90-7 100-41-4 1330-20-7 75-25-2 79-34-5 541-73-I 106-46-7 95-50-1 110-75-8 1868-53-7 2037-26-5 460-00-4 17060-07-0 Date: 03/11/04 ionhelHaec: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'Thi~ r'epn~ shall n~t I~ r~pro~u~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00003399 Page: 6 of 33 [pT 3M MN01539190 iceAAnnaallyyttiiccaall eto Pace Analytical Semices, Inc. en 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.60Z 1700 Fa~: 612.607.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test PE ) ET Lab Sample No: 105362768 EE cv il Client Sample ID: E04-0126-67611 Sample Port Lead IB Project Sample Number: 1085104-003 Matrix: Water Date Collected: 02/25/04 11:03 Date Received: 02/25/04 18:00 iar erie on 85SmSer ei ifm iE Parameters Microbiology Results _ Uni_ ts Report Limit Analyzed By CAS No. mm 4 ero Lattin Biochemical Oxygen Demand, 5 d Prep/Method: / SM 5210B i EEE cron sn Sm . BOD, 5 day 7 m9/l 6 03/02/04 JPHI Qual RegLmt 1 Date Prepared -- Wet Chemistry SL, re Phenolies Total. in Water enPhenol SI GC/MS Semivolatiles OL 625 wastewater GC/MS SVOA eyPhenol VR bis(2-Chloroethyl) ether So 2-Chlorophenol rm 1,3-Diehlorohenzene mee 1,4-Diehlorobenzene Filo 1,2-Dichlorobenzene mr bls(2-Chloroisopropyl) ether fide N-Nitroso-di-n-propylamine Le Nitrobenzene ps Isophorone fe2-Nitrophenol 3 ile 2,4-Dimethylphenol 02/26/04 10:30 02/26/04 10:30 wigs mingmit, Method: EPA 420.4 ND ug/l re mens wi 25.0 03/05/04 08:41 VAF 108-95-2 ima tin Prep/Method: EPA 625 / EPA 625 Din imas ie ws ND ug/l ii. obi ~D ug/l ii. P 2 amma ND ug/l ~. 2 2 0 Samm ND ug/l ii. Doom on emu ens ND ug/l ii. PE ZL Danes ND ug/l ii. BL RL RS ee ~D ug/l ii. 2 2 EF Unnan ~D ug/l ii. Doom on ama a ND ug/l 11. EEL ND ug/l ii. FEEREE ND ug/l n. 22 23b m gusum aiis en ND ug/l ii. 03/03/04 20:58 KSK 03/03/04 20:58 KSK o~/o~/o4 20:58 KSK 03/03/04 20:58 KSK 03/03/04 20:58 KSK o3/o3/o4 20:58 KSK 03/03/04 20:58 KSK 03/03/04 20:58 KSK 03/03/04 20:58 KSK 03/03/04 20:58 KSK 03/03/04 20:58 KSK 03/03/04 20:58 KSK 108-95-2 111-44-4 95-57-~ 541-73-I 106-46-7 95-50-1 39638-32-9 621-64-7 98-95-3 78-59-1 88-75-5 105-67-9 bis(2-Chloroethoxy)methane 2,4-Dichlorophenol jar. 1,2,4-Trichlorobenzene EANaphthalene Hexachloro-l,3-butadiene Dhogmde 4-Chloro-3-methylphenol me 2,4,6-Trichlorophenol a 2-Chloronaphthalene LoDimethylphthalate nim Acenaphthylene 2,6-Dinitrotoluene boAcenaphthene Et 2,4-Dinitrophenol Ty 4-Nitrophenol EL, 2,4-Dinitrotoluene an Diethylphthalate ~D ug/l ND ug/l I 3 OL mamas ND ug/l EZ aia ND ug/l ND ug/l 3 3 Luan ND ug/l Doom on aman ND ug/l 2: Zp tae ~D ug/l Doom un samaamoe ~D ug/l ERLE ~D ug/l ~D ug/l 2 2 nA ND ug/l FEE ND ug/l EI~D ug/l 2 ZL Smee ~D ug/l 2 ZL omnes ~D ug/l ii. 03/03/04 20:58 KSK 111-91-1 ii. 03/03/04 20:58 KSK 120-83-2 11. 03/03/04 20:58 KSK 120-82-1 ii. 03/03/04 20:58 KSK 91-20-3 ii. 03/03/04 20:58 KSK 87-68-3 11. 03/03/04 20:58 KSK 59-50-7 11. 03/03/04 20:58 KSK 88-06-2 ii. 03/03/04 20:58 KSK 91-58-7 iio 03/03/04 20:58 KSK 131-11-3 ii. 03/03/04 20:58 KSK 208-96-8 ii. 03/03/04 20:58 KSK 606-20-2 ii. 03/03/04 20:58 KSK 83-32-9 56. 03/03/04 20:58 KSK 51-28-5 56. 03/03/04 20:58 KSK 100-02-7 ii. 03/03/04 20:58 KSK 121-14-2 ii. 03/03/04 20:58 KSK 84-66-2 Date: 03/11/04 Page: 7 of 33 ionhelHaec: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS This repor~ shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00004400 pr 3M MN01539191 iceAAnnaallyyttiiccaall ee ton Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.607,1700 Fax: 612.507.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test PE ) ET Lab Sample No: 105362768 EE cv il Client Sample ID: E04-0126-67611 Sample Port Lead iB Preject Sample Number: 1085104-003 Matrix: Water Date Collected: 02/25/04 11:03 Date Received: 02/25/04 18:00 Rto ear merit fon O81 rie ie EE Parameters rag i 4 Chlorophenyiphenyl ether oe 5D amen Fluorene CEE gs & Th mmm nD 4,6-Dinitro-2-methylphenol ims 3 2 LF Honan 4-Bromophenylphenyl ether Lar Doom on semua Hexachlorobenzene bd 2 2 maa Pentachlorophenol [oe 2 2 fsiasia Phenanthrene fea, 2b omen Anthracene Di-n-butylphthalate fr 2 Zo dmmadeud Fluoranthene bo Doom on amma Pyrene En --_-- Doom on nama ae Butylbenzylphthalate Spmewess EA pasa wen 3,3'-Dichlorobenzidine Da : 2 mmaih Benzo(a)anthraeene i 2 2 0 JmmErs Chrysene is BTA Dn nes bis(2-Ethylhexyl)phthalate se PZ fase Di-n-octylphthalate [a Doom on aman wa Benzo(h)fluoranthene re PZ OL Hamma Benzo(k)fluoranthene es Doom on ama Benzo(a)pyrene Solow Lf ob Tmama Indeno(l,2,3-cd)pyrene bi EM JET 1 Dibenz(a,h)anthracene a 2 2 memes Benzo(g,h,i)perylene feres I5 Laan ieas Hexachloroethane Results HD HD ND ND HD ND ND ~D ~D ~D ~D ND ~D ND ND ND ~D ND ~D ~D ~D ~D ND ~D Units ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l Report Limit Analyzed By ii. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK 56. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK 26. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK 22. 03/03/04 20:58 KSK ]]. 03/03/04 20:58 KgE ii. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK ii. 03/03/04 20:58 KSK CAS No. 7005 72 3 86 73 7 534-52-1 101-55-3 118-74-1 87-86-5 85-01-8 120-12-7 84-74-2 206-44-0 129-00-0 85-68-7 91-94-1 56-55-3 218-01-9 117-81-7 117-84-0 205-99-2 207-08-9 50-32-8 193-39-5 53-70-3 191-24-2 67-72-1 Qual RegLmt Nitrobenzene-d5 (S) 83 % 03/03/04 20:58 KSK 4165-60-0 2-Fluorobiphenyl (S) 84 % 03/03/04 20:58 KSK 321-60-8 ~erphenyl-dl4 (s) Phenol-d6 (S) amet 2-Fluorophenol (S) 2,4,6-Tribromophenol (S) a Date Extracted A GC/MS Volatiles EIS Volatile GC/MS by 624 rs Chloromethane ShVinyl chloride on es Bromomethane Sre e Chloroethane 86 % 1 % FE6 % 24 % i, 03/01/04 wep Method: EPA 624 1% wr 7.8 ug/l 1.0 > 3 ~D ug/l 1.0 Si RT 4.1 ug/l 1.0 2 23B3 ~D ug/l 1.0 03/03/04 20:58 KSK 1718-51-0 03/03/04 20:58 KSK 13127-88-3 2 Semin pm 03/03/04 20:58 KSK 367-12-4 2 03/03/04 20:58 KSK 2 we 03/01/04 mm 02/27/04 0{:03 RJS immsnrm 02/27/04 04:03 RJS EAE Eats 02/27/04 04:03 RJS a mEmn isna nd 02/27/04 04:03 RJS 74-87-3 75-01-4 74-83-9 75-00-3 Trichlorofluoromethane ~D ug/l 1.0 02/27/04 04~03 RJS 75-69-4 Date: 03/11/~4 Page: 8 of 33 iS nelE ac: momen RREEPPOORRTT OOFF LLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'Thi~ r'ep(:,~ shall n~t I~ r~pro~u~. ~ept i. f~ll, without th~ written consent of Pac~ ,a, nalytical Servi~e~, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00004411 aw mrsarez 3M MN01539192 iceAAnnaallyyttiiccaall ee tn o Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.607,1700 Fax: 612.507.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test PE ) ET Lab Sample No: 105362768 EE cv il Client Sample ID: E04-0126-67611 Sample Port Lead IB Project Sample Number: 1085104-003 Matrix: Water Date Collected: 02/25/04 11:03 Date Received: 02/25/04 18:00 S erg ofon KOR n ilfm Parameters Methylene chloride re Fn amare I,i Dichloroethene Dame EZ nm mmmmew ol trans-l,2-Dichloroethene Sn PZ Lane l,l-Dichloroethane Le Doom ammaem on Chloroform ri : 2 4 aeanam l,l,l-Trichloroethane Fn EZ i fpaiabie Carbon tetrachloride = Doom ammo Benzene 1,2-Diehloroethane fn Ful ELE Trichloroethene Fer oom ammo nen 1,2-Dichloropropane s meete E DE m ny B mmma mewe on Bromodichloromethane Results 2.6 ND ND ND ND ND ~D ~D 3.6 ND ~D ~D Units ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l Report Limit Analyzed By 1.0 02/27/04 04:03 RJS 1.0 02/27/04 04:03 RJS 1.0 02/27/04 04~03 RJS 1.0 02/27/04 04:03 RJS 1.0 02/27/04 04:03 RJS 1.0 02/27/04 04:03 RJS 1.0 02/27/04 04:03 RJS 1.0 02/27/04 04:03 RJS 1.0 02/27/04 04:03 RJS 1.0 02/27/04 04:03 RJS 1.0 02/27/04 04:03 RJS 1.0 02/27/04 04:03 RJS CAS No. 75 09 2 75 35 4 156-60-5 75-34-3 67-66-3 71-55-6 56-23-5 71-43-2 107-06-2 79-01-6 78-87-5 75-27-4 Qual RegLmt trans-l,3-Dichloropropene ~D ug/l 1.0 02/27/04 04:03 RJS 10061-02-6 Toluene els-l,3-Diehloropropene Sra 1,1,2-Trlchloroethane Tetraehloroethene fe Dibromochloromethane in Chlorohenzene a Ethylbenzene SaXylene (Total) neBromoform mes l,l,2,2-Tetrachloroethane Lp 1,3-Dichlorobenzene 1,4-Dichlorobenzene ho1,2-Dichlorobenzene are 2-chloroethylvinyl ether Soar Dibromofluoromethane (S) Toluene-d8 (S) FER 4-Bromofluorobenzene (S) Patten 1,2-Dichloroethane-d4 (S! ND ug/l 1.0 ND ug/l 1.0 Doom ND ug/l 1.0 ~D ug/l 1.0 Doom ~D ug/l 1.0 2 Zi ~D ug/l 1.0 oom ND ug/l 1.0 PS ND ug/l 3.0 Doom ~D ug/l 1.0 3 BO ~D ug/l 1.0 I 2 OB ND ug/l 1.0 ~D ug/l 1.0 2 Zi ~D ug/l 1.0 2 2B ND ug/l 5.0 4} 123 % 3 77 % 105 % 117 % 02/27/04 04:03 ~JS 02/27/04 04:03 ~JS ammo wen 02/27/04 04:03 RJS 02/27/04 04:03 RJS mma ma 02/27/04 04:03 RJS amnae 02/27/04 04:03 RJS maemo 02/27/04 04:03 RJS Haan 02/27/04 04:03 RJS mae nen 02/27/04 04:03 RJS mana 02/27/04 04:03 RJS maaan 02/27/04 04:03 RJS 02/27/04 04:03 RJS imag 02/27/04 04:03 RJS Earns 02/27/04 04:03 RJS Trad 02/27/04 04:03 RJS 02/27/04 04:03 RJS ae 02/27/04 04:03 RJS PAAR va, 02/27/04 04:03 RJS 10S-SS-3 i0061-01-5 79-00-5 127-18-4 124-48-1 108-90-7 100-41-4 1330-20-7 75-25-2 79-34-5 541-73-I 106-46-7 95-50-1 110-75-8 1868-53-7 2037-26-5 460-00-4 17060-07-0 Date: 03/11/04 ionhelHaec: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'Thi~ r'epn~ shall n~t I~ r~pro~u~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00004422 Page: 9 of 33 aw mrsores 3M MN01539193 iceAAnnaallyyttiiccaall eto Pace Analytical Semices, Inc. en 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.60Z 1700 Fa~: 612.607.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test oe es i er SO cs Lab Sample No: 105362776 sev on il Client Sample ID: E04-0126-67612 Sample Port Lead 4A Project Sample Number: 1085104-004 Matrix: Water Date Collected: 02/25/04 ii:Ii Date Received: 02/25/04 18:00 iamnowSeiifm iE Parameters Microbiology Results _ Uni_ ts Report Limit Analyzed By CAS No. mm 4 ero Lattin Biochemical Oxygen Demand, 5 d Prep/Method: / SM 5210B EEveiEn cron sn Sm . BOD, 5 day 7 m9/l 6 03/02/04 JPHI Qual RegLmt 1 Date Prepared -- Wet Chemistry SL, re Phenolies Total. in Water enPhenol SI GC/MS Semivolatiles OL 625 wastewater GC/MS SVOA eyPhenol Pre bis(2-Chloroethyl) ether So 2-Chlorophenol rm 1,3-Diehlorohenzene mee 1,4-Diehlorobenzene Filo 1,2-Dichlorobenzene nmr bls(2-Chloroisopropyl) ether fide N-Nitroso-di-n-propylamine Le Nitrobenzene ps Isophorone fe2-Nitrophenol 3 ite 2,4-Dimethylphenol 02/26/04 10:30 wigs mingmit, re Method: EPA 420.4 ND ug/l 25.0 ima tin Prep/Method: EPA 625 / EPA 625 Din Bat ND ug/l 10. 3~D ug/l 10. PZ I ND ug/l ~o. 2 2 OF ND ug/l 10. Doom ND ug/l 10. EZ 5 ND ug/l 10. BL RL ~D ug/l i0. 2 2 OF ~D ug/l 10. Doom on ND ug/l i0. CIND ug/l i0. ERND ug/l i0. 22 Z 3 p ND ug/l i0. 02/26/04 10:30 mens wi 03/05/04 08:41 VAF 108-95-2 Le ws 03/03/04 21:51 KSK Lope 03/03/04 21:51 KSK amma o~/o~/o4 21:51 KSK mE 03/03/04 KSK pemanm ens 03/03/04 KSK fimnas 03/03/04 21:51 KSK Ye 03/03/04 21:51 KSK Unnan 03/03/04 21:51 KSK seman a 03/03/04 21:51 KSK 03/03/04 21:51 KSK EE 03103/04 21:51 KSK tgumsenasnuieen 03/03/04 21:51 KSK 108-95-2 111-44-4 95-57-~ 541-73-I 106-46-7 95-50-1 39638-32-9 621-64-7 98-95-3 78-59-1 88-75-5 105-67-9 bis(2-Chloroethoxy)methane 2,4-Dichlorophenol jar. 1,2,4-Trichlorobenzene EANaphthalene Hexachloro-l,3-butadiene piel 4-Chloro-3-methylphenol 2,4,6-Trichlorophenol a 2-Chloronaphthalene Lno im Dimethylphthalate ~D ug/l ND ug/l I 3 5 maaan ND ug/l EZ bin ND ug/l ND ug/l SER EL EE ND ug/l ND ug/l 2 Zk tian ~D ug/l E Doom R semanEmoae ~D ug/l i0. 03103/04 21:51 KSK 111-91-1 10. 03/03/04 21:51 KSK 120-83-2 i0. 03/03/04 21:51 KSK 120-82-1 10. 03/03/04 21:51 KSK 91-20-3 i0. 03/03/04 21:51 KSK 87-68-3 i0. 03/03/04 21:51 KSK 59-50-7 i0. 03/03/04 21:51 KSK 88-06-2 i0. 03/03/04 21:51 KSK 91-58-7 i0. 03/03/04 21:51 KSK 131-11-3 Acenaphthylene 2,6-Dinitrotoluene boAcenaphthene Et 2,4-Dinitrophenol Ty 4-Nitrophenol EL, 2,4-Dinitrotoluene an Diethylphthalate ~D ug/l ~D ug/l 2 2 hed ND ug/l iP = ZmmEin ND ug/l EI lr ~D ug/l 2 ZL Lmmemie ~D ug/l 2 Zk mide ~D ug/l 10. 03/03/04 21:51 KSK 208-96-8 10. 03/03/04 21:51 KSK 606-20-2 i0. 03/03/04 21:51 KSK 83-32-9 51. 03/03/04 21:51 KSK 51-28-5 51. 03/03/04 21:51 KSK 100-02-7 i0. 03/03/04 21:51 KSK 121-14-2 i0. 03/03/04 21~51 KSK 84-66-2 Date: 03/11/04 Page: i0 of 33 ionhelHaec: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00004433 aw rsores 3M MN01539194 iceAAnnaallyyttiiccaall ee ton Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.607,1700 Fax: 612.507.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test oe es i er SO cs Lab Sample No: 105362776 sev on il Client Sample ID: E04-0126-67612 Sample Port Lead 4A Preject Sample Number: 1085104-004 Matrix: Water Date Collected: 02/25/04 ii:Ii Date Received: 02/25/04 18:00 Rto ear rtm fn E8188 rie ie EE Parameters rag in 4 Chlorophenyiphenyl ether oe 5 aes Fluorene CEE gs & TAM mma nn 4,6-Dinitro-2-methylphenol ims 3 2 EF Gonna 4-Bromophenylphenyl ether Lar Doom on semana Hexachlorohenzene bd ? 2 maa Pentachlorophenol [oe 2 ZB fuiasia Phenanthrene fea, 2B ommEin Anthracene Di-n-butylphthalate fr PZ & dmmaeeud Fluoranthene bo Doom on ammanm Pyrene En --_-- Doom on naman ae Butylbenzylphthalate Spmewess EA pasa wen 3,3'-Dichlorobenzidine Da : 2 EB ammnid Benzo(a)anthraeene i 2 2 EF FmmErE Chrysene is BTA MDa meas his(2-Ethylhexyl)phthalate se PZ b&b fame Di-n-octylphthalate [a Doom aman wa Benzo(h)fluoranthene re PZ bE Hames Benzo(k)fluoranthene es Doom on ema we Benzo(a)pyrene Solow fo Tmaea Indeno(l,2,3-cd)pyrene bi EM EAS 1 Dibenz(a,h)anthracene a 2 Zp Lmesis Benzo(g,h,i)perylene feres IEo PL anaEe Hexachloroethane Results HD HD ND ND HD ND ND ND ND ND ND ND ND ND ~D ND ~D ~D ~D ND ND ~D ~D ~D Units ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l Report Limit Analyzed By i0. 03/03/04 21:51 KSK i0. 03/03/04 21:51 KSK 51. 03/03/04 21:51 KSK i0. 03/03/04 21:51 KSK i0. 03/03/04 21:51 KSK 23. 03/03/04 21:51 KSK i0. 03/03/04 21:51 KSK i0. 03/03/04 21:51 KSK i0. 03/03/04 21:51 KSK i0. 03/03/04 21:51 KSK 10. 03/03/04 21:51 KSK i0. 03/03/04 21:51 KSK 20. 03/03/04 21:51 KSK ]0. 03/03/04 21:5] ~SE i0. 03/03/04 21:51 KSK i0. 03/03/04 21:51 KSK i0. 03/03/04 21:51 KSK i0. 03/03/04 21:51 KSK i0. 03/03/04 21:51 KSK i0. 03/03/04 21:51 KSK i0. 03/03/04 21:51 KSK 10. 03/03/04 21:51 KSK 10. 03/03/04 21:51 KSK 10. 03/03/04 21:51 KSK CAS No. 7005 72 3 86 73 7 534-52-1 101-55-3 118-74-1 87-86-5 85-01-8 120-12-7 84-74-2 206-44-0 129-00-0 85-68-7 91-94-1 56-55-3 218-01-9 117-81-7 117-84-0 205-99-2 207-08-9 50-32-8 193-39-5 53-70-3 191-24-2 67-72-1 Qual RegLmt Nitrobenzene-d5 (S) 90 % 03/03/04 21:51 KSK 4165-60-0 2-Fluorobiphenyl (S) 94 % 03/03/04 21:51 KSK 321-60-8 ~erphenyl-dl4 (S) Phenol-d6 (S) amet 2-Fluorophenol (S) 2,4,6-Tribromophenol (S) a Date Extracted A GC/MS Volatiles EIS Volatile GC/MS by 624 rs Chloromethane ShVinyl chloride on es Bromomethane a Se e Chloroethane 93 % 0 % co0 % 0 % Coe 03/01/04 wep Method: EPA 624 1% wr 7.1 ug/l 1.0 > 3 ND ug/l 1.0 So3.9 ug/l 1.0 2se 23B3 ~D ug/l 1.0 03/03/04 21:51 KSK 1718-51-0 03/03/04 21:51 KSK 13127-88-3 2 Geman a 03/03/04 21:51 KSK 367-12-4 2 03/03/04 21:51 KSK 2 we 03/01/04 sen we 02/27/04 0{:30 RJS ummm 02/27/04 04:30 RJS ee at 02/27/04 04:30 RJS m HaEnAa 02/27/04 04:30 RJS 74-87-3 75-01-4 74-83-9 75-00-3 Trichlorofluoromethane ~D ug/l 1.0 02/27/04 04~30 RJS 75-69-4 Date: 03/11/04 Page: ii of 33 iS nelE ac: momen RREEPPOORRTT OOFF LLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'Thi~ r'epn~ shall n~t I~ r~pro~u~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00004444 [p-- 3M MN01539195 iceAAnnaallyyttiiccaall ee tn o Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.607,1700 Fax: 612.507.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test oe es i er SO cs Lab Sample No: 105362776 sev on il Client Sample ID: E04-0126-67612 Sample Port Lead 4A Project Sample Number: 1085104-004 Matrix: Water Date Collected: 02/25/04 ii:Ii Date Received: 02/25/04 18:00 Soon g KOR rin lfm Parameters Methylene chloride re ST amare I,i Dichloroethene Dememe EZ ummm trans-l,2-Dichloroethene Sn 2 Zi Laan l,l-Dichloroethane Le Doom amma nn Chloroform ri 22 0 aenam l,l,l-Trichloroethane F = n E DooZm i faamnambiae Carbon tetrachloride Results 3.0 ND ND ND ND ND ~D Units ug/l ug/l ug/l ug/l ug/l ug/l ug/l Report Limit Analyzed By 1.0 02/27/04 04:30 RJS 1.0 02/27/04 04:30 RJS 1.0 02/27/04 04~30 RJS 1.0 02/27/04 04:30 RJS 1.0 02/27/04 04:30 RJS 1.0 02/27/04 04:30 RJS 1.0 02/27/04 04:30 RJS CAS No. 75 09 2 75 35 4 156-60-5 75-34-3 67-66-3 71-55-6 56-23-5 Qual RegLmt Benzene 1,2-Diehloroethane fn Trichloroethene Fer1,2-Dichloropropane s meete Bromodichloromethane ~D ug/l 3.9 ug/l $5 ND ug/l Doom ~D ug/l EDI mI ~D ug/l 1.0 02/27/04 04:30 RJS 71-43-2 1.0 02/27/04 04:30 RJS 107-06-2 Eee ve 1.0 02/27/04 04:30 RJS 79-01-6 am nen 1.0 02/27/04 04:30 RJS 78-87-5 a mmm nn 1.0 02/27/04 04:30 RJS 75-27-4 trans-l,3-Dichloropropene ~D ug/l 1.0 02/27/04 04:30 RJS 10061-02-6 Toluene els-l,3-Diehloropropene Sra 1,1,2-Trlchloroethane Tetraehloroethene fe Dibromochloromethane in Chlorohenzene a Ethylbenzene SaXylene (Total) neBromoform oLorpWE l,l,2,2-Tetrachloroethane ND ug/l 1.0 ND ug/l 1.0 Doom ND ug/l 1.0 ND ug/l 1.0 Doom ND ug/l 1.0 2 Zi ~D ug/l 1.0 Doom ND ug/l 1.0 PS ND ug/l 3.0 Doom ~D ug/l 1.0 E I 2EBH ~D ug/l 1.0 02/27/04 04:30 RJS 02/27/04 04:30 RJS am wen 02/27/04 04:30 ~JS 02/27/04 04:30 RJS amma man 02/27/04 04:30 RJS aman 02/27/04 04:30 RJS amma wen 02/27/04 04:30 RJS Emam 02/27/04 04:30 RJS mma ne 02/27/04 04:30 RJS E gmmEanni 02/27/04 04:30 RJS 10S-Sg-3 10061-01-5 79-00-5 127-18-4 124-48-I 108-90-7 100-41-4 1330-20-7 75-25-2 79-34-5 1,3-Dichlorobenzene ND ug/l 1.0 1,4-Dichlorobenzene ~D ug/l 1.0 ho 2 Zi 1,2-Dichlorobenzene ~D ug/l 1.0 are 2 2B 2-chloroethylvinyl ether ND ug/l 5.0 mid Dibromofluoromethane (S) 124 % Toluene-d8 (S) 78 % WE nw 4-Bromofluorobenzene (S) 107 % Prien 3 1,2-Dichloroethane-d4 (S! 117 % 02/27/04 04:30 RJS 02/27/04 04:30 RJS maaan 02/27/04 04:30 RJS EAE 02/27/04 04:30 RJS Trad 02/27/04 04:30 RJS 02/27/04 04:30 RJS a 02/27/04 04:30 RJS PAANRR va, 02/27/04 04:30 RJS 541-73-I 106-46-7 95-50-1 110-75-8 1868-53-7 2037-26-5 460-00-4 17060-07-0 Date: 03/11/~4 ionhelHaec: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'Thi~ r'epn~ shall n~t I~ r~pro~u~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00004455 Page: 12 of 33 aw rsores 3M MN01539196 iceAAnnaallyyttiiccaall eto Pace Analytical Semices, Inc. en 1700 Elm Slreet, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.60Z 1700 Fa~: 612.607.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test NT) i er SO i is Lab Sample No: 105362784 sev il Client Sample ID: E04-0126-67613 Sample Port Lead 4B Project Sample Number: 1085104-005 Matrix: Water Date Collected: 02/25/04 11:25 Date Received: 02/25/04 18:00 iamnowSeiifm iE Parameters Microbiology Results _ Uni_ ts Report Limit Analyzed By CAS No. Tm ome 14 ergs Ltn Biochemical Oxygen Demand, 5 d Prep/Method: / SM 5210B EEveiEn a rss Sm en . BOD, 5 day 6 mg/l 6 03/02/04 JPHI Qual RegLmt 1 Date Prepared -- Wet Chemistry SL, re Phenolies Total. in Water enPhenol SI GC/MS Semivolatiles OL 625 wastewater GC/MS SVOA eyPhenol Pre bis(2-Chloroethyl) ether So 2-Chlorophenol rm 1,3-Diehlorohenzene mee 1,4-Diehlorobenzene Filo 1,2-Dichlorobenzene mr bls(2-Chloroisopropyl) ether fide N-Nitroso-di-n-propylamine Le Nitrobenzene ps Isophorone fe2-Nitrophenol 3 ile 2,4-Dimethylphenol 02/26/04 10:30 02/26/04 10:30 wigs mingmit, Method: EPA 420.4 ND ug/l re mens wi 25.0 03/05/04 08:41 VAF 108-95-2 ima tin Prep/Method: EPA 625 / EPA 625 Dinas Le ws ND ug/l ii. 3 ob Login ~D ug/l ii. PZ mniagl ND ug/l ~. 2 2 0 TE ND ug/l ii. Doom on pomaim ens ND ug/l ii. PE ZL Himpsel ND ug/l ii. BL Le ~D ug/l ii. 2 2 EF Uhnana ~D ug/l ii. Doom on amma ND ug/l 11. POZE miagan ND ug/l ii. EE ND ug/l n. 22 23b L gusenann lsen ND ug/l ii. 03/03/04 22:44 KSK 03/03/04 22:44 KSK o~/o~/o4 22:44 KSK 03/03/04 22:44 KSK 03/03/04 22:44 KSK o3/o3/o4 22:44 KSK 03/03/04 22:44 KSK 03/03/04 22:44 KSK 03/03/04 22:44 KSK 03/03/04 22:44 KSK 03/03/04 22:44 KSK 03/03/04 22:44 KSK 108-95-2 111-44-4 95-57-S 541-73-I 106-46-7 95-50-1 39638-32-9 621-64-7 98-95-3 78-59-1 88-75-5 105-67-9 bis(2-Chloroethoxy)methane 2,4-Dichlorophenol jar. 1,2,4-Trichlorobenzene EANaphthalene Hexachloro-l,3-butadiene Dhogmde 4-Chloro-3-methylphenol 2,4,6-Trichlorophenol a 2-Chloronaphthalene Lno im Dimethylphthalate ~D ug/l ii. ND ug/l ii. I 3b ND ug/l 11. EZ NB ug/l ii. NB ug/l ii. 3 3b ND ug/l 11. ND ug/l 11. 2: Zp ~D ug/l ii. 2Doo2m ~D ug/l iio 03/03/04 22:44 KSK 03/03/04 22:44 KSK mien 03/03/04 22:44 KSK aE 03/03/04 22:44 KSK 03/03/04 22:44 KSK mages 03/03/04 22:44 KSK 03/03/04 22:44 KSK tapas 03/03/04 22:44 KSK m semaainmone 03/03/04 22:44 KSK 111-91-1 120-83-2 120-82-1 91-20-3 87-68-3 59-50-7 88-06-2 91-58-7 131-11-3 Acenaphthylene 2,6-Dinitrotoluene boAcenaphthene Et 2,4-Dinitrophenol Ty 4-Nitrophenol EL, 2,4-Dinitrotoluene an Diethylphthalate ~D ug/l ii. ~D ug/l ii. 2 2 ND ug/l ii. 2 ZL ND ug/l 53. 22 ~D ug/l 53. 2 2 5 ~D ug/l ii. 2 ZL ~D ug/l ii. 03/03/04 22:44 KSK 03/03/04 22:44 KSK nied 03/03/04 22:44 KSK damm 03/03/04 22:44 KSK En 03/03/04 22:44 KSK Tmpamies 03103/04 22:44 KSK mie 03/03/04 22~44 KSK 208-96-8 606-20-2 83-32-9 51-28-5 100-02-7 121-14-2 84-66-2 Date: 03/11/04 Page: 13 of 33 ionhelHaec: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS This repor~ shall not be reproduced, except in full: without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00004466 aw mrsarer 3M MN01539197 iceAAnnaallyyttiiccaall ee ton Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.607,1700 Fax: 612.507.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test NT) i er SO i is Lab Sample No: 105362784 sev il Client Sample ID: E04-0126-67613 Sample Port Lead 4B Project Sample Number: 1085104-005 Matrix: Water Date Collected: 02/25/04 11:25 Date Received: 02/25/04 18:00 Rto ear mettre ie EE Parameters rag ir 4 Chlorophenyiphenyl ether oe 5 LD a=Es Fluorene CEE gs & Th mmm an 4,6-Dinitro-2-methylphenol ims 3 2 EF Honan 4-Bromophenylphenyl ether Lar Doom on amas en Hexachlorohenzene bd 2 2 mma Pentaehlorophenol [oe 2 2 5 fuiesra Phenanthrene fea, 2b omen Anthracene Di-n-butylphthalate fr 2 Zo dmmsaeud Fluoranthene bo Doom on amma Pyrene En --_-- EE Butylbenzylphthalate Gpmewess EA pass wen 3,3'-Dichlorobenzidine Da PZ amninah Benzo(a)anthraeene i 2 2 0 JmmmEie Chrysene is BTA bmi meas his(2-Ethylhexyl)phthalate se PZ Lb fame Di-n-octylphthalate [a Doom on ama wa Benzo(h)fluoranthene re 2: ZZ Ob Hamma Benzo(k)fluoranthene es Doom on ammo Benzo(a)pyrene Solow fb Tmaemam Indeno(l,2,3-cd)pyrene bi EN JE i Dibenz(a,h)anthracene a 2 Zp Lens Benzo(g,h,i)perylene feres IEo Laa ne e ia Hexachloroethane Results ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ~D ND ~D ND ND ~D ~D ~D Units ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l Report Limit Analyzed By ii. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK 53. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK 24. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK 21. 03/03/04 22:44 KSK 11. 03/03/04 22:44 K~K ii. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK ii. 03/03/04 22:44 KSK CAS No. 7005 72 3 86 73 7 534-52-1 101-55-3 118-74-1 87-86-5 85-01-8 120-12-7 84-74-2 206-44-0 129-00-0 85-68-7 91-94-1 56-55-3 218-01-9 117-81-7 117-84-0 205-99-2 207-08-9 50-32-8 193-39-5 53-70-3 191-24-2 67-72-1 Qual RegLmt Nitrobenzene-d5 (S) 90 % 03/03/04 22:44 KSK 4165-60-0 2-Fluorobiphenyl (S) 91 % 03/03/04 22:44 KSK 321-60-8 ~erphenyl-dl4 (s) Phenol-d6 (S) amet 2-Fluorophenol (S) 2,4,6-Tribromophenol (S) a Date Extracted A GC/MS Volatiles EIS Volatile GC/MS by 624 rs Chloromethane ShVinyl chloride on es Bromomethane Sre e Chloroethane 92 % 0 % CoI % 19 % a 03/01/04 wage Method: EPA 624 FlIPs RwEr 5.7 ug/l 1.0 2se~D 1.9 ~D 23B0 ug/l 1.0 ug/l 1.0 ug/l 1.0 03/03/04 22:44 KSK 1718-51-0 03/03/04 22:44 KSK 13127-88-3 2 Sema a 03/03/04 22:44 KSK 367-12-4 2 03/03/04 22:44 KSK 2 we 03/01/04 mm 02/27/04 04:57 RJS 02/27/04 04:57 RJS ae 02/27/04 04:57 RJS HEmeiannnad 02/27/04 04:57 RJS 74-87-3 75-01-4 74-83-9 75-00-3 Trichlorofluoromethane ND ug/l 1.0 02/27/04 04~57 RJS 75-69-4 Date: 03/11/~4 Page: 14 of 33 iS nelE ac: momen RREEPPOORRTT OOFF LLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'Thi~ r'epn~ shall n~t I~ r~pro~u~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00004477 aw rsoren 3M MN01539198 iceAAnnaallyyttiiccaall ee tn o Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.607,1700 Fax: 612.607.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test NT) i er SO i is Lab Sample No: 105362784 sev il Client Sample ID: E04-0126-67613 Sample Port Lead 4B Project Sample Number: 1085104-005 Matrix: Water Date Collected: 02/25/04 11:25 Date Received: 02/25/04 18:00 Sg lpn SOR n pilfm Parameters Methylene chloride re STE are I,i Dichloroethene Dame EZ nm mmmmowon trans-l,2-Dichloroethene Sn 2 OZ aes l,l-Dichloroethane Le Doom ammona Chloroform ri 22 0 Haenam l,l,l-Trichloroethane Fn EZ i fpsiehie Carbon tetrachloride = Doom amma Benzene 1,2-Diehloroethane fn $Z mma Trichloroethene Fer oom aman ne 1,2-Dichloropropane s meete E DE m ny mmmmmae anen Bromodichloromethane Results 3.1 ND ND ND ND ND ~D ~D 2.3 ND ~D ~D Units ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l Report Limit Analyzed By 1.0 02/27/04 04:57 RJS 1.0 02/27/04 04:57 RJS 1.0 02/27/04 04~57 RJS 1.0 02/27/04 04:57 RJS 1.0 02/27/04 04:57 RJS 1.0 02/27/04 04:57 RJS 1.0 02/27/04 04:57 RJS 1.0 02/27/04 04:57 RJS 1.0 02/27/04 04:57 RJS 1.0 02/27/04 04:57 RJS 1.0 02/27/04 04:57 RJS 1.0 02/27/04 04:57 RJS CAS No. 75 09 2 75 35 4 156-60-5 75-34-3 67-66-3 71-55-6 56-23-5 71-43-2 107-06-2 79-01-6 78-87-5 75-27-4 Qual RegLmt trans-l,3-Dichloropropene ~D ug/l 1.0 02/27/04 04:57 RJS 10061-02-6 Toluene ~D ug/l 1.0 eis-l,3-Diehloropropene ND ug/l 1.0 Sra Doom 1,1,2-Trichloroethane ND ug/l 1.0 Tetraehloroethene ND ug/l 1.0 fe Doom Dibromochloromethane ND ug/l 1.0 in 2 Zi Chlorobenzene ND ug/l 1.0 a oom Ethylbenzene ND ug/l 1.0 Sa PS Xylene (Total) ND ug/l 3.0 ne Doom Bromoform ND ug/l 1.0 oor WE EE l,l,2,2-Tetrachloroethane ND ug/l 1.0 Lp I 2 OB 1,3-Dichlorobenzene ND ug/l 1.0 1,4-Dichlorobenzene ~D ug/l 1.0 ho 2 Zi 1,2-Dichlorobenzene ~D ug/l 1.0 are 2 2B 2-chloroethylvinyl ether ND ug/l 5.0 Soar Lf Dibromofluoromethane (S) 129 % Toluene-d8 (S) 78 % WE na 4-Bromofluorobenzene (S) 106 % mA 1,2-Dichloroethane-d4 (S! 119 % 02/27/04 04:57 RJS 02/27/04 04:57 RJS ammo wen 02/27/04 04:57 RJS 02/27/04 04:57 RJS amma ma 02/27/04 04:57 RJS aan 02/27/04 04:57 RJS amma 02/27/04 04:57 RJS Eman 02/27/04 04:57 RJS aman ne 02/27/04 04:57 RJS EE 02/27/04 04:57 RJS mani 02/27/04 04:57 RJS 02/27/04 04:57 RJS imam 02/27/04 04:57 RJS EarEs 02/27/04 04:57 RJS Trad 02/27/04 04:57 RJS 02/27/04 04:57 RJS a 02/27/04 04:57 RJS PAs k va, 02/27/04 04:57 RJS i0~-8~-3 ~0061-01-5 79-00-5 127-18-4 124-48-I 108-90-7 100-41-4 1330-20-7 75-25-2 79-34-5 541-73-I 106-46-7 95-50-1 110-75-8 1868-53-7 2037-26-5 460-00-4 17060-07-0 Date: 03/11/04 ionhelHaec: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'Thi~ r'epn~ shall n~t I~ r~pro~u~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00004488 Page: 15 of 33 [pT 3M MN01539199 iceAAnnaallyyttiiccaall eto Pace Analytical Semices, Inc. en 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.607.1700 Fa~: 612.607.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test oe es i er SOE i cs 7 Lab Sample No: 105362792 rr il A Client Sample ID: E04-0126-67614 Comb Effluent 1/2 Project Sample Number: 1085104-006 Matrix: Water Date Collected: 02/25/04 11:37 Date Received: 02/25/04 18:00 agement on 85SmSer ei ifm iE Parameters Microbiology Results _ Uni_ ts Report Limit Analyzed By CAS No. Tm ome 14 egos Lattin Biochemical Oxygen Demand, 5 d Prep/Method: / SM 5210B i EEE csetss om t Smm . BOD, 5 day ND mg/l 6 03/02/04 JPHI Qual RegLmt 1 Date Prepared -- Wet Chemistry SL, re Phenolies Total. in Water enPhenol SI GC/MS Semivolatiles OL 625 wastewater GC/MS SVOA eyPhenol VR bis(2-Chloroethyl) ether So 2-Chlorophenol rm 1,3-Diehlorohenzene mee 1,4-Dichlorobenzene Filo 1,2-Dichlorobenzene mr bls(2-Chloroisopropyl) ether fide N-Nitroso-di-n-propylamine Le Nitrobenzene ps Isophorone fe2-Nitrophenol 3 ile 2,4-Dimethylphenol 02/26/04 10:30 wigs mingmit, re Method: EPA 420.4 ND ug/l 25.0 ima tin Prep/Method: EPA 625 / EPA 625 Din Bat ~D ug/l 10. CE ~D ug/l 10. PZ I ND ug/l ~o. 2 2 OF ND ug/l 10. Doom ND ug/l lo. EZ 5 ND ug/l lo. BL RL ~D ug/l i0. 2 2 OF ~D ug/l 10. Doom on ND ug/l i0. CIND ug/l i0. ERND ug/l i0. 22 23 ND ug/l i0. 02/26/04 10:30 mens wi 03/05/04 08:41 VAF 108-95-2 IE We 03/03/04 23:37 KSK dbo 03/03/04 23:37 KSK aman o~/o~/o4 23:37 KSK mE 03/03/04 23:37 KSK ema ens 03/03/04 23:37 KSK Dimi 03/03/04 23:37 KSK ae 03/03/04 23:37 KSK Unnan 03/03/04 23:37 KSK semana 03/03/04 23:37 KSK ons 03/03/04 23:37 KSK EE i 03103/04 23:37 KSK m guseiae ileen 03/03/04 23:37 KSK 108-95-2 111-44-4 95-57-~ 541-73-I 106-46-7 95-50-1 39638-32-9 621-64-7 98-95-3 78-59-1 88-75-5 105-67-9 bis(2-Chloroethoxy)methane 2,4-Dichlorophenol Jar. 1,2,4-Trichlorobenzene EANaphthalene Hexachloro-l,3-butadiene Dhogmde 4-Chloro-3-methylphenol me 2,4,6-Trichlorophenol a 2-Chloronaphthalene LoDimethylphthalate nim Acenaphthylene 2,6-Dinitrotoluene boAcenaphthene Et 2,4-Dinitrophenol Ty 4-Nitrophenol EL, 2,4-Dinitrotoluene an Diethylphthalate ND ug/l ND ug/l I 3 5 mania ND ug/l EZ bie NB ug/l NB ug/l 3 3 Lunes ND ug/l Doom on aman ~D ug/l EE ~D ug/l Doom seman ~D ug/l Ea ND ug/l ~D ug/l 2 2 heii ND ug/l FEE ~D ug/l EI lr ~D ug/l 2 2. thm ~D ug/l 2 Zk mies ND ug/l i0. 03103/04 23:37 KSK 111-91-1 10. 03/03/04 23:37 KSK 120-83-2 i0. 03/03/04 23:37 KSK 120-82-1 10. 03/03/04 23:37 KSK 91-20-3 i0. 03/03/04 23:37 KSK 87-68-3 i0. 03/03/04 23:37 KSK 59-50-7 i0. 03/03/04 23:37 KSK 88-06-2 i0. 03/03/04 23:37 KSK 91-58-7 i0. 03/03/04 23:37 KSK 131-11-3 10. 03/03/04 23:37 KSK 208-96-8 10. 03/03/04 23:37 KSK 606-20-2 i0. 03/03/04 23:37 KSK 83-32-9 51. 03/03/04 23:37 KSK 51-28-5 51. 03/03/04 23:37 KSK 100-02-7 i0. 03/03/04 23:37 KSK 121-14-2 i0. 03/03/04 23~37 KSK 84-66-2 Date: 03/11/04 Page: 16 of 33 ionhelHaec: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS This report shall not be reproduced, except in full, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00004499 [p-- 3M MN01539200 iceAAnnaallyyttiiccaall ee ton Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.607,1700 Fax: 612.507.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test oe es i er SOE i cs 7 Lab Sample No: 105362792 rr il A Client Sample ID: E04-0126-67614 Comb Effluent 1/2 Project Sample Number: 1085104-006 Matrix: Water Date Collected: 02/25/04 11:37 Date Received: 02/25/04 18:00 Rto ear meron cin 8188 pte ie EE Parameters rag i 4 Chlorophenyiphenyl ether oe 5 Tams Fluorene CEE gs & TAM mmmET nD 4,6-Dinitro-2-methylphenol ims 3 2 EF Donn 4-Bromophenylphenyl ether Lar Doom on semana Hexachlorobenzene bd ? 2 mms Pentachlorophenol [oe 2 ZB fuiasra Phenanthrene fea, 2B mein Anthracene Di-n-butylphthalate fr 2 IZ & dmmsaeud Fluoranthene bo Doom on amma Pyrene En --_-- Doom on naman ae Butylbenzylphthalate Spmewess EA paso nen 3,3'-Dichlorobenzidine Da : = EB amannad Ben~o(a)anthraeene i 2: 2 EF Fm Chrysene is BTA le Dmnu nes hls(2-Ethylhexyl)phthalate se PZ b&b faseeue Di-n-octylphthalate [a Doom aman Benzo(h)fluoranthene re PZ bE Hansa Benzo(k)fluoranthene es Doom on mama Benzo(a)pyrene Solow fo mmatean Indeno(l,2,3-cd)pyrene bi EN Ep 1 Dibenz(a,h)anthracene a 2 Zp tmeens Benzo(g,h,i)perylene feres I=BL anaI irai Hexachloroethane Results ND ND ~D ~D ~D ND ~D ND ~D ~D ~D ~D ND ND ~D ~D ~D ND ~D ND ~D ~D ~D ~D Units ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l Report Limit Analyzed By i0. 03/03/04 23:37 KSK i0. 03/03/04 23:37 KSK 51. 03/03/04 23:37 KSK i0. 03/03/04 23:37 KSK i0. 03/03/04 23:37 KSK 23. 03/03/04 23:37 KSK i0. 03/03/04 23:37 KSK i0. 03/03/04 23:37 KSK i0. 03/03/04 23:37 KSK i0. 03/03/04 23:37 KSK i0. 03/03/04 23:37 KSK i0. 03/03/04 23:37 KSK 20. 03/03/04 23:37 KSK 10. 03/03/04 23:37 K~K i0. 03/03/04 23:37 KSK i0. 03/03/04 23:37 KSK i0. 03/03/04 23:37 KSK i0. 03/03/04 23:37 KSK i0. 03/03/04 23:37 KSK i0. 03/03/04 23:37 KSK i0. 03/03/04 23:37 KSK 10. 03/03/04 23:37 KSK 10. 03/03/04 23:37 KSK 10. 03/03/04 23:37 KSK CAS No. 7005 72 3 86 73 7 534-52-1 101-55-3 118-74-1 87-86-5 85-01-8 120-12-7 84-74-2 206-44-0 129-00-0 85-68-7 91-94-1 56-55-3 218-01-9 117-81-7 117-84-0 205-99-2 207-08-9 50-32-8 193-39-5 53-70-3 191-24-2 67-72-1 Qual RegLmt Nitrobenzene-d5 (S) 79 % 03/03/04 23:37 KSK 4165-60-0 2-Fluorobiphenyl (S) 82 % 03/03/04 23:37 KSK 321-60-8 ~erphenyl-dl4 (s) Phenol-d6 (S) amet 2-Fluorophenol (S) 2,4,6-Tribromophenol (S) a Date Extracted A GC/MS Volatiles EIS Volatile GC/MS by 624 Srh s Chloromethane r Se e Vinyl chloride Bromomethane Chloroethane Trichlorofluoromethane 84 % 5 % HE19 % 47 % "a 03/01/04 03/03/04 23:37 KSK 1718-51-0 03/03/04 23:37 KSK 13127-88-3 2 Sema me 03/03/04 23:37 KSK 367-12-4 2 03/03/04 23:37 KSK 2 we 03/01/04 wep Method: EPA 624 S Beun mmwme 2.7 ug/l 1.0 02/27/04 05:24 RJS 74-87-3 s2 23B0 m Haimannna ~D ug/l 1.4 ug/l ~D ug/l ND ug/l 1.0 02/27/04 05:24 RJS 75-01-4 1.0 02/27/04 05:24 RJS 74-83-9 1.0 02/27/04 05:24 RJS 75-00-3 1.0 02/27/04 05~24 RJS 75-69-4 Date: 03/11/~4 Page: 17 of 33 iS nelE ac: momen RREEPPOORRTT OOFF LLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'Thi~ r'ep(:,~ shall n~t I~ r~pro~u~. ~ept i. f~ll, without th~ written consent of Pac~ ,a, nalytical Servi~e~, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00005500 p-- 3M MN01539201 iceAAnnaallyyttiiccaall ee tn o Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.607,1700 Fax: 612,507.6444 Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test oe es i er SOE i cs 7 Lab Sample No: 105362792 rr il A Client Sample ID: E04-0126-67614 Comb Effluent 1/2 Project Sample Number: 1085104-006 Matrix: Water Date Collected: 02/25/04 11:37 Date Received: 02/25/04 18:00 Satoei cpon EO81 8g urile fm Parameters Co , tcp teSue Jak gr S83 Methylene chloride re Pn amare I,i Dichloroethene Dame E Zu mmm trans-l,2-Dichloroethene Sn 2 OZ ane l,l-Dichloroethane Le Doom mmm Chloroform ri : 2 3 nam l,l,l-Trichloroethane Fn 2 ZB fpsaabie Carbon tetrachloride = Doom amma Benzene er ? ZB Bama 1,2-Diehloroethane fn FE ELE Trichloroethene Fer Doom aman ne 1,2-Dichloropropane se EI I mae Bromodichloromethane mete Dm mms on trans-l,3-Dichloropropene Results ND ND ND ND ND ND ~D ND ~D ~D ~D ~D ND Units ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l Report Limit Analyzed By 1.0 02/27/04 05:24 RJS 1.0 02/27/04 05:24 RJS 1.0 02/27/04 05~24 RJS 1.0 02/27/04 05:24 RJS 1.0 02/27/04 05:24 RJS 1.0 02/27/04 05:24 RJS 1.0 02/27/04 05:24 RJS 1.0 02/27/04 05:24 RJS 1.0 02/27/04 05:24 RJS 1.0 02/27/04 05:24 RJS 1.0 02/27/04 05:24 RJS 1.0 02/27/04 05:24 RJS 1.0 02/27/04 05:24 RJS CAS No. 75 09 2 75 35 4 156-60-5 75-34-3 67-66-3 71-55-6 56-23-5 71-43-2 107-06-2 79-01-6 78-87-5 75-27-4 10061-02-6 Qual RegLmt Toluene ND ug/l cls-l,3-Diehloropropene ~D ug/l Sra Doom am wen 1,1,2-Trlchloroethane ND ug/l Tetraehloroethene ~D ug/l fe Doom amma man Dibromochloromethane ND ug/l in 2 Zi aan Chlorohenzene ~D ug/l a Doom amma wen Ethylbenzene ND ug/l Sa PS Him Xylene (Total) ND ug/l ne Doom mma nen Bromoform ~D ug/l oor WE EEOELE l,l,2,2-Tetrachloroethane ~D ug/l Lp I 2 BH gman 1,3-Dichlorobenzene ~D ug/l 1,4-Dichlorobenzene ~D ug/l ho 2 Zi maim 1,2-Dichlorobenzene ~D ug/l are 2 2B EAEEL 2-chloroethylvinyl ether ND ug/l Soar f Srna Dibromofluoromethane (S) 127 % Toluene-d8 (S) 73 % WE nw a 4-Bromofluorobenzene (S) 103 % mA SE Saar va, 1,2-Dichloroethane-d4 (S! 117 % 1.0 02/27/04 05:24 ~JS i09-9~-3 1.0 02/27/04 05:24 ~JS i0061-01-5 1.0 02/27/04 05:24 RJS 79-00-5 1.0 02/27/04 05:24 RJS 127-18-4 1.0 02/27/04 05:24 RJS 124-48-1 1.0 02/27/04 05:24 RJS 108-90-7 1.0 02/27/04 05:24 RJS 100-41-4 3.0 02/27/04 05:24 RJS 1330-20-7 1.0 02/27/04 05:24 RJS 75-25-2 1.0 02/27/04 05:24 RJS 79-34-5 1.0 02/27/04 05:24 RJS 541-73-I 1.0 02/27/04 05:24 RJS 106-46-7 1.0 02/27/04 05:24 RJS 95-50-1 5.0 02/27/04 05:24 RJS 110-75-8 02/27/04 05:24 RJS 1868-53-7 02/27/04 05:24 RJS 2037-26-5 02/27/04 05:24 RJS 460-00-4 02/27/04 05:24 RJS 17060-07-0 Date: 03/11/04 ionhelHaec: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'Thi~ r'ep(:,~ shall n~t I~ r~pro~u~. ~ept i. f~ll, without th~ written consent of Pac~ ,a, nalytical Servi~e~, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00005511 Page: 18 of 33 aw rsenez 3M MN01539202 iceAAnnaallyyttiiccaall eto Pace Analytical Semices, Inc. en 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.60Z 1700 Fa~: 612.607.6444 oe Lab Sample No: 105362800 TT Client Sample ID: E04-0126-67622 azar Parameters Microbiology Tm ome 14 Biochemical Oxygen Demand, 5 d vein BOD, 5 day EEE Date Prepared -- Wet Chemistry SL, re Phenolies Total. in Water enPhenol SI GC/MS Semivolatiles OL 625 wastewater GC/MS SVOA eyPhenol Pr bis(2-Chloroethyl) ether So 2-Chlorophenol rm 1,3-Diehlorohenzene mee 1,4-Dichlorobenzene Filo 1,2-Dichlorobenzene mr bls(2-Chloroisopropyl) ether fide N-Nitroso-di-n-propylamine Le Nitrobenzene ps Isophorone fe2-Nitrophenol 3 2,4-Dimethylphenol ile bis(2-Chloroethoxy)methane 2,4-Dichlorophenol jar. 1,2,4-Trichlorobenzene EANaphthalene Hexachloro-l,3-butadiene Dhogmde 4-Chloro-3-methylphenol 2,4,6-Trichlorophenol a 2-Chloronaphthalene LoDimethylphthalate nim Acenaphthylene 2,6-Dinitrotoluene boAcenaphthene Et 2,4-Dinitrophenol Ty 4-Nitrophenol EL, 2,4-Dinitrotoluene an Diethylphthalate Lab Project Number: 1085104 ITI ir Client Project ID; E04-0126 CG Carbon System Test rt in i eirlSO i is Field Blank Project Sample Number: 1085104-007 Matrix: Water Date Collected: 02/25/04 12:00 Date Received: 02/25/04 18:00 mon 85SmSer ei ifm iE Results _ Uni_ ts Report Limit Analyzed By CAS No. Qual RegLmt egos Lattin Prep/Method: / SM 5210B csetss om t Smm . ND mg/l 6 03/02/04 JPHI 1 02/26/04 10:30 02/26/04 10:30 wigs mingmit, Method: EPA 420.4 ND ug/l re mens wi 25.0 03/05/04 08:41 VAF 108-95-2 ima tin Prep/Method: EPA 625 / EPA 625 Dinas Ie ws ~D ug/l ii. 3 ob Limam ~D ug/l ii. P 2 Imma ND ug/l ~. 2 2 0 Fem ND ug/l ii. Doom on pemim ens ND ug/l ii. PE ZL Hanes ND ug/l ii. BL RL Se ~D ug/l ii. 2 2 FE Ghani ~D ug/l ii. Doom on amin a ND ug/l ii. CI one ND ug/l ii. ER Et ND ug/l n. 2 2 memes ND ug/l ii. 2 3b guile ND ug/l ii. ND ug/l ii. I 3b maaan ND ug/l ii. EZ nei NB ug/l ii. NB ug/l ii. 3 IL umes ND ug/l ii. ~D ug/l ii. 2: Zp Hamman ~D ug/l ii. Doom semEia s ~D ug/l ii. 03/09/04 20:36 KSK 03/09/04 20:36 KSK o~IO9/O4 20:36 KSK 03/09/04 20:36 KSK 03/09/04 20:36 KSK 03/09/04 20:36 KSK 03/09/04 20:36 KSK 03/09/04 20:36 KSK 03/09/04 20:36 KSK 03/09/04 20:36 KSK 03/09/04 20:36 KSK 03/09/04 20:36 KSK 03/09/04 20:36 KSK 03/09/04 20:36 KSK 03/09/04 20:36 KSK 03/09/04 20:36 KSK 03/09/04 20:36 KSK 03/09/04 20:36 KSK 03/09/04 20:36 KSK 03/09/04 20:36 KSK 03/09/04 20:36 KSK 108-95-2 111-44-4 95-57-~ 541-73-I 106-46-7 95-50-1 39638-32-9 621-64-7 98-95-3 78-59-1 88-75-5 105-67-9 ii1-91-I 120-83-2 120-82-1 91-20-3 87-68-3 59-50-7 88-06-2 91-58-7 131-11-3 ND ug/l ~D ug/l 2 2 iad ND ug/l 2 2 imams ~D ug/l EI lr ~D ug/l 2 ZL Sammie ~D ug/l 2 ZL anes ND ug/l ii. 03/09/04 20:36 KSK 208-96-8 ii. 03/09/04 20:36 KSK 606-20-2 ii. 03/09/04 20:36 KSK 83-32-9 55. 03/09/04 20:36 KSK 51-28-5 55. 03/09/04 20:36 KSK 100-02-7 ii. 03/09/04 20:36 KSK 121-14-2 ii. 03/09/04 20~36 KSK 84-66-2 Date: 03/11/04 Page: 19 of 33 ionhelHaec: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'Thi~ r'epn~ shall n~t b~ r~pro~u~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00005522 awisons 3M MN01539203 iceAAnnaallyyttiiccaall ee ton Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.607,1700 Fax: 612.607.6444 oe i IerTSIO i iis r Lab Sample No: 105362800 TT rt in il Client Sample ID: E04-0126-67622 Field Blank Rto ear meetr e fin 8188 ge ie EE Parameters rg i 4 Chlorophenyiphenyl other oe 5D Lam=Es Fluorene CEE gs & Th mmEam nD 4,6-Dinitro-2-methylphenol ims 3 2 EF Donan 4-Bromophenylphenyl ether Lar Doom on semis Hexachlorobenzene bd ? 2 Laas Pentachlorophenol [oe 2 ZL fades Phenanthrene fea, 2D mammal Anthracene Di-n-butylphthalate fr 2 2 mamas Fluoranthene bo Doom on pmmam ou Pyrene En --_-- Doom on naman me Butylbenzylphthalate Spmewess EA naan wen 3,3'-Dichlorobenzidine Da : 2 ammnih Benzo(a)anthraeene i 2 2 0 JmmErs Chrysene is BTA Dm meas hls(2-Ethylhexyl)phthalate se PZ Lb Fame Di-n-octylphthalate [a Doom on pamim wa Benzo(b)fluoranthene re PZ Basa Benzo(k)fluoranthene es Doom on aamnm we Benzo(a)pyrene Solow Lf ob Tmahean Indeno(l,2,3-cd)pyrene bi EM JE a 15 Dibenz(a,h)anthracene a 2 2 Lmmes Benzo(g,h,i)perylene feres I5 Lume irias Hexachloroethane Results ND ND ND ND ND ND ND ND ND ND ND ND ND ND ~D ~D ~D ND ~D ND ND ~D ~D ~D Lab Project Number: 1085104 Client Project ID; E04-0126 CG Carbon System Test Project Sample Number: 1085104-007 Matrix: Water Date Collected: 02/25/04 12:00 Date Received: 02/25/04 18:00 Units ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l Report Limit Analyzed By ii. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK 55. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK 25. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK 22. 03/09/04 20:36 KSK 11. 03/09/04 20:36 KSE ii. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK ii. 03/09/04 20:36 KSK CAS No. 7005 72 3 86 73 7 534-52-1 101-55-3 118-74-1 87-86-5 85-01-8 120-12-7 84-74-2 206-44-0 129-00-0 85-68-7 91-94-1 56-55-3 219-01-9 117-81-7 117-84-0 205-99-2 207-08-9 50-32-8 193-39-5 53-70-3 191-24-2 67-72-1 Qual ReqLmt Nitrobenzene-d5 (S) 73 % 03/09/04 20:36 KSK 4165-60-0 2-Fluorobiphenyl (S) 82 % 03/09/04 20:36 KSK 321-60-8 Terphenyl-dl4 (S) Phenol-d6 (S) amet 2-Fluorophenol (S) 2,4,6-Tribromophenol (S) a Date Extracted A GC/MS Volatiles EAI Volatile GC/MS by 624 rs Chloromethane ShVinyl chloride on es Bromomethane Sae e Chloroethane 95 % 77 % 5 73 % 80 % Cs 03/01/04 wap Method: EPA 624 per ~D ug/l 1.0 EZ 3 ~D ug/l 1.0 Doom ~D ug/l 1.0 22 23B4 ND ug/l 1.0 03/09/04 20:36 KSK 03/09/04 20:36 KSK Sn 03/09/04 20:36 KSK 03/09/04 20:36 KSK wh 03/01/04 Vn 1718-51-0 13127-88-3 367-12-4 mn fn 02/27/04 05:51 RJS ummm 02/27/04 05:51 RJS amma ne 02/27/04 05:51 RJS Hadmaannna 02/27/04 05:51 RJS 74-87-3 75-01-4 74-83-9 75-00-3 Trichlorofluoromethane ~D ug/l 1.0 02/27/04 05~51 RJS 75-69-4 Date: 03/11/~4 Page: 20 of 33 iS nelE ac: momen RREEPPOORRTT OOFF LLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'Thi~ r'epn~ shall n~t I~ r~pro~u~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00005533 aw rsenos 3M MN01539204 iceAAnnaallyyttiiccaall ee tn o Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.607,1700 Fax: 612.507.6444 oe i IerTSO I i iis r Lab Sample No: 105362800 TT rt in il Client Sample ID: E04-0126-67622 Field Blank Sig ion Om 81 o pilfn m Parameters Co , tcp te Sue Jak i 83 Methylene chloride re Pn oamerw I,i Dichloroethene Dame E Zu mmmmaaon trans-l,2-Dichloroethene Sn 2 OZ Laan l,l-Dichloroethane Le oom mmm on Chloroform ri PZ 0 faianam l,l,l-Trichloroethane Fn 2 Zi fpsiabie Carbon tetrachloride = Doom mmm Benzene er ? ZB ama 1,2-Diehloroethane fn 2 ZW amma Trichloroethene Fer Doom amma ne 1,2-Dichloropropane se EI I ae Bromodichloromethane mete Dm ny mmmmue nn trans-l,3-Dichloropropene Results ND ND ~D ~D ~D ND ~D ND ND ~D ~D ~D ~D Lab Project Number: 1085104 Client Project ID; E04-0126 CG Carbon System Test Project Sample Number: 1085104-007 Matrix: Water Date Collected: 02/25/04 12:00 Date Received: 02/25/04 18:00 Units ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l us/l ug/l ug/l Report Limit Analyzed By 1.0 02/27/04 05:51 RJS 1.0 02/27/04 05:51 RJS 1.0 02/27/04 05~51 RJS 1.0 02/27/04 05:51 RJS 1.0 02/27/04 05:51 RJS 1.0 02/27/04 05:51 RJS 1.0 02/27/04 05:51 RJS 1.0 02/27/04 05:51 RJS 1.0 02/27/04 05:51 RJS 1.0 02/27/04 05:51 RJS 1.0 02/27/04 05:51 RJS 1.0 02/27/04 05:51 RJS 1.0 02/27/04 05:51 RJS CAS No. 75 09 2 75 35 4 156-60-5 75-34-3 67-66-3 71-55-6 56-23-5 71-43-2 107-06-2 79-01-6 78-87-5 75-27-4 10061-02-6 Qual RegLmt Toluene cls-l,3-Diehloropropene Sra l,l,2-Trlchloroethane Tetrachloroethene fe Dibromochloromethane in Chlorohenzene a Ethylbenzene SaXylene (Total) neBromoform m Lpes l,l,2,2-Tetrachloroethane ND ug/l 1.0 ND ug/l 1.0 Doom ND ug/l 1.0 ~D ug/l 1.0 Doom ~D ug/l 1.0 2 Zi ~D ug/l 1.0 oom ND ug/l 1.0 PS ~D ug/l 3.0 Doom ~D ug/l 1.0 3I B 2 OBH ~D ug/l 1.0 02/27/04 05:51 ~JS 02/27/04 05:51 ~JS amma wen 02/27/04 05:51 RJS 02/27/04 05:51 RJS aman man 02/27/04 05:51 RJS amnus 02/27/04 05:51 RJS aman 02/27/04 05:51 RJS Emam 02/27/04 05:51 RJS mma ne 02/27/04 05:51 RJS m gmEmana ia 02/27/04 05:51 RJS I08-8S-3 i0061-01-5 79-00-5 127-18-4 124-48-1 108-90-7 100-41-4 1330-20-7 75-25-2 79-34-5 1,3-Dichlorobenzene 1,4-Dichlorobenzene ho 2 Zi maaan 1,2-Dichlorobenzene are 2 2B Hanmi 2-chloroethylvinyl ether mid Sradam Dibromofluoromethane (S) Toluene-d8 (S) We en an 4-Bromofluorobenzene (S) Prien 2 Saar va, 1,2-Dichloroethane-d4 (S! ND ug/l ~D ug/l ND ug/l ~D ug/l 119 % 106 % 105 % 114 % 1.0 02/27/04 05:51 RJS 541-73-I 1.0 02/27/04 05:51 RJS 106-46-7 1.0 02/27/04 05:51 RJS 95-50-1 5.0 02/27/04 05:51 RJS 110-75-8 02/27/04 05:51 RJS 1868-53-7 02/27/04 05:51 RJS 2037-26-5 02/27/04 05:51 RJS 460-00-4 02/27/04 05:51 RJS 17060-07-0 Date: 03/11/04 ionhelHaec: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'Thi~ r'epn~ shall n~t I~ r~pro~u~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00005544 Page: 21 of 33 [p-- 3M MN01539205 aceAAnnaallyyttiiccaall esteon, Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Frewne: 612a607170 Minneapolis, MN 55414 Phone: 612.607,1700 Fax: 612.607.6444 Lab Project Number: 1085104 BLIER Se win irason Client Project ID; E04-0126 CG Carbon System Test ET PARAMETER FOOTNOTES J . ND Not detected at or above adjusted reporting limit NC Not Calculable ee he posh id ton ts sk ee he id i J Estimated concentration above the adjusted method detection limit and below the adjusted reporting limit I Deters MDL Adjusted Method Detection Limit Sa Surrogate Bs sr st titeson oat svt a rine Sinn smite Ill The BOD dilution blank QC criterion was not met. Acceptable method performance is based upon the remaining mr batch QC. OE, The surrogate recovery was outside of acceptance limits. Date: 03/11/~4 ionhelAtaec,: momen RREEPPOORRTT OOFF LLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'This r'epn~ shall rio'( I~e repro~ucs~, ~ept i. f~ll, without ths written consent of Pace ,a, nalytieal Services, Inc. CSONEFIDE-NSTUBIIAECLT T0 A PROTECTIVE OROER ENTERED CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00005555 Page: 22 of 33 au orssszos 3M MN01539206 iceAAnnaallyyttiiccaall eto Pace Analytical Services, Inc. 1700 Elm Slreet, Sm'te 200 Ee Minneapolis, MN 55414 IT Phone: 612.607,1700 Fax: 612.507.6444 QQUUAALLIITTYY CCOONNTTRROOLL DDAATTAA rm rotsnpcte OOO QC Batch: 104879 5 Th QC Batch Method: EPA 625 Lab Project Number; 1085104 Client Project ID: E04-0126 CG Carbon System Test Analysis Method: EPA 625 Analysis Description: 625 Wastewater GC/MS SVOA Associated Lab Samples: 105362743 105362750 105362768 105362776 105362784 105362792 105362800 METHOD BLANK: 105373757 Associated Lab Samples: pen htesh aun Parameter pa es S3e g=h 5 Phenol 105362743 Units us/l 105362750 105362768 105362776 Blank Result ND Reporting Limit Footnotes i0. niepwo.d bis(2-Chloroethyl) ether us/l 2-Chlorophenol ug/l 1,3-Dichlorobenzene ug/l 1,4-Dichlorobenzene ug/l 2SEJND 10. ND i0. ND i0. ND 10. bb1il,se2(i-2aD--iCCchhhlilooorrroooithseeeonppzrreoonppeyyll)) eetthheerr nemo N-Nitroso-di-n-propylamine Le Nitrobenzene fie Isophorone tl 2-Nitrophenol St 2,4-Dimethylphenol HE bis(2-Chloroethoxy)methane J 2,4-Dichlorophenol uuuggg///lll NNDD 1i1000..0 worn ug/l ND i0. FOug/l ND i0. 2 =: = ug/l ND i0. EAug/l ND i0. EAug/l ND i0. WL OX ug/l ND i0. worn ug/l ND i0. 1,2,4-Trichlorobenzene ug/l ND i0. Sianaty Naphthalene Nexachloro-l,3-butadiene 4-Chloro-3-methylphenol EEE ug/l ND i0. ug/l ND i0. ug/l ND i0. 2,4,6-Trichlorophenol ug/l ND i0. 2-Chloronaphthalene ug/l ND I woe Dimethylphthalate ug/l ND i0. Sa EE Acenaphthylene ug/l ND i0. 2,6-Dinitrotoluene ug/l ND i0. Tr EA Acenaphthene ug/l ND i0. 2,4-Dinitrophenol ug/l ND 50. 4-Nitrophenol ug/l ND 50. Lee ee 2FE 2 1 2,4-Dinitrotoluene ug/l ND i0. Diethyiphthalate us/l ND 4-Chlorophenylphenyl ether us/l ND i0. Fluorene us/l ND i0. 105362784 105362792 1053628G0 Date: 03/11/~4 Page: 23 of 33 ionhelAtaec,: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'This r'epn~ shall n~t I~ r~pro~ucs~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00005566 aw rsenor 3M MN01539207 iceAAnnaallyyttiiccaall eto Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Ee Minneapolis, MN 55414 MiIgs dTois Phone: 612.607,1700 Fax: 612.507.6444 QQUUAALLIITTYY CCOONNTTRROOLL DDAATTAA ------------rot-- snpcte--O--O-- O METHOD BLANK: 105373757 Lab Project Number; 1085104 Client Project ID: E04-0126 CG Carbon System Test Associated La5 Samples: 105362743 donne bdte StoErtie pe Parameter mmm 4,6-Dinitro-2-methylphenol DT 4-Bromophenylphenyl ether Site EE Hexachlorobenzene a RE Pentachlorophenol fe woe ow Phsnanthrene oy 2 3: = Anthracene Pres = 2 I Di-n-butylphthalate er EE Fluoranthene foWOEmoorSE Pyrene Units ug/l ug/l ug/l us/l u~/l u~/l u~/l u~/l ug/l 105362750 105362768 105362776 Blank Result HD HD ND ND ND ND ND ND ND Reporting Limit 50. i0. 10. 23. 10. 10. 10. 10. 10. Footnotes 105362784 105362792 105362800 Butylbenzylphthalate ug/l ND i0. 3,3'-Dichlorobenzid~ne ug/l ND 20. ChBCrehnryzyssose(nnaee)anthracene uuuggg///lll NNwDD 11i000..0 She 3 L bis(2-Ethylhexyl)phthalate ug/l ND i0. Di-n-octylphthalate ug/l ND i0. dene 2 i Benzo(b)fluoranthene ug/l ND i0. aaI NE BA Benzo(k)fluoranthene ug/l ND i0. oe EA Benzo(a)pyrene ug/l ND i0. EEC Indeno(l,2,3-d)pyrene ug/l ND 10. idl SEE Dibenz(a,h)anthracene ug/l ND i0. Benzo(g,h,i)perylene ug/l ND i0. a wor Hexachloroethane ug/l HD i0. Nitrobenzene-d5 (S) % 79 memmesd 2 2-Fluorobiphenyl (S) % 81 mn : 3 Terphenyl-dl4 (S) % Phenol-d6 (S) % 82 Lt : : 2-Fluorophenol (S) % 78 2,4,6-Tribromophenol (S) % 84 LABORATORY CONTROL SAMPLE: 105373765 rr. Giff Parameter E i en me Phenol Units us/l bis(2-Chloroethyl) ether us/l we oH Spike ie Sp Cone. 2f2g 2i Esg 50.00 LCS Result 42.51 LCS % Rec 85 50.00 41.58 83 rite Footnotes Date: 03/11/04 Page: 24 of 33 ionhelAtaec,: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'This r'epn~ shall n~t I~ r~pro~ucs~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00005577 aw rsonon 3M MN01539208 ceAAnnaallyyttiiccaall eto Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Ee Minneapolis, MN 55414 eIn 2T60 Phone: 612.607,1700 Fax: 612.507.6444 QQUUAALLIITTYY CCOONNTTRROOLL DDAATTAA --------------------------ro--tsn--pct--e ----O--O--O---- LABORATORY CONTROL SAMPLE: 105373765 pene S woe S 5 pe Parameter Units Lab Project Number; 1085104 Client Project ID: E04-0126 CG Carbon System Test Spike Cone. LCS Result LCS % Rec Footnotes 2-Chlorophenol 1,3-Dichlorobenzene Gimmes 1,4-Dichlorobenzene eS, 1,2-Dichlorobenzene ie bis(2-Chloroisopropyl) ether Spi. N-Nitroso-di-n-propylamine fred Nitrobenzene Jn Isophorone el 2-Nitrophenol EL2,4-Dimethylphenol meee bis(2-Chloroethoxy)methane us/l 50.00 41.34 83 ug/l 50.00 39.64 79 om oue ua 3 ug/l 50.00 40.08 80 haa ug/l 50.00 40.57 81 0 S272 us/l 50.00 43.03 86 of BR oan us/l 50.00 43.87 88 2 Miso u~/l 50.00 45.23 90 2 sais us/l 50.00 44.35 89 ERus/l 50.00 40.51 81 Zhen, ug/l 50.00 16.12 32 1 WE uw mx ug/l 50.00 42.95 86 2,4-Diehlorophenol ug/l 50.00 39.97 90 N1aa,gp2hh,tt4hh-aaTllreeinneeshlorobenzene inte SR iE 1 Nexachloro-l,3-butadlene idl SE 4-Chloro-3-meth1phenol 2,4,6-Trichlorophenol II 2-Chloronaphthalene oR SS Dimethylphthalate a moun ose Acenaphthylene ie 5 Bui 2,6-Dinitrotoluene Ns 2 hha os Acenaphthene rm EI 2,4-Dinitrophenol wuas/nl us/l ug/l us/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l s50n.0o0 3a9.698 580 50.00 41.60 83 50.00 42.62 85 50.00 43.14 86 50.00 41.26 82 50.00 44.07 88 50.00 45.04 90 50.00 44.17 88 50.00 44.25 88 50.00 43.78 88 50.00 30.01 60 4-Nitrophenol 2,4-Dinitrotoluene Li Diethylphthalate on 4-Chlorophenylphenyl ether neFluorene ooSNE 4,6-Dinitro-2-methylphenol Gomme 4-Bromophenylphenyl ether a Hexachlorobenzene Soar Pentachlorophenol es Phenanthrene ronAnthracene Di-n-butylphthalate ion Fluoranthene hePyrene ug/l 50.00 39.86 80 ug/l 50.00 41.91 84 AE ug/l 50.00 42.08 84 SERA ug/l 50.00 44.50 89 moun ou ug/l 50.00 45.01 90 EE NS ug/l 50.00 34.83 70 wo nE oun) ug/l 50.00 46.48 93 EA us/l 50.00 47.58 95 2 isso ug/l 50.00 25.06 50 1 EEug/l 50.00 43.99 88 2 Agios ug/l 50.00 45.12 90 us/l 50.00 46.00 92 2 uz us/l 50.00 46.88 94 ag iah us/l 50.00 42.96 86 Date: 03/11/04 Page: 25 of 33 ionhelAtaec,: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'This r'epn~ shall n~t I~ r~pro~ucs~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00005588 aw rsenon 3M MN01539209 iceAAnnaallyyttiiccaall ee tn o Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 a IT Phone: 612.607,1700 Fax: 612.507.6444 QQUUAALLIITTYY CCOONNTTRROOLL DDAATTAA -- --------ro-- tsnpcte -- OO-- O LABORATORY CONTROL SAMPLE: 105373765 Lab Project ttumber; 1085104 Client Project ID: E04-0126 CG Carbon System Test pene SS Parameter mE NCU a Butylbenzylphthalate 3,3'-Dishlorobenzidine Lon EC Benzo(a)anthracene ne 5 uo: Chrysene Units us/l ug/l ug/l ug/l Spike Cons. 50.00 50.00 50.00 50.00 LCS Result 43.22 27.07 44.03 44.37 LCS % Rsc 86 54 88 89 pe Footnotes bis(2-Ethylhexyl)phthalata us/l Di-n-oetylphthalate us/l a AE Benzo(b)fluoranthene us/l juke 2 Benzo(k) fluoranthene us/l an ER Benzo(a)pyrene us/l rn I Indeno(l,2,3-cd)pyrene ug/l Tony Z Dibenz(a,h)anthracene ug/l ebipeis 3 Ben~o(g,h,~)perylene ug/l 50.00 43.75 88 Badr 50.00 41.74 84 50.00 42.91 86 50.00 45.12 90 nfaadeo 50.00 42.59 85 50.00 44.18 88 50.00 44.76 90 50.00 44.21 99 HWeixtarcohbloonrsoaenteh-aan5e (5) us/l Nitrobenzene-d5 (S) fm, 2-Fluorohiphenyl (S) rd Terphenyl-dl4 (S) LY Phenol-d6 (S) TA 2-Fluorophenol (S) FR. 2,4,6-Tribromophenol (S) :i2ii :50.00 41.51 83 86 86 89 86 80 88 Date: 03/11/~4 or, inelac: REPORT OF LABORATORY ANALYSIS REPORT OF LABORATORY ANALYSIS momen 'This r'epn~ shall n~t I~ r~pro~ucs~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00005599 Page: 2~ of 33 [pT 3M MN01539210 iceAAnnaallyyttiiccaall ee tn o Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 RaIi nTd Phone: 612.607,1700 Fax: 612.607.6444 QQUUAALLIITTYY CCOONNTTRROOLL DDAATTAA rm rotsnpcte OOO QC Batch: 104706 TE En QC Batch Method: EPA 624 Lab Project ttumber; 1085104 Client Project ID: E04-0126 CG Carbon System Test Analysis Method: EPA 624 Analysis Description: Volatile GC/MS by 624 Associated Lab Samples: 105362743 105362750 105362768 105362776 105362784 105362792 105362800 METBOD BLANK: 105362867 Associated Lab Samples: pen htesh aun Parameter Si he FaE= a7 Chloromethane 105362743 Units u~/l 105362750 105362768 105362776 Blank Result ND Reporting Limit Footnotes 1.0 Vinyl chloride us/l ND 1.0 Bromomethane ug/l ND 1.0 mm a i Chloroethane ug/l ND 1.0 tm 2 E 2 Trichlorofluoromethane ug/l ND 1.0 E- i Methylene chloride u~/l ND 1.0 ms ei 2s i l,l-Dichloroethene us/l ND 1.0 Re ZOE 3 trans-l,2-Dichloroethene ug/l ND 1.0 fe 2: i l,l-Dichloroethane ug/l ND 1.0 oy 2 = 2 Chloroform ug/l ND 1.0 SEne AE i l,l,l-Trichloroethane ug/l ND 1.0 hee 8 i Carbon tetrachloride ug/l ND 1.0 fea IEE i Benzene ug/l ND 1.0 i wo 1,2-Dichloroethane ug/l ND 1.0 an F- 2 Trichloroethene ug/l ND 1.0 mame 32 i 1,2-Dichloropropane ug/l ND 1.0 Bromodichloromethane ug/l ND 1.0 pane 22 i trans-l,3-Dichloropropene ug/l ND 1.0 frie, a i Toluene ug/l ND 1.0 cis-l,3-Dichloropropene ug/l ND 1.0 Smee m2 i l,l,2-Trichloroethane ug/l ND 1.0 by COE i Tetrachloroethene ug/l ND 1.0 Dibromochloromethane ug/l ND 1.0 on 2 i Chlorobenzene u~/l ND 1.0 Sa a i Ethylbenzene ug/l ND 1.0 ne nn a Sa ii Xylene (Total) ug/l ND 3.0 r Lut ma 2 ii Bromoform ug/l ND 1.0 l,l,2,2-Tetrachloroethane us/l ND 1.0 1,3-Dichlorobenzene us/l ND 1.0 1,4-Dichlorobenzene us/l ND 1.0 105362784 105362792 1053628G0 Date: 03/11/~4 Page: 27 of 33 ionhelAtaec,: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'This r'epn~ shall rio'( I~ r~pro~ucs~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00006600 p-- 3M MN01539211 iceAAnnaallyyttiiccaall eto Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Ee Minneapolis, MN 55414 MiIgs dTois Phone: 612.607,1700 Fax: 612.507.6444 QQUUAALLIITTYY CCOONNTTRROOLL DDAATTAA SoMETHOD BLANK: 105362867 rotsnpcte Lab Project Number; Client Project ID: Associated Lab Samples: done bdte StoErtie pe Parameter 1,2-Dichlorobenzene FT i 2-Chloroethylvinyl ether Sets = Dihromofluoromethane (S) 105362743 Units ug/l ug/l % 105362750 105362768 105362776 105362784 Blank Result ND HD 107 Reporting Limit Footnotes 1.0 5.0 Pgieiems, } = Toluens-d~ (S) % 104 4-Bromofluorobenzene (S) % 106 1,2-Dichloroethane-d4 (S) % 106 OOO 1085104 E04-0126 CG Carbon System Test 105362792 105362800 LABORATORY CONTROL SAMPLE: 105362875 i-- i ee oe Parameter pm a a se Chloromethane Ser 2 ne Vinyl chloride Bromomethane ite 2 No = Chloroethane GE WA hm Eu Trichlorofluoromethane a 5 pus Methylene chloride J ie moan oan om l,l-Diehloroethene in EE trans-l,2-Diehloroethene Sa 2 Wiz l,l-Dichloroethane an EE Chloroform l,l,l-Trichloroethane rN Re Carbon tetrachloride fred 5 mins Benzene nen EC 1,2-Diehloroethane Lm EA Trichloroethene ee 2 Dan % 1,2-Dichloropropane Units ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l ug/l Spike Cone. 20.00 20.00 20.00 20.00 20.00 20.00 20.00 20.00 20.00 20.00 20.00 20.00 20.00 20.00 20.00 20.00 LCS Result 21.65 20.88 27.46 23.23 20.62 21.55 20.16 22.50 20.02 20.88 20.65 20.71 20.39 20.79 20.53 20.59 LCS % Rec i08 104 137 116 103 108 101 113 100 104 103 104 102 104 103 103 Bromodichloromethane ug/l 20.00 20.55 103 em 5 trans-l,3-Dichloropropene ug/l Toluene ug/l cis-l,3-Dichloropropene ug/l i 20.00 20.99 105 20.00 20.32 102 20.00 20.24 101 1,1,2-Trichloroethane ug/l 20.00 21.08 105 sri Tetrachloroethene DDiibbrroosmoocchhlloozroommeetthhaannee Chlorobenzene ZA SS us/l 20.00 19.99 100 uugs//ll w20.w00 2a 1.29 110066 us/l 20.00 19.88 99 sits Pootnotes Date: 03/11/~4 Page: 28 of 33 ionhelAtaec,: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'This r'epn~ shall rio'( I~e repro~ucs~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00006611 aw mrseniz 3M MN01539212 iceAAnnaallyyttiiccaall ee tn o Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 a IT Phone: 612.607,1700 Fax: 612.507.6444 QQUUAALLIITTYY CCOONNTTRROOLL DDAATTAA ------------------------ro--ts--npc--te ----O--O--O ---- LABORATORY CONTROL SAMPLE: 105362875 Lab Project ttumber; 1085104 Client Project ID: E04-0126 CG Carbon System Test pene SE 5 Parameter Er a ee ae Ethylbenzene Xylene (Total) ne EC Bromoform mms I L222 l,l,2,2-Tetrachloroethane Piippuose o 28 22 1,3-Dichlorobenzsns hae RAE 1,4-Dichlorobenzsns gE EE 1,2-Dichlorobenzene Power. = RHE 2-Chloroethylvinyl ether en = DiSromofluoromethane (S) i 2 Toluene-d8 (S) mul i 4-Bromofluorobenzene (S) Units us/l ug/l ug/l ug/l us/l u~/l us/l u~/l Spike Conc. 20.00 60.00 20.00 20.00 20.00 20.00 20.00 20.00 LCS Result 20.32 61.60 19.80 23.73 20.16 20.2~ 20.70 22.99 LCS % Rec 102 103 99 119 i01 i01 104 115 104 96 97 pe Footnotes 1,2-Diehloroethane-d4 (S) 100 Date: 03/11/04 ionhelAtaec,: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'This r'epn~ shall n~t I~ r~pro~ucs~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00006622 Page: 29 of 33 aw mrsenra 3M MN01539213 iceAAnnaallyyttiiccaall ee tn o Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.607,1700 Fax: 612.507.6444 QQUUAALLIITTYY CCOONNTTRROOLL DDAATTAA rm rotsnpcte OOO QC Batch: 104728 P50 arate' QC Hatch Method: Lab Project Number; 1085104 Client Project ID: E04-0126 CG Carbon System Test Analysis Method: SM 5210B Analysis Description: Biochemical Oxygen Demand, Associated Lab Samples: 105362743 105362750 105362768 105362776 105362784 105362792 105362800 METHOD BLANK: 105364194 Associated Lab Samples: Hp r en 2shtesh SaEupny Parameter 105362743 Units 105362750 105362768 105362776 Blank Result Reporting Limit Footnotes 105362784 105362792 I053628G0 BOD, 5 day ms/l ND 6 2 ---------------------------------------------------- LABORATORY CONTROL SAMPLE: 105364202 dem E om S we 1% Parameter Hy He he BOD, 5 day Units mg/l Spike Cone. 198.00 LCS Result 201.0 LCS % Rec 102 Footnotes 2 SAMPLE DUPLICATE: 105364210 f eyee. iSe i Parameter BOD, 5 day Units mg/l ae 2p9 105360739 DUP Result Result RPD 3385 3181 6 pie Footnotes 2 Date: 03/11/~4 ionhelAtaec,: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'This r'epn~ shall rio'( I~e r~pro~ucs~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00006633 Page: 30 of 33 aw mrsente 3M MN01539214 ce Aniamliynteiscoanl Facehat soe, Pace Analvtical Services, Inc. Sh 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 Ie 257170 Phone: 612.607,1700 Testa Fax: 612.507.6444 Emme Qc Batch: 105063 Gc ato thd In 40.4 QC Batch Method: EPA 420.4 Reomiuted sphereTosni Associated Lab Samples: 105362743 105362792 QQUUAALLIITTYY CCOONNTTRROOLL DDAATTAA Cb prec mbes, 1851CH Lab Project ttumber; 1085104 hit procs To 340146 Cs Curbs apstem Test Client Project ID: E04-0126 CG Carbon System Test mwewse wan Analysis Method: EPA 420.4 Snsleis baeeiption, Hosatice otal. in tates Analysis Description: Phenollcs Total. in Water Some soi whee Se 105362750 105362768 105362776 105362784 METBOD BLANK: 105384945 Restated Lah Splens SHDO WSS seme ane usa Associated Lab Samples: memes mie d[eIl i--e-- mess Parameter = wn 0 ie Phenol 105362743 Units us/l 105362750 105362768 105362776 105362784 Blank Result ND Reporting Limit Footnotes 25.0 DELABORATORY = ome Parameter Phenol CONTROL SAMPLE: 105384952 mie cmhee slwer Units WATT Tees me ug/l Spike Cone. i000.00 LCS Result 1116 weLCS Sac mes % Rec Pootnotes 112 sam 105362792 MATRIK SPIKE: 105384960 =ome Parameter Phenol me ewamnt Gwoweo iseedwVie eta Units wo CT ee hes een ug/l 105362743 Result 0 Spike Cone. 1000.00 MS Result 598.5 MS % Rec Footnotes 60 1 SAMPLE DUPLICATE: 105384978 B =ossa mwnie el0s Parameter Phenol Units ug/l 105362750 Result ND l wB R DUP Result RPD ND NC fs Footnotes Date: 03/11/04 `onwela ac: Rm EPORT Om F LABORm ATORY . ANALYSIS REPORT OF LABORATORY ANALYSIS 'This r'epn~ shall rio'( I~e reproducs~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPRUROROTTT.EECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00006644 Page: 31 of 33 S_MNo1S39215 3M MN01539215 iceAAnnaallyyttiiccaall ee tn o Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 Minneapolis, MN 55414 fri Id T Phone: 612.607,1700 Fax: 612.507.6444 FO Qc Batch: 105064 SuTaERTS QC Batch Method: EPA 420.4 Associated Lab Samples: 105362800 -- i mBad METBOD BLANK: 105384986 Associated Lab Samples: 105362800 wm y s HSeito Parameter Phenol Units ug/l QQUUAALLIITTYY CCOONNTTRROOLL DDAATTAA rotsnpcte Lab Project ttumber; 1085104 Client Project ID: E04-0126 Pi Analysis Method: EPA 420.4 Analysis Description: Phenollcs Total. in Water OOO CG Carbon System Test vat tier Blank hie oS iain, Result 5ND Reporting Limit Footnotes 25.0 LABORATORY CONTROL SAMPLE: 105384994 Be om Eai Parameter Phenol Units ug/l i jen 4 sits Spike Cone. i000.00 LCS Result 1017 LCS % Rec 102 ~ootnotes MATRIX SPIKE: 105385009 p i en Er Parameter Phenol Units ug/l Ss ---- SAMPLE DUPLICATE: 105385017 oBu=r Ea Parameter Phenol Units ug/l wE o wmS . 105362800 Result Spike Cone. MS Result MS % Rec Footnotes 0 1000.00 1087 109 wim 105364046 Result a a ND DOP Result ND es RPD Footnotes ttC Date: 03/11/04 ionhelAtaec,: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'This r'epn~ shall rio'( I~e repro~ucs~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00006655 Page: 32 of 33 aw mrsents 3M MN01539216 aceAAnnaallyyttiiccaall esteon, Pace Analvtical Services, Inc. 1700 Elm Slreel, Sm'te 200 howe: 6126a071700 Minneapolis, MN 55414 Phone: 612.607,1700 Fax: 612.507.6444 Lab Project Number: 1085104 BLIER Se win irason Client Project ID; E04-0126 CG Carbon System Test one concn en ABER ToS QUALITY CONTROL DATA PARAMETER FOOTNOTES con in tn, td so rp kt 3 Consistent with EPA guidelines, unfounded concentrations are displayed and have been used to calculate % Rec and RPD values. 0 arn oes sore ton LCS (D) Cp mee MS (D) 3 ZT aHT mn DUP Laboratory Control Sample (Duplicate) Matrix Spike (Duplicate) Sample Duplicate D I DDiorabre wine ait te 8 ipa ac ND Not detected at or above adjusted reporting limit NC Not Calculable J Estimated concentration above the adjusted method detection limit and below the adjusted reporting limit MDL Adjusted Method Detection Limit RPD Relative Percent Difference BBaT ne ITNT onto i be te semi [1i] ThTShueerrmosygpatitkhee rreeccoovveerryy wwahse oouuttseiiddee ooff ascocceeppthaannccee lHiamtites.. [2] The BOD dilution blank QC criterion was not met. Acceptable method performance is based upon the remaining batch QC. Date: 03/11/~4 ionhelAtaec,: momen RREEPPOORRTTOOFFLLAABBOORRAATTOORRYY AANNAALLYYSSIISS 'This r'epn~ shall rio'( I~e repro~uce~, eept i. f~ll, without the written consent of Pace Analytical Services, Inc. CSONEFIDE-NSTUBIIAECLT T0 A PROTECTIVE OROER ENTERED CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00006666 Page: 33 of 33 aw orssszt? 3M MN01539217 FFlluuoorroocchheemmiiccaallss FFIINNAALL RREEPPOORRTT EEVVEENNTT 22 EE0044--00112266 FFeebbrruuaarryy 2255,, 22000044 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 1939.0067 3M MN01539218 XYos r ns hc.TSEARCH '.. Proven Results. AAnnaalylyttiiccaall RReeppoorrtt FFlluuoorroocchheemmiiccaall CChhaarraacctteerriizzaattiioonn ooff AAqquueeoouuss SSaammpplleess CCoottttaaggee GGrroovvee AAccttiivvaatteedd CCaarrbboonn SSyysstteemm FFCC MMoonniittoorriinngg ((EE0044--00112266)) EExxyyggeenn RReesseeaarrcchh LLaabboorraattoorryy RReeppoorrtt NNoo.. LL00000011995588 TTeessttiinngg LLaabboorraattoorryy ... EExxyyggeenn RReesseeaarrcchh ". 33005588 RReesseeaarrcchh DDrriivvee SSttaattee CCoolllleeggee,, PPAA 1166880011 Brian Mader "PProrojjeecctt LLeeaadd Brian Mader 33MM EEnnvviirroonnmmeentnatall,, HHeeaaltlthh,, aanndd SSaaffeettyy OOppereartaitioonnss: Buildin 0002-06-E.09 993355 BBuusshh AAvveennuuee Building 0002-03-E-09 PPOO BBooxx 3333333311 SStt., PPaauull,, MMNN 55551i,3333--33333311 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALUL-N- STSUUYBBDJJIEESCCTTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00006688 ~3058 Research Drive R3Ek sine Bleonn, usa A ~l~State College, PA 16801, USA PaceRgt aaa san PAGE ~: 80~.281.3219 Sa am, ~F: 814.272.1019 exygen.com m_morsaozta 3M MN01539219 11 IInnttrroodduuccttiioonn R(RoEesxsyuuglletssna)afrrreormereptpohorotr3tee1ddCfofootrriahthgeeeaGanrnaoalvlyyefsisaocoff.aaqquTueheeoouEusxsygsaaommnspptleussrernecuceemiivbveeoddrbabsyysEiEgxnxyeygdgeetnontFheReseposreaoarerccchht (sELxoycgoetne) sfaro.m the 3M Cottage Grove facility. The Exygen study number assigned to the project is.L0001958. `SS(ppLeecGciMifiScfMfolSuro)orecwchahesemmircoicqaaullecschthreaadracficteoerarzilzaatstiioaonmnpblbyeysq.liquuiAiddctcohthrarloommoafat2to3oggrsraaappmhhpyyle//fstaan(nddnoeimmmnmagassfsiseslsdppdeoucpctlrtiocmoateretsry,y Blanks,andspikes) oro 906od or analysis. (LC/MS/MS) was requested for all samples. A blanks, and spikes) were received for analysis. total of 23 samples (including field duplicates, Thosamples wero propre and analyzedbyLGMSAfoSr he folowing is of fuorochericals: The samples were prepared and analyzed by LC/MS/MS for the following list of fluorochemicals: Tabl 1:TargetAnas Table 1: Target Analysis CCoommppoouunndd Name Perfluorobutanesulfonate Perfiuorohexanesulfonate Foruorshexanot: Acid Perfluorooctanesulfonate Perfluorohexanoic Acid Perfluorooctanoic Acid ooom Acronym C4 Sulfonate (PFBSI C6 Sulfonate (PFHS/ C8 Sulfonate (PFOSI C6 Acid (PFHA) C8 Acid (PFOA) TTvhheeaaanlncalbliyctyicatEalxl ymemgeeetdnthh.ooddTsshueussveeadddwaewtreoreenporororiitggonincaalolllyadndedevrveeelsloouppleesddfarofoorrogngrrfooiuunnwdciwahlateEerxrsya,gsmaepmnlp.elOesnslaaynnddthwsweeCrree8 `qvSuSaauulltliifdootannytacaetotdeonatbanoynlddEcCCxey88mgAeeAcnncit.iddswTwehecreroelviacnellcidluuadidtieeotddnisiipnartntohhatooelocyorosriliiggsaninndaadellmmrmaeenestsuthhtltooasddtvaovarteachleaiodtnaaitpiofoipnlnei..IcwtaIittbshsihyEooxuh fyldgtebhbneoe.o1mneoO0ttendu hdlyoPtdthhttaeodttttChhh8eee adatonal anaes quality control elements additional analytes. included in this analysis demonstrate the applicability of the method to the 22 SSaammppllee RReecceeiipptt "tTTenheemwpwaetaretaerrtssuaoarmmfeplp0ele1sswCwo.errSeassmuupbblmmeiittsteowddeirinneppsaltassottoicdccaoontnt4taaiinneerrssr..oSmSarmaempclpoelpesstwweuenrtraeaarnecacloyeisivviees.ddooTnnwwewenetktycicoeavatct eaa intirneecdmchievpdiiedvureuaadaltluocrcneoon2nto2tafa6ii1n0n0e.e1r4rs.sCCw.whoeraSreanmrroepcccleaeusnisveetwddo.e.dryFeiFiosineltfoldodrrsemsadaamtmpaioltpnel4esisCpwrweforesorromednCicroooedllcleoenccipteAetdduaonoctnnilh2a22en/25an5l0y/0C!s4.4is...SSaTawmmeppnletys-wtwhererereee received on 2J26/04. Chain-of-custody information is presented in Attachment C. 33 HHoollddiinngg TTiimmeess 1FFaiiekldd90aanndddayalsab.booSrraaattmorrpyylsssppwiikkoeerssooaofnf atthlheyeszseeedfwfluoiorhroiocnchh3ae0mmciaiccyaaslssofhhcaaovvloeocssthhooonww.nn stabfo stability for periods periods crear greater than 90 days, Samples were analyzed within 30 days oi collection. | `CHGEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00006699 pacezcrs PAGE2 OF5 3M_MNO1539220 3M MN01539220 44 MMetehthooddss -- AAnnalyaticlalaaynnddtPPrireeppacarraaattoolrryy 444.1111 SLLamCCp/MMleSSP/MMrSS epfaorrLOaMStMSiAnaolynsis 4.1.1 Sample Preparation for LC/MS/MS Analysis WraoWtmaootervressaramompsplcleeussawlwecerhroeorninnii.taiaSllloyittrrepeaahttaeedsdweweixiththr2a20c0t00iuouln(L.SoofPf E22)55v00mamshug./sLsesododd1iiuupmmrottphhaiirososutulhlafaottseaSsm9opulluettiosnnf1ot0ro GLrLieuCGmi/MMoonvSSew/MMarSeSssiapadnnauaaalrlylyfssciosihsm.l.oerdiAAnpeppo.oorSrrtoiot0lindooeonfxpfthssaaaacsmmieoppnleloexiwtnrwaaoacrsstdioedinriblu(i0tSedPdoEst0so)afwnfooatrrtstyhy-mumisaieillfdieleitrtceosrsspowwrfeiitmphhaarTTteyypptheeneh|I wsawaanatmcteeprarl,.emsaTTnfhhoteer s"cdTTrirhliuiosstmiroaimntnawrgtiarrisxxuenpnesenhrpfhaoeanrrnmcfcoeeermdmmeependrnitoot rwnwtaoashseexcstobreabsscsaoteimovrvnpeeldidenisoni.nrdeeaTerrhaietroilaierlreessssadaemmnpslptahelemsespelfffefrerosocmmwtsetotrhhfioissmtalaltoorcicnxaatteisoonnnhlaaano(nnc0ddreamofrCeroondmumt.. iSsSnPcPrEneEce6acnorainhtrtgitridd{rggu0oenk..scToTpnhehcoreefconctaramrrrateitrdiicdoggoneenowwftahtasehsesseeelusutadetmdewpdwilseithash.m55pmTmeLhs.Lepoodrffilu11ot00el00od%%ansmaamelmfyeshtphilasean,sncowll.TeThrehiisstratvrnoesaafttemmrereenndtt esuled to a C18 resulted in an eight-fold concentration of the diluted samples prior to analysis. 412 SempleAnalbyyLOsMiSMsS 4.1.2 Sample Analysis by LC/MS/MS IonInolHHuPPmLnLC.C,B,aaannsaoaldliioqquunootttohoffeaextxfrtraatccticifs itjnoojeiacotneddaaannddpfpaoasrsstseeesddttathhtrirooouungagrhhyaaphqlaiqusuieidd-ipphhtaahsseececohclrhuorommmnataeotiogagrtrahaepphhiicc inctHhoePelLuqlCmiqusuniei.ddpaBmmroaoabsbteiiildeoepnoh,pnaEhsatShseeIe,,Sahtfphfierenoiatavynniaoadlfleyytstheieaissarrnaropaeailtydaiatinneneefddoarffcootchrrueaarsacctlhahoatairromaancecattareeynrriisspsthitfcaocrsaaemamnoionauulntnhyttezooifcfno&tglmiumwemei.n.derFFegoolalll~oeovwweinntoggof mocHirrPggLaannCtiieccsmpecceporamaratoputoirouenmns,;dEsmp,Sioi/lnMcecoSciluundpliuregnosgvafifdnrluueeoosrrodooaccnhrhazesepmemiid,cic,afaasnrls.ad.gamEEcelecnctulterradot,seapemrnaedyacdfinssestggeoeftconntreoearrdoanl.lalyyIlyospozneipnsregarcpaiahteeadwdrraidaatetcrrtaroeaellnaartgviiyveeosleoylefyf mnioldwtemorpoecrahteumreisc;amlsolaercouolebssearrveedioannizded,afnrtaigamteondteadga, iannsdtsdaentdeacdtesd.. Ions characteristic of known fluorochemicals are observed and quantitated against standards. AAaHHeewnwielettatt:h-PPeaaslccakkamarpryddlHHePePz1xl11a00ce00tsHH.PPALLOnCassyyysssttseemmwcacusosuplpleeeddr1to0oa)MMiiccUrrsooimnmgaassssseUUtelitimmdaa rMMeSSaI/cMMtSSownwamasosunuissceerddintoog a(1(SnS7RaA1lMM0y)z4),e.SSathSmaepamlmpseplaeslmsowpsweleweroreoerxeeteraaxxnctrtaastl.cyteazAdendcaoolbynntse3ist35o/w5w0e/d0a4n4s,.3p1eAA2rdfddo0drtmi4toioanendanaldlumsmain1alg8tiri0cxse4sls.eppciiRtkeeeadsswwrweeaaerncreetaioelnexxtytmartacocdiintaeeitcdtdoaraoinoln8ng proivnAaichdmeentDd. 3/17/04. Samples were provided in Attachment D. analyzed between 3/12/04 and 3/18/04. Raw analytical data is 55 AAnnaallyyssiiss 55,11 CACa7al-lipibobirrnaatttciiaoolnbnraoncirvo wasanalyzedattebeginningandendoftheanalyticalsequence f5ofA0or0r7t,t-hhpoeeacinncoctomcmp1aplo0ibo0uru0annntdidogsnoofcfuorinpveteter)rweesfsaot.s.rTaTLnhhOaoelcMycazaSlelbdiMbrraaSaittoaitohnnnepapbyooesnignsitsn.snwTwinohegrereaipnnrpdsereieppnuaadrmreeooddnfattahter0o0,as,2np25ao5,rly,o5tio50c0a,e,l s1r1e00o0q0,u,s2e25nt50ch0,eo, Voc5aon0nnc0lec,rencanientrrpdaatttiooa1nn0nw0dw0acasosnpmgpo/lLloitttoe(pndptfctfo)ooreefieoafarcccheLhepCnop/ioMd(nintS)t..a/MnUUSsdsiincnaggonfalnilinyecesiiaaser.rtreeToggfhrreceessasislniiosootnnmruwiwminitheahni11tn/Xxr(eww7s)epawiogeinhrstoigengdhe,velththreseemnu3nss0ilgopnpteeh,e,de, `A caltraon curves acceplabio 12.0865 (12 0570) y-intercept and correlation coefficient (r) and coefficient of A calibration curve is acceptable if r >_.0.985 (r~ _> 0.970). determination (r2) were determined. ' Calbraton sandarcsaopreparedusingthesameSPEprocedureusedorsamples. Calibration standards are prepared using the same SPE procedure used for samples. | aCoavuliabgrthaootiounntcchhhoeocckkasnstataalnynsddiaasrrddssswoweqerrueeaeanonaa.llyCyzzoeemddppplreadrinocdcaielcallly&y ((eebvveearryyaPth9dr0ee11t0o ffaivo.essstaaammnpdpalerdinnajetcntsioan)se) tchrooughnoutcthaeeroanwnailtyhsis+r/2se0aq%uoetnfcfeie.aCocomanpvliaasnkcee is obtained if the. standard analyte concentrations are within +/-20% of the actual value. , Aicaltraton crtriaweromatforthisanayss. All calibration criteria were met for this analysis. 1 | `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSTUUYBBIDJJIEAESCCTLTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00007700 eacesors PAGE 3 OF5 3MMNo1sse221 3M MN01539221 55.22 ExBBtrllaaacnntikkossnbankswerepreparedandanalyzedwith very extractionbatch ofsampis.The e0exEtxxrttoraracanctcvtitiiioooonnnveibblnalacnknaklskstsrsswahhtooeouurneldspntnoraoetntpdhhaaararedvvd.eeaFaanonnrydytttahaarenrggsaeeelytstzaaennadadlwyymtiethsppieprhvrleeeeessrxeyeetnnrettaaxscattrtaoi,ocoratnioabbnboovbveaeathctwhheeerrcoceofoncsncaekconmemtnprptalrseatlsiti..oonnTohofef the low-level calibration standard. For these samples, the extraction blanks were compliant. IlnInesvsettlrumcmoaleninbtrtbabtailaornnkksssaiinnntdhteheref,foorarmmndoofffdecerleaannnommnoetthhfaaninogolhlsisoeovvlvseensntatwmweprleoeresa.laslsAoogaaainnna,allyyizzeoeddbalafafenterkrseevsveherryoyuhhiiggnhoht-- hslhaeaavvmveopeliacoaannslyiybptrraatoatrsirogganenelttsaotadnananhaiedlryyaoretedsts, poarpneirdessoaennfnttetarsatktontboorrwaarnnabbkohousvigvaeehrm-toltehhcveeeoelmllpoonskwwaakm-rtlvtepe.vleelslc.acaiAlibgbarraianti,ootnnhsetstabanlnaddnaakrrsdd..shFoFouolrdr thenot the samples presented here the instrument blanks are compliant. 55.33 `SSSuuutrrorrgooagglaastpteekssos aro no a componento ho LOMSIMSanaytcalmathods. Surrogate spikes are not a component of the LC/MS/MS analytical methods. 55.44 FMMlaadttrariinxxdSSlappbioikkraeetssoryspiesweropraparedusingallcompoundsof rest.Fedspieswere p`rpaFenrieeaplpldaayraroeesndbddbyblyaybtaaoocdriladantibongorgryaaastopmmriekyeaeapssrsuiwuroreereroddevsvpohorlieluuppmmaierneeogdocffofunfsieteinalddigsnsaaealrmlmpcfpololrmeesp1taoomuaapncldoconsoctnooatfaliiiennnecetertrsroespnsp.lti.LkeaeFdbdieowrwldiaitthshoptrtihkhyeesstptaiwarkmegeereestt cocaofonnenasxsiltyisrsteattecsetddbioooyfnfta.haFlelioqlluaukobotobssrloaoaftfnoukrunysnvp-pssirppkiioiekkrseetoddcfosfonihelsilpiddspstsianeamgdmpoclpoeflensslttaatihbhnoaetrtrwasweofreroeyrrewsfafaoortmtreitipffriilefeeddrcaoaifltleetthhcdeetlaioallnab.obrhoLeartaaloabtorboyroryraaataottrotyhrheyseapttiiknimemdese LSasothhfiiiopeprpxpateertaddocwrtwtiyocihntho. ntFthhtieoeoldsssapabmkmlapenplskle(sCspco0oin0ktnseatesaiicnnceoeornrnsss5fis.toot6e)tdtahhroeoof fiileasilbaddomarpaanontosddrbyobafwaclcaakktbetortrooafotttrohhtrioefyivleadalablboaoortrratasthtpoeoriryyloafdbofoarorfraaatntonroaayillyamsyniso.d. oeoLfxfatbexaoxtcrtataraoctoncttroiyonncf..oincEitEraeoanclcchshyp,taitkypnepsodeo(msofeafsetsppsieikkceetfpiofrpneorcov5tvi.si6ddte)ehsasaretrinlsfmooarammmyapatlteoiosnpnanofencleeatedbadoeneradady(toit0orcyaaawlsssasreteeesssrssusaspan.iknaeadMtlyaotaeitsrtsahteabsbtiiiilmikt,yee, extraction efficiency, and matrix effects that may impact mfoacotvesripos arreecogivveernsi.n AtachmenBt.Pleasesee Secon recoveries are given in Attachment B. Please see Section 5.7 oraddonal Gscusson of analytical results. Matrix spike 5.7 for additional discussion of matrix spike recoveries. 55.55 DDiukupiplaliinccdaatlteaebssoratorydupicaleswerepreparedfo eachfledsample.Duplicaeresulsare givenalongwith sampleresus AtachmentA. Field and laboratory duplicates were prepared for given along with the sample results in Attachment A. each field sample. Duplicate results are 55.66 FLoLaarbbLoorOraMattSooMrrSyy aCCnoaonlnytstrreoosl,l SSilaaimmpwpaltleeorsswas kod wihall compoandsof inkrestat 100and 55F100o00r3nLngCng/0//ImcmVIaLLS%c/cIdhuVrulSiLrinGnagSgn.eaeaRlayceschseheus,elxxsMttrrriallaicoqtgcioiwtnvasietseeonernt.a.wlAaoAlsllwsrripeelicckohoevvdeherewirieeirtsshafwfcaroalrlatcalaollimcncopAomotmpuaponcohduuisnnmddoesfsnwtinwetDee.rrroeebsbteetattwwe1ee0e0nn7a70n0-d- 130% in each LCS. Results are given along with the raw data in Attachment D. 55.77 BaSStstaaettdeeommneenrntetosouffsAoAcfcfcclueurraaspcciyykes,laboratory forfedfkdsamples,fodbankspas,and IealBxabcaboesorperatadtitoooorrnynycocfroeoPnsnRuttrBlotosSls,owpsfpiikifckieeehslsd,,htashtspheeikaaeanssn,atayallatyabctmiocaoralanltaooacrfcyccaufucrorcaratcuicfyriyeadcfoyffaoielfaldlll =sccao5om0mm%ppp.oloeuusSnn,ddfssieeildsis vob+lbaen33ekr00%%sc,rp,owimkwepiaisothh,utnalthdnhesde `SseahhcxococwuewrepeatddcioynieeistoehbferaPrslFlaeaBbbdSooor,ranawttaohorirncyyhoaovhrefarfiseadlladassssptpsaiikotkeesemrsermeeconocntvoteovoref irfaieeacsscoluorsiuaptcskydidorefoaocffotvt5hho0oer%ssyeed.raarStanneag(gveee1srsa.6.lT,oThthhleaeesbr,siactanaotmidecompoomenuennttnodootsflf SaccupracUiysiesdkbfaosreehdoospnroaj)encto.vSeprailkl earsesceosvsemreynt toaf lasll nckcd n Atochmon8t. spike recovery data (field, lab, and control spikes) used for the project. Spike recovery data is included in Attachment B. 66 DDaattaa SSuummmmaarryy pPalProlteasasspaeors0eb0eAiAtntatac(ch5h9mm0a)enn(ttOAALf)foo.rr a e detalod detailed Ising of1h anayicalous listing of the analytical results. Reasuapolresd n Results are reported in parts per billion (ppb) (ng/mL). `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSTUUYBBIDJJIEAESCCTLTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00007711 racesoes PAGE4 OF5 IM_MNotS39222 3M MN01539222 77 DDaattaa//SSaammppllee RReetteennttiioonn `oSSlaaicmmippolleonsscaadrroae cdiisipspoaosrsecechdoiovffeadonnoeenmmroionrntethhvaaafbftlterer ttmhheedriroeappraotrntidisshsaisurseudecddopuunlylreeesspsoortothtsheerrawwriiossseeossrppecediciifioe1dd..tAAalll foes maintained electronic data is folders maintained by Exygen. archived on by Exygen. retrievable media and hard copy reports are stored in data 8& AAttttaacchhmmeennttss 81 AchmenAt Resuts 8.1 Attachment A: Results 82 AtactmentB: Maric Spike Recoveries 8.2 Attachment B: Matrix Spike Recoveries 838.3 AAtttiaacchhmmeenntt CC:: CChhaaiinnooffCCuussttooddyy 848.4 AAtttaacchhmmeennttDD:: RRaawwAAnnaailyyiticcaal DDaataa 99 SSiiggnnaattuurreess 2 A CU, PPaauull Goomnnnoolllyy, T Tea~ m L~ ead:eM -r SCHS. Sha lo Daattee j=hn MM.. FFalahhoerryty,, VViicoe PPrroessiiddeennt! Dato Date Other LabembersContributing 0 Data Other Lab Members Contributing to Data KKaarreenn SSmmiitthh `CHGEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00007722 pPAaGcEeSsoOrFs5 IM_MNO1S39223 3M MN01539223 ----------ee------ SECTION A `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALUL-N- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00007733 3M_MNO1539224 3M MN01539224 ExyegseRESnEARCH Precise Research Vote, Proven Results. 2 RlaR Summaryof C8and C8Acids andC4, G8and C8Sulfonates inWater Samples Summary of C6 and C8 Acids and C4, C6 and C8 Sulfonates in Water Samples Ee GanaPAhria Found iSme)ren Sample ID a = = Influent 3 Influent 3* hens pS 5% Influent 3 Dup CumsEheniz dia os Comb Effluent 1/2 Com ean oi oe Comb Effluent lf2" Analyte Found (ng/mL) C6 Acid PFHA Perfluorohexanoic Acid C8 Acid PFOA Perlluorooctanoic Acid 45.9 301 47.3 44.3 0.462 298 319 0.0835 0.398 0.114 Comb Effluent 112 Dup 0.387 0.111. Port 4A Port 4A* Pons bh Port 4A Dup Toren ne on Port 4B [or] = io Port 4B* er J in Port 4B Dup 8 5% hit Influent 1/2 -- in ne Influent 1/2" ho 7 Jo Influent 1/2 Dup fry 5 us Trip Blank 13.4 12.6 11.9 15.6 ",.,15.3 ~r5.7 3.90 3.73 3.77 ",, ND ,, 5.59 5,41 6.91 4.42 4.64 4.72 11,6 13.4 14.5 NQ Bm Sample ID --SmEel Influent 3 ueInfluent 3* a Influent 3 Dup cote Comb Effluent 1!2 Som Ene Comb Effluent 1]2" cota Comb Effluent 1/2 Dup Tenn Pod 4A Fon Port 4A* Paro Port 4A Dup TarPort 4B or) Port 4B* flePort 4B Dup hr Influent 1/2 a. Influent 1/2" hes up Influent 1/2 Dup re Trip Blank Cosutonnavros C4 Sulfonate PFBS Perfluorobutanesulfonate ewes36.9 io40.0 2532.9 50.476 he0.449 jo0.482 o30.1 229.3 523.3 221.9 322.7 225.2 =42.1 pol45.0 @46.1 wvND Anat Fund gin Analyte Found (nglmL) "Sonatas. C6 Sulfonate PFHS Perfluorohexanesulfonate eiessoses 6.20 s8i6.12 6.34 ND J]-ND JbHi115a%1,54 1%1.65 Jet4.63 24.55 is4.56 2ND Suen Pros C8 Sulfonate PFOS Perfluomoctanesulfonate tebe 37.7 ifoosf40.5 36.9 ND ND I+]ND 53.44 Ft3.34 i3.27 bo2.61 mn2.73 in2.90 =n13.4 ji11.3 HH11.1 wND JEAro os m TI ND = Not detected = Response between 0 and 0.025 ng/mL. NQ = Not quantifiable = Response between 0.025 ng/mL and LOQ (0,050 ng/mL) *Laboratory Duplicate CHOENNFNIEDPEINNTCIAOLUN- TSYUBDJIESCTTRTICOTACOPURROTT.ECNTG.IV2E7-O0R1D1E0R.8E8N6T2ERED IN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00007744 Y058 Research Drive ORBe, ~' ~State College, PA 16801, USA anon, IT: 814.272.1039 ~F: 814.231.1580 su_wmoresezzs exygn.com 3M MN01539225 STANDARD TERMS AND CONDITIONS STANDARD TERMS AND CONDITIONS Sences provided by Exysen Research re ited o ho torms Services provided by Exygen Research are limited to the terms and ondions stated bree, unless otherwise agreed oma and conditions stated herein, unless otherwise agreed to in a fom contact formal contract. 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A 15% Ee ar i ke ne em ces 1 same tot SOT ho monthly service charge sha![ be added to all past due balances. Norm ntanans my pyur oy ev 24 rte md gp min ds No~withstandm~ any pay~en~ terms ~o the conhary set forth in this Doon Cc ofa ee aon es aH Bos Purchase Order, Exygen, in ~s sole discretion, leserv~s the dglff !o request mn srk ror cncero Sn pT p~yment in advance from client In the event o~ default in paymen~ For ees ene. on3k coed et ot ofhs in, THISPOICY--Goyen Bess sso rouce ens wih serwces rendered, Exygen shalt be entitled to reasonable costs of collection, in, ak ot mi i Fly a0 i re Sane including, but no~ limited [e, attorneys' fees HUNG 48 us Bi ty to De drt OE to ti po hg ok pel he BILLINd--AII fees and charges are billed directly to tt~,e client requesting ves ea i ek rd iy wiht or csr EL i ge ec omeofnpes 08 services. Exygen will not bill a third party without prior noti(}cation in he yh " writing, via a signed statement acknowledging and accepting responsibillty pat wh a ppt 03 for payment. Exygen wiil assume that the paperwork, submitted with a oTbrs od vs root oe10 s pcs SPECIAL REPORTS.-Ad ml ngs yb es be csr sample describes the desired testing profocol Any cha~ges to the protocol lo ern rms must be submitted }n writing. Please fax changes to Exygen marked, URGENT" yo mpd sti a Tube ee tL ei compan sy ins "URGENT" to your assigned representative It changes are made after the ral cursed sing as betted coi he ert Scum ft ray of or 1 te originally requested testing has been initated or (-ompieted, the client cpt porortgyrse fn nti rho ewe to mcg accepts responsibility for payment. 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Rush ana!ysis services are contingent upon availability and erat wihsnaeried Gn er SSCS oguCATON, UU ANDISURANCE-toyn sre prearrangement with an autholized Exy~en ~epresentative A surchar~e is ty ah ay sre ny, Goan, ov ero har, en oye. usually added to the list fee if rush analysis is requested~ AML FET ifi onoma ar co did S50 14 ora Puri HO 3 oi ges, er A4INI/I/IU44 FEE--The minimum fee for commercial services is one hundred en vs ar cht Hc cers nye: HS dollars ($100)~ SAMPLECOLLRCTIONSUBSSIOU-Clen rits espre cx CorcHecan oyWega rw aH 8Ai14PLE COLLECTtON/SUB~IS~IOfC--Client shall be responsible for oer lk, prsnaton puking 2 kag, METI L 1s nhoyes age epee omar wi proper collection, preservation, packin~ and packagin~,, and shipment of he arensed wih sptbom godcomecl Fo of acsn udetsSer ac 0 erin tile sample(s) in accordance with applicable law and good commercial che Taak ob i au Ee CES kr srr, vest oe eto practice. Title and risk of loss with respect to submitted samples shall at all a op Et rs ec. ce, ton. pes times remain with client prior to acceptance by an Exygen sample Coda ywa k terhae coh yh unl et and ae ort wh AoC da custodian. Exygen will iniliate a chaimof-custody upon sample receipt rin to a so hh i yO, SO Sn on eo unless the client include~ one with the sarnple(sl, t~y request, Exy~en will ows afc rmctsse aeas yo com or eh orl Oc provide chain-of-custody forms for client's use 0p hed he crgiet dty. poweis,oryvps SFTOaeryEen for I wah ceed pen, All samples submitted must be accompanied by: purchase order, or signed ct. ari rhs sac hoo 15t. quotation: sample description, includin~ sample type, source, time and onnnn, get qs, gcc SHCA AOE ne orgs date of collection; specific analyses requested; estimated concentration ov ecep t coer Hg re 0d She et WARAORIAT ONFABTRITYY1 ip ac w, levels; requested report date: current biling address: and other relevant mine Cen rates sc) of wr re 1 information. Up ret, by ipoesd i poe re cranes SOA winn ts toh in SOP a cr ary Upon request, Exygen will provide and ship appropriate sample containers car on SamvaantdsBt a EE vera, xe se idd tybo Ege doe 0 try to clients. ]hose containers will include the appropriate preservative if tsiaaneyseeaesv. Wea teerseps pervde BAlanpnt ctapy ppsnforewoh lyroitsvseoer wlt,ht particular analyses require one. It is the responsibility o~ the client to handle these preserved containers safely, and using all appropriate safety ators hs eqn Omagh yo ae oan wl 0036 ors tu or hos Src Conors precautions. Clients requesting overnight delivery of sample containers wilt EaT mi en on 5 EP TES 6 0 ATH ACCEOPF PTURCAHANSEOCRDEER Th rchOrr xs be invoiced for freight. Exygen reserves the right to charge a fee for sample noes ing genase rn sd contr ed containers. SAMPLEDISPOSAL Eryn esas sor r ve ee n afer ern. henFycomeofrven SA/t4PLEDISPOSAL--Exygen retains samples for one month after Erna ead hen Son ocom he ange Ue ert reporting results, then disposes of or returns the sample. Unless the client custody Js rnakffained for each tot of samples received. MAZ~Rg CO~UNIEATIO~ The ctienk has the responsibility te inform the laboratory of any known or suspected hazardous characteristics of the sample, and to provide information on hazard prevenkion ~nd personal protection as necessary or otherwise required by applicable law. ~UALtTYA~SU~A~CE E~ygcn will perform services consistent with its Quality Assurance Standard Opera~mg Procedures (SOPP, the terms of which are expressly incorporated herein by reference; provided, however, it shall be the exclusive responsibility of the client to confirm that Exygen's stand,~rd p~acUces will mee~ the client's needs prio~ ~o placing an order for work. In the even~ client desires an alternative to these SOPs, such requests must be m~de in wr tins pr}or to sample submission and acceptance by Exygen. ETHIC~ POUC~Exygen Research strives to provide its client:s with the highest qualit), data in the tagtest realistic turnaround time. We balance the high s~andards of this goal by insisting that each employee also perform within the ~:uidelines of the highest possible pmfe%ional ethics. Each E~ygen employee is required to sign a ~tatement of personal and professional inte~[rity. ~PECI~L REPORT~.-Additional char~es may be necessary for custom report formats. LITIgaTIOn.All costs associated with compliance to any subpoena documents, for testimony h~ a court of law, or for any other purpose relat~n~ to won performed by Fxygen Research ~hall be i~voiced by Exygen and paid by client. These co~t~ shall include, but are n~t limited hourly charges for the persons involved, travel, mileage, and accommodations, and for ~ny and all other expenses associated with said litigation. INDEf~INIFICATION, LIABILITY, AND INSURANCE--Exygen agrees indemnify, defend, and save the client, its officers, directors, employees. agents, and representatives harmless from all losses, e~penses, demands, and claims made against the client, its officers, directors, employees, agents and representatives because of any personal injuries, death or property damage to the extent caused by lhe negligence or willful misconduct of Exygen, its employees, agents, or representatives in connection with the perfo,qnance of services under this agreement, except to the extent such losses, expenses, demands, or claims, occur as a result of the negligent or willful acts or omissions of the client, its officers, directors, employees, agents, and representatives; however, such indemnification and damages shall, in the a~?~rega~e, be limited to the amount equal to the lesser of damages suffered by the ctien[ as the direct result thereof, or (b) the ~.ol.al amount paid to Exygen for the work heren covered. Eygen will, if requested by the client, furnish certificates of insurance from its carrier evidencing appropriate insurance coverage. WARRANTY AND LI/t4tT5 OF LIABILITY--In accepting analytical work, Exygen guarantees the accuracy of the test results for the sample as submitted within the tolerances set forth in the SOPs. We disclaim any other warranties, epressed or implied by law. Exygen does not accept any legal responsibility for the purposes for which client uses the test results. Exygen will not accept any purchase order or any other order for work that indude~ conditions that vary from these Standard Conditions. ACCEPTANCE Of PURCHA..CE ORDER ]'his Purchase Order becomes a binding agreement, subject to the specific terms and conditions stated herein, upon Exygen's commencement of work `CHGEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTTT.EECNCOTT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00007755 SW_MNo1S39226 3M MN01539226 SECTION B `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALUL-N- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00007766 3M_MNo1S39227 3M MN01539227 oF ec'se Research Proven Results. aSample Description [I EE eT ee Recovery Summary for C6 and C8 Acids and C4, C6 and C8 Sulfonates in Water C4 Sulfonate PFBS C6 Sulfonate PFHS C8 Sulfonate PFOS Amount I Amt Found Amount Amt Found Amount Amt Found Amount .,, SpikedJ In Sample Recovered Recovery in Sample Recovered Recovery in Sample Recovered Recovery ' (ng/mL) (ng/mL) (ng/mL) (%) (ng/mL) (ng/mL) (%) (ng/mL) (nglmL) (%) Influent 3 Low Spk '10 ppb Spike '.. 10 36.9 ND 0 6.20 17.2 110 37.7 46.1 84 Influent 3 High Spk 100 ppb Spike '.. 100 Influent 3 Spk C Laboratory Spike 500 = Comb Effluent 1/2 Low Spk lO ppb Spike 10 oER Comb Effluent 112 High Spk lo0 ppb Spike 100 EE Comb Effluent t/2 Spk D Laboratory Spike 10 = Port 4A Low Spk 10 ppb Spike 10 lz Port 4A High Spk 100 ppb Spike 100 = =me (000 Port4ASpk E 36.9 163 36.9 529 0.476 8,17 0..476 77.5 0.476. 10.1 30.1 30.1 '. 31.1 , 86.7 ' Laboratory Spike Port 4B Low Spk 10 ppb Spike w= Port 4B High Spk 100 ppb Spike =Port 4B 6pk F Laboratory Spike ZF Influent 1/2 Low Spk 25 30.1 10 21.9 100 21.9 25 21.9 57.~, 31.5 145 46.8 10 ppb Spike 10 42.1 170 126 6.20 98 6.20 77 ND 77 ND 96 ND 10 1.97 LD 57 1.97 108 1.97 ",, 98 1.48 ' 123 1.48 '.., 100 " 1.48 , * .4.63 91.9 86 37.7 123 85 488 96 37.7 577 108 8.58 86 ND 8.24 82 82,3 82 ND 85.9 86 10.1 101 ND 9.44 94 10.7 87 3.44 10.9 75 LID 76.1 7,~ 26.8 99 3.44 3.44 72.1 69 27,5 96 10,2 87 2,61 11.0 84 107 106 2.61 111 108 25.0 94 2.61 25.2 90 14.6 100 13.4 23.2 98 Influent '1/2 High Spk 100 ppb Spike 100 42.1 191 149 4.63 99.9 95 13.4 112 99 Influent 112 Spk G Laboratory Spike TrTriilp~BBllaannkk LLoowwSpk lO ppb Spike 10 42.1 i 10 ND 137 * 8,05 81 4.63 NQ 83 13.4 28.3 149 101 ND 10.9 109 Trip Blank High Spk 1 o0 ppb 100 ND 70.7 71 NQ 95.6. 96 ND 104 104 r S EeEE m ND -- Not detected -- Response between 0 and 0.025 ng/mL. Rn, en NQ = Not quantifiable = Response between 0.025 ng/mL and LOQ (0.050 ng/mL) a-- gaupn *Sample residue exceeds spiking level significantly; therefore, an accurate recovery cannot be calculated. ~3058 Research Drive ,~ ~State College, PA 16801, USA IT: 800.281.3219 @ F: 814.272.1019 exygen.com CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00007777 3M MN01539228 E ygen Xysen.. PreHcovReensReeaurcsh. Proven Results. Rocovery Summaryfor C8 andC8Acids and C4,C6 and CBSulfonates in Water Recovery.Summary for C6 and C8 Acids and C4, C6 and C8 Sulfonates in Water Samp Sample , oscrpton Description " oan 3 Cow SK Influent 3 Low Spk Toman 10 ppb Spike ', Ifuont 3bigh pk Influent 3 High Spk pr 100 ppb Spike o3t 5p C Influent 3 Spk C Laygoa Laboratory Spike Com Eft1u2Laownstpk Comb Effluent 1/2 Low Spk msn 10 ppb Spike ComEu12aighn85k. Comb Effluent 112 High Spk Toran 100 ppb Spike CorbEfent 1285K0 Comb Effluent 1/2 Spk D Layta Laboratory 8pike Port 4Low spk Tose0sok Port 4A Low Spk 1o ppb Spike Port Higspc Port 4A High Spk Toone 100 ppb Spike Portanssre Port 4A Spk E ie Laborato~ Spike Port 8Low spk Port 4B Low Spk Tomer lO ppb Spike Port48 Highspc Port 4B High Spk Tommie 1 O0 ppb Spike Pots Port 4B 8pk F Corton Laboratow Spike ofo12oLonwStk Influent 1/2 Low Spk omer lO ppb Spike uot172 High spk Influent I/2 High Spk ip 100 ppb Spike t1o 2 55k6. Influent 1/2 Spk G Ly one Laboratory Spike Tip BlLaownsokx Trip Blank Low Spk ome 10 ppb Spike Trip BlankHighSk Trip Blank High Spk oo 10o ppb FouncdsAcAimsoupnrtin iracancAmioaupnrton Amount nSampie. Rocovesd Recovery| inSample RecoveredRecovery Spiked 5 0 opm). tog) (ng/mL) C6 Acid PFHA Amt Found Amo'~nt Recovery in Sample Recovered (nglmL) (ng/mL) (%) C8 Acid PFOA Amt Found Amount in Sample Recovered Recovery (nglmL) (ng/mL) (%) w | ws ms | wm a 10 45.9 51.5 " 301 318 w| we wm om | om '-. 100 45.9 129 83 301 wm ow 363 62 m | we me we | wm 250 45.9 516 188 301 sm om 572 108 wo | ew rm ow | oms wi we 10 0.462 7,84 74 0.0835 13.1 130 w | oe wr om [ows ww 1co 0,462 74,7 74 0.0835 130 130 || ce wo ws | ooms ow lO 0.462.. 19.0 185 0.0835 12.0 119 10 | 413.4 201 '. 20.7 n73 5s.s59 215.2 ow 96 wow wm on [ss ww 100 13.4 71 5.5 107 101 | we ms ow | ss wm ow 25 13.4 53.6" 5.59 36.1 122 wo | ws 10 15.6 mew | we 23.8 . 82 4.42 ws we 15.3 109 wo| ws 100 15.6 ww | ae 107 ~1 4.42 we ws 109 105 s | ws 25 5.6 ws oe | se 56.6 164 4.42 me ow 33.6 117 of se 10 3.90 wo | [a0 lO0 3.90 we wo [ws 14.9 110 ',11.6 ms sw | we 93.5 90 11.6 we ow 18.4 68 wm we t20 108 wo | aw sr ose | ome amr ws 10 3.90 55.1 512 11.6 29.1 175 of wks ows | ow me we lO ND 12.5 125 ND '11.6 116 wl wo mr om 1 ow ws ws lOO ND 77.7 78 ND 105 ND =Ho acted ResponseBan 0 an 0.25 pn. ND = Not detected = Response between 0 and 0.025 ng/mL. 0 Notcuanbol Resp bowen 0.025ng 3ndLO 000k) NQ = Not quantifiable = Response between 0.025 ng/mL and LOQ (0.050 ngfmL) Sail edo coeds sng vet gnc, rte, a ers recor core 046.I 15 ncOre *Sample residue exceeds spiking level significantly; therefore, an accurate recovery cannot be calculated. ~3058 Research Drive SEEi, Teor, Usa '~tate College, PA 16801, USA 1;F fonasR 20 ~F: 814.272.1019 enpncim e~gen.com `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACPOPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 3M_MNO1539220 3M MN01539229 11993399..00007788 --e _-- eee e e-- SECTION C `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALUL-N- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00007799 3M_MNO1539230 3M MN01539230 , 'E ygen E n 33St00a55t88e RRCoeelssleeeaagrrecc,hhPDDArrii1vv6ee801 RREESSECAARRCCHH State College, PA 16801 ogin PPhhooFnnaexe::: 888111444---222737122---111050383909 Fax: 814-231-1580 PCroogenc 2P0o60D004a 4 = CooFnnfloorrEmm CCOOCC: Sampler FaTrsoeie Project: P0000644 Conform COC: Conor Samgie: Tre Conform Sample: Company Name: aM Conform Recvest: Tre Company Name: 3M Conform Request: Sibmiled By KENT LINDSTROM Submitted By: KENT LINDSTROM LognTyoe: Immediate Recep of Samples Login Type: Immediate Receipt of Samples Sten 7 Started: T Oras Cuzeao0s Date Start: 02/26/2004 DueDate: Ga12004 Due Date: 03/11/2004 Recoved Doe: 031262004 Received Date: 02/26/2004 Rocovod By: AUMERMAN, MARK Received By: AMMERMAN, MARK Spread Samp Spread Sample: Cover Label: Projoc To Type: Gotago Grove Acvated Corban System Florachemica Moning | ROUTINE Project Title/Type: Cottage Grove Activated Carbon System Fluorochemical Monitoring / ROUTINE Eon SOL GHA, KAREN Exygen SD/PI: RISHA, KAREN Logh Notes: Login Notes: Comfort Notes: lotsa 2 sel havi ho io ihoon. MEA52004 Conform Notes: Client send only 2 of 3 pages of the chain-waiting for the third to finish the Iogin. MSA 02J26/04 rue False True True prc Package aaser PK0002581 canon Carton Packages/ Containers Packages I Containers sous conan Spi Mall Date I Condition ~hlpper/_ID prep-- reoex 2/26/2004 3:15:26PM Package Cots Uncmana tS SROrTzST) Package & Contents Uncompromised FEDEX 3168015711000001792579 Topconommp Temp. Control/Temp. an Wet Ice a0.1 lscion/Handessy Direction I Handled By seco RECEIVED J AMMERMAN, MARK Comoe GouWegn Container # Cre mere C0028072 cuamrs sea C0028073 come sss C0028074 comers zm020 C0028075 comers e210 C0028076 own ano C0028077 cuasrs mrss C0028078 [, C0028079 coer aan C0028080 com eas C0028081 mem mean C0028082 coer as570 C0028083 [oR C0028084 comes saz C0028085 J -- C0028086 wasn 430 C0028087 Gross Weight 580.2 g 579.0 g 258.6 g 258.2 g 612.1 g 601.0 g 257.6 g 254.9 g 611.3 g 614.4 g 256.4 g 255.7 g 584.0 g 582.2 g 253.2 g 254.3 g pH CousearTipe pH Container Type Som Gor ite 500 ml Clear Plastic ron Narrow 00m Garp 500 ml Clear Plastic il Narrow som Gps 500 ml Clear Plastic Narrow 00m Gump 500 ml Clear Plastic Narrow 200m)Goapate 500 ml Clear Plastic Narrow 500m Got ote 500 ml Clear Plastic Narrow Soom Grae 500 ml Clear Plastic row Narrow mmr 500 ml Clear Plastic Narrow 500m Copa 500 ml Clear Plastic Narrow som Gupte 500 ml Clear Plastic en Narrow 00mGeaPastc 500 ml Clear Plastic on Narrow 00mGr postc 500 ml Clear Plastic ren Narrow soon pit 500 ml Clear Plastic aren Narrow 00m Gampaste 500 ml Clear Plastic raw Narrow som Cuarpastc 500 ml Clear Plastic jor Narrow 00m GonPastc 500 ml Clear Plastic pot Narrow 510193201 usenet Preservative oeNONE oreNONE oreNONE oreNONE oreNONE oreNONE oreNONE none NONE oneNONE noneNONE oneNONE noneNONE noneNONE noneNONE noneNONE noeNONE frMfg._Lot wo L2o7on000 2/27/2004 Login.rpt ReportVerson: F020 200 35800 Report Version: Feb 20 2004 11:35AM Pan 1014 Page 1 of 4 `CHCEOONNNNFFEIIDPDIEENNNTTCIIAOALUL-N- TSSUYUBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCR\R-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00008800 nance: Instance: [RRR roosssos R0088309 a_Mo1saoz31 3M MN01539231 CLI Ta ee-- a = ProLjoegict#. PO200000B44 i ot " C`Coonnffoorrmm COC: ample: Project: P0000644 CCSuoobmmmppiaatnneyydNNBaya.mmee:: K33MENT LINDSTROM Conform COC: Conlon Sample: Conform Sample: Conform Request: Conform Request: StSLLaoourggbitimnneiTdTttyyeppdee:B: y: KENT LINDSTROM TImmedte RecofeSamppl!es Immediate Receipt of Samples SDDDautaaletretoeDSSadtit:aear:tt: 00T03221/221667/222000000044 DRRReoeuccceeooDivvvaeeetddde:DDByaa:ttee:: 000A232M7//12M2166E//722R200M0000A444N, MARK RSSLappebrrceeeelaa:ivddeSSdaaBmmpypl: lee:: AMMERMAN, MARK LPEPraxroobyjjegeclec:tnt TTSHitolDer/TPTyyppoe:: CRCoIotStttHaaAgg,ee KGGrArooRvvEeeNAAccitivaattoedd Carbon Carbon System System Fluorochemica Fluorochemical Monitorin|g ROUTINE Monitoring / ROUTINE L`LECooxoggyniignfneoNnNromolSteNeDsos:/tP:eIs:: RISHA, KAREN Glensendony2ot3 eges fhchn-watinforo iofh loin, VSA 022504 Conform Notes: Client send only 2 of 3 pages of the chain-waiting for the third to finish the Iogin. MSA 02/26/04 Package Package procuzsen PK0002581 Consiners Container # oz C0028102 oases C0028103 ow C0028104 owas C0028105 comes C0028106 wom C0028107 comms C0028108 canon PackaMaaCao0lgia0ntesse C3Un1oc5na2md6oo0ro0nmisPedacka3gTe60s1E/SgToCFThpeoIoOneeOetr0xya0iTnS2e5r7sS Carton Packages / Containers Mail Date I Condition 8hipper/ ID 2/26/2004 3:15:26PM Package & Contents Uncompromised FEDEX 3168015711000001792579 510193201 Gross Went pH Conainer Type presente Gross Weight pH Container Type swag 500mGorPlacte hore 580.3 g santo 500m NCaoraorwplaste Nore 593.1 g aro s00m Caarplaste one 266.7 g 2180 500m NCaorropwlaste nore 251.6 g 2ses0 500m Corpiste rove 258.5 g 230 00m GearPast Nove 257.3 g 500 ml Clear Plastic Narrow 500 rnl Clear Plastic Narrow 500 ml Clear Plastic Narrow 500 rol Clear Plastic Narrow 500 rol Clear Plastic Narrow 500 ml Clear Plastic Narrow 2490 500m Coarplste roe 256.9 g 500 ml Clear Plastic Preservative NONE NONE NONE NONE NONE NONE NONE TempConsolTenp. Terop. Control/Terop. Wate Wet Ice a0.1 oot Mfg._Lot Narrow True "ue False False TrueTrue TreTrue Desc MandaaBy Direction I Handled By recenen RECEIVED AERA WARK AMMERMAN, MARK wo 22m00 2/2712004 Loon pt Login.rpt Report Report VVeerrssPiiooann::gFFeeebb2202001242000084 11:35AM 11:35AM Page 2 of 4 `CHGEOONNNNFFEIIDPDEIENNNTTCIIAOALU-LN- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00008811 Instance: Instance: WN I Rooes0 R0088309 IM_MNO1539232 3M MN01539232 Spe Sample ID La01968001 L0001958-0001 torossoon L0001958-0002 Lootos80003 L0001958-0003 Losotossc00s L0001958-0004 Lorossoons L0001958-0005 [r---- L0001958-0006 Locotoss00 L0001958-0007 [r-- L0001958-0008 totossoon L0001958-0009 Locorossonno L0001958-0010 Loorasscots L0001958-0011 Lcorossaniz L0001958-0012 Lorossonns L0001958-0013 Lcorossonne L0001958-0014 rer L0001958-0015 wemorosscors L0001958-0016 Loooresmcorr L0001958-0017 wnnosscors L0001958-0018 torsos L0001958-0019 Loorosso L000t958-0020 Cow Container coorz C0028072 covers C0028073 conre C0028074 comers C0028075 coors C0028076 coors C002807 coners C0028078 coors C0028079 cones C0028080 coon C0028081 C0028082 coonnons C0028083 conmons C0028084 conse C0028085 C0028086 cooaeer C0028087 cosiez C0028102 conan C0028103 comes C0028104 conasies C0028105 Maw Matrix UGUD LIQUID UGUD LIQUID UQUD LIQUID UQUD LIQUID UD LIQUID GUD LIQUID GUD LIQUID GUD LIQUID UGUD LIQUID WUD LIQUID UQUD LIQUID UQUD LIQUI D UQUD LIQUID UQUD LIQUID UOUD LIQUID UQUD LIQUID Uo LIQUID Wo LIQUID OUD LIQUID UGUD LIQUID Fock Fraction Wet Water `Samples Samples Same Sample inePhase 1200012) Inf]uent Phase 1/2 (Inf 1/2) Weer nent Pass 20 2100p Water Influent Phase 1!2 (Inf 112) Dup Wer nkent1P20h01e2s)Leo Water Influent Phase 1/2 (Inf 112) Low Wer nent Phase 20120Hoh Water Influent Phase 1/2 (Inf 1/2) High Wer Cond Cent 1206612) Water Comb Effluent 1/2 (Eft 1/2) Wel CondEnt 1266120000 Water Comb Effluent 112 (Eft 1t2) Dup el Cond E1e 2 1n 2 ow Water Comb Effluent 1/2 (Eft 1t2) Low Wel Com Efe 12(8 12 Hon Water Comb Effluent 1/2 (Eft 1/2) High Wel UstAPatALsas Bonn Water Unit 4 Port A Lead (Port 4A) Wek akaPartAPLon4e0sOep Water Unit 4 Port A Lead (Port 4A) Dup Wel UtdPathLesd Potohw Water Unit 4 Port A Lead (Port 4A) Low Wels UndPatALene Port Hon Water Unit 4 Port A Lead (Port 4A,) High Wale UtdPoLesnsGordd) Water Unit 4 Port B Lead (Port 4B) Wale UndPatsLess GonO)u Water Unit 4 Port B Lead (Port 4B) Dup Wal UtdPan LendPort 8)ow Water Unit 4 Port B Lead (Port 4B) Low Wer UntLAondP(Poart 8t)Hon Water Unit 4 Port B Lead (Port 4B) High ew ene3onts) Water Influent 3 (Inf 3) wes Water ea 0 Influent 3 (Inf 3) Dup We ens Oo)HohSp Water Influent 3 (Inf 3) High Spike Wer te(fnLowtSpe Water Influent 3 (Inf 3) Low Spike 22004 2/27/2004 Log Login.rpt RRepeoprortt VVeerrssiioonnP::aFgFoeebb3202001242000084 1111::3355AAMM Page 3 of 4 `CHGEOONNNNFFEIIDPDEIENNNTTCIIAOALU-LN- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00008822 OuiSamp Do cond Date Sampled Date Received cars ozs 02/25/2004 0212612004 Dato ve Data Due canine 03/11/2004 ouzsaoos ovens ovnvanes 02/25/2004 02/26/2004 03/11/2004 oss omen 02/25/2004 02/26/2004 ovis 03/11/2004 oases oven 02/25/2004 02/26/2004 ove 03/1112004 oases ose 02/25/2004 02/26/2004 ovnaok 03/11/2004 onsen osmos 0212512004 0212612004 ows 03/11/2004 cozsaoos ovzmnee 02/25/2004 02/26/2004 owas 03/11/2004 casaoos oven ovivztok 02/25/2004 02/26/2004 03/11/2004 [Ee 02/25/2004 02/26/2004 03/11/2004 oases onsen 02/25/2004 02/26/2004 oyna 03/11/2004 [ET 0212512004 02/2612004 03/11/2004 cosas comes 02/25/2004 02/26/2004 ove 03/11/2004 cansaoos come 02/25/2004 02/26/2004 oak 03/11/2004 oonsoo0s Comezaes oven 02/25/2004 02/26/2004 03/1112004 oomsaoos oumaznes owas 02/25/2004 02/26/2004 03/11/2004 cosas consis 02/25/2004 02/26/2004 ovis 03/11/2004 [I 02/25/2004 02/26/2004 03/11/2004 [TR 02/25/2004 02/26/2004 03/11/2004 oss ooze 02/2512004 02/26/2004 ove 03/11/2004 azsaoos oan 02/25/2004 02/2612004 owas 03/11/2004 Insance: instance: WIRRo0o0Rs8z8s3T009n H IM_MNO1539233 3M MN01539233 ono L0001958-0021 wos L0001958-0022 nas L0001958-0023 coms C0028106 cnr C0028107 con C0028108 woLIQUID woLIQUID woLIQUID ogin wa Tes Water Tdp Blank waWater Tmo Trip Blank Low Spike vw Tose Water Trip Blank High Spike amis 02/26/2004 ovr 03/11!2004 cman 02/26/2004 oun 03/11/2004 [-- 02/26/2004 03/11~004 saraon 2/27/2004 fin Login.rpt RootesFaFn0aa04 TA Report Version: Feb 20 2004 "11:35AM Page 4 of 4 CROENNFINDEENRTICAOLUNSTUYBDJIESCTTRITC0TACPORUORTTE.CNTG.IV2E7 OORuD1E0.R28E8N6T3ERED N CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00008833 ross Instance: rostio0 R0088309 [Rawmaorssnzss 3M MN01539234 Ey)gen N,, CHAIN ORF T CPUSTEODAYNALYSISREC ro CCHHAAIINN OOFF CCUUSSTTOODDYY//AANNAALLYYSSIISS RREEQQUUEESSTT FFOORRMM `CClliieenntt ((nnaammee &&adaddedersess)s:): 3M Cottaqe Grove 10746 Innovation Road `PPrroojjeeccttMMaannaaggeerr ((NNaammee && EE-mmaadilAAdddrderessss)):: __ Kent Lindetrom kdindstrom~,mmm.com Cottage Grove, MN, 550~1 ~...... Project Name: e esn e e n Lm i crnes Phone: 651-768-1206 Fax: 651-458-2029 Sa.mpler: Cottage Grove Activated Carbon Testing. P.O. #: E04-0t2~2-~ Quotation Please fill out this form omplete/yto ensure correct analysis and proper handling of your samples, Te GPL ANALYSIS mi. E l =m=eR rr E eihEr se -e ----iITHH essay SAIN OF iCISTOnDY di) -- Hlcpm=crag, -- come-- ES Co Results Deadline: At > aBr |Emssrii)on Laboratory Report Options: S CouPTAL.R sie 04 poTEETORERENTERECE CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 fp 3M_MN01539235 11993399..00008844 Exygen CCHHAAIINN OOFF CCUUSSTTOODDYY//AANNAALLYYSSIISS RREEQQUUEESSTT FFOORRMM Ee oa Client (name & address): 3M Cottaae Rates 10746 Innovation Road Coton Gove IN SE01E Cotta,qe Grove, MN 55016 Phone: 651-766-1206 a Fax: 651-4~8:__2.~L29...... ae Sampler: EE gre ero re Project Manager (Name & Dmait Mttress): Kent Lindstrom EET ProkjrleinctdNsatrmoem:~mm.m,com Project Name: Cottaqe Grove Activated Carbon Testinq a R P.O. ,~: ~R o~-~x'-- -'R ~'~,~(-- ~_ ---- __ Quotation #: Please fill out this form omp/et#/yto ensure correct anatysis and proper handling of your i Page ............. of EE i II} ET D a Te M-| [eepinceTcheeSpecna |3] tBI Unit 4 Port A Lead (Port 4A) Unit 4 PortA Lead (Port 4A) Du Unit 4 Port A Lead (Port 4A) Lo, emma LINE EE UUnniitt 4 Port B Lead (Port 4B) C ere e e e EH HEH 4 Prt A Lead (Prt 4A) Hic I H fo [comms [0 Unit 4 Port B Lead (Port 4B) Lo~ Unit 4 Port B Lead(Port 4B) Hi~ EEttTTaulli]] rtigiBe, t]) |sermr Date T~e Result; Deadline: Laborato~ Repor~ Options: -- Tm 1 | sn sR CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 3M_MN01539236 11993399..00008855 ExN ygen,, coi rcusrn onvmiaurss reauest rors CCHHAAIINN OOFF CCUUSSTTOODDYY//AANNAALLYYSSIISS RREEQQUUEESSTT FFOORRMM SZ = ` hse irs to Ett ER = esa Aeer Sree ' eames rey or emeerie | BlEm Ses fP SoAnMeP]LE AE NALYSIS E LIl e le e ie eEemmemEeeRH eeH e HHHe == -- tH I CHpAss INOF> CUSTToeOTDYee lcacy [IT iy ri Ee [OTe GRATE ---- im fBoarmmaen R CONFIDE ENTIALSSUBJES CT T0 h A PROTECTGRIOVEER ENTERED HENNEPIN COUNTY CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 swmersizs 3M_MN01539237 11993399..00008866 MMaarrkk AAmmmmeerrmmaann From: mmSent: :To: Eee Cc: Subject: mm tmgallowayl @mmm.com TFREEERSToIenr . Friday, February 27, 2004 10:12 AM SE mark.ammerman@exygen.com EE bmader@mmm.com; krlindstrom@mmm.com; plferretti@mmm.com CoC 2/25/04 cn, oC Influent Phase 3 2.25.0#... Mark - attached is the CoC for the influent phase 3 sample. any confusion this may have caused. Sorry about (See attached file: CoC Influent Phase 3 2.25.04 .pdf) The travel blank was not listed in LIMS, and therefore did not get a CoC created. I spoke with Brian Mader this morning, and the travel blank will be added to the LIMS system. A CoC will be created and enclosed with the next scheduled sampling event (3/8/04). Once again, sorry for any confusion this bringing this matter to our attention. Tina M. Galloway 3M Cottage Grove 145-i US-MNCG05 Tel: 651-768-1206 Fax: 651-458-2029 email: tmgallowayl@mmm.com may have caused. Thank you for CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00008877 3M MN01539238 -_-- ; \Pereg cHgisoeeRRsee esseBeaairrncchhdn. Proven Results. SSaammppllee ""CCoonnddiittiioofni UUppoonn RReecceeiipptt"" FFoorrmm Pproottooccool ls______ mM EExxyyegecnn SSttuuddy#y# acaoasoa~bqt~y DDatae&&tTTiiemmee RReecceeiivveedd __AH z2 fralee 425 CCoonnddiittiioonnooff SSaammpplleess __ tlt otras TTeemmppoorraarryy SSttoorraaggee LLooccaattiioonn puso sis WIniitviaalsls&&DDuatee lesfaly W Wayabyiblilll ## Tr25 pst or93 ~ CCoommmmenenst:s: _ oo whdii d ad t geod de Lord pp lfdime curly centyheen He fine soage fo comple J login fleefog op TT MMaayy 2244,.22000022 33 0 NORD proceso Sample ondept `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV27EE-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00008888 058 Rc's{,arc h [ )rix~, GRE ate College. I?\ 1~31)I. t %\ ~11.Epp : 800.21H 121q SW_MNO1839239 3M MN01539239 ----r-- ere-------------- SECTION D `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALUL-N- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00008899 33MM_MMNNO011553399224400 Eh. En EB RAW DATA REPORT Gh. oy rT i As~ rr EE 25 7367 116O6 41297 10000 1000 100 100 IOO 100 20~ 200 200 100 100 t00 1035 1330 9427 1000 10OO 100 1000 100 100 100 100 ND 919000 * 53900 52700 500000 500000 23000 25000 175^ 162^ 148^ 3000 3770 .36^ 90 462 398 387 7840 74700 10000 100000 13400 12600 11900 100 1000 100 100 100 1000 250 - 1ooo i00o 18o 1oo 1oo 20700 100~0 15600 15300 1570O 23800 10000 82 107000 100000 91 45900 47300 44300 E-- 1oo lO00 100o 1oo 100o 129000 1080OO 83 * I0e000 $15OO 10000 56 ND 12500 lO~O 125 pr 77700 106000 78 PE -- sale `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTTT.EECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00009900 aW_Notssset 3M MN01539241 IIAWDATAREPORT r woeC w enBE 1738 13789 5O 100 42736 85438 1000 342142 57617 2290 85028 58932 123658 115423 100917 29298 200 24224 42512 11600 48556 13400 52029 322432 297100 14500 298313 13232 28100 1oooo 165 16338 iooo 120000 100000 108 21925 31624 41830 40608 1oo 47456 13100 I0000 130 lOOO 47234 130000 100000 130 1oo too 40521 1oo 44693 IOO 1000 233473 54279 39560 33768 5410 6910 15200 107000 1oooo lOOOOO 1oo 30518 1oo 27073 150817 4420 157839 4640 4720 54634 15300 10000 109 1ooo 40009 109000 100000 105 100o lOOO tooo lOO 30100O 2980~0 319000 ioo -- SE FEES 1oo lOOO 3630O0 I ~0000 62^ * 100000 3180O0 10000 170 NQ TT 11000 134000 10000 100000 116 134^ Liar,= (I/x Slope = 332.081 enBald CCHEOONNNNFEIDFPEIINNTDCIAOELU-NN- TSSTUYUIBBDJJIAEESCCTLTTRTITCOOT AACPOPRUROROTTT.EECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00009911 su umorsssze 3M MN01539242 = I ~ Stray No: L|95~ == RAW DATA REPORT fea aw lnjec~oa Volmr~: 40.0 mL 5.0mL -- - [= . 030504A-401 030504A402 030504A,403 030504A404 030504A-405 030504A-406 030504A-407 Co~c. Dilution o 50 250 500 I000 I0000 I000 1oo ioo ioo 2o0 200 100 I00 I00 Recove~ 147 97 98 96 108 to0 .4^ 1000 100 I000 5O 1000 IOO IOO 1oo 1ooo IOO 1oo Ioo IOO 1ooo lOOO o^ 149 476 $170 77500 30100 29300 101000 100000 31100 86700 10000 1ooooo 25200 96 145000 100~00 123 36900 4O000 32900 iooo 126 * 100(300 ND I0000 o lo0 228 5500 I0000 55^ I000 186 46200 1000~ 46^ lOOO 3509 amount =~d (ppt) EERE en Boel CCHEOONNNNFEIDFPEIINNTDCIAOELU-NN- TSSTUYUIBBDJJIAEESCCTLTTR ITTCOOT AACPOPRUROROTTT.EECNCTGT.IIVV2EE7-OO0RR1DD1E0E.RR8EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00009922 su_wmoresezss 3M MN01539243 RAW DATA REPORT = --_---- = 47.2 $0 94 4630 4550 4560 EEE = IO200 IOOOO 6200 6120 6340 100000 ND 95600 TE 1oooo~ 96 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTTT,EECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00009933 IM_MNO1539244 3M MN01539244 RAW DATA REPORT XC030504-0 XC030504-3 (ppQ 0 25 100 250 lO00 Factc~ rE (pptt ND lw ~ppt~ lOOOo 1o0o 1o0 lOO lo0 1oo 25 200 200 2oo 1oo 1oo 577000 500000 108 9440 10o00 94 27500 25G00 96 25200 25000 90 18200 I0000 48^ 13400 113OO I000 I00 Iooo ND 11200o 10000 10000 100000 LI95g-12 Port 4A High Spk IOO 100o Io0 IOO 1o0 1o0 1oo 100 1DO0 IOO0 100 ioo 3340 10900 72100 1oooo IC0~00 2610 2730 290O leOOO 84 iiiooo iooooo 108 37700 40500 pg 500 030504A-~71 030504A-t72 030504A-,173 anvunt a~ded (PPO EERE. 1000 IOo0 123000 46109 1O000 1oo lOOO ND 10900 1O000 109 104000 I00000 104 SmndardC'wv:Liatar(l/xwdght~d) hatetce~t ffi 66.8162 SIoFc = 24.1350 ell COENAFINDEEPNITICAOLUNSTUYBDIIESCTTRITCOTACPORUORTT.ECNTG.IV3E71O0RD2E8R8E6N3TEREDIN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00009944 swmorssszes 3M MN01539245 EE -- ~ E SANNT Soacrceo nmso AnFaex Sse3z1rz151800 ~ ~ .~ ~/~ ~.: c: ~.q 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 E~In~ternal Chain of CustodyForifcaSdhoeent Internal Chain of Custody/Fortification Sheet BcosuNabe Los Ns: Wir Exygen Study Number: L1958 Matrix: Water SorSuir Kn 5 Sponsor Study/Protocol No: N~A To me Hod lo reemes fomegreKro. The samples listed below were removed from refrigerator No. Toe 0850 ne 34570 ins CH Time 0~ Date ~ Initials ~/ [CLICELINENTTSSAAMMPPLLEETIDD TT -- -- i-- ---- ------ na C osemsane wo[os] ila a osmsasT Too [we] l~a FERXVYGGEENNTIDDNNUUMMBBEERR 0106020 Control 0106020 Spk A 0106020 Spk B |] VVOOLLUUM MEE(~mmiL)) |[ FFOORRTTIIFFIICCAATTIIOONN ((nagg)) 40.0 40.0 2.0 40.0 20.0 Irffluent 3 [omens| tesssioTwo Twn | Comb Effluent 1/2 -- ry---- TS----r------ Port 4A re 1 ownsar ToeTimo] Port 4B mei stimo TooTow Influent 1/2 ete 1wm we Influem 3 [tm dosing we Influent 3 eso 1 masTe Influent 3 Dup sims | men Two Influent 3 Low Spk tigen| ma Tee Influent 3 Hi[h Spk cmtmanis | bows 1 we | Comb Effluent 1/2 cmbemaanis| wowing Two [| Comb Effluent 1/2 [Goemeninoe| tome | wo [| Comb Effluent 1/2 Dup [ConEte bow | poser |e Comb Effluent 1/2 Low Spk [Com pteeriaigsp| wwses woo [| Comb Effluent 1/2 High Spk Co fenTomwe o s Port 4A rea doeTwo Port 4A [rwoe TT wes wo [1] Port 4A Dup [heatsTes wo i Port 4A Low Spk Crimes Twos Twp Port 4A High Spk L1958-17 Spk C L1958-5 Spk D L1958-9 Spk E L1958-13 Spk F L1958-1 SpkG L1958-17 L1958-17 P.ep L1958-18 Ll958-19 L1958-20 L1958-5 LI958-5 Rep L1958-6 L1958-7 L1958-8 L1958-9 L1958-9 Rep L1958-10 L1958-1l L1958-12 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 ~.0000.0 400.0 1000.0 1000.0 400.0 [-- om--a--n--| r rooriotonyms) |m0r coosmTemre |1 TT ) 0106020 Spk A [ooensn|romossmeges) |sou contence | (2 onl 0106020 Spk B [issn simmer fous on renee | V0 Cafehll L1958-17 Spk C [omessin Tom | io ca ote |n A fat L1958-5 Spk D S Er T Ter 27 L1958-9 Spk E [useniar 1romero ages) | ious coureansens |VE oalobty L1958-13 Spk F ----r----T-- TTWE L1958-1 SpkG Spiking Solution Used F012004-10 (10 n~/mL) F012004-9 (100 n~/mL) F012004-6 ( 100000 n$/mL) F012004-8 (1000 n~jmL) F012004-7 (10000 n~/mL) F012004-7 (10000 n~mL) F012004-8 (1000 ng/mL) Volume Used for Spiking 200 ~tL (200 pL micropipet) 200 gL (200 ~aL micropipet) ~00 pL (200 ~tL micropipet) 400 ~tL (200 pL mieropipe0 100 p.L (200 ~tL mieropipe0 100 laL (200 ~L mieropipet) 400 laL (200 p.L micropipet) Aten wsmses TATinlml eseamp0]Je00s0w00ere measured: ouDeate_3/,5/84. Age 3% After meast~hng samples were returned to re,rigor_at~oy No. __ wInaittiasls _ EH sA Initials Comma mt int i one s BOSISI Comments: 200 itL of250 rag/mL sodium thiosulfate was added to all samples before spildng, lnitiah/Date: Anais Summarys owBBaaasssee _= C3=USIUA Analysis Snmmary: Data Set: Data Set'. Data Set: ~)1~/.,~-i~IL~ t~ ~ " ~ i Set extraetiordanalysis data verified by: (~ ]~F 3wmaodud 3 Hh, rbeidnseo= s ae IInniteials/DDaatte:: B/wajia]od Initials/Date: Initials/Date: Date: Suis `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00009955 _MNO1S39246 3M MN01539246 Exygen rr 3058 Research Drive messin Phone: 814-272-1039 State College, PA 16801 Fax: 814-231 - 1580 SAMPLE EXTRACTIONANDANALYSIS TRACKING SET SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET emma a at 1 EXYGEN STUDY NUMBER: L1958 METHOD: ss PR.OTOCOL NUMBER: NA MATRIX: Water ANALYTES: CA, C6, C7 & C8 Acids, C4, C_6 & C8 sulfonates Client ID [Foerm1m=e= TP orrTa e y[ame e| em|wn] na Free Hee | na Eee HTTo me 0 na [ F eas e Tumnse [11m Ba ||m -- e -- Comb Effluent 1/2 Port 4A EeH e e Fe T e ry rr Port4B F e eet He e = Influent I/2 lnfluent 3 F e me e e e H e ee ie lnfluent 3 LOw Spk hflluent 3 High Spk rn nr ne cf a i | Comb Eftluem l/2 FEEame ee Comb Effluent 1/2 Exygen ID 0106020 Control 0106020 Spk A 0106020 Spk B L1958-5 Spk D L1958-9 Spk E L1958-13 8pk F L1958-1 Spk G L1958-17 STEP 1 STEP ,2 DiMtiorts (mL/mL) -~ - STEP 3 [ [ Dilutions (mL/rnL) - STEP 4 -~ O"tJlO " _ *"AO - '~/tO ~ ~O~t*,0'~ " geagenLs Materials Metlmol Ct8 Sl'E "Iyp I Water Initials/Date 1.1958-19 L1958-20 LI95g-5 L195g-5 P-.ep a a'aO,'~t.O e ~ - ~0~t0,"'~tl.0 i Lot # NA Comb Effluent 1/2 Dup Comb Effluent 1/2 Low Spk Fe HHe m H a Fema Comb Effluent 1/2 Port 4A El# 1 Spk L1958-6 Ll958-7 uesse L 1958-8 L1958-9 FF ee H e HR R = Te e me ] ] [roaPom rt4As Dup [rma venTV Ty ee Ye Port 4A High Spk ussen L1958-10 L1958-12 TTT O'~|0 Ree ~O'~/it).a'l/I .O ~0"~ ~0aA, ITT / ~/ ~S 05 "g07 "~TE/T ~O'YtO 0"1!1,1) - - " = annrLte-- | 17 . 1 va| Ammoraum a.... a | - *Initials/Date ~]S/~ OSI BEETNEIL S eee ESm ER Campuses! TEP2. Fmalvolumeto5 mLenllectedtn lSmLpolwrotmlenetubes ~',~. q ,^ .... -~ ,~'-'~. } Initials/Date ..... ~,~. mBa EEssesQi , HER where *~tialsanddate~ehsl~indicates~epe~o=el~tperro=~sst~. ~, 10~0 ~ e 2.TOI $$ Me~od of ~talysis for the D~emination of P~fluor~c~ne sulfo~ (PFOS), P~ugio~mne sulfonyl~de (PFOSA) and P~fluoro~oate (POAA) in Wat~ coma CO~ENTS: Foesc eigeu n Ss w: 2_owe: 3/57. rr July 19, 200l/4 fGONrIDEeITAAL SpUATBOAPJROTEECTIVCE GRTOGR ENTIN HEENNREP ECOUDNTY CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 swmorsozer 3M_MN01539247 11993399..00009966 Ee os sugyNi unter InCtW LeiragHshl CEainN ofCSustocdyFoortifticonatShipeosntresFoc 1423 150 Exygen StudyNumber: JY ~ .~.~ ossrewanme State College, PA 16801 Phone: 8142721039 Phone: 814-272-1039 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet L1958 Matrix: Water Te URSS 3750 Sponsor Study/Protocol No: N~A The samples listed below were removed from refrigerator No. Time 0~'0 Dale was_H Initials ~ [coECLNIENTT sSAM oPwLEEID_TexvEXoYeGEnNiIDn NNUuMmBeERr TVVOOULUUMMEE((mmiL)) |I FFOORRTTIIFFIICCAATTIIOOI~N"w(ngg)] [PonPs ort 4B TeL1s95s8-13 Two 40.0 1 [rmaPon rt 4B ToLs19w58i-1i3 eRegp | w40e.0 [eosTeTe] Port 4B Dup L1958-14 40.0 ITTT TTSE ETSI Port 4B Low Spk [ponspmignsp | L1958-15 wwLe19s5s8-a1s6 | 40.0 4w0e.0e | CT tweeTos wee e Port 4B High Spk lnfiuent 1/2 L1958-1 40.0 [mewn Influent 1/2 CLw19s58i-1 rRegp | w40e.0 [oteeIwnfluientn1/2oDuep | wLe19s58e-2s Tee 40.0 EYTYP hafluent 112 Low Spk LT1T958-3SY 40.0 S [Toto ia ignspk| tL1e95s8-4a | w40e.0 |] [pou Influem 1/2 Hi~zh Spk weL1s9s58a-21r | w40e.0e |] [rpblloTriwp Bslanpk ke| weL1s958-22 | w40e.0 Io] [pbusTkripmBglanpk LsowpSipikee | wLv1o95s8-e2x3 | w40e.0 |] -_ Trip Blank High Spike Tr rr 1 -- rr 1 -- rr rrr rr rr 1 T -- p ---- ) rr rrr ------ mT 11] 1 [SC pSipkikiinn~gsSooiluwtiioonnUUsseedd |VoVloulummT eeUUsseedd ffoorr SSppiikkiinngg| iInniiatitatl/oDaattee| rr r T 1 rrr -------- rr 11 ------ r------ -- TT rT Tr 1 -------------- --------1] TBE All samples were measured: Time ,/0~(1 ue _3/5/4 Date I1 _7/S"/6r~/ wis_EH haidals mR ok irk AerAfter mmeaseuringssspamlpeelesswweyrereerrieetumrneneddtyo re,frigprator nNoo. ._33~2" wiiaEHs Comm smn tn testi oH Comments: 200~tLof 250 mg/haL sodm' m thi"osulfate was added to all,amp,es before,pi'ki"ng. ,m"O'als/Date: .11 , AnalytSummary: Dua sec DBS. nse: 4 oafelod mar Data Set ~ (~L~k Dua = fro t a Data Set: - a = Data Set: .~- Imtlals/Date Initials/Date: Initials;Date: a "Ha7giasoe Set extraetioWanalysis data veri~ed bye/. Date: /luly'26", 20t)1/6 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00009977 _Motsao2es 3M MN01539248 E MN oem Se 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 A SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET enob e amsnnann EXYGEN STUDY ~ER: L1958 METHOD: i~ PROTOCOL NUMBER: NA MATRIX: Water ANALYTES: C_4, C6, C7 & C8 Acids, C4, C6 & C8 sulfonates A Port 4B Port 4B A et ee Eer e e eree ER Port4B Dup [emia visas TT wpT= -- Port 4B Low Spk ee Port 4B m~ Spl~ FEE me) Lrffluent 1/2 N=SN !nfluent 1/2 eee [tematoms Influent 1/2 Dup Influent 1/2 Low Spk E Es ee hafluent 1/2 Hi~la Spk FT e Eme Trip Blank ee e Trip Blank Low Spike manshee Trip Blatlk Hish Spike Exygen ID L1958-13 L1958-13 Rep L1958-15 L1958-16 STEP 1 STEP 2 I ! Dilutions (mL/mL) oat'e,a'A'o ~)#'~ ~'4/t D 03/~ ~*,~,0 STEP 3 Dilutions (mL/mL) "-- -- STEP 4 Reagents,' Materials Type I Water TN L1958-2 | wwsss | 7% 7%,YO I I 7 Initials/Date ~ "~Oi0(~g~ 0 TT Qek ol | |. |-| L 1958 -21 ~ L1958-22 ~ '~10 Lot # /g3.~33q~ bv'337-7 g / (= 277 | --1 -- r f r tC t E f ----a -- eeTabi | e TT ein| a Elo2Tsomeer | m T--TB 7 |Ecue llns ofthe] =| | sre[cold| STEP 1: SPE oltmm clean-up (omitting 40% wash) os STEP 2: Final volume to 5 mL collected in 15 mL pol)propolene tubes STEP 3: Lc,q~IS/MS analysis hans, yD om eC HH STEP 4: LC~IS/IVIS reanal)~is. FE rrrtre a cern cCo00n27n26e2 ENE, $$ Method of Analysis for the Determination of Perfluorooctane sulfonate (pFOS), P~fluorooctane sulfonylamide (PFOSA), and Perfluorooctanoate (POAA) in Water LiCOMMENTS: Find coms eieine33 seEHowe fff , July 19,200 i,'4 Sum sep CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 3M_MN01539249 11993399..000098 p==Sponsor Sample E NT ose [-- 3058 Research Drive en ose pi State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 E FREPAeRATInON OF EXTRACTED CALIBRSATATNIDAORDNS: PREPARATION OF EXTRACTED CALIBRATION STANDARDS i: ---- po Protocol No.: None -- a Mamas eve Ba Method No.: .~ wr Tr Ty Exygen Se | Sdn | aon | Vote ta | shan [w] Sample Sample Exygen Study No.: Analytes: Fort. Solution Fort. Soln. Conc. NA C4.C5.C6.C7 and C8 Acids; C4 C6 & C8 Sulfonates Fort. Volume Micropipet used FOgt. Level Matrix: Type I Water~ Sample VoI: 40 mL Final Solution Reagems/ Lot # [aTooeon0 [perme|1-1. ID ID Description ID (n~/mL) /~L) /~L) fPPt) NA 0106020 Type I Water" ID # ** Materials xouesies | vebant [433053] [xa|ovosoz0 |myperwaer[vorosie| 0 | tee| ae| as | XxcCm03e0s5o0e4-r0 | ciMeethsanol Ware)| NA 0106020 Type I Water~ F012004-10 10 100 200 25 XC030504-1 1218 SPE {aToiosoz0 |"peiwater [rorzoosie | 10 [aw am so |woomwsoer |mpeiwaer| wa | NA 0106020 Type I Water~ F012004-10 10 200 200 50 XC030504-2 Type I Water NA [oun oioso20 |"rype water [rovzonaie| 10 | aso | a0 wo [wowmsoes |] NA 0106020 Type I Water^ F012004-10 10 400 200 100 XC030504-3 NA 0106020 Type I Wate~ F012004-9 100 100 200 250 XC030504-4 TO IT ST ETE BT NA 0106020 Type I Water" F01201M-9 100 200 200 500 XC030504-5 [naToro | ypewater|roraons[0| w00|a0[wow[nesses NA 0106020 Type I Wate~ F012004-9 100 400 200 1000 XC030504-6 --] [| 1 1 1 -- TT11-711 yi Vertical arrows in a column indicate identical values. a ame ae YC **This must be a unique number. Use this system." Extracted Calibration Soln [D #: XCMMDDYY-O, 1,2,3. etc. er et ae ir BI 3p Samples removed fro~ freezer # 5~ Time: STIS, | en GA 40 mL of each sample measured using a 20 mL graduated cylinder. Initials/Date: Initials!Date: rors Sore won 1 After measuring, samples returned to @ / freezer # ~:~: Time: InitialsfDate: ~/- Seo etd ne Be Sh Samples fortified: Initials/Date:~ STvs on SPE clean-up (omitting 40% Wash): a Final volume adjusted to 5 mL: Erbe 33 anton ST Ye oo TON A _sin0s Extrams placed in refrigerator # ~" initials/Date: ,.,~"3-t~// Initials/Date: e'-~4 Initials/Date: ~"/~ /~</' / / :~/,.~'/~-/ Initials/Date: STANDARD EXPIRATION DATE: 3!19104 I Comments: ^This type I water has been filtered through a hypercarb filter Bt irom TSA $$ Mefliod of A~mlysis for the Detemfination of Perfluorooctane stdfonate (PFOS), Perfluorooctane sulfonylamide (PFOSA), and Perfluorooctanoate (POAA) in Water rion July I0, 2001/0 GfONrIDEeITAAL SUpBJEACTTOA PROTECTIVE GROGR ENTERED IN HENNEP COUNTY CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 swmorsoszso 3M_MN01539250 11993399..00009999 ote Masslynx - Sample List FERS Eonmacan Sample List: C:~MASSLYNX\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM.SPL Printed: Fd Mar 12 15:42:23 2004~'~. M "~,,.'~' ExEyxyggeennsSuTUoDyYNNoO., LSB -- Page 1 PPaaggeePPoosstitoionn:: ((11,.11)) Pt 80 Ci sm ectn Vial File Name LIMS ID ClientID Sample Description PimmmmsoCo m BEm NEa ER 1 1 030504A-401 ..... Ig - mE 2 2 030504A-402 ..... PIER C gmusmss 3 3 030504A-403 ..... PPiEEEEER - gmdwEs 4 4 030504A-404 ..... C C BEMEER 5 5 030504A~05 ..... PiEEE- oc EmERES 6 6 030504A-406 ..... XC030504-0, 0 ng/L Standard XC030504-1, 25 ng/L Standard XC030504-2, 50 ng/L Standard XC030504-3, 100 ng/L Standard XC030504-4, 250 nglL Standard XC030504-5, 500 ng/L Standard a Si Conc Gore Gore Tton Matrix Sampla Type Conc(ng/L) Conc B ConcC Test lD DF OC gBmRO:go: g o-o | -- Standard 0 --- ER OC: -- Standard 25 -- CoE 5 - C fd -- Standard 50 --- BE OB oc oof --- Standard 100 -- CoE OE Oo: fo | -- Standard 250 --- CEE OB o-oo -- Standard 500 --- o 1 o 1 o 1 o 1 o 1 o 1 7 7 030504A-407 ..... XC030504-6, 1000 ng/L Standard -- Standard 1000 --- o 1 8 92 030504A-408 ...... 9 11 030504A~-09 ...... pEEERT 10 12 030504A-410 ...... 11 13 030504A-411 ..... 12 14 030504A-412 ..... Borsmbic oo 13 15 030504A-413 ..... EEE 14 16 030504A-414 ...... fig: 15 17 030504A-415 ...... 16 18 030504A~416 ...... jig: 17 19 030504A-417 ..... - 18 2 030504A-418 ...... Pale: 19 20 030504A-419 ...... - 20 21 030504A-420 ...... Tamme: - 21 22 030504A--421 .... 22 23 030504A-422 ...... PESEEC C 23 24 030504A-423 ...... PEEEEC C 24 25 030504A-424 ..... PimmEc 25 26 030504A-425 .... 26 27 030504A-426 ..... 27 28 030504A-427 ...... 1PE:E5E:- - 28 29 030504A-428 ..... 29 30 030504A-429 ..... Pig 30 31 030504A~30 ..... BigaEEs: 31 3 030504A-431 ...... Methanol Wash -- 0106020 Control --- 0106020 Spk A, 50 ng/L --- EEETaw cE BoC ood 010G020 Spk B, 500 ng/L L1958-1~Spk C, ~ ng/L, DF=IO00vn..f~:~)"--- Gemcmmenal X00 mmc - 1 L1958-1~'Spk C, 2.T~O~ng/L, DF=1000 U~)-- mEEEEese BoBC Cf OB L1958-5 Spk D, 10000 nglL, DF=100 --- mmmEaER CF 0B - Cf 8 L1958-9 Spk E, 25000 ng/L, DF=100 --- L1958-1,3 Spk F, 25000 rig/L, DF=100 --- Eas cL. PF -: | E L1958-11[ Spk G, 10000 ng/L, DF=100 -- XC030504-1, 25 ng/L Standard -- Ean =: ly L1958-1,DF=200 -- L1958-1 Rep, DF=200 --- EEE IE: 1 8 L1958-2, DF=200 --- L1958-1, DF=100 --- BNRdNee CT AE - - Ci 8 L1958-1 Rep, DF=100 -- mmEbeguc ME oC CoD fF L~'534 2, DF=100 L~,~,~,-Z i~ ,, EEL SEE oc oz oz ff L1958-1, DF=10 L1958-1 Rep, DF=10 L1958-2, DF=10 ~ i~\~t~l~ i ,. ~ --- Er IE eC il Ek L1958-3, DF=1000 -- mEm SE om o-oo} E L1958-3, DF=100 --- EER. CEL BCC} R L19584, DF=1000 --- =Eo E Sof E BUE C Cb XC030504-2, 50 ng/L Standard --- Blank Blank QC QC QC QC QC QC QC QC Standard Analyte Analyte Analyte Analyte Analyte Analyte Analyte Anelyte Analyte QC QC QC Standard ..... ...... 50 -- 500 --- ~ --25~0(~0.9,)=9~n~ ___ 10000 --- 25000 --- 25000 -- 10000 --- 25 --- ..... ...... ...... ..... ..... ...... ..... ...... ..... 10000 -- 10000 --- 100000 --- 50 -- o 1 o 1 o 1 o 1 o 10000 o lOOO o lOO o lOO o lOO o lOO o 1 o 2o0 o 2o0 o 2o0 o lOO o lOO o lOO o lO o lO o lO o lOOO o lOO o 1000 o 1 32 32 030504A-432 ...... L1958-5 .-- Ana[yte ...... o 1 33 33 030504A-433 ...... 34 34 030504A-434 ...... FORBSENNT CT Ue S8 mm II 35 35 030504A~,35 ..... PiEEEE.c - EEEERE... CEEE. BFB i o- c C}}B 36 36 030504A-436 ...... 37 4 030504A-437 ..... 38 37 030504A-438 ...... i i@Eowmomma-n =-o E EEE R R:faow := =ozo:siw B 39 38 030504A-439 ...... Pigmmc ED ESE 40 39 030504A-440 ..... 41 40 030504A-441 ...... Hi ERREE E:ECER " EEBCEEEtiA t 42 41 030504A-442 ...... L1958-5 Rep --- L1958-6 -- L1958-7, DF=100 -- L1958-8, DF=1000 -- XC030504-3, 100 ng/L Standard --- L1958-9, DF=100 .L---=N~.4-~Rep, DF=100 L~q..~.-~l"{~ . ~ L1958-10, DF=100 L1958-9, DF=10 L1958-9 Rep, DF=10 ~)(~"~1~._ Analyte Analyte QC QC Standard Analyte Analyte Analyte Analyte Analyte ...... ..... 10000 --- 100000 --- 100 -- ...... ...... ..... ..... ..... o 1 o 1 o 100 o 1000 o 1 o 100 o 100 o 100 o 10 o 10 43 42 030504A-443 ...... L1958 10, DF=10 --- Analyte ...... o 10 44 43 030504A=444 ...... Osh L1958-11, DF=100 ist--- QC 10000 -- o 100 Cr ONIGEATAt L.$4817p 104 PeROTECTIVE ORDER TERED I HEANEPN COUNTY CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 nme 3M_MN01539251 11993399..00110000 isan ET Masslynx - Sample List Sorpes unsa on PROSaneOSDACOACSMS ExygensTupyNO _LAISD. Sample List: C:\MASSLYNX\Fluoroche[nicals.PRO\SampleDB~030504A CG ACSFM.SPL ai Ed -- Printed: Fri Mar 12 15:42:23 2004 . .L~ ~--I I ~ Exygen STUDY [ET MS Method HPLC Method 1 Gnoociisur ges 1 C68 ACIDS C4 6 8 SULF pfbswater ISSR ma 2 C6 8ACIDS CA 6 8 SULF pros water i GEEERE EE 3 C68 ACIDS C4 6 8 SULF pf'os water 4 C6 8 ACIDS C4 6 8 SULF pfbs water PogiERn mm 5 C6 8 ACIDS CA 6 8 SULF pf~s water i ognanny mn 6 C68AClDS C4 6 8 SULF pfbswater oEmEmEany mur 7 C6 8 ACIDS C4 6 8 SULF pf~s water i ogmmanny mu 8 C68 ACIDS C4 6 8 SULF pfbs water 9 C6 8 ACIDS Czl 6 8 SULF }fbs water bh Sided mmr 10 C6 8ACIDS C4 6 8 SULF )fbswater Susman mor 11 C6 8 ACIDS C4 6 8 SULF )fl~s water id Quem mmr 12 C6 8 ACIDS C4 6 8 SULF fibs water guano "13 C6 8 ACIDS C4 6 8 SULF ~s water Sumani mn '14 C6 8 ACIDS C4 6 8 SULF }fbswater git am t5; C6 8 ACIDS C4 6 8 SULF }~s water 16 C6 8 ACIDS C4 6 8 SULF )fbs water # gusmanay mmr 17 C6 8 ACIDS CA 6 8 SULF ~s water Suemgnay mmr 18 C6 8 ACIDS C4 6 8 SULF fibswater 3 Snemanar mn 19 C6 8 ACID8 CA 6 8 8ULF ~fbswater 3 Susman Amr 20 C6 8 ACIDS CA 6 8 SULF ~fbswater 21 C6 8ACIDS CA 6 8 SULF ~fbs water I GUSH Mii 22 C6 8 ACIDS C4 6 8 SULF )fbs water 23 C6 8 ACIDS C4 6 8 SULF }fbs water gusmanar mmr 24 C6 8 ACIDS C4 6 8 SULF )fbswater guemeni nn 25 C6 8 ACIDS C4 6 8 SULF )fbs water ommnne am 26 C6 8 ACIDS C4 6 8 SULF )ros water guemEni or 27 C6 8 ACIDS C4 6 8 SULF )fbs water 28 C6 8 ACIDS C4 6 8 SULF )fbs water 3 oavemcni mor 29 C6 8 ACIDS CA 6 8 SULF fibs water gueRinl mmr 30 C6 8 ACIDS C4 6 8 SULF >fbswater 3 guemenmy mmr 31 C6 8 ACIDS C4 6 8 SULF fibs water 3 oguemoniy mor 32 C6 8 ACIDS C4 6 8 SULF )fbswater oguemon mor 33 C6 8 ACIDS CA 6 8 SULF )los water gimnnn mor 34 C6 8 ACIDS C4 6 8 SULF )fbs water 35 C6 8 ACIDS C4 6 8 SULF )f'os water Emmy mm 36 C6 8 ACIDS CA 6 8 SULF )fbs water 37 C6 8 ACIDS CA 6 8 SULF )fbswater 38 C6 8 ACIDS CA 6 8 SULF )fbs water 3 SuSRENML mmr 39 C6 8 ACIDS C4 6 8 SULF fibs water 3 ouemanmy mn 40 C6 8 ACIDS C4 6 8 SULF fibs water 8 suemnany mn 41 C6 8ACIDS CA 6 8 SULF )ft)s water 4 gnemsiny mE 42 C6 8 ACIDS C4 6 8 SULF )los water 4 gnamoniy mn 43 C6 8 ACIDS C4 6 8 SULF )f'bs water SSNS MNT 44 C6 8 ACIDS C4 6 8 SULF )fbs water ---- MS TuneFile Inj.Volume noes 15 Fiuorochems 15 Raven Fluorochem~ 15 EEE Fluorochems 15 Fluorochems 15 ams Fluorochems 15 dem Fluorochsms 15 Aman Fluorochems 15 heen d Fluorochems 15 Fluorochems 15 Re Fluorochems 15 hem Fluorochems 15 Amd Fluorochems 15 hmm Fluorochems 15 Mme Fluorochems 15 mR Fluorochems 15 Fluorochems 15 bem Fluorochsms 15 mm Fluorochems 15 ben Fluorochems 15 mem Fluorochems 15 Fluorochems t 5 heen 1 Fluorochems 15 Fluorochems 15 mem Fluorochems 15 Aman p Fluorochems 15 mm Fluorochems 15 Fluorochems t 5 Aman Fluorochems 15 nen Fluorochems 15 nmam ld Fluorochems 15 mony F~uorochems 15 Amen Fluorochems 15 hmom f Fluorochems 15 mm Fluorochems 15 Fluorochems 15 mm Fluorochems 15 Fluorochems 15 Fluorochems 15 nom Fluorochems 15 nm Fluorochems t 5 pmen Fluorochems 15 pmen n Fluorochams 15 fm Fluorochems 15 ARR Fluorochems 15 ot PagePeston:2.1) Page Page Position: (2, f CONFIi DENTItAL SUeBJEaCTtT0 A PaRO)TECTIVE OROER ENTERED IN HENNEPA COUNTY CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 aw morsuzsz 3M_MN01539252 11993399..00110011 Massy SamoleUnt. Masslynx - Sample List TT fangs Cues Dror 4s PRO\SepeOBU0SOACGACSFM.SPL Sample List: C:\MASSLYNX~Fluorochemicals.PRO\SampleDB~030504A CG ACSFM.SPL ii Halolu EE Printed: Fd Mar 12 15:42:23 2004 ~ ~)~.~ll~i~L( anorvor LE Le LEexysen STUDY NO. ~ res Page 3 PaPgageePPoostsiitioonn:: ((11,,22)) na 131 cvs Vial File Name LIMS ID Client ID 5IEEEEE a 45 44 030504A-445 ..... 46 4 030504A-446 ...... [iS - 47 45 030504A-447 .... FEiEE: - 48 46 030504,~-448 ..... Fis 49 47 030504A-449 ..... 50 48 030504A-450 ..... JES. - 5'1 49 030504A~51 ..... EEE - 52 50 030504A-452 ..... IES: : 53 51 030504A-453 ..... Bigs: 54 52 030504A.-454 .... 55 5 030504A-455 .... BaEms- 56 53 030504A-456 ...... 57 54 030504A-457 ..... 58 55 030504A-458 .... EAgEE: 59 56 030504P,-459 ..... EEE: : 60 57 030504A-460 ...... sper Sample Description UADnew L1958-'12, DF=1000 XC030504-3, 100 ng/L Standard ERY. L1958-13, DF=100 ENP L1958-13 Rap, DF=100 EIEE L1958-14, DF=100 L1958-13, DF=10 BE. L1958-13 Rap, DF=10 L1958-14, DF=10 EEEEE L1958-15, DF=100 EE... L1958-16, DF=1000 XC030504-4, 250 ng/L Standard Ems L1958-17, DF=1000 L1958-17 Rep, DF=1000 L1958-18, DF=1000 L1958-17, DF=100 EEErE. L1958-17 Rap, DF=100 61 58 030504A-461 -- -- 62 59 030504~.-462 .... 8 BMEC C0 63 00 030504/~-453 ...... 64 61 030504A-464 ..... iEmE- - 65 62 030504A-~65 .... IFREE ESH:EE: 66 63 030504A-466 ...... L1958-18, DF=100 L1958-17, DF=10 HETEU. L1958-17 Rep, DF=10 L1958-18, DF=10 EES ~_L1958-~., DF=1000 Bowe (t~'LL1958-~,~, DF= 100 67 64 030504/k-467 ..... 68 B 030504A-468 ...... 1100: = 89 92 030504A-469 ..... 70 65 030504A~t70 ...... 71 66 030504P~-471 ..... BnYo Em : -CC 72 67 030504A-472 ...... 73 7 030504A-473 .... ~-J)1958-2~, DF=1000 "-"XC030504-5, 500 ng/L Standard Methanol Wash To L1958-21 L1958-22, DF=100 BREEEE,... L1958-23, DF=1000 6-H 0 s /0% XC030504-6, 1000 ng/L Standard at Sm Cor) Gn Gc en 8 Matrix Sample Type Con(; (nglL) Conc B Conc C Test ID DF ET eT --- QC 100000 .... 0 I Bu 5 ZC --- Standard 100 .... 0 ET fot. --- Analyte ........ 0 --- Analyle ....... 0 T"EE:* i1 F8 --- Anatyte ........ 0 --- Analyte ....... 0 cE: tt -- Anaiyte ....... 0 -- Analyta ......... 0 IEEE,mi Di IEBh -- QC 10000 ..... 0 1 E. BDI fF --- QC 100000 ...... 0 -- Standard 250 ...... 0 --- Analyta ......... 0 ET lg -- Analyle ....... 0 --- Analy|e ......... 0 -- ,~nalyte ........ 0 STEEEE:OC CZ S iE B -- ,~,nalyte ........ 0 1000 1 100 100 100 10 10 10 100 1000 1 1000 1000 1000 100 100 -- Analyte ....... 0 --- Analyte ......... 0 I Mem = Tozo8 0B -- Analyte ....... 0 --- Analyte ....... 0 FF wm IIb --- QC 1~000 ..... 0 -- QC 10000 ..... 0 C EBeLe EBB I i I B -- QC 100000 ...... 0 --- Standard 500 ...... 0 -- Blank ......... 0 DoE oT o-oo --- Analyle --- ...... 0 -- QC 10000 ...... 0 zC o EBee ZZ: 817 --- QC 100000 ...... 0 -- Standard 1000 ...... 0 100 10 10 10 1000 100 1000 1 1 1 100 1000 1 fGONrIDEeITAAL SUp BJECTTOA A PROTECTIVE GROGR ENTERED IN HENNEP COUNTY CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 swmorsozss 3M_MN01539253 11993399..00110022 Massy -SamgloLit TT ee Masslynx - Sample List FREE ExygensrpvNouLAB. PagePostin: 0.) Sample List: C:\MASSLYNX~Fluorochernicals.PRO\SampleDB~030504A CG ACSFM.SPL Exygen STUDY NO= ~ Page 4 Page Position: (2, 2) MoManos MS Method 45 C6 8 ACIDS C4 6 8 SULF Susman 46 C6 8 ACIDS C4 6 8 SULF ausmsmmy 47 C68 ACIDS C4 6 8 SULF 4 guemsnnr 48 C6 8 ACIDS C4 6 8 SULF 3 ghsmamar 49 C6 8 ACIDS C4 6 8 SULF 4 gpa 50 C6 8 ACIDS C4 6 8 SULF Enea 51 C6 8 ACIDS C4 6 8 SULF ERAN 52 C6 8 ACIDS C4 6 8 SULF 53 C6 8 ACIDS C4 6 8 SULF Sams 54 C6 8 ACIDS C4 6 8 SULF giSmana 55 C6 8 ACIDS C4 6 8 SULF i 56 C6 8 ACIDS C4 6 8 SULF 57 C68 ACIDS C4 6 8 SULF 4 EiERANS 58 C6 8 ACIDS C4 6 8 SULF 3 anoRalsl 59 C6 8 ACIDS C4 6 8 SULF gifSanay 60 C6 8 ACIDS C4 6 8 SULF 61 C6 8 ACIDS C4 6 8 SULF gus 62 C6 8 ACIDS CZl 6 8 SULF 3 ghsmuny 63 C6 8 ACIDS C4 6 8 SULF gusmnny 64 C6 8 ACIDS C4 6 8 SULF gusmdity 65 C6 8 ACIDS C4 6 8 SULF 66 C6 8 ACIDS C4 6 8 SULF SGRGGT 67 C6 8 ACIDS C4 6 8 SULF 68 C6 8 ACIDS C4 6 8 SULF B BUERENUL 69 C6 8 ACIDS C4 6 8 SULF ananty 70 C6 8 ACIDS CA 6 8 SULF 71 C6 8 ACIDS CA 6 8 SULF noSIGEELNE 72 C6 8 ACIDS C4 6 8 SULF 7 oaumanmr 73 C6 8 ACIDS C4 6 8 SULF conse HPLC Method pfbs water mur pfbs water mor pfbswater mor pfbs water mor pfbs water mer pfbs water mur pfbs water mur pfbs water pt'bs water mime pF~s water mur pfbs water pfbs water aE pfba water mur pfbs water mur pfbs water Es pfbs water pfbs water mor ~bs water mur I:#bs water mur pfl3s water mms pfbs water pfbs water Mw pfbs water pfbs water mWT pfbs water mur p~s water pt~s water Sn pfbs water mI pfbs water Turin MS TuneFile Fiuorochems Amen F~uorochems Rodan Fluorochems dean Fluorochems edn Fluorochems Res Fluoroch~ms sem Fluorochems sm Fluorochems Fluorochems Ama Fluorochems wen Fluorochem$ Fluorochems EE Fluorochems Amen Fluorechems mem Fluorochems mem Fluorochems Fluorochems Rodm Fiuorochems hom Fluorochems fem Fluorochems fem Fluorochems Fluorochems owe Fluorochems Fluorochems ATI Fluorochems mem Fluorochems Fluorochems ARES Fluorochems Amen Fluorochems youn Inj.Volume i15 15 15 '15 15 15 15 15 15 15 15 15 15 15 15 15 15 d15 15 15 d15 15 1315 15 15 15 15 15 15 SCOTNRFIICDTENCTOIUALR.T:SUNOB.JE3C7T.TO10A ePR6O0T3ECTIVE ORDER ENTERED IN HENNEPIN COUNTY CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 wmorsaszse 3M_MN01539254 11993399..00110033 LCAMSIMS SYSTEM AND OPERATING CONDITIONS LC/MS/MS SYSTEM AND OPERATING CONDITIONS `SSppoonnssoorrPPrroottooccooll NNoo:: NNAA EExxyyggeennSSttuuddyyNNoo:: LL1199558 et: MicomsesQuan li (LCMSAS Unit 6) Instrument: Mieromass Quattro Ultima (LC/MS/MS Unit #6) Con: COPrMofsPVArsQ APIO Computer: COMPAQ Professional Workstation AP200 Sota NomsI Lond ys Spanso-- o Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Mieromass Limited: MassLynx 3.4 Build 004 WLCEquipment: HeToreeAFmacokanndg(11) Ss ODi0VCaomroDroegar HPLC Equipment: Hewlett Packard (I!P) Series 1100 HP Bin Pump HP Vacuum Degasser HP Autosampler HP Colunm Oven HPLC: GOenNesSCC4H. RmOVxAT21OmRiAdH,xFios(ysSoID:)4A) HPLC Column: Genesis C-8, 5 cmx 2.1 mm i.d. x4 ~t (Exygen ID: 74A) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mile Phase (4): 2 Armin Acc n Tope [War Mobile Phase (A) : } Mobil Phe (3). Vihano! got Mobile Phase (B) : 2 mM Ammonium Acetate in Type I Water Methanol | Ai TSa FeoanrPeresRcea sDaie, SFtRol0l,-PA1106801 Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 ' NNOOTTEE:: TThhee nneexxtt 33 ppaaggeess aarree ccoommppuutteerr ggeenneerraatteedd pprriinnttoouuttss ffrroomm tthhee mmaassssllyynnxx ssooffttwwaarree pprrooggrraamm.. TThhee ppaaggeess ccoonnttaaiinn tthhee | Avtar ek sb ce ' iinnssttrruummeenntt sseettttiinnggss uusseedd ffoorr tthhee aannaallyyssiiss ooff tthhiiss ddaattaa sseett.. , , . ) ` ` ` GONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTEREDIN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN NE COTY TRIE Soar N37 ure zeses HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 swmorszezss 3M MN01539255 11993399..00110044 ------ SSccaannnniinngg MMeetthhoodd RReeppoorrtt MLaMeattshhtooddM::odified: MCC:o:\n\MMAAJSSaSSnLL2YI0NNXX\\1FF5LL:UU3GO2RR:O3OC8CHHEE2MM0I0IC3CAALLSS,PRPROO\VAACCQQUUDDBB\\CC6S 88 AACCIIDDSS CC44 66 88 SSUULLFF Last Modified: Mon Jan 20 15:32:38 2003 PPrriinntteedd:: EFxrti Mvaarr 1122 1155::4444::5599 22000084 4 PPaaggee 11 SSoollvveenntt DDeellaayy (( mminnss )) :: 00..0000 AAFnnaaanllcotoiggonCChhaa| nnnn1eell 44 M::RUUMnnuuosfseedd5 Mass Pairs ( ESp- ) Function : 1 MRM of 5 Mass Pairs ( ESP- ) SSSIIptpnnaaattnrnee.trr ((TCC_ihhDTnaaaeennllnntteeoo(llnnsMsiDDee)n) llsaa:)yy (( SSeeccss )) :: 00000.....0200003003 | RESEentnpdaderatTTtiism.mTeeime{(MMi( innMssin)s) ) : : 0111.220..00000 RepeatsCChhaa: nnnneell PPaarreenntt Dbaauugghhtteerr DD1uweellll ((SSeeccss)) CCoollll EEnneerrggyy [(0e9V)) CCoonnee (V) ' 21 1 223091993..0000000 299996..000.0C0 000...222000 04100 2a490 | 23:5 333319193939...000000000 28350660.93.0..0C0000 0000....22220000 33i150 1525OO00 4 5 5 54419339i..000000 939596..900.0000 000...222000 i4"00 3i300O ' ' ' ' ` ` " a a,1tl `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTYUBBIDJJIEAESCCTLTTRTITCOOT AACPOPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00110055 3M_MNO1539256 3M MN01539256 ------ MMeetthhoodd RReeppoorrtt. MaMeesttthhooMddodFFieilleee::d: Last Modlfiedl Pprriinntteedd~: Fcie:\i\mamanasys,ssllyaymnrax\\ef1l3uu7oo,rroocs2hh00ee1mmiicc1aa5ll:e3s4.p7pr3ro8o\\aaccqquud~bbi\ppifhbss water water Friday, March 12, 2004 15:38:56 FFersiddaayy,, MNaarcchh 1122,, 22000044 1155::4435::0099 % slot rPaaggee 11 HPP1I1I0000 LLCC PPuummpp IInniittiiaall CCoonnddiittiioonnss sSootlavAvB%eennttsa 9Ts00o..o00 oBC5b%% 10o[0.'x.0030 D% 0.0 | SHFSFittllnooooppwwrTrT((eiimmsmml/see/ummriie((nn.nm))itnn(ssb))ax) 220000...00330000 | MMvFOOiavavenxeexnnnFPPrrTTTroeeeoeasmsmmssspppuuueearcrrrreeeaaattcuuu(((rrrbhbeeeaaarrrL)))LReeicfgtth(t(:(CC0))) 410O3i300550..e00 Oven Temperature Right(C) 35.0 PHP1I1I0000 LLCC PPuummpp GGrraaddiieenntt TTiimmeettaabbllee |e seediens Tinctabic containe 5 entries shich are The gradient Timetable contains 8 entries which are TTii020mm..ee500000 905AOa0%000 I11aB000%.%00 coPox% loo Doo00%.u'0 F0F00l.l.3o33o0w00w000 pPrree0i4sOs0asOsuurree ' Sl255s9 :lo5000o0000 oii91000ol0ls0000 15090I95000000...0000000 o0xoool.1s0ooo o00oo0'..'.l00s0 00000a....333333000000000000 011444000000OOO0 ' 11211440900153550000000 955O00300100000 1i1000I000100030...00000 oooooo iisooo 0oxo00.'..1s0s00 000oae...17t33333t00000)00000 i0p4440OO0iOOO 20 00 90 0 I0.0 o o 0.0 0.300 4O0 | HWPPIL1L0OD0 LLcC PPuummpp EExxtteerrnnaall EEvveenntt TTiimmeettaabbllee The Timetable contains entries which are : ' The ITTTniiiinmmteeeitalable coCCnootllauuimmSnnneseSS6wwiiettncethnriCCeoosnmttowaeahccittcilh areCCo:onomttfaarcctt22 In005i00...t..20i000005a08l oiOOooOiffifeefffe oooOOOnetnffreff ooOOOonffrffttfff ' 11105..9i000 aOOiffff oOOffeff OOofnkf: 12.00 off off Off CCoonnttFaaeccttss orOSOOOeffftetfff &,Off On Off CCoonnttoaaeccstts4 OSoSOOiitffftftfff BOOffiff Off . HHPPlII10000 Aauuttoossaammpplleerr IInniittiiaall CCoonnddiittiioonnss DDDEBjrrrjeeaaaccwwwttsSPpSSpoeppesceeeiaeedtddion((u~1I(/iemmm)iinn)) 2322000000000...0000 4 SIVDSInrtnAjoaojTewpecctTWTtPiiiioinmmosoeebnnietVriVG(ooormlnliiuunnssmse())em(m(~)1l)) 2121530510.3...0000000 . Vial Number 2 " ui a w `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACPOPRUROROTTT,EECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00110066 3M_MNO1539257 3M MN01539257 -------------------------------- J Tuning Method Repost --.--" PPaaggee 11 Tuning Method Hathoa: RepCo\rMtASSLINOX\FLUOROCHENLCALS. PROVAGQUDB\FLOGROCHENS. Method: printed: CFe: i\MvAaSSrLY1N2X\1F5L:U4O5R:O2C2HE2M0I0C4ALS. go PRO\ACQUDB\FLUOROCHEMS PrintQd: Fri Mar 12 15:45:22 2004 fannie aa [ DsiohA teislE 633 Ea ain ean, perl TT TY Ea \ a E E iE Re , FEE i esta = Sun RN ETE o TEElGenao ed Ree] I x SERGE LASSE TAL VETS Ti01 1 BATE Jas! ie SN a "an ALC oS hint ` DDaauu 449999..0000 some ( 5p ) SOURCE ( ESP- ) Vo SGCCpoooarnnpieeaig!noltaaery1 o AHHSHepeeoueexxsarraaptttppoeuouotrlrleeseeBro21121ck Ter. erotvation Source Block Desolvation TTTeeemmmppp... - PR-- Pressures AG Annaallyh ysseers Vacuum Vacuum " Gas Cell oo SSeetr mRdabsk 32o220%..l0000 "-222.b.9983 -20 1o000$..X.o00003 100 FEi00 300 i00 299 RRadbkk oOr$FeFe 3.0e-3 - AnAnaatlyyssoerr i1LHTMMEneRRRoeeerssssay111 1 CZCESIononElnttlnlrsleiearinsngscciyieeoonn1 DELixiMi'tfRheeesss 222 wH1IaMEEenniReeeprrsgglyyi2e22r Multiplier GGaess FFlioowwss SeCCsooonneeLvGGaaatssion Desolvation ,.m . . " `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTYUBBIDJJIEAESCCTLTTRTITOCOT AACOPPURRROOTTT,EECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR-2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00110077 sSeetr mak 1111h544o...0000 51-1Pn2.50ooua11o24w 21i14s.0o0 16 [Ea212..400.0 650 -648 Rndabkk 51122930.99 751.3 SM sezse 3M MN01539258 QQSuutaaunndtytiiWtfoyy. CCLaa1ll9iibb6rr,aattiiSooatnn NRRoeepp.oo0rr3tt0504A, Ext.Date:03/05/04,Analyst:K.Risha PPaaggee 11 Study No.=LI958, Set No.--030504A, Ext.Date--03/05/04, Analyst:K.Risha BCGLCraaaalssliititnbbrremmaaoo:ttddiiiiooffnnii=:eedr= oMTPioo:n\ne\DDaNvMataaatarrra\\LL311C565CHMSS101M37H3:1S=S5256E666\\0:=MM133aa299ssssl222y000yx000n\484xF\lFulcuorroocchheemmiiccaallss..PPRROO\\CCuRrEfovdveADDBB\\003300S50044AA CCGG AACCSFSM pps Printed= Tue Mar 16 07=26=23 2004 ran | C(CoomCmppooouuncnddofT1frDniaeatmmissem:m:eiCCn6nBtiAAotcGni:dGPP0F9FR9H5AA935 Coefficient Reaslpbornastoen Calibration yoccpufuerDev::eeE:tex11trm55o2m2in.a22al22ti33Sotn*+d:,xx0A++.r9e229a775449996..50088 | iRnevspaonbsee:tyLpien:eaEr,xteOrrnianl :StEdx,cAlurdeea, Weighting: 1x, Axis rans: None Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None 1.55e5- v || || a ReRsepspoonnssee)- 4 || 1 | || || | | [] | 1| a -- Go | ao ao acho abo 0058" 200.0 400.0 600.0 800.0 1000.0 EExxyyggeenn RReesseeaarrcchh,, 3300558% RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 16801 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACOPPURRROOTTT,EECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00110088 _MNO1S39259 3M MN01539259 GQCuuanynstiiatfyyyCCcauElsLiibbEreaattiioonn ToReppioorrttos0un, mxt.aces03/08/00, Amsdyesimnish sage 2 Page Study No.=LI958, Set No.=030504A, Ext.Date=03/05/04, Analyst=K.Risha Calibration: pi\oataar\sLeCFlHuorBoshMenSs cEals F0\GarvaBeN 0205048 Calibration= P=\Data\LCMSMS6\Masslynx\FluQrochemlcals.PRO\CurveDB\030504A rniapter AUA RI SENN BN Last modified= Mon Mar 15 13=56=39 2004 3CG Acs ACSFM Printed= Tue Mar 16 07=26=23 2004 Compound rams: CORGAFROR Compound 2 name: C8 Acid PFOA Cooohf Daecrmionatinon: 0.996490 Coefficient of Determination: 0.996490 Coltrane: 352.081 x + 3900.44 Calibration curve: 332.081 * x + 3900.44 Resyppe Eoxomna $s0. erea Response type: External Std, Area (Ce pe: Linear, Ori: Exlode, Weighing: 1x, Ad rans: None Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trens: None | = 3.42e5- | | | 1 -- Response- |i | | | L %o ho whe eoha acho 0 0.o 200.0 400.0 600.0 800.0 oxygen Research, 3058 Research Drive, Siate Collage, BA 666% Exygen Research, 3058 Research Drive, State College, PA 16801 CCHEOONNNNFEIDFPEIINNTDCIAOELU-NN- TSSTUYUIBBDJJIAEESCCTLTTRTITCOOT AAGPOPRUROROTTT.EECNCTOTIIVV2EE7-OO0RR1-DD1EE0RR.0E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00110099 | | 008" 1000.0 sw umorssszso 3M MN01539260 QqSuuaaannyttiiNftEyy.CcCaaLtlsEibb,eraattiioooaknn RNReeesppooTrrottR0S0A, Bxs.Date:03/05/04, Analysts.Risk sage Page CLCE[SaaatnrllsuteiitdrbbyrrmmuaaoNemttdodiii.ioof=nniLT::eIid9a:58B,MMP:oo:\nn\SDeDatoMtataatabrrNa\vo\L.L1TOi:5oCH0ME3S1ThN0M33S5:SiEf056\o46\WaA:Mear,3ass9sssiEl22yx0y0n0tnn04.x\D\FaFltlueuo:oz0ro3oc/ch0he5en/mi0ic4ca,allsAs.n.aPRlROyO\s\GtCr:uvKre.vDReiBDs\Bh\0a03300550044AA CO CG ACS ACSFM Printed= Tue Mar 16 07:26:23 2004 Compmemoe CuASonmda FES Compound 3 name: C4 Sulfonate PFBS Goufioant of Determination: 0.866207 Coefficient of Determination: 0.995207 Colbralon curve: 478620 + + 35 1105 Calibration curve: 4.78826 x + -35.1105 Response ype: Extmat Sid Area | Response type: External Std, Area Curve pe: near, Orig: Excude, Weighing: 1, As rans None | Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None . i i |! || 4.75e3- | | | || | : RReessppoonnssee'| | 1 | || |! | -35.1 [10.0 r 3000 e ao p ey) r acho e "oa0 200.0 400.0 600.0 800.0 n /L 1000.0 Exysen Research, 3058 Research Drive, State College, FA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIEAESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00111100 au_Notssszet 3M MN01539261 qB Quuaannttiitfyy cCE aalliibbrraattiioonn tRTaepTpeoTrrttutotn, Bxe.oares03/05/58,Analyst.vish [IPage 4 CSatluidbyraNtoi.o=nLsI958,PrSe\tDNaot.=a0\30L50C4HA,USEEx\t.WDaatses=0i3/y0m5/e0\4,FlAnuFaRolOyrsoCtu:ceKhv.eReDinIsNhiaGc30a8l04sA CB ACS Calibration: P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\030504A CG ACSFM Last modified= Mon Mar 15 13=56=39 2004 Printed: Tue Mar 16 07=26:23 2004 isin rama:CF Sullonta PFS Compound 4 name: C6 Sulfonate PFHS antof Devmeaten: 0o54261 Coefficient of Determination: 0.994244 von comet18 81S 107 480 Calibration curve: 45.6617 * x + 187.490 Raepanen oa: Exoons St Ara Response type: External Std, Area orepe or, Sg Ei, Weighing: 1s,As an: Non Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None ss200) 4.82e4- -- | | | ||RReessppoonnssee- x || | * | | || | | || # || v00 0.0 7000 oho 200.0 400.0 000 600.0 00 800.0 Exygen Research, 3058 Research Drive, State College, PA 16801 CHEONNNEFPIINDCOEU-NNTSTYUIBDJIAESCTLTRITCOTACPORUORTT.ECNTG.IV2E7-O0R1D1E0R.8E8N6T2ERED IN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00111111 T0008" 1000.0 su_woreseas2 3M MN01539262 QqSuuiaannndttyiiNtfoyy. CC(aaLlliii3%bb6rr,aattiiSooannt NRRoeepuposor0rt3t.0504A, Ext.Date:03/05/04, Analyst:K.Risha PPaaggee 55 Study No.:LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst=K.Risha CLCGSaraaaillnsnlitttbbmerrmoaaaodrttdiiiiooffnnii=:eedd=:r\MNTPDooo=aenn\tDaNMMa\aaatLxrxaC\H11L156S5CMMS10S137M3S11=S\5256M666\a11:Ms323as939slsyl222m000ye000n\484xF\lFuluoorroocchheenmiiccaallss.PPRROO\\CCuUrrvveeDDBB\\003300550044AA CG CG ACS ACSFM Printed= Tue Mar 16 07=26=23 2004 (C(CCCCooooolmmeobfpfrpfiioaccoiiuiueeonnnnnddtt oco5fufrnnDDvaoaeetmm:taeeer2:rm:4mi.CCni1naB83tai5SStio0uounlnl:xff:oo0n0n+.aa.9t9t6e9e9688.PP558FF551OO906SS2. - TT ([CRCRuaeerlsivsbpeprotoanyntispsoeeen:ttycyLpupioernv::eeaEE:rxx,2tt4eOor.rm1inag3ail5nl:0SSttE*ddx,,xcAAl+orrdee6eaa6,.8W1e6i2ghting: 1x,Ai tans: None | Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None 2.47e4- | x || Response i| | | | J J | | || | o TT 0 0 Tao 000 G00 8000 0.0 200.0 400.0 600.0 800.0 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00111122 1059!mt 1000.0 _MNO1S39263 3M MN01539263 QqI uuaannttiitfyy sSe aammppllee RReeppoerrtesos0s0an, xe.Dater03/03/04, Basiyesixnisna rage 1 Page 1 LE asSSauattssmuhptpdeilyna cmesoNdoGLi.ief:s, titL::eId9:5B8,wBMPeio:\n\SoDDeaeMatattataarNa\\o\LL.L1T o=C5CU0UME3SS10NHM35SSS:R 0\264M2\WAa:Ma,4sas6ssI sisylyE2nx0ymtm0na.4\xFD\lPaFLutluoeuor:oro0ro3soc/hch0ehe5nen/imi0cic4aca,llasal..Asn.PRaPOlOR\y\OMs\SetSaC:asKhmp.pO1RlReieCDsDoEhBt\a\G003E30o05v500a44.AATUCCDGoESAACCS63FS1M504 MLaTeaatsnhttodmm:esoadtitfiieadd:s Hon wat oases soot J P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mort Mar 15 13:25:12 2004 NPDES 031504 JsoebivCeotdee:| Brains nines 90a fee SE Ir~tials_ . Date 051~oL}"v --' ' ----' Printed: Tue Mar 16 07:26:27 2004 Run#~l~-'~At To ~'^ "-~ [Ep Name= 030504A-401 T1.extc~e acia ven _ i: C6 Acid PFHA XC(C003300550044--00,, 00 nngg//LL SSttaannddaarrdd | 0033000s550044A44-40011S5mm (in, (Mn, 20)2x3) 1( h 2I58.34 2645~ 1122--MMaarr--22000044 1166::4444::55661 LLCC//MMSS//MMSS ##~6 MRM of 5 Channa E5- MRM of 5 Channels ES3135 260 313 > 269 er| Tries 1.74e4 Rn 30 abo ab r bs TT oo 2.00 4.00 6.00 8.00 1000 | Time 3. co nid pron_ /2X:C0C3805A0c4i-d0,PF0OAng/L Standard XC030504-0, 0 ng/L Standard { LCMSIMS #6 1003300550044A4-440011 SSmm ((MMnn,, 22xx33)) I| e oe NS Hes2230608 1 8.80 1738-~ 1122--MMaarr--22000044 1166::4444::5566 MRM of LCCh/aMnnSe/lMsSES#-6 MRM of 5 Channels ES- I 413 > 369 ,v/-%/~h ~,~ 2.24041 | *m A e20ee abo _ ab a8" F0I5 NN|; Mee 2.00 4.00 6.00 8.00 3. ct sultonace pens [X:C0C3405S0u4l-f0o,na0tengP/FLBSStandard |XC030504-0, 0 nglL Standard fear smn 2 \ Jor Grama 5 030504A-401 Sm (Mn, 2x3) 10w0,ind078 000 Aa NBisBssR o oRuts ow N05Y0SR Prom \295298 10 i =r '2.~7 328361 430840;086 5.~59 6;44 RAAB 7.2 7.55 8.67 ~0.00 1122--MMaarr--22000044 1166::4444::556 LLCC/IMMSS//MMSS ##t6 MRM of 5 Channels ES- ANNE 10.58 299 > 99 /~ ~..10.87- 1.08e3 r 1 rr 2002.00 ab 4.00 obo6.00 aoe pe, r= TH Time 8.00 10.00 Sxygen Reseasch, 3058 Research Drive, State College, EA 16802 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00111133 aunorsaszes 3M MN01539264 Smell Ses rh Quantify Sample Report ret Page 2 Study No.=LI958, Set No.=030504A, Ext.Date~03/05/04, Analyst=K.Risha gonpie ies ELON TEV Fnceaeten ein SOASALSTESOSO4A OF ACT Sample List: Last modified: ee Lexbabt hess ym 7iuorochenicals.PRO\KCeoSAGrDoBv\e NODES 031504 Method: Last modified= fags Job Code= P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13:22:46 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13=25:12 2004 Printed: Tue Mar 16 07=26=27 2004 Name= 030504A-401 Text= 1.05 Gass X4X:CC003C~3005S50u04l4-f-0o0,n,a00ntgenlgLP/LF.HSSSttaannddaarrdd I 003300550044AA--440011 SSmm ((MMnn,, 22xx33)) ; op 576 420 gua 168 210 %"Rm an . _ 12-Mar-2008 16:44:56 12-Mar-2004 16:44: 56] LLCC//MMSS//MMSS ##66] ! ,~, MMRRMM ooff 55 CChhaannnneellss ES- 10 am ox H. e re A7.05.RRAR VAP on 3 pr) iw SE5 ws oe -- /i I 2.0, 0 , 4.0I 0 I 6.0, 0 , 8.0, 0 , 10.,00 , Time += cr sustonsee pron ~ ~ 5:C8 Sulfonate PFOS KC0305040-ng0i,L Standard 12.War2004 16:44 XC030504-0, 0 ng/h Standard 030501401 5m (0 2) MRMof 5 Grame5l. 030504A-401 Sm (Mn, 2x3) % ! Tino 100~ i" as or om r *K soso S_m swan ree 12-Mar-2004 16:44:56 LLCC//MMSS/M/SM#S#6 t MRM of 5 Channels ES- TRINA 06 [| 14763 11.40499 > 99 spr 9% 10.56 ~ |, 1.17e~ .... , ....20~ 0.... ~ ....40, 0.... ~ ....6.-- ,00.... , .-- .8..00, ....E .. fo,,or , .... TTimee]| 2.00 4.00 6.00 8.00 10.00 spin Fwseaseh, 3050 Baseseeh Drive, Seace Sobiege, Th 2053 Exygen Research, 3058 Research Drive, State College, PA 16801 COENAFNIEDEPNITICAOLUNSTUYBDIIESCTTRITCOTACPOURROTT.ECNTG.IV3E71OR0D2E8R8E6N3TEREDIN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00111144 sw_morssszss 3M MN01539265 [OT rages Quantify Sample Report TE the. 030504a, Bxt.Dat0163/058/04, Amaiyet Knish Study No.:LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst=K.Risha Page 3 Sample List: Bi\aca\LCHNSEWassyme\FiucroRcO\hesps1aiTRc\3a0Sl04.A CO ACS Sample List: Last modified: noms Lexis aes syoe\FAorocPhROe\NOmCihBcCoatGlrosve NEBES 631504 Method: it Raateteas won var 15 Torists Soot Last modified= a Job Code: P:\Data\LCMSMS6\Masslynx\Flucrochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13:22:46 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25:12 2004 Printed: Tue Mar 16 07:26:27 2004 on Name= 030504A-402 Text= I: C6 Acid PFHA XC(C003300550044--11,, 2255 nngg//LL SSttaannddaarrdd loyaiosoan-402 5m vn, 2) MRMof Chommel5-s| 030504A-402 Sm (Mn, 2x3) easrt Toorsaees 100! 8.31 7367~ 1122--MMaarr--22000044 1177::0066::33i7 LLCCIIMMSS/M/SM#S#t6 MRM of 5 Channels ES313 > 269 4.54e4 Area |lwl h I -- ~rr me | 0~, ,~,, T~, ,-7~ .... ~ .... , .... , .... ~ .... , .... , .... , .... ~ .... , .... Time LT ee am ee eee awe 2.00 4.00 6.00 8.00 10.00 2: co neta pron [X2XC:C030C083500A54c0-i41d-,1P,2F2O55Anngg//LL SSttaannddaarrdd | 0305044.402 Sm tn, 26) RM of Channe5l- 030504A-402 Sm (Mn, 2x3) 0%0 oer edae 1001 8.81 13788 121-2M-Mara-r-22000044 1177::0066::337 LLCC//MMSS/M/SM#S#6 MRM of 5 Channels ES413 > 369 77..6600e44 Area 1378~ | -- | " Ee rr, r , , TTiimmee Zab bo ao im J 2.00 4.00 6.00 8.00 10.00 PR -- oo : C4 Sulfonate PFBS X[XCC003300550044--11,, 2255 nngg//LL SSttaannddaarrdd | 1122--MMaarr--22000044 1177::0066::33;7 LLCC//MMSS//MMSS #6 305088.402 Sm (40,24) MRM of GrameEl5s- 030504A-402 Sm (Mn, 2x3) MRM of 5 Channels ES- [a is po 10n_ 7.83 299 > 99 | J Togo 112 1003 Lan AogA181 z200s5z a8ss ssa ps SaRm sseCnt |Vii fa95n2 SA104an1A 1/.823 1.68e3| 3b i aio abo fo | crepe Ti | ,,, ~ .... , .... , .... ~ .... , ~ Time 2.00 4.00 6.00 8.00 10.00 EExxyyogeenn RReessaeaasrccnh,, 33005588 RReesseeaarrcchh Drive, Drive, Scace State College, College, 7A PA 16501 16801 CCHOEONNNFNIFEDIDPEEINNNTTICIAAOLLU--NSTSUYUBBDJJIEESCCTTTRTITCOOT AAGPOPRURROOTT.ETCENTCIOTVIVE2E7O-O0RR1D-D1EE0RR.0E8E8NN6TT2EERREEDDIINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00111155 sw umorssszss 3M MN01539266 QSQueuaaanyntitNfbyy.1Ss1aa1mm3pp5ll8ee, RReeSppeo%orrttNo.:030504A, 3xt.Date:03/05/04, Analyetik.Risha Page 4 Page 4 Study No.=LI958, Set No.=030504A, E~t.Date~03/05/04, Analyst=K.Risha STVLSaeaaartsmmehtppollmameerooddLLiiiifssztiti::eedd:P:NMPF\oo:ADnn\baDitMNataaatar\ra)u\LLH1155CoEMMuS11SsM336S:i\e26aM23\aK:iMsa44asg6tslssyl221m0y0ye00nm\48x\F\lPFLuluuooorxroooccchhheeemsmiLicecaaalllsss..PPPRRROOO\\\SNSaBazEmpRplDleReD\DBCB\o\0t03G30r05o50v04e4AANPCCDGGESAACCS0SF3T1M504 MGTLeaoatsnshttocdmmo:eomdedriitfiieedd:: Wen Nar 15 13143112 204 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 Job Code: Printeds Printed: TTuuee MMaarr 1166 0077::3266::3277 22000084 spNaarmmeeod:: 003300S80044A5-440022 Text= 4&: :OCF6SuSluflofomnaavtee P PFMPS E |XxCC003300550044--11,, 2255 nngg//LL SSttaannddaarrdd 1|ozos04n450m2 (in, 2x0) 030504A-402 Sm (Mn, 2x3) 100- 1 -- - ka MRM of5 ChannoTlWeo5-a| 8.662_ 1122--MMaarr--22000044 1177::0066::37 LLCC//MMSS//MMSS #6 MRM of 5 Channels ES- 339999 >> 8800 8.10e3 Area ~| To i e 200 e"ho 5. ca sulfonate 2.00 pros _4.00 5X:C0C3805S0u4l-f1o,na2t5e nPgF/OLSStandard C030504-1, 25 ng/L Standard p00o330"0550|044A4-440022 5m Sm (Mn, (Mn, 2)2x3) 1100 i * | re ah 2.00 a 4.00 Te | a 500 abo 000 6.00 I ~ ' ' ' I ' ' ' ' I * ' ' ' I ' ' ' ' 8.00 10.00 TTiimmee| 85s _ MRMof 5 Crann0ol5s 050. 8.98 728 peenend 728~ 1122--MMaarr--22000044 1177::0066::3377 LLCC//MMSS//MMSS ##66 MRM of 5 Channels ES499 > 99 4.51e3 Area sho a0 00 Time 6.00 8.00 10.00 Exygon Research, 3058 Reseach Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00111166 _Motsaoze7 3M MN01539267 _-- SqQuueaaannrttiiNtfEyy.TSSaaBmmsppll,ee RReeippoo.orrttcos0s0mn, Bxt.Date:03/05/04, Analystix.misha Pages Page 5 Study No.=LI958, Set No.=030504A, Ext.Date:03/05/04, Analyst=K.Risha VLSLSaaauatssamhttppollameemooddLLiiiifrssiitte:e:dd::peMMPB\oo:pDnn\aaDttMWaeaata\rra\L\O11LU56CNSMME21SS33MES1:S3\2632W\W1:aMa44sa6ssasl3l2yy00ymm00nc44x\\\FFulluouozororocochchahememimiicccaaalllsss...PPPRRROOO\NNSASaEAmRppDElRDe\BDoB\\t00G33r00So50v04e4AAOCCDGGESAACCS03FS1M504 MLTeaatsrhttmocdamo=odedriifiiaedd:: Mon war 16 13135413 2008 P:\Data\LCMSMS6\Masslynx\F1uorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25=12 2004 NPDES 031504 JPorbintCeodd:e: Tue war 36 07:26:27 2004 Printed: Tue Mar 16 07:26:27 2004 TsNaammoee:= 003300S5004A6-440033 T3:extc=s neta orn XC030504-2, 50 I: C6 Acid PFHA XC030504-2, 50 nnggi/LL SSttaannddaarrdd w1003n0350h0540A4-440033 Sm Sm (Mn, (Mn, 233) 2x3) i [*10% 7122:-MMaarr2-20r 00044 11y 77.:22887:118 d8a.r1st1 MRM MRM of of 55LCCChh/aMannnSnee/lM>lssSEE25$#0--60 a2604 313 > 269 ea 11, _60L \ 6.26e4Area ho I 2060.... , abo .... , .... , 600 .... , .... ,, 2.00 4.00 6.00 m2:(eCC08e30A5sc0i4s-d2s,PFa5O0AwngeiLnStandard XC030504-2, 50 ng/L Standard (130504A.403 Sm (Mn, 213) 030504A-403 Sm (Mn, 23) || 1001 0), , 8.00 2a83.s6e7 _ ee ,, .... ~ .... Time 000 10.00 | 1122-MMaarr--22L00C00/44M11S77/::M22S88::1#1868 MMRMRooff 55LMCCChha/Mann3nSno5e/lM.lssS3E65S#.0-6 413T>7e0356a89 1.37e5A~a o Tam memae w 3. ca suitomate ses 2.00 4.00 3X:(CC0C043300S55u004l4-f-2o2,n, a55t00e nnPggFI/BLLSSSttaannddaarrdd 6k abo ET To re 235~ 6.00 8.00 ! 1030504403 Sm (Mn 263) 100, 030504A-403 Sm (Mn, 2x3) 152 879 | 10w07{foAn A100 L1252B16 O322Z382IEAzeeq aarrenT7.17A7X52VieR7.8a88n,~f7[92~A 1r T00e r Tine 10.00 | 1T22:-MMaarr--22L00C00I44M11S77I:;M2268S::118 MM10RR1M4 of of 55LCCChh/aMannnSn2e/e9lMl9ssSEE6SS#9--6) \0to%se 10.14~ J t 1096 178 1505 11.792991.>5(]9e93 x 3) vearkorepe5r00 pprmBhor pretr0mrrpees Ti 2.00 4.00 6.00 8.00 10.00 xygen Ressssch, 3056 Ressacch Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTYUBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993390.00111177 m_Morsaozes 3M MN01539268 gQSuueaaendnyttiiNtfoyy. sS(aaLmm5pp5ll0ee,nReeSppetoorrttNo.1030S04, Ext.Date:03/05/04, Analystik.Risha Page 6 Page 6 Study No.=LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst=K.Risha LvLSSaaaaessmmtttppllomeme:ooddLLiiiiffssiittee::dd::PiMMPB\oo=nnDa\aDMMzacaataarra\\\LLL11CC55CHHMSS1S1HH33MSS:=SSS22622\\H::MWa44aas66sssss2ll2l0y0yy0n0nn44xx\\\FPFilluuuooorrroooccchhheeennmtiicccaaalllsss..PPPRRROO\\OSSMaasmEppDllBee\DDCBBo\\0t03G30z05o50v04eA4ANFCCDOGESAACC0SS3FT1M504 LTMLaoeatsnshttocdmom:sooedd:iifeiteeddr: Mon Mar 15 13:23:11 2004 P=\Da~a\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25=12 2004 NPDES 031504 Job Code: Printed: Tue Mar 16 07:26:27 2004 Printed: Tue Mar 16 07:26:27 2004 NNTaaommea!:: 020504A-403 030504A-403 Text= 44::(CCc06e30sS5uu04il-tf2oo,nnas5tc0ee nPpgFrlHiLSsStandard XC030504-2, 50 ng/L Standard 00"3300550044A7-440033 Sm Sm Mn,(Mn, 259) 2x3) 1001 _ 12-Mar-2004 17_:28:18 1R2.MMaorf-25LL0GCO0nIM4aMnS1nSI7o/l:MM2s8SSE:1S##8-6611 20880.55600 MRM of 5 Channels ES- 3d9ed>80] 399 > 80 1.`4A4reea4l Area io 200re 300 500Ts 269~j~ 500 i000ee Tim|e| Time 2.00 4.00 6.00 8.00 10.00 55[:X:CCC08o305sS0uu4ll-ff2oo,nnaa5tt0ee nPpgFriOoLSsStandard 12-Mar-2004 17:28:1 XC030504-2, 50 nglL Standard 0305044403 5m (Mi, 253) 1M 2-MoafrR -52LL0OCC0hII4aMM Mnn1SSa7I/iM:sM2S8SE:S1#-8~ 030504A-403 Sm (Mn, 2x3) 1s84.e88r79 MRM of 5 Channels ES- 4989s>t9e39) 499 > 99 1469-~ "hea 8.51e3 , 200 50 e 550 e 800 1050 Time 0-[ ' ' '[ ' ' ''I ' 2.00 .... , .... , .... , ...._, _ .... , .... , .... , .... , .... Time 4.00 6.00 8.0~ 0 10.00 Area t i Exygen Research, 3056 Research Drive, State College, 7A 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 i `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00111188 SW_MNO1839269 3M MN01539269 QQStuuaaacnnyttiiffNyyo.:sSiaa1mm5pp%llsee, RReeSppeootrrtNto.:030504A, Ext.Date:03/05/08, Analyst:X.Risha PPaaggee 77 Study No.=LI958, Set No.=030504A, Ext.Date:03/05/04, Analys~:K.Risha aLSTSataaasmsmhtpkpollmdemeo:oddLLiiiffssitite::edd::B:NMp5\oo:Dnn\oaDnNtMataaatarr\a\\LLL1O1C55CMHMSSS11SHM33EES::\S236M23\aN::Mas44ass66salslyl22yny00mx00na\44x\P\FlFluluouoroTrooocchchehenenimicicacalalals.s..PPPRRROOO\\\SSKaaezEmphplIleReD\DBCB\o\0t03a30z0So5Ov04e4AANPCCDGGESAACCSS0TF3H1M504 MLLJeaaotsabhttoCmdmoo:odddasiftiieedd:: Mon Nar 15 13125132 2008 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13=25=12 2004 NPDES 031504 Job Code: Pprriinntteedd:= TTuuee NMaarr 1166 0077::2266::2277 22000044 HNaamzee=: 003300550044A--440044 0504-40Sm4 4, 220) Text= 1I::(CcC0e630aA5cc0ii4a-d3,PsFm1H0nA0 ngiL. Standard XC030504-3, 100 ng/L Standard 030504A-404 Sm (Mn, 23) 100,i1 110~ ar8.17 16840 "19540~ MRMofChammel 5- 12-MarT-2T00T4 17:50:01 LOMSIMS #5 12-Mar-2004 17:50:01 LC/MS/MS #6 MRM of 5 Channels ES- 313> 260] 313 > 269 1015] 1.0"1e5 Aral Area cs0s04405m4 i, 3) NROof 5 ramets 5-| h |{ 0', ,~-,e , , ....20, 0.... ~ ....43, 0.... , ....6,%....pe,ep.ee...0T ,0.... E , ....10S ,00.... S , ....~ TNimle 2.00 4.00 6.00 8.00 10.00 2: ce acta von 2:(CC0830A5c0i4-d3,PF1O0A0 ng/L Standard _ 1_2-Mar-2004 17:50:01 XC030504-3, 100 nglL Standard 12-Mar-2LL0CC0I/4MM1SS7I/M:M5SS0:0##166 oy | 030504A-404 Sm (Mn, 2x3) a88r.7711s MRM of 5 Chan44n11e332ls>2>36E366S695-9]) S 42736I__ |ososounaos sm vn, 20) , A 250 400 600 800 110/~ 2.00 4.00 6.00 8.00 3: C4 sultonate prs 3[XX:CCC00433005S50u04l4-f-3o3,n, a11t00e00 PnnFggB/lSLL SSttaannddaarrdd ' 11010, 030504A-404 Sm (Mn, 2x3) T7is.57 | wp 1 0 So r c rep yb 256 44.0000 600 6.00 800 8.00 2.00 1000 10,00 > Tima ~.2T.i2m6eAere5a NRW of 5 Ghmels 5-| 1122--MMaarr--22L00C00I44M11S77I::M550S0::0#0151 LC/MS/MS #6 MRM of 5 Channels 209>9 299 > 99 26003 2.60e3 Area Area | p10e 00 er Time|j 10.00 | Exygen Resascch, 3058 Reseazch Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00111199 S_MNo1839270 3M MN01539270 | | qQSuutauadnnyttiiffoyy.:SSLaaimm3pp5ll8ee, RReSepapotorrttNo.:030S04A, Ext.Date:03/05/04, AnalystiK.Risha Study No.:LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst:K.Risha Praaggee 88 LSSaaasmmtpplleemodLLiiifsstti::ed:P:MPo\:nD\aDNtaatara\\L1LC5CHMSS1M3MS:SE36\2\M:Ma4as6sssll2y0yn0ne4x\\FFlluuoorroocchheeamiiccaallss..PPRROO\\SSaamspplleeDDBB\\003300550044AA CCGG AACCSSTFHH | MMLLeeaattsshhttooddmm::ooddiiffiieedd:: MPMPoor:nn\\DDNMaaatatrara\\L1L1C55CHMSS11N3M3S1S:S22652\\1:MM14aa76ssasll2200yy00nn44xx\FFlluuoorroocchheeamiiccaallss.. PPRROO\\MNeOtEhRDDBB\\CCoottGGEroovvee NNPPDDEESS 003311550044 6LJoabbStCComoddoeeds:ified: MOn Mar 15 13:25:12 2004 PPrriinntteedd:: TTuuee MMaarx 1166 0077:=2266::2277 22000084 NNTaaemmxeet:=: 0023005S0044AA--440044 Text= 44::CC66 sSuullffoonnaattee PpFrHsS XXCC003300550044--33,, 110000 nngg//LL SSttaannddaarrdd |001330000550044A4-440044 SSmm ((MMnn,, 226x33)) 100! oo 889.515444 po 1122--MMaarr--22L00C00M44 S11I77::M55S00::0#0116 MMRRMM ooff 5LCCChh/aMannnSn33ee/9lMpl9ss9>Sr>EE889S#8o-0-06 2.66e4 Area |L re r 200 400p 600 m 8409014~ s 1000 - Tine Time 2.00 4.00 6.00 8.00 10.00 55: :Cc8s sSuullffoonnaattee pPFrOoSs X[XCC003300550044--33,, 110000 nngg//LL SSttaannddaarrdd 10To03300550044A4-440044 Sm Sm (Mn, (Mn, 263) 2x3) _-- 1122--MMaarr--22L00C00/44M11S77/::M5500S::0011 ses MRM MRM of of 5LCCChhlaMannnSn4ee/lM9lss9SEE9SS#9--6 285.2889 4919.r4>3e90a94 | |o= r 200 abo e 600 8e 00 0 e 0M) Time 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACPOPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00112200 3M_MNO1539271 3M MN01539271 | | gQSuutaaundntytiiNfoyy.:sSLaaimm3ppSllSee, RReeSppeootrrtNto.:030504A, Ext.Date:03/05/04, Analyst:X.Risha PPaaggee 99 Study No.=LI958, Set No.:030504A, Ext.Date:03/05/04, Analys~:K.Risha LSSaaesmmtpplleemodLLiiifssitte::d:P:HP\o:Dn\aDWtaaatr\aL\1LC5CHMSS1U3MI:SE36\3\a4Ms4as6slsyl2n0yx0n\8xF\lFulcuroroocchheenmiiccaallss..PPRROO\\SSaarmpplleeDDBB\\003300S50044AA CCOG AACCSSFTM NMLLoeaattsshhttooddmm::ooddiiffiieedd:= HMPoo:\nn\oDaHMataatarra\\LL31C55CHMSS11HM33S:S=E32632\N:=Ma14as36sas1l22y00ym00ne44x\\FFlluucorroocchheenmiiccaallas..PPRROO\\MAeEtHhDDEB\\CCoostdGrroovvee NNPEDDEESS 003311550044 Job coder Last modified: Job Code= Mon Mar 15 13:25:12 2004 PPrriinntteedd:: TTuuee MNaar 1166 0077::2266=:2277 22000084 NpNaarmmeey=: 003300550044A3--440055 Text= iX1::C0Cc36o05Aa0cc4ii-dd4,PpFr2Hi5An0 ngiL _ Standard XC030504-4, 250 ng/L Standard 00y3300550044AA--440055 SSmm ((MMnn,, 22:x33)) " 810 ai8.s19" . 1122--MMaarr--22L00C00I44M11S88I::M111S1::4#4858! MRM MRM of of 55LGCChh/aMann3nSno3e/lMl5ssS2EES6S#-69-1 3132.>o1266a095 2"16e5~Area | ok 200~ .... ~ py .... , .... , 650 .... , .... , N 800 "1E 000 ..4.1.29, 7.~.L..__, _.... , .... ~ ....-Time 2.00 4.00 6.00 8.00 10.00 2:: cCa8 Ancoiidd pPrFoOnA XC(C003300550044--44,, 225500 nngg//LL SSttaannddaarrdd 1122--MMaarr--22L00C00I44 M118S8::M111S1::4488) 00;3300550044A4-440055 Sm Sm (Mn, (Mn, 2:3) 2x3) 873 MMRRMM ooff 5LCCCh"hIaMan1nnSn3ee/lMl>ssS3EE6SS#-0-6 e84.7335 4134p.>5A93rre6e59a % | Area o | 0.~-~, -, ~ 20~ 0 ~ at~ h ~ 50~ 0 2.00 4.00 6.00 oF XC: 0cC340r i5S0u4sl-f4o-- ,una2tf5e0-- oPnFgB/nSL Satatndaerdnemss [XC030504-4, 250 nglL Standard J00b03300055)0044A4-440055 Sm Sm (Mn, (Mn, 20) 2x3) | 1 O01 |* | o In T 22.0000 44.0000 56.0000 B00 ~ "~ , , , 8.00 000 10.00 ee Time|| Time | 1122--MMaarr--22L00C00I44M11S88/::M111S1::48 1277.75599 MMRRMM ooff 5LCCChhIaMan2nnSn0e/elM9lssS>EE0SS#-9-6 29395>0939 area 3.93e3 Area | me TT ime | 88.0000 1100.0000 , , , Time EExxyyggeenn RReesseeaarzcchh,, 33005588 RReessesaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, 7PAA 1166380011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00112211 S_mots39272 3M MN01539272 - | | QQSuutaaunndtytiiNtfoyy.:sSuaaimmpppSlleee, RReeSppaootrrNtto.:030504A, Ext.Date:03/05/04, Analystik.Risha PPaaggee I200 Study No.:LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst:K.Risha GSSaaasmmtpplleemodLLiiifsstti::ed:P:WP\o:Dn\aDNatatara\\LL1C5CHMSS1WM3S:SE36\3\saM4assssll2y0yn0nx8x\\PFlluuoorroocchheemiiccaallss..P7RROo\\SSasmspplleeDDBB\\003300S5004&AA CCOG AACCSSFTM MMLLTLeeaoaattsbSshhtttooCddmomm::doooedcdsiiiftfiiieeeddds:: MMPPooi:nn\\DDMMaaaactrara\\LL31C55CHMSS11NM33S1S=S226\32\K1:Ma14as26sssLl22y00ym00nx44x\\FFiluuoorroocchheenmticcaallss..PPRROO\\MNeOtEhRDDBB\\CCoottGrroovvee Mort Mar 15 13:25=12 2004 NNPPDDEESS 003311550044 Job Code: PPrriinntteedd:: TTuuee Mvaarx 1166 0077::2266:=2277 22000044 NpNaammeee=s 003300550044A2--440055 Text= 44: :Cc6s sSuullffoonnaattee PpFrHiSs _ [XXCC003300550044--44,, 225500 nnggi/LL. SSttaannddaarrdd 1122--MMaarr--22L00C00M44 S11I88::M11S11::#44858 LC/MS/MS #6 |oaosoi.4s0m5 on, 223) MRMof 5 ranma 5- 100030504A-405 Sm (Mn, 2x3) 88,5544 MRM of 5 39580 Channels ES399 > 80! ||TM 1111662255] 66..2"2A22re0e44a | Area | | =ot , ....20, 0.... , ....40, 0.... , ....6.,00.... , ....80, 0.... , ....10,00.... , .... TTiimmee| 2.00 4.00 6.00 8.00 10.00 55::Cc8b sSuullftoonnaattee pPrFoOsS _ So XCCo0s3n0s50d0-44-4,, 225500 nngg/lLL SSttaannddaarrdd 1122--MMaarr--22L00C00I44M11S88I::1M11S.1:o4r8 003300550044A4-440055 SSmm ((MMnn,, 22:x33)) MofR 5LCGhlaMM nnSo/lMs SES#-6 MRM of 5 Channels ES- [oo 8% esa 8.90 | % Ed 32e1n4 5985L 499 > 99 3.21e4Area { 200 400 690 850 1000 Bi | | , .... , .... , .... , .... , .... , .... , 2.00 4.00 6.00 , .... , .... , .... , .... TTiimme|e 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005586 RReesseeaarrcchh DDrriivvee,, SSttaatcee CCoolllleeggee,, PPAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00112222 S_MNo1S39273 3M MN01539273 1 1 QQBuuaaEnnttiiEffyy sSaaEmm5ppil6ee,RReeSppOoorrWtto. 1030504n, Exe.pate:03/05/04, Analystx.Risha Page 11 Page ii Study No.=LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst:K.Risha | MSLLSeaaaassomtttpphllommeedooddLLiiiitfssiittee::dd::B:oMP\o:\nDn\DaDaMNtataataarta\\\LLL11CC55CHHMSES11NHM33SE:S:ES226\22\WM::Maa44as6s6ssasl1l22y00yym00nex44x\\\PFFlluuLoorruoocchoheenmriiccoaallscs..PRPhR0RO\Oe\SMSaSmasEmppAlilDaeBDcDBoB\ta\00d33rl00o55vs00e44ANCPCDGGESAACCSS03FT1MH304 MLLTeaaotsnshttocdmma:ootdad:iieftieedd:: won War 15 13:35:13 2008 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 | sJooibntCeoedse: Tuo Max 16 07:26:27 2004 Printed: Tue Mar 16 07:26:27 2004 | emer o30504n-406 Name= 030504A-406 Text= 1(: X: Cc0c6o30r5A0ec4ii-dd5,pPF5oH0nA0 ngiL Standard . 12.-Mar-2004 18:33:2 XC030504-5, 500 ng/L Standard 12-Mar-2004 18:33:29 030504406 Sm (Mn, 248) [10030504A-406 Sm (Mn, 2x3) a88s.11s99r MMRRMM ooff 55LLCCCChh//aMaMnnnSSn3e/e/lMl%MssSS2E05S#9--6] 313a>t2e6s9 Area 4.37e5 Area %] A 200 2.00 22::cCa8 nAectiad pPrFoOnA T rrr r------------ Tiinmee 20J 0 500 00 1000 4.00 6.00 8.00 10.00 cXoCs0o30s5a0a4s-5,, 550000 nngg//LL SSttaannddaarrdd p00r3300a550044A8-440066 SSmm ((MMnn,, 226x33)) 1 ||"> |lo LTT 2.00 Ta4.n0s0 "66.0000 w88e.7733r 88.0000 1122--MMaarr--22000044 1188::3333::2299 LLCC//MMSS//MMSS ##66 MRMof 5 Channels ES- MRM of 5 Channels ESWas309 413 > 369 8405, 9.84e5 Area) Area 1000 TTiimmee|| 10.00 2.3: 0C1~ SuSullffoonnaatte PPrFeBsS -- X(CC003300550044--55,, 550000 nngg//LL SSttaannddaarrdd I]| 10o0303r500540A4-440068 100 Sm Sm (tn, (Mn, 26)2x3) -- -- i757.58 ee 1122--MMaarr--22000044 1188::3333::22S9 LLCC//MMSS//MMSS #6 MRM of 5 Channels ES- MRM of 5 Channels ES209 99 299 > 99 7263) 7.42e3 =Area |% | ----------------m rrr || ~~_._ re ................ , .... , .... , .... , .... , ........ , .... ~ . , LT a0 ane eo" e001 doo TTT 2.00 4.00 6.00 8.00 10.00 Time Exygen Research, 3058 Reseach Drive, state College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00112233 _mNots3927s 3M MN01539274 - , PO, re 1 Quantify Sample Report SSttuuddyy NNoo..::LL11995588,, SSeett NNoo..::003300550044AA,, EExxtt..DDaattee::0033//0055//0044,, AAnnaallyysstt::KK..RRiisshhaa Page 12 Sallie LI FrN ------_--G --_ita te eTR Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM 1 MeMLetatshhtooddm:=odified: PMPo=:n\\DMaDatraa\tL1a5CM\S1LM3S=C262H\=MS4a6HssSl26y00n\4xM\Falsuosrlocyhnemxi\caFlls..uPPoRROOr\\oMMeectthhhDDeBBn\\CCioocttGGarrloovvsee NNPPDDEESS 003311550044 I Last modified: Mon Mar 15 13:25:12 2004 Ean Job Code: ! PPrriinntteedd:= TTuuee MMaarr 1166 0077::2266::2277 22000044 Name= 030504A-406 =Text= ste me 4:C6 Sulfonate PFHS [rXcCo0s3o0s5o0s4s-5,, 550000 nngg//LL SSttaannddaarrdd wl100; (003300550044AA--440066 SSmm ((MMnn,, 22xx33)) O0 854 8.54 2328381100| hs 1122--MMaarr--22000044 1e 8:33s :29 LC/MS/MS #6 MMRRMMooff 5 CChhaannnn3eellss9>EES8S9-0-! 399 > 80 11..2266ee55 Area ok L 22.0000 44..0000 m-- 5:C8 Sulfonate PFOS cososos-s, 500 ng/L Standard 12:Mar-200418:33:28 XC030504-5, 500 ng/L Standard .... , .... , .... , .... , .... , .... , .... TTiimmee 66..0000 88..0000 1100..0000 12-Mar-2004 18:33:29 [Ae] | oo 030504A-406 Sm (Mn, 2x3) [ | ol 2.00 ETE 4.00 6.00 588.5900 8.00 LLCC//MMSS//MMSS##66 5we MRM of 5 Chann44e99l9s>>E9S99-9) 6.54e4 Area TE Tim|e Time 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00112244 3M MN01539275 QQSuutaaannyttiiwtfoyy. SsLaa3ms5ppll8ee, RReeSppaotorsNtto. 1030504, Ext.Date:03/05/04, AnalystK.Eiska PPaaggee 13 13 VLSSTSaaaatascmumtttppdolmlymeeoroNddoLLii.iif=ssFittLr:e:Ied9d:5:8,MMpBBoe:iDnn\\SADDeNMtaaCaattrrNaa\o\\L.LL11=sC5C0HMH3SS110MM33S5SS:10S236423\\KA1:NMa,44aag66ssssslEl212yxy00yn0t0n4x4.x\\D\PaFLtlleuOu=ooX0rr3ooC/ccH0hhe5eeR/nmL0iiC4cca,aaLllEsAs.n..7aPPRlRROOyO\s\\StWSa:aOmKmEp.pNlRlDeieBDsD\EhBC\a\OG0L33E00O55v00S44AANCFCOGDEASACCS0F3T1M504 oMLTeaantsshktmocdomd=soadi:ifeileodd~s Mon Nar 16 13128133 200 p~\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Men Mar 15 13:25~12 2004 NPDES 031504 JPorbintCeoddse= Tue wax 16 07:26:27 2008 Printed= Tue Mar 16 07:26=27 2004 TNNaammmeet:= 030504A-407 030504A-407 Text= |oossososns07 sm vn, 260) ALi:CC66AAvciiddPPRFHAA______ -- xXCCo03300550044--56,, 11000000 nngg//LL SSttaannddaarrdd [ 030504A-407 Sm (Mn, 2x3) {% c--------e-- Ro 1122--MMaarr--22000044 1188::5555::1144 LLCC/IMMSS//MMSS ##66 MRM of 5 Channel ES- MRM of 5 Channels ES- a0 33>260 8.19 313 > 269 i617 seg 7.58e5 eaArea 200 +00 - 50 2.00 4.00 6.00 n2:(cGC0o83n0A5cc0i4i-d5a,PoF1On0A00 ng/L Standard XC030504-6, 1000 ng/h Standard 00:3300550044AA.-440077 Sm Sm (Mn, (Mn, 2:3) 2x3) {| | 8B.0000 s88i.7733i 000 Time Time 10.00 12-Mar-2_004 18:55:14i 12-Mar-2004 18:55:14 MRMof MRM of LLCC//MMSS//MMSS ##66 5 Cha3n5n.a3=65-0 5 Channels E8- 413 > 369 Tor2eea6 1.82e6 Area 200 IY) 3X3:C:0Cc34s05sS0uu4il-tf6oo,nnaa1tt0ee00PprFnaBgsS/L Standard XC030504-6, 1000 ng/h Standard |0ep3so0os5s0a- 4snA--4s0o77 smn, Sm (Mn, 2:5 2x3) " 500342142~ 77e6.6s5 000 Time | | 12:Mar2E0E04 18:55:14 12-Mar-2004 18:55:14 MRM MRM of of LLCC//MMSS//MMSS ##66 5Channe2l9s595-9 5 Channels ES- 299 > 99 Taerao 1.37e4 Area Oh 200 abo 60E 200 e 1000 ee TTiimme|e 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseesazrcchh DDrriivvee,, State State College, College, 7A PA 16301 16801 `CHEOCNNONFEINDPIEFNNITCIDAOLEU-N-NSTSUTYUBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00112255 _MNo1s39276 3M MN01539276 QSQtuuiaadnnyttiiNftoyy. sS1aa1mm1pp35ll6ee, RReSepeptoorrttNo.:030504A, Ext.Date:03/05/04, AnalystiK.Risha PPaaggee 1144 Study No.:LI958, Set No.=030504A, Ext.Date:03/05/04, Analyst=K.Risha LSSaaasmmtppllmeeodLLiiifssitt:=ed:PrWP\e=Dn\aDtNaaat\raL\CL1HC5SMWS1S3M:ES26\2\a:Ms4as6slsyl2n0yx0n\4xF\lFulouzoorcohcheenmiiccaallss..7PRROO\\SSAaTmDpLlaeDDEBN\003300550044AA CCOG AACCSSTFHM NoMLLteaatsshhttooddmm:=ooddiiffiieedd=: 5MMP7oo=\nn\DDAMNaEaatArra\\LL11C5C5HMES11N3M3S1S=22652\N1=Ma14as26sss1l22y0y0m00n8x4x\\Fluuioorroocchheenmticcaallss..PPRROO\\NMSeEtDhDBB\\CCoottGGrroovvee NPDES NPDES 031504 031504 Tob coda Last modified= Job Code= Mort Mar 15 13=25=12 2004 pPrriinntteedd:= TTuuee MMaarx 1166 0077::2266::2277 22000084 NNpaaesmeeed:: 003300550044rA--440077 Text: 4: C6sulonace pris 4XX:CC0C0363005S50u04l4-f-6o6,n, a11t00e0000PFnnHggS//hL SSttaannddaarrdd 00y33o0n05501044A4-440077 Sm Sm (Mn, (Mn, 2:3) 2x3) i % _ _ 1122--MMaarr--22L00O00M44 S11/88::M55S55::1#1454 w88.z5556 MRM MRM of of 5LCCChh/aMannnSn3ee/lM%lssSEE8SS#-0-6 2555 399 > 80 aoa 2.53e5 Area io 250 "00 2.00 4.00 5[: X: CcC08o305Ss0uu4ll-ft6oo,nnaa1tt0ee00pPrFnOogSs/L Standard fXC030504-6, 1000 ng/h Standard {00p3300550044A2-440077 Sm Sm (bin, (Mn, 253) 2x3) | 660.000, i. 88.0000 a88u.5900s 1000 TTiimmee 10,00 1122-.MMaarr--22L00C00I44M11S88I::M55S55::1#1454 MMRRMM ooff 5LCCChh/aMannnSn4ee/lMlss9>SEE99S#S9-6 49119..2o2>99e9a0595 Area | 256 400, 500 800 000 Time Time 2.00 4.00 6.00 8.00 10.00 EBxxyyggeenn RReessseaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PA PA 16801 16801 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00112266 S_Mo1S39277 3M MN01539277 QSquuhaaannyttii1ftyy1dS3au5mmp5plse,RReeSpp0oo0rrNtto. 1020304A, Ext.Date103/05/04, Analyst.hehe pPaaggn~ 1155 LTSSSraoaatisnm~uteppdtllyeSmeeooNddoLLii.iifr=ssiiLttee=I.d9d:5s8B,MHP.oo:\nn\SoDeDauMtwartaataarrNa\o\LU.L11HC:55CHE0ME3S11NM03MS3S5=S0S26.W4\2\Aa3a:M,4sas36ssslsy2yE2l00xmny00tnce04.x\\D\FFaFiitluueuoo:orz0roo3occ/chh0hee5esn/mi0tic4cca,aalilssAs.n..aPPPlORRy\OOsS\\tASN=SaAKmPE.pLARlABieD\sDBChB\oa\Ik03d30r0So50v04e4AAJECCDOGESAACCS0E3FP1M504 MHetehodm=atted: Hon par ETT Toor P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Last modified: Mon ~ar i~ I~:2~=12 2004 srinteds Job Code: Printed: Tue war 36 G7i261a7 2004 Tue Mar 16 07=26:27 2004 sues 0308048408 Name, 030504A-408 TIM3.:eexttCch,e6anaAoccliiddWaPosFmHhA Methanol Wash )0305044408 5m hn, 20) 030504A-408 Sm IMn, 23) 100,i 100~(~ a0t3e58.19 1035~ Tar 200 EES LCIMSIMS #5 12-Mar-2004 19:16:58 LC/MS/MS #6 MofR5 haM nna E5- MRM of 5 Channels ES15200 313 > 269 I T1004 1.10e4 UM nem \ II ~\ Area ft 04 , , , , , , , , .... , .... , .... , .... , .... , .... , .... , .... , .... ~ .... Time 0% I) o hs 50 2.00 4.00 6.00 8.00 10.00 socenelwor 2:C8 Acid PFOA Methanol Wash 12-Mar-2004 19:16:58 Methanol Wash 0o3e0s504450m8 tn,20) MofR 5LCChIaM MnnSoIlMsS5#-6 030504A-408 Sm (Mn, 2x3) y sotnatir Heeaedna 10 8.71 5761 12-Mar-2004 19:16:58! LC/MS/MS #6 MRM of 5 Channels ES- / .07e5/ ||| %0r b rr Bee Time CoL 0 ,~'~,,., 20 .... , .... 2.00 , 400 .... , .... 4.00 , 600 .... ~ .... 6.00 , 800 .... , .... 8.00 , too .... , .... 10.00 7) ,~Timel I 3. cu suitonate ores 3: C4 Sulfonate PFBS [MMeetthhaannooll W Waasshh: 030504408 Sm (n, 20) MRM of 5 Channels ES- 030504A-408 Sm (Mn, 2x3) w/R A sillPe $031:Voam AA5 rEnsR. | USA NN VU sears, AT0.72 112.76 2A. 3.61 319 4.11 66.3344.. 654 | CAVA 8.87 :82 880.086 1122--MMaarr--22000044 1199::1166::5518]] LLCCI/MMSSI/MMSS #6 MRM of 5 Channels ES- 9.25 299 > 99 AMAA1..1199e3 250 Pr) oh ahs Too j | Tim|e Time 2.00 4.00 6.00 8.00 10.00 | Sysen Research, 3058 Ressaceh Drive, State College, Ph 16601 | Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTYUUBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7 -OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00112277 au_mnotsaszre 3M MN01539278 QqeuuaaynnttiiiftyyTsS5eaammppeltee,RReeFppaoorrtWto. 1020504, Exc.Dates03/05/04, Analyst.Risha PPaaggee 1166 TSSSaat~rumntdppyllmeeoNdoLLi.iif:ssittL:=eId95:8,MPPer=n\\SDeDNtaaattrNaso\\.1LL6CC:MH0S1S33M0S15SE036\43\WA1Ma,4as6sssll2Ey0xym0tnc4.x\D\FaFltlueuc:or0ro3oc/ch0he5en/mi0ic4ca,allsAs.n.FaPRlROyO\s\StSa:asKmp.plRleieDsDShB\a\003300550044AA CO CG ACST ACSFM aMLLeaactsshhttoodmm:=eoddiiftiseadd:s MMBPeoo=nn\DDaNMataatarra\\1LL1s5CCMHS11EM33AS:1E2632\W0:Ma04as16sssl220y0100n84xy\FlmuorXoc\hemPiccalallssu..PPRcROO\\rMMeettohhODcBB\\CChootteGGzrooRvvee NFDES NPDES 031504 031504 Last modified: Mon Mar 15 13=25:12 2004 Printed: Job Code= Printed: Tue ax 16 07:26:27 2008 Tue Mar 16 07:26:27 2004 same: 030504408 Name: 030504A-408 T4:extc=o sultonsse pens 4:C6 Sulfonate PFHS MMeetthhaannooll WWaasshh = 0 10am 0305044Sm4(0Mn8, 253) 030504A-408 Sm (Mn, 2x3) sw 408%sm A TRACIBENIN er - 613871 on |/ 11M 22--MMaoarrfR --22LL0C0CCh00aM/44M MnSn11SI9e9/:lMM:1s1S6S6:E#:5S5#-86 817 B12 93M0 RM10.o5 f 51.64.Chann3e9ls97E0S0- | oe'/iI I 25, 0 , 5. ca sutonate 2p.0r0os 5[M:oCt8hanSoullfWoanasthe PFOS Methanol Wash 0305044Sm4(0Wn8, 29) 030504A-408 Sm (Mn, 2x3) 1 3.19 lW w 12N gm 1.22 2.01 tw , , .... , , , bo, 500 500 i000 4.00 6.00 8.00 , , 10.00 Time _ 12-Mar-2004 19:16:58 { 12-Mar-2LL0CC0//4MMS1S/9/MM:1SS6::5#86 J~ canceoxis ping Cancel E]x is printing [] 68>09 22 ra 3sss oo K pa SIA 6.96 7 8.87 8.63 9.98 To 2 AAT | 3.92 :07 5.88 wn wr oY 499 > 99 11.02 915 11.77 200 00 5% 00 i000 | Eerie TTiime 2.00 4.00 6.00 8.00 10.00 BExxyyggeenn RReesseeaarcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee College, College, PA PA 16601 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00112288 _MNo1s39279 3M MN01539279 QQSuutauandntytiitfNyyG.1sSLaaAmmSppSllHee, RRSeeepptoorrttNo.:030504A, Ext.Date:03/05/04, Analystik.Risha sPaaggee 1177 Study No. :L1958, Set No. :030504A, Ext.Date:03/05/04, Analyst:K.Risha SLSaaamsmptpllemeodLLiiifssitte=:d: MPo=7m\D:Ma\atraD\aL15CtMa1S3M\:SL363\C:M4Sa6sNsSl20yS0n4\x\NFalusorsolchyenmixc\alPs.l.RPuORo\OS\raSoasmpcplhleeDeDBnB\\0i03c300a5500l44sAA CCGO AACCSSTFHM Mathod: Last modified: Method~ MPPo~In\\DDMaaatara\\LL1C5CHMSS1NM3SS:E262\\=MM4aa6sssall2y0y0n4x\lFulouorroocchheenmdiccaallss.. PFRROOV\MMeetthhDDBB\\CCoottGGrroovvee, NNGPDDEESS 003311550044 JLoabmtcmooad,ifi~d~ Moenm Maanrs IX 13=2~=I~ 2004 Job Code= sPreinntteedd:: Tue Maz 16 07:26:27 2004 Tue Mar 16 07:26:27 2004 NNaammea=: 003300550044AA--440039 Text: I1:.cCo6 Areciiad PpFHnA SE B01R06E02:0CConotntrrooll | wl ||{00133050500540A4-440089 5m Sm (tn, (Mn, 250) 2x3) IE 1122--MMaarr--22L00C00I44MT 1S9/:M3S8y :38#5 MRMof MRM of 5LCCChh/aMan3nnS1ne/e3lMlss5SE2S#6-96 | % dedArea 8.21 313 > 269 Ar 1.14e4 | O/o_~ \V \ in O~ , , , ~ .... I .... ~ .... I .... ~ .... ~ .... ~ 2 0 6% 2.00 4.00 6.00 2: co reid pron 2:C8 Acid PFOA (0106020 Control 0106020 Control p00o3300550044A4-440090 SSmm ((MMnn,, 226x33)) 1( ~ v ~_, \ | es\ Tine .... I .... ~ .... ~ .... ~ .... 800 1000 8.00 10.00 Time ----1r 2-Mar-2004 19:38:31 1M2R-MMaorf-26LL0CCO0h/4aMMn1nSSe9/MlM:3sSS8E:S3#-86 28a.7%3 MRM of 5 Channels ES- 13>369 413 > 369 en 1.e92a04 1.92e4 A~a [I I ~~ \Ud nggranon 122.0000 3:: CC44 sSuullffoonnaattee pPFeBeSs [00110066002200 CCoonnttrrooll 030504A-409 Sm (Mn, 2x3) [10w0l7A70 ERgAp ,2% 00 0"39~0"68 68 2"51 ao4.00 66.0000 88.5000 0100.000 Time | wn 1122--MMaarr--22L00C00I44M11S99I::M338S8::38 LC/MSIMS #6 om amd sanyo NRO rian 02) sar 742 811861 gop M10R4M5 1080 of 5 Channels 10 90 299 29 %ES- > 99 7.42 RANTS 3.473.93 4.825.11 / V ''~ A "\~11.08 926 11 [I La... ................ .......... , | 200 prs 600 800 1000 2.00 4.00 6.00 , ,,, = .... ~ .... , .... , .... 8.00 10.00 Time EExxyyggeenn RReesseeaarrcchh,, 32005588 RReesseeaazrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00112299 SW_MNO1839280 3M MN01539280 J-- [ Quantify Sample Report SEL He aa0nomn, mt. paters3/03/04, aiystir.nish Study No.=LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst:K.Risha Page 18 Sample List: 31\DaCa\LCHEMES\asslyn\Fiuerochesloals.PRO\SAspLATBA30504A CO ACEP Sample List: Last modified: oa eee\LEARNS MagsLYot\Pluorochanieai. FRO\NethDI\Cotarove DES 031504 Method: LaSt modified: Sano Job Code: P:\Da~a\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSI~I Mon Mar 15 13:22:46 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDR\CotGrove NPDES 031504 Mon Mar 15 13:25=12 2004 Printed= Tue Mar 16 07=26=27 2004 Name= 030S04A-409 = Texts 41 c6 suitonate prus 4:C6 Sulfonate PFHS [00110066002200 CCoonnttrrooll csosoin4o0 Sm in, 20) 030504A-400 Sm (Mn, 2x3) : 010.14 0.991.53 Koos an2.76 a 29RawSXree tn 5 3.57 4'244.80 5.456"01 7.09 1122--MMaarr--22000044 1199::3388::3388 LLCC//MMSS/lMMSS #6 MRMof 5 ChomclE5o- MRM of 5 Channels lEG- yo CE or 2 0.75 ~( 10.00 nw 11i39 399 7> 80 733 [sIeeYs JI Aon 8.11,8.6,1~,, 9.~ FS 2% iE an 1) do ---- 2.00 4.00 6.00 8.00 10.00 5. co suitomte pros 5:C8 Sulfonate PFOS Time [00110066002200 CCoonnttrrooll 1003300550044AA--440099 SSmm((MMnn,, 22xx33)) fi Bags 4 RSS 100-1 06 1p 2 ss on oy \ ! 0/16 1.72 2 18 301 ny 4.2~2 4.63 3.72 '~ A 505 1122--MMaarr--22000044 1199::3388::338 LLCC//MMSS//MMSS MMRRMMooff 55 CChhaannnenlseEElSSs-- 700 77 03% wm, IAL eo8 0.13 7.71 8 38 8.94 7.~00 /~/'k-~,-'/~ ~ 10.7711.14 499>99 668 f O i m sFm T Vee 28T RNAI | Time 2 py 5 5 oe 2.00 4.00 S.00 8.00 I 0.00 Exygen Research, 3058 Research Drive~ State College, PA 16801 CCROONENFNIFNDIDEEENRNTTICIAAOLLUN-- TSSYUUBBDJJIEESCCTTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OO0RR1D-D1EE0RR.2E8E9NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00113300 awmorsaezst 3M MN01539281 GQSuuhaaennyttiitf0yy. sSTaaEmmTpp0all8ee,RReeSppioorsNtee. 1020804A, xt.Date:03/05/04, Aaalyerix.Aisha J Page 19 Vp LSSSaaaattsmmuhtppdollyameeroNdoLL.iiifss:r ittLes:1d9:58P,M2Pio:\n\SoDDeaaMtae ctataarNa\\o\L.L1C5C:UHM0IS1E3NM30GS=S5S026g 42\WA:Ma,a4as6ssssblE2i0yxy0ntm4.xnD\FaFiatlueuo\:or0rFo3oc/cl0hh5eeu/im0ic4oca,alolsAs.cn.PFaPRRhlROOyO\\es\SMtSRae:aEKmhpt.pAORlABcieD)sDBCahB\oa\Itl03G30rs05o50v.04e4AANPCCDGOESAACCS03FS1M504 MSTLeaatsathtondmm:aooadiicfiieedn:s wn Har Bo ToS 1504 P=\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\MethDB\CotGrove Mon Mar 15 13=25:12 2004 NPDES 031504 PJobrCoodte:ease ar 36 07136127 2008 Printed: Tue Mar 16 07:26:27 2004 Manes 030504120 Name: 030504A-410 T3cextc=o acta pn . _ : c6 Acid PFHA 00110066002200 SSppkk AA,, 5500 nngg//LL. [[oxsaans150m in 2c 030504A-410 Sm (Mn, 2x3/ *l1 _ usEd8.19 1122--MMaarr--22000044 2200::0000::11!5 es LC/MS/MS #6 MoR f 5GraM mnois 5- MRM of 5 Channels ES- oes52504 313 > 269 EH 5.25e4 ho i} ~ a * oe2e 00 i oo m ab oe 2.00 2: cs seid oron _ _ 2:C8 Acid PFOA 4.00 6.00 8.00 10.00 Time 01110066002200 SSppkkAA,, 5500 nngg//LL. loosaosoen-451m0 vn, 26) RofSCM hamois 5- 030504A-410 Sm (Mn, 2x3) ar a>300 " 1007 . [ eal | wl 19908 8.73 19908~ 1122--MMaarr--22000044 2200::0000::1155 LLCC/IMMSS//MMSS ##66 MRM of 5 Channels ES- 16a 413 > 369 1.18e5 | Area I _ | | 0o ~-- ,,~, ,,-- r .... -- , .... -- ~ .... -- , .... -- , .... -- , .... -- , .... -- ~ .... -- , ...r . -- , ..r .. -- , r .... TTiimmee | 2 Ww a a Tom 2.00 4.00 6.00 8.00 10.00 5. ct sulfonate sro 3: C~ Sulfonate PFBS 0106020 Spk A, 50 ng. T2-Mar2004 20:00: 0106020 Spk A, 50 ng/L 12-Mar-2004 20:00:12 i 0h30504410 030504A-410 5m Sm (tn. (Mn, 20)2x3) 100~ ||| wd 2)V . PAAMAA AAa A 0a oho 2.00 4.00 6.00 LLCC//MMSS//MMSS #6 102 RMof 5GhannSel855- 7.82 MRM of 5 Channels ES299 > 99 i Toes 316 1.40e3 i" A ea WASAam ws DeoAC 8.00 10.00 Time Ixygen Research, 3058 Ressarch Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 CCHEOONNNNFEIDFPIEINNTDCIAOELU-NN- TSSTYUUIBBDJJIAEESCCTLTTRTITCOOT AAGPOPURRROOTT.TEECNCTOTIIVV2EE7-OO0RR1-DD1EE0RR.0E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00113311 suumorsssze2 3M MN01539282 qa QuuaannttiiTftyy sSIaammppSllee RSeEppoeorretsos0soan, xn.Daser03/03/04, amadyesix.nisne Praaggee 2200 SF SLSSaaaattmsmuhptpdollydemer :oNdoLLi.iif=ssittL:=eIa d9:58B,MPio:\n n\SDDDeaaMtattataarNa\o\LL.L1pC=5COH0aMS3SS1Ht0M3S5SS:E0264r2\KaA:Ma,4sago6ssesl1lE2ny0xyy0mtnm4c.xH\D\Ta\FltlPueuho:ori0ro3ooc/crh0heo5enc/mi0hic4acec,alanlslss.As.n.PFaPlRORyO\Os\S\tWaS=ezaKEpm.HlpRDaliBDes\eDhCB\ao\0t03G30E05o50v04e4AANCFCDGGESAACCS0S3FF1M504 MoTLeaantishttocdemo=oiaadtritfiiaedds: Hon wat To Tease Soot P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 PJrotbncCeoddre= Tue Mar 16 07:26:27 2008 Printed: Tue Mar 16 07:26:27 2004 oNfamemeed:= 030504430 030504A-410 T4(: e0: x1tc0C=e6602sS0uuilStfpooknnaaAct,ee 5P0pFonHmSsgiL _ 0106020 Spk A, 50 ng/L p00r33s00550044AA-441100 5m Sm (i, (Mn, 230) 2x3) 11 %] _ _ 72-Mar-2004 20:00:1 1M2R-MMaorf-25LL0CCC0hI/4aMMn2SSn0I/o:MlM0S0S:51##.56 8a.s5t4 MRM of 5 6 a0 Channels ES- 244 ea 39119..22>660e8440] Area oB h1 2% r "ho ha o 50 e Too Tine Time 50. 7: 0cC68a02Ss0uultSfoponknaaAct,ee52pP0.0Fr0nOoSgsiL 4.00 6.00 8.00 ee 10.00 2Mar2004 20:00:13 0106020 Spk A, 50 ng/L 2:05044410 8m (in, 230) aot 1MM2RR-MMMaoorff-255LL0hCCC0hIa/4MaMnn2SSnn80IeI:MolM50sSS00E:5S1##9--566 030504A-410 Sm (Mn, 2x3) " 183.9615 ea 4959.>99993 6.99e3 *| ] Area 202e.000 ee a4.0o0 5 Te Aiom n e-- ] 6.00 8.00 10.00 Time Sxygen Research, 3058 Research Drive, State Collage, 7A 16001 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- TSSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00113322 aunorsaszss 3M MN01539283 QqSuuiaaonnattiiNftoyy. sS1a1am1lp35le0e, RReeSppatoorsttNo.1020504n, Ext.Date:03/05/04, Analyst:k.Riska Page 21 Page 21 SGSSuatasnumptdplylemeoNoLLdi.icss=ittLe::Id9s58,HPPo::n\\SDDeNtaaattrNeao\\.LL1:sCC0HM3SS10MM35SS:0E634\3\AN:M,a8a6ssssllE2yyx0nt0nx8.x\D\PaFltleuu:oo0xr3oo/cc0hh5ee/nm0ii4cc,aallsAs.n.PaPRlROyO\s\BtSa:asKmp.plRleieDsDBhB\a\00330050540A4A CO CG ACS ACSFM NMLCSLaeaaaottssnhhntttooosdmmm::doooddsaiiifftiiieeoddd=:: HMPBoo:\nn\DDaNMataatarra\\LL11o5sCKMSS11HM33SS:1S2632\5K:M1a4a1g6sssl2y2y00m0n04x\\FPLluuoorroocchheenmiiccaalls..PPRROO\\HMSeEtAhDDBB\\CCoottGGrroovvee Mon Mar 15 13:25:12 2004 NEDES NPDES 031504 031504 JPorbintCeodd:e= Tue ar 16 07:26:27 2008 Printed: Tue Mar 16 07:26:27 2004 [ER Name: 030504A-411 3: ce seis pen Text= 0i0:1100C6660022A00ciSSdppkkPFBBH,,A550000 nngg//LL 0504411 Sm Mn, 263) 030504A-411 Sm (Mn, 2x3) % 810 MRMof 5 ChanSnealsshE2eS8-a0 883.61794 1122--MMaarr--22000044 2200::2211::561 LLCC//MMSS//MMSS #61 MRM of 5 Channels ES- 31344.>.11222e6559 Area o 200 ks 500 1(o/1 2.00 4.00 6.00 2: co ncsd pron _ [001: 10C06860022A00ciSSdppkkPFBBO,,A550000 nngg//LL 003e03e5004A5-401145S4mm01(M,1n, 265) 2x3) i 1 O01 500 83674~ r1e00 pre Tine 8.00 10.00 J 1122--MMaarr--22L00C00I44M220S0:I2:M211S::55#6 adr86e.77s33 s LC/MS/MS #6 MRMof 5 Channels ES- MRM of 5 Channels ES55Ta3t0e 413 > 369 241653~ res 1.31e6 Area | SE 2% 0 50 800 1000 Tim|e 2.00 .., .... , .... , .... , .... , .... , .... , .... , .... , .... 4.00 6.00 8.00 10.00 Time 3. co sutfonae peas 3: C4 Su]fonate PFBS 010 Spk6B, 5000 n2g 0 12 Mar 2004 20:21:51 0106020 Spk B, 500 ng/h (20s30504411 Sm (Mi, 2x3) 76 RofCM hanne9l9s9rE5Se-0a 030504A-411 Sm (Mn, 2x3) 7.60 288 12-Mar-2004 20:21:56 LLCC//MMSS//MMSS #6 MRM of 5 Channels ES299 > 99 77..6655ee33] Area 1001 | | E2E00 O 400 T 550 228 8E0E] Tr on1000Eons Tre Time j 2.00 4.00 6.00 8.00 10.00 Rxygen Research, 3056 Resesseh Drive, State College, 9A 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00113333 a_otsaozes 3M MN01539284 QqSuuaaannyttiiTftyy sSIaammppDllee RREeeppoorrNtte. co20s04n, xe.Dates03/08/04, Amalyesik.nisha rage 22 Page LSENSSaaaatetsmmuehtppdollyaemem:oNodoLLdi.iiifs:sittLt:e:Iid9a:58,MMpPoo:inn\SoeD\kMvtataaDtarrNaa\o\.L1L1t:5CU0eME3ST1\0M3o5:SLs026t4O2\WaA:MaEa,4asc6sNssbSl2E200yxSym0ntm4.x\oD\aaFatlseu\:os0rF23o/cyl0h5emu/m\0i4ocF,aollAsucn.aPRFohlRORxyO\Oes\S\otSaMn:acsLKmphih.plORleacRieDsDmCrahBoi\a0tl0c3a30ra0a5o5l0.0v44a.ANPCCDOGESAACC6SE3FP1M504 LEaYst eating Method: Last modified: Non Wax 1s 13153113 200 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 I~DES 031504 JProibnvCeoddse: Tue Mar 16 07226127 2004 Printed: Tue Mar 16 07:26=27 2004 Homes 030804111 Name: 030504A-411 4T:extc:s sultonace ors 4:C6 Sulfonate PFHS 01110066002200 SSppkk BB,, 550000 nngg//LL. 00T33o00550044A4-41111 Sm Sm (i,(Mn, 220) 23) | |* { 4. 0,%2.00 sos satemcesros poy [5001:10C06860022S00ulpSfpokkna8Bt,e, 55P00F00OSnnggi/LL- | |o0s3o0s5o0a4nA--a4r11s SSmm ((MMnn,, 22x33)) | 1 O01 || % { 25% 2.00 [, ase MRM of 5 Granneol5s 5ES0- 8.56 area 2709 1122--MMaarr--22000044 2200::2211::55~6 LLCC//MMSS//MMSS ##~6 MRM of 5 Channels E$- 39119..2>255e8550 Area we P10) o wo Time|| 4.00 6.00 8.00 10.00 Time 1122--MMaarr--22000044 2200::2211::56 LLCC/IMMSS//MMSS #6 MMRRMMooff 5CChhaannnneellss EESS-- 801 490>0 8.91 499 > 99 sas e7e6a4| 6.76e41Area . _ Time ~..., .... , .... ~-~,-, 1.2.7.2.5~, .... ,, , ~ Time x 3) 5 05 4.00 6.00 8.00 10.00 SExxyyggeenn RReesseeaarrcchh,, 3200558 RReessseaazrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PA PA 16001 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00113344 aunorsaszss 3M MN01539285 qQSuuiaainnattyiitNfoyy. ssTaaEmmIpp5ll55ee,RReeSppaoocrrNtto.:030504A, Ext.Date:03/05/04, AmalyetiK.Risha PSaaggee 23 23 Study No.:LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst:K.Risha NLSLSaaaaatssmmhttppollmameeo:oddLLiiiifssfittl:e:edd::PrMMP5\oo:Dnmo\aDncMMataaat\arra\L\LCL11CH55CHSMEN1S1NS3M3E0SS:326\W32\W1:Maa44as66ssssll22y0y0ma00nx44x\t\PFllyuuoormroocachhae\mmiiccPcaaalllusss...oPPBRRROOrO\\\SSMoAaATmEPcpALlDaeRhID\BCB\eo\0t03a3m0r0So50iv04e4AANFCCDGGESAACCSS03FT1MH504 MLTJeaaotsnnhttoCdmmo:aodeddriitfiioedd:~ om Mar 18 33.38.32 2008 P~\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar IS 13~2S:12 2004 NPDES 031504 Job Code: srinted: Tuo Max 16 07:26:27 2004 Printed= Tue Mar 16 07:26=27 2004 Noma. 030504n-412 Name= 030504A-412 Tveoxtc=saciawma EE (~iii+L:6~..C5..6_8.1-Ac4i~-dpSkPpFCkH,A-=.v.;v.u.2u.3.u0gr0iyt0aL0,, DDFF==1100000000 1122--MMaarr--22L00C00I44M22S00/::M44S33::4#4353 00o3300e550044A4-441122 Sm Sm (Mn, (Mn, 2)2x3) lO%Y 1886.1713990 MRM MRM of of 55LGCCnh/aMann33nSn1o1e/3lM3wlss5>oS2EEb2S6Se#6-9-s96 i Area 4.88e4 Area " o N 200 400 60_ e 500 E10d 60 Time | 2.00 4.00 6.00 8.00 10.00 22:: cCo8 Ancoiidd pPrFoOnA ___ Q[-L4-19-5fl~85-8+-4--SSppkkCC;,223500000000ngg7LiL,, DDFF==1100000000 1122-.MMaarr--22L00O004M4 S2200/::M443S3::4#4363! 00.3300550044A--441122 Sm Sm (Mn, (Mn, 253) 2x3) or MR MRM of of 55LCCChhIMaan4nSnee/M1ll>sS3E365S#-69-1 8580.7215 413 > 369 43o50a5 4.35e5 Area | sh acai n VIMNAA AAA |J I---------- WY| 0~....,., --~... ,., .... , .... , .... , .... , .... 8, 5.0.2.8.~ , .... ~ .... ,... ~-Time | Taw aw 600 800 1000 | 2.00 4.00 6.00 8.00 10.00 , 3: C4 sursonate ores (9L3L4:.A995C5488--~S4.u-lSSf~po.k[n: aCt,e226P6~F"6B~S00~6nr,gt3ffL'-,., DDFF==1100000000 :' (w030y5, 044412 Sm (tn, 223) o8n9A MRM of 5LGOhaMnSe2lM0Ts9Sw5E5eSe0-) 030504A-412 Sm (Mn, 2x3) 7.69 1122--MMaarr--22000044 2200::4433::4433 LC/MS/MS MRM of 5 Channels ES299 > 99 1.82e3 Area | A NAN | 272.| ~ ' 200 r a0 r 500 80r 0 p1000Time Time 1~i2.~ 00 4.00 6.00 8.00 10.00 | LIAsh-11 SKC 500,000. @tf ous EBxxyyggeenn RReesseeaarrcchh,, 23005588 RReesssesazrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, 7PAA 1166860011 ' `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00113355 SW_No1S39285 3M MN01539286 QQSuunaaennyttiiNtfFyy.TsSiaaamm5ppallsee,sRae"SppaooxrrtNto.:020504, Ext.Date:03/05/04, AaalystiK.xisha Page 24 Page 24 Study No.:LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst=K.Risha VLLSSaaaaatssmmhttppolldmeme:ooddLLiiiiffssitti::eedd:: BMMPPioe:\\nn\DDDaaMNattaataarra\\\L1L1LC55CCHMHEST1NMM33SSi:SEEa26\i2\aMi:Mae4dase6ssssLlbL2y0yon0ntye4x\\TFniluueoorroo\cchhFeenmiilcccaaalullsss...oPPFRRRrOOO\\\doSNaaemmtcppAlDlaBheD\DBCBe\o\0t03am30r05o50iv04e4AAN CCGO AACCSFSM FDES 031504 MLpLeaatsshrttod~m:eoodcii~tiiee~a:: Non Nar 15 13135133 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove MOn Mar 15 13:25:12 2004 NPDES 031504 PJroibntCeodd:e: Tue Nar 16 07:26:37 2004 Printed: Tue Mar 16 07:26:27 2004 [I Name= 030504A-412 4: co sutsonate pris _ Text= (V]L41:9~5C586~+-4S1-uSl~pfpioX-naC:t,-e225P50F6H~0S00-m,g,gf/tL,, DDFF==1100000000 030504412 5m (i, 22) |"TM .0c030504A-412 Sm (Mn, 2x3) _ 2884.55744% 1122--MMaarr--22L00o00m44 s220I0::M443S3::443 MoR f 5LCCha/MnM nSel/Ms SES#-e MRM of 5 Tod 399>80) Channels ES399 > 80 veal 2476~ 1.20e4Area Or Time | ,, ~ .... = .... ~ .... ~ .... ~ .... ~ .... ~ .... ~ .... ~ ~ Time 20 ato 50 800 000 2.00 4.00 6.00 8.00 10.00 5: co sulfonate pros _ _ 5: C8 Sulfonate PFOS (D)L|IE~54~9,5-~843-i5~kpkC-, 6~;.,-,,2,,5,,0,,0,0,~0,,--.n,-gD/F==:10DF0=1000000 | 1003%00}i 5044Sm4(142, 23) a1s50s3 MRMof 5 Chann9el68s0-eE255a0-0,3 030504A-412 Sm (Mn, 2x3) 1122--MMaarr--22000044 2200::4433::44:3 LLCC//MMSS//MMSS #6 MRM of 5 Channels ES- 8.88 499 > 99 8.62e3 Area e EE 2% er "0 5e 60 1) 000 Seen Tithe Time 2.00 11958-1759 4.00 00,000 nSL 6.00 t eae 8.00 10.00 Exygen Research, 3038 Research Drive, State College, PA 16601 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00113366 _otsaozer 3M MN01539287 eQQuuaaynnttiiTftyy sSouammppellee RReTeppToorrNtte. 1020504, Bxt.Date:03/05/04, Anadyssik. isha rage 25 Page 25 STSSaaatvmmuEppdllymeeoNdoLLi.iizss:ittL::eId9:58B,WPio:\n\SDDeaWtatetarNa\o\L.1LC:6CH0MS3S1U03MS51S0E3643\WA1Ma,aassssElL29xy0tny4.xD\maFtleeu:o\0r3oT/c0hi5e/mu0i4co,alrAsn.PoaPRlRcOyOs\hStS:aaeKsm.ppnRlLieaisDDhB\ca\G03a3005l50044sAA CCGO AACCSSFCM VMSLLLaeoaaattnsshthttoocsdmmmo::ooonddasiisffiiiaeeddd::: MvPoo:nn\DDaMamtaatarra\\OL1155CMMES31NM33SS:123628\::Ma41as63sssl20Ly000n4y4x\Fmlueoro\chFemilccaalulss..oPPRRrOO\\KMoeeCtchhDDBBh\\CCaoottGGnrrooivvee Mon Mar 15 13:25:12 2004 NEDES NPDES 031504 031504 PJroibntCeodd:e: Tae var 16 072602 2004 Printed: Tue Mar 16 07:26:27 2004 [E---- Name= 030504A-413 3. ce noid smn Text= )~:4Li9-:15~C636-8-A+Ic-iGdSppkPkFCH-,A2C5;G26~500n0gg0Lih0,, DDFF==11000000 10y030350045A0-44143 S1Smm3 bn, (Mn, 223) 2x3) || % pa8.r1sr7 1122--MMaarr--22000044 2211::0055::33001 LLCC//MMSS//MMSS##66 MRM of 5 Crannols E5- MRM of 5 Channels ES5260 313 > 269 "40es 4.09e5 ea | Area 2% Pry 5% 3: co ncid pron 2.00 4.00 (|Li:95C88-A+cSidpPiF,OA250608mgt, DF=1000 _6.00 ..I "~o~a-~ ep,.,"_., ...,,,,,,,u"=~^^^ ~;,~/L, DF=1000 0023035004A5-401345S4mm1(Mi3nn,, 233) 2x3) % a0 NS 8.00 ort8.71 375441 00S-------- | 10.00 2ar2004 218_.39 12-Mar-2004 21:05:30 LLCCIlMMSS//MMSS #6 MRMof 5 Channais E5- | MRM of 5 Channels ESpp 413 > 369 11..9922e66| eaArea | 111/! Wa 2.00 4.00 6.00 : C4 Sulfonate PFBS ()/~ 4958.1.Spk-6;, -25n0g0rt0.0, DDFF==11000000 305044159m in, 230) y 030504A-413 100, Sm (Mn, 2x3) 13 | | ee 200 ko 5b 2.00 4.00 6.00 L1353-7 SpkC | 0,000POIL@HE helo ah 0m 375441~ 8.00 10.00 id TTiimmee | h i17.6655 1122--MMaarr--22000044 2211::0055::33(0 Leiusims LC/MS/MS #6 MRMof Channa E5- MRM of 5 Channels 229999 >>ES999-9] Tied 1.13e4 resArea abe 0m e 8.00 10.00 Time EExxryggeonn RReesseeaarrcchh,, 33005586 RReesseeaarrcchh DDrriivvee,, SStiaattee CCoolllleeggee, PPAA 1166880011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00113377 a_orsaozes 3M MN01539288 I | QqBuuaaEnnttiiI ftyy SSaaI mmppllee RRMeeppoorrett os0son, mne.oates03/05/04, Amaiystik.nisha PPaaggee 26 SESSaatammupdplylmeeoNsoLLi.iitss:ittL::eIa9:58,HP5o::n\S\DeDMtaaattrNaao\\.LL1:CO0MM3TSM03MS5iSE0a6\43\NAuaM,asaesslsylEPmyxoennts\.xFD\alFtuleou:ro0or3co/hc0eh5ne/im0ci4ac,lasl.Asn.aFPlRRyOOs\\tSS=aaKsm.pplRleieDsDBBh\\a003300550044AA CCGO AACCSEFHM prMLLTreaaaitssthettdoedmmm:eooodtdiiiftfiiieeoddd::: MHPoo:nn\pDaMHaeattrraa\\L11L56CMGS11EM33S:92652\1i:M1a4a5s6sssd7l2y0y0m00n44ax\FFlluouroochxemiocaclsh.PFeREOO\\mMNeeiEtHhcODRBa\CCoolttaGsrroo.vvee MOn Mar 15 13:25:12 2004 NEDES NPDES 031504 031504 JPorbintCeoddie: Tue mar 36 07126027 2008 Printed: Tue Mar 16 07:26:27 2004 snes 030808413 Name= 030504A-413 4: ce suitonate ors _ Text= (O[L#~:995C586~-4S'lu-~l8.fppokin~-a,t~-e225~P6OF0H0S0000T-rQg/3L/L,, DDFF==11000000 00%330055004A4-441133 Sm Sm (in, (Mn, 230) 2x3) | 1( % Lo 25; % ho o% 2.00 4.00 6.00 ---- (~)ILD5I:.~A.C38~9,S-iu5l3fp8o;~nCa-C,t,e2+255P00-F00O06S68~-,np~g.~#pkkq~,, DDFF==11000000 /"00o33y005y054A0-44143S1Sm3m (Mn, (Mn, 230) 2x3) wl1 100~ Lo ost 22471 8.54 22471 5 i 8.00 a183s.0960s 139931 1122--MMaarr--22000044 2211::0055::3300 LLCCI/MMSS//MMSS##66 MRM of 5 Channel ES. MRM of 5 Channels ESSenos 39119..0>088e86505 onaArea Wo Time | 10.00 Time 1122--MMaarr--22000044 2211::0055::33(0 LCIMSIM#S LC/MS/MS #6 MofR5 haM nno 5- MRM of 5 Channels ES- eso 499 > 99 T2204) 7.22e4 eaArea 7% pr) Ir) 5 Tom Time 2.00 4.00 6.00 8.00 10,00 Time 1811 SpkC , 50,00 BIL Ehealule Exysen Research, 3058 Research Drive, State College, BA 16801 Exygen Research, 3058 Research Drive, Sta~e College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00113388 aunotsaszss 3M MN01539289 | | QSQtuuuaadnnyttiiMffoyy.:SSLaa1mm3ppSll6ee, RReeSppeotorrttNo.:030504A, Ext.Date:03/05/04, Analysti.Risha Page 27 Study No.:L1958, Set No.=030504A, Ext.Date=03/05/04, Analyst=K.Risha SLSaaamsmptpllmeeodLLiiissftti::odsP:MP\o:Dn\aDNtaatara\\LL1C5CHMSS1HM3SS:S622\\:MM4aa6ssssll2yy00mn4ex\\PFlluuoorroocchheenmiiccaallss..PPRROO\\SSaamapplLeaDDBp\\003300550044AA CCGG AACCSEFRM XMLLaeaattashhttoomddmo:oddiiftiieedd=: N?MPoo:nn\1DMNaaat\rra\DL115C5MaS11M33S::C236\25\K::aM14aa36ss\ssLl22y0y0L00nm44xeC\PFllHuuoorrSoocchNheenmEticcaaSllss..PPRROO\\NMeetthhDDRB\\CCoottGGrroovvee NNPPDDEESS 003311550044 GJLaoabbs.tcComoddoead::ified= Mon Mar 15 13:25~12 2004 SPertiantteedd:~ TTuuee MMaarr 1166 0077:~2266:~2277 22000084 NNTaaommeees:: 003300550044aA--442144 Text~ I1:: 06 C6 Aacciidd PpFriHnA LL11995588--55 SSppkk DD,, 1100000000 nngg//LL,, DDFF==110000 030504A-414 Sm (Mn, 213) 100,y 030504A-414 Sm (Mn, 2x3) 12-Mar-2004 21_:2_7:_1 1M2R-MMaorf-25LL0CCC0hI/4aMMn2nSSe1I/l:MM2sS7SE:S1#-86 Ea82.1147 MRM of 5 31395720694) Channels ES313 > 269 ea 9.70e4 Area | oP meme lO " 220.000 24.0000 22: :Cc8a AAcciidd PpFroOnA [LL11995588--55SSppkk DD,, 1100000000 nnggi/Lh,, DDFF==110000 3~ 66.0000 808.00 p10r03300550044AA--441144 Sm Sm (Mn, (Mn, 2x) 2x3) | sea8.n7st1 |% 1100.0000 ~ TM ~Time 121-2M-Mara-r-22L00C00I44M22S11I::M2277S::11#886 RM MRM of of 55LCCChhIaMann1nSne3e/lMl>ssSEE3S8#6--06 4133.>A0r38ee65a9| 3.08e5Area | ok > 1001%~ 0 ,~'~-~,, ..... ~ .... ~ .... ~ .... ~ .... ~ .... 1 200 400 600 2.00 4.00 6.00 3: ca sultonate pros 3:C4 Sulfonate PFBS [LL1o95s8e-s5 SSppkk DD,, 1100000000 nngg//LL,, DDFF==110000 p[0305042414 030504A-414 5m Sm (an. (Mn, 20) 2x3) 100-~ | % PANNA A an 5893~L eB tie | ~ .... ~7,,, ~ .... ~ .... ~ .... ~Time 850 1000 8.00 10.00 rea 1122--MMaarr--22000044 2211::2277::18 LOMSIMS # MRM of LCCh/aMnnSe/lMsSES#-6 MRM of 5 Channels ES- 78 2955 59) 7.63 299 > 99 E 23163] 450- 2.3 le3 Area AreANAA | L 22.0000 44..0000 66..0000 88.0000 1100.0000 i EExxyyggeenn RReesseesarzcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHGEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00113399 SW_MNO1839260 3M MN01539290 i | qQSuutaaunndttyiitfHyyo.SS:aa1mm9pp5ll8ee, RReSepeptoorrttNo.:030504A, Ext.Date:03/05/04, Analyst:k.Risha PPaaggee 2288 Study No.=LI958, Set No.=030504A, Ext.Date:03/05/04, Analyst:K.Risha I sLLSSeaaaatssmmrttppmollameoe:oddLLiiiifssfitte:=edds=PrNPMP\1oo:D\nn\DaDaMNatcaataarra\\\LLL11CC55CHHMSS1S1HN3M3SS::SS622622\\\H=:Ma44aMn66sssaLl22yy00sn00nx44x\a\FFllluuooyzrooncchhxeenmi\icccaaPalllsssl...PPPuRRROOOo\\NSNGraeAmtSophPlD1ecBeD\DBhBC\\o00et33r00om55v00ei44ANPCCDGGESAACCS0F3S1M504 aMLLeaabtsshttocmdomo:dodedisiffioedd:= Non Nar 15 13:35:13 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Me~hDB\CotGrove Mon Mar 15 13:25=12 2004 I~PDES 031504 Job Code= I Perriinntteedar: TTuuee MMaarr 1166 0077::2266::2277 22000044 | NaTaommeee!s= 0033005S0084rA--441244 Text= I 44[:L:1Cc965s8-Ss5uuSllftpooknnaaDtt,ee10PoF0rH0sS0 ngiL, DF=100 L1958-5 Spk D, 10000 ng/h, DF=100 lI003300550044AA--441144 Sm Sm (Mn, (Mn, 2:3) 2x3) | 100 | 1122--MMaarr--22L00C00/44M22S11/::M227S7::11#886 853 MRM MRM of of 5LCCChhIaMann3nSne9e/lM9lss>SEE8SS#-06-. 488.0533 ea 24104) 399 > 80 2.41e4 Area | Ober | ~-~ .... , 20 .... , .... ~ e4r 00 rr 500 800 , .... , .... , .... , .... , .... ~ .... , r100e 0 re .... , .... ~ .... Tvs Time ' 2.00 4.00 6.00 8.00 10.00 551::L19cCB588-Ss5uullSffpooknnaaDtt,ee10pPrF0Oo0Ss0 ngiL, _ DF=100 12-Mar-2004 21:27:18 L1958-5 Spk D, 10000 .g/L, DF=100 (0305045m4(1Vn4, 263) 1M 2-MoafrR -25LL0CCCh0a/4MM MnS2nSeI1/lM:M2sSS7E:S1##-~I5 030504A-414 pny Y1 Sm (Mn, 2x3) 288.59800 MRM of 5 Channels ES- 49>or99e9 499 > 99 i `Areal TM | 234~L~ fsSES SS SS ------ 0001-%~ ....~ ...., ...., ...., ...., ...., .., .., ... , : ; .., .....~ .. --, , , 200 40 65 500 ooo Ba 2.00 4.00 6.00 8.00 10.00 1.27e4Area -Time EExxyyggeenn RReesseeassrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00114400 S1_MNo1835291 3M MN01539291 1 | QEQuuaaEnnttiiTftyy SSEaammpp.llee RReeSppioorrttNe so0soen, Ext.pace:03/08/04, Anatystik.nisha Page 29 Page 29 SfSSaaatnmmutppdllyeemNooLLi.iits=sittLe::Id9:58,MPPo:rn\\SDeDwtaaatcrNaao\\.L1U:5CO0MN3STS0M3E50S\056W43\MAMa1,a4s%sssll1Ey0yxn0ntek.x\D\FaFitlueuo:or0ro3oc/ch0he5en/mi0ic4ca,allsAs.n.aPFlRRyOOs\\tSG:asKmz.ppRl1ieesDDhBBa\\0O3300550044AA CO CG ACSI ACSFM I G0antmcooddeir ted: MMLeeattshhtooddm:=odified= Last modified: Mon Nar 15 13133133 Tod MPPo:1n\\DDMaaattraa\\LL1C5CMMSS1NM3S=S6262\\:MM4aa6ssssll2y0y0nn4xx\\FFlluuoorroocchheenmiiccaallss..PPRROO\\MMeetthhDDBB\\CCoo~tGGrroovvee Mon Mar 15 13:25:12 2004 IN~PPDDEESS 003311550044 | JeoibnCeodse: Tue war 6 07.26027 200 Printed: Tue Mar 16 07:26:27 2004 | eTNammeoer: o30s0tr-as 030504A-415 T3:extc=s neta ven i: _ C6 Acid PFHA I LL11995588--99 SSppkk EE,, 2255000000 nngg//LL,, DDFF==110000 |003300550044AA--441155 SSmm ((MMnn,, 22xx33)) ' 1100 100~ | *Ls%1_ 260 2. co acid pron 2.00 2: C8 Acid PFOA a_ 4.00 "506.00 88.1177 8844882233~ 800 .~ ~-8.00 1122--MMaarr--22000044 2211. :o49o:0d4 LC/MS/MS #6 LCIMS/MS #6 MMRRMMooff 5 CChhaannnneellss EESS-- | 3 3131 >>2263 699/ 22..4455e55] eaArea 00e 0 _ e Tim | 10.00 ~ Time LL11995588--99 SSppkk EE,, 2255000000 nngg//LL,, DDFF==110000 (003300550044AA--441155 SSmm ((MMnn,, 22xx33)) 100, ii 88.771 123658 ea 1122--MMaarr--22000044 2211::4499::00:4 LLCC//MMSS/M/SM#S#:6 MMRRMMooff 55 CChhaannnneellss EESS-- 441133 >> 336699) 6.4765) 6.47e5Area 1001 123658~ | Time 0~, , , ,,,, ,~-7 .... , .... , .... , .... ~ .... , .... , .... ~ .... r ,,,, ~ .... 1 Time . 250 a 500 a0 000 2.00 4.00 6.00 8.00 10.00 5. ca sutonace oras 3: C4 Sulfonate PFBS 1L9195588--99 SSppkk EE,, 2255000000 nngg//LL,, DDFF==110000 030504415 Sm (Mn, 260) 030504A-415 Sm (Mn, 2x3) ,110000-t1 Il 227777.0806,8=55 MRMof 5 Channels ES- 1122--MMaarr--22000044 2211::4499::0044 LLCC/IMMSS/M/SM#S#t6 MRM of 5 Channels ES- 2299199.1>>7e99499|| 1.1AAr7reeeaa4l |% O2% e a Se ho ko e 1000 Tine | | die gies gees ais Time 2.00 4.00 6.00 8.00 10.00 Exygen Rosesrch, 3058 Research Drive, State Collage, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00114411 m_orsaozse 3M MN01539292 ' QQSuuaaEnnttiiEcfyy sSIaammppEllee RReeNppeoorrttcov0s0un, mxt.Date:03/05/04, Hamtyack.nisha rPaaggee 2300 SLSSaaatsmmutppdllyeemNooLLt.iis:sittL::Il9e58,MPPe:rn\S\DeDNtaaatraNto\a.L1\:5C0LM3S1O0M3S54SE056W43\AaMi,aesssssllETyoxontytx.D\maFtleue:o0r3o\/c0hF5e/m0ilc4c,aalulsAs.n.oaPFlRRryOOs\\tSSo:aaKma.pcpRllieDhsDBBh\\ae00330n05500i44AA CCOG AACCSEFPM [T= artmcoonaes tea: Last modified: Method: Last modified: NMP2oo:nn\DDaNMataatarar\\LL11oC55oMES11wM33sS:1e623\\21KM:3aa4s36sassl22yy00mn00ex44\\FFlluuooxroocchheesmiiccaallss.. PFRROO\\MeeEtHhDDBB\\CCoortGGrroovvee Mon Mar 15 13:25:12 2004 NNPFDDEESS 003311550044 | eJoibnCeodre: rue war 6 07.2627 200 Printed: Tue Mar 16 07:26:27 2004 [ Toe ---- Name: 030504A-415 T4:extC:6 surtomace pee _ 4: C6 Sulfonate PFMS 1 |LL11995588--99 SSppkk EE,, 2255000000 nngg//LL,, DDFF==110000 |ososoun-st6 5m vn, 2) 030504A-415 Sm (Mn, 2x3) pw 1" 1 O01% *] _ 18a2.s451o34 1122--MMaarr--22000044 2211::4499::00:4 LLCC//MMSS/M/SM#S#6 MRM of GrreeE5l- MRM of 5 Channels ES- 5-550 39a9 e>d8]0 5.97e4 eaArea ot 20 pry i ako To 2.00 4.00 6.00 5. ca sulfonase pros _ _ _ [5L1:18C955888--S99ulSSfppokknaEEt,,e2255P00F0O0S00 nngg//Lh,, DDFF==110000 (0a305044415 Sm (Mn, 2) am MRMof 5AChanen5el5s5nE0S-0 030504A-415 Sm (Mn, 2x3) 8.00 8.90 8655 10.00 TTiimmee 1122--MMaarr--22000044 2211::4499::0044~. LC/MS/MS #~ MRM of 5 Channels ES- 49339.55>33e9449 | * ea| | 6696~ | 1to0/"! .... , ......... - 200 "0 13) a 0m | 2.00 ' ....4.00.' ... ' ....6.00.' ... ' ....8.00'; ' ' ' ' ....10.00.'... ' .... | Area TTimmee | ESxxyyggeenn RReesseeaarrcchh,, 32005588 RReesseesasrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PFAA 1166380011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00114422 m_morsaozss 3M MN01539293 ' I qQSuutaaunndyttiitfNyyo.isSLaa1mm5pp5ll0ee, RReeSppetoorrttNo.:030504h, Ext.Date:03/05/04, Analyst:K.Risha Page 31 Page 31 Study No.=LI958, Set No.:030504A, E~t.Date:03/05/04, Analyst:K.Risha 1 iLLSSaaaaatssmmhttppmollaomeeroddLLiiiifsshittee::dd:: MMPPooP:rnnr\\\DDNMDaaaaatttrraaa\\\LL11LC55CCHMHSS11SH3M3MS::SS226S\22\\N=:Maa44ass66ssaslll22yy00ynm00nex44x\\\PFFllluuuocorrroooccchhehenenimicicecalalsls.s..PPPRRROOO\\\SNSaSnmEpLplDlaEeD\DPCB\o\0t03G30r0So50v0e44AAXFCCDGGESAACCS03FS1M504 MLoLeaabtsshttoGdmmo=ooddd:iiffiieedd:: Non Na 15 13:23:13 2004 P:\Data\LCMSMS6\Massllrnx\Fluorochemicals. Mon Mar 15 13=25:12 2004 PRO\MethDB\CotGrove NPDES 031504 Job Code: | Perriinntteeadr: TTuuee MMaarr 1166 0077::2266::2277 22000044 | eTNammoea= 003300550044nA--443166 Text= (1: : cCLo6 aAcc1itSda kpP9rFiHFnA,8250080 ng-/L, 1OF=3 100 L1958-13 Spk F, 25000 ng/L, DF=100 10v03o300550044AA-.441166 Sm Sm (Mn, (Mn, 2x3) 2x3) 1 * ~ ER 2580.114553 1Z2a-Mrar-22L00O004M8S22I22:M11S00:4433#5 MRM MRM of of 55LGCChh/aMan3nnS1no9e/lMl.ssS2EE6SS#.0-6 3132>5e20a5, Area 0 + 200 "00 600 800 e100e 0 Time Time 2.00 4.00 6.00 8.00 10.00 [22:L:19cC58a8-AA1cc3iiddSppPkrFOoFAn, 25000 ng/L, DF=100 _ _ _ 12-Mar-2004 22:10:43 L1958-13 Spk F, 25000 rig/L, DF=100 LC/MS/MS #5 12-Mar-2004 22:10:43 i00e33s0055004A4-441166 SSmm ((MMnn,, 221x33)) 871 MMRRMM ooff 55LGCCnh/aMann1nSne3/elMl>ssS3EE6SS#-0-6~ || 111 1185.74123 Area 41366..>11434e6e595 " Area 1 | i| 0~',, ,,,,, 2-00 ,,~'~ .... , 40% .... , .... , 650 .... , .... , 85 ....11, 5.4.2.3.~ , 1-- 000 -- .... ~ .... , .... Time 2.00 4.00 6.00 8.00 10.00 33[::L1c9Ca~58-Ss1uu3llfSoopnnkaattFee, 2pP5rF0eB0Ss0 ng/L, DF=100 i} _ 12-Mar-2004 22:04 L1958-13 Spk F, 25000 rig/L, DF=100 03050444S1m6 (Mn, 223) 1R2-MMaor-f52LL0GC0Oh/4aMMn2nSS2a/Il:M1sMS0E#:SS4#-36 1" oy 030504A-416 Sm (Mn, 2x3) 22770.6817 MRM of 5 Channels ES- 296958939 299 > 99 | 1 io/~ 2207~ eal 8.83e3 Area ITM ~ oe | anew ae ae 2.00 4.00 a e n n_ Time| 6.00 8.00 I0.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00114433 SW_MNO1S39204 3M MN01539294 QQSuueaaannltytiiftHoyy. Ss1aa0mm10pp5ll8ee, RRSeeepptoorrttNo.1030504A, Ext.Date:03/03/04, Analystik.Risha Praeggee 3322 Study No.:LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst:K.Risha SLSaaamsmptpllemeodLLiiifssitte=:d:P:MP\o=Dn\aDtMaaat\raL\CL1M5CSMM1S3SM:SS26\2\N:Ma4as6sssll2y0yn0nc4x\\PFlluuoorroocchheenmiiccaallss..RPROO\\SStapmlpelDeBD\B\003300S50044AA CCGO AACCSSTFHM wethod: Last modified= Method: MPPo=rn\\DDMaaattraa\\LL15OCHMSS1NM3SS=2662\\=M4aN6ssal2y0s0n4x\aFlluoyronchexmi\ccaalllss.u.PPRRoOO\\rMMaeotthhDcDBB\\hCCooettGGnrrooivvee NNPPDDEESS 003311550044 oLabstcomdoedrifisd= Mon Mar 15 or 13~25~12 2D04 Job Code= PPrriinntteedd:= TTuuee MMaarr 1166 0077::2266=:2277 22000044 NTNoaemmxeet:= 003300550044AA--441166 Text= 44L::19Cc56o6-sS1uu3llffSoopnnkaattFee, 2pP5rF0iHsS00 ngiL, DF=100 L1958-13 Spk F, 25000 rig/L, DF=100 10103030005,50044A4-441166 SSmm ((MMnn,, 223x33)) 1i wl SE 88.5522 11586 12-Mar-20-- 04 22:10:43 1M2R-MMaorf-2LL0GCC0hI/4aMMn2nSS2oI/:lM1Ms0SSE:4S##3-6511 MRM of 5 39> 60 Channels ES- I 399 > 80 55.66A33r0ee44a Area 22.0000 44.0000 55: :Cc8o sSuulltfoonnaattee [L1956-13 Spk F, PpFrOoS s 25000 ng/L, DF=100 L1958-13 Spk F, 25000 nglh, DF=100 10033005l50yy044A4-441166 Sm Sm (Mn, (Mn, 233) 2x3) | 6%6.00 88.0000 _ 888.88 3 6142-~ 10.00 Time Time || 10.00 1122--MMaarr--22L00C00I44M22S22I::M110S0::4#4363 MRM MRM of of 55LCCChh/aMannnSn3ee/l9Mlss9S>EES0S#.0-6 499 > 99 32n50a4 3.25e4 Area | BeeTime ,, .... , .... , .... ~ .... , .... , .... , .... , .... , .... , .... Time 200 400 600 800 i000 2.00 4.00 6.00 8.00 10.00 EBxxyyggeenn RReesseeaarrcchh,, 3200558 RReesseeaarcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PA PA 16801 16801 `CHGEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00114444 IM_MNO1539295 3M MN01539295 uQSuiaalnndttyiifNyoy. 1saTam1mp5p5ll8ee, RReeSppaoocrrttNo.103050(A, Ext.Date:03/05/04, Analystik.Risha PPaaggee 3333 Study No. :L1958, Set No. :030504A, Ext.Date:03/05/04, Analyst=K.Risha LeLSSaaaatssmmhttpplolmemesooddLLiiiiffssiittee::dd::P1MMP5\/oo:D\nn\aDDtaMMaataata\rra\L\CLL11M55CSMHHS11SM33SE=S:2\6222M\W::Maa44ass66ssssll2y21y00n00nxy44x\\PnFlluxuoos\roocPchheLemmiuiccoaallzss..oPPPRRRcOOO\\\hNSSeaaeEmmhppnDllReei\DDCBBco\\t00aa330z0l5o50v0s4e4AANPCCDGGESAACCS0SF3T1M504 LSMLeaaatsSbhttocdomm:dooeddsiieftieedd:: Mon Mar 15 13:23:12 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 Job Code: PPrriinntteedd:: TTuuee HMaarr 1166 0077::2266::2277 22000044 HTNaeazxmete:s= 003300550044AA--441277 Text= (p/LFI1o:95C86-A#c7iSdpPkFHGA, 10000 ngiL, DF=100 L-19.58.4"/Spk G, 10000 ng/L, DF=100 (l003as0500540A4-4A1-74SS1mm7 (in, (Mn, 263) 2x3) 1.,,~ Y #3 T 12-MaR r-2L0C0A 4M2S2M:3E S2:30 as MRMof MRM of 55LCCChh/aMan3nnS1nae/3iMlss5SEE2SS6#-9-6) ES 8.15 313 > 269 69r3e4a)l 8.93e4 Area ~ Oe A O I.."~-, ,, .... , .... , .... , .... , .... , .... , .... , .... , .... , .... ~ .... 236 400 600 ado i000 2.00 4.00 6.00 8.00 10.00 Time 2: co acid pron cer @[42b:-10JC838688A4c+-i7Sd-SppPkkFOGGA,, 1100000000 nngg/lLL,, DDFF==110000 l1 {103"05048.417 Sm (in, 23) 108969917 MRM of 5LCChIaMn1nSe3Il5M>s7SAE3r3S#6e-50a5 030504A-417 Sm (Mn, 2x3) 8.69 109917-~ 1122--MMaarr--22000044 2222::3322::3300 LC/MS/MS #6 MRM of 5 Cl~annels ES413 > 369 5.73e5 Area | o SR SER ~ , , ,--'- .... , .... , .... , .... , .... , .... , .... , .... , .... , ....- Time 200 "00 600 800 1000 il 2.00 4.00 6.00 8.00 10.00 3: ca suitonate prs ( 3L:4i9~C5848--1S4u77lfSSoppnkkatGGe,, P11F00B00S0000 nngg//LL,, DDFF==1I0000 / (0305042-417 Sm (tn, 253) MRM of 5LChIaMnSInMoS:ES- 030504A-417 Sm (Mn, 2x3) | oy 175660 20B95r>3e0)a9 1'" 7.59 1122--MMaarr--22000044 2222::3322::3310 LClMS/MS #6 MRM of 5 Channels ES299 > 99 8.93e3 Area | A. | Nene UE SI | TE Time 0 .... , .... , .... , .... , .... , .... , .... , .... ,, T,,,~,,-,,~-~-,,~.---~--,.,--~, Time 200 400 500 800 1000 2.00 4.00 6.00 8.00 10.00 BLEs8-1 blo EIxxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHGEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00114455 SW_MNo1839296 3M MN01539296 QiQuunaadnnyttiiNtfoyy.1Ss5aa3mm3pp5ll0ee, RReeSppaororrttNo.:030504A, Zxt.Date:d/05/04, Analyet:K.Risha Page 34 Page 34 GSSSaatanmumtpdplylemeoNdoLLi.iif=ssittLe::Id9:58,MPo:Pn\rSD\eHtDaaatrtNaao\.\L3=L5C0CM3HS10SM35MS10S634G3\A\1M,M4aa6sssslE2ly0~y0ntm4.xcD\\aFFtlleuu:oo0rr3oo/cc0hh5ee/mn0ii4cc,aallAssn..aPPlRRyOOs\\tSG:aaKmm.ppRllieasDDhBEa\\003300550044AA CG CG ACSF ACSFM NMLSLLaaeaaatbtnSs.nhettoocddmmom::doooeddd:iiifffiiieeeddd::: MMP5oo:\nn\oDaNMaaattrraa\\LL3155CCMHS11SM33HS=E362\32\1N:M14aa36sssl22y00a00nl44x\yFlmuoar\ocPhelmiuccalrs.oPPRcRO\hOMSeettnhADDiBB\\cCCoaottlGGrrsoovv.ee Mon Mar 15 13:25:12 2004 NPDES NPDES 031504 031504 Job Code: Printed: Tue Max 16 07:26:27 2004 Printed: Tue Mar 16 07:26:27 2004 Nama: 030504A-427 Name= 030504A-417 Text= 4. ce sulfonate prs L4956+47 Spk G, : C6 Sulfonate h-~958=l-7-Spk G, P11F00H00S0000 nngg//Lh,, DDFF==110000 0305044417 Sm (Mn, 213) 10030504A-417 Sm (Mn, 2x3) 1 O01 % 1122--MMaarr--22L00O004M4 S222I2::M332S2::33(] 822 MRMof MRM of 55LCCChh/aMannnSnEae/lMlssSEEaSS#--6 Eg8.52 399 > 80 25e30a4 2.93e4 Area 1 IiI .... , ....20, 0.... , ....40, 0.... , ....60, 0.... , ....50, 0.... ,-,,,,1s0,r00.e.e..p,~e-~,r, Tie Time 2.00 4.00 6.00 8.00 10.00 5: co sultanate pros ( [~ L: 19C8886S=1u7lfSSoppnkkatGGe,, P11F00O00S0000 nngg//LL,, DDFF==110000 1122-.MMaarr--22L00O0044MS2222I::M332S2::33(0 00;330050540A4-47174S1Smm7 (Mn, (Mn, 253) 2x3) ass RMof MRM of 55LCCChh/aMannnSn9ee/lM9lss>SEE9SS#-9-6 ast 8.88 499 > 99 23"20o4a) 2.32e4 Area %!i | olor pen Bee Tina 2002.00 4004.00 6006.00 8008.00 1000 10.00 Time | OLass-| eo ESxxyygoeenn RReessesaarrcchh,, 32005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PA PA 6601 16801 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 1993399..00114466 SW_MNo1S39267 3M MN01539297 QquuaannttiiT ftyy Ssaae mmppllee RReeMgpToorrttNe. sososaun, mx. Daterc3/05/04, Analyscix.Risk sage 35 Page 35 NLSESSaaaaattsmvmuhtppEdollyaemem:ooNddoLLii.iift:ssiitLt:ee:Iad9::5P8i,MMFP\eo:DDnn\SaaeDttMwtaaaata\rrNa\Lo\O.L11LH:55CEI0MNN3S110SM33S5E:iSE0\2E64M2d\A:iaMa,4esan6esss:sEl2yTyx0hyoo0tnxs4.x\D\PaFl\tlueuc:orF0ro3oc/chl0he5en/mui0ic4ccaa,aolllssAs..nz.PaPFRlRROyoOO\s\\GtSWac:aesKmSp.phlhRlDeieBDsD\EehBC\a\o00t3n3a00s5o5d0v04e4AANFCCDGOESAACCS0TF3H1M504 MLLeaatSshttocdmmn:oodcaitftiieedd:: Non War 35 13:35:13 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 JProibntCeoddre: Tue Max 16 07.26.27 2004 Printed: Tue Mar 16 07:26:27 2004 sNaammee: 003300550044A--441188 Tiecxte= ciao _ i IXX:CC00C336005A50c04i4-d-11,,PF22H55A nngg//LL SSttaannddaarrdd 1122--MMaarr--22000044 2222::5544::2233 03050444S1m8 (Mn,2) MRM of 5LLCCCh//aMMnnSSo//lMMsSSE#5#-56 030504A-418 8m (Mn, 2x3) 100; 8540 8a.117 5549- 30e20a4 MRM of 5 Channels ES33131 >>2263699) 3.02e4 % Area \I 200 T E 400 , 500 e abo po sriS00a0nrAme-- e Tine Time copeiamron 2.00 4.00 J 6.00 8.00 10.00 (C030504-1, 25 2: C8 Acid PFOA XC030504-1, 25 nngg//LL SSttaannddaarrdd 1122-.MMaarr--22000048 2222::5544::2233 00o330n0550044A8-441188 Sm Sm (Mn, (Mn, 263) 2x3) io8a.7nr1 MRM MRM of of LLCC//MMSS//MMSS ##66 5 Crannols 5. 5 Channels ESeasseed 413 > 369 ea 6.56e4 ">1001 10181 Area A ee Ning 200 "0 500 800 000 2.00 4.00 6.00 8.00 10.00 Time \ onanr7s8 5. ca eulfonate bras _ X3X:CC00C343005S50u04l4-f-1o1,n, a22t55e nnPggF//BLLSSSttaannddaarrdd , 1122--MMaarr--22000044 2222::5544::2233 LC/MS/MS #6 030504S4m(1Mn8, 263) a MRM of 5Channels ES. 030504A-418 Sm (Mn, 2x3) 2959 owtMagP\aCmRaX o| /\ PeVoW A 91 arR s E uz S pv 1563 / h100~ 0.82..0~9 1.~55 2~32.78 3.5, 474 553 4.7~4 ~ 7.,38 . MRM of 5 Channels ES- "11r.s7 ;. 299 > 99 oer,. 286 +00 500 %]0.I"~, "_-_"/~" 2.00 \, 4.0, 0.... 6.00 r abo rooor Time , .... , .... , .... ~ .... , .... Time 8.00 10.00 xExyyggoenn RRaesseeaazrcchh,, 33005588 RReesseaaarrcchh DDrriivvee,, SSttaactee College, College, APA 16803 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00114477 m_orsaozse 3M MN01539298 QQSutuauandntytiiNffoyy.1sS1aa1mm5pp5ll8ee, RReeSppeootrrtNto.:03004A, Ext.Date:03/05/04, Analyst:X.Risha aPaggee 3366 Study No. :L1958, Set No.:030504A, Ext.Date=03/05/04, Analyst:K.Risha SLSaaamsmptpllemeodLLiiifsstti:=ed: oPP=n:\\DMDaaatrtaa\\1L5LCCMHS1S3MM:S2S62\\:MM4aa6ssssll20yy0nn8ex\\FFlluucorroocchheenmiiccaallss..PPRROO\\SSaammpplleeDDBB\\003300550044AA CCOG AACCSSFPM MLoMLaeattsshhttooddmm::ooddiiffiieedd:: MPMPoor:nn\\DDNMaaatatrara\\L1L1C55CHMSS11KM33S1S:S22652\\1:MM14aa26ssssll22y00yn00nc44x\\FFlluuoorroocchheenmiiccaallss.. PPRROO\\NMSetthhDDBB\\CCoottGGrroovvee NNEPDDEESS 003311550044 JLJooabbstcCmoododeed=rified: Mon Mar 15 13:25=12 2004 PPrriinntteedd:: TTuuee MMaarr 1166 0077::2266:=2277 22000048 NNaammee:= 003300550044aA--441280 Text= s4X::C0cC36605sS0uu4ll-ft1oo,nnaa2tt5eenpPgrFiiHLcSStandard XC030504-1, 25 ng/L Standard 10T03o300550044AA--441188 Sm Sm (Mn, (Mn, 263) 2x3) * i; 1122--MMaarr--22L00C00/44M22S22/::M55S44::2#2~63 854 MMRRMMooff 5LCCChh/aMannSnn3/eoMlls9S>EE8S9S#.06-1 181.5640 39779..1A1>r55ee86a303l Area 22.0000 44.0000 56.0000 X55:C:0Cc38o05sS0uu4ll-ff1oo,nnaa2tt5ee npPgF/rOLoSSs_tandard XC030504-10 25 ng/L Standard 0305044S1m8 (Mn, 263) 100 030504A-418 Sm (Mn, 2x3) P-- 200 r 400 p 600 2.00 4.00 6.00 800 1000 re Time Time 8.00 10.00 1122--MMaarr--22L00C00I44M22S22I::M55S44::223 888 M MRMoofR f 55LCCChhaIMM annnSn4e/elM9lss>SE9SS#9--6) 8s.i8z8 49339.22A>116e9l339 Area A --8-- 00 ------1--000 rrTima Time 8.00 10.00 xExyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACPOPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00114488 3M_MNO1539209 3M MN01539299 QSquueaunnyttiitfIyy sSaaB mmppllee RReeEppRoorrRtto1020504, Bxt.Date:03/05/04, Analyser.Richa sage 37 Page 37 VSESSLaaataTtsmumhEtpdpolylSseme:oNodoLLi.iiiTfss:iti~Le:=e1ad9:=585,wMBp:oo:D\nn\StDDeaaMMtaC\aatarrNaL\o\OL.L31NC65C:HEM0SNS113HMS330S51S=ES0a26432\WA:1Ma,4aaag6sssLlE22s0x9y00tnyl44.xD\yaeFtlmeu:\oc0r3o\/Fc0hP5e/lmi0i4ccu,uaallosAso.nr.PaPPolORRryOMOcsN\eS~Stoha=ahrKmDep.pSclRl\neieCDsDhioBhBt\a\cGG0er33ao00v55nl0e04.4sAANECCDGGESAACCS0F3T1M504 MoSLeaantsnhttocdom~=dooaddriiffiieedd=: Hon Mar 15 13135115 2908 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13=25:12 20D4 NPDES 031504 JPoribntCeoddse= Tuo Mar 16 07:26:27 2008 Printed: Tue Mar 16 07=26:27 2004 p-- Name= 030504A-419 Toms Text= 1: ce rca smn I: C6 Acid PFHA LL11995588--11,, DDFF==220000 003030s50054A0-44149 1SSm9m in,(Mn, 233) 2x3) \ =i|l 1122--MMaarr--22000044 2233::1166::1111 LomsIMS LCIMS/MS #6 MRMof 5 Channol 5. MRM of 5 Channels ES- sro 31200 482,1590 31311.>.6A62r44e06ea494l) rey Area 1 WN |a d 260 r a e 60 500 e i000 2.00 2. co reid pron _ 2:C8 Acid PFOA LL11995588--11,, DDFF==220000 0i3%05044410 Sm (Mn, 2:3) 25s25e8 MRMof 5 ChaannsaToeme5a.s 030504A-419 Sm (Mn, 2x3) me ee em" 4.00 6.00 8.00 8.69 10,00 \ Time 1122-.MMaarr--22000044 2233::1166::1111 LLCC//MMSS//MMSS ##66 MRM of 5 Channels ES413 > 369 1.61 e5 Area - ee Tine ~ 200 4% 506 00 i000 2.00 4.00 6.00 8.00 10.00 \ Time 3. ca surtonace oem 3: C4 Sulfonate PFBS |LL11995588--11,, DDFF==220000 0504-41S9m (in, 233) MRMof 5LGCrIaMnSeIM#5-S6 030504A-419 Sm (Mn, 2x3) | ; a15s7t 292>5e90a93 100! 1122--MMaarr--22000044 2233::1166::1111 LCIMS/MS #6 7.57 MRM of 5 Channels ES299 > 99 3.96e3 Area | %| PAPA AATIN Arm [-- Sn -------------- , ...........................~ , .... ~ .... ~ .... , .... ~ .... 200 4d 650 500 1000 j 2.00 4.00 6.00 8.00 10.00 Time EExxyyggeenn RReesseeaarrcchh,, 33005388 RReesseeaarrcchh DDrriivvee,, State State College, College, TA PA 16001 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00114499 _Mo1539300 3M MN01539300 QgSiuuaaaannyttiiNfsoyy.s1SLaa1mm3pp5ll0ee,RRee$pp6oorrtNto.:030504A, Rxt.Date:03/05/04, Analyst:X.Riska PPaaggee 2308 Study No. :L1958, Set No. :030504A, Ext.Date:03/05/04, Analyst=K.Risha MLGSSaaaaacnmsmhtptpollammee:ooddLLiiiiffssiitt:e:edd:: MMPoo::\nn\oD\NMnaaattDrraaa\\1L1Lt55CeMaHS11M\3M3S:S:EL32632\OM1=Ma44Maa66sSss1l22My00ym00Snx44x\S\PF\lluuMcorarooscchhseenlmiicyccaaamlllaess...\PPRRRFOOO\l\\SSAauaEnmpEoplDlxeEeD\oDBCB\co\0t0h3G30re0So5Onv04a4iAAKCECDOGESAACCS0F3S1M504 LaMLaeabtsshttocdmom=dooeddriitfiieedd:: Mon Mar 15 1312311 2008 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 Job Code: Printed: Tue Mar 16 07:26:27 200 Printed: Tue Mar 16 07=26=27 2004 NNTaaommeees:= 003300550044AA--441199 Text= [44L::scsC66ss1Su,ulltDfoFonn=aa2tc0ee0 pPrFiHsS L1958-1, DF=200 00033000,55)0044A4-441199 S5mm (Mn, (Mn, 2:3) 2x3) ] ] frerene ee 2062.00 a04.00 5006.00 5: co sulfonate pros oo 5[LL:11C9858588--S11u,,lDDfFoFn==a22t00e00 PFOS l0305044410 Sm (Mn, 253) 100. 030504A-419 Sm (Mn, 2x3) 100 || [ee a 500 J 0~ ee A .... , .... , .... ,~,, .... , .... , 2.00 4.00 6.00 12-Mar-2004 23:16_:11 1M2R-MMaorf-25LL0CCO0h/4IaMnS2nS3Ie/:lMM1s6SSE:1S##1-651I 8180.551226 MRM of 5 Channels ES- 39S>at8e0 399 > 80 `wea 5.41e3, me 850 1000 8.00 10.00 1122--MMaarr--22[000044C2233:T:1166::1111 as MRM MRM of of 55LCCChhlaMannnSn4a/ei9Mlss9S5EES9S#-9-6 13%8~86 499 > 99 7.r01e6a3 7.01e3 || Area 800" T de M ~ Seer So lg, WO| .... ~ .... , .... ~ .... , .... Time 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 1199339..00115500 SM_MNo1839301 3M MN01539301 Tr SEA ae re Quantify Sample Report Study No.=LI958, Set No. :030504A, Ext.Date:03/05/04, Analyst:K.Risha Page 39 HL. LOE stern eames Co aso Sample List: fe sh neem Last modified: i a 0 erocentoste mooncore mrs 3351 Method= i RE GT Last modified: a Job Code= P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13=22:46 2004 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25:12 2004 Printed: Tue Mar 16 07:26:27 2004 =Name= 030504A-420 Text= : C6 Acid PFHA |LL11995588--11 RReepp,, DDFF==220000 :|0300350045A-04240AS8-mm4(M(2Mn0n,, 22xx33)) | aa eSpL | %ih \ Vo Nee 8.21 4466 meee me rE 2.00 4.00 6.00 8.00 Ey = 2: C8 Acid PFOA [L1858-1 Rop, DF=200 12-Mar-2004 23:38:06 L1958-1 Rep, DF=200 100003300550044AA--442200 SSmm ((MMnn,, 22xx33)) 00 88.8699 33113322 2 "% 1122--MMaarr--220000442233::3388::0066 LLCCI/MMSSI/MMSS ##66 MMRRMMooff 55 CChhaannnneellss EESS--| 313 > 269 11.T77eed4 mmAAA Area1 10.00 A Time 12-Mar-2004 23:38:06 LLCC//MMSS//MMSS ##66 MMRRMMooff 55 CChhaann4nn1eel3lss>EE3SS6-9-, 413 > 369 11.66556e55 Area | on T - m rrr T ak e Tie 0~,"---~,,,,, ,':q- .... , .... , .... , .... , .... , , , , , 2.00 4.00 6.00 8.00 ,, .... , .... ,,,, ,~'Time 10.00 losoaznsm. 20 [3L:19C548-S1ulRfeopn,atDeF=P2F0B0S L1958-1 Rep, DF=200 | 030504A-420 Sm (Mn, 2x3) O0 |% % 0 urna Ssme 1122--MMaarr--22000044 2233::3388::0046 LLCC/lMMSS//MMSS ##6 MRM of 5 Channels ES- 7.60 299 > 99 874- 4.29e3 Area mm NANA A em ae 01 .... r ' ' ' ' I ' ' ' ' I ' ' ' ' I .... I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' a ae ae 2.00 4.00 6.00 8.00 10.00 Time j Exygen Research, 3058 Research Drive, State College, PA 16801 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00115511 3M MN01539302 gSQtuuuaadnnyttiiMtfoyy.rsSiaa1mm3pp5ll6ee, RRSeeapptoorrNtto.:030504, B<t.Date:03/05/04, Analyst:K.Risha PPaaggee 4400 Study No.:LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst:K.Risha LSSaeaammtppllmeeodLLiiisstti::eds PMPro:\n\DDaHatatara\\LL1C6CHMS1SH3MS:SE36\3\N:Ma4as6sssll2y0yn0nx4x\\TFilvuoorroocchheenmiiccaallss..PPRROO\\SSaanmpplleeDDBB\\003300550044AA CCOG AACCSFSM HLLMaeaattsshhttooddmm::ooddiifeiieedd:: FMMPieo:\nn\DDaMNataatarra\\L11C5C5HMIS11M33N:S:E26232\M::Ma34ag36sss1l22yy00m00nx44x\\FFlluuoorroocchheenmiiccaallss.PPRROO\\MMeStAhDDEB\\CCoottGGrroovvee NNPPDDEESS 003311550044 Job codes Last modified: Job Code: Mon Mar 15 13:25:12 2004 pPrriinntteedd:: Tue Max 16 07:26:27 2008 Tue Mar 16 07:26:27 2004 NNTaaemsxeat=:! 003300550084AA--442200 Text= 44[:L:1C9c6568-Ss1uulRlftooopnn,aaDtteeF=Pp2Fr0Hi0Ss L1958-1 Rep, DF=200 00;3300550044A4-442200 Sm Sm (Mn, (Mn, 253) 23) 100t " 1122--MMaarr--22L00C00I44M22S33I::M33S88::0068 852 MRMof MRM of 55LCCChh/aMannnSn3ae/iM9lssS>E5S#8.0-6) 10858.52 1095 399 > 80 54e50a3 5,45e3 Area |1 E- = ---- ee Ta2b.00 44.0000 66.0000 88.0000 1100.0000 Time 55[:1:9CC58o6-sS1uullRffooopnn,aattDeeF=Pp2Fr0Oo0Ss 12-Mar-2004 23:_36:06 L1958-1 Rep, DF=200 0305044420 Sm (Mn, 253) 1M2R-MMaorf-25LL0CCC0hIl4aMMnS2nSI3e/MlM:3sSS8#E:S#06-66 030504A-420 Sm (Mn, 2x3) 881.808779 MRM of 5 Chann14e9969s93>>E40S00-3 "area * | 11o/~_1109~_ ~ 634e939Area | T 200 T Pry T 500 850 r 7000 ea| 2.00.' ... ' ....4.00.' ... ' ....6.00.' ... ' ....8.00.' ... ' ....10.00.'... ' .... Time | xExyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 | `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00115522 SW_MNO1839303 3M MN01539303 QSQeuueaalnnyttiiTtfyyTSSaaBmmppll.ee RR"eeSppeoorrNtto. 020504, Ext.Dates03/05/04, Analyst.isha Page 41 Page 41 SGSSeaatmnmupptdllyeemNooLLt.iii:ssttLl::Ie9:58,MPBe::n\\SDDeWataettNraao\\.LL3=OC60HM3SS10M3M5S1S0E3643\WA1Ma,4as6ssslE2L9yx0tyn4.xDm\aFteleu=\o0r3Fo/c0ih5e/um0i4oc,arlAson.aPPclRRyOOhs\StSea:aKzmn.ppRlliieesDDchBBa\a\033l0055s0044.AA CCGG AACCSFTM VGMLLeaeaatntsshhtttmoocdaommo:rdoodeddiriiffliiaeeddds:= PMMPeoo:nn\loDMaeatatrara\\LL13O5C5NMES11M331S=36232\1=Mk34aa36gseslL329y0y00no44xn\FFluioruocohermiocalcs.hPRReOO\\nMMeedtthhDcoBB\a\CColottGrsroov.vee Mon Mar 15 13:25=12 2004 NNEPDDSESS 003311550044 PJroibntCeodd:e= Tue war 16 07:26:27 2004 Printed: Tue Mar 16 07:26:27 2004 NaTamemeen:= 0308008431 030S04A-421 1T.extc=e nia sen i: C6 Acid PFHA |LL11995588--22,, DDFF==220000 00;330055004A4-442211 Sm Sm (in, (Mn, 235) 2x3) 100q |i1 aznEY8.21 3898~ 1122--MMaarr--22000044 2233::5599::4444~. LLCC//MMSS//MMSS ##66 MRMof 5 Grannols 5. MRM of 5 Channels ESS280 1.5804 313 > 269 et ea 1.58e41 ASN rm mee \ 200 pr) 5 B50 re000er Tin /iIfl~~-~,-2~.0,0' 4.00 6.00 8.00 10.00 ~~~~~ TimeArea scour J 2: C8 Acid PFOA |LL11995588--22,, DDFF==220000 1122--MMaarr--22000044 2233::5599::44 LLCC/lMMSS//MMSS #6 0:305044421 Sm (i, 22) an MRMof 5 Gr5a5n30e50- 030504A-421 Sm (Mn, 2x3) 8.71 24224 MRM of 5 Channels ES- 4131>.3356695 ea 1.35e5Area i | O epr rr Time| 1001%1_ 242~ 0 ~.."--~,, i-...";-C-.... , .... , .... , .... , .... , .... , .... , .... , .... , .... \ Time L 200 abo 500 800 0% 2.00 4.00 6.00 8.00 10.00 3: co sulfonate pris : C4 Sulfonate PFBS [LL11995588--22,, DDFF==220000 (0305044421 Sm (21) MRMof 5LCChiaMnSnIeMlsS.E5- 030504A-421 Sm (Mn, 2x3) | ; % f7e61 0357e609a3) 1001 PA 1122--MMaarr--22000044 2233::5599::44 LC/MS/MS #6 MRM of 5 Channels ES- 7.61 299 > 99 3.79e3 Area NA ~ INN Oe yr Tine ~ ,, ,, , , , , , ., ....., ...., ....... ~ .... ~ .... ~ .... , .... ~ .... Time 200 abo 500 ako 00 | 2.00 4.00 6.00 8.00 10.00 xygen Tasearch, 3036 Research Drive, State Collage, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00115533 a_Motsaoa0s 3M MN01539304 gSQeuuiaatnnyttiiwfeoyy.2Ss1aa5mm5ppll5ee, RRe"eSpphooerrNtto.1030504A, xt.Date:03/05/04, Analyst.x.Risha Pago 42 Page 42 Study No.:LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst=K.Risha NSLLSoaaaatasmmrttppomlldmoee:oodLLiiiifssfitti=e:edd=:2:MM5P\oo:D\nn\aDDtaMNaataat\arraL\\LCL11H5C5oSMMS11wSM33S:s=S3\2622N\a:~Maa44asa66sslslyl22ym0yDm00enc44x\\\PFFllluuucoorrroooccchhheeenmmiiicccaaalllsas..PPFRRROOO\\\SSKaaSsEmpNplDlaPeD\DCsBo\\t00G33r00oS5v00e44AANPCCDGGESAACCS0F3T1M504 MLTLeaoatsbshttocdmom:dooadd:iifeileodd=s Non Nar 15 13:35:33 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2D04 NPDES 031504 Job Code: Printed: ue Mar 16 07:26:27 2008 Printed: Tue Mar 16 07:26:27 2004 NNoaammtee=: 003300550044AA--442211 Text: 44: :Cc6e sSuuliftoonnaattee PpFrHiSs 15L11995588-"22,, DDFF==220000 00:330055004A4-442211 Sm Sm (Mn, (Mn, 253) 2x3) 100~ = 8528.52 969666- 1122--MMaarr--22000044 2233::5599::444~4 LCL/CM/MS/SM/MSS##68I MRM of 5 Channel ES. MRM of 5 Channels ES-I 50980 39449.77>33e8330 rea Area | mm 256 emE ior 2.00 4.00 5:: cC8o sSuullffoonnaattee PpFrOoSs [LL11995588--22,, DDFF==220000 (00p330s0550044A7-442211SSmm (Mn, (Mn, 253) 2x3) 505 ----p850reti00i 0 re Ti 6.00 8.00 10.00 o 121-2M-Mara-r-22L00C00I44M2ZS3Ie:M5vS9#a:46d4 8T8i.280880 M MRMoofR f55LCCChhaIMM annnSna4le/Msls9S>EE5S9S#-9-6 49G9a>de9,9 `ea 6.44e3 Area | 3% RT) "0 I) Too * 1 or 2.00 4.00 Tere 6.00 8.00 10.00 TTiimnee BExeyygoeenn RReesseeaarrcchh,, 23005586 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PA 16801 PA 16801 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00115544 SW_MNo1839305 3M MN01539305 gQSuutaaundnyttiiefNyyo.:SsLaa1mm9pp5ll6ee, RReeSppetoorrttNo.:030504A, EXt.Date:03/05/04, Analyst:k.Risha Page 43 Study No.:LI958, Set No.:030504A, Ext.Date:03/05/04, Analys~:K.Risha SaGLSScaaaahnsmmttoppllameme:ooddLLiiiiffssiitte:e:dd::P:H5MP\oo:\Dnn\DaDatHMataaata\rra\L\LCL31eH55CNSMEHS11NSM33SE:S:6263\23\M:1MaK44aas6ssssslI22Lyy00m00nyx44x\\aPFllxuuoo\rrooFcchhLeenmuiiccoaallzss...oPPPRRRcOOO\\\hKSSSRaeLImRppaDLlEeie\DDCEcBoN\tOa0G330rl05o50a0v44eAKECCDOGESAACCS0F3S1M504 MLoLeabatss.httocdmom:dooedd:iiffiieedd:: Non Nar 15 13123112 2008 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25=12 2004 NPDES 031504 Job Code: PPrriinntteedd:: TTuuee MMaarz 1166 0077::2266::2277 22000084 NNTaaemmeeer:: 030504A-422 030504A-422 Text= 1. ce rcia pen [iLL:1199C55688--A11c,,iDDdFF=P=F11M00A00 001,3030005)0540A4-47224S2Smm2 (Mn, (Mn, 253) 2x3) 1( oo in\ JENN 250 2.00 450 4.00 66.5050 22L::19cC5a88.AA1cc,iiDddF=PpFr1Oo0nA0 i} L1958-1, DF=100 00;3300550044A4-42222 Sm Sm (Mn, (Mn, 253) 2x3) 00 * 88.19 7656765888.0000 _ 1133--MMaarr--22L00C00M44S00I00M::2S211:::24 MRMof MRM of 55LCCCnh/aMann3nSno1e/l3MlssSEE2SS#6--60 31322.>55A882r0e6e44a9 BE | Area i} \rime 1100,0000 Time 13-Mar-2004 00:21:24 1M3R-MMoafr-25LL0CCC0hI/4aMMn0nSS0eI/:lM2Ms1SS:E2S##4.66~ a8a7.s71t1 z MRM of 5 41335030659 Channels ES~ 413 > 3691 rea 2.30e5Area 200 a0 ew 800 1000 Olesya ES Time | .... , .... ,, ~T-4~2-r5-,1,,~,, .... , .... , .... Time 2.00 4.00 6.00 8.00 10.00 33[:.L14~9458Ss1u,ullDffFoonn=aa1tt0ee0 PpFrBoSs _ 13-Mar-2004 00:21:2- L1958-1, DF=100 p10o30y03500540A4-442222 Sm Sm (Mn, (Mn, 253) 2x3) 1M3R-MMaorf-25LL0GCC0hlI4aMnM0nSSe0/lM:M2sSS1E:S#2-64 5 MRM of 5 Chann2e6ls9599 17.6681 7 29889.66A>33r0e9e339a Area *IA e a 200 2l 00 600 80e 0rmre1m 000em, Time 100o/I 2.00 4.00 6.00 1982 8.00 10.00 BExxyyggeenn RReesseeasrzcchh,, 33005588 RReessesaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, P7AA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00115555 SW_MNO1839305 3M MN01539306 QgSuueaeannyttiiNfsYyy.TSSiaaTmmapp5lleee. RR"eeSppaooxrrWtto. 030504n, Ex.Date103/05/04, AnaiyeciK.Risha rage 44 Page 44 SGSSaaatnmmueppdllymeeoNdoLLi.iiz:ssittL:e:Id9:58B,WP:e:\n\SDDeawtatataraN\o\L.L1O:C5U0MM3S1S03ME51S0\a64N3\Aa1M,s4aeeslsylE2ym0x0nte4x.\D\FaFltlueuo=or0ro3oc/ch0he5en/mi0ic4ca,allsAs.n.aPFlRRy0Os\\tSS:aaKma.ppRllieasDDBhB\a\00330050044A CCOG AACCSFSM TMLLGoeoaaactnnsshttthocodmmma:=oooedddriiiftfiiieeeddd::: WMPeo=nn\DDaMMataatarra\LL13E5C5MNS11S3M31S=E32632\N1=Ma34ag36sssl22yy0000no44x\aFl\uoFrolchuamoicralos.PPcRROOh\\NMaaettnhhDDiRB\\CcCootatGGlzroosvvee Mon Mar 15 13:25:12 2004 NNPPDDEESS 003311550044 JPoribntCeoddie: Tue Mer 16 07:26:27 2004 Printed: Tue Mar 16 07:26:27 2004 ---- Name: 030504A-422 T4:extc=o suitonate pens 4L:195C66-1S,ulDfFo=na1t0e0 PFHS L1958-1, DF=100 |00o3300o550044A4-442222 Sm Sm (4,(Mn, 2)2x3) 1 ll _ 13-Mar-2004 00:27: 1M3R-MMoafr-25LL0CCC0h/4IaMnM0nS0eS/lM:I2sS1M#E:5S2#-46 ast8.54 MRM of 5 5 > 80 Channels ES- 2038 9.943) 399 > 80 9.94e3 A~a L| 200 Ea0EE 00 a0 000 Time Time, 5. ca sulfonate 2p.0r0os 4.00 oo 6.00 8.00 10.00 5:C8 Sulfonate PFOS LL11995588--11,, DDFF==110000 lo:s0s04n422 5m (un 2) MRMof 5LCChIaMnnSeIlMsSES#-6, 030504A-422 Sm (Mn, 2x3) =} EsSs 50165e600a04 1 O0! 1133--MMaarr--22000044 0000::2211::224~4 LC/MS/MS #6I MRM of 5 Channels 8.88 499 > 99 1.66e41 329i Areal "| obs | 200 ao 50 abo 000 ' I . , .... , .... , .... , .... , .... r .... , .... , .... Time 4.00 6.00 8.00 10.00 SExxyyggeenn RReesseeaarrcchh,, 33005388 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, P7AA 1166880011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00115566 _Morsaa0r 3M MN01539307 QSqtuuuaadnnyttiiNftoyy. 1ssLaa1mm3pp5ll6ee, RReSepeptoorsteHo.:030504A, Ext.Date:03/05/04, Analystik.Risha PPaaggee 4455 Study No.:L1958, Set No.:030504A, Ext.Date:03/05/04, Analyst:K.Risha LLSSoaaaassmmtttpphllemmee:ooddLLiiiiftssitit:e:edt:s PNPMPIoo=i\n\nDD\MsaNDtaatarraa\\cLL11C5C5eHM\SS11NM33LSS::CE632\22HNM::aaS44ss66MsslSL22l00Er00yn44\xM\mFalseuosr\locyFhemmleicc\aaulFlssio.FPvPRRRroOOOV\r\SMoSoSuaCmmcchpphDleEheeDADBnCBe\o\i0t0d3mc3z00ao55iv0l0e44sAANECCDGOESAACCS0SF3TM1504 TLMLeooatsbshttocdomm=dooeadriicfiieedd:: on Mer 35 13038113 2004 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 3004 NPDES 031504 Job Code: PPrriinntteedd:: Tue war 16 07:26:27 2008 Tue Mar 16 07:26:27 2004 NTsaeamxmetes:: 003300550044A2-442223 Text= I11::95cC8o6-Aa1cciiRdaeppP,eEDnHnAF=100 oo !L1958-1 Rep, DF=100 p0o30504A423 Sm (Mi, 266) ' 030504A-423 Sm (Mn, 2x3) ! 100-~ | wy\ hr 200 00 2.00 4.00 22[: :18cC5o88-rA1eciRiddepPp,FrODonAF=100 L1958-1 Rep, DF=100 030504423 Sm (4n, 23) 0030504A-423 Sm (Mn, 2x3) | . 13-Mar-2004 00:43:01 810 1M3R-MMaorf-25LL0GCo0h/o4Mmn0nsSo0/mlM:4sSS3:50#76 33>269 a0008.19 I ,C ) 313 > 269 20o50a4] 2.69e4 my ! ree 500 500 000 TJme 6.00 8.00 10.00 oo 13-Mar-2004 00:43:07] 1M3R-MMaorf-25LL0CCC0hI/4aMMn0nSS0eI/lM:M4sSS3E#:0#S667] as8a.7ns1 MRM of 5 326310695 Channels ES- / 413 > 369 `roa 2.61e5 Area | 11o/~ 200.-~-. 3: ct sulfonate 2s.0p0as [LL:1198C55488--S11ulRRfeeoppn,,atDDeFF==P11F00B00S 40v0 RY) 4.00 _6.00 00:3300550044A4-42233 5m Sm (Mn(Mn, 253) 2x3) 1(~ % || ot NA ............................ 200 400 500 2.00 4.00 6.00 ~ 800 Tao c 4855I-r 6~ 8.00 10.00 Tim|e "" Time 1133:-MMaarr2-20L00C04I4M000S0:I4:M433S:0:0;7 76 RM MRM of of 55LCCChh/aMannn2Sne9/elMl6ssS5EE6SS#9--6) 270.6139 298897.7`0>0r6ee93a39) Area r reye ve , .... ~ .... ~ .... ,.. ~ Time 800 10% j 8.00 10.00 Exygen Research, 3056 Research Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTYUBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00115577 M_MNO1S39308 3M MN01539308 QgSEuuuaadnnyttiiRfcuyy.sS1aa1mm3pp5ll6ee, RReSepaptoorrttNo.1030504n, Ext.Date:03/05/08, Analyst.Risha Page 46 Page 46 GSSSaaatnmmu%ppdllyemeoNdoLL.iiifss:titL::e1d9:58B,NP\o:Dn\SaDetNtaaat\NraLo\.3LC5:CH0MS3STH03MS5iSS0a64d\WAuMa,eassssslbLExyotnky.xD\aFmtleuc:o0r3o\/c0h5Fe/m0ii4cca,alulsAs.n.oPaPlRRyOOrs\\tSGo:aaKms.pcpRl1ieahsD0hB\a\e00330n05500i44AA CCGG AACCSFSM MLpMLLeeeraattnysshhtttooddmmm::oosddaiiifftiiieeeddn:=s MNPProo:nn\DDaNMataatarra)\L1L1o55CMuS11s3M31S=e32682\K0:M34aa36ssal2200ys00n84x\lFlyuooronche\miFccaalllssu..PPoRROO\\rMMeaotChAcDDBEh\ACCooettGGsrrooivvee Mon Mar 15 13:25:12 2004 IN~FPDDEESS 003311550064 PJroibntCeodd:e: Tua Nar 36 07136137 2004 Printed: Tue Mar 16 07:26:27 2004 NsTaammoee:= 00330055004A4-442233 T4:extc=o su1sonace peu _ L7958-1 Rop, DF=100 4: C6 Sulfonate PFHS L1958-1 Rep, DF=100 I00o3300o550044A7-442233 Sm Sm (4,(Mn, 2)2x3) |% 1133--MMaarr--22L00O00M44S00I00::M44S33::#006~7 a28s.574 MRMof MRM of LC/MS/MS #~ 5 Channa 5. 5 Channels ES5%> Toio80d 399 > 80 ea 1.04e4 1001%~L. ~ Area | o mpo eeDn U ve 0',',, , .... , ......... , .... , .... , .... , .... , .... , .... , .... , .... Time 200 400 50 800 000 2.00 4.00 6.00 8.00 10.00 5. co sulfonate pros ] 5:C8 Sulfonate PFOS !LL11995588--11 RReepp,, DDFF==110000 a(i03005| 044423 5m (4, 2) 28032 MRMof 5 Chan4n9aT9aeE9sSe9a-d) 030504A-423 Sm (Mn, 2x3) 1133--MMaarr--22000044 0000::4433::00'7 LLCC//MMSS//MMSS #6 8.88 MRM of 5 Channels ES499 > 99 1.45e4 Area * | |L ob 200 e a0 r em re 8A 00 000. Tine Time 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, 7A PA 16003 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00115588 _Motsaoa0 3M MN01539309 QQGuuuaaannyttiiWtfoyy. SS1aa1mm3pp5ll0ee.RReeSppaootrrttNo.:030504%, Bet.Date:03/05/04, Analyst:X.Risha PPaaggee 4477 NLSSLSaaaaattsmmnuhtppedollyaemem:ooNddoLLii.iiffs=sittiL:=eeId9d:5:8,MPMPPooro=\n\n\SbDeDsMtaNatatatekreNa\o\\L.L1L1e:6C5Cx0HMS3SS11N0M3M3s5S1S:0EE5264W32\HA1a=Ma,44ras66ssslsyl2LE2m00yxyc00mtn4\4x.xF\D\lPaFultluceucr:or0oro3coc/hch0ehe5mea/imi0cic4aca,lalsls.As.n.aPPPlRRRyOOos\\\tSMS:aSaKmtz.hppRDlliBees\DphCBaao\\t00O33z00o55v00e44AANECCDGOESAACCS0F3T~14504 MLoLeaabtsshttocdomm:dooada:itfeiieeda:: on Mer 35 13135113 2004 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 PJroibntCeoddse: Tue war 16 07:26:27 2004 Printed: Tue Mar 16 07:26:27 2004 Nspaormmeoe:s 0305042424 030504A-424 T1:extc:o Act ven L9IL:5985C486-42"A~,c,iDDdFF==PF11H00A00 [020504S4m(2Mn4, 263) 100,] 0~0g04A-424 Sm (Mn, 2x3) 1 _ annste8.10 8014- 1133--MMaarr--22000044 0011::0044::5511 LLCC//MMSS//MMSS ##66 MRA of 5 Channels ES- MRM of 5 313>269 Channels ES313 > 269 ei 2.7Ar5eea4) 1 ry,\ e 200 3e 00 500 80e 0 Toco me 2.00 pT. J, - DF=100 2: C8 Acid PFOA L~, DF=100 0;3050484S2m4 (Mn, 263) MRMof 5 Channels ES. 030504A-424 Sm (Mn, 2x3) ! 52o0n29 W1325735659 1 O01 || *o 200 Goo eon esoro Bidoee Tiemae 2.00 3: c4 sulfonate bras I (0 [39:6C844-S2u7lDfFo=na1t0e0 PFBS | ~DF=100 0130005,i 04424 Sm (Mn, 263) 2782 MofR 5ChaM nne2l09s55`5Ere9Se)-9a 030504A-424 Sm (Mn, 2x3) 4.00 6.00 _ __~ ~,~,~.,~.~.~...~..~_~ TAimreea 8.00 10.00 1133--MMaarr--22000048 0011::0044::5511 LLCC//MMSS//MMSS ##66 MRM of 5 Channels ES- 8.71 413 > 369 52021 2.73e5Area 4.00 .... , .... , .... , .... , .... , .... , .... " Time 6.00 8.00 10.00 7.63 21721 1133--MMaarr--22L00C00/44M00S11/::0M044S::5511 LC/MS/MS #6 MRM of 5 Channels ES299 > 99 9.93e3 Area [s | 100~ 1 200 prs 500 Meo 2.00 4.00 6.00 OLASB2 ot abo ooo 0 ee snes | - Time 8.00 10.00 Exygen Resessch, 305% Xeseazch Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00115599 _MNO1S39310 3M MN01539310 QQSuueaaannyttiiNffoyy. Ss1aaLmmiDppSllSee. RReeSppuotorrttMo.:030504A, 3xt.Date:03/05/04, AnalystiK.Risha PPaaggee 4489 Study No.:LI958, Set No.:030504A, E~t.Date:03/05/04, Analyst:K.Risha SaGLSScaaaanshmmttppolldmeme:ooddLLiiiiffssiitt:ee:dd::PiMF MP\oo:Dnn\aDtWMa\ aaat\rraL\CL11D H55CSMHS11SM33a =SS:226\23\Na::Ma44sat s66sssslIl22yy0y0ma 00nxx41x\\\FFFlL\ luuuooororoL cocchhheaeanmC iiicccaaalllH sas.PPPRRROE O0\\\KSSeaatmN hmpDplBle\eDS CBBo\\t00G336 r00o500v44eAANECCDGGESAACC0SS3FF1M504 MLSLeaaotssbhttocdmmo:oodded:iiffiieedd:: Hen Nar 35 13:23:13 2008 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 Job Code: Printed: Printed: TTuuee Mwaarx 1166 0077::2266::2277 22000044 L NsTaaommtaes:= 020504A-424 030504A-424 Text: 4: c6 sultonace pes ( |Lt-:9e5C5868=I4=2S'Z,u,lDDfFoFn==a11t00e00 PFHS o00o330055004A4-442244 Sm Sm (Mn, (Mn, 2:3) 2x3) 1 O%01] % 1133--MMaarr--22L00C00/44M00S11/::M0044S::5511 8st MRM MRM of of 55LCCChh/aMannnSn3ee/lM0lss9SEE5SS#-0-6 288 8.54 2284-~ 39119..1A1>44r0ee84a40) Area 250 a0 500 500 1000 ph IE Tne| , ,, .... ~ .... , .... , .... , .... , .... ~ .... , .... , .... Time 2.00 4.00 6.00 8.00 10.00 5: co sulfonate pros _ _ T)_lL~e:,.s9sC5848-4-2S~,u,lDDfFoFn==a11t00e00 PFOS LCIMSIMS #5 0305044424Sm (Mn, 2x3) | p 2s%s "4ag>o9e5da90] 030504A-424 Sm (Mn, 2x3) 1133--MMaarr--22000044 0011::0044::5511 MMRRMM ooff 55LCCChha/MannnSnee/lMlssSE8S#--6| 8.88 499 > 99 1.46e4 Area O;h 250 40 2.00 4.00 (ouU58-2 @W ely 600 e 850 10e 00 TTiimneg 6.00 8.00 10.00 xExyyggeenn RReesseeasrscchh,, 33005588 RReessesaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 616680031 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00116600 SW_MNo1839311 3M MN01539311 JO Quantify Sample Report rer Page 4~ Study No.=L1958, Set No.=030504A, Ext.Date:03/05/04, Analyst:K.Risha tts L SF A ANSE AR 0 $50F Sample List: me, Jey Last modified= EE iat oats foPiaoroshF emihcaClonaGov.e MESES CFIS04 Method: Last modified= wR Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13:22:46 20G4 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove B-PDES 031504 Mon Mar 15 13=25=12 20G4 Printed: Tue Mar 16 07:26=27 2004 Name: 030504A-425 ALI Text: I: C6 Acid L19195588--11,, DDFF==1100 0a3w0el5:1 00425 Sm, 29) 030504A-425 Sm (Mn, 23) oo 1133--MMaarr--22000044 0011::2266::4411 LLCCIIMMSS//MMSS #6 or MAM 6 raHe5. 8.17 MRM of 5 Channels ES313 > 269 La Yo 2.26e5 --Area Oberle To 0 ' "- Time To prs wh Pr) om 2.00 4.00 6.00 8.00 10.00 re on acts vm 2: C8 Acid PFOA LL11995588--11,, DDFF==1I 00 ausossosn25 5m in,26) ory MRM ofSLCormTaemieSm65ls, 030504A-425 Sm (Mn, 2x3) 1133--MMaarr--22000044 0011::2266::4411 LC/MS/MS #6 MRM of 5 Channels ES- 6.73 413 > 369i : sie roex 1.68e6Area |h%i v| 2% pr) ww Th 5 ~-~ .... , .... , .... ~ .... , .... , ....32~ 2.4.3.2.~ , .... , .... , .... TTiimme|e 2.00 4.00 6.00 8.00 10.00 3:C4 Sulfonate PFBS rosa oreto 51958-1, DF=10 0305040425 5m in, 2) 030504A-425 Sm (Mn, 2x3) [7 % ||I orabspob 2.00 4.00 6.00 721 oWaMror23L0CC0h8hi0as1i7mv2Egs--565i:. 377.16538 13-Mar-2004 01:26:41 LC/MS/MS #6 MRM of 5 Channels ES- 9.374] 299 > 99 9.31e4 el FATT in| 8.00 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 GFOENAFNIEDREINTCIOAU-NTSYUBDJIESCTTRITC0TACPORUORTTECNTGI.V2E7OGRunOiEoR26E8N0T3ERED CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00116611 sw_otssss12 3M MN01539312 guanciey sample Repose Quantify Sample Report ream 50 Page 50 Study No.=LI958, Set No.=030504A, Ext.Date:03/05/04, Analys~:K.Risha Sample Lists |31\oRCA\LCHEMECWasaymehusrochPReOVntLeATIaVOtI0a50.4N C3 ACH Sample List= Erna, ar IRI Last modified: a adiefaayot\PlsozoFcRGhWaeChsoat\Ccokndrlovse ODES 031504 Method: Last modified: Ee Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13:22:46 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25:12 2004 Printed: Tue Mar 16 07:26:27 2004 Name= 030504A-425 Text: 4:C6 Sulfonate PFHS [956:, OF=10 L1958-1, DF=10 030504426 5m in,203) 030504A-425 Sm (Mn, 2x3) {|' 1( 851 221813:.5443 Totar2004 612641 13-Mar-2004 01:26:41 LLCC//MMSSlM/SM#S#6 Mi5Crona 5 399> 80 MRM ~ 5 Channels ES39119..00>77ee8550) eaArea 7% pr) I) ~ 2.00 4.00 6.00 o; a0s015nm42i5, 2) : C8 Sulfonate PFOS |LL11995588--11,, DDFF==1100 1 030504A-425 Sm (Mn, 2x3) % Wake 2.00 4.00 6.00 To ww 8.00 10.00 TTiimmee. Rsst8.89 1133-.MMaarr--22000044 0011::2266::4411 LLCC//MMSS//MMSS ##66 W5o rans 5. MRM of 5 Channels ESsl 499 > 99 Hi] 1.34e5 oa |Area ww Tine 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 CORNEFNINDEERNTICAOLUNSTUYBDJIESCTTRITC0TACPOURROTT.ECNTG.IV3E7.O0RV-DTEoR26E0N6T3ERED N CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00116622 awmorssnara 3M MN01539313 QSguutaaunndttyiisfnoyy.1sS5aa1mm5ppll8ee, RReeSppeootrrttNo.1030504A, Ext.Date:03/05/04, Analystik.Risha Pago 51 Page 51 Study No.=LI958, Set No.=030504A, Ext.Date=03/05/04, Analyst=K.Risha SLSaaaammtppmlleeoLiLiissftti::ed: NPPo::n\iD\NaDatarat\aL1\5CLMCS1HM3SS:H36S3\E:M\4aM5sasssl2ly0y0nn4xx\\FPlluuoorroocchheemmiiccaallss..PPRROO\\SSaammpplleeDDBB\\003300S5O0044AA CCGG AACCSSFTM NMLLaeaattsshhttooddmmr=ooddiiffiieedd:: ?MNP1oo:\nn\DDaMNataatarra\\LL11C55CHMES11NM33S=S:S23625\:K:M4a3a6s3sssl22ly0000~y44x\nFlxuo\roFchlemuicoalrs..oPPRRcOOV\hHMeeetthhnDDBBi\\CCcoottaGGrrloovvsee NNPPDDEESS 003311550044 ab codes Last modified= Job Code: Mon Mar 15 13:25:12 2004 SPreianntceeds= ue Mar 16 07:26:27 2008 Tue Mar 16 07:26:27 2004 HoNaazmlee:: 0033005S0044AA--442266 Text= i1[::L19Cc56o8-AA1cciiRdaepPo,FrHDaAF=10 L1958-1 Rep, DF=10 10"3003500540A4-442266 Sm Sm (Mn, (Mn, 263) 2x3) 1 O01 . 1133--MMaarr--22L00O0044M00S11:I:44M88#::S227 ey M MRMoofR f 55LCCChha/M Mannn3Sne1e/lM3lss>SE2ES6S#-9-6 5985.1471 313222.>2e0020ea6559] Area ;o/l^ 200 40 2.00 4.00 22[::L19cC58o8-aA1cciiRddopPp,rFoDOnAF=10 L1958-1 Rep, DF=10 (0;3003500540A4-442266 Sm Sm (Mn, (Mn, 23) 2x3) " 500 l 5985040~ e 1000 Time Time | 6.00 8.00 10.00 _ 1133-.MMaarr--22L00C00I44M00S11I::M44S88::2#2757 25a78r1.7s03 0 MRMof MRM of 55LCCChh/Maan4nSn1en/3Mlse5SZ3lE56S#s-9-6 15706 413 > 369 rea 1.57e6 Area | D- ...... , ....~-, .... , .... , .... , .... , .... , .... , .... , .... , .... , .... { 200 "00 600 800 10.00 1001o/I1 2.00 4.00 6.00 82.9070 100~ 10.00 TTiimmee 3: ca suitonate pris 3: C4 Sulfonate PFBS L1958-1 Rep, DF=10 13-Mar-2004 01:48: L1958-1 Rep, DF=10 1;0%30504426 Sm (Mn, 253) 272833 MofR LCGh/aM MnnSo2/l99sM6>SAE2rS00e-)a9 030504A-426 Sm (Mn, 2x3) 13-Mar-2004 01:48:27 LC/MS/MS #6 7.63 MRM of 5 Channels ES299 > 99 9.62e4 Area Io E et o rArrpprpeeeperee Tote 22.0000 4".0000 56.0000 88.4000 1100.0000 Time EExxyyggeenn RReessseaaxrcchh,, 33005586 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880013 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00116633 SW_MNO1S39314 3M MN01539314 QQSuutaaundntytiiffyyo.rSsLaa1mm3pp5ll3ee, RReeSppetoorrttNo.1030504A, Ext.Date:03/05/01, Analyst:K.Risha PPaaggee 5522 Study No.=LI958, Set No.=030504A, Ext.Date=03/05/04, Analyst=K.Risha LSSaaasmmtppllemeodLLiiifssitte::d: NPo:Pn\:D\MaDatarat\aL1\5CLMCS1MM3SS:S26S2\\:MM4aa6ssssl2l0yy0nn4xx\\FPlluuocrzoocchheemmiiccaallss..PPRROO\\SSaampplleeDDBB\\003300550044AA CCGG AACCSSFTMH MMeLLeaattsshhttooddmm::ooddiiffiieedd:: NMPPoo:inn\\DDMMaaaattrraa\\LL11O55CHMSS11NM33SS::662252\\::MM41aa62ssssLl22yy00n00nx44x\\FFlluucorroocchheenmiiccaallss..PPRROO\VMNeGtthADDBB\\CCoottGGrroovvee NNPPDDEESS 003311550044 3LJ5oab5stcComoddoeeds:ified: Mon Mar 15 13=25:12 2004 PPrriinntteedd:: TTuuee Mwaarx 1166 0077=:2266=:2277 22000044 NNaammae:: 003300550044A3--442266 Text~ 44: :CC65 Ssuullffoonnaattee pPFrHsS L[L11995588--11 RReepp,, DDFF==1100 10%03300550044A4-442266 Sm Sm (Mn, (Mn, 263) 2x3) 00 |% % 20880s.5844 _ 1133--MMaarr--22L00C00I44M00S11I::4M48S8:2:2;7 MRMof MRM of 55LCCChhIaMannnSn3ee/l9Mlss9S>EESS#8--06 39119..0A>0r8e8e8a550) Area Time 0",, ,",, .... , .... , .... , .... , .... , .... , ....20, 9.8.4.~. ~ .... , .... , .... Time 200 400 600 8.00 1000 2.00 4.00 6.00 8.00 10.00 55:: CCo8 sSuullffoonnaattee PpFrOosS , L1958-1 Rop, DF=10 ~ -- 13-Mar-2004 01:48:27. L1958-1 Rep, DF=10 10305044426 Sm (Mn, 263) 1M 3-MaorfR -25LL0CCoh0a/w4MM nsn0Sei1/l:Mn4s8sSE:2S#77-6g1 1001 )30504A-426 Sm (Mn, 2x3) 28s4.e085e80 MRM of 5 Chann44e99l19s9.>2>E3S9909-95) 1 1."2a3ree5a Iw | Area |l 200 400 600 800 1000 TTiimmee 2.00 4.00 6.00 8.00 10.00 ESxxyyggeenn RReesssesazrcchh,, 23005588 RReesseeaarcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACPOPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00116644 IM_MNO1539315 3M MN01539315 QQCuuaaynnttiiTtfyyISsTaammEppllAee ReeRppotosrNtteo30504R, mxt.Date103/08/04, Amaiyesik.niaha PPaaggee 5533 atLSSsaatahEsmumtppdallySmeeoeoNtdoLLii.iif:sstitLti:e:Iad9n=58,mMPPO:inr\\StDDeMantataatearNra\\o\L.LL1TC:5oCuH0MbS3eS1uH0M3S5ss=SE0264t2\hKA:Ma,ae4as6ssssyhilE20xyoa0tnynr4.xD\maFFtileeuu:oo\0rr3oo/sPc0hh5euen/mt0icc4ca,arllsAso.n.PaPPclRRRyOOOhs\\\tSSNe=aaaKmmE.ppnARLlDiaeiBsDD\hBBcCa\\o03at30r05lo5v00es44AMCFCOGDESAACCS0F3O3M504 e= et edited: Method: Last modified= Hon War To Tate oot P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13=25=12 2004 NPDES 031504 PJroibntCeotdie: me dar 26 07s26137 2008 Printed: Tue Mar 16 07:26:27 2004 Nsfaammtea= G30504A-427 030504A-427 T1:extc=e acid pen I: C6 Acid PFHA oo [LL11995588--22,, DDFF==1I 00 ic:scsots27 Sm un 25) csiers MRM of Channaelpsser05ee0- 030504A-427 Sm (Mn, 2x3) 8.17 61 1133--MMaarr--22000044 0022::1100::1199 LLCC//MMSS//MMSS##66 MRM of 5 Channels ES313 > 269 2.24e5 Area | wl LL ,, .... , .... , .... , .... , .... , .... , .... , .... , .... , .... , ....~ Time 35 i 5% So tose J 2.00 4.00 6.00 8.00 10.00 22:: CC88AAcciiddPPFFOOAA LL11995588--22,, DDFF==1100 [;oscsosns.msoznz, 210) 030504A-427 Sm (Mn, 2x3) || 00 _-- _ 1133--MMaarr--22000044 0022::1100:1:1: 9 Lmsims LClMS/MS #6 ors MofR 5GhaM nnpelseES- 8.73 Eh sses 298313~ MRM of 5 Channels ES413 > 369 1.55e6 vee |Area | . Tim|e Lo 22.0000 .., 4.00 .... , .... 4.00 , 6.00 .... , .... 6.00 , 800 .... ~ .... 8.00 , 10.00 .... , .... 10.00 , .... -Time } 2: cx suttonste pres _ : C4 Sulfonate PFBS L1956.2, OF=10 74-Mar-200402:10:19 L1958-2, DF=10 ljo osososns27 5m vn, 230) MofR haM nna ES- 030504A-427 Sm (Mn, 2x3) a. ! sriess fS0ei0a0 1 O01 13-Mar-2004 02:10:19 LLCC//MMSS//MMSS##6~ MRM of 5 Channels ES- 7.63 299 > 99 9.00e4 Area ober rae Tine L2 2.000440 0.000 660.000 808.000 100100 .00 Time = J i Sxsen Rosessch, 3056 Resaasch Drive, State College, A 16802 Exygen Research, 3058 Research Drive, State College, PA 16801 i CCHEOONNNNFEIDFPEIINNTDCIAOELU-NN- TSSTUYUIBBDJJIAEESCCTLTTRTITCOOT AAGPOPURRROOTT.TEECNCTOTIIVV2EE7-OO0RR1-DD1EE0RR.0E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00116655 su umorssssis 3M MN01539316 qSQEuuoaaannyttiiNftayy.(sS5aa1mm3pp8ll0ee, RReeSppaootrrttNo.:010504n, Ext.Date:03/05/04, Analyst:k.Riska PPaaggoe 5544 SaSSaatnmmutppdllyemeoNdoLLi.iif:ssittL::eId95:8,MPPoi:n\\SeDDWtaaattrNeao\\.LL1:sCC0HM3SS10MM351SS0aE643\\AiNM,daaessssllE2xyy0t0mn4.xxD\\aPFtlleuu:oo0rr3oo/cc0hh5ee/nm0ii4cc,aallAssn..aPPlRRyOOs\\t8S:saKsm.ppRllieesDDhEBa\\003300550044AA CCOG ACE ACSFM vMLTLLeeaoaattsssnthtttoecdmmdma:oootddde:iiiftfiiieeeddd::: MMP7oo:\rn\tpDaHMataatasra\\LL1155CsMuS11M33sS:1e23623\\=1Mi34aa36ssssl212y00y0n0x44x\\PFLluuooorocchheenmiiccaallss.PPRROO\\MHeetthADDBB\\CGoOttGEroovvee Mon Mar 15 13:25:12 2004 NNPEDDEESS 003311550044 Job Code: PPrriinntteesds: Tue Nar 16 07:26:27 2004 Tue Mar 16 07:26:27 2004 aTNamomeet:= 003300550044An--442277 Text= 44::CC6o Ssuullftoonnaattee PpFeHsS |LL11995588--22,, DDFF==1100 (0"3003500540A4-442277 Sm Sm (Mn, (Mn, 263) 2x3) 1133--MMaarr--22000044 0022::1100::119 LOIMSIM#S LClMS/MS #6 ass WofR 5ChaI nn3el>9ES8-0 8.54 MRM of 5 Channels ES399 > 80 2100 10805, 1.09e5 Area 1001%! y 200 200 500 5. cosulfonate 2p.0r0os _ 4.00 6.00 [L19582, DF=10 : C8 Sulfonate L1958-2, DF=10 PFOS |ososoasnmsv2n7, 2x0) 0030504A-427 Sm (Mn, 2x3) 1| ol 20a 500 2.00 4.00 6.00 21008~ B00 _8.00 2184.78]885 B008.00 Tin|e| 000 | 10.00 1133--MMaarr--22L00o00m44 s00i22::m11s00::19 LC/MS/MS #6 Rof5M Channoels ES- MRM of 5 Channels ESrea) 49119..22>666e9559) Area ao Time 10.00 Time | I I Bxygen Research, 2058 Roseazeh Drive, State College, A 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 1 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00116666 _MNO1S39317 3M MN01539317 QgeuuaeynnttiiftEyy ESSaaRmmppll.ee RReeSppioorrRtto. 1020504A, Bxt.Dace:02/05/00, Analyt. Risk rage 35 Page 55 pLSESSraatasamumtpdptlylmemeooNdkoLLii.iift=ssittiLe::Ied9a:5:8,HMPPoo:inn\SbDe\awMtatDaatrsNaaa\o\t.LL31=55Ca0MS3S\130M33LB5S::02a6C42d\KAHr:Ma,e4aSse6ssUslhE2LS0xyyo0\tnms4.xtMD\\aFaPtlLpeuu:osc0rz3loo/cyc0hh5mee/mmx0iL4c\o,aaFllAsisn..PuaPPRlRcROyOONrs\S\tSoaM~areKcmCg.phhlRlDeieeRDsDnB\hBAoa\i0t03cG30r0a5a5v0l0e44sANPCCDOGESAACCS0E3FI1M304 TMLSeoaatSnnhttocdmmo:ooedariiftiieedd:: Hon Max 1s 13.3511 2008 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 JPorbintCeodd:e: Tue ar 16 07.26.27 2008 Printed: Tue Mar 16 07:26:27 2004 ---- Name: 030504A-428 To Text: 3. co reid orm a _ I: C6 Acid PFHA 1958.3, DF=1000 73-Mar-2004 02:32:04 L1958-3, DF=1000 1030504426 Sm (Mn, 213) MRM of 5 Channa ES- 030504A-428 Sm (Mn, 2x3) 107,"A1, 2aA16z1 A35r2ie8ea0d 100 13-Mar-2004 02:32:06 LLCC//MMSS//MMSS #6 MRM of 5 Channels ES- 8.27 313 > 269 2761 1.72e4 A ~~~~,~~ Area Aee re me mn fo L | rn repre Tine o" .... , .... ,, ,,, .... , ,,,TT .... ,,,, .... , .... , .... , .... , .... Time 260 bo 5b abo 1050 2.00 4.00 6.00 8.00 10.00 3. ca ncid pron : C8 Acid PFOA L1958.3, DF=1000 3:Mar-2004 02:32:08 L1958-3, DF=1000 0:305047426 Sm (Mn, 2:3) o[r4S MRM of 5 Chan0nelis0E)S- 030504A-428 Sm (Mn, 2x3) 13-Mar-2004 02:32:0t~ LLCCIlMMSS//MMSS##66 8.73 MRM of 5 Channels ES413 > 369 7.96e4 Area |% { eTar w e aE w oh aE boreS e0r5E 0re, e Tine 2.00 4.00 6.00 8.00 10.00 Time 5. ca sulfonase pres i : C4 Sulfonate PFBS [LL11995588-33,, DDFF==11000000 oo V 030504428 Sm (Mn, 203) 030504A-428 Sm (Mn, 2x3) 1 ( ;8 1.01 | TM Vogron 220 322353 39g sra5n710 7007o8t8s asut 92 Z|toot 1izn1203 lw/VV AERCRAANR SA 2.20 3.22 3.53 ;934.69 5.71 6.'1 '1 7.02 7.65 8.44 9.27 002,00 208550 MRM of 5 Channels ES- 1133--MMaarr--22000044 0022::3322::06 LLCC//MMSS//MMSS #6 MRM of 5 Channels ES- 10.02.10.23 299 > 99 1.26e3 WIRE ~11.23 Plr3g%m )psT rr "0 re r5r % mr pko e ooo TiO Time j 2.00 4.00 6.00 8.00 10.00 cExyyagenn RReessesaazrcchh,, 3300568 RReesseeaarrcchh Drive, Drive, State State Collage, College, PA PA 16801 16801 | `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00116677 m_morsaoate 3M MN01539318 PI RET oe Quantify sample Report Study No.=LI958, Set No.:03~504A, Ext.Date:03/05/04, Analyst:K.Risha Page 56 Se IT LL SSE SASSO 5 EEE sa~ple Lis~= Gr. Pry Last modified= Bats a Ei ivrssmmtors. aotaossomeosseres ces sss Method: BEE, AER Last modified: En Job Code= P:\Da~a\LCMSMS6\Massly~x\Fluorochemicals.PRO\SampIeDB\030504A CG ACSFM Mon Mar 15 13=22:46 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25:12 2004 Printed: Tue Mar 16 07=26=27 2004 Na~e: 030504A-428 Text: 4:C6 Sulfonate PFHS LL11995588--33,, DDFF==11000000 oscars sm. 2c 030504A-428 Sm(Mn, 2x3) | fJoJnCasitionsesanmanssuweem s90 1, 20.12 .1.642.57 3.38 4.20 5.07 5.67 6.75 1133--MMaarr--22000044 0022::3322::06 LLCC/lMMSS/lMMSS #6 Lr MRM of 5 Channels ES- mt 10.08 1 399> 80 sis 927 NA nJ\ 740 8.48 9.27 740 zmSEU | 7.69 Oe TR ew ee Time 2.00 4.00 6.00 8.00 10.00 Time 5:C8 Sulfonate PFOS [ILL11995S88--33,, DDFF==11000000 cootsioien285m in. 25 re ~j WghGarns 030504A-428 Sm (Mn, 2x3) EROS, 0.12 | " vm ws sosm elfBs gsoaafminenNT 1.20 | J R_a _se SR 20m m BIN ~ 207 4.15 3.43 5.40 5.82 7.82 7.63 1133--MMaarr--22000044 0022::3322::06 LC/MS/MS #6 MRM of 5 Channels ES- 8.94 10.75 499 > 99 9.71 10 770 ES | -- 22.0000 44.000 0 66..0000 88..0000 1100..0000 | Time I | 1 , Exygen Research, 3058 Research Drive, Stat~ College, PA 16801 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00116688 3M MN01539319 qQSuuaaannyttiiTftyyEsSaaEmmppll.ee RReeMppEoorrNttecoa0s0un, mat.Date103/05/04, Ammiyesix.isha Page 37 Page 57 LSSSataasumm?dppyllmeeoNdLoLii.ifss:ittL:e:Id9:5B8i,MP\o:Dn\SaeDMttaaa~rNa\o\L.LLO=sCU0MM31SE03MO51S\0364M3\Aa1M,4sassls2Ely0xym0tr\4.~FD\iaFutloeur=oo0r3co/hc0eh5en/mi0ic4ca,allsAs.n.aPBlRAyOOs\\tSS=aAKmp.pLRlieesDDhBBa\\0033005S004AA CCGG AACCSFSM MaTS LLeaaattsrshhtttoee dmmm:=oomdddiiiffciiieeeddd:=: vMP2oo:nn\DDaHMataatarra\\L11c5C6MuS11M3s3S:6232\W:Ma84as63sssly229y0m60ne04x\\FFlluuoorroocchheeamiiccaallas.PFRROO\\MNeAtEhADDBB\\CCootrGarroovvee Mon Mar 15 13:25:12 2004 NNEPDDIEESS 003311550044 Job Code= Printed: Tue war 16 07:26:27 2004 Printed: Tue Mar 16 07:26:27 2004 same: 0305048429 Name: 030504A-429 Text: 1iL::19Cc56e8-rA3,eciiDddF=PoF1rH0nA0 L1958-3, DF=100 [|oy py 003300550044AA--442299 SSmm ((MMnn,, 22x33)) ) s8ar.2z7 13:Mar2004 02:53: 13-Mar-2004 02:53:50 LLCC//MMSS//MMSS #6 MMRRMMooff 55 CChhaannnneellss EESS-- 35260 313 > 269 Tord 1.67e4 rm eaAma Or e Te T re ~3272 Tine ' I ' ' ~ ~ I ' ' ' ' I ~ ' ~ ~ I ' ' ~ ' I ~ ' ' ' I ' = ~ ~ I ' ' Time = 240 Woah abo 10% ) 2.00 4.00 6.00 8.00 2: co noid oro 2: C8 Acid PFOA [LL11995588--33,, DDFF==110000 |0003s0s0550044AA--442299 3m Sm vn,(Mn, 23)2x3) !| 1133--MMaarr--22000044 0022::5533::50 LCMSIMS. LC/MS/MS #6 or MRMof 5 Chan4n1e3ls E356-9 8.73 MRM of 5 Channels ES413 > 369 ES Yoreoan, 9.50e4Area 1001 |{ 200 ao 500 800 0% J| .... Ch t--| 163~ .-..-i"~--....-~,, .... ,.-~,..,, rT. , .... , ....-,,,, ~-,,,,, .... , .... Time 2.00 4.00 6.00 8.00 10.00 3: co sulfonate sess 3:C4 Sulfonate PFBS LL11995588--33,, DDFF==110000 ! (1305044.429 Sm (Mn, 253) Rof5CM hannels ES.| 030504A-429 Sm (Mn, 2x3) 1133--MMaarr--22000044 0022::5533::55(0 LLCC//MMSS/IMMSS #6 / | MRM of 5 Channels ES- 8.65 299 > 99 10) A gs CARI Rsf RV BROeS stW eer 0sVAP00 i |"] N 108 ~1.08 218 2.18 ass 3 033 53 amem 4.344.88 Sw5.92 \7J0\120a7e .19 TA8.59. Ay ARSesIsC010.58 vig1gy1.6o71.0s 5~3 AR pee ) CTT a2.0b0 TT T4.0a0b eb6.00 Ta8.0e0 og10.00 TTT Time i Exygen Resaarch, 3058 Research Drive, State Collage, BA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 1 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTTT.EECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00116699 _Mo1sa0320 3M MN01539320 Pt IHL ES Quantify Sample Report op Page 58 Study No.=LI958, Set No.=030504A, Ext.Date:03/05/04, Analyst:K.Risha pp Sample List: pt ME Last modified: ies BE nvemieniceio ecw oteave FFOF% 153904 Method: Last modified: Lr Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13:22:46 2004 p:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25:12 2004 J Printed: Tue Mar 16 07:26:27 2004 = Name: 030504A-429 Text: 4:C6 Sulfonate PFFIS LL11995588--33,, DDFF==110000 csosotn 420 5m (2:0) 030504A-420 Sm (Mn, 2x3) To100 0 12 * 9 20 ap mye -~" 0.74 .. ..... . 3.68 3.99 SRORew 538 559 53~8 5 99 " \ 6.38 rum 7.307.81 1133--MMaarr--22000044 0022::5533::5500] LLCC//MMSS//MMSS##6~ [issih I, MRM of 5 Channels ES- EEE 830929954 /\n _, /\\ 734 ~ 10.02 10.94 399 > 80/ 8 569.299 54 734 OSAMA -~.- 2~9F~~/~/'~ 3% pr I a U a fr, ) 2.00 4.00 6.00 8.00 10.00 , ER ] _ 5:C8 Sulfonate PFOS L956, DF=100 3 Mar 2004 02:53:50 L1958-3, DF=100 cree sn | mE sh 1003008 126 197 300 93% 4 030504A-429 Sm (Mn, 2x3) 10030.08 JAR men se se R AAA J/ 1.24 1.97 ~ 3683"86AA~ 5...... spr 6.75 7.32 13-Mar-2004 02:53:50! ~ LLCC//MMSS//MMSS##66! A848 R sgrE 0s A 0%) 719 ~/ MRM of 5 Channels ES- ! 10 89 11.75.~499 > 99 8.4,8 8.92 9.52 " ""~ /~ J~ /~ ~ /~, ~ \ /~ \ 719I Sy L 2.00 4.00 6.00 8.00 10.00. 25vive essnzise 1% Saseseoh Teive, Seven Selbege: VA UHL Exygen Research, 3058 Research Drive, State College, PA 16801 GFOENAFINDEERNITICAOU-NTSYUBDJIESCTTRITC0TACPORUORTTECNTGI.V2E7OGRunOiEoR26E8N0T3ERED CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00117700 swoss921 3M MN01539321 QSgueuauanlntytiiNfeayy. sSTaa2mm5pp5ll0ee,RReeGpp6oo8rrNtto. 030504A, Bxt.Date:03/05/04, Analyet.E.Risha sPaaggee 3539 Study No.:L1958, Set No.:030504A, Ext.Date:03/05/04, Analyst:K.Risha VLLSSeaaaatssmmht?ppollmameeo:oddLLiiiifssfittl::eeda= PMFNP:Too:\nn\DDDaaMaattaterera\\LLL11Ce55CHMSnS11UsM33S=S1S:262\2(3\W:1Ma44aas65ssssl2l2ys00ym00nxsv4x\\FmFllueuoor\roocFchhelemmiuicceoallazs..oPPPRRRcOOOV\NhNSSAaseCmmHppmDLlDeeiDDCBBcoA\E00aG33i00l5o50v0s4e4AR CCGO AACCSFSM IDES 0315 0 4 oTMLaeantsrhttocmdomo:dodedriitfiieedd:: Non dar 35 33138111 2004 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mun Mar 15 13:25:12 2004 ~PDES 031504 PJroibntCeodd:e= Tue war 36 07:26:27 2004 Printed: Tue Mar 16 07=26:2? 2004 same: 0305048430 Names 030504A-430 T1.extc=e acta pen i[:Lf9C566-A4c,iDdF=PF1H0A00 h1958-4, DF=1000 00"33005500442A.-443300 Sm Sm (Mn, (Mn, 25)2x3) 01100 - 1133--MMaarr--22L00C004I80M033S1:7I185M#7:S333 6815.17995 LC/MS/MS #6 MRM of 5 Channa 5. MRM of 5 Channels ES2S88604 313 > 269 ea 5.86e4 1 Area o 200 +0 5e 00 800 100TT cs heidoer 2.00 4.00 6.00 ~ 8.00 10.00 2[L:L1199C55868--A44c,,iDDdFF=P=F11O00A0000 133M.Maarr--22L00O00M44 S00I33::N11S55::3#3363 (0i0330"0550044A--443300 Sm Sm in, (Mn, 263) 2x3) aa8r.703 MMRRMM ooff 55LCCChh/aMann34nSn1e5e/3lM2lss3>4SEE203SS0#60--596 rea) 2.42e5Area enna | ! 250 4,0 500 B00 100 a oe] ,~,, , ,-,,,-~ .... , .... , .... ~ .... 4~ 3.8.9..8~, .... , .... , .... \Time 2.00 4.00 6.00 8.00 10.00 3. ca suitomace ors 3:C4 Sulfonate PFBS [L7958-4, DF=1000 73-Mar-2004 03:15:3 L1958-4, DF=1000 "0505T042A430 Sm (in, 233) oIo MRM of 5LCChaInMnSeS0l2I5s7Mr#E6oeS53-oa)| 030504A-430 Sm (Mn, 2x3) 13-Mar-2004 03:15:33 LCIMS/MS #6 7.63 MRM of 5 Channels ES299 > 99 3.76e3 Area | o20r 0 ae 50r0r,m ee ab erfor c or TTiimTMSe) 2.00 4.00 6.00 8.00 I0.00 | Sxygen Research, 2058 Reseaceh Drive, State College, PA 16603 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTYUBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993390.00117711 m_morsaaz2 3M MN01539322 QgSuueaansytciiRftLyyTsSaaImmppllEee RReeSppiooerrttcos0s0un, me.Date103/05/04, Anaiyatin.nish sage co Page 60 LESSStaaaatssmmuhttppdellymmeenooNdoLLd.iiiifssi:ittLe::e1ad9:=58B,MHPioo:\nn\SoDDeuawMtattaataaerNao\\.LL1155CO:MM0UES133NN3M03SS5:S\s026Mt4W2\auA=Ma,se4ase6ssslsay2El200xym00ytnck4.x\D\ePaFitl\ueuo:ous0r3oo/coc0hh5eer/mi0ico4ca,alclsAs.hn.PaPPlReRRyOOOs\\ntSSN:aatKmmA.ppDcRllBiee\sDaDChBBoa\Glk0Sd30sr0So50.v044eAANECCDGGESAACCS03FS1M504 [wReoI Method: Last modified: ie P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13=25:12 2004 I~PDES 031504 PJroibsiCeotdse: me ar 36 07126137 2008 Printed: Tue Mar 16 07:26:27 2004 [E-- Name: 030504A-430 - Text~ 4: co suitonate prs 4:C6 Sulfonate PFHS 0r30504430 Sm (in, 239) ILL11995588--44,, DDFF==11000000 030504A-430 Sm (Mn, 2x3) 100t % 1133--MMaarr--220000440033::1155::333 LLCC//MMSS/M/SM#S#6 ase MofR5ChaM nne8l5500.| 8.54 5 CP 4751 MRM of 5 Channels 399 > 80 2.38e4 eaArea 0-~ .... I .... ~ .... I 3h2.00 5. co suttonate sr0s 5:C8 Sulfonate PFOS [LL11995588-44,,DDF=F=11000000 0p3s0504453m0 in. 233) 030504A-430 Sm (Mn, 2x3) * id CL(~T , eT , , 2.00 PP) oh ab Too mre Tie .... I .... I .... I .... ~ .... ~i ,, ,~ .... I .... I .... - Time 4.00 6.00 8.00 10.00 ee, 4.00 TT, a28s.9%0 1133--MMaarr--22000044 0033::1155::3333 LLCC//MMSS//MMSS ##66 MofR5 haM nna E5- MRM of 5 Channels ESone 499 > 99 ne 1.50e4 ee|Area A _ ~ , ,~ ......... ee wooo 6.00 8.00 10.00 Time , | | \ Ergon Research, 3058 Research Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 I `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00117722 aumnorsasszs 3M MN01539323 qCQuuaaTnnttiitSfyy sSEaumspilEee sRReeppoorrRtte. ososotn, Bxt.aces03/a8/06, daeiyecik. isha sage 62 Page 61 oESLSSatarusumnetpdpylseomeoNbdoLLii.iif=ssittLas:eIad9:58,MPHpo:ian\S\nDeDvMtaaaattrrNaao\\L.L13L:5o5CC0MuH3ST1N0iM3oS5S:rsE026s42\HtA:Maaa,4assr6sssslE2L2yx05ya00tnys4.xD\mFaFltl\ueuo=orF0ro3ocl/ch0hau5em/imo0ci4acr,laalo.Asn.FFcaPROlROh\yO\sS\NetSsG=azEmKmpA.pDiLRlRieD\csDEChB\oaa\L00ol33z00ao550v04.e4ANCEC5DGEASACCS0F3SM1504 MSaLeaiatSthtnotdmm=oosdaniifciieoda: Won war 35 Toss as 208 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 PJroibntCeoddse: mua ar 16 0726127 2000 Printed: Tue Mar 16 07:26:27 2004 [Rp Name: 030504A-431 Text= Loo peia pom IXX:CC00C363005A50c04i4-d-22,P, F55H00Anngg//hL SSttaannddaarrdd csosoun-4a1 mn,2:0) 030504A-431 Sm (Mn, 2x3) "1~ sr MRMof 5I CramTealss250-0 8.19 po Lad 1133--MMaarr--22000044 0033::3377::2244. LLCC//MMSS//MMSS ##66 MRM of 5 Channels ES- 31355>..00727e6449 Area Ne 20 a 2.00 4.00 2: coreidorn 2XX:CC0C0383005A50c04i4-d-22,P, F55O00Anngg//LL SSttaannddaarrdd x1030504A431 030504A-431 Sm Sm (bn, 23) (Mn, 23) om 550 fry 6.00 ] ~-~ --~ Time 8.00 10.00 _ i 1133--MMaarr--22000044 0033::3377::2244 Lams6 MofR5LCChaIM MnnSel/Ms S5#6- MRM of 5 Channels !=S- ors Tae 281.67235 4131.>3300659) joArea L aT) ib 1773 5 ow o ee r eer errr Time 0r, ,"-~-'~-,, ,, .. ~.....~ ..,., .~ ..., .... , .. , .... , .... , .... , .... ~ .... -Time 2.00 4.00 6.00 8.00 10.00 31 co suttonate sons 3: C4 Sulfonate PFBS [XXCC003300550044--22,, 5500 nngg//hL SSttaannddaarrdd oCws05; 0~1 Sm in, 20) E7S1 MRMof 5 ChanEelToeHr5ae-y) 030504A-431 Sm (Mn, 2x3) 1133--MMaarr--22000044 0033::3377::2244 LLCC//MMSS//MMSS ##66 MRM of 5 Channels 7.61 299 > 99 1.51e3 aa Area pl Vo Ann -------- 22..0000 44..0000 66..0000 88..0000 1100..0000 Tim--e | axon Resuazch, 3053 Ressazch Drive, State Cotloge, TA 16601 Exygen Research, 3058 Research Drive, State College, PA 16801 | CCROEONNNFNIDFEEIRNTDCIAOELU-NN- TSSTUYUIBBDJJIAEESCCTLTTRITTCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7 -OO0RR1-DD1EE0RR.2E8E9NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00117733 awmorsaoaze 3M MN01539324 QQSuuEaa0nnyttiiffHoyy. SsTaaLmmDppllSee, RReeepptoorrttNo.1030504A, Ext.Date:03/05/08, Analyeti.Riska Praaggee 6622 Study No.:LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst:K.Risha LSSaaasmmtppllmeeodLLiiissftti::ed: MPo:7m\:D\MaDatarat\aL\15CLMCS3M3MS:SN26S3\6:M\4aN6sassls20yl0ny4xn\xF\lFulouroorcohcehemniiccaallsa..PPRROO\\SSaAmpp1laeDDEBN\O03300550044AA CCOG AACCSSFFM HoMLLeatatsnhhteomoddma::oddiiftiteodd:: MMP7oo:1nn\\DDMMaaaatcrraa\\LL115CC5HMSS11N3M3S:S:326652\H::Ma14as36sssl2L20y000ny84x\Fnluxoro\chFemilccaaullss..oPPRRrOO\NoMSeCtAchDDBhB\\CCeooLtGaGrrooivvee NNFPDDEESS 003311550044 ab" coder Last modified: Job Code: Mon Mar 15 13:25:12 2004 PPrriinntteedd:: TTuuee MMaarx 1166 0077::2266::2277 22000048 NNaammae:: 003200550046A--443311 Text: 44X::C0cC3e605sS0uu4li-fo2on,naa5ct0ee nPpgFr/HiLSsStandard XC030504-2, 50 ng/L Standard 10305044431 Sm (Mn, 263) 100) 030504A-431 Sm (Mn, 2x3) 1133--MMaarr--22L00C00I44M00S33I::M337S7::2"244 sss MRM MRM of of 55LCCChh/aMannnSn3o/elM6lssS>EESS5.0-) 2487.596 3919.3>68004 veal 1.36e4 Area 1 r 200 400) r 500 800B100E 0 TTimiTMe| 2.00 4.00 6.00 8.00 10.00 55[: X:CCc083o05sS0uu4il-ft2oo,nnaa5tt0ee nPpgF/rOLsSStandard _ _ 13-Mar-2004 03:37: XC030504-2, 50 ng/L Standard (0:03300550044A4-443311 Sm Sm (Mn, (Mn, 233) 23) 1M3R-MMaorf-25LL0CCC0h/4aMMn0nSSe3/Ml:M3sSS7E:S2.4 850 MRM of 5 49959 Channels 1a8.90 1331~ 49779.22`>1a1r6e9e339al Area ~ 1j0i0:1 { - R _ e A EE ents Wie | 0" .... , ....20, 0.... 2.00 ,,,,~,a,b,o,,, 4.00 ....60, 0.... 6.00 , ....80, 0.... 8.00 T, .o...l,e.... 10.00 , T...T. TTime | i | | | Reygen Research, 2056 Research Drive, State College, 7A 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHGEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00117744 SW_MNo1S39325 3M MN01539325 QqSutuuaadnnyttiitfHyoy.1sSLaaIsmOppBllSee, RRSeeepptoorrttNo.:030504A, Ext.Date:03/05/04, Aualysti.Rlska rege 63 Page 63 Study No.=LI958, Set No.=030504A, Ext.Date:03/05/04, Analyst=K.Risha SSSaaanmmtppllemeodLLiiifssitt:e:d:PrMP\o:Dn\aDtNaaat\raL\C1L5HCSMHS1SM3E:S36\3\M:Ma4as6sasll2yy0n0nx8x\\PFlluuoorroocchheenmiiccaallss..P5RROO\\SSaammpplleeDDBB\\003300550044AA CCOG AACCSSFFM MaMLLeaattsnhhtcoomadma::oadtiftiieedd:: M5wP7oo:nn\\oDMaMaatatarar\\L11o55CMuS11M33d:S123625\N:/Ma41as63sastl22y00y0n04xm\Falu\orFocuheomircaolsc.PFhRROOe\MMneEtDihDRcB\\CaCootltaGzsroov.vae NNPFDDEESS 003311550044 Sab coder Last modified= Job Code= Mon Mar 15 13=25:12 2004 PPrriinntteedd:: mae ax 16 07:26:27 2004 Tue Mar 16 07:26:27 2004 NNTaaammtea!:: 002300550044AA--443322 Text= IL1::19cC5o66.5Aacctiad PoFrHaA L1958-5 p10o03300560044A4-443322 Sm (bn, Sm(Mn, 253) 2x3) | 1133--MMaarr--22L00C0044M00S33M::55S99::12 2 58.15 MRM MRM of of 55LCCChh/aMann3n3Sn1ee/3lM%3lss>2S2EE72S6S0#6-05-69 ea, 3,27e5 Ama | ee Time 0~;",,,, , .... , .... , .... ~ .... , .... ~ .... , .... , .... , .... , .... ~ .... Time 200 ao 500 B00 1000 2.00 4.00 6.00 8.00 10.00 2: co acid pron _ _ -- _ [!2L:1199C55888-A55cid PFOA | 0305044432 Sm (Mn, 263) 71 MRM of 5LCChManS1nIe3lM>sS3E0S9-] 030504A-432 Sm (Mn, 2x3) 1133--MMaarr-.22000044 0033::5599::11;2 LC/MS/MS #6 MRM of 5 Channels ES- 8.71 413 > 369 l1 ||{ sez 71e6a8l]| 1.71eSArea ele ime , %1_ ~250 _ 2.00 L33:1:9C5c4a8_-sS5uuiltfoonnaattee PpFrBeSs ' L1958-5 030504A-432 Sm (Mn. 2x3) | 100 030504A-432 Sm (Mn, 2x3) | %| 260 600 800 1000 4.00 6.00 83.00162~ 10.00 \ Time ~ 72524754 2244 1133--MMaarr--22L00C0044MS003I3::M550S9::112 MMRRMM ooff 5LCCChh/aMannnSn2eIelMl0ssS9EE9SS#>--6 29292>70g89) rea 2.27e4 Area fle A , 225.000 44.0000 56.0000 so 8.00 dw 10.00 | Sxygen Ressaxch, 3056 Reseach Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00117755 SW_MNo1839326 3M MN01539326 I Quantify Sample Report -- Page 64 Study No.:L1958, Set No.:030504A, Ext.Date=03/05/04, Analyst=K.Risha Fp Sample List: np ME pg Last modified: He Lowige4 hiseiyo\Fiverochenioals.PRO\KACSR\GoEGrove NFDRS 071508 Method= EEE tie SRE Last modified: Ee Job Code= P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\SampleDB~030504A CG ACSFM Men Mar 15 13:22=46 2004 P=\Da~a\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Men Mar 15 13:25=12 2004 J Printed= Tue Mar 16 07:26:27 2004 Name= 030504A-432 Text= 4:C6 Sulfonate PFHS [LL11995588.-55 asosnta432 5m i,269) 030504A-432 Sm (Mn, 2x3) | foom m vam ae 1100 0 18 % oIaRn en"eso Traya reJ UsAeMCsRIsoVf CN hEaInne5l 453 4.92 6.50 7.2.1~71,~.8 1133--MMaarr--22000044 0033::5599::11::2 | LLCC/lMMSS//MMSS #6 MRM of 5 Channels ES- 0 8.52 1111.,6622 3 3999>>89800) 9.58 10;43 A 979 ~2~/ . /_ / aT | errrerr----------------------------------r------eeeye--ee Ti Time Lo 202.000 440.000 66.0000 880.000 1100.0000 1 5:C8 Sulfonate PFOS 1LL11995588--55 |1030504S4m4(3Mn2, 2x3) 030504A-432 Sm (Mn, 2x3) 100- = MRMof Channels ES- 889.900. 185 1133--MMaarr--22000044 0033::5599::1122. LLCCI/MMSS//MMSS #6 MRM of 5 Channels ES- 449999 >>9999| 11..5500ee33| A 1001 NNAN AA esp ] tlrere--mm--------r------------------------ TTimie -- _ 22.0000 44..0000 _ 66.0000 80 8.000 10010.000 I | 1 Exygen Research, 3058 Research Drive, State College, PA 16801 GFEOANNEFRIICDOUE-NNTSYUTBDJIIESCATTRITC0TAPCROOUTRETCNTGI.V2E7OGRunOiEoR26E8N0T3ERED 1 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00117766 swotss9327 3M MN01539327 GQSuueaalnnittyiiNefoyy. SSTaaLmmIDpp5lleee, RReeSppuoosrrtNto..030504A, Ext.Date.03/05/04, Analystik.Risha PPaaggee 6655 Study No.:LI958, Se~ No.:030504A, Ext.Date=03/05/04, Analyst:K.Risha NSLSSoaaaatsnmmhttppollameem:ooddLLiiiiffssiitte:e:dd:: PMMPreo:\nn\\DDnaMaattataaxra\\\LL1L1CO55CHHMSS1S1NN33MSE::SES326\23\WH::Maa44ass66ssssll221y00yny00nxm44x\\\FFFlluluoorruooccohhaenrmiicocaalclss..hFPPRRReO0O\\MmSSeaatimmBppDlcleBeDDaBCB\o\l0t033G0s0r55o0.0v44AeANCECDGGESAACCS0F3SM1504 MLLoeaabtsshttocdmom:dooeddsiiffiieedd:: Non Nar 15 13135133 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 I~PDES 031504 Job Code: PSrriinntteedd:: TTuuee MMaarr 1166 0077::2266:,2277 22000044 NpNaame=e:= 003300550046A--443333 Text= I1L::19cC5e66.AA5cciiRddoppPFrHA L1958-5 Rep 00133000055,0044A7-443333 Sim Sm (Mn, (Mn, 265) 2x3) 1i I es88.1t13 1733--MMaarr--22L00O004M4S004I4::M22S00::5#5363 MMRRMM ooff 55LCCChh/aMann3nSne5e/lMlss2SEE6S#S0-6 313 > 269 28A5a5 2.89e5 Area | 2066 400 630 8.00 e 1000 e TTiimnge 2.00 4.00 6.00 8.00 10.00 22L:1o9Cc588e.A5nciRcdaip.PaFOeAon 13-Mar-2004 04:20:53 L1958-5 Rep 00;3300550044A4-44333 Sm Sm (Mn, (Mn, 253) 2x3) 1M3R-MMaorf-25LL0CCC0h//4aMMn0SnS4e//lM:M2sSS0E#:5#56-63 an MRM of 5 13> Channels E3S60-) | a0 8.71 413p>"ra3r6oea9, |% | 2.33e5Area , 200 400 1001%1 _ 2.00 4.00 p------ 3: C4 Sulfonate PFBS [L1958-5 Rep L1958-5 Rep ' [0p3e0u5s0o4aAn-a43s3s SSmm ((MMnn,, 226x33)) 100, \ ' | 650 800 Me 1000 n Time 6.00 84.010 83~ 10.00 "" Time 1133--MMaarr--22L00C00I44 M00S44::M22S00:553 MMRRMM ooff 299>59 LCChIaMnnSe/lMsSES#-6 5 Channels ES- 2705%2 Area 29119..11>660e9449) Area | | A , | obi s 200 r a0 e 550 850 mms1n00a0 eet Tie| Time 2.00 4.00 8.00 8.00 10.00 | Sxygen Research, 3058 Reseacch Drive, State College, 7A 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 ' `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00117777 SW_MNo1839328 3M MN01539328 [OP ------ Quantify Sample Report [iPage 66 Study No. :L1958, Set No.:030504A, Ext.Date:03/05/04, Analyst:K.Risha Semple Lise: | Po\oata\ LOBES Wasstym Porochamical.PRO\SaspleDP\036584R C3 ACS Sample List: r as pg bis HassoFliozocFhEOa\HmBEAiDBc\CaotOlzo. Last modified: re HODRS 033504 Method: EE hastens hon has 15 heb ee Last modified: sae Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13:22:46 2004 p:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25:12 2004 primtaas Tun ar 36 07136030 2000 Printed: Tue Mar 16 07:26:27 2004 mn Name: 030504A-433 Text= 4[L:L11C9965588-S55ulRRfeeopp.nate PFHS cosoan22 5m in, 50) w5Co ran co. 030504A-433 Sm (Mn, 2x3) S poe 2A 2sswan E mem188ooToMgA o L 7\ Slow 100q q.1212 00..6688 1133--MMaarr--22000044 0044::2200::5533] J LLCC//MMSS//MMSS##661 937 A L 8~.56 MRM of 5 Channels ES- .9.6 7 10,77 3919.0>1e830 FS 22.00 5: co susgonate secs 51L:19C958588--S55ulRRfeeoppn.ate PFOS cososn5sm 0z,a 263) 030504A-433 Sm (Mn, 2x3) 1! 1 O01 | FUN, i, 4.00 en , 7% i 2.00 4.00 a, 6.00 AA ah6.00 pm 0% ad ,, .... , .... , .... , .... Time 8.00 10.00 o=m8.88 oko8.00 1133--MMaarr--22000044 0044::2200::5533 LLCC/M/MSS//MMSS##66 WR of 5 Cl 5. MRM of 5 Channels ESow 499 > 99 Tae 1.45e3 Area am ~NALAN io ee Tine 10.00 Time , | 1 berson Ressaceh, S058 Rasessch Drive, State Collage, A 16901 Exygen Research, 3058 Research Drive, State College, PA 16801 CORNEFINDNEENRTICAOLUNSTUYBDJIESCTTRITC0TACPORUORTT.ECNTG.IV3E7.O0RV-DTEoR26E0N6T3ERED N v CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00117788 awmorssnze 3M MN01539329 qQSuueaaannyttiiNtfbyy. SSeaAmmDppEll0ee, RReeSpp4o5orrttNo.:020S04A, Bxt.Date:03/05/04, Analystik.Risha Psaaggee 6671 Study No.=L1958, Set No.=030504A, Ext.Date=03/05/04, Analyst=K.Risha VfLSSaaaatsrmmhtppolrldmee:oedLLiiifssittA =e:d= MP3o:.n\\bDDaMaatatCeraa\\LE L1L5CECMHNS1ES3MNE=SSr S26S2\WH:Maa4ass6ssssllL2y0yym0nmx4x\\\FFilvFuooriroocuchheeonmiizccealolss..c.PPFRRhROOO\\NeSSAaaCmmmRppDilLReeDoDCBBo\Aas00G33lr00o55sv00e44AANPCCDGOESAACCS0F3E1M504 Mf TLeaatrshttoy dmm=omdeiiftiieodd=: wen war 16 1313503 Tos P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 Job Code= PPrriinntteedd:s TTuuee Mwaarr 1166 0077=:2266::2277 22000044 p---- Name= 030504A-434 Tot: Text= 1: co Acid pen : C6 Acid PFHA LL11995588-66 2050 003300550044AA--443344 SSmm ((MMnn,, 22x33)) lOO~ " oo ca8i.a1rr3 z _ 1T3M-Maarr2-20000840044::4422::3311 LCMSIMS MRMof 6LCCh/aMnnSe/lMsSES#-6| MRM of 5 Channels ES- 05260 313 > 269 27005 2.76e5 ea| Area - 246 +o 50 r 5.00 1000 re Time Time 2.00 4.00 6.00 8.00 1000 Bconewmen 2: C8 Acid PFOA [5L11995588--66 003s05y 04434 Sm in, 233) dainon MRM of LCOhaMnTnSeMal2sS2aeE6Sam0-)5 030504A-434 Sm (Mn, 2x3) 1133-.MMaarr--220000440044::4422::3311 LC/MS/MS #6 MRM of 5 Channels ES- 8.71 413 > 369 2.26e5Area | | 1001%~ 40608~ ------ 0- .FT~.~. , .... , . .., .... , .... , .... , .... , .... = .... , .... \Time , 200 a 500 ab 00 2.00 4.00 6.00 8.00 10.00 3: ca sulfonate pms ] _ 3: C4 Sulfonate PFBS T9586 13 Mar2004 04:42:31 51958-6 ' |020s048-434 5m 4, 223) MRM of LCehamnnsemlsSE5- 030504A-434 Sm (Mn, 2x3/ vo fe 1 1470s 50Ba0s5e9d 100 13-Mar-2004 04:42:31 LC/MS/MS #6 MRM of 5 Channels ES- 7.48 299 > 99 f resArea C1 [ % A = ae | 0-t"/"J~"~ ,,, .... , , ,, ~ .... , .... , , , , 260 abo 550 1) foo 2.00 4.00 6.00 , 8.00 i ~ . ,. 10.00 Time | Sxygen Research, 3058 Research Drive, State College, PA 16861 Exygen Research, 3058 Research Drive, State College, PA 16801 ` `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00117799 _Mo1520330 3M MN01539330 quantity sample tapers rose 68 Quantify Sample Report Be ETB. Eh en os0sotn, But. Dates03/08/04, Analyssin.isha Study No.=LI958, Set No.=030504A, Ext.Date=03/05/04, Analyst=K.Risha Page 68 Semple Liski r\Data\LOHUSS assLym\FivorocPRhONeamnpiacDB\aO3l05a04.A CO ACS Sample List: frig Re ng Last modified: eo Leu HageLYof\FiuoroRcO\hNaaLhnOiB Ccotaalro.ve NPDES 031504 Method: Pr NE Cy Last modified= Sano Job Code= P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13:22:46 2004 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25=12 2004 peiteds Tue Mar 36 0726127 2004 Printed: Tue Mar 16 07:26=27 2004 amas S3050AAT Name= 030504A-434 = Text= 40 56 suitonase prve 4:C6 Sulfonate PFHS rose L1958-6 os4 os0in-424 Sm tn, 220) 030504A-434 Sm (Mn, 2x3) 1,~,_, *uu~~ ww samen ! | peA8.52 Sssaram n ssww ew vreze n7ws)~/ U,9.6_0~0E5.5_, 3Mar2004 04:42:31 13-Mar-2004 04:42:31 LLCCI/MMSS//MMSS #6 VRS of 5 ChaTmolss5e- 2003 MRM of 5 Channels ES399 > 80 1.20e3 moezrsozpsst0gssroaner .1,0u.2z~31.0~.;8,~5.,11,.u0o81..1.87 r 35 ie w a5 r a5 oe o ee Tiede 2.00 5: co ouitenste pros oo oo 5:C8 Sulfonate PFOS Lisses Ta-Mar2008 08:4Z:3] L1958-6 s;0s04A-434 5m i, 223 WofR5LCheamI nsneilmss5. 030504A-434 Sm (Mn, 2x3) 02s prTioereesdy 100~ 4.00 6.00 8.00 8.86 142 10.00 13.Mar-2004 04:42:31 LC/MS/MS #6 MRM of 5 Channels ES499 > 99 1.27e3 A~a Oe eee Te || FIN N, AN eA od 200 2.00 a0 4.00 65.0000 88.0000 ML 1100..0000 Time | | i 1 Exraen Rasensch, 3050 Rasenreh Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 CHEONNNEFPIINDCOEU-NNTSTYUIBDJIAESCTLTRITCOTACPORUORTT.ECNTG.IV2E7-O0R1D1E0.R8E8N6T2ERED IN ' CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00118800 sw_wmoresosst 3M MN01539331 qQIuuaaLnnstiitTfyyIsSTaammEppllRee RRTeeppeoorrtto30s0tn, met.Date 03/08/04, Amalyatix.Risha sage 60 Page 69 LSFeSSaat~trsmumhtdppoyllsS mee:oNdLoLii.ifs:srtitL::eId9:58,MPHPoi:on\S\uDeDMtaasatteraNa\o\LL.L1OC:5CUH0MSS3tS1N0U3Mb5S:Se0E264\r2\hAM:M,a4aas6ssssilE2yD~yn0ntnx4e.x\\D\FFaFiitlvueuoo:orr0ro3ooc/cch0hhe5een/nmi0tic4cca,aalllssAs..n.aPPRlRROyOO\s\\StNSu:SasKEmp.AplRDleBieD\sDEChB\oa\Ot03a30r05o50v04e4AANCPCODGEASACCSG3FS1M504 Titeaetten: Method: Last modified: Hon war 15 rises 2008 P:\Da~a\LCMSMS~\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 JPorbintCeodd:e: Tue ar 26 07:26:37 2004 Printed: Tue Mar 16 07:26:27 2004 seme: 0305048435 Name~ 030504A-435 pertText~ 3: ce neia om I: C6 Acid PFHA 1L9159588--77,, DDFF==110000 30508A.4S3m5 n,20) 030504A-435 Sm (Mn, 2x3) ps1( I An 2: ct acid 2ron 22.0000 21:95C68.7A,ciDdF=PF1O0A0 L1958-7, DF=100 a023000500sn 4A0-4435a5S4mm3(Mi5nn,, 233) 2x3) ] % -- 44.0000 66..0000 a8.17 1e46a8o88..0000 aSr8.i7t1s 1133--MMaarr--22000044 0055::0044::11.4 LLCC/lMMSS//MMSS #~ MofRChaMngs ES- MRM of 5 Channels ESro 200 313 > 269 56..5555ee44| reaArea | err---- | Te 1100.0000 Time 1 ) 5-Mar-2004 05:04:7 13-Mar-2004 05:04:14 LCMSIMS LC/MS/MS #6 MRMof annalESs- MRM of 5 Channels EST>aot0e 4"13 > 369 Areal i 2.68e5Area 0 rrp Ar Time | 111/1 , L2020 .00 440.000 860.000 8804.0700 45~ 1100.0000 I 3: ct suitome peas ~ 3:C4 Sulfonate PFBS L1958-7, DF=100 Ta-Mar2004 05:04:1 [I L1958-7, DF=100 1003300550044AA--443355 SSmm ((MMnn,, 22xx33)) , H: N i proeea 11(00, 5 7.59 356- 13-Mar-2LL0CC0//4MM0SS5//M:M0SS4:1#46 MMRRMM ooff 55 CChhaannnneellss EESS-229999 >> 9999 2.32e3 Area | "iPnN AANA Nn Nomen | , I| TTT a a0 eo 800 7000 wy Time 2.00 4.00 6.00 8.00 10.00 I Ervoen Raseacch, 3058 Research Drive, Stace College, FA 16803 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIEAESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00118811 aunorsassaz 3M MN01539332 QqCuuaaannttiiofteyyTSsaaammppell.ee RReeSppEoorrttho. 030504, Bxt.Datas03/05/04, Analysts.Risa Page 70 Page 70 SEYLSSaeaatetmsmuehptpdollynememsooNdtoLLii.iift:ssiitLt:ee:Iad9::58,mMpPeo~Pnn\SDieDMwta\EaatDrrNao\\a.L11Lt:55C0MaH3S11\0M33S5S:Li026aO42\WuA:HMae,4asEe6ssNslE22iS0xy0yE00tn2k4.x\\D\PMaFltlaueuos=ox0rso3oci/ch0yhe5enn/mi0xic4c\a,alFlsAsl.n.uaPPFlRRRcyOOOrs\\\StSoNa=aScKmmL.hHppRDleeiDeDns\DBhCBi\ao\c0t03O3a0F0lo55v00se44.AAKCICODGESAACCSS0FT3M1H504 MTLeaatsrhttoedmma:oocdeiitfiieedd:: Men ar 35 13135112 2004 p:\Data\LCMSMS6\Masslynx\Fluoroch~micals.PRO\MethDB\CotGrove Mon Mar 15 13=25:12 2004 NPDES 031504 PJroibntCeodd:e: Tue Nar 16 07:26:27 2008 Printed: Tue Mar 16 07:26=27 2004 NsTaammoee=: 0205048435 030504A-435 4T0ext6= sulfone pus 4: C6 Su]fonate PFHS LL11995588--77,, DDFF==110000 |0;3o025004sA-04345a5S-mm4v(3Mn5n,, 223) 2x3) 100 % _ ass8.o5s4s _ 1133--MMaarr--22000044 0055::0044::1144 LLCC//MMSS//MMSS ##66 MRMof 5Channa 5. MRM of 5 Channels ES5% > 80 399 > 80 Saved 1.99e4 As Area 200 00, 00 5. co sulfonate pros 5[LL:11C9958588.-S77u,,lDDfFoFn==a11t00e00 PFOS |ososo4snmt25 y030504A-435 Sm (Mn, 200) 2x3) % 500 oo or8e.9sy0 MofR 5GraM mnels 5.| Time 1000 __hl_ 1133--MMaarr--22000044 0055::0044::1144 LLCC//MMSS//MMSS ##66 MRM of 5 Channels ES- 95589 499 > 99 TiedAreal 1.1 le4 Area . | o 200 b 400 e 600 80r 0 01'o'0.o~ TTiimmee | | i ` Exygen Research, 3058 Research Drive, State College, FA 16601 Exygen Research, 3058 Research Drive, State College, PA 16801 1 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00118822 _Motsaeass 3M MN01539333 QSQuueaaannyttiiNftoyy. 1sS3aamm5pp6llee,RReeSppetoorrttNo.:030S04R, Ext.Date:0/05/04, Anslyst:XRisks Page 71 Page ?i VGSLSSaaoaatnstmmutthppdlolymmeaeooNdodLL.iiiiffss:iittL:=ee1dd9::58,PMPMPeoro:n\n\SDDDeuMNtaataattakrNas\o\\L.LL11C5C6C:NMH0S11S33M30M15:SS0s26E432\\HAe:MWa,a4aass6ssssslE2i2y00xyym00tnie44.x\\D\FTaFlltluueuoc:orr0roo3occ/chh0hee5ean/mii0icc4caa,alllssAs..n.aPPFlRRRyOOOs\\\tSSN:aaaKmxt.pphRLDliaDesD\DhBCBa\o\0t03a30s05o50v04e4AAPCCDOG EAACCS03FS1M504 MLoLeaautsshttocdmom=sooeda:iifeiseedd=: won Nak 15 13133013 2008 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 Job Code: PPrriinntteedd:: TTuuee aMaxr 1166 0077::2266::2277 22000084 aTNamomate:s= 0305042436 030504A-436 T1:extc=s neta ven I[:L19C568-A8c,iDdF=PF1H0A00 L1958-8, DF=1000 | 00p3300o550044AA.-443366 Sm (Mn, Sm(Mn, 2)2x3) | 1( I 1133--MMaarr--22L00O0044M00S55:M:22S66::0077] w81.1z77 MRAM MRM of of 55LCCChhlaMann3nSne3/elMl>ssSEE2SS#6.-06 pr 313 > 269 14120- `ea 4.55e4 Area | *h ~ 1 eee A 200 a0 600 500 0 Time j 2 conciamror 2.00 4.00 6.00 _ 8.00 10.00 |2L1:915908588--8A8,c,iDDdFF=P=F11O00A0000 1135-HMarar2-20L00O04M4 S00I5::2M26S6.:0#077 r00o3300550044A8-443356 Sm Sm (Mn, (Mn, 243) 2x3) an MRM MRM of of 55LCCChh/aMann3nSnee/l5MlssSEE3SS0--0 *] 78.2714 26p05e, 413 > 369 2.65e5 Area BE | 1 i | 0 ,.~'---, , 2,q0- 0 ~ 20I 0 50, 0 ~ 00T~ ..... fooee " TTiimmee 3: ct sulfonate ems 2.00 4.00 6.00 8.00 10.00 [I [L1958-8, DF=1000 3: C4 Sulfonate PFBS L1958-8, DF=1000 1733:-MMaarr-22L000C044MS005I5::M226S6::0017 | 10o0330n0550044A4-443366 Sm Sm (Mn, (Mn, 265) 2x3) 775.66s11 MRM MRM of of 55LCCChh/aMannnSn52ee/9lM2l9ss90SE>E5S6S#39-3-699 | wh `rea Area | PINT SAAANA NAN rn SU ....................... ~q ........ , ................ Time Lo TTT eee ae eo Toe ooo 2.00 4.00 6.00 8.00 10.00 0 Bxrgon Research, 3058 Research Drive, State Colloge, PA 16001 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV27EE-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00118833 _MNO1S39334 3M MN01539334 quantity sasple napore sage 2 Quantify Sample Report SERRE ANe onosoun, x oacer03/05/04, Analyecik.nsane Study No.=LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst:K.Risha Page 72 Sample List: Pi\DACA\LCHSO\Manslyme\FlBuRoO\rSoamcphLeeTImNi0c30a50i4s CO ACEP Sample List: frre rrr Last modified: Eo eeR\Lobe agLyam\Luosochontcals. PRO\HSEAOD\CotOrove NODES 033504 Method: rr NE op rhe Last modified: a Job Code= p:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13:22:46 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25:12 2004 printed: Tun war 36 0ni26137 2004 Printed: Tue Mar 16 07=26:27 2004 [Rp---- Name= 030504A-436 wa Text= 4: co surtonae omg 4[LL:11C9956588--S88u,,lDDfFoFn==a11t00e0000PFHS 0;205044436 Sm 4, 223) 030504A-436 Sm (Mn, 2x3) % bsrs8.52 3946 _ 1133--MMaarr--22000044 0055::2266::0077 LCMSIS 76 LC/MS/MS #6 MRA of 5 Chanel 5-| MRM of 5 Channels ESTe 5| 399 > 80 To2od 1.82e4 po|Area 10oiI e 200 r prey erormr r re500d r Tow Tine 2.00 4.00 6.00 8.00 10.00 Time 5: ct sulfonate secs oo 5:C8 Sulfonate PFOS !L511995588--88,, DDFF==11000000 |i0s005048436 Sm 4, 223) sss MRMof 5LheamrsniTevls~w5#:6 |030504A-436 Sm (Mn, 2x3) 1133--MMaarr--22000044 0055::2266::0077 LC/MS/MS #6 2109 00d] 8.88 MRM of 5 Channels ES499 > 99 1.19e4 Area 2 ak ex a 000 re Or .... = .... = .... = .... ~ .... = .... , .... ee = .... I~ ? .............. 2.00 4.00 6.00 8.00 10.00 i Time Time | | | | I Berson Resaaseh, 3050 Raseasch Drive, State College, PA 16003 Exygen Research, 3058 Research Drive, State College, PA 16801 | CONFIDE-NSTUIBJAECLT TO APROTECTIVE ORDER ENTERED IN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN RENNER COUNTY DISTRICT COURT. NO. 27-01-10.28962 HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00118844 awmorsaoass 3M MN01539335 | qQSuuaaannrctiiTefyyISsDaaEmmppSlle.e RsoeppoorrtNteooj0son, mut.pater03/05/04, Analyanixnisha page 72 Page 73 LSESSraataaismumttpdptlylememeoNodoULbi.iiif:sslittLee::Ind9::58B,NPM.Poo\:onn\DSaeDatMvtataaatasrNa\\o\LL.1L1CO6:5CH0MEB31S1UN033MSS5::SN02a6W\42i\WA:nMaa,4eas6sssssllET2yso0xym0ctn\4a.xkPD\laFytu1eou:oro0or3oce/ch0he\5em/mi0Ficc4ca,aailllssAsu..n.PaPRRolROOyO\\sr\SNtSsG:aopEKmAL.pcDeRlRDie\hEsDCh\BoaO\eE03G30nz0So50iv04e4AANCECDoGESAACCS0F3S1M504 MTm Leeatnshttoadmm=ooddiifciieadd:: won War 35 33138015 004 P:\Da~a\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 eJroibntCeoddse: Tue war 16 07.36.27 2004 Printed= Tue Mar 16 07:26:27 2004 sane: 0308048437 Name: 030504A-437 Ti1X::eCx0tcC3:o605An0ce4it-ad3,oPFm1H0aA0 ngiL Standard XC030504-3, 100 ng/L Standard 00233000500540A-4-48374S3Smm7 n(Mn, 239) 2x3) "100~ i saatns8.17 17416-~ Mar2004 05:47:51 13-Mar-2004 05:47:51 LLCC//MMSS//MMSS ##66 MRM of 5 ChanEnSa- MRM of 5 Channels ESro 260 313 > 269 ro| 8.9AA2rreeea4a, DN rrp %@ 250 0 2.00 4.00 Rp2: C8 Acid PFOA XC(0C30300550044--33,, 110000 nngg//hL SSttaannddaarrdd ||0p3or0oss5004As-40347snSmmau(3Mn7n,, 2x0) 23) 1 * m EIR y 1 os 800 00 6.00 8.00 10.00 _ 1133--MMaarr--22000044 0055::4477::5511 LLCC/IMMSS/M/SM#S#(i an MRMof5GhapneneEaSs- 8.73 BH MRM of 5 Channels ES- 4132>.1366e95 rea|Area Brrr------------pIVSSE 0r,,~.-~--.. ,-,, ,,, .... , , ,-~,, .... , .... .... , .... ; -- , .... , .... , ....\Time . 250 Pro) 50 6 fr 2.00 4.00 6.00 8.00 10.00 3. ct sursomate seus 3:C4 Sulfonate PFBS XC030504-31,00 ng/L Standard 73-Mar-2004 05:47:51 ro XC030504-3, 100 nglL Standard 13-Mar-2LL0CC0I/4MM0SS5I/M:M4S7S:5#16 |os0s04n.453m7 vn, 200) MRM of 5 hanna E5- 030504A-437 Sm (Mn, 2x3) , h w Toreesa 100, 71.86,3 MRM of 5 Chann22e9l9s9>>E99S99-9 1.83e3 Area " A | "AA AAA ANA SV , || 4 26ee apkoeepaehe p am eTW er Ti || 2.00 4.00 6.00 8.00 10.00 Time I Sxygen Research, 3058 Research Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 I `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIEAESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00118855 aunorsassss 3M MN01539336 QQBuueaannyttiiftyy sSTaaEmmppsllee, RReeSpphoorrNtte. coj0s04n, 2xt.Date:03/05/04, Analystik.Risha PPaaggee 7744 Study No.:LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst:K.Risha HoLLSStaaaasammhttppolldmeme:ooddLLiiiiffsstiit::eedd=: MPNPooI:Pnn\\DD:NaMataat\arraD\\LL11aC55CHMtSS11Ha3M3S=1S\E23623\\L:1MM44Caa66ssHssll22Sy00y00nnH44xxS\\FP6lluu\ooMrrooacchhseensmiilcccaaaylllsssm..PxPFRRR\OOO\\\lSSMauaemtmophplDlreSe\oDDCBBco\\t00ha33ze00o55av00e4i4ANPCCDGGESAACCS63FS1~504 MLTLeaoatsbshttmocdmoo=dodediriftiieedd:: Non Nar 15 13:33:32 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13=25:12 2004 NPDES 031504 Job Code: PPrriinntteedd=: TTauoe aMaxr 1166 0077::2266::2277 22000044 NNaasmee=: 003300558044A--442377 Text= X44:C:0Cc36e05sS0uu4li-ft3oo,nnaa1tt0ee0 pPnrFgHi/SsL Standard [ XC030504-3, 100 ng/L Standard cao0y50r437 Sm 4, 215) ;030504A-437 Sm (Mn, 2x3) 1133--MMaarr--22L00C00I44M00S55I::M447S7::5#5151 LC/MS/MS #6 MoR f5ChaM mnols 5-| sss8.56 MRM of 5 980 Channels ES399 > 80 io Tedea 2.58e4 Area || I200ree 400 2.00 4.00 5: co sulfonate srs X5XC:C0C0383005S50u04l4-f-3o3,n,a11t00e00 PnnFggO//SLL SSttaannddaarrdd 10;03300550044A4-443377 Sm Sm (Mn, (Mn, 213) 2x3) =1001 22.0000 44.0000 600- 8500062~e Tr e oe Ti ime | 6.00 8.00 10.00 _ _13-Mar-2004 05:47:51 1M3R.MMaorf-25LL0CCC0rI/4MaM0nSS5eI/M:sM4S7SE:S5##-165 2885.9%40 MRM of 5 Channi4e99lT9s92>>7509949 231 ea 1.21 e4 Area 600 e8e00 e doe c) TTimee 6.00 8.00 10.00 i Exygen Research, 2050 Research Drive, State College, PA 16801 E~ygen Research, 3058 Research Drive, State College, PA 16801 t `CHEOGNNONFEINDPIEFNNITCIDAOLEU-N-NSTSUTYUBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRVR-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00118866 SW_MNO1839337 3M MN01539337 QQSuutaaunndttyiiffNyoy.1sS1aa1mm3pp5ll3ee, RReSepaptoorrttNo.:030504A, Eet.Date:03/05/04, AnalystiX.Risha Page 75 Page Study No. :L1958, Set No. :030504A, Ext.Date:03/05/04, Analyst:K.Risha SLSaaasmmtppllmeeodLLiiifsstti::ed::\NPDo:an\tDaNa\atrLa\CLH16CSMSS1S3M\:SN36a2\s:M4sa6lssyl2m0ye0n\4xP\lFulouroorcochheenmiiccaallss.PPRROO\\SSaammpplleeDDBBN\O03300S5O044AA CCGO AACCSSFFM NoaMLLLeaaatbtssshhtttoocadmmmar:oooddddatiieffiiteeoddd:=: MN5Poo:nn\\DoMNaaaattrara\\LL11C56CHMES11HM33S:S=622652\M::Ma14as36sas1l22y00yn00nx44x\\PFlluucorroocchheenmiiccaallas..PPRR0O\\MNeatthHDDBB\\CCuottGGrroovvee Mon Mar 15 13=25=12 2004 NNPPDDEESS 003311550044 Job Code: PPrriinntteedd:: TTuuee MMaaxr 1166 0077::2266::22?7 22000044 NHaammea:: 003300550044AA--443388 Text: [Lp I:1aCs6c 8sA,cis DdF=PF1h H0A0 cidee L1958-9, DF=100 =|os0s04n438 5m (un 20) i 030504A-438 Sm (Mn, 2x3) 100 [uf 28B3.1015559 = 1133--MMaarr--22L00C0044MS006I6::M009S9::34 MRM of 5LCCh/aMnnSe/lMsSES#-6 MRM of 5 7.8004 313 269] Channels ES313 > 269 7.80e4 Area | ohore T EgT an ie [Te2.00 44.0000 66.0000 ~ 88.0000 1100.0000 22:: cCa8 aAcciidd PpFrOoAn _ [LL11995588--99,, DDFF==110000 1133--MMaarr--22L00C004I4 M00S66::M00S99::3344 0003300550044A4-443388 SSmm((MMnn,, 22x33)) art MRM MRM of of 55LCCChh/aMann4nSn1eeI3lMl>ssSEE3SS6#-0-6) | 100 880.7218 413220.>0A1r136ee65a59)l |* Area | 0 .... ,,,, 2~ 40 ,,,, ....40, 0.... , ....66, 0.... , ....8300802B~eL 2.00 4.00 6.00 8.00 33[:L:1C9c45u8.sS9uu,ilDtfFoonn=aa1tt0ee0 pPrFoBsS _ L1958-9, DF=t00 | os p0r03300550044A4-443388 Sm Sm (Mn, (Mn, 263) 2x3) 701 In~ 7.61 I 000 \ TTiimmee | 10.00 Sus 1133--MMaarr--22L00O004M4 S006I6::M00S99::3"344 MMRRMMooff 5LCCChh/aMannnSn2oe/0lMlss9S>EE9SS#-9!-~ 299 > 99 real %] lL PA alee ttiteoe s S nAAN com ANNei rresir | 200 a0 eo 800 ido 2.00 4.00 6.00 8.00 10.00 SExxyyggeenn RReesseeaarrcchh,, 33005580 RReessesaarxcchh DDrriivvee,, SSttaattee CCoolllleeggee,, TPhA 1166080011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00118877 SW_MNO1839338 3M MN01539338 1 | QqS uuaannttiiR ftyy SsaaI mmppllee RReeRppIooNrrtstos0s0an, mee.Dater03/05/04, maiyetixnisha rage 76 Page 76 | aeLSSSaaatnsmmuttppdellyeemeoNdLoLiii.ifss=tittL.e=I,d9=58B,Mt2PiO=o\n\SDoDeAwMtauLaataerrNa\\o\LL.BL1e:5OCE0IMN3S1ST03MOSe5:S\026eW42\WasA:Msa,4aes6ssisyhloE2n0yxo\y0tnnF4.xnlD\uaFttoleus\:oo0rcF3oh/cel0hs5eui/mc0ioa4cl,zasl.oAsn.PPcaPRRlROOhyO\\s\SeWtSae=annKmhp.pia1RlepiecD)sDBGhBa\oa\Or0l3G3Or0sSo5Ov.0Ie4AANPCCDGOESAACCS0F3SM1504 Be MLeaitsthtoedhm:ooaditfciieedn=: tamer To Toto Hon P:\Da~a\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Co~Grove Mon Mar 15 13:25:12 2004 I~PDES 031504 1 pJorbimCoedse= ee sar 16 07136127 2008 Printed= Tue Mar 16 07=26=27 2004 | es sous Name: 030504A-438 4T:extc:e suitonate prs 4:C6 Sulfonate PFHS 1 [LL11995588--99,, DDFF==110000 as0s08a.428 Sm in, 23) MEM of 6a Chomnon l 5- 030504A-438 Sm (Mn, 23) fe s ess | 100-~ ; = Loe 8.52 1082 1133--MMaarr--22000044 0066::0099::34 LC/MS/MS #6 MRM of 5 Channels ES- 399 > 80 55.6611ee33 Area | | aaa | 0 , ~ , , , .... , .... , .... , .... , .... , .... , .... , .... , , , ,~Time | 5% aio 5% abo oa 2.00 4.00 6.00 8.00 10.00 5. co surtomsee pros - i 5:C8 Sulfonate PFOS 1958-9, DF=100 Mar2004 06:09:34 L1958-9, DF=100 3:0504438 Sm (vn, 20) ase MRM of 5 Chamm5el059. | 030504A-438 Sm (Mn, 2x3) | oa) * 13-Mar-2004 06:09:34 LLCC/IMMSS//MMSS ##66 or Sted 8.88 MRM of 5 Channels ES499 > 99 5,34e3 | Area n | | e 2 ae k eh ako ow Time 2.00 4.00 6.00 8.00 10.00 Time Ergon Research, 3058 Research Drive, State College. EA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 CCHEOONNNNFEIDFPEIINNTDCIAOELU-NN- TSSTUYUIBBDJJIAEESCCTLTTRTITCOOT AAGPOPURRROOTT.TEECNCTOTIIVV2EE7-OO0RR1-DD1EE0RR.0E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00118888 Sw umotsssss 3M MN01539339 qQuuaannttiitfyy sSaammppllee RReeppoosret rage 77 Page 77 Study No.:LI958, Set No.=030504A, Ext.Date=03/05/04, Analyst:K.Risha Surple Lists 3:\ata\LGHNSSWassLym Fiuorochemioala. PRO\SespleDE\O30S04A CG ACEP Sample List: Last modified: tons Rese wins has yma Fivorochentcals. PRG\NeCADS\Gotreve NFDES 651504 Method: Ratio mon bar To Toes LaSt modified= = Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13=22=46 2004 P:\Data\LCMSMS6\Massly13x\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25:12 2004 Printed: Tue Mar 16 07=26=27 2004 - ~ame= 030504A-439 Text: [ciLt:~a'8C76Ta~:AJ5c-RiRedepp,P,FDDHAFF==110000 scooso. Sm 4, 250) MRMof 5 Cranngs ES. 030504A-430 Sm (Mn, 2x3) ars assNeesa 1 Io/~ ~ A ~ eee | A 3% ib p15) ato Wo 2.00 2conciarin _ oo : C8 Acid PFOA DF=100 15-Mar-2004 06:31:21 J~'~87"4~1~, DF=100 |oacsossnmsuans, 220) VoR f3 GrM ama' 5- 030504A-439 Sm (Mn, 2x3) i sss rose 1 7 s.15 2211890022~ 1133--MMaarr--22000044 0066::3311::2211 LLCC/lMMSS//MMSS #6 MRM of 5 Channels ES- 313 > 269 66..6633e44) Area ---------- I rrr Time 4.00 6.00 8.00 10.00 8.69 40821 13-Mar-2004 06:31:21 LLCCl/MMSS/M/SM#S#6 MRM of 5 Channels ES413 > 369 2.11e5| Area) 2.11e5Area | * rs Tava|| \ ,,,. 200 ~ .... 2.00 , 400 .... , .... 4.00 , soo | soo | wooo 7 .... ~ .... , .... 4, 0.5..2.~I .... , .... ~ ....~ Time 6.00 8.00 10.00 3:C4 Sulfonate PFBS 0A.1874-9-Rep, DF=100 ' 30504438 5m in223) Rof M Chamois 5- 030504A-43 Sm (Mn, 2x3) | oe i7e38 ECaires 1( | |, | obSor o2n80 A hs sooA n abo Te | 2.00 4.00 7.59 6.00 8,00 1133--MMaarr--22000044 0066::3311::2211) LLCCI/MMSS//MMSS #6 MRM of 5 Channels ES299 > 99 6A,r3A1ereeaa3, 10.00 Time OLA Rep. Ehslulot I Exygen Research, 3058 Research Drive, State College, PA 16801 ] CCHEOONNNNFEIDFPEIINNTDCIAOELU-N-NSTSTUYUIBBDJJIAEESCCTLTTRTITCOOT AAGPOPURRROOTT.TEECNCTOTIIVV2EE7-OO0RR1-DD1EE0RR.0E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 su umorssssio 3M MN01539340 11993399..00118899 QqSuutaaunndctyiiefHoyy. sS1aa2mm5pp5ll9ee, RseSoupproorrFtto. :030504A, Bet.Date:03/05/04, AnalystiK.Risha Page 78 SLSSaaatsmmutppdllymeeoNdoLLii.icss:ittLe=:Id9:|58P,NP:o=\n\SDDeaWattateraN\\oLL.15C:CM0H3SS20M3N5S:S062S4\3\AM:M,a4as6sssl2Ely0xyn0tmx8.\\DFFa1ltuueoo:rr0oo3cc/hh0ee5nm/ii0cc4ea,llasA..naP5lRRyOOs\\tSS:aaKmm.ppRllieeDsDBhI\aN0O3300550044AA CO CG ACSTH ACSFM HMLLSTeeaaoattssbrhhtttoocadmmmor=aodoedddriiitffiiieeeddd:== MPNPoo=lnn\aDtMWaaatara)\L1L165CEMS11N3M3S=S.2632\5k=Ma74aa16sssil22yy00o06nx44x\\FFiluuoosroocchheenmiiccaallss.PPRROON\SMCetHhDDDB\\CCoottdGzroovvee Mort Mar 15 13:25=12 2004 NNPPDDEESS 003311550044 Job Code= PPrriinntteedd=s Tue Mar 16 07126127 2004 sNaamnees: 003200550040A8-442399 Text~ 4: cs surconsce pes D [4~ L:sC76 4S0uRl, afpon,DatFDe=F=1P1F00H00S 00o33005y500444A.-443399 Sm Sm (in, (Mn, 235) 23) |1 as11811.500244 1133--MMaarr--22000044 0066::3311::22111 LLCC//MMSS//MMSS ##66/ RA of 5 Chann3el9s85E58-0 5.7803 MRM of 5 Channels ES- / 399 > 80 5.78e3 eaArea |L oOreeOT TT T ase 2.00 4.00 55: :Cc8o sSuullffoonnaattee PpFroOsS @ L&4,-8!~2Z449.~--RReepp,, DDFF==110000 3050443Sm9 (n 233) 030504A-439 Sm (Mn, 2x3) pos7] 1007 J | wl . | TE 200 400 2.00 4.00 0 111584 fep @Bfesfidoy ' ee6.00 IXa ) 6.00 S mpMoosE Time 8.00 10,00 a 131-3M-Mara-r-22L00o00m44S00I66M::3S311:::2211 r5a8.87 M MRMoofR f 55LCCChha/MaM nnnSn0ee/lMl5ssS5EESS#9--6 49592>50939 5.2"AA5rveee3aal soo ow 8.00 10.00 Tie Time | | | | Exygen Resescch, 2058 Reseaxch Drive, State College, BA 16601 Exygen Research, 3058 Research Drive, State College, PA 15801 | `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT,IIVV2EE7:OOCRRV-DD1EE0RR-2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00119900 SW_MNo1859341 3M MN01539341 guunciey ape neport sage 70 Quantify sample Report SEAR Neon0s0an, x.oases03/08/04, Amaiyetik.Risha Study No.=LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst:K.Risha Page 79 Sample List: Pr\Daca\LCHIMSE\Manslyme\FiBRuO\oSramopclahTaI\n0i30e5a04l Co Aco Sample List: ro Rr Last modified: og bist assyag\iozoshPReO\nWAiEAcDIaGoltdsro.vs NFDES 031308 Method: Fro He Last modified= Lone mous Job Code: P=\Data\LCMSMS6\Mass1ynx\Fluorochemicals.PRO\SampleDB\O30504A CG ACSFM Mon Mar 15 13:22:46 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25=12 2004 peiness nun sar 36 20ar7 2004 Printed= Tue Mar 16 07=26=27 2004 seme cos Name: 030504A-440 Text~ 11_co reid ora SE i: C6 Acid PFHA Li938-10, BF=100 TWar-2008 08.5314 L1958-10, DF=100 caoson440 5m (bn, 20) MRMof 5 Carmel 5: 030504A-440 Sm (Mn, 2x3) 01 us reeds 1 100~ 2080.1357 13-Mar-2004 06:53:14 LLCC//MMSS//MMSS##66 MRM of 5 Channels 313b6>.a4t21e6ed94 Area || \re207 eprrr)r -- 7S A : 7 Toso > tine 2.00 pean 2: C8 Acid PFOA [L1838-10, DF=100 73Mar2008 067831 L1958-10, DF=100 |ocus0sa440 Sm i, 223) MRMof 3LGhaCrnelSs 5. 030504A-440 Sm (Mn, 2x3) fra us pt~e 1%0-01 4.00 6.00 8.00 8.69 44693 10.00 Time 13-Mar-2004 06:53:14 LC/MS/MS #6 MRM of 5 Channels ES413 > 369 22..44006e55, Area | o rrr Te | /0~,,,,~ . , , .'~. ~ 44693~ ~ Time ' ' ' t ' ' '~l .... I .... I ' ' ' i .... ~-' ' ' ' I ' ' ' ' I .... I .... | 20 prey a5 a0 ooo 2.00 4.00 6.00 8.00 10.00 7258 Exttomete sre 3:C4 Sulfonate PFBS f|LL11995588--1100,, DDFF==110000 Josososn40.5m tn, 230 MRI of 5 Camels5- 030504A-440 Sm (Mn, 2x3) pe 71 oie || 100-~ 7.57 11008811- 1133--MMaarr--22000044 0066::5533::11:~1 LLCC//MMSS/M/SM#S#6 MRM of 5 Channels ES- Arco, 299 > 99 55..0066ee33| Area Pt A | | Me e ee ee Pr, | Tn | ............................ i .... ~ .... ~ .... ~ ........ Time , 260 ek ase io 2.00 4.00 6.00 8.00 10.00 | Bergen Research, 3088 Rosasreh Drive, State Collage, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 CHEONNNEFPIINDCOEU-NNTSTYUIBDJIAESCTLTRITCOTACPOURROTT.ECNTG.IV2E7-O0R1D1E0.R8E8N6T2ERED IN I CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00119911 su_wmoresose2 3M MN01539342 qQSuueaaannyttiiNtfoyy. Ss1aaLmmI3ppSllSee. RReeSppueoorrttMo.:030504A, Ext.Date:03/05/04, Analystik.Risha sPaaggee 8800 LSSSaeatsmmutppdllymeeoNdoLLi.ii=ssftLti::Ie9d:58,HPoP:nr\S\DeDNtaaattrNaaO\\.L1L:5CC0MH31SS03MM5:SS036E43\\A1MM,4aa6ssssl2lEy0xym0tnx4.x\D\FaFltlueuo:or0ro3oc/ch0he5em/mi0ic4ac,lasl.Asn.aPFlRRyO0s\\tSG:aAKmT.ppRLliaesDDhBBa\\003300550044AA CG CG ACETH ACSIV~ NLMLaeaactsshhttooddmm:=ooddiiffiieedd:: 5HMPoo:nn\\DDNMaaaattarra\\LL31e55CHMES11N3M3S:S:632652\::MA14aa36sss1l22y0y0a00~x84x\\FFluLoruocohemricoalcs.PPhRROeO\MSneEtHhiDDBBc\\CCaoottGlrroosvvee KFDES NPDES 031504 031504 SLaaSbtcmodoedsified: Mon Mar 15 13:25:12 2004 Job Code: pPrriinntteedd:: nue Max 16 07:26:27 2004 Tue Mar 16 07:26:27 2004 Nasa: 030504A-440 Name: 030504A-440 Text: 441::9C5c86s-1sS0uul,ltfDoonnFaa=tt1ee00PpFrHsS L1958-10, DF=100 10:3003500540A4-444400 Sm Sm (Mn, (Mn, 268) 2x3) |% 849 1M3R-MMaorf-520C0r4a0n%6e:9s5>3E:8S1-04 8.49 `rea 1046" 13-Mar-2004 06:53:14~ LLCC//MMSS//MMSS ##666 MRM of 5 Channels ES-, 39550..44>88e80033: Area | 200 60 505 500 i000 2.00 5: co sulfonate pros _ _-- : C8 Sulfonate PFOS 1L9159858--1100,, DDFF==110000 a 4.00 0130005,h047440 Sm (Mn, 253) aTsiso MRM of 5 Chann0el95s15E65S-30 030504A-440 Sm (Mn, 2x3) i oestati TY Time 6.00 8.00 10.00 8.86 1100-~ 1133--MMaarr--22000044 0066::5533::1144 LLCCI/MMS/SM/SM##6S6 MRM of 5 Channels ES499 > 99 6.16e3 '1 Area 1001 L aeTRT T Tr ab TaE boo ~ 1000 TT Time 01,,, ,~ Area , .... , .... , .... , .... , .... , .... , .... , .... , .... ~ .... , .... Time 2.00 4.00 6.00 8.00 10.00 | Exygen Research, 1058 Research Drive, State College, PA 16301 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00119922 SW_MNO1839343 3M MN01539343 QqSuueaannytsiiT ftyy sSaaE mmpplleeSnReeppoorrNttecosus0an, mx.Date103/08/04, Anaiystin.nish rPaaggee 0811 NLCSSSeaaeattsnmmuhttppdollysmmee:ooNddoLnii.iiff:ssiiLttee::Idd9::58p,WMP:oo:\nn\SooDeaaWMtatatatasrNa\o\U.L11C5:5C.HM0MSE3S13H0NM33S5:S1S0263\423\WA:1Maa,44ass66ssssl2yEl2y00xyom00tnec44.x\\D\FPaFlltluueuoo:ozr0roo3occ/chh0hee5enr/mti0icc4ca,aaillssAs..n.aPPPlRRRyOOOsV\\tNSS:AaAKEmE.ApPRDlLiHeAs\DDhCBBao\Gk03G30r0So50v04e4RANECCDOGESAACGS03FS1M504 r SMLaeatnshttoadmm:ooadtiefiiaedd:: hon war 1 3313511 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 JBorbimtCeotdse: Tue dar 36 07:26127 2004 Printed: Tue Mar 16 07:26:27 2004 Ns-aammtea:: 0308008442 030504A-441 TiLL:e7ox9ctC5o~689An,cetiDadFmP=F1nH0A h1958-9, DF=I 0 0:30804441 030504A-441 $m Sm vn,(Mn, 230) 2x3) 100 % 1%-1, . 013 _ 1M 3-MaorfR -20C0re8M m0neo7lss1520500.| 162855 8.13 ea|| 192855~ 13-Mar-2004 07:15:00 LLCC//MMSS//MMSS #6 MRM of 5 Channels ES- 65205 313 > 269 6.52e5 Area | ak 2.00 4.00 2conciasen 2: 08 Acid PFOA |LL11995588--99,, DDFF==1100 (0:33005500445A.-444411 Sm Sm in,233) (Mn, 2x3) eK ao Toe 6.00 8.00 10.00 TTiimme|e a188e5.679s 1133-.MMaarr--22000044 0077::1155::0000 LLCC/IMMSS//MMSS##66 MRM of 5 ChannESa- MRM of 5 Channels ESpeed 413 > 369 etey 9.84e5 aArea i : Tine ~' , , , , ' , ,~7-.... , .... , .... , .... , .... , .... , .... , .... , .... , .... Time . 200 0 5% 10% 2.00 4.00 6.00 8.00 10.00 3: co suitomte pens 3:C4 Sulfonate PFBS [LL11995588--99,, DDFF==1100 o0;3s005s0044Aa-444411 5m Sm vn,(Mn, 29)2x3) | I O0I 1133--MMaarr--22000044 0077::1155::00(~ LLCCIIMMSS/MISM#S#6 70 MofR5 haM n2n6o'>E9S-9 7.56 MRMof5 Channels ES299 > 99 380 510d) 5.11e4 ovaA~a H 2% abo a0 sy 80 00 | ober rrp Tine | iI-.... I ....2.0I 0.... I ....4.0~ 0.... I ....6.0, 0.... , ....8.0I 0.... , ....10., 0.0... , .... Time | Sxvoen Research, 2054 Rassacch Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00119933 auotsassss 3M MN01539344 qSQtuuiaadnnyttiiNffoyy.1sS1aa1mm3pp5ll6ee, RReeSppeotorrtNt.o.:030SO4A, E<t.Date:03/05/04, Analystik.Riska age 02 Page 82 Study No.=LI958, Set No.=030504A, Ext.Date=03/05/04, Analyst=K.Risha MLSLSeaaaatssmmhttppolldmeem:ooddLLiiiiffssitti:=eedd=: 7MMPPioo=i\nn\\DDDMaNaataattraraa\\\LL11LC5C5CHMHIS11SN3M3HS:S:S6226E22\\\::MM44aKa66sssasl22l00ysy00nu44xxs\\FP1lluuyoorrnoocchxheem\niicccFaaallllsss...uPP?RRRoOOO\\\rSNSaSamoErpHplDlceBeD\DhCBEo\\et00d33nr00o55iv00e44AANCPCOGDESAACCS0F3SM1504 MJLLeaaatsSbhttocdmmo=oodded:titfiieedd:: Hon Nar 15 13123112 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 Job Code: Printed: Tue Maz 16 07:26:27 2004 Printed= Tue Mar 16 07:26:27 2004 NNaammee=: 003300550044rA--444412 Text= 441: 1:9CC56o8.9sS,uullDffFoonn=aa1tt0ee pPeFHwSs L1958-9, DF=10 00%3300550044AA--444411 SSmm ((MVnn,, 226x33)) *1 (o/l 1133--MMaarr--22L00C00I44M0S07I7:M:11S55#::00600 852 MMRRMM ooff 5LCCChh/aMannnSn0ee/lMlss9SEESSa>#-0-6)| Ex8.52 39496`6>r0e84a0]l 4.66e4Area 0] .... ~ 250 .... , .... , 2 .... 5,0 .... , 600 .... , .... , 800 ....9,16..1.~. , 1000 .... , .... ,, ~--. Time: Time | 2.00 4.00 6.00 8.00 10.00 5: co sulfonate pros i} _ __ 5L1:11C9955888-9S9,u,lDDfFoFn==a11t00e PFOS 1133--MMaarr--22L00C00I44M00S77I::1M15S5:0:010 101300030-500540A4-444411 SSmm ((MMnn,, 213) 2x3) csCaannn( M MRMoofR f 55LCCChhIaM MannnSne44e/l99Mlbs9s9aS>>EEsSeS#99-d-96 | 00 8371 ea 4.35e4 * Area , 200 400 600 800 A 10.00 Time 2.00 4.00 .... , .... , .... , .... , .... i...., .... Time 6.00 8.00 10.00 i EExxyyggeenn RReesssesazrcchh,, 33005568 RReessseaaxrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSTUUYBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00119944 IM_MNO1539345 3M MN01539345 QQSuuoaaonnlttiitf0yy.iSs5aamm5pp0llee, RReeSppRoorrNtto. 1030504, Ext.Dates03/05/04, Analystik.Riska Praaggee 383 Study No.=LI958, Set No.=030504A, Ext.Date=03/05/04, Analyst:K.Risha NLSLSaaaaatsmsmhtptpollmdmeeo:oddLLiiiffssiitte:e:dd:: MMP7Poo:inn\\DDDaNMaataattarraa\\\LLL11oC55CuHMSS1S1nH3M3sS::S2S262\2\K::MMa44aag66sssssll22Lyy0y0m00nxx44x\\\FPFlluuLoorruoocchoheenmziiccaoallscs...PPPhRRROOOe\\\MSSSanaEsmRppLDllBeec\TDCEBo\a\E00G33lE00o55vs00e44ANCFCDGGESAACCSS0TF31HM504 GMLLeoaatSbshttocdomm:dooeddriiftiioedd:: Non Nar 15 13:25:12 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethD~\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 Job Code: pPrriinntteedd:: nTuuee MMaarx 1166 0077:=2266::2277 22000044 NsTaaemmxate:s: 003200550044AA--444422 T3.extc:e acia pen IL1:1995C5868--A99ciRRdeeppP,,FHDDAFF==1100 100303500540A4-444422 SSmm (Mn, (Mn, 268) 2x3) 11 |= } 1866.1r1a33 2 1133--MMaarr--22L00C00I44M00S77/::M3366S::5#5115 MMRRMM ooff 55LCCChh/aMann3nSne1e/lM3lss5S2EES6S#-0-6 31366>.00A772v6e6e595n Area 250 50 500 800 i000 Time Time 2.00 4.00 6.00 8.00 10.00 2[:L: 19cC5o88.AA9cciiRddopPp,FrODoAnF=10 _ _ 13-Mar-2004 07:36:51 L1958-9 Rep, DF=10 0003300,550044A7-444422 Sm Sm (Mn, (Mn, 2:3) 2x3) 1M3R.MAaorf-25LL0CCC0rI/4MaM0nSS7eI/:Ms3M6SSE:5S##-165]i ses MRM of 5 13>360 C~annels ES- i 1683.65985 4139>6730659 1 ea "1001 183585~ 9.6Areaile5 ory _-- , 0~.,.., 200 ....'~-T- .... 2.00 , ato .... ~ .... 4.00 , 600 .... , .... 6.00 , 550 .... , .... 8.00 ~ i000 .... , .... 10.00 ~ .... -Time 33[: L:1C9c45o6.Ss9uullRftaoapnn,aattDeeF=pD1rF0BiSs 13-Mar-2004 07:36:51 i|Lo1s9o5s8o-s9nsRae2ps, mDFa=nI0200) 1M3R-MMaorf-25LL0CCO0hI4IaMnM0nS7Se/l:MI3sS6M#E:SS5#-16 {0030504A-442 Sm (Mn, 2x3) 1772.5452860 MRM of 5 Chann22e904l9s97>>E600S994-9) eal 4.78e4 |% Area ! | o20h 0 abom 600 2.00 4.00 6.00 "a0E0 E -- 1000 T=ime, 8.00 10.00 i Exygen Research, 3050 Research Drive, State College, 7A 16301 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00119955 SW_MNO1839346 3M MN01539346 gSQtuuuaadnnyttnifoeyy. Ss1a5~m1p5pl5le6e, RReeSppeootrrttNo.:030504A, Ext.Date:03/05/04, Analyst:K.Risha PPaaggee 8844 Study No.=LI958, Set No.=030504A, Ext.Date:03/05/04, Analyst:K.Risha NLSLSeaaaatasmmhttppolldmmee:ooddLLiiiiffsstiit:=eedd::3:MN7P\oo::Dnn\\aDDtNMaaaaact\teraL\\cL1H1H55CSMS1SS1S33M:\:S226M6 22\aa::Ms44ass66slasy2l2n0Dylx00n\44xyF\lFuilouroxorco\hcheenFmiicclcaaalllusss...oPPPRRROrOON\\SSSoAaETmAcppDLlBAeh\DDCEBeoN\t00G33nr005o5i00v44eAANCPCODGEASACCS0S3FF1M504 MLoLeaabtsshttocdmmo:ooddedriiftiieedd:: Non Mar 15 13:28:37 2004 P:\Da~a\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2D04 NPDES 031504 Job Code: Printed: Tue ax 16 07:26:27 2004 Printed: Tue Mar 16 07:26:27 2004 KNTaaemmxeet::= 030500a-442 030504A-442 Text= 4: co sultonate prs 41L:91C955688--S99ulRRfeeoppn,,atDDeFF==P11F00HS 1i0003300055,0044AA--444422 Sm Sm (Mn, (Mn, 263) 2x3) 852 1i oz8.52 |= | dlr2p 6 ear 0 pee o n 800 2.00 4.00 6.00 8.00 5: co sulfonate pros 5[LL:11C9958586--S99ulRRfeeoppn,,atDDeFF==P11F00OS 101030300055,0044AA--444422 Sm Sm (Mn, (Mn, 2x3) 2x3) sar 881.3827' || wli , he- 200 am 60 80r0e 2.00 4.00 6.00 8.00 1133--MMaarr--22L00C00I44M00S77I::M3366S::5511 MRM MRM of of 55LCCChhIaMannnSn3e/elMlss9S>EE8S9S#-)1-] 394497,7h4>40ee84a40) Area 1000 Time -- Time 10.00 1133--MMaarr--22L00C0044I00M77S::33I66:#:M55S151 MRM MRM of of LC/M$1M5 #6 Chann1el9s 9E5S> 5 Channels ES- 49A9 z> a9d9 4.2AA7rreeea4al 700r0 ee 10.00 | TiTimmee| | i | 1 1 EExxyyggeenn RReessesaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaactee CCoolllleeggee,, PPAA 1166880011 1 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSTUUYBBIDJJIEAESCCTLTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00119966 IM_MNO1539347 3M MN01539347 QgSuuuaeennyttiiNtfGyy. sS(aaLmm3pp5ll8ee, RRSeeapptoorrttNo.1030504A, Ext.Date:03/05/08, AnalystiK.Risha PPaaggee 8855 Study No. :L1958, Set No.:030504A, Ext.Date:03/05/04, Analyst:K.Risha VTLSSaaaaatrsmmttoppllameme:ooddLLiiiiffssiitte:e:dd:: 3MFMP:ooo:\nn\\DDbaMWaataattarraa\\\LL11LC5C5HCMSHS21HEM33SSS:iEE264\2\HMi:Maa4aase6ssssll2L2y00yn00nyx44x\\F\FlluFuoorLrooccuhheeommiicxcaalolas.c.PPPRRRhOOO\\SeHSAeaZnEmpApLDilaBeD\DcRCE\o\a0t02G3l0r0So50sv04e4AANECCDGGESAACCS03FS1M504 MLLeaatsnhteocdamm:tooedaritftiaedd:: Won Har 15 13138113 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 PJroibntCeodd:e: Tue Mar 16 07:26:37 2004 Printed: Tue Mar 16 07:26:27 2004 Rp Name: 030504A-443 3: ce ncia seus Text= I: C6 Acid PFHA |LL11995588--1100,, DDFF==1100 00:3300550044AA.-444433 Sm Sm vn,(Mn, 223) 2x3) " _ +a88n.11s33zs _ 1133--MMaarr--22000044 0077::5588::229 LOMSIMS LC/MS/MS #6 MRMof 5 Channels ES- MRM of 5 Channels ES- 315.200 313 > 269 650es| 6,50e5 ra)Area 22.0000 44..0000 22L::198cC58o8-nA1oc0ii,ddBFPrF=oO1nA0 L1958-10, DF=10 01;33005500444A--444433 Sm Sm (un, 253) (Mn, 2x3) ree Tine | 86.0000 88..0000 10100.000 Time 1133--MMaarr--22L00o004m4 s007I7::M55S68::29 28s80.e46o793 MRMof MRM of 55LCCChh/Maan44Snn11/en33M"lse>S23EEl3S20S#s6-89-69 ea 1.23e6 Area 10%01 233473~ i - Time | %0~,, , , , ,, ,,,--;-- .... , .... ~ .... , .... ~ .... , .... , .... , .... , .... , .... , To 0 500 800 Too 2.00 4.00 6.00 8.00 10.00 Time 3: ct sultanate orms 3:C4 Sulfonate PFBS [L1958-10, DF=10 13 Mar2004 07:58: . L1958-10, DF=10 130504A-443 Sm (n, 213) RM of Channels ES- 030504A-443 Sm (Mn, 2x3) ro " 15765 srteea| 100- 13-Mar.2004 07:58:29 LLCC//MMSS//MMSS #6 MRM of 5 Channels ES- 71.5586 CCaanncceellEO~| 4,86e4 Area mee ae ' | rere 2.00 4.00 -- 6.00 8.00 10.00 Timo|E Time I Exygen Research, 3058 Research Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 I `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00119977 _MNO1S39348 3M MN01539348 QQSuutaaundntytNiiotfyy. SsLaa5mm5ppll8ee,RReeSppotoorrttNo.:030504A, Bet.Date:03/05/04, AnalystiK.Risha PPaaggee 8866 Study No.:LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst=K.Risha NTSLSaaaaatssmmhktppollaemem:ooddLLiiiiffssitti:e:edd=: MPo5o:n:n\D\DaNMacDaatarraa\\tL1L1a55CeM\n1S1L3M3s:=SeC2262H2\H::MSa44as66HsssSLl22y(00y0m0n\84mxM\PFeLlsuoosorclohcyhenesmxii\caalFlsls..uPPPoRRROOOrV)\oHSSSaacmCmhpAplOleeBenD\DBCBi\o\cOL03a3a0E0lSo50V0s4e4.AAPCCDGOESAACCS0SF3FM1504 MLGLoeaabtsS"httocdmom:dooedsritftiieedd:: on Mar 15 13:25:11 004 P:\Data\LCMSMS6\Masslyllx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 Job Code: PPrriinntteedd=: TTuuee MMaarr 1166 0077:=2266:=2277 22000044 NKTaeaxmntee!=: 00330055004AA--444433 Text= 44L:1:9Cc5668-sS1uu0ll,tfDooFnnaa=tt1ee0 pPFrHiSs L1958-10, DF=10 030501A4S4m3 (Mn, 223) [030504A-443 Sm (Mn, 2x3) % s08s.8520 1133--MMaarr--22L00C00I44M00S77I::M5588S::29 MRM MRM of of 55LCCChh/aMannnS3ne0/elM5lss.SE65S#0--6) 39e40.26A>2r0ee84a40 Area r 250 r 400 r --5--00 -- 2.00 4.00 6.00 551: :9C5c88o.1sS0uu,llffDoonnFaa=tt1ee0pPrFoOsS L1958-10, DF=10 1000330005,50044A4-444433 Sm Sm in,(Mn, 213) 2x3) ?i Bo6.00 78o9.e488r7 000 TTiimmee 10.00 1733--MMaarr--22L00o004m8 s007i7::m55s68::229 MRM MRM of of 55LCCChh/MaannS1nn9/eeMl9lsS5EE0SS#-9-6 499 > 99 1A2r0e0a 4,12e4 Area . ol 260 a0 ep amo 00e0 er TTiimmee 2.00 4.00 6.00 8.00 10.00 | | i | Exygen Resancch, 2058 Ressarch Drive, State College, BA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 ' `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00119988 SW_MNO1839349 3M MN01539349 QSquuEaaNnnGttiiftNoyy.EsSiaa5mm5ppll0ee,RReepp0ootrrNtto.1030504n, Ext.Dates03/05/04, Analystix.Riska PPaaggeo 8877 SLSSaAatmTmupEpdlmlyeeoNdoLLi.iis:sFttLr:=Ie9d5:8,MPPo:rn\S\DeMtaDatcANao\C.L1=5aC0M\3S10LM35S1C0364H3\A1MS,4a6MssSlE2Exy00tn\%.xND\aFatlseu:os0r3lo/cy0h5ne/mc0i4\c,aFllAsn.uaPFolRRyOrOs\\o~SS=acAKmph.pLRleaieaDsDEhBiNa\o0033a00l5500s44.A CG CG ACS ACSFM sMLLaeaattsshrttoodsmm::oodaitfeiseedd:: HMP5oo:nn\DDmMataatarra\\LL11e55CwMsS11nM33sS:1s26223\H:1Ma41as63sssl22Ly0000ny48x\F\luLorouchoemizcaols..cPRROhO\\MMeGeEtRnhDDBBt\\CCocoEtGGaEroolvvee NFDES NPDES 031504 031504 LaSt modified: Mon Mar 15 13:25:12 2004 Printed: Job Code: Printed: Tue ax 16 07:26:27 2004 Tue Mar 16 07:26:27 2004 aTNamomert: 030504A-444 030504A-444 T2:extc:e nos sen i[:L19C568-A1c1i,dDFPF=~1A00 L1958-11, DF=100 00p330y0550044A4-444444 Sm Sm (Mn, (Mn, 213) 2x3) 100 % sai8.1s05 1133--MMaarr--22L00O0048M00S68M::22S00::1#1363 MRM MRM of of 55LCCChh/aMannSanne/eM>llsS2S6#0-6 313 > 269 94e70a4) 9.47e4 Area 0 rrr 250 r4-- 00 ---- 500 ---- I50 ----i0E0-- 0IS-- EN .... , ,~-,~~-,,, ,~,, .... ~ .... ~ .... ~ .... ~ .... , .... ~ .... Tine Time 2.00 4.00 6.00 ~ 8.00 10.00 221::9C5c88o-1An1cii,ddDFPpFr=Oo1An00 _ 13-Mar-2008 08:20:13 L1958-11, DF=100 10;3003500540A4-444444 Sm Sm (Mn, (Mn, 263) 2x3) 1M3R-MMaorf-25LL0CCO0h/M4aMnS0nSIe8/lM:M2sSS0E:S1##-366 as MRM of 5 a5360 Ci~annels ES- st8a.6r9 413 > 369 29Ar2e5a 2.92e5 " Area || |{ 2=00 500 530 500 S 000 S" Te Time 2.00 4.00 6.00 8.00 10.00 33[:L:1C9c45t6-Ss1uu1ll,ftDooFnnaa=tt1ee00pPeFBaSs 13-Mar-2004 08:20:13 L1958-11, DF=100 00o330o0550044A4-444444 SSmm ((Minn,, 225x33)) 75 1MM3RR-MMMaoorff-255LL0CCOC0hhI/4aMaMnn0SnSn28eI/el0M:Ml2ss9SS05EE:S9S#1#.9-636 : | 100q ist7.56 299 > 99 52a2r0e3a 6.22e3 Area ! | LNA ram Am aNr | rn EE ------------ 0 .................... , .... , .... , .... , .... , .... ~ .... , .... Time , 200 400 em en ido 2.00 4.00 6.00 8.00 10.00 ! Exygen Research, 3050 Ressarch Drive, State College, 7A 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 1 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00119999 _MNO1S39350 3M MN01539350 SQQutuauanndttyiifNfyoy.:SS5aa1mm5pp5ll8ee, RReeSppeotorrNtto.:030504A, Ext.Date:03/05/04, Analyst:K.Risha PPaaggee 8888 Study No.=LI958, Set No.=030504A, Ext.Date=03/05/04, Analyst:K.Risha SLSaaasmstpplleemodLLiiifsstti:=ed:p\MPDe:an\tDaNa\atLraH\LS1C5HMSS1E3M\1SM26a2\s1Ms4a6lsysl2n0yx0n\4xP\lFulouroorcochheeamiiccaallss.PPRROO\\SSaazmpplleeDDEB\\O03300550044AA CO CG ACSF ACSFM MMLLeeaattsshhttooddmm::ooddiiffiieedd:: M7HPioo:\n\nDDaMaNtataaarr\\LL11cC55HMsS11wM33SS::6622\32MH:=aa14ss26ssl22ly00l00yl44xn\Fxlu\orFoclheumiocarls.o.PPcRROOh\\KMeeetthnhDDBiB\\CcCootatGGolrovsvee NNEPDDEESS 003311550044 Gob code: Last modified: Job Code: MOn Mar 15 13:25:12 2004 PPrriinntteedd:: Tue Mar 16 07:26:27 2004 Tue Mar 16 07:26=27 2004 NNTaaemmxeet=:s 030501A-444 030504A-444 Text= 44::Cc6e sSuulltfoonnaatree pRES PFHS ~ [|LL11995588--1111,, DDFF==110000 0403300550044A4-44444 SSmm (bin, (Mn, 2:3) 2x3) )1 1133--MMaarr--22L00C0044IM0088S::I220M0#::S1133 850 MMRRMM ooff 55LGCChh/aMannnSn3oe/9lMl9ss>SEESS#8-0-6) so8.s50 39229.44e>000ea8440 Area e re p 200 2.00 55[: L:1C9C8588-Ss1uu1ll,ffDooFnnaa=tt1ee00pPrFOoSs L1958-11, DF=100 030504A-444 Sm (Mn, 233) 1001 030504A-444 Sm (Mn, 2x3) 1 O01 --4--00 --------60retro-80B 0 ri 100r0e r -- rTiTimmee 4.00 6.00 8.00 10.00 _ 13-Mar-200_4--08:20:1 1M3R-MMoafr-25LL0CCC0h//4aMMn0nSSe8//l:MM2sS0SE:1#S36| 2880.308567 MRM of 5 Chann41e99l19s9a>dE9eS99,-9) 269~ `rea 1.44e4 Area | 4Ore Bere Time , 22.6000 a04.00 66.0000 88.0000 1I 00.0000 Time | Exygen Research, 2058 Reseazch Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSTUUYBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00220000 3M_MNo1539351 3M MN01539351 qQSuueaaannyttiiNtfyy. sSTaaEmm5pp5ll0ee, RReeSpp68oorrYtto. 1030504A, Bxt.Date:03/05/04, AnalystK.Risha PSaaggee 3895 Study No.=LI958, Set No.=030504A, Ext.Date=03/05/04, Analyst:K.Risha SLSaaamsmptpllmeeodLLiiissftti::ed: NLaatsrtoam:odified: MMPB7:oo=:\nn\\DDDaNMaataatterraa\\\LL11LC55CMHMSSS11HHM33SS:S:S6262\23\Ma::Ma44ass66sssslLl22y0y0n0y0nx44x\n\PFlxluuo\orroFocchlheenumiicocaalxlss.o..PPPRRcROOO\\h\HSSeAeaERmhpnpD1lBeie\DDCEcBo\\taG0a33rl00o5Svs0Oe44AANCPCDGGESAACCS0F3S1M504 MLLJeaaotsabhttocmdomo:dodad:iftioedd:: Non Nar 15 13:25112 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethD~\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 Job Code: Pprriinntteedd:: Tue wax 16 07:26:27 2004 Tue Mar 16 07:26=27 2004 aNammae:: 003300550044AA--444455 ) Text= 1: ce acid pea_n {[iLL:1199C55688--A11c22i,,dDDFPFF==H11A000000 {00f3o3e0s50045A0-44454SS5mm (Mn, (Mn, 230) 2x3) as 815 8.15 1133--MMaarr--22L00C00I44M00S88I::M442S2::0#0151 LC/MS/MS #6 MRM of 5 Ghamnels 5. | 3135 260 MRM of 5 Channels ES313 > 269 "onodArea 4.62e4 Area *(7 CE o 10o~ 22.0000 22L::c79eC588.Aa1cc2ii,ddDFPpFr=oO1nA000 51958-12, DF=1000 cosoun-445 Sm 4, 220) MRMof ramets 5.| 030504A-445 Sm (Mn, 2x3) " %yi 11! -------- 400 Ea 630 r5r 00 r 1000 r TTiimmee 4.00 6.00 8.00 10.00 _ 13I Mar-2004 08:42:01 LCIMSIMS #5 13-Mar-2004 08:42:01 LC/MS/MS #6 2I89.65)960 MRM of 5 Channels ES- 43>369 413 > 369 21A0r0ea5l| 2.A0reea5l | | . O= rr200 0 ~,"~, ., .... , .... , 460 .... ,.. , 6,0 , 8003~9- 56~ 1100.0000 ~-TTiimmeei 2.00 4.00 6.00 8.00 3: c4 sulfonate ors 3L:19C548-S1u2l,fDonFa=t1e00P0FBS 13-Mar-2004 08:42:01 : L1958-12, DF=1000 LOMS/MS #5 13-Mar-2004 08:42:01 LC/MS/MS #6 30504-4455 in 20) MoR f5CraM mnels 5-| | i | 00, 030504A-445 Sm (Mn, 2x3) 1( E773d.558550 || EA AAAAS ees eo MRM of 5 Channels ES- 26> 969) 299 > 99 21503) 2.15e3 Area NA AAA , O 0 i , 20, 0 r ~ 40, 0 ,g 60, 0 , 8=0~r 0 ~ e 10~00 ~ e TTiime|j 2.00 4.00 6.00 8.00 10.00 | Eeygen Research, 3038 Ressazch Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00220011 SW_Mo1S39352 3M MN01539352 QQSuueaaannyttiiNtfbyy. SSLauImx5pp5ll0ee. RReeSppeoeorrNtto. :030504A, Bxt.Date:03/05/04, AnalystiK.Risha PPaaggee 9900 NDLSSSaaaatatvsmumhEtpdpollyameem:ooNddoLLii.iifz:ssiitLt:ee:Idd9::58,BMPMe:o:nn\\SDDDeaMMatRteatCurrNaako\\.L1L1:5C5C0MH3S11S03M3W51S:S0326S432\\KA1:MWa,44aage6sssss1l2E2l0yx0y0ntym84.xxD\\oaFFtlleuxu:oc0rr3\oo/cc0hFh5ee/m0nli4icc,caaulalslAs.no.aP.FlRPRryOROs\O\toSSa:aACKmSEc.pPDRlBLihe\EsDCDhBeoBa\LG0G3n3E00o55sv00e44AANCECDOGESAACCS0F3T1M504 MLLeaatsShttoedmm:ooasdiiefiiaedd:s Non Nar 35 13135137 2008 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove MOn Mar 15 13:25:12 2004 NPDES 031504 PJroibntCeoddse: Tue Mar 16 07:36:37 2008 Printed: Tue Mar 16 07=26=27 2004 [ To -- Name: 030504A-445 T4:extc=o sultonace pee [L: 19C566-S1u2l,fDoFna=t1e00P0FHS L1958-12, DF=1000 030504445 Sm (Mn, 253) 030504A-445 Sm (Mn, 2x3) =| *|i r 260 prs 0~ ' i ' ' ' ' I ' ' ' ' I .... I ' ' ' ' 850 7M3RMMarof2L0G0Cr4Ma0S8n3:9eI425-M:#550S-610 as8s.520 13-Mar-2004 08:42:01 LC/MS/MS #6 MRM of 5 Channels ES- 1.7004 399 > 80 1.70e4 Area r50r0 rerea0 1050 Tne ||J ' ' ' ' I ' ' ' ' I .... I ' ' ' ' I ' ' ' ' I .... I ' ' ' ' Time 5. co sulfonate 2p.0r0os 4.00 _ 6.00 L7958.12, DF=1000 5:C8 Sulfonate PFOS L1958-12, DF=1000 003p300y550044nA--444455 sm Sm (tn, (Mn, 2)2x3) fee *00l ~% 1 200 a0 50 2.00 4.00 6.00 A8.00 10.00 13-Ma r- 2i 00 4 06 :4 2: 01 ase 13-Mar-2004 08:42:01 LoMSIMS LClMS/MS #6 MRMof 5 Chann5el5s E5s 0 MRM of 5 Channels ES- T8o.8n6e 49S95r>0ee9ad9, | 180~L~9 .60e3Area abo 060 8.00 10.00 EExryggoenn RReesseeaarrcchh,, 33005586 RReesseeaarxcchh DDrriivvee,, State State College, College, PA PA 16803 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00220022 _Motsaoass 3M MN01539353 aunty amps Repose rere Quantify S~mple Report Be EES. TESo.030804, Bet.Date103/08/04, Anaiyenek. Misha Study No.=LI958, Set No.=030504A, Ext.Date=03/05/04, Analyst~K.Risha Semple Lists 9r\BaCa\CHENEY WassLym Phuosochenicnls. PRO\SamplaBR\G3OSOUA GG ACSF Sample List= P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM pre rE Last modified: Mon Mar 15 13:22=46 2004 oa He LeNbS hogssyot\Fiuorochentcals. RO\HethaM\GotGrove NPDES 033504 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 FI a ri LaSt modified: Mon Mar 15 13:~5:12 2004 prtnteds Job Code= Printed: mon va 36 S267 2008 Tue Mar 16 07=26:27 2004 ama: 030504446 Name= 030504A-446 = Text= NP I: C6 Acid PFHA 1XXCC003300550044--33,, 110000 nngg/lLL SSttaannddaarrdd |osos44a6u5mn i, 20 I 0130005.04A-446 Sm (Mn, 23) ;100 * Mme emer epre 200 oa nn 2: C8 Acid PFOA pree 400 600 c;sosnaaas sm (i, 223) XXCC003300550044--33,, 110000 nngg//LL SSttaannddaarrdd 030504A-446 Sm (Mn, 23) pod88..1177 ~ 800 Aon8.73 33768i } LCIMSIMS 13-Mar-2004 09:03: 13-Mar-2004LC/MS/MS09:03:54#6 MRM of 3 Crm5 MRM of 5 Channels ES331133 >> 226699) Sted 8.59e4 potArea Tio Tm Tne 1133--MMaarr--22000044 0099::0033::54 Lemsms LClMS/MS #~ MRM of Gran E5- MRM of 5 Channels ES- sey 413 > 369 rooodd 1.93e5Area hy | | 1(1!. 0 rep7r5 eeape a eao IETE osEeT)ine 0 ~'"-'z--~' ' i .... I .... I .... I .... I .... I .... I - ..- .. ~ .... I .... I .... ~ ....\ Time 2.00 4.00 6.00 8.00 10.00 JAP 3:C4 Sulfonate PFBS ' XXCC003300550044--33,, 110000 nngg/lhL SSttaannddaarrdd csosnan-44 5m (20) wy UR of Chann5a. 030504A-446 Sm (Mn, 23) , | oJo,I7VNozOsRnes am 52RY3WS argent Rgn JAARw ofWVwoRLossioe | AOR OOq 0.74 0 95 92 38 ers V/ 7.48 gS ais LOMSIMS #6 1133--MMaarr--22000044 0099::0033::5544 LC/MS/MS #6 MRM of 5 Channels ES- 299 > g9 OF O78E10P13 oer 1.14e3 7 | | 0 ,,,,, .... , .... , .... , .... ~ .... I .... I .... I .... I .... , .... ~ .... Time ! 200 0 bo soo roo TM 2.00 4.00 6.00 8.00 10.00 I 257m sass 3028 Busoni Seiwa, Shute Oobiage, WA ATES Exygen Research, 3058 Research Drive, State College, PA 16801 CHEONNNEFPIINDCOEU-NNTSTYUIBDJIAESCTLTRITCOTACPOURROTT.ECNTG.IV2E7-O0R1D1E0.R8E8N6T2ERED IN I CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00220033 su_wmoresosse 3M MN01539354 QSQuuEaaannittyiiffWoyy. SS1aa1mm1pp0llSee,RReeSppatoorrttNo.:030504A, Ext.Date:03/05/04, AnalystiK.Riska PPaaggee 9922 Study No.:LI958, Set No.=030504A, Ext.Date:03/05/04, Analyst:K.Risha NLSLSaaaaacsmsmhtptpollmaemeo:oddLLiiiifssfitti::eedd:: MMpPoo:\:nn\oD\aNMatDaatarraa\\LtL11C55CaHM\S1S1H33MLE1=SC22\623\HN:1M4S4aa66sHssSl220y0a600n4l4\x\NyFalmusoars\olcFhyelmmicuc\calrsl.oPPPuRRRcoOOO\h\\rSMSoeaeamEcsnhpphDltlSeee\DcECnBoa\\it00ld3c3r00sao55v00l.e44sANCPCDGGESAACCSS0T3F1HM504 MLFLeaoatsnahttocmdomo:dodedritftioedd:= Mon Nar 15 13125+32 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 JporbiatCeodd:e: Tue Mar 16 07:26:27 2004 Printed: Tue Mar 16 07=26:27 2004 HT~aaozmtees:= 030500A-446 030504A-446 Text: 4: ce suigonate pris 4X:(CCC0063300S55u00l44-f-3o3,n, a11t00e00 PnnFggH//SLL SSttaannddaarrdd ca050.440 Sm 4, 213) 100,1030504A-446 Sm (Mn, 2x3) % SE s08s.3594 1133--MMaarr--22L00C00I44M00S99I::M00S33::5#5454 LC/MS/MS #6 MoR fSChaM mois 5-| MRM of 5 Channels ES- 36> 590) 399 > 80 21701) 2.17e4 ElCan~ { 1'o/l - 200 -- 40 2.00 4.00 55: :(CCc08o30sS5uu0ll4t-fo3o,nnaa1tt0ee0 PpnFgrO/oSLs_Standard XC030504-3, 100 ng/L Standard 110%0303500540A4-444466 Sm Sm (Mn, (Mn, 2:3) 2x3) # 600 soo \ 1000 es Time 6.00 8.00 10.00 _. 13-Mar-2004 09:03: 1M3R-MMaorf-25LL0GCC0h//4aMMn0nSSe9//lM:M0sS3SE:S5#-46 28881.39200 MRM of 5 199> 99 Channels 491929>0949) oa 1.29e4 Area | , r 200 450 63r 0 800 dos) TTimee 2.00 4.00 6.00 8.00 10.00 | i Bxygen Ressarch, 3058 Reseasch Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 1199339..00220044 SW_MNo1S39355 3M MN01539355 qQSuuvaaannyttiiNtfoyy.SSLaaAsm3pp5li8ee,RReeSppoooxrrtNto.:030504, Ext.Date:03/05/04, Aaalyst:.Risha Sage 52 Page 93 frTLSSSeaaataersmumetpdpslylmeneoNedoLLiii.itfss:ittLa::eIad9s:58vB,Mp:eo:\nn\SDDevDaaMtaattatararNa\o\LL.1L1OC:55CHN0MSE3ST1W03M3S5iS:S0a264d2\\Ai:MMn,e4aags6ssssslEl0y2y0xy00mtn44e.cxD\\a7F\tileuu:ooF0rr3oo/ccl0hh5ee/nmu0ti4ccc,aaaolllssA.s.nx.RaPFlORRoy\OOs\G\tSaWc:aemKmSp.phlhRlDeieBDsD\eehBC\a\o00tn33a00r5o5i0v04e4AANCFCDGGESAACCS0SF3F1M504 MLTeaatrshttocdmme:oedtaiifziieedd:: wen Nar 36 13138113 2000 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 JsoribntCeoddse= Tue Mar 16 07:36:37 2008 Printed: Tue Mar 16 07:26:27 2004 -- Name: 030504A-447 |oaceosns.m4o4u7, 213) T1:extC=6 reid ven 1LL:1199C55688--A11c33i,,dDDFPFF==H11A0000 asy 030504A-447 Sm (Mn, 2x3) %1 MoR f 5CraM mnols 5.| 1133--MMaarr--22000044 0099::2255::3355 LOMSIMS #6 LC/MS/MS #6 MRM of 5 Channels ES- a1s a2 &15 313 > 269 zed v= 7.9AAr4reeeaa4) preRT IT Tne rrr pram rrTime 200 ho ob 560 Too 2.00 4.00 6.00 8.00 10.00 2. ca ncta sron - SE 2: C8 Acid PFOA LL11995588--1133,, DDFF==110000 0T3o05044447Si (4, 2) on MRMof 5 Chananelss Em5- 030504A-447 Sm (Mn, 2x3) 1133--MMaarr--22000044 0099::2255::3355 LLCC//MMSS/IMMSS ##66 MRM of 5 Channels ES- 8.71 413 > 369 a0iss Tae00a5 1.66e5Area " |i 100%]_ i0 or260 e abo 50e0 e m 500 000 Tie 0 r,,'-...~, , ,~..~, 2.00 4.00 3. ca surtonsce piss : C4 Sulfonate PFBS [LL11995588--1133,, DDFF=--110000 ' 030504447 Sm (4, 219) MRM of 5 Ghannols 5- 030504A-447 Sm (Mn, 2x3) I 70 25699 vo 6.00 3- 0355~ 8.00 107.1589 10.00 \ Time 1133--MMaarr--22000044 0099::2255::3355 LLCC//MMSS//MMSS ##66 MRM of 5 Channels ES- 4.1963 299 > 99 4.A9reea3l % ea 1001 ' J mn A NP | omer ~ errr eee TiS ) 200 400 6b Tao ido TTT 2.00 4.00 6.00 8.00 10.00 i Sxygen Research, 3058 Kassurch Drive, State College, PA 16601 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00220055 _Motsaoass 3M MN01539356 qQSuuEaannUttiitfHoyy.1sS1aa1mm5pp5ll0ee,RRSeeeppvoorsNtto. 1030504, Ext.Date:03/05/04, Analyetix.Risha Page 34 Page 94 SLSSaaatsmmutppdllymeeoNdoLLii.ifss:titL::eI9d5:8P,:MP\o:nD\SaeDHtataterNa\o\L.L1C:sCH0MS31SH03MS51S0S364\3\A1M,4Na6ssa2lE0xys0tn4.xDs\aFtlleu=oy0r3o/nc0h5es/m0ic\4ca,alFlsAsn.laPPlRRuyOOs)\SotSa:asKmrp.plRloaieDsDBchB\a\0h03300e55004n4AA CCOG AACCSFSM NaMLLToeaatantssrhhtttoocddammms=soooedddsiiitffiiseeeddd::: wMP7oo:nn\bDaHMataatarra\\L1L15sCMSS11M33S:S123623\\:1kM43aa63ssssly22y00m00na44x\Flluuoorroocchheenmiiccaallss..PPRROO\\MKeetEhLDDBBA\CCOoLtGGEroovvee Mon Mar 15 13:25:12 2004 NEDES NPDES 031504 031504 JPorbintCeosd:e= Tue Max 16 07:26:27 2004 Printed: Tue Mar 16 07:26=27 2004 [I ---- Name~ 030504A-447 Text~ 4: ce surtonace poms 4L:19C568-S1u3l,fDonFa=t1e00PFIqS L1958-13, DF=100 p00r330055y0044A4-44477 Sm Sm (Mn, (Mn, 263) 23) i 88i.5522 71 1733--MMaarr--22L00o00m44 s00/9::2M25S57:335 MRMof MRM of 55LCCChh/aMannnSn33ee/9lM9Tl9ss6So>EE5SS#88d.~-00 rea) 3.91e3Area T L 1~i/o ~o r e ae ese a0 roe"fn | 5: co sutonate 2p.0r0os 4.00 6.00 8.00 10.00 5[L:L~198C55888--S~1u33l,,fDDoFnFa==t~1e0000PFOS 1~ 33--MMaa~r--22L00O0048M008S9::I225M5::3S#3:15 0003300s550044A4-444477 Sm Sm (hn, (Mn, 213) 23) oo8sa.8r7 MRAM MRM of of 55LCCChhIMaannSn41ee/99M"ll9s9oSrE>E5eSS5#93--699) 1001 653i oes 4.07e3 ma | J :/i~'-/~~ ~ Area oA e o e no T ne Be me || Time 2.00 4.00 6.00 8.00 10.00 | | i | Exygen Reseaceh, 3058 Research Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00220066 _MNO1S39357 3M MN01539357 QQSuuiaaannyttiiNfthyy.TSsIaa5mm5ppll8ee,RRee3pp0oo%rrNtto. 10305048, Ext.Date:03/05/04, Analysts.Risks page 35 YeLSSSaaatatTsmumhtpdpolylnmeensoNidoLDi.iilfs=sittLa:=eId9,:58,M3Po::nS\DeD\aaMtataDtrarNaAo\L.iL1C=e5CE0aMa3S13\0SM35:SLi026a4S2d\eA:MaE,a4ase6s\ssWEl2LBxy0oyan0tmna4e.xsD\\saFFtilleuu~oyo0rrn3oos/cxh0he5\en/miF0ic4cia,aluleAs.on.PaPrPRlRROoyOO\s\\cKtSGA=ashCKmmAe.ppDRlLnEiea\snDiChaBcoa\0t0a3G30r0l3o50sv04a4.AANECCDGGESAACG0SS3FT3MI504 MTr Leoatsrhttoa dmm:oadciifciieedd:: won wan ie 1313801 206 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove MOn Mar 15 13:25:12 2004 NPDES 031504 PJorbinCtoedde: me ar 16 07.26.37 2004 Printed: Tue Mar 16 07:26=27 2004 Ns.aummees: 0305008-448 030504A-448 n T1:extc:e nec ta omaorlawa i: C6 Acid PFHA 013000.504445m8 tn. 23) LL11995588--13 RReepp,, DDFF==1100 | 030504A-448 Sm (Mn, 2x3) 100C E2w8.i41r7 1133--MMaarr--22000044 0099::4477::111~ LLCC//MMSS//MMSS MRM of hans ES- MRM of 5 Channels ESion 200 313 > 269 Tred 7.77e4 eaArea *% | rere | L 22.0000 44.0000 66.0000 88.0000 010.0000 TT TTimTe [22L4:1C9c85t8-A1cc3iiadRoePprF,OnADF=100 _ ~ T3-Mar-2008 094TH L1958-13 Rep, DF=I00 !J30304448 5m (vn. 233) 030504A-448 Sm (Mn, 2x3) 13-Mar-2004 09:47:1 LCMSIMS LC/MS/MS #~ ant MRM of 5 Ghanpnars EeS- MRM of 5 Channels ES- || oo8.71 413 > 369 areeas, 1.69e5 |% | A~a 1 |OH rrrSerpe -------- I -- Tr Tine | , 22..0000 44.0000 86.0000 88.0000 1100.0000 3: co sulfonate peas _ 31L:91C954588--S11u33lfRRooenppa,,teDDFFP==F11B00S00 1133--MMaarr--22000044 0099::4477::1188] l (0p0303o500540A4-444488 Sm Sm hn, (Mn, 233) 2x3) rot MRM MRM of ChannTel0s6E0S-0 LLCC//MMSS//MMSS #6 of 5 Channels ES- ' 1 hO01 \ 170.6510] rea 38003) 299 > 99 3.80e3 w [| A~a Fd %~ Nereo AAA | ' rrr [Ow ETP TT errr ee al o1s0.e00 Ti Time 2.00 4.00 6.00 8.00 I Bryson Research, 3058 Reseacch Drive, State College, BA 16802 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIEAESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00220077 au_mnorsasse 3M MN01539358 queneity sample Rapers ae Quantify Sample Report fr NN Study No.=LI958, Set No.=030504A, Ext.Date=03/05/04, Analyst:K.Risha Page 96 apie Liat: 5\oaeeLHS eign iuceschenicnls PRO Sama 020304 C3 AcE Sample List: I ee I Last modified= 0 vinceLyot\riorochenicaia FRO\KeEhDR\GoGzov DRS 035304 Method= ER eirton naan AL Last modified: ree Job Code: p:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13=22:46 2004 P=\Data\LCMSMSS\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25=12 2004 primed ve sar 36 07267 2008 Printed: Tue Mar 16 07:26=27 2004 -- Name: 030504A-448 =Text= PN 4: C6 Sulfonate PFHS [iososoun-454m8 i, 2) |LL11995588--1133 RReepp,, DDFF==110000 030504A-448 Sm (Mn, 2x3) ] 1133--MMaarr--22000044 0099::4477::1188 Lomas 30 LC/MS/MS #6 Wt 5 Channa 5. MRM of 5 Channels ES- or ER l8.a5d1 39339.66>55ee8330 poArea 1001 > %1 To a 2.00 4.00 P---- 5: C8 Sulfonate PFOS 1958.13 op, DFo100 L1958-13 Rep, DF=100 occaasssm 20) 030504A-448 Sm (Mn, 2x3) 100. ek A ew AioeT s w || 6.00 714~ 8.00 10.00 Time _ oH 2008 00:47:18 13-Mar-2004 09:47:18 Lomsiv #5 LC/MS/MS #6 WRbt 5 ranas 5. 888.888, MRM of 5 Chann44e99l9s9>>ES999-9) 5 Tor 3.91e3 po |Area , Ta a em aww ee eeeseems 2.00 4.00 6.00 reat 8.00 Ae ASmmswmenes 10.00 | sTit me , | | ' I Ecroes Reseseh, 2058 Raseseeh priv, Sate College, 5A 36861 Exygen Research, 3058 Research Drive, State College, PA 16801 COENAFNIEDEPNITICAOLUNSTUYBDIIESCTTRITCOTACPOURROTT.ECNTG.IV3E71O0RD2E8R8E6N3TEREDIN I CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00220088 sw_morssssss 3M MN01539359 quantity sample Repos: Quantify Sample Report rege 97 Page 97 Study No.=LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst=K.Risha Sample List: 3:\Data\LOISUES\Nasslymc\Fiuosochenicals. SRO\SaspLeDE\030504A Ca ACS Sample List= rg re ey tr Last modified: Yathoa: Four LOMBkSe Wassyme\FLcualcs FrRO\oNecEADhR\CeotnGrotvs WBBES 031504 Method: rR tite Last modified: En Job Code: P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13:22=46 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25=12 2004 Printed: Tue Mar 16 07:26:27 2004 Name: 030504A-449 11 ce neta orn Text= i: C6 Acid PFHA LL11995588--1144,, DDFF==110000 308504449 Sm tn, 230) MRMof 5 ChangESs 030504A-449 Sm (Mn, 2x3) | 25 A ik x ~ soasraok 0 To"a sTSie3me0as0, 2.00 4.00 Ep ---- oo _ I 2: C8 Acid PFOA 8.17 6.00 8.00 1133--MMaarr--22000044 1100::0099::0011) LLCC//MMSS//MMSS #6 MRM of 5 Channels ES313 > 269 7.26e4 Area | 10.00 |LL11995588--1144,, DDFF==110000 c||s;osoenaassm in,22) aort MRM of5LhCaIManS>veIEpaMes#5ee-S6| 030504A-449 Sm (Mn, 23) 1133--MMaarr--22000044 1100::0099::0011] LC/MS/MS #6 MRM of 5 Channels E$- 8.71 413 > 369 1.58e5Area ||lo* > ETT res, | 1001%t_ 2797_~ a | 0 r ,-.---.~,,. ~ ,~, , ~ .... ~ .... ~ .... i .... i .... ~ , 256 i sm ab 0G ie 2.00 4.00 6.00 8.00 ~ .... ~ .... ~ .... 10.00 Time 3:C4 Sulfonate PFBS 3;05044449 Sm 4, 2) |LL11995588--1144,, DDFF==110000 . 030504A-449 Sm (Mn, 2x3) I Cw , Se amew ! ee ee NAN II 2.00 ~ 4.00 6.00 1133--MMaarr--22000044 1100::0099::0011 LLCCI/MMSS//MMSS #6 rat RM of hanTonpEs5o5-9 7.61 eal 170 MRM ~ 5 Channels ES- 29559..22>77e9e393 ew we me 8.00 10.00 1170 1 Time i Exygen Research, 3058 Research Drive, State College, PA 16801 I H`ECCNOONNNFEFIIPDDEIENNNTTICIAAOLLU-N- TSSUYUBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT.TEECNCTGTI.IVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00220099 aW_Notsassso 3M MN01539360 QSQutuauandntytiisNfyoy.:sSLaa1mm9pp5ll3ee, RRSeeepptoorrttNo.:030504A, Bxt.Date:03/05/04, Analystik.Risha aPaggee 9988 Study No.=LI958, Set No.=03GS04A, Ext.Date:03/05/04, Analyst:K.Risha SLSaaasmmtppllmeeodLLiiifsstit::ed: MPoP:n:\\DMDaaattraa\\L1L5CCMM1SS3MM:SS3662\\:MM4aa6ssssl2l0yy0nn4xx\\FFlluuoorroocchheemmiiccaallss..PPRROO\\SSaamspplleeDDBB\\003300550044AA CCOG AACCSSFFM MeMLLeatatsshhttooddmm::ooddiiffiieedd:: MMPPoo:1nn\\DDMMaaaactrraa\\LL11C5C5HMSS11M3M3S:S:632652\\:=M1M4a76sasl22s0y000ns44x\LFylumorxoc\heFmlicualos..zPPoRROOc\\MMheettehhDDnBBi\\CCcoottaGGrrloovvsee NNPPDDEESS 003311550044 LJaoabbstCCmooddoeed:=ified: Mort Mar 15 13:25:12 2004 PPrriinntteedd:: Tue Mar 16 07:26:27 2000 Tue Mar 16 07=26:27 2004 NNaammee=: 003300550064RA--444459 ~ Text= 441::9C5c86o-1Ss4uu,llffDoonnFaa=tt1ee00PpFrHiSs L1958-14, DF=100 (003300550044A4-444499 SSmm ((Mbnn,, 226x33)) 100,1 ] 100~l %% 1133--MMaarr--22L00C00I44M11S00I::M0099S::00#116) 887.535252 MMRRMM ooff 55LCCChh/aMan3nnSn6oeIlM9lssS>EE6SS#.-06| 394925>6830] 735~ `Area, 4.25e3 Area | O0'E,~,~,, ,, 2-00- ,, ....4, 0...0. ,6..0..0, .... , ..T..o,o.... , ....o,g.o... , .... TTiimmee 2.00 4.00 6.00 8.00 10.00 55::CC8o sSuullffoonnaattee PpFrOoSs ; [LL11995588--1144,, DDFF==110000 1133--MMaarr--22L00C004I4 M11S00::M00S99::0011 103003500540A4-444499 SSmm ((MMnn, 225x33)) a9 MMRRMM ooff 5LCCChhIaMannnSn"eeIlMl4ss$>9EESS#99--6] 5%8.89 493398,8`6>A60ree93a39)l Area , anaes | ~~ 2.00 4.00 6.00 aw ew te rv e wen er TY | Time 8.00 10.00 ' | i | | Zaygen Research, 3058 Research Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACPOPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00221100 3M_MND1539361 3M MN01539361 QQSuutaaunndttyiitfHyoy..sSLaaimm5pp5ll0ee, RRSeeepptoorrttNo.:030504A, Ext.Date:03/05/04, Amalysti.Risha PPaaggee 9995 Study No.:LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst:K.Risha NLSLSaaaaatssmmhttppollmdmeeo:oddLLiiiifssfittl=e:edd:: MMPPoo:ronn\\DDaMMaataattarraa\\\LL11LC55CCHMSSS11HH3M3SE:S:E226\\22\MH:=Maa44asn66saasl1l22yy0y0nm0nx0x4x\\\PPFllluuuooorrroooccchhhaeenmmiiicccaaalllass...PPFRRROO0\\\NSSSaaEmmHpplDleeBDDCBBo\\t003G30r0So50v04e4AANECCDOGESAACCS0S3FF1M504 oMLLeaabtsahttmocdoma=dodedsitfhieead:: von Nar 15 13035/13 3008 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mort Mar 15 13:25=12 2004 NPDES 031504 Job Code= Printed: Tue Mar 16 07:26:27 2004 Printed: Tue Mar 16 07=26:27 2004 NNaammae:s 003300550044A8-445500 Texts I11::95cC8o6-1Aa3ccti,adDFPoF=He1A0 L1958-13, DF=10 10305044450 Sm (Mn, 233) 030504A-450 Sm (Mn, 2x3) au8as.i1es52d 249624 1133--MMaarr--22L00C00I44M11S00I::33M00S::551~ MRM MRM of of 55LCCChh/aMamn3Snn1e/l3Mlss5SEE2SS#6.96- 313 > 269 7."7r65e)a 7.97e5 Area Io _ TTT ao em 800 Trerrr TTiimmee 2.00 4.00 6.00 8.00 10.00 22[.:"L19cC58o8-aA1cc3ii,ddDFPpFr=Oo1An0 13-Mar-2008To053 L1958-13, DF=10 ( 0:30504-450 Sm (Mh, 233) 030504A-450 Sm(Mn, 2x3) 1M3R-MMaorf-25LL0CCO0h/4MaMnS1nSIe0/lM:M3sSS0E:S5#-06 | 871 MRM of 5 13>39 Channels ES- 1580.70117 41388..>00A223r0e6e559a) | Area 1001 | | , ~ 260 150817~ , ,~ 0 .... ~ .... i 500 .... i .... t 500 .... i .... i owee .... i .... i , , , Timo Time /i~,',, i ,,, ,2<.-0~0, , 4.00 6.00 8.00 10.00 33L: 1:9Cc54o8-S1su3u,llffDoonFnaa=tt1ee0 PpFrBeSs ~ 13-Mar-2004 10:30: ' 51958-13, DF=I 0 0305044450 Sm (hn, 2x3) 1R3-MMaorf-25LL0CCC0h/4aMMn1nSSe0IMlM:3sSS0E:S5#-06 | 030504A-450 Sm (Mn, 2x3) 71672.061619] MRM of 5 Channels ES- 29`9s>5t0d) 299 > 99 IB 4.58e4 rea| Area ~ , A Pe2e 00 pbEoe T r60 Tr ew ew eoeo] ) 2.00 4.00 6.00 8.00 10.00 | Seygen Research, 3056 Research Drive, State College, 7A 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00221111 SW_MNo1S39362 3M MN01539362 gQSuutaaunndyttiiHftoyy.1SsLaaimm9pp5ll8ee. RReSeupptoorrttNo.:030S04A, Ext.Date:03/05/04, Analystik.Risha PPaaggee 1i0000 Study No.:LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst=K.Risha NLSLSaaaaatssmmhttppolldmmee:ooddLLiiiiffssiittee=:dd:=PrMMP\oo=bDnm\aaDtMMataaata\rra)L\GL1L1H55CeSwMEN3S1MS3M3S1E=SE2\2632M\M1:aMa44as6a6sssslll2y2y0y0nm00nxc44x\\\PFFllluuuooorrroooccchhhaeennmiiicccaaalllass...PFPRRR0OO\\\SSKaeastmphplDleRel\DBCB\O\0t03G30E05o05v40eA4AKVCCDGGESAACCSS0F3T1MH504 LMaesthtodm:odified: Non Nar 15 13135133 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Last modified: Mon Mar 15 13:25:12 2D04 SJeosbntCeoddse= Printed: Tuo Maz 16 07.26.27 2008 Tue Mar 16 07:26:27 2004 Nama: 0305047450 Name= 030504A-450 4T:ext6= sulfonate prs ~ |4LL:119C955688--S11u33l,,fDDonFFa==t11e00 PFHS 11000330005,50044A4-445500 SSmm ((MMnn,, 226x33)) =- 200 460 500 2.00 4.00 6.00 551: :9C5c88o.1sS3uul,ltfDoonnFaa=ct1ee0 pPrFoOsS h1958-13, DF=10 | 10v3003500540A4-4A5-04SS5mm0 (tn, (Mn, 225) 2x3) | ~ ao8o.as5st4 008.00 a=8s.8s8 1133--MMaarr--22L00C00M44 S11I00::M33S00::5#5050 MMRRMM ooff 55LCCChh/aMannnSn3eeIlMlss0>SEE8SS9#0--6)| 393398.6A0>0r6ee84a40] Area 1000 Time "rime J 10.00 13-Mar-2004 10_:30:50 1M 3-MoafrR -25LL0CCCh0Ia/4M MnMn1SSe0IlIM:sM3SS0:55##06.5 MRM of 5 Chann44e993l99s2>>6909949 ves 3.26e4 Area | , Ober200 ao mw 800 1000 TTiimmee 2.00 4.00 6.00 8.00 10.00 | | | cygen Research, 3058 Research Drive, State College, FA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 i `CHEOGNNONFEINDPIEFNNITCIDAOLEU-N-NSTSUTYUBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRVR-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00221122 SW_MNO1839363 3M MN01539363 qQCuuaaynnttiiaftryySssuaEmmpptlTee nReeppoorrhtse. cososoan, met.aces03/08/00, Amelik.yieshta sage 101 Page i01 eELSSSataaasummtdppoyllnemeoNtdoLLi.iitfss=ittLi::eId9::58,MwPpoo1:nn\\SDeDewMtAaaatttrarNaa\o\\L.L31LC:05CuH0MB3DSD1A0MM3Sa5SS:E0G26r42\MaAe:Ma,4assh6sas:El2b7mx0yo30tn\n4.xcPD\laF\itleouP:or0ro3Loc/ch0uhe5e/nmo0i4ccr,aallsoAs.n.PacRPRlROOyOh\)s\KStSeCa:asIKmnp.OplRDleiie\ssDCBhBco\a\t03nO3s00lo54v0seA4ANCPCOGDESAACCS0EF3P3M504 MLneaatsehtoadmm:oaedgiiciieadn:: Hon kar 15 T31aSri 2008 p:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 PJroibncCeosdse: ue var 36 07:36:27 2008 Printed: Tue Mar 16 07:26:27 2004 sama: ca0800n-452 Name= 030504A-451 fed Text= 1c reid pm : C6 Acid PF~A |LL11995588--1133 RReepp,, DDFF==1100 0a3t0e504A4515m (i, 228) 030504A-451 Sm (Mn, 2x3) %100~ wis8.15 2626516711711 _ 1133--MMaarr--22000044 1100::5522::3399. LLCC//MMSS//MMSS ##66 MRM of 3Cranes 5- MRM of 5 Channels ESTas200 313 > 269 99..0077ee55 HeaArea o 2. i oh 200 Too ~ TTiimm]ee s21:9o8Ca88.sA1cc3idaRePrpF,nOAOF2=.0100 4.00 6.00 8.00 So 10.00 13-Mar-2008 105239 L1958-13 Rep, DF=10 0a3e0504451 Sm (i, 223) an 13-Mar-2004 10:52:39 Lomsivs 76 LC/MS/MS #6 MRMof 5 Ghapnele5- MRM of 5 Channels )i030504A-451 00 Sm (Mn, 2x3) reas8.71 15783 wahraesl 413 > 369 8.31e5 Area ! | i Time | 0~,,,, ,, ,~.... ~ .... , .... , .... , .... , .... ~ .... , .... , .... ' .... Time , Tam 7 5% wm 000 2.00 4.00 6.00 8.00 10.00 3: ct suitonato smas _ 3:C4 Sulfonate PFBS ' L11995588--1133 RReepp,, DDFF==1100 , cyaosoun.ss1 5m in, 25) i7ssts MRMof 5 Chan2e5"l8aR5re5e5as0:| 030504A-451 Sm (Mn, 2x3) 1133--MMaarr--22000044 1100::5522::3399 LLCC//MMSS//MMSS ##66 MRM of 5 Channels ES- 7.50 299 > 99 4.87e4 Area , Pr YS cw amo woo | olrrmmerrrrrrerrra rrr Time| bo .... , .... , .... , .... I .... , .... ~ .... ~ ....', .... , .... , .... Time 2.00 4.00 6.00 8.00 10.00 1 Eevaen Sasench, 3038 Resenzch Drive, State College, FA 16001 Exygen Research, 3058 Research Drive, State College, PA 16801 | CCHEOONNNNFEIDFPIEINNTDCIAOELU-NN- TSSTYUUIBBDJJIAEESCCTLTTRTITC0OT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRVR-DD1EE0RR.2E0E0NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00221133 a uorsssaes 3M MN01539364 Trtenn rn en Quantify Sample Report Study No.:LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst=K.Risha Paga 102 at eehE einesArsen er Sample List: st, Losin Last modified: re EL matesstovrsomcotaron oss 1134 Method: Last modified: re Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13:22:46 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25:12 2004 Printed: Tue Mar 16 07:26:27 2004 -- Name: 030504A-451 =Text~ et atmce sms 4:C6 Sulfonate PFHS rm --_ L1958-13 Rep, DF=10 casos smn2 030504A-451 Sm (Mn, 2x3) iIv "| So "me 8.52 WEE 13-M ar-2004 10: 52:39 LLCC//MMSS//MMSS #6 roir2 MRM of 5 Channels ESweet 3939.6>48004 ETT CH .... , .... , .... , .... , .... , .... , ....7~23..5.~. ~ .... ~ .... , .... Ti~e 2.00 4.00 6.00 8.00 10.00 3.64e4Area p---- oe -- 5:C8 Sulfonate PFOS [tL11e95588--1133 RReepp,, DDFF==1100 -sons smn,29 =ws rior SH3 S5| 030504A-451 Sm (Mn, 2x3) 1133--MMaarr--22000044 1100::5522::3399 LLCC//MMSS//MMSS #6 MRM of 5 Channels ES- 8.88 499 > 99 3.51e4 Area * ETE TE | ot I ' ' ' 2' .0I0~ ' ' I ' ' ' 4''.100' ' ' ' I ' ' ' 6' .~ 0'0' ' ' ' i ' i , 8, .0I 0'66' 5' 7' ~I ' ' ' 1_' 0_.I 00' ' ' ' I ' ' ' ' TTiimme|e I I I 1 Exygen Research, 3058 Research Drive, State College, PA 16801 1 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00221144 3M MN01539365 QqSuuaaennttiitfTyy sSIaammppSllee RReeSppeoo.rrtot 20804A, xe.Dave103/08/04, Anayetik.Risha sage 103 Page 103 SfeiLSSStaaatrhssmutppdog llyseemroNdoLLii.ir fss:titL::eId9:58,MEBPo:r:n\SaDe\e MtasDaterNaAo\L.La1:5oC\0Mu3S1Lr 03Ms5O:S026I42\hA:MM,e4aS6sss\LlE2yM0xya0tnae4.x\D\sFaFistlueulo:or0yro3ocm/ch0hee5en/\mi0icF4ca,lallsuAs.n.oaPPRrlRROyOOo\s\\NtcSSS=ashEKmah.pepRTllsieEasDAirhBC\a\co0ta30r0l5o50vs0e44.ANFCCDGOESAACCS0S3FF1M504 MLSCeaaatsrhnttocdnm:oaoad!iitfiieadd=: Kon ker 10 Tiss iis The P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13=25:12 2004 NPDES 031504 JPorbimCoedre: Tue Nar 16 0716137 2008 Printed: Tue Mar 16 07=26:27 2004 [ES Name: 030504A-452 fi Text= Rp i: C6 Acid PFHA L511995588--1144,, DDFF==1I 00 (0;0303500540A4-445522 Sm Sm (tn, (Mn, 20)2x3) 100! % [ol 75% oy 2: co acta pron 2.00 4.00 : C8 Acid PFOA o0sscso45m2 an, 213) 1LL11995588--1144,, DDFF==1100 030504A-452 Sm (Mn, 2x3) |1001 | | oho %0~.. , . 3% 5% 3: co sutfonace 2p.0r0es 4.00 3:C4 Sulfonate PFBS for3asces0452 5m in, 210) [LL11995588--1144,, DDFF==1I00 030504A-452 Sm (Mn, 2x3) %/1001 sis80.i11s5 240487i oh a0 6.00 8.00 adr8o.7te1r 0% wh 6.00 8.00 i77.55=88 1133--MMaarr--22000044 1111::1144::2299] LLCC//MMSS//MMSS ##~6 MRM of Crannol 5- MRM of 5 Channels ES3135260 313 > 269/ Sates 8.35e5~ NeaArea Tene oe _ 10.00 Time 1133--MMaarr--22000044 1111::1144::29 LLCC//MMSS//MMSS #6 MRMof 5 Grane 5- MRM of 5 Channels ESpe 413 > 369 ares) 8.47e5 piArea oe Time ]| 10.00 13-Mar-2004 Tria 13-Mar-2004LLCC/M/S/MMSS1/1:M14S:29#~ MRM of hanna ES- MRM of 5 Channels ES29> 069 299>99 esol 4.69e4 eeeArea FS0/~ .... , . . ,,, , 352.00 hs sw am os ;,, .... , .... , .... , .... , .... , .... , , . .;~T~;~ Time 4.00 6.00 8.00 10.00 Sxygen Reseaceh, 3058 Ressaseh Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 CCHEOONNNNFEIDFPEIINNTDCIAOELU-NN- TSSTUYUIBBDJJIAEESCCTLTTRTITCOOT AAGPOPURRROOTT.TEECNCTOTIIVV2EE7-OO0RR1-DD1EE0RR.0E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00221155 Sw umorssssss 3M MN01539366 QQSuutaaunndttyNiiffoyy.1SS1aa1mm9pp5ll8ee, RReeSppeootrrttNo.:030504A, Ext.Datei03/05/04, AnalystiK.Risha PPaaggee 110044 Study No.=LI958, Set No.=030504A, Ext.Date:03/05/04, Analyst=K.Risha SLSaaamsmptpllemeodLLiiifsstit::ed: MLeatshtodmsodified: MWPPoo1P=nn\:\D\DNaMDaataat4rrta\a\L\L11CL55CHCMSHS11HS3M3SH:S:6S226E22\N\:1MaM48asa66s8sssl221l0y0y00nyn44xx\m\FFlxluuo\orroPocchLheemuniicocaalrlss..o.FPPRRcROOO\\h\MSSeaeaEmnhpnpDllEeieADDCBcEo\\t0aOa33z0l0o55vs00e44AAKFCCDGGESAACCS0F3S1M504 MLLJeaaotSsbhttocdomm:dooeddriiftiieedd:: Mon Mar 15 13125137 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13=25=12 2004 NPDES 031504 Job Code: Pprriinntteedd:: Tue Max 16 07:26:27 2006 Tue Mar 16 07:26:27 2004 TNaammeer: 003300550044AA--445522 Text: [44:L:1C9c56o6-sS1uu4ll,ffDoonnFaa=tt1ee0 PpFewHsS _ / 51958-14, DF=10 11003300550044A4-445522 SSmm ((MMnn,, 22xx33)) *] 1001 1133--MMaarr--22L00C00I44M11S11I::M11S44::2#2959 7887.505228 MMRRMM ooff 5LCCChh/aMannnSn3ee/lM%lssS>EESS#8.-60 30399>00840 rea 3.99e4 Area ES /i , .... 200 .... , .... , 400 .... , .... , 650 .... , .... , 500 ....7,70..3.~. , 1000 .... , .... ere ,~-, , , TTiimmee 2.00 4.00 6.00 8.00 10.00 55[:L:1C9C85o8-sS1uu4ll,ffDooFnnaa=tt1ee0 pPrrooss _ _ 13-Mar-2004 11:14:29 L1958-14, DF=10 10;03300550044AA--445522 Sm Sm (Mn, (Mn, 263) 2x3) 1M3R.MMaorf-25LL0CCC0h//4aMMn1nSSe1//lM:M1sSS4E:S##2.669 a7 MRM of 5 499>99 Ct~annels ES- | o8.r8e7 49339.66A>22r0e9e449a Area | | 200 400 600 800 1000. TTiimmee 2.00 4.00 6.00 8.00 10.00 I Exygen Reseszch, 3058 Research Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHGEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00221166 IM_MNO1539367 3M MN01539367 QSQtuuuaadnnyttiiNffoyy.1SsLaa1mm5pp5ll8ee, RRSeeepptoorrttNo.:030504A, Ext.Date:03/05/08, Analystik.Risha PPaaggee 110055 Study No.=LI958, Set No.=030504A, Ext.Date=03/05/04, Analyst=K.Risha SLSaaasmmtppllmeeodLLiiifssitt:o:d: MPPo:in\\DDNaaattraa\\1LL5CCMHS1S3MM:SS2662\\:MM4aa6ssssl2l0yy0nm4xx\\FFlluuoorroocchheemniiccaallss..P?RROO\\SSaamxpplleeDDBB\\003300550044AA CCOG AACCSSTFMM MMLLeeaattsshhttooddmm:=ooadiitfiieedd:: PoMP1o=n\n\DDMaNataatarra\\L1L1C55CHMSS11NM33S::S622652\\::MM14aa26ssss1l22y00y00mn84xx\\FFlluucorroocchheenmiccaallss.. PPRROO\\NMeeEthhDDBB\\CCoottGGrroovvee NNEPDDEESS 003311550044 LJ0oabbstCCmoododede::ified= Mon Mar 15 13:25:12 2004 PPrriinntteedd:= Tas Max 16 07:26:27 2004 Tue Mar 16 07:26:27 2004 NNaammee:= 003300550044A2--445532 ~Text: 1. : cCe6 AAcctiad PpFewHsA L[L11995588--1155,, DDFF==110000 1 10y0303000550044A4-445533 SSmm ((MMnn,, 22633)) *% 2880.1017700 oo 1133--MMaarr--22L00C00/44M11S11/::M336S6::115 MRM MRM of of 55LCCChh/aMann3nSne1e/lM3lss2SEE65S#9--6)| 31311>..1A126r66ee09a55 Area | 200 400 600 850 10.00 O0S~,~, r , , ....r , ...r . , ...r . , ..-- .. , ..-- .. ~ ..-- .. I , .-- ... , .-- ... , -- .... , -- .... ,-- .... TTiHmvee | 2.00 4.00 6.00 8.00 10.00 22::Cc8o AAcciidd pPrFOoAn [LL11995588--1155,, DDFF==110000 0103000350.50044A4-445533 SSmm ((MMnn,, 226x33)) 100! | 1133--MMaarr--22L00C004I4 M111S1::M33S66::115 an MRMof MRM of 5LCCChh/aMann4nSne3/elM>lssSEE3SS6#--96 sa8o.71 4132>8A73r6e0a95 2.87e5Area | err20r,0~O , r, , , r, , ,~a0~ .... ,r..E .e.80,r0...e. , ....85 0, 04 ..6 ..E ~, ..T..100, 0.... , , , , ,~TTiimmee ! } 2.00 4.00 6.00 8.00 10.00 33::CC44 Ssuullffoonnaattee bPrFaBSs L[L11985588--1155,, DDFF==110000 1133--MMaarr--22L00C004M4 S111I1::M33S66::115 003o3s00550044A4-445533 Sm Sm (Mn, (Mn, 2x3) 2x3) 781 M MRMoofR f 5LCCChhIaMM annnSn2e/e9lMl9ssSEEgSS#-g-6 | 747.61 29559.08A>77re6e9a339) [En 1 Are~ :| AMeme --n -- siondt -- o So -- st 22.0000 44.5000 66.0000 500 8.00 11001.0000 Time | EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 i `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACPOPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00221177 3M_MNO1539368 3M MN01539368 qQSuutaaundntytiiNffoyy.:SSLaa1mm3pp5ll6ee, RReeSpptoorrttNo.:030S04A, Ext.Date:03/05/04, AnalystiX.Risha PPaaggee 110066 Study No.=LI958, Set No.:030504A, Ext.Date:03/05/04, Analys~=K.Risha NoLSLSaaatassmmhttppollmdemeo:oddLLsiiifssfitti::eedd::B:MMPP\ooi:Dnn\\ADDtNMaaaatat\4rraL\\CLL11HC55CHSMSSS11HSM33S:S\16262M22\aN:1Mna44ass66slssy1l22my0y0cm00n\x44xP\\lFFLuluouoroxorococchhheeennmiticccaaalllsss..PPPRRROOO\\\SSNaaemmEppRlDleEeDADBCB\O\0t03O30F05o50v04e4AAKCFCGGDESAACCSS0TF31IM504 JMLLeoaatsbshttocdomm:dooedd:iiffiieedd:: Mon Nar 15 13:12:32 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13=25:12 2004 NPDES 031504 Job Code: Printed: Tue Naz 16 07:26:27 2008 Printed: Tue Mar 16 07:26:27 2004 NNTaaemxmote:s: 003300550044AA--445533 Text: 4: c6 sultonate prs 4L1:91C596568--1S15u5,l,fDDonFFa==t11e0000PFMS 10103003050.0540A4-445533 Sm Sm (Mn, (Mn, 253) 2x3) | | 1133--MMaarr--22L00C00I44M11S11I::M33S66::1#1565 852 MRM MRM of of 55LCCChh/aMannnSn3ee/l9Mlss9S>EES8S#.0-6 a8e.52d 399 > 80i 22`5W0e4a 2.25e4 Area 200 2.00 5: Co sulfonate ros 5L51:199C55888--S11u55l,,fDDoFnFa==t11e0000PFOS 10v03300550044A4-445533 Sm Sm (Mn, (Mn, 28) 2x3) * a 400 4.00 6-- 00 6.00 'I ' '' ' _8008.00 2881.s8581 I e100a 0 e ' 7 ' ' I ' ' ' ' I ' ' ' ' Time 10.00 13-Mar-20I 08 11:36:15 1M3R.MMaorf-25LL0CCC0hI/4aMMnS1nSIe1/MlM:3sSS6#E:S#16-65 MRM of 5 Channels ES- 9"95>0540 499 > 99 1.4`a5ree4a Area o O 200 e 400 600 800 1000 Tine Time 2.00 4.00 6.00 8.00 10.00 i | | I | Beygen Research, 3058 Research Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSTUUYBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00221188 3M_MNO1539369 3M MN01539369 qQSuutaaundnyttiiNffoyy.1SSLaa1mm0ppSllEee, RReeSppeootrrttNo.:030S04A, Ext.Date:03/05/04, AnalystiX.Riska Page 107 Page 107 Study No.=LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst:K.Risha LsSaaasmmtppllmeeodLniiissfttl::ed:P:NP\o:D\naDtNaa~ara\\LL1C5CHMS1SS3MS:S\26M2\a:Ms4as6slsy2ln0yx0n\8xF\lFulouroroocchheemmiiccaallss..PPRROO\\SSaammpplleeDDEB\\G03300S5O044AA CCGG AACCSSFFM NoaLMLLeaaatbtssshhtttoocddmomm::doooeddtriitffliieeeddd::: MPWPoIo:n\\nDDaMaWtaa~arsa\\LL11C55CHMS1S1H3M3S::S326\23\::MH41a67sasl22s0y000n44sx\Flluyoruocnhe\miccFaalllss.uPPRRoOO\\rMKeeotChhDcOBB\AhCCooettGGnrrooivvee Mun Mar 15 13=25:12 2004 NNPEDDEESS 003311550044 Job Code= PPrriinntteedd:: Tue Mar 16 07:26:27 2004 Tue Mar 16 07:26=27 2004 NTNaeamxmete::: 003300550064aA--445544 Text: LILedr:195C68-A1c6i,dDFPF=H1A000 13-Mar-2004 11:57:5 L1958-16, DF=1000 0305042454 Sm (Mn, 25) 1M3R-MMaorf-25LL0CCC0h/4aMMn1nSSe1/MlM:5sSS7E:S5#.86 a030504A-454 Sm (Mn, 23) av8.17 MRM of 5 33>260) Channels ES- 100 313 > 269 ) 10084 bored`rea 5.97e4 Area l % e A er ~ er------T--ine| (} 20am ........ ~ .... ~ .... , .... , 600 .... , .... ,. 8~0 ~ 1000 .... , ........ Time 2.00 4.00 6.00 8.00 10.00 221::9C5c88s-1AA6ccii,ddDFPp=FrOo1nA000 13-Mar-2004 11:57:54 L1958-16, DF=1000 l0a0s04a-454 Sm (in, 253) 1M3R-MMoafr-25LL0CCO0h/M4aMnS1nSI1e/lM:M5sSS7E:S5#-86 ` |030504A-454 Sm (Mn, 2x3) e08r0.7015 MRM of 5 Chan41n13e32l>s.>13E0360S659-9) | 40009] 2.1A9reea5) Area [I | Co | 2mN, .... , ew .... , .... , 6r 00 850 Ae 000 .... ~ .... , .... ,, ."-;-: , .... , .... , ....\ TTiimmee 2.00 4.00 6.00 8.00 10.00 33:1:9c5Co84-1sS6uul,lffDooFnnaa=tt1ee00Pp0FeBnSs oo 13-Mar-2004 11:57: : L1958-16, DF=1000 1030504454 Sm (Mn, 253) 1H3R-MMaorf-25LL0CCC0h/4MaMnS1nSIe1/lM:M5sSS7E:S5#-86 o 100, 030504A-454 Sm(Mn, 2x3) 1, e87o.63 MRM of 5 Channels ES- 23393>99093 299 > 99 | 661 rea 3.39e3 Area |A , fo nN SAA 200 400 Teo Tao "ioo0 TTiimmee|i 2.00 4.00 6.00 8.00 10.00 | EExxyyggeenn RReesseeaarrcchh,, 33005586 RReesseeaarcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 | `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00221199 SW_MNO1839370 3M MN01539370 TT TH JS Quantify Sample Report te eo Study No.:L1958, Set No.=030504A, Ext.Date:03/05/04, Analyst:K.Risha Page 108 SE YEE LE eeeTT EASERS 0 04TH Sample List: rr terre Last modified: EE Method: Last modified: em Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13:22=46 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25=12 2004 Printed: Tue Mar 16 07:26:27 2004 Name: 030504A-454 Text~ 4:C6 Sulfonate PFHS |hL11995588--1166,, DDFF==1IO00000 as.oass Smo,20) 100, 030504A-454 Sm (Mn, 23) 1133--MMaarr--22000044 1111::5577::558 LLCCI/MMSS/M/SM#S#6 Wet nt 5. 88.5522 MRM of 5 Chann33e9l9s9>>E8S980-0] = 52.56e4 odArea 5Oi Or Ee EE 10010%r1 .... , .... , .... , .... , .... , .... , .... , .... , .... , .... ~, ,-.,, 2.00 4.00 6.00 8.00 10.00 nmm---- 5:C8 Sulfonate PFOS | .... -Time L1915985-8-1166,, DDFF==11000000 o]nsounace sm,2c on wets Crmwe0s 030504A-454 Sm (Mn, 2x3) 1133-.MMaarr--22000044 H11E:57:58 LLCC//MMSS//MMSS #61 8.88 2746 MRM of 5 Channels ES499 > 99 11..55220e44] * Area } r ETEe wm a~A , .... , .... , .... , .... , .... , .... , .... , .... , .... , .... , .... -Time 2.00 4.00 6.00 8.00 10.00 | , Exygen Research, 3058 Research Drive, State College, PA 16801 I CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00222200 3M MN01539371 QQSuuiaavnnasttiiwftpyy. SaamSmpEpllSee,RRee3pp0oo%rrttNo.1030504A, Ext.Dater03/05/04, Analyst.Risa rage 103 Page 109 TSSSaaatrmmutppdllyemeoNodLL.iiifss:ittL:e:1d9:5P8i,MP\o:Dn\SaDetWatata\aNLo\.GLIsIC:MS0SU13M30SS51e036\43\MA1Ma,4as6sssllE2yy0xm0nt\4x.FD\laFut1oeu:ro0ro3oc/ch0he5en/mi0ic4ca,allsAs.n.aPPlAROyO\s\StSA=aIKmp.pLRleieDsDRhB\a\0O330OSSDO44AA CG CG ACS ACSFM VoTMLLeaaanetrsshttttocomdmmo=mmooesddriitffiiieeeddd::: MwPoDe:nn\EDMwaAaatrra\LL1165CEMS13M33ES:12632\8a:M04as36sssl2L2y00y0n0m44x\\FPlAsuoorrooschheemmiiccaallas.PPRROO\NMeBtEhRDDBR\CCootGGrroovvee Mon Mar 15 13:25:12 2004 NEDES NPDES 031504 031504 PJroibntCeoddse= Tue mar 26 07:26:27 2008 Printed: Tue Mar 16 07:26:27 2004 [ Tort! -- Name= 030504A-455 Text~ I1[::XCcC06e305Ar0co4is-ad4,pPrF2iH5nA0 ngiL Standard XC030504-4, 250 ng/L Standard 00%330055004A4-445555 Sim Sm (4n, (Mn, 263) 2x3) % "8i5r7e8.17 4.1764~ 313-MMaarr-22L00O0084MS11I22::M11S99::44#116 MMRRMM ooff 55LCCChhIMaan33Snn11eI33Mgrls5>oS2EEd256Ss#6-9-)96 ea 2.04e5 Area Eoreprr2,g5,0r..e.r. r, ....P,-.I.,,,T...) . , .... ~ a0 .... ~ .... , tom .... , .... , a ....~Time soconciaseon 2.00 4.00 6.00 8.00 10.00 X2:C0C3805A0ci4d4,PF2O5A0 nglL Standard XC030504-4, 250 nglL Standard 1133:-MMaarr--22L00o0044m11s22m::11s99::4411 (0p3003o50y0y540A4-445555 Sm Sm in, (Mn, 265) 23) si88.77d11 LC/MS/MS #6 MRMof 5 Cramls ES- MRM of 5 Channels ESp"eatees 413 > 369 % 11 i/1 a 4.4 le5 Area amaaan mama) , 20 pry 50 800 1000 0 ~-,, , , .... -T .... , .... , .... , .... , .... , .... 8~1.4.4.~.~L, .... , .... ~ ...."-Time oC 2.00 4.00 6.00 8.00 10.00 3: co surtomare sess _ 3:C4 Sulfonate PFBS XC030504-4, 250 ng/L Standard 73Mar2004 12:19:41 XC030504-4, 250 ng/L Standard : 1030504455 Sm (Mn, 233) MRMof 5LCOhManSnIelMsSES- 030504A-455 Sm (Mn, 2x3) f|1TM o I75 939>0e15a39 10h 7.59 -1150 13-Mar-2004 12:19:41 LC/MS/MS #6 MRM of 5 Channels ES299 > 99 3.01e3 Area | Vr rae na egt s ere gPA pore Ti | ,L 22.6000 404.00 bo 6.00 ab8.00 10 10.00 j | Bysen Resaacch, 3058 Resaaxch Drive, State College, BA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00222211 m_orsaoar2 3M MN01539372 qSQuutaaunndttyiitHfoyy.1ss1aa1mm5pp5ll8ee,RReeSppeootrsNtto.1030504, Ext.Date:03/05/04, Analyetik.Risha Page 120 Page 110 Study No. =L1958, Set No. =030504A, Ext.Date:03/05/04, Analyst~K.Risha soSTLStaaaarsmmrttppollammeeooddLLiiiiffsstiit:e:edd=: MMPPPoo:\inn\DD\aWMatDaatarraa\\tLL11C65CaMH\S11SM33LH:S1SC26323\HK=1MaS44an66sUssS2l2y00ySm00n44a\x\NPFlaluuuoorrsoolcchhyeennmtiscca\allFssi.PPPuRRROoOO)\rSSMuoasEmsppDlhlBeeedADBnCB\\o0i03tc30G05ao500lv44AsANCECODGEASACCS0F3S1M504 MTaLeoastnschtocdomm=sooead:siefiseoda:: won War 1s 13135113 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mort Mar 15 13:25:12 2004 NPDES 031504 PJorbintCeodd:e: Te Max 16 07:26:27 2008 Printed: Tue Mar 16 07:26:27 2004 NNTaeamxmet::= 00330055004A4-445555 Text~ 4X4: C:0Cc36o05sS0uu4al-ft4oo,nnaa2tt5ee0 pPnFegHw/SsL Standard XC030504-4, 250 ng/L Standard 0003300055.0044AA.-445555 Sm Sm (Mn, (Mn, 2:3) 2x3) i || | 20. 0 PES 2.00 4.00 55: :(CCc08o30sS5uu0l4l-tf4oo,nnaa2tt5ee0 PpnFrgOo/SsL_St_a_ndard XC030504-4, 250 ng/L Standard o(003300550044A4-445555 Sm Sm (un, (Mn, 253)2}(3) || * . 200 50 2.00 4.00 1133-MMaarr--22L00o00M44S11/22M::S1199:::4411 aTs82.a5et47 MRM MRM of of 55LCCChh/aMannSnn33e/e9M0Tll9so6S>ErE2SeS#8.0y-06 rea) 6.64e4 Area 00 B00 00 Time i 6.00 8.00 10.00 | Time 1133--MMaarr-.22L000O048M11S22M::11S98::4411 ses MRM MRM of of 55LCCChh/aMannnSn0e/elMl9ssS5EESS#%--6 EY8.88 499 > 99 32h5e6a4 3.23e4 Area !| 500 85a 0 1000" Time 6.00 8.00 10.00 , i | Exygen Research, 2058 Research Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00222222 _MNO1S39373 3M MN01539373 QQSuuEaa0nnattyiiTtfoyy. sS1aa1m1m5pp5ll0ee, RReeSppetoorrttNo.:030504A, Ext.Date:03/05/04, Analystik.Risha sage 111 Page iii STSSaaatmrmuptpdllyemeoNdoLLii.ifss:ttiL::eId95:8,MPPe:rn\\SDeDMtaaattrNaeo\\.LiL:sCC0MH3S1S0M3M5S:S06aE43\\A1MN,aaasssslE2iyx9y0ntm4.xxD\\aFFtlueuo:or0ro3oc/ch0he5em/mi0ic4ca,allsAs.n.aPFlRRyOOs\\tSS:aaKmS.ppRlLieesDDhBBa\\003300550044AA CO CG ACS ACSFM sTMLLTaeoaaattssnthnttoocdammma:soooedddriiitffiiieeeddd::: HMPFoo:\nn\DDaWMataataart\\LL11oC55uMSS11mM33sS:16e23\28HM:0aa41ss63ssl2L2y09y-00\n40Pxl\uFlouxoorcohcehseimciaclalss..PPRROO\\MMeGtLhEDDBB\\CCoottGzroovvee Mon Mar 15 13:25:12 2004 NNFPDDEESS 003311550044 PJorbinCtoedre: Tue Mar 16 07:36:27 2004 Printed: Tue Mar 16 07:26:27 2004 sama: 030504A-455 Name= 030504A-456 Text= i1:: cCs6 Arcetied PoFrHnA LL11995588--1177,, DDFF==11000000 B002;300550046A8-445566 Sm Sm (i,21) (Mn, 2x3) "I | L 200 00 00 2.00 4.00 6.00 sir8.17 0904489 5008.00 1133--MMaarr--22000044 1122::4411::1199 LLCC//MMSS//MMSS ##66 MofR 5ChaM nnels ES- MRM of 5 Channels ESS20 313 > 269 ea 33..1144e044 000 \L 10.00 Time [L1956-17, DF=1000 2.: 0C88 AAccid PPFFOOAA L1958-17, DF=1000 030504A.456 Sm (Mn, 2x3) 030504A-456 Sm (Mn, 2x3) | 11 % a87r.711s ea) 1133--MMaarrrr--22000048 1122::4411::1199 MRM MRM LLCC/M/MSS//MMSS##66 of 5 Cranes 5- of 5 Channels ESe5S0a0 413 > 369 5.34e5Area | = Time , ,~ .... ~ .... , .... , .... , .... , .... , ....10, 3.7.7.3.~ ~ .... t .... , .... ~ Time 200 a0 500 B00 1000 2.00 4.00 6.00 8.00 10.00 3. co surtonae peas _ ] _ : C4 Sulfonate PFBS Lemsims |LL11995588--1177,, DDFF==11000000 1133--MMaarr--22000044 1122::441:11:71: 9 LCIMS/MS #6 030504.45m6 (bn, 2:3) MRMof 5 Channels ES- 030504A-456 Sm (Mn, 2x3) MRM of 5 Channels ES- too ONfas asez2% aa3 maap so eess 727607788 azn 8707040987094o%r7e0 1083. 10831410 raced | TW RAKANZA] BEA NEN 1( 0.74 32 3.32 4 94 4 22 " 7 ~" ...... 7.36 ,:.~o " ""9 049.79 .~n ~ .... ,. .,. ~, ~ ,.,.,-, A- / ~ ~. \ ..... 299 > 99 1 30e3 IdE2N 60 a0 600 -- ato i050 | 2.00 4.00 6.00 8.00 10.00 Time BExxyyggeenn RReesseeaarrcchh,, 33005386 RReesseeaarrcchh DDrriivvee,, State State College, College, TA PA 16801 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00222233 _MotsaoaTs 3M MN01539374 I qSQuuRaannEttiiS tfyy Ssauesmppilee.RReeppoorrttcor0s0an, met.Dates03/05/04, eadyatixnish rage 112 Page 112 peLSSSrataaesummgtdppsyllmeeoNdoLLi.iif=ssittL=e:Id9|:58,MP3o::pn\\SeDeDMtaatattaarNa\o\.LLr1c:O5C0HuM3ES1sa0NM35S:Ss0S2642\MrA=Maa,4ags6ssssEl2yi0xym0tnm4.xD\eaFFtll\euu:so0sPr3oo/ccL0hh5eeu/sm0iioc4ca,alzlaAs.no.FFaPRRlRcOOyO\\s\hS~HSE:SameKmCp.pDLsRlEeie\TsDtCBhBoNa\ct00G33ar00o55lv004e4nAOCCD5GESAACC0S3FS1M504 R= at moatesass Method= Last modified: hon Nat 55 ToS 0s 250k P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25=12 2004 NPDES 031504 sJroibntCeoddse: mae ar 26 o7i36027 2000 Printed= Tue Mar 16 07:26:27 2004 sama: 0205008456 Name= 030504A-456 ro Text= 4: co sutonace seus 4:C6 Sulfonate PFHS (Coser, DF=ton0 T3-Mar-2008 12:41:19 L1958-17, DF=1000 |E oco45s6 o5muonn, 220) ss MRMof 5 CranToosesE5ao- 030504A-456 Sm (Mn, 2x3) 13-Mar-2004 12:41:1 LLCC//MMSS//MMSS ##66[ MRM of 5 Channels 8.52 399 > 80 3 22.2233e33I Area; |= -- 2h i ao a N Wo m me 2.00 4.00 6.00 8.00 10.00 5. co sultonace eros 5:C8 Sulfonate PFOS I1L915985-81-177,, DDFF==11000000 0oss0804A455 5m (Mn, 2:3) MRIof 5Chnnol E5- 030504A-456 Sm (Mn, 2x3) |! ) afose sTeaoae 1O01 1133--MMaarr--22000044 1122::4411:11199 LLCC//MMSS//MMSS #6 MRM of 5 Channels ES- 8.88 499 > 99 7.34e3 Area A 25 r 0 r abo abo eaM 2.00 4.00 6.00 8.00 10.00 Time Exvgon Reseach, 3058 Rasaazch Drive, State College, 7A 16001 Exygen Research, 3058 Research Drive, State College, PA 16801 CCHEOONNNNFEIDFPEIINNTDCIAOELU-NN- TSSTUYUIBBDJJIAEESCCTLTTRTITC0OT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7 -OOCRRV-DD1EE0RR.2E0E0NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00222244 au umorsssars 3M MN01539375 | PS QquuaannttiitfRyy eSSaaemmppll.ee RReeSppioorrNtte. 030504h, Bet.Date103/05/04, Amaiyetik.Risha PPaaggee 313133 TSSSaatarmumtpdplylmeeoNdoLL.iiTs:sittL::eId95:8B,WPio:\n\SDDeaMtacatarNa\o\L.L1C6:CH0MS3S1U0M3S51SE0364\3\AN4M,a4as6sssllE2y9yxm0nte8.x\D\FaFitlueuo:or0r3oo/cc0hh5ee/nm0ii4cc,aallsAs.n.PaPRlROyO\s\StSa:aaKmp.plRleieDsDahB\a\003300550044AA CCGG AACSSFTM Last modified: [2 Method= y Tat emoditiod: Last modified: HMPoo:nn\DDaMMataatarra\L1L165COMS11SM33SS:12632\8a:M14ad36sssl2$yy0900nm44x\Feluo\roFchelmiccuaaslos..PPrRROO\\oMMeecEtAhDDhIB\\CCeoottnGGrrooivvee Mon Mar 15 13:25:12 2004 IN~EPDDEESS 003311550044 PJroibntCeoddse: Tue Nar 16 07:36:37 2004 Printed: Tue Mar 16 07:26:27 2004 fr -- Name: 030504A-457 ! TTeexxtt=: 1: ce acid ben _ S-- i: C6 Acid PFHA ILL11995588--1177 RReepp,, DDFF==11000000 0;30504A-457 Sm (bn, 2:3) MRM of 5 Channol ES. | 030504A-457 Sm(Mn, 2x3) Eat1 S2O6e0 1( wl ea Nn | An o 2h "m 500 TTae b To Me 2.00 4.00 2. co ncid pron 2: C8 Acid PFOA 986.1171- - 6.00 8.00 1133--MMaarr--22000044 13:03:0]6 LLCC//MMSS//MMSS #6 MRM of 5 Channels ES- 313 > 269 3.32e4 Area PUSS \ 10.00 Time iLL11995588--1177 RReepp,, DDFF==11000000 00033000s550044A4-445577 Sm Sm (Mi, (Mn, 2:3) 2x3) |100!oAt a"c8z.a6o9g 102853~ 1133--MMaarr--22000044 1133::0033::006 LLCCl/MMSS/M/SM#S#t6 MRM of 5 Channels E5- MRM of 5 Channels ESper 413 > 369 Sates 5.3A`A1rreeea5al 1 ' 5% 3: cs sultonsee 2p.0r0es 3:C4 Sulfonate PFBS Pr4.0)0 50 B00 00 A Time 6.00 8.00 10.00 LL11995588--1177 RReepp,, DDFF==1I000000 030504457 Sm (Mn, 2:3) 030504A-457 Sm (Mn, 2x3) 100 | 072007 100~ N27 181520 sss agoasr wn SRA? 3 sf ~ 0"720.97 ~'" 1;61 2.22 3.38 4.094.57 { 1133--MMaarr--22000044 1133::0033::006 | LCIMSIMS. LC/MS/MS #6 RM of 5 Channels Es- MRM of 5 Channels ES- iy 931 ey \ ......... 7.58 /~ A195 1045 1179 10263 9;~19;56 10.46 299 > 99 11.79 1.68e3 E 99 S200S7 A17 |LaS 0 [\AAn3A OiUO bi~5~} b.'~ 7.1~7/\ 8.40 / ~ /~ ~ 250 0 5h sto i050 eee Tine 0 ....[ .... r .... i .... , .... , .... , .... * .... , .... , .... , .... , .... Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State Collage 7A 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00222255 _Mo1sa3Ts 3M MN01539376 | | SQQtuuuaannyttiiNffoyy.rSsLaa1ma9pp5ll3ee, RReSepeptoorrttNo.:030504A, Ext.Date:03/05/04, Analystik.Risha rPeaggee 313144 Study No.=LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst:K.Risha LSSaaasmmtppllmeeodLLiiifssitt::ed: NPoP:ni\\DDNaatatara\\L1LC5CMHS1SM3HS:S63E\3\M:N4aa6ssssl2ly0yn0nx4x\\FPlluuoorroocchheemniiccaallss..PPRROo\\SSaammpplleeDDBB\\003300550044AR CCGO AACCSSFTM | NMLLaeaattssrhttmoodaom:roddiitfiieedd:= M?MPoo:=n\\nDDMaaMttaaaarr\\LL11CC55MHSS11MN33SE:=6622\32\M::Ha14as26sssll22yy00r00n~44xx\\FFlluuoorroocchheenmiiccaallss.. PPRROO\\MNeStEhLDDBR\\CCoOtEGGrEoovVe NNPPDDEESS 003311550044 ab codes Last modified: Job Code: Mon Mar 15 13:25:12 2004 | pPertinncteead:s ue Mar 16 07:26:27 200 Tue Mar 16 07:26:27 2004 | Neaemer= 0w3o0s5o0n4nAe-a4s5t7 Text= 4: : C6 C6 sSuullffoonnaattee PpFrHsS {[L11995588--1177 RReepp,, DDFF==11000000 . __ 1133--MMaarr--22L00C0044M11S33M:00S35:0068 LC/MS/MS #6 030504457 Sm in, 213) vo MRoMf 5 Gramel 5- | 030504A-457 Sm (Mn, 2x3/ 0 EQ8.52 MRM of 5 38293-68003) Channels ES399 > 80 oa 2.36e3 |* , Area Raine O 26 pr) 6e 00 800 000 Tie Time 2.00 4.00 6.00 8.00 10.00 5[5:1:9CC58o8-sS1uu7llffRooennpaa,tteeDFPp=Fr1Oo0Ss00 13-Mar-2004 13:03: L1958-17 Rep, DF=1000 .003300550044AA--445577 Sm Sm (Mn, (Mn, 26) 2x3) M1R3-MMoafr-2LL0CCO0hl4aMMn1nSSe3/MlM:s0SS3E:S#0-66 a7 MRM of 5 49> 599 Channels ES- | 968.87 49598r>5e09a93) " Area|| ~ T 0J .... , ....20, 0.... , ....ab, o.... , ....6r 5, 0.... , ....85, 0.... , ....10,00.... , .... TTiimmee 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, 7PAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 1199339..00222266 SW_MNO1839577 3M MN01539377 | | SgQtuuuaadnnyttiiNfeyoy.sS,aaLmm9pp5ll0ee, RReSeepptoorrttNo.:030504A, Ext.Date:03/05/04, Analyet:k.Risha PPaaggee 111155 Study No.:LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst:K.Risha | eGSSLautaanrsmntptpolldmemesooddLLiiiiffssiitt::eedd:: MNPPoo2I:nn:\\\DDMDMaAaaatLrtraaa\\\1L1LL55CCCMHHS11SS33MHM::SSS326\S32\M\::MaM44asa66sssslsI22yl00yny00nxm44x\c\\FFFllluuuooorrroooccchhheeenmniiicccaaalllsss...PPPRRROOO\\\SMSaSamEmpLplDleEaD\DBCB\o\0tO3GI0r05oS0vO44eAANCPCDGOEASACCS0SF3FM1504 MLLeaatSshttodmm:ooddiiffiieedd=: Non Nar 15 13:25:12 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals. Mon Mar 15 13:25:12 2004 PRO\MethDB\CotGrove I~PDES 031504 Job Code: printed: Printed= Tae az 16 07:26:27 2004 Tue Mar 16 07:26:27 2004 NTNaaosmtaes:= 003300550044AA--445589 Text: I31::95Cc86o-1rA8eci,iddDFPvF=eH1nA000 L1958-18, DF=1000 i10e0303500540A4-445588 SSmm ((Mbnn,, 22x33)) %i| om mtr 25 abo 2.00 4.00 22L:1:9Cc58a8-AA1cc8ii,ddDFpPrF=oO1An000 L1958-18, DF=1000 |0o:3s0o5s004sA--a4s58s sm Sm un, (Mn, 263) 2x3) 100! * 10882.11098 1133--MMaarr--22L00O004M8 S113I3::M224S4::5516 MMRRMM ooff 55LCCChh/aMann33nSn11oe/33lMrlss>oS2EE2o6SS#69-d-69) Area 3.10e4 Area TT \ Time 600 800 1000 Time 6.00 8.00 10.00 10986.7871132 109832~ 7133--MMaarr--22L00C00M44 S11I33::M224S4::5#56561 MMRRMM ooff 5LGCCnh/aaMnn4Sne1el/3Mlss5$3EES6S#-9-~ 413 > 369 57r2e0a5 5.72e5 Area 0 Taw 400 2.00 4.00 3c[.L: 1a9C548-sS1uu8ll,tfDooFnnaa=ct1ee00Pp0FrBeSs L1958-18, DF=1000 [UA 8 0 a0 sm 001330000,550044A40-44855888 Sm Sm (Mn, (Mn, 253) 2x3) 100 0.68 wid VAINN Aa2 smse5 /~ 1.X45 2.16 2 93 ~ ~ / \ /~\ /~ ~ '~"1 4.26 503 600 6.00 some st 6.036.5 1 88.0000 000 10.00 -" TTiimmee| SN, Kon0N%IT0 TM ,|I L. 7.69 ~ WW 8'658 92 / ~ \/, 1133--MMaarr--22L00C0044M11S33M::22S44:56 MMRRMM ooff 55LCCChh/aMannnSn2e/elM9lssS>EESS#9--96 299 > 99 \10~21 ~0.56 | 1.50e3 11.~71 | | ol a 200 200 600 800 i000 i ............................... ] .... I ' ' ' ' I ' ' ' ' I ' 2.00 4.00 6.00 8.00 10.00 ' ' Time EExxyyggeenn RReesseesazrcchh,, 33005586 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00222277 SW_MNO1839378 3M MN01539378 ' | QBQeuuuaadnnyttiiNtfoyy..SsLaa1mm3pp5ll6ee, RneeSppetoorrteNo.:030504A, Ext.Date:03/05/04, Analysti.Risha Page 116 Page 116 Study No.:LI958, Set No.=030504A, Ext.Date=03/05/04, Analyst:K.Risha | vLSLSeaaaatssmmhttppollammeerooddLLiiiiffssiitte:e:dd:= oMPFPo:\nin\DD\aMWaLDaatarraa\\LtL11C55CaHMS\S11HM33LSS=1SC23623\H1:Ma44Ias66sNssLSl22yy00S00nm44\x\MFFalluusoorrsoolcchhyeemmniieca\allFs.i.FPRvRROOoO\)\MrSSAoaaEnmNcppDlhlBeee\DDCBnB\o\i0t03Oc30r05ao50v0l4e4AsANFCCDOGESAACCS0S3TF1HM508 MLTLeaaotasnhttocdmom=ocoada:iifeiseodd:: won War 15 13135113 2000 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 pJoebimCeoddse: Tue Mar 16 07:26:27 2008 Printed= Tue Mar 16 07=26=~7 2004 Nasa: 030504A-458 Name~ 030504A-458 Text= [44:L:1C9C56s8-sS1uu8ll,tfDooFnnsa=tc1ee00pP0eFnHsS 13-Mar-2004n13m:24:56 | L1958-18, DF=1000 1;030504458 Sm (Mn, 20) 1M3R-MMaorf-25LL0CCO0h/M4aMnS1nSIe3/l:MM2sS4SE:S5##-6~6] as 90>80 i EQ 21ar1e3a * Meee emANTAN O200r 00 p 500 e 800" n 05"0~," " " " .... TiO Time 2.00 4.00 6.00 8.00 10.00 55::Cc8o Ssuullftoonnaattee pPrFoOsS _ [LL11995588--1188,, DDFF==11000000 0305048458 Sm (Mn, 263) 11M33R--MMMaaorrf--252LL00CCO00hl4a4MMnT 1nSSe3/MlM:a2sSS4E:Sn5#-66 [1030504A-458 Sm (Mn, 2x3) 1s08.a28s38 MRM of 5 Channels ES- Cancels CancelE] s0Aere3a| 6.09e3 | of Area | | 200 00 600 800 e 00 r TTiimmee 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaa~tee CCoolllleeggee,, PPAA 1166880011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00222288 _MNO1S39379 3M MN01539379 1 | QQSuutaaundnyttiitfNyyo.rSSLuaimm5pp5ll8ee, RReeSppetoorrttNo.:030S04A, Ext.Date:03/05/04, Analyst.k.Risha rage 17 Page 117 Study No.=LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst:K.Risha LSSaaasmmtppllmeeodLLiiissltte::ds MPo:Pn\r\DNDaaatrtaa\\L1L5CCMH1SI3MN:SS36E2\\1MN4aassssl2ly0y0nn4xx\\FFlluuoorroocchheemniiccaallss..PFRROo\\SSaemmpplleeDDBB\\003300550044AA CCGO AACCSSFTM | MoMLLLeeabaatts"sshhtttoocddmomm::doooedddriiiftfilieeeddd::: WMPPoo:Inn\\DDMNaaaattrraa\\L11L55CCMH1S1S33MH::SS226\52\M:=Ma14as26sssl2l2y00yn00nx44x\\FFlluuoorroocchheenmiiccaallss..PFRROO\VMKeetEhADDBB\\CCoottGGrroovvee Mon Mar 15 13:~5:12 2004 NNPPDDEESS 003311550044 Job Code: I pPrriinmteesd:: Tue Max 16 07:26:27 2008 Tue Mar 16 07:26:27 2004 NNaamsea=: 003300550044AA--445599 Text~ 3i:: cC6e aAcciidd PmFmHA LL11995588--1177,, DDFF==110000 10p300y3500540A4-44559 Sm Sm (Mn, (Mn, 253) 2x3) 1 1007 i' |% 2586.111775-- m _ 1133--MMaarr--22L00O004M4 S113I3::M446S6::4#4666) MRM MRM of of 5LCCChh/aMann33nSn1e1e/3l3Ml"ss5>0SE02266#S695691I rAereaa | OB1 rrr /i 200 ~ 2.00-- 44.0000 a2L:1i9cC588e-nA4c7ci,adDwFPoF=O1rA00 rL1958-17, DF=100 0305044459 Sm (Mn, 253) 100, 030504A-459 Sm (Mn, 2x3) * | 200 pry 2.00 4.00 33:: CC44 sSuurlffoonnaattee PpFrBsS [1L915985-81-177,, DDFF==1I0000 {001330000550044A4-445509 SSmm ((MMnn,, 221x33)) " 6r00 rr 800 6.00 8.00 s88o.7711i 650 850 6.00 8.00 377.5509 1000 Time Time 10.00 1133--MMaarr--22L00C0044M11S33M::44S66::46 RMof MRM of 55LCCChhIaMann41nSn1o3e/3iM"l>ss>2SEE133S0S#66-8-996 "rea 4.21e6 Area | 000 TTiimme|e 10.00 1133--MMaarr--22L00o004m4 s113i3::m446s6::46 RM MRM of of 5LCCChh/aMannnSn22ele9lM91l9ss5S>>EE06SS#39-9-96] 6.1A5reea3) Area O |S nen r a---- Time 200 abo 500 500 1000 Time 2.00 4.00 6.00 8.00 10.00 EErxyyggoenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166680011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00222299 SW_MNO1839380 3M MN01539380 1 sere TE ra Quantify Sample Report Study No.=LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst=K.Risha Page 118 emt ers Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM 1 MeMLetatshhtooddm::odified:P:MP\o:Dn\aDMtaa~ara\\LL1C5CMMSS1HM3S:S6262\\=MM4aa6ssssll2yy00nn4xx\\FFlluuoorroocchheemmiiccaallss..PPRROO\\MNeetthhDDBB\\CCoottGGrroovvee NNPPDDEESS 003311550044 En, in SE Last modified: Mon Mar 15 13:25:12 2004 Ha Job Code: ! PPrriinntteedd:= TTuuee MMaarr 1166 0077::2266::2277 22000044 Name~ 030504A-459 Text= 4:C6 Sulfonate PFHS fae rson smn |LL11995588--1177,, DDFF==110000 030504A-459 Sm (Mn, 2)2x3) | %] =se8.52 21 1133--MMaarr--22000044 1133::4466::446 os LC/MSIMS #6 dls MRM of 5 Channels ES- w5e) 399 > 80 1.43e4 =Area i | , .... , .... , .... , .... , .... ~ .... ~ .... , .... , .... , .... , .... rE 2.00 4.00 6.00 8.00 10.00 a : C8 Sulfonate PFOS Time l a2 sin 20 1LL11995588--1177,, DDFF==110000 030504A-459 Sm (Mn, 2x3) [ 5oe8.88 9171~ 1133-.MMaarr--22000044 1133::4466::44661 Ar LLCC//MMSS//MMSS##6~ MRM of 5 Channels ES- ui=h 499 > 99 4.68e4,Area TIT J | y here Time| 2.00 4.00 6.00 8.00 10.00 rae Sens, 309 nsec pio, sie Coie, Bn 6k Exygen Research, 3058 Research Drive, State College, PA 16801 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00223300 3M MN01539381 I pay Te es rare 110 Quantify Sample Report | LEE reson, we tecanea essen, rmipeemasane Study No.:LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst:K.Risha Page 119 sample Lists 7\outeNIEHEHSE apse aoroshemiceLe FRO\SRRASSILOTOS00 CSTE Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM La I MMLeeattshhtooddm::odified: MPPo::n\\DDMaaattraa\\LL1C5CMMSS1XM3S:S6262\\M:Ma4a6ssssl2ly00ny4x\nFlxuo\roFchlemuicoalrs..oPPRRcOO\\hMMeeetthhmDDBBi\\CCcoottaGGrrloovvsee NNPPDDEESS 003311550044 Last modified: Mon Mar 15 13:25:12 2004 Job Code: ' PPrriinntteedd:: TTuuee MMaarr 1166 0077::2266::2277 220D0044 | res seas Name= 030504A-460 Text= i: C6 Acid PFHA Ce ------ i LL11995588--1177 RReepp,, DDFF==110000 030504A-460 Sm (Mn, 2x3) | *1001 |1 OL ,,, 2.00 2: C8 Acid PFOA Cfuss.17 Rap, DF=ico L1958-17 Rep, DF=100 soso 405m in 253 030504A-460 Sm (Mn, 2x3) 00 ol ] ETE .... , .... , .... , .... 4.00 6.00 1133--MMaarr--22000044 1144::0088::33:3 LLCC//MMSS//MMSS #6 a NR ofS CrTopS5. 8.15 MRM of 5 Channels ES313 > 269 bi yore 2.07e5 iArea ~ | ~3 .... ~ .... E, .E..E. , .... , ...."" TTiimmee 8.00 10.00 o8855585.9794149 [Ermer 13-Mar-2004 14:08:33 LLCC//MMSS//MMSS ##66 WR of Cron 28. MRM of 5 Channels ESeS 413 > 369 44..3322e66: etArea oR aL _ | L200 2.00 3: C4 Sulfonate PFBS 440.000 660.000 T 880.000 11000.000 TTiimmee LL11995588--1177 RReepp,, DDFF==110000 e ro p ror Grama 5. 030504A-460 Sm (Mn, 2x3) .} I=. BTpiEcht 100 1133--MMaarr--22L00C00I44M11S44I::M0088S::33#396] LC/MS/MS #!] MRM of 5 Channels ES- 7.61 299 > 99 7.49e3 Area Is 4 L HE rT r2r00 r2e 00 e 6.00 t80o 0 p 10.00 s Tie | 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00223311 3M MN01539382 | qQuuaannttiitfyy SSaammppllee RReeppoorrtt Page 120 Page 120 | SSttuuddyy NNoo..::L1I1995588,, SSeett NNoo..::003300550044AA,, EZxxtt..DDaattee::0033//0055//0044,, AAnnaallyysstt:=KK..RRiisshhaa LSSaaaammtpplleemodLLiiifssitte::d:P:MP\o:Dn\aDtNaaat\raL\CL15HCSMSH1MS3S:S36\3\M1Ma4as6sssll2yy0m0nx4x\\PFlluuoorroocchheenmiiccaallss.PPRROO\\SSaasmppLleeDDBB\\003300550044AA CCGG AACCSFSM | MeLLeaattsshhttooddmmr:ooddiitfiioedds= MMPPeo:inn\\DDNMaAaaCtrraa\\LL11C55CHMS1S1M3M3S1S:326652\\1:aM14as36sas2Ll20y000yn44xm\Fxlu\orFocLheumiocazls.o.PPcRROOh\\MMeeetEnhhDDiBEN\CcCootatGGlrEoosvvee NNPPDDEESS 003311550044 Sab code: Last modified= Job Code: Mon Mar 15 13:25:12 2004 | eines: Printed= Tue Tue Maz Mar 16 16 0077::2266:=2277 22000044 | aNammee:~ 003300550044A3--46600 Text~ G0 [44c:L:e1Cc9s6s5u8sSf10 uu7ollftRnooesnnpaa,etc0 eewDFePp=sFr1His0Ss000000000 13-Mar-0 2004 140 :08:33 L1958-17 Rep, DF=100 LCIMSIMS #6 13-Mar-2004 14:08:33] |o0a0o,so4n-460 sm vi, 2x3) 852 MMRRMM ooff 5LCCChh/aMa3nnnSn9ee/lMl>ssSE6S#.06 saat 39119.6r6>33e08ea404 IK Area | 1Or 200 a0 600 8A00 000 Tine Time 2.00 4.00 6.00 8.00 10.00 55[:L:1Cc98o58.sS1uu7llffRooonnpaa,tteeDFPp=Fr1Oo0Ss0 13-Mar-20045] L1958-17 Rep, DF=100 00:3035004A5-40604SS4mm(6(MMn0n,, 22533)) M1R3-MMoafr-2LL0CCC0hIl4aMMn1nSSe4I/lM:Ms0SS8E:S#363.|!#5 88 MRM of 5 Chann`el4s>E95S99-]I || 100! 988.3887 494s9.tgA>rele9ed49a! "> Area o%0t .... 200 am 660 8009837~ 10r00 eper Tie| 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166680011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00223322 SW_MNO1839383 3M MN01539383 ' | QSQtuuuaadnnyttiiNffeyy.:sSLaa1mm9pp5ll8ee, RReSepeptoorrttNo.:030506A, Ext.Date:03/05/04, Analyst:K.Riska PPaaggee 112211 Study No.=LI958, Set No.=030504A, Ext.Date:03/05/04, Analyst:K.Risha | eLLSSaareassmmrttppemlldmeoe:oddLLiiiifsslittee::dds: PNPro:\n\DDaNatatara\\LL1CC5HMSS1H3MS:SE36\3\M1Ma4as6sssll2y0yn0nx4x\\FFlluuoorroocchheenmiiccaallss..PPRRoO\\SSSammppLleeDDBB\\003300550044AA CCGO AACCSSFTMH MPEo\nDAMLaAr\L1C5ME1N3S:22N:a4a6s12y0m0x4\Pluorochenicala. PRO\NAERDE\CotGrove NPDES 031504 MLFLeaoatSnshttocdomm:dooeddriiffiieedd:: Non Nar 15 13:35:13 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2D04 NPDES 031504 Job Code: I eeinteas Printed: Tue Tue Max Mar 1166 0077::2266::2277 22000084 to aTNammeae:: 003300550040AA--446611 Text: 3i.:cCe6 aAcciidd pPeFuHrA _ i || LL1199s588--1188,, DDFF==110000 ph00r33ee00]55g0044A44-46611SSmm (Mn, (Mn, 2:9) 2x3) La we 10n_ } . 1T3-MEarT-2L0O04M1S4I:3M0#:S19 2880.1113s51 NRof MRM of 5LhCCho/MamnSnee/aMsl.sSE2S5#6-60- 3131>7820659) 1.78e5 Area ~ | oo0J,,~.-~'~--, 200 .... , .... , 430 .... ~ .... , ...6.50, 0.... ~ , 2.00 4.00 6.00 22::Cc8o AAcciidd pPrFoOnA [LL11995588--1188,, DDFF==110000 003300550044A4-446611 SSmm ((MMnn,, 22:x33)) 100, ) J 800 E10E 00 T Tine , i, ,-, , .... , .... ~ ....~Time 8.00 10.00 1133--MMaarr--22L00C00I44M11S44I::M33S00::1#1959 e888.77511 9 MRM MRM of of 55LCCChh/aMann1nSne3e/lMl>ssS3EE6SS#-9-6 asses 413 > 369 Area 3.95e6 Area 1 22.0000 44.0000 331::95CC84t-1sS8uu,llffDoonnFaa=tt1ee00PpFrBesS IL1958-18, DF=100 |!00.3300550044A7-445611 Sm Sm (Mn, (Mn, 2x) 2x3) _66..0000 800 795459~ 8.00 775.846111 1100.0000 Tim|e 1133--MMaarr--22L00C004/4 M1144S::/3300M#::S119 MMRRMM ooff 55LCCChh/aMann2nSne%/elM9lssS>EE5SS#-96- 29693>76939 ea 6.37e3 Area tN | r r s m eM AA 22.0000 400ew 4.00 6.00 sw 8.00 do 10.00 |re)| 7) Time~ ESxxyyggeenn RReessseaarrcchh,, 33005586 RReesseeaarcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 1199339..00223333 SW_MNo1S39384 3M MN01539384 -- -------------------------------- ' ) QSguuhaadnnyttiisfWyey.isSLaaim5pl5lese,RReeSppeooesretNo.:020504r, Ext.Date:03/05/04, AnalystiX.Risha PPaaggee 112222 Study No.:LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst=K.Risha CSSaaarmmtpplleemodLLiiitssitte::a:Po\P:Dn\aDtWaeat\raL\CLisCHMSS1UM3SS1E62\3\M1Ma4as8sssll2yy0m0nxsx\\FFlluuoorroocchheenmiiccaallss..PFRROO\SSS~EmppLlAeDDBB\\O03300S5O044AA CCGG AACCSSFYM 1 MMLTLLeaoeaatsbtsshthttoocddmomm::soooedda:itifefiiieeeddd::= won War is 13135113 2004 MPPo::n\\DDMaaat~raa\\LL1C5CMMSS1NM3SS=6262\\=M4Ma6sasl2sy00ns4x\lFylunorxoc\heFmlicualos..rPPRRoOOc\\MMheettehhDDnBB\\iCCcoottaGGrrloovvsee Mon Mar 15 13=25:12 2004 NNPPDDEESS 003311550044 | etotear Job Code: Printed: Tue war 16 07:26:27 2004 Tue Mar 16 07=26=27 2004 p-- i TeNTaexmxtet:== 0 30504hAese-461 4: co sulfonate pons 4:C6 Sulfonate PFHS | 1L9159858--1188,, DDFF==110000 yo | 0305044461 Sm (Mn, 213) 030504A-461 Sm (Mn, 2x3) | 1 |* sn8.52 33336666.~ 1133--MMaarr--22000044141:43:03:01:919 LomsiMs LC/MSIMS #6 MofR 5ChaM nnels ES- MRM of 5 Channels ES- 566a0 3919.5>5e840/ ea 1.55e4 1 Bl | {| pr 200 , , ~ 400 .... ~ .... ~ 50 .... ~ .... ~ 800 .... ~ .... ~ E 1000 E .... = .... = .... Tee lime J 5: co sulfonate 2p.0r0os 4.00 6.00 _ 8.00 I 0.00 oo [|5LL:1198C55888-.S11u88l,,fDDonFFa==t11e0000PFOS -- 1133--MMaarr--22L00O00M44S114I4::M3300S::11#9961) 1030504Sm4(8Mn1, 263) MofR 5LCCr/aMM nSe/MsSES#.6 || 100, 030504A-461 Sm (Mn, 2x3) E88S.8888 MRM of 5 4004 "4>9999) Channels ES499 . 99 I 4 56e4 0~ fd = *% 200 200 00 ao i000 1 , , , , .... , .... , .... , .... , .... r ....~, , ,-,89, 6, 8, ~-, -, , ~ rr , , , r --~TTiim Amreee.a, 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00223344 M_MNO1S39385 3M MN01539385 1 | QQSutuauandntytiiNfeoyy.iSsLaaimm3pp5ll8ee,RReeSppaootrrtNto.:030S04A, Ext.Date:03/05/04, Analyetsk.Risha PPaaggee 112233 Study No.:LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst:K.Risha [I LLSSaaaassmmttppllmmeeooddLLiiiiffssiitte::edd::P:MoPP\oI:nDn\\aDDtAMwaaCaat\arraL\\LC11LCH55CHSMSNS11NS33MS::ES32\6\32\MM1:Ma44asa66ssslsl22y00ysn00nx44lx\\FyFilunuooxrro\occhFheelmmiiuccaoallzss..oPPPRRcROOOh\\SSSeaaEmmnhppDlliEee\DDcCBBaAo\Ot0l3G30r0sSo5Ov0.4e4AANPCCDGOESAACCS0S3FF1M504 LaMLeaabtsshttocdomm:dooeddriiftiieedd:: Hon War 35 13133013 2004 P:\Da~a\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25=12 2004 h-PDES 031504 Job Code: 1 princes Tue Max 16 07:26:27 2004 Printed: Tue Mar 16 07:26:27 2004 Nama: 030504A-462 Name~ 030504A-462 voText~ | i[3::L19CC5o68-Aa1cc7ti,adDFPpF=rH1aA0 | L1958-17, DF=10 (030504462 Sm (Mn, 2 63) ,1 030504A-462 Sm (Mn, 2x3) { | | o1 20. 0 2.00 | 2[3::LicCso8s8Aa4cc7iidd,DPpFFr=Oo1nA0 iL0310955084-1774,52DFS=m1(0Mn, 223) In030504A-462 Sm (Mn, 2x3) | 1 rr "200 2.00 3: Ca sulfonate pres {[LL:1199C55488--S11u77l,,fDDonFFa==t1Ie00 PFBS p0033o0055y0044A4-446622 Sm Sm (Mn, 253) (Mn, 2x3) 1 1O01 % 200 4.00 i} 440.000 soo8se.i12r7s 630 800 6.00 8.00 | 1133--MMaarr--22L00C00I48M11S44I::M552S2::112 MMRRMM ooff 5LCCChh/aMann33nSn1o0e/3lMl">ss>SoEE22sSS#6.0e-960. Area 1.93e6 ~ea 1000 TTiimmee 10.00 eo088i.771s1 t 131-3M.Marar--22L0000O44M1Sm4M:5S2T:12 RMof MRM of 55LCCChh/aMann4nSn1ee/3lM>lSss>sSEsE33eSS#66r-960-! roa 3.55e7 Area | 66.0%0 880.000 tee10.o00 Time | Time 1133--MMaarr--22L00C00M48S11I44M::5S522#::11622 7777.866338 MM RMoofR f 55LCCChh/aMM annnSn2e/elM0lss9SEE0SS#-9-6 556d 299 > 99 177(~ rea 5.98e4 Area, Oh r2e 00 e <0 500 800 - 1000 Time 2.00 --~i , , ~ .... ~ .... ~ .... ~ .... i .... i .... i .... i .... i~, , , 4.00 6.00 8.00 10.00 Time EEexyyggeenn RReesseeaarrcchh,, 33005588 RReessseaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880013 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 1199339..00223355 SW_MNo1S39385 3M MN01539386 1 1 QSQuuaaanyntiitTfyy SsEaammppTllee RReTepEpoRorrNtto. o20s0sn, xt.Date:03/05/04, Aalystix.Risha Praaggee 112244 Study No.:LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst=K.Risha I aLLSSataaassmmht?ppollammeesooddLLiiiiffssiitte::edd:: MM7Poo:Pnnr\\\DaDMWataaateCrra\e\\LiL1L5sCCOMEHS11NS33MNS1:SS326E32\\Mi:MWaa4aase6sssssill22yy00ynm00nce44x\\\FFFllluuuoooFsroooccchhheeenrmiilccacalalsls.s..PPPRRROOO\\\MSSeaatmmHppOllRae\DDCBBO\\tO0G33E00o35v00S44AANUCCDGOESAACCS0SF3I1M504 oMLLeaabtsshttocdomm=dooecdritfeiteoda:: Non wa 15 1312311 2008 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 | eJroibncCeoad:e: Tue war 16 07:26:27 2008 Printed: Tue Mar 16 07:26:27 2004 same: 030500n-462 Uo NmTaeemxxett:r= 030504A-462 | 44[:L:fCce6eseSs1uu7ll,ffDoonFnaa=tt1ee0 pPrFHuSs L1958-17, DF=10 1(03002500540A4-446622 Sm Sm (Mn, (Mn, 268) 2x3) {1 Low] I ! | ol 200 200 2.00 5. ce suonate pros 4.00 5L:T9C388-S1u7l,fDonFa=t1e0 PFOS L1958-17, DF=10 [1007 [iw030504452 030504A-462 Sm Sm (Mn, (Mn, 263) 2x3) IE Iw | | ober LTT2.00E aw4.00 a20s85.5t043 500 500 6.00 8.00 Ao8.s8s8 500 - 500 6.00 8.00 _ 1133--MMaarr--22L00C008I4M11S44I::55S22#::11622 MRRMMooff 55LCCChh/aMannnSn3ee/lM9lss>SEES0S#-0-6) 391T9.a4r>s3oee8as50)! ! Area 000 10.00 TTiimmee| oTsroe 1133--MMaarr--22L00C00I48M11S44I::M5522S::112 MMRRMM ooff 5 hal ES. LC/MS/MS #6 5 Channels ES- 499 > 99 4.17e5 roa,| Area 000 Time 10.00 Time EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00223366 _MNO1S39387 3M MN01539387 i I QQSuutaaunndttyiiffNyoy.iSsLaaImmSppSllEee, RReeSppeootrrttNo.:030504r, Ext.Date:03/05/04, AnalystiK.Risha Page 125 Pag~ 125 Study No. :L1958, Set No. :030504A, Ext.Date=03/05/04, Analyst:K.Risha LSSaaasmmtppllmeeodLLiiifsstit::ed:?:MP\o=Dn\aDtMaaat\raL\C1LH5CSMNS1SM3S1S2\62M\1Ma4as6sssll2y0ym0nc4x\\PFlluuoorroocchheemmiiccaallss..PPRROO\\SSaammppLlaeDDBBA\G0I3O05S0O4AAA CCGO AACCSSFFM | eLaMLLeaaatbtssshhtttocodommms=doooeddd:iiiefftiieeeddd::: MPPKroo=\nn\DDaMaWaaatrra\\LL11C55CHMSS11HM33SS=1E22623\\=1MM41aa67ssssll22yy000m0n44xx\\PFlluuoorroocchheenmiiccaallas..PFRROO\KMeetthhDDRB\\CCoottGGrroovvee Mon Mar 15 13:25:12 2004 NNPPDDEESS 003311550044 Job Code= 1 pPrriinncteeds:: Tue Max 26 07:26:27 2008 Tue Mar 16 07:26=27 2004 NNr~ammaea:: 003300550044AA--446633 Text= 2I::cCe6 aAcctiad PseFwHnA | [LL11995588--1177 RReepp,, DDFF==1100 |ocos46o3u5nm un, 220) 1 [ECS 030504A-463 Sm (Mn, 2x3) 1007 no | ~ 1 | 0 ol 200 2.00 2: : cC8a AAcciidd pPrFoOAn [5L11995588--1177 RRoepp,, DDFF==1100 cs|oaosoan-aes 030504A-463 sm Sm vn, (Mn, 2:3) 2x3) = E[EE or 200 2.00 3[:1: 9cC5a48-sS1uu7llftRoaennpaa,tteeDFpP=rF1eB0Ss | L1958-17 03050474 Rep, 63 Sm DF=10 (Mn, 253) Oe | 030504A-463 Sm (Mn, 2x3) | 100! % | Ol , 200 .... , .... 2.00 E _ soa8a.172705 598295~ ~ 44.0000 6% 6.00 88.0000 Toso8t.7na1ro _ _ 1133--MMaarr--22000044 1155::1135:558e LCMSIMS LC/MS/MS #6 MRM of 5 Chomels 5: 31320026669, MRM of 5 Channels ES313 > 269 2.00e6 ven| Area 000 TTiimmee! 10.00 al 1133-MMarar--22L000O044MT1S5M:a1S3s:58 MRM of 5LGCr/aMnSn/iMsSES#.6 MRM of 5 Channels ES413 > 369 36507 3.65e7 Area Area to 600 800 1000 Timo Time 4.00 6.00 8.00 10.00 rea, 1133--MMaarr--22000044 1155::1133::5588 MRM of 5LLCCho/aMnmnSe/lMesSES5#-6 r87a.6z3e MRM of 5 Cha2nn62e99Sl9s75>E0S9909-9) 6.22e4 | Area RA rrr Time , .... , ......... ~ .... , .... , .... ~- .... ,,.,, ,.,, .--Time a0 so 800. 1000 | 4.00 6.00 8.00 10.00 Exygen Resessch, 3058 Research Drive, State College, PA 16601 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00223377 S3MW_NMoN10S135399338888 _-- i quantity sample Report sage 126 Quantify sample Report 1 SSttuuddyy NNoo..::LL1I995588,, SSeett NNoo..::003300550044AA,, EExxtt..DDaattee::0033//0055//0044,, AAnnaallyysstt=:KK..RRiisshhaa Page 126 Sample List: B:\Data\LCHSMSSWasslymc\iuorochesicals. PRO\Gasp1aD2\030S04A C3 ACS Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\SampleDB\030504A CG ACSFM fant moditied: Wen Mer 16 13133146 Fook 1 MMLeeattshhtooddm::odified: MPPo1:n\\DDaMata~ara\\LL1C5CMMSS1M3MS:SS262\\:MM4aa6ssssll20yy0nn4xx\\FFlluuoorroocchheemmilccaallss..PPRROO\\MMeetthhDDBE\\CCoottGGrroovvee NNPPDDEESS 003311550044 Tartmattetod: won War 35 33135133 2004 Last modified: Mon Mar 15 13:25:12 2004 a ceaes Job Code= printed rue war 16 07i36037 2004 Printed: Tue Mar 16 07:26:27 2004 [rp -- ` NTTaeemxxtet:=: 030504A-463 4: co suisonate pews 4:C6 Sulfonate PFHS 1 |LL11995588--1177 RReepp,, DDFF==1100 f0033o00,550044A7-446653 Sm Sm (bn, (Mn, 2:0) 2x3) volIe {I i 2062.00 5. co sulfonate ores 5:C8 Sulfonate PFOS LL11995588--1177 RReepp,, DDFF==1100 ||osos04n483 Sm vn, 230) 030504A-463 Sm (Mn, 2x3) ||100,103 | of 200 2.00 oo ho. 550 4.00 6.00 a 5% 4.00 6.00 ais8.5te4 308.00 7883.996007_ 508.00 ___ 1133--MMaarr--22000044 1155::1133::5588 LLCC//MMSS//MMSS##66 MRMof Channols E5- MRM of 5 Channels ES30> 0 399 > 80 io 1.39e5 oa,! Areai Ta00 Time | Time 10.00 1133--MMaarr--22000044 1i 5:13E :58 LLCC//MMSSI/MMSS #6 MofRGroM mnels 5.| 43605, MRM of 5 Channels ES449999>>9999 4.36e5 eal Area To00 Timo. 10.00 Exygen Research, 3056 Reseacch Drive, State College, TA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00223388 _Motsaoaes 3M MN01539389 | | QSQtuuuaadnnyttiiMffoyy.:SSLaa1mm3pp5ll8ee, RRSeeepptoorrttNo.:030504A, Bxt.Date:03/05/04, Analyst:X.Risha rPaaggee 112277 Study No..'LI958, Set No..'030504A, Ext.Date~.03/05/04, Analyst:K.Risha LSSaaasmmtppmlloeedLLiiissfttl=:ed:P:NP\o=Dn\aDcNaaat\raL\C1LH5CSMM1SS3MG:S2\62N\:aM4sa6sssl2ly0ym0ne4x\\PFilvuoorroocchheenmiiccaallss..PPRROO\\SSaammppLleeDDBB\\D0I300S5O0N4AA CCOG AACCSSITVHM | MoLLeaattsshhttomoddom:=oddiifflieedd:: PMNPioo:\nn\DDaNMacaatarra\\L1L1C55CHMSS11N33ME1:SS32652\\1:MK34aa36ssssll22y00y00nn44xx\\FFiluuoorroocchheenmiiccaallss..PPRROO\\MNeStLhADDBB\\CCoottGGrroovvee NI~PPDDEESS 003311550044 Fob Coda: Last modified: Job Code: Mon Mar 15 13:25:12 2004 I Psretinnttaeads: TTuuee MMaaxr 1166 0077::2266::2277 22000084 | Ne~mmeer~ 0o3a0o5s0o4Au-n4a6e4 Text: 1I:: cCo6 aAecsiad sPFmHnA | [JLL11995588--1188,, DDFF==1100 Cs003300550044AA--446644 Sm Sm (Mn, (Mn, 233) 2x3) % |-- { 200 2.00 2[.L: 198C586-AA1cc8ii,ddDFPpFr=Oo1An0 L1958-18, DF=10 G00o33e00s550044A7-446644 SSmm ((MMnn,, 221x33)) a0 4.00 _ -- so88e.11s77ta 56.0000 800 8.00 eca2Cna8nec0 1133--MMaarr--22000044 1155::3355::5511 MRMof LLCCCh//aMMnnSSe//lMMsSSES#-6 MRM of 5 Chan33n11e33l1>s.>9E9220S6669-9]) ea 1.99e6 Area | 10.00 Time Time | 10.00 _ 1133--MMaarr--22L00C00I44M11S55/::M3355S::5#5115 MRM MRM of of 55LCGCnh/aMann4nSn1ee/l3Mlss>S3E56S#-9-6 413 > 369 35a7o0a7 3.57e7 Area | 200 400 2.00 4.00 3: [3L: 1 9cC5a48-sS1uu8ll,ffDoonnFaa=tt1ee0 PpFrBsS | L1958-18, DF=10 10o3003n500540A4-445644 Sm Sm (Mn, (Mn, 253) 2x3) % 66.0000 88.0000 T77e.6i66337 7000 TTiimmee 10.00 1133--MMaarr--22L00C0044MS115I5::M335S5::5#5111 MMRRMM ooff 55LGCChh/aMannSnn2e/oMl0ssS9EE5S#9--6 29G69a.4et>1eae9dl49) Area | Ere terre pee Tie 0~, ,,,~ .... ~ .... , .... , .... , .... ~ .... , .... , .... , .... ~ .... ~ Time L 200 am 500 800 1000 2.00 4.00 6.00 8.00 10.00 BExxyyggeenn RReesseeaasrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHGEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00223399 SW_MNO1839390 3M MN01539390 I coms sete ser ran 0 Quantify Sample Report Study No.=LI958, Set No.=030504A, Ext.Date:03/05/04, Analyst:K.Risha Page 128 HELE. PTE esto AAT HEN 99 EY Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\SampleDB\030504A CG ACSFM Last modified: Mon Mar 15 13:22:46 2004 EE Method: P:\Data\LCMSMS6\Massllnlx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Last modified: Mon Mar 15 13:25:12 2004 Job Code: Printed: Tue Mar 16 07:26:27 2004 Name= 030504A-464 Text= : C6 Sulfonate PFHS fT emme eams L1958-18, DF=10 {i A wnar SS 030504A-464 Sm (Mn, 2x3) [o3e vst wTe= ] 2081.5543 13-Mar-2004 15:35:51 LLCC//MMSS//MMSS##66 MRM of 5 Channels ES- 319.950>e58|0 i .... , .... ~ 2.00 RT 5: C8 Sulfonate PFOS t; oe man200 LL11995588--1188,, DDFF==1100 , 030504A-464 Sm (Mn, 2x3) 1~ mE Toe 2915~~ 1.50eSArea .... ~ .... ~ .... , .... ~ .... ~ .... ~ .... ~ .... ~ .... Time 4.00 6.00 8.00 10.00 EwoS8.90 1133--MMaarr--22000044 1155::3355::5511 LLCC//MMSS/M/SM#S#t6 ue 2 MRM of 5 Channels ES=on 499 > 99 3.95e5 | Area EEE Tone 2.00 4.00 6.00 8.00 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00224400 3M MN01539391 | J-- Quantify Sample Report Page 125 Page 129 Study No.:LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst=K.Risha Sacple List. B.\DALa\LOUSMS\Massiyne\FiuPoROr)oSsamhpleenDBl\c03a0lSOs4.A CO ACEP Sample List: Last modified: Hathoss ERoata\ HENS Wags1yoe\FiuorocRhO eMeahiOBcCaotlGrsov.e ODES 631504 Method= Tart mbaicions men Har Bo Tosti is 1308 Last modified: EY Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13:22:46 2004 P:\Data\LCMSMS6\Massllrnx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 MOn Mar 15 13:25:12 2004 Printed: Tue Mar 16 07:26:27 2004 Name: 030504A-465 Text: i: C6 Acid PFHA ( [L e495~ 8-49,; DDFF==11000000 00p3300o55004A4-446655 Sm Sm (in, (Mn, 20)2x3) 1 | rp 2b2.00 2: cs pci pron (b 2LL:4-t99C58988=A1~c99i,,dDDFPFF==O11A000000 0305044S6m5 (Vn, 240) 030504A-465 Sm (Mn, 2x3) 100 |" re 22428 1133--MMaarr--22000044 1155::5577::4400 LCMSIM#S6 LC/MS/MS #6 MoR f 5 GrM ane 5- MRM of 5 Channels ES- esas 3136B..>44d42ee6d49. eaArea i a0 abo T50 a-- reneTH Time 4.00 6.00 8.00 10.00 Tahnits8.71 124346 1133--MMaarr--22000044 1155::5577::44(0 LLCC//MMSS//MMSS #6 MRMof 5 ChanneElSs- MRM of 5 Channels ESa5 200 413 > 369 Gsies 6.A5r4eea5l Area 75% Ww 0) We 00~'~,~ ~-, , .... qT-".... , .... 2.00 4.00 6.00 8.00 = 10.00 TTiimmee| 313.:6C40SSnuilffqounattee DPEFBSE cr -- --------TT-- (D |~ #958<, 19, DDFF==11000000 | | 10003300550044AA--446655 SSmm((MMnn,,22xx33)) | %1001 1133--MMaarr--22000044 1155::5577::40 LLCC//MMSS//MMSS #6 "MMRRMMooff 5 CChhaannnenlseEElSSs-- 783 299569 7.63 299 > 99 Ti e2r6e3a 745 3.62e3 o IN6A NAkoNA n he o e 550 AA ooA o Ame, Time 2.00 4.00 6.00 8.00 10.00 uISe- 20 fp Kosi Enyaen Research, 3058 Resasseh Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 HE`CNOCNNOEFIPNDIEFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIEAESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00224411 au_mnorsasss 3M MN01539392 | | QSQtuuuaannyttiiNftoyy.rsSLaa1mm9pp5ll3ee, RReSepeptoorrttNo.:030504A, Ext.Date:03/05/04, Analystik.Risha PPaaggee 113300 Study No.:LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst=K.Risha | LNLSSaaaeessmtrttpnlloemmeaooddLLiiiiffssiitt::eedd::7:MFNP\ooi:Dnn\\aDDtaMNaataat\arraL\\CLL11HC5C6HSMSMS11NE3M3SS::S3\2632M\a::aM44sas66ssssl1l2y2y0y0mm00nxc44x\\\FFFllluuuocorrroooccchhheeennmiiiccceaalllsas...PBPRRROOO\\\SNSaAamCmpHplDleEeD\DBCB\o\0t03G30r05o50v04e4AANPCCDGGESAACCSS03FT1MH504 MLLFeaaotssbhttocdmmo:oodddaiiffiieedd:: Non Nar 15 13:35:33 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 Job Code: Pprriinntteedd:: ue Mar 16 07:26:27 2004 Tue Mar 16 07:26:27 2004 NTNaaommtaes:= 030504A-465 030504A-465 Text= O44o: :Czc6oeSs,uullffDoonFnaa=tt1ee00Pp0FrHsS L--dgfiS=19, DF=1000 030604A-485 Sm (Mn, 2:3) | ro030504A-465 Sm (Mn, 2x3) % 4e2s9t8.54 4429| 13-M_ ar-2004 15:57:41 1M3R-MMaorf-2LL0CCO0h/4MaMnS1nSIa5/iM:M5sSS7E:S4#-06 MRM of 5 3%219>0840, Channels ES399 > 80 Areal 2.'19e4 Area Brrr rrr~BeLnt ~ in| O pr r rp200mer30p 0 rm6e 00 rrr 5.0.0.o.. e~e,10~ 0n 0, e~ s ive Time 2.00 4.00 6.00 8.00 10.00 55::CC8o sSuullffoonnaattee pPFrOoSs 0 L-1998-~,, DDFF==11000000 1133--MMaarr--22L00C00I44M11S55I::M55S77::4#4060 1030504465 Sm (Mn, 263) 100, 1 030504A-465 Sm (Mn, 2x3) 820 MRM MRM of of 55LCCCah/MannnSn1ee/5Mlls9S>EES0S#-9-6 0%8.90 1500 499 > 99 al| rea 1.59e4 Area { 202.00 44.0000 600 800 1000 .... , .... , .... , .... , .... , .... , .... Time 6.00 8.00 10.00 L19%- 20 @Eolilol EExxyyggeunn RReessseaarrcchh,, 33005588 RReesseeaarcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00224422 SW_MNo1839393 3M MN01539393 -- Quantify Sample Report yose 372 Page 131 Study No.:LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst=K.Risha Sample List: 7r\bute\LHONSE assimFisorochenicaleFRO\SRSELEOP\ASOSONA C3 ACEP Sample List: Last modified: ads Ha aestwas om\iuosochestcnts. PRO\WACIDR\Cotzove ODES 031504 Method= Last modified: wa Job Code: P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\030504A CG ACSFM Mon Mar 15 13:22:46 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25:12 2004 Printed: T1/e Mar 16 07:26:27 2004 Name= 030504A-466 = Texts i [L~ 4: 9C5684A, 9c,idDDFPFF==H11A0000 c5so4s66oSmt(inn, 2:8) 030504A-466 Sm (Mn, 2x3) 1 [|I * To2.00 Pp 2: 08 Acid PFOA os%0s04n455 5m (i, 29) E~r,eDsF,=D1F=01000 i 030504A-466 Sm (Mn, 2x3) |* pros 4.00 or8.17 118811E689 oo } 1133--MMaarr--22000044 1166::1199::2255] LLCC//MMSS//MMSS ##66I MRMof Grmele 5. MRM of 5 Channels ES~ Togo 31344.>.77222e6e5.~~ podArea. wm 5!0 Tosre Tine 6.00 8.00 10.00 Time o8oi.7n1s 1133--MMaarr--22000044 1166::1199::2255 LLCC//MMSS//MMSS #6 WofR5 haI mmels 5. MRM of 5 Channels ESTe 413 > 369 a 4.98e6 eeArea. po) pr) o ow Tow b , .... , .... ~ .... , .... , .... , .... , ....96, 3.9.1.3.~ , .... , .... , .... TTiimmee 2.00 4.00 6.00 8.00 10.00 3:C4 Sulfonate PFBS 0u3s 050454m68n, 2:5) () |Lc'lere3s5e8==tteg,, DDFF==110000 030504A-466 Sm (Mn, 2x3) | % 7a RMof 5Lhoamrsioeves=ls5s. 567.7663 1133--MMaarr--22000044 1166::1199::22-5 LC/MSIMS #6 MRM of 5 Channels ES- 229.291.18>8ee9449| Area i YT) a aA50 Too 0- ,~-~,, ,-, ;-, . , i . ..... ~ .. ... . ~ ... .. . i , , .~ .. ~ ". I ' ' ' ' I ' ' ' ' I ' ''-' -'~' ''' - Time 1156-20 @ BK fel 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 GFEOANNERFI ICDOUE-NNTSYUTBDJIIESCATTRITC0TAPCROOUTRETCNTGI.V2E7OGRunOiEoR26E8N0T3ERED CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00224433 swNos39394 3M MN01539394 QSgutuauandntytiiNfsoyy.1SSLaa1mm3pp5ll8ee, RReSepapocorrNtto.:030504A, Ext.Date:03/05/04, Analyst:X.Risha PPaaggee 113322 Study No.=LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst=K.Risha NLGSSaaaeatssmmhtptpollamemerooddLLiiiiffssitit:e=edd:: MMPPeoo=P\nn\D:DNMaa\aattrrDaa\\a1L1L55tCoMxaS11S\3M3s5:SLE326C32\H1=MMa44as66SsssMl22S00yy00n644x\\mFMlxauosr\soclFhyemmlicecaua\llFssc...lPPPuRRRFOOOo\\\oxSSMaaEomCmcpcHpLDlhheBeeD\DBCBne\O\i0t03nG3c0z0aSo5i0v0l4e4sAANCECDOGESAACGS0F3S1M504 MLLTeaaotsnshttocdmmo:otoead:tifeiteedd:s hon Har 15 13133113 2008 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 NPDES 031504 Job Code: sPrriinntteeads= Tue Max 16 07:26,27 2008 Tue Mar 16 07:26:27 2004 NsTaaemmxeet::s 003300550044A2-445666 Text= 44L::isCcs6o8.sS3uu9ll;ffDoonnFaa=tt1ee00PpFrHsS _ !L1958=-1~, DF=100 0305044465 Sm (in, 2:5) 100,1 030504A-466 Sm (Mn, 2x3) *100! | 200 abo, 500 2.00 4.00 6.00 5: ca sultonate pros 0 , DF=100 5:C8 Sulfonate PFOS L-C958,A~, DF=100 10p03300550044A4-446865 Sm Sm (Mn, (Mn, 29)2x3) | % a48s2,51t40 42130~ 008.00 20888.599007 .13-Mar-2004 16:19:25 1M3R-MMoafr-25LL0GCO0h/4MeMnS1SnI6/oM:Ml1SS9E:S#2#.556| MRM of 5 Chann33e992l9s0>>0680500] real 2.03e5Area Too Time 10.00 1133--MMaarr--22L00O0044M11S66:M:119S9::22:5 MRM MRM of of 55LCCChh/aMannnSnoee/lMlssESE>SaS#-r-6] 499 > 99 T4`0r0e5a 1.49e5 Area 200 00 600 500 000 Tim|e 2.00 4.00 6.00 8.00 10.00 -, .., Time 0145-20 @ Kali ESxxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarcchh DDrriivvee,, SSttaattee CCoollllaeggee,, PPAA 1166880011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00224444 M_MN01S39395 3M MN01539395 QQSuutaaunndtytiiNtfoyy. Ss1a1a1mm9pp5ll8ee, RReeSppetoorrttNo.:030504A, Ext.Date:03/05/04, Analyst:K.Risha PPaaggee 11333 Study No.=L1958, Set No.=030504A, Ext.Date=03/05/04, Analyst:K.Risha LSSaaasmmtppllmeeodLLiiifssitte::d:PrMP\o:Dn\tDNaaa\traL\CL1H5CSMH1SSM3SS.\63N\3aMs1as4slsyl2my0x0n\4x\lFuluoorroocchhaenmiiccaallss..PPRROO\\SSaammpplleeDDEB\\003300550044AA CCGG AACCSSFFM NMLLoeaattsshhttooddmm::ooddiiffiieedd:: HMP5eo:\nn\DDnMNatataaar\\LL11CC55MHSS11MH33SS1:632\\52MN1=a1a4s36ssal2l2y00y~00mI41\xF\uFolruoorcohcehneimciaclasl.s.PPRROO\\KMSeLthhDDEB\\CCoottGGzroovvae INPDDEESS 003311550044 Tob Goda: Last modified: Job Code: Mort Mar 15 13:25:12 3004 PPrriinntteedd:: TTuuee MMaaxr 1166 0077::2266::2277 22000044 NNaammee:: 003300550044A--448677 Text: 1:: cco6 aAccitda pPFrHaA oF , E't998,.-Z~, DDFF==11000000 101300030.50)0540A4-446677 Sm Sm (Mn, (Mn, 263) 2x3) ioo *% 11IA ~2: ca Acid pron 22.0060 2: C8 Acid PFOA {eL-s-'IeJo58~ZsOD', FD=F1=1000000 00;330055004A4-446677 Sm Sm (Mn, (Mn, 243) 2x3) 10 I _ 10885.11996] '10596~ 1133--MMaarr--22L00C00I44M11S66I::M441S1::1#1555] MRM MRM of of 55LGCCrh/aMann3Sno1e/lM3las5S2EES6S#-96~I 313 > 269 26e70a4 2.87e4 200 EE 600 ~800 000 a\ Te 4.00 ~,~\ Area ' '6.0I 0'' ' ' ' I ' ' ' 8.0I 0'' ' ' ' I ' ' ' 1'0.00' ' ' ' ' ' ' ' ' ' m me 108670158 1089.7615 8~ 1133-.MMaarr--22L00C00I44M11S66I::4M41S1:1:15#55 M MRMoofR f55LCCGhhlaM Mann44nSna13e/l3MSsl5s>oSEEc33SeS8#6-06s-9II! rea 5.69e5/ Areal fa wa,~ Ha | ola Be Time | /0l,~--~-~, ~ .... -- .... ~ .... ~ .... ~ .... ~ .... ~ .... ~ .... ~ .... ~ .... ~ .... - Time 200 50 650 850 000 2.00 4.00 6.00 8.00 10.00 3: co sulfonate pres _ 3:C4 Sulfonate PFBS |L1358-20, DF=1000 73-Mar-2004 16:41:1 ~, DF=1000 |0o3o0s5o0s4sAa-4a6r7 SSmm ((MMnn,, 22xx33)) | 13-Mar-2LL0CC0I/4MM1SS6IIM:M4SS1:1#56 MMRRMM ooff 5 CChhaannnneellss EESS-- 1 ~ 0.62 [loot 120 276 37030 | wl VAAN 5.11 Ji sPas I azn N7a.s4e2/. 7.6|3WNA21!1AN99.0S0N88 I09..4444AE1100.3B 5308107.7wK 77 b21a91r1.9e6.n20>8e939 { 200 2.00 abo 4.00 500 6.00 800 8.00 1100.0000 Time OLrst-1Eesluled EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaazrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166080011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 1199339..00224455 SW_MNO1839396 3M MN01539396 J -- page 134 Quantify Sample Report ETB Rt he. cos0s0th, mvt. oacer03/05/04, Amatyeor. nish Study No.:LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst:K.Risha Page 134 Sample List: Pi\Daca\LCHSKSE\Massiyme\PiRvOorSoancplheeDBn\iG3cOaSOiUAs C3 ACS Sample List: iti momen Te Taree ite Last modified: os pat Leubis assLyot\Fiuorachemicats .FRO\MOChDE\CokGrova DES 03150 Method: prog IE oes gr oo Last modified: te Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13:22:46 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25:12 2004 NT Printed: Tue Mar 16 07:26:27 2004 [E-- Name: 030504A-467 ft Text= 4: co suttonace seus _ _ 20, DF=1000 4:C6 Sulfonate PFHS L-19b'8:20, DF=1000 cjacsson457 Sm vn, 23) oEsA MRoMf GramSnoeFl55H55-0 030504A-467 Sm (Mn, 2x3) 1133--MMaarr--22000044 1166::4411::1155] LLCC//MMSS//MMSS ##66 8.52 MRM of 5 Channels IES~ 399 > 80 5.06e~ || % _ en~ 0' .... , .... ~ .... , .... , .... ~ .... , .... , .... , .... , .... , .... ~ .... Time ' 2% i Bs ab Tos 2.00 4.00 6.00 8.00 10.00 5. co sultomste pros 5: C8 Sulfonate PFOS oO ~ 1958-2, 6, DDFF==11000000 30506487 Sm n,23) 100, 030504A-467 Sm (Mn, 2x3) 1!1 O01 1133--MMaarr--22000044 1166::4411 3 : 15 LLCCI/MMSS//MMSS #6 VoR f ChaM mois 5- 888.88 MRM of 5 Chann44e99l9s9>E9S99-9) i a 6.49e3 =Area 1Or A me Time 2b a ab abs ET) 2.00 4.00 6.00 8.00 10.00 01458-14 lel Savon Research, 3058 Reseaceh Drive, State Colles, PA 16803 Exygen Research, 3058 Research Drive, State College, PA 16801 CCHEOONNNNFEIDFPEIINNTDCIAOELU-NN- TSSTUYUIBBDJJIAEESCCTLTTRTITCOOT AAGPOPURRROOTT.TEECNCTOTIIVV2EE7 -OO0RR1-DD1EE0RR.0E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00224466 Sw uotssssor 3M MN01539397 | | QqSutuuaadnnyttiiffoyy.rSSie1~m5pl5l8ee, RReeSppaootrrtNto.:030504A, Ext.Date:03/05/04, Analyst:K.Risha sage 123355 Study No.:LI958, Set No.:030504A, E~t.Date:03/05/04, Analyst=K.Risha SSSaaanmmtppllemeodLLiiifssitt=e:d:PiNP\o:Dn\aDtMaaat\raL\C1L5HCSMMS1EM3SS136\3\N1Ma4as6sssll2yy0n0nx4x\\PFiluuoorroocchheenmiiccaallss..PPRROO\\SSaazmppLleeDDEBN\G03300S5O044AA CCGG AACCSSFFM MMLYeeaattsnhhtkoomddmo:=oddsiftiiendd:: MPMPoo=rnn\D\MMaaatDrraa\L31t55CMaS11\M33S::L32652\C:=M34aH36sSsl22My0900nS44x6\F\luNoraoschaemLicycaanllssx..PP\RROFO\\LNMeeuCthohDDxRB\\oCCocctthGGrreoovvmee NNPPDDEESS 003311550064 Ton coda Last modified= Job Code= Mon Mar 15 13=25=12 2004 PPrriinntteedd:: TTuuee MMaarr 1166 0077::2266::2277 22000084 NNaamsee=: 003300~50044An--446688 Text= I[1::XC0Cco6305Aa0cc4ia-d5,PoF5rH0nA0 ng/L Standard . XC030504-5, 500 ng/L Standard 10030003.50045A0-446484SS6mm8 (Mn, (Mn, 233) 2x3) 10 1 | "| 1133--MMaarr--22L00O00I44M11S77I::0M03S3:0:#506~5 7831635 MRMaf MRM of 5LCCChh/aMann3nSno1/elMl>ssSEE2SS#6--96 37005 7396 3.7Ar0eea5, Area! Io0 ,~'~-,,, ~ 200 .... r .... ~ 300 .... i .... ~ 600 .... ~ .... ~ B00 .... ~ .... ~ 1000 re .... ~ .... ~ .... - TTiimmee 2.00 4.00 6.00 8.00 10.00 22:: cCo8 aAcciidd PpeFoOrA -- X(CC003300550044--55,, 550000 nngg//LL SSttaannddaarrdd 1133--MMaarr--22L00O0044M11S77M::00S33::0055 030504468 Sm (Mn, 233) 100030504A-468 Sm (Mn, 2x3) 16886.0699996 MRM MRM of of 5LCCChh/aMann1nSne3IelMl>ssSEE3SS#6--96 85005 413 > 369 | = a 8.90e5 Area |A erepenerrpeeeer Tie 1~O!-~, , , ~ 200 .... ~ .... 2.00 ~ 400, .... ~ .... 4.00 ~ G00 .... ~ .... 6.00 ~ 500 ....16~ 5.9.9.6.~ ~ 8.00 000 .... ~ .... 10.00 ~ .... -Time 33: :Cc4o sSuullftoannaattee [XC030504-5, 500 sPneFgsB/sSL Standard _ _-- 13-Mar-2004 17:03:0: XC030504-5, 500 ng/h Standard 10305044468 Sm (Mn, 2x3) 1M3R-MMaorf-2LL0CCC0hI/4aMMn1nSSe7I/lM:M0sSS3E:S0#.56 10n0h, 030504A-468 Sm (Mn, 2x3) 2177.5%82 MRM of 5 Channels ES- 20592>30593) 299 > 99 `roa 5.23e3 Area || BEdre ene mn re Tine La 2.00 44.5000 606.00 80 8.00 1100.0000 Time EExxyyggeenn RReesseeaarccchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHGEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00224477 SW_MNo1839398 3M MN01539398 | | QQuuaannttiitfTyy sSaaE mmppilee SReRopep.oerrtososoen, mnt. ates03/05/00,Amaiyerik.mish sage 126 Page 136 SSESaaatmmsupptdllymeeoNsoLLt.iitss=ittLe::Id9:58,HP3o::n\S\DeDMtaaetsNato\a.L1\=5C0EM3S2M0M3S5SaS0634\sAMaa,assssilE3Fy0xm0tn4.xlD\aFtuleu:oo0r3o/sc0h5eo/m0i4cc,alhAsn.FaePRlROyOs\s\StSs:iaKmm.ppcRlLieasaDDhBNa\0l02300s5500.44A8 CO CG ACS ACSFM Last modified: Sathosr Method= Treynt meditiad Last modified: HFoan tWaat\ LTo E3S45W1a3g 2y0m04 FLuoroches cals.FROWSCIDE\GotGrove Mon Mar 15 13:22:46 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mort Mar 15 13:25:12 2004 N~FPDDEESS 003311550044 PJorbinCtoedde: Tue Mar 16 Gazer 2004 Printed: Tue Mar 16 07:26:27 2004 Name= 030504A-468 4T:extc=s suitonate sre : C6 Sulfonate PFHS XXCC003300550044--55,, 550000 nngg//LL SSttaannddaarrdd 30p300y55004A4-4A648 S6Sm8m (in, (Mn, 230) 2x3) 11 %l 1133--MMaarr--22000044 1177::0033::0058 LLCC//MMSS//MMSS ##66 MRMof 5 Cranes 5- MRM of 5 Channels ES- 052 Seh550 8.52 399 > 80 zn Tres 1.17e5 eaArea | Tine 01 ' ' ' ' 1 ' ' ' ' i ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' 1 ' ' ' ' I ' ' = ' I ' ' ' ' I ' ' ' ' I ' ' ' ' 7% pr) PY) W Tom 2.00 4.00 6.00 8.00 10.00 Time 5. ca suisonate pros 5: C8 Sulfonate PFOS XC030504-5, 500 ng/L Standard 0508-455 5m 4, 23) 1 1I~0300,1~0-44:~'S 5rn0;M ~i~3~tandard 111886~.869897711 1133--MMaarr--22000044 1177::0033::0055 LLCC//MMSS//MMSS #6 MRM of 5 Cramos 5- 6.2404] MRM of 5 Chann44e99l99s >>ES999-9| 6.24e4 reaArea | y 7% ww o% PI) Wo Time | 2.00 4.00 6.00 8.00 10.00 Time Savon Research, 3058 Rosaasch Drive, State College, PA 16001 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00224488 au_Notsassss 3M MN01539399 i | QQSuueaaenndttyiiwfteyy.1SSiaaimm3pp8llsee, RReSepaproorrttNo.:030504n, Ext.Date:03/05/04, Analystik.Risha PPaaggoe 113377 Study No.:LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst:K.Risha [I LSLSaaaassmmttppllmeemoodLLdiiiifssfitti::eedd:prMBoP\oo:nDn\\aDRtMHataataa\art\\LLLO11C56HMHSS11SM336SS1:\622M\32aWM::sa4a4ss6s6lssyl2y2my00mcn00c\x44\T\PlFhluuuooorrroooccchhheeenamiiicccaaalllsss...PPPRRROOO\\\SSNAaAzmEppRLlDaReD\DDCB\o\0t03G30E0SO5Dv04e4AAXPCCDOGESAACCS0F3S1M508 MJTLeoaatnnshttocdmom:sooeda:itftiseeda:: won maf 1s 1313501 2004 P:\Data\LCMSMS6\Masslyllx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25:12 2004 I~PDES 031504 PJrobintCeodd:e= Tue Mar 16 07:26:27 2008 Printed: Tue Mar 16 07:26:27 2004 maze: 030504A-465 ' NTTaeemxxett::: 030504A-469 A[i1:MeCtC6h6aAnAuoclliddWPaPRsFRMhRA Methanol Wash [ LOMSIMS: 003300550044AA--446699 SSmm ((MMnn,, 22xx33)) 100,) 202%5 To 269 100 l \ Toeiond ~ 1133--MMaarr--22000044 1177::2244::48 LC/MSIMS #6 MMRRMM ooff5 CChhaannnneellss EESS-- | 8.25 313 > 269 2030 1.64e4 P IN V AN\ /if [Em20i 0 ne 300 nt500 500 R 000 S .... I .... , .... ~ .... , .... , .... I .... ~ ....i.I.I.. ~ .... I .... ~ .... tATrimeae , 2.00 4.00 6.00 8.00 10.00 2: co acid pron : C8 Acid PFOA |[MMeetthhaannooll WWaasshh y0o3r0*504459 5m (Mn, 263) 2o54n3 MRM of 5 CraWn1e32s583E6S60-05 030504A-469 Sm (Mn, 2x3) 1133-.MMaarr--L22LC00CI00/M44MS11SI77/M::M22S4S4#::4#46868!i MRM of 5 Channels ES- 8.71 413 > 369 2.86e5Area ~ , | 0I 200 a0 "500 reneB 85002543j~e _ 0e 00 y e~- TT-iimmee 2.00 4.00 6.00 8.00 10.00 3. ca sutonase peas 3:C4 Sulfonate PFBS ! MM0e3ett0hh5aan0no4oll4WW4aS6asms9hh:(4, 2:3) v yop MRMGSCRamol ES. 1133--MMaarr--22L00C00I44M11S77I::M224S4::48 LC/MS/MS #6 , 030504A-469 Sm (Mn, 2x3) | 100I,02/ 1u08ss 5"1p aos 11 .22 1.08 2.12 am agesessaz ewo1o0 7r/.6e7\ae i8[B0, 0RsJnAmlhn a2nos9s9e 8.98 MRM of 5 Channels ES- 10.92 299 > 99 1.09e3 | of VYve ARB 3.05 4.36 RAR 4.68 5.42 6.40 SAN PAN 10.33 Tl .11.50 L 200 prs 500 800 1000, ! 2.00 4.00 6.00 8.00 10.00 Time xygen Resessch, 3056 Research Drive, State College, PA 16601 Exygen Research, 3058 Research Drive, State College, PA 16801 I `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00224499 _MNO1S39400 3M MN01539400 | ME rage 138 Quantify Sample Report |B I Ne ovosuan, Bes.pate:03/05/04, Anstyatik. aisha Study No.:LI958, Set No.=030504A, Ext.Date:03/05/04, Analyst:K.Risha Page 138 Semple List: \Dasa\ICHGS assLymn\risoroROc)hSaempnLatBEo\ds30l5O4s CO ACEP Sample List: Last modified: a evi haos oy\PHusrochentel.FROUHALADE\Cotarove NUDES 031504 Method: FR Last modified: Ee Job Code: P:\Data\LCMSMS6\Massly~x\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13:22:46 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25:12 2004 Printed: Tue Mar 16 07=26:27 2004 = Name= 030504A-469 Text: 4:C6 Sulfonate PFHS MMeetthhaannooll WWaasshh 030504A469 Sm (Mn, 233) : es eee 030504A-469 Sm (Mn, 2x3) ly wp A 32 I FL) ws 1 128 289 100~ 0.18 1.99 wr RN20 sza se "| sw 3 ~ 1.26 A 2.~89 328328 ..~"-'3.74 i. | 7.~8~'l' MRMof 5 ChanneElSs- 1133--MMaarr--22000044 1177::2244::48 LLCC/IMMSS//MMSS #6 MRM of 5 Channel8 E$- 707 5.22 6.0.5 / 8~5~0 Jy 9.~5/10:42J 11.7,'1399>88205\ 3 prey 0~ .... , ........ , , , , ~ , 2.00 4.00 5:coouitomste pros [5M:eCt8hanSoullfWoanasthe PFOS Methanol Wash } |Jocosoanss sm in. 2x3 030504A-469 Sm (Mn, 2x3) | |0 11 00..1144 A SRC sae, 1.47 1.81 ab , , ~ .... ~ , ,,, 6.00 sm2 stu 249 55.0099 .49 86.55117.07 woo oe , ~ .... , , , , , 8.00 10.00 , .... Time 1133-.MMaarr-.22000044 1177::2244::48 LLCC//MMSS//MMS8 #6 WER of 5 Channe5l I, MRM of 5 Channels ES- LE 17s Ege] LM ~/ RANRES WA 7.A75 8N.86T 10.44 499 > 99 \ 1111.a4221n17.7s5 998533 \ Io 35 i 5 a5 ioe Tene 2.00 4.00 6.00 8.00 10.00 Time Saran Reseaseh, 3058 Research Drive, State College, PA 16301 Exygen Research, 3058 Research Drive, State College, PA 16801 CHEONNNEFPIINDCOEU-NNTSTYUIBDJIAESCTLTRITCOTACPOURROTT.ECNTG.IV2E7-O0R1D1E0.R8E8N6T2ERED IN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00225500 su_woresosor 3M MN01539401 1 ---- [op Quantify Sample Report | TIE IE Te. cos0noun, awe. oucer03/05/04, Amalpati.nisha Study No.:LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst:K.Risha Page 139 Semple Lists Pi\Duta\MBISEWassiyne\Fisorochenicels.FO\SAIpLESR\ASOSOIA C0 ACEP Sample List: fre ph pg Last modified: | emt uheersomt\FisorFRoOcNAhLeADnNiCcoragrlovse MYLES OTIS0R Method: BE ttn Ss TT amet Last modified= nae os Job Code: P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13:22:46 2D04 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25:12 2004 Printed: Tue Mar 36 0726177 2004 Printed: Tue Mar 16 07:26=27 2004 sums: cresIn-470 Name: 030504A-470 = Text= 1: cs acid smn I: C6 Acid PFHA w Fen es L1958-21 |oscsoan470.5 0, 20) NROof Ghomelo 5. 030504A-470 Sm (Mn, 2x3) 1107, hi Eoei --SBeow| | +Le 13-Mar-2004 17:46:28 LLCC//MMSSI/MMSS #6 MRM of 5 Channels 313 > 269 1.57e4 AA Area | | or d e3 m it rea5 m T Ir) Toss \Tee 2.00 4.00 6.00 8.00 10.00 Time 7. cn seta ron I 2: C8 Acid PFOA Liossz1 Mar2008 17:46:28 L1958-21 | oisosotn5m4(7vn0, 2) MRMof Chomnl5s. 030504A-470 Sm (Mn, 2x3) Honz eieve 00 13-Mar-2004 17:46:28 LLCC//MMSS//MMSS##66 MRM of 5 Channels ES- 8.71 413 > 369 || + 1.17e5Area | do 2 prey oon 50 ios | 2.00 2: ca seitonsce pree 3: C4 Sulfonate PFBS TP 4.00 Tp 6.00 TTI IT er err 201~ 8.00 10.00 vite] LL11995588--2211 1 S04780 5m 0 (25) MRIof 5 Chamls 5. [0 or 030504A-470 Sm (Mn, 2x3) 0.74 Rearres wren me Sem2 pm Fie 100~ ~1.371.64 3 SW A 220s2083a0 sssatmasso A p5oRaRrnmL BMAVMNAAAS|| ~ ~ / \ ~/~ 2.80 3..Ol ~.8~4.~84.9o ~.74 1133--MMaarr--22000044171:7:4466::2218] LLCCIIMMSS//MMSS##66 I1 078gen 8M7R0M of 5 299>69) Channels ES299 > 99 ~ 7.82 8~ 1~0.52 11.19 1.16e3 ~, , , 1.~ | SE........................ ~ .... ~ .... ~ .... ~ .... ~ ------ a .... , .... Time | 35 pr) 13S a6 Too 2.00 4.00 6.00 8.00 10.00 Ergon Reseazch, 3058 Reseach Drive, State College, PA 16061 Exygen Research, 3058 Research Drive, State College, PA 16801 CHEONNNEFPIINDCOEU-NNTSTYUIBDJIAESCTLTRITCOTACPOURROTT.ECNTG.IV2E7-O0R1D1E0.R8E8N6T2ERED IN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00225511 su_woresoso2 3M MN01539402 I J sore 0 Quantify Sample Report Study No.=LI958, Set No.=030504A, Ext.Date=03/05/04, Analyst:K.Risha Page 140 A Sample List= rr ME rg Last modified= 0 erechniert moe casseoe Reo 5150 Method= IN Last modified: wa Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13=22:46 2004 P:\Data\LCMSMS6\Massllrnx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25=12 2004 Printed: Tue Mar 16 07:26:27 2004 ~am@= 030504A-470 Text= : C6 Sulfonate PFHS resszt L1958-21 -- 030504A-470 Sm (Mn, 2x3) po 016 10~r~ 0.16 072 239 i 2 J/~" 0/72,1.14 2.~39 swarmTas 13-Mar-2004 17:46:28 LLCC//MMSS/IMMSS ##66 Wo3 orafmi 5. MRM of 5 Channels ES- EE 838 870038 1027/7 A 847) a8 688 8.38~ ~W^ 9A.33 AA seinBsn200 SR ra,SAN \ 3.45 4.03 4~,8 5,~30 6.99 6.~88 Z.92~"~~ 11.00 fv 399 > 80 847 orH eRr ew r ae r hw Tee 2.00 4.00 6.00 8.00 10.00 J } 5: C8 Sulfonate PFOS Time LL11995588--2211 osuE'7S0 smi, 29) pt VR0oo%sf h1a5r0i8e5, 013050~4VA~-4710_4,~tl Sm (Mn. 2x3) [floss sarast? 42ssaralm A As E | 058 2.24 2893'~39 4.4~3 4.86 5.866.36 6;9,2 $'~|~ 8,50 1133--MMaarr--22000044 1177::4466::2288 LLColMmSs/mMsS ##66 9.58MRM of 5 Chann4e9l9s >ES9-9 10.8,6 1 . ,,> 1.02e3 ~ , / , ~ , ,/'/ Toa a eh io J ~ 0I .... , .... , .... , .... , .... , .... , .... , .... , , .... , ..-- .. , .... "TTiimmee | 2.00 4.00 6.00 8.00 10.00 Draen Roesch, 088 Rens rive Sate College 26883 Exygen Research, 3058 Research Drive, State College, PA 16801 B EE Cr h TH-- Cosme 5Ohne CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT. NO. 27-CV-10-28862 11993399..00225522 s_orszons 3M MN01539403 1 quantity sami Report rege 160 Quantify Sample Report 1ST Ne oaesoun, mxmacer0a/05/04, ansiyseix Riana Study No.=LI958, Set No.=030504A, Ext.Date=03/05/04, Analyst=K.Risha Page 141 Sumpie List: |3:\Daca\CHNSS WassLym Fluosochemicals.FRO\SR=pLADBAO30504A CO ACS S~mple List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM preg re rp rr i) I MeMLetatshhtooddm::odified=P1MP\o=nD\aDMatatara\\LL1C5CMMS1SM3MS:S626\2\M:Ma4as6sasll2y0~n0nx4x\\FFlluuoorroocchheemmiiccaallss..PPRROO\\NMeetthhDDBB\\CCoottGGrroovvee NNPPDDEESS 003311550044 Caan maaicied: om war 10 23138005 Fhe Last modified= Mort Mar 15 13:25:12 2004 = Job Code= I Perriinntteeda:: TTuuee MMaarr 1166 0077::2266::2277 22000044 same o30s04n-472 ' TNTeaexmxtet:== 030504A-471 I1:: CC66 AAcciiddPPFFEHAA -- i L1958-22, DF=100 (6305042471 5m hn, 2) 030504A-471 Sm (Mn, 2x3) y i 110000.~ 1~ MoR f LCorMM oSmIeMSE5- 38..1155 sie a2H0ee4a 21~ 1133--MMaarr--22000044 1188::0088::11 ~= LCIMS/MS MRM of 5 Chan33n11e33ls>> E22S669-9) 6.20e4 Area i *] A ' 28 bo | \ _ 2.00 4.00 2: co noid seo 2:C8 Acid PFOA LL11995588--2222,, DDFF==110000 c;ao0y504.471 Sm 4,223) 030504A-471 Sm (Mn, 2x3) oh _ oh IE oo 6.00 8.00 10.00 " TTiimmee asi8s.6mo9 1133--MMaarr--22000044 1188::0088:1:1:5 LLCC//MMSS//MMSS #6 MRM of 5 Crannos E5- MRM of 5 Channels ESe32305005 413 > 369 2.33e5Area h 20 ao ow am oo 1001%1_ 2.00 4.00 6.00 3. co sutonace seas _ 3:C4 Sulfonate PFBS [LL11995588--2222,, DDFF==110000 . Ga0504A.4S7m1 4,215) MoR f 5CraM mets 5- 030504A-471 Sm (Mn, 2x3) x 52 EH i A A A = A AAA SAN 1 Err Tie] 4247~ 8.00 10.00 "" Time 1133--MMaarr--22000044 1188::0088::1155 LLCC//MMSS//MMSS ##66 MRM of 5 Channels ES- 72.2582 29119..88>66e9e393 PANNAAA Area |e Tae 2.00 ao eno e 173 e 00 Tine i 4.00 6.00 8.00 10.00 Time I Srygen Research, 3058 Research Drive, Stace Cotlege, A 16001 Exygen Research, 3058 Research Drive, State College, PA 16801 i CCHEOONNNNFEIDFPEIINNTDCIAOELU-NN- TSSTUYUIBBDJJIAEESCCTLTTRTITC0OT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E0E0NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00225533 a uorsssa0s 3M MN01539404 1 cenit eve vee re Quantify Sample Report Study No.=LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst=K.Risha Page 142 cre is SP PEE 65 KTS Sample List: Last modified: LE rat seveaomcasorrs st Method= Eo LaSt modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\030504A CG ACSFM Mon Mar 15 13:22:46 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031504 Mon Mar 15 13:25:12 2004 ! PrPirinntteedd:: TTuuee MMaarr 1166 0077::2266::2277 22000044 Name= 030504A-471 Fr Text: 4:C6 Sulfonate PFHS L1958-22, DF=100 ii "wo |030504A-471Sm(Mn, 2x3) i *| FA rT MTNR rrr pre 2.00 4.00 6.00 8.00 ET 13-Mar-2004 18:08:151 wieh MRMof 5LLCCCh//aMMnnSSe//lMMsSSES##-66~ MRM of 5 Channels ES- ' 399 > 80 `Areal 2.28e4, Area pee Yew Time[ 10.00 5:C8 Sulfonate PFOS s>nare smn 1L9159588--2222,, DDFF==110000 030504A-471 Sm (Mn, 2~<3) =we na nosn 1133--MMaarr--22000044 1188::0088::115 LLCC/lMMSS//MMSS #6I MRM of 5 Channels ES- I 8.86 499 > 99 | "Areal 1.47e4 Areal 1001%1 269L | TT ew |] o0-i" .... i .... i .... ~ .... , .... , TRE ANN .... , .... , .... ,-- 2.00 4.00 6.00 8.00 , Tr. , r.e..T.E-TTiimmee | 10.00 vpn arn, 45 sen evn ssn eg, 7 38 Exygen Research, 3058 Research Drive, State College, PA 16801 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00225544 3M MN01539405 I I 1 | QQSuutaaunndttyiiffNyyo.sSLaa1mm9pp5ll0ee, RReeSpeptoorrtNto.:030504A, Ext.Date:03/05/04, Analyst:K.Risha age 100 Page 143 Study No.:LI958, Set No.:030504A, Ext.Date=03/05/04, Analys~=K.Risha LSSaaasmrtppllmeeodLLiiissftti::ed: NPPor:n\\DDNaaattraa\\LL15CCHMSS1MM3S:SS262\\:MM4aa6ssssll2y0ym0n4ex\\FFlluuoorroocchheenmiiccaallss.PPRROO\\SSaammppLlaeDDBB\\D0I300S5O0R4AA CCOG AACCSSPFNM | sMLLFLeeaaoattssbsnhtttooCmdamomo::doodeddriitffiiieeeddd::: NMPPoo=onn\\DDNMaRaatttraa\\L11L55CCMHS11SM33HS1:S226\52\M1:Ma34as26sasll22yy00m00ne44x\\PFlluuoorroocchheenmiiccaallss..PPRROO\\MNeStEhRDDBE\\CCoottGdrroovvea Mon Mar 15 13:25=12 2004 NEPDDEESS 003311550044 Job Code: | erinteas Printed: Tue Tue Naz Mar 1166 0077::2266::2277 22000044 , aNammees: 003300550044An--447722 Text= 3. csrca prin a i |Pen DF=1000 I: C6 Acid PFHA L1958-23, DF=1000 Co | 00133(00550044A7-447722 SSmm ((MMnn,, 225x33)) o 1a84.11574 _ 1133--MMaarr--22L0000O44M11S88:M:330S0::0031 MRM MRM of of 55LCCChh/aMann3nSne1e/lMl3ssS2EE6SS#-96- I! 313 > 269~ 41Adreeda 4.13e4I Area n|. 202.00 04.00 66.0000 22L::19Cc5888-AA2cc3ii,ddDFPpFr=Oo1nA000 L1958-23, DF=1000 000330005,50044A7-447722 SSmm ((MMnn,, 22x23)) 1| 880.000 88.77111s _-- UPNTT tre 1100.0000 Time _ 1133--MMaarr--22L00O00M44 S11I88::M33S00::0#0363 MRM MRM of of 55LCCCrh/Maan1nSne3e/Mls>sS3EE6SS#-0-6 413 > 369 26r7e0a5 2.67e5 Area 110*01 LTT 2.00 33.: CCo4 sSuullffoonnaattee pPrFeBsS [LL1195588--2233,, DDFF==11000000 00133000055,0044A4-447722 Sm Sm (Mn, (Mn, 2:9) 2x3) T1 AN A SVT WA | wo em .... ~ .... ~ abo .... 4~ 8.4..7.~ ~ fa oo .... ~ .... ~....'Time 4.00 6.00 8.00 10.00 _ 1133--MMaarr--22L00C00I44M1S188I::M33S00#::00633 5 MRM MRM of of 55LCCChh/aMannnSn2ee/l9Mlss9S>EES9S-9- A 71.859A J, 29192>16939 ren Ama ASAAANA -,1186 ~/~1.21e3Area | 1 S 0' .0 ... 0 , , ,,~ 20, 0..% .. ~ ,, a,, .... , ....60, 0.S ... , ....80, 0.... , ....10,00.... , .... Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Reseach Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00225555 SW_MNO1839405 3M MN01539406 1 | QSQtuuuaadnnyttiiHfteyy..sSLaa1mm9pp5ll8ee, RReSepeptoorrNtto.:030504A, Rxt.Date:03/05/04, Asalyst:K.Risha PPaaggee 114444 Study No.:LI958, Set No.:030504A, Ext.Date:03/05/04, Analyst:K.Risha 1 aLSLSaaaatasmmittppollnmeemsooadLLiiiifssfittie::edd::P:FNMP\ooo:\Dnn\DaDatMaateatrer\a\L\LLO1155CMEMSNS11S3SM3S::S\E326M32\Ma1:Msa44ass6slssy2l2Lm00yx00n\y44xF\lFTulouro\orocFchheenImiicccuaaalllsoss...PPFFRRROOO\\o\MSSAaacLmspEplOlheBeD\DpCeB\o\0t03RG30z0So5i0v04e4AANPCCDGGESAACCS0SF3IM1504 MLTLeaoatsbshttocdmma=ootaedrtiefiteodd:: hon Har 15 1313311 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13:25=12 2004 NPDES 031504 | JporbimCoedre: ee mar 16 07:26:27 2004 Printed: Tue Mar 16 07:26:27 2004 aNazmaer= 003300550044nA--447722 ' TTeexxtt:= 44: :Cc6e sSuulltfoonnaactee PprFuHsS i LL11995588--2233,, DDFF==11000000 (030504472 8m (Mn, 268) Ca|| 030504A-472 Sm (Mn, 2x3) |% . . 4885.05227 __ 1133--MMaarr--22000044 1188::3300::00:31 LLCC//MMSS/IMMSS #6! MRM of 5 Channels 5- MRM of 5 Channels ES- ~ 39> 60] 399 > 80~ 20e00a4 2.08e4/ 451 Area;i thre -------------- res ime .... ~ .... ~ .... ~ .... ~ .... ~ .... ~ .... ~ .... ~ .... ~ .... ~ .... TimeI 200 ato 500 500 1000 2.00 4.00 6.00 8.00 10.00 i 5: ca sulfonate pros -- _ RSS 5: C8 Sulfonate PFOS LL11995588--2233,, DDFF==11000000 1030504S4m4(7Mn2, 2:3) Mof R 5ChannM els ES. 030504A-472 Sm (Mn, 2x3) 100,h 258s7 10T9405094 I] 1 O01. 1133--MMaarr--22000044 1188::3300::00331 LLCC//MMSS//MMSS ##66I MRM of 5 Channels ES- ! 8.88 499 > 99 1.`4AA0rreeea4a~ % teh e akr80e 0 800_ NS E0E0ETT Tine 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReessseaarrcchh,, 33005588 RReesseeaarcchh DDrriivvee,, SSttaatLee CCoolllleeggee,, PPAA 1166880011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00225566 _MNO1S39407 3M MN01539407 ! | qQSuutaaundntytiiffNyyo.:sSLaa1mm9pp5ll0ee, RReeSppetoorrttNo.:030504A, 3xt.Date:03/05/04, Analyst.K.Risha PPaaggee 11445s Study No.=LI958, Set No.:030504A, Ext.Date=03/05/04, Analyst=K.Risha SSLaaammspptllmeeodLLiifssitte::d:P:PM\=oDn\aDtNaaat\raL\CL15HCMSSH1MS3S:663\3\M:Ma4as6sssll2yy0m0nx4x\\FFlluuoorroocchheeamiiccaallss.PPRROO\\SSaasmppLleeDDEB\\003300550044AA CCGG AACCSSFIM I dMLLeoaattashbttoomddmo:roddiiftiieedd=: NMPPoo=rnn\\DDNMaaaattrraa\\LL11C55CHMS1S1H3M3S1:S6326\52\1=MN43a63sasl22sy0000na44xL\Fylunorxoc\hFemlicualos..rPPoRROOc\\MSheEteRhDDnBB\i\CCOcoEtaGGErloovvse NNPPDDEESS 003311550044 Jab coder Last modified: Job Code: Mon Mar 15 13:25:12 2004 [-- Tue Max 16 07:26:27 2004 Printed= Tue Mar 16 07:26=27 2004 *NTNaaommteas:: 003300550044A--447723 Text~ i1:: cC6o eActiad PpFoHnA [XXCC003300550044--66,, 11000000 nngg//LL SSttaannddaarrdd 10;03300550044AA--447733 Sm Sm (Mn, (Mn, 23) 2x3) | ae! 12586.1175557 1133--MMaarr--22L00C00I44M11S88I::5M51S1::4#74517 MRM MRM of of 55LGCChh/aMann3nSno1e/l3Mlss5SEE25S#6-6-0!/ 313 > 269/ 63w0e0a5 6.30e5/ Area~ 1 , 2 .... 5,6 .... , pr) .... ~ .... , 500 .... r .... , 8.00 .1.2.9.79,7~.... , 1000 .... ~ .... , .... Tmo Time 100~% 2.00 4.00 6.00 8.00 10.00 22X::C0Cc38o05AA0cc4ii-dd6,PpFr1Oo0An00 ng/L Standard 13-Mar.2004 18:51:47 XC030504-6, 1000 ng/L Standard [0305048473 sm in, 223) 1M3R-MMoafr-25LL0CCC0hI/4aMMnS1nSIo8/Ml:M5sS$1E#:S#46-67 100,1 030504A-473 Sm (Mno 2x3) atoo8.r7rt1s MRM of 5 Chan41n13e3l1s>>73E136S0608-9] | `area 1.71e6 Area | | | 22.0000 a04.00 33X::C0Cc34t05sS0uu4il-tf6oo,nnaa1tt0ee00pPrFneBgsS/L Standard XC030504-6, 1000 ng/L Standard 1 [i0033050054A0-447325S4mm7M(Mn3n,, 253) 2x3) 1 100t * 66.0000 58.0000 759 33575.050399 000 TTiimme|e 10.00 es 1133--MMaarr-22L00C00/44M11S88/::M55S11::4#47 MRRMMooff 5LCCChh/aManSnn2e/nM0lseS>EElSS#5s-9-61 28989..6>66e9339 | Area | ober 200 400 2.00 4.00 500, 800S 00 N 6.00 8.00 10.00 Time EExxyyggeenn RReesseeaazrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00225577 SW_MNO1839408 3M MN01539408 i | qQSuuaanntEtiifyy SsEaammppEllee RReeMppeo.orrttcos0504n, mxt.Date:03/05/04, Amalyasix.isha PPaaggeo 114466 Study No.=LI958, Set No.:030504A, Ext.Date=03/05/04, Analys~:K.Risha | eTSLSaaaatrsmmhetppllommeesooddLLiiiiffssiitte:e:dd:: 5WMPPoe:rnn\\\DaNMDataaatartra\s\L\L11LC5C5OMHHS11ES3M3SM1S:ESa26E32\M\1:MaWd4akae6sssssl212ly0y0y0ne8m4x\e\\FFFlluLuoorurooccohheermmiioccaalclss.h.PPPRRReOOO\\\mMSdaatimzpDplcBlee\DaDCBEo\\lt00G33ar00o55.v00a44AANECCDGOESAACCS0SF3IM1504 MLLeaatsshttocdmme:ooaddariiffiieedd=: Non Nar 15 13135113 2008 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Mon Mar 15 13=25:12 2004 NPDES 031504 | eJcoibntCeoadse: Tue dar 16 0736127 2008 Printed: Tue Mar 16 07:26:27 2004 sama: 0308000-473 Name= 030504A-473 Text= |44'X.:XCC0c0Co36300s5S50uu04il4-ff-6oo6,nn,aa11tt00ee0000vPFennHggsS//LL SSttaannddaarrdd p10o3003500540A4-447733 Sm Sm (Mn, (Mn, 263) 2x3) | 00 * 3Mar-20o04o18:57:47 1M3R-MMaorf-25LL0CCO0h/M4aMnS1nSIe8/lM:Ms5SS1E:S##4-6~~, 28o9.s56225 MRM of 5 5> % 2200805 Channels ES399 > 80 ea 2.26e5 Area ! 256, a 5. ca sulfonace 2p.0r0os 4.00 XC0305044, 1000 nll 5:C8 Sulfonate PFOS XC030504-6, 1000 ng/L SSttaannddaarrdd [0305042473 5m vn, 2:3) 100030504A-473 Sm (Mn, 2x3) Joy |1 | *|= | olTTT a 2.00 4.00 550. ako 000 Time Time 6.00 8.00 10.00 A ss8.88 Vooey 13:Mar 2004 18:51:47 MRMof 5 Channpois ElS. LCIMSIMS#6 13.Mar-2004 18:51:47 LC/MS/MS #6 MRM of 5 Channels ES499 > 99 1.2Ar6ereeaa5] 5% a ww 6.00 8.00 10.00 | ine| Time Exygen Ressarch, 1058 Research Drive, State College, 7A 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00225588 m_Motsaod0n 3M MN01539409 EE -- sos Sponsor Study No: fampmdogie E~ygen Study No: SE ni Amaly~: pic Ions Monitored: = > Site: NA L1958 Perfluorohexanolc Acid 313 -> 269 NA RAWDATA REPORT RAW DATA REPORT nu Limit of Qt~anfitation: m------ Injection Volume: = un Matrix: Mem ow Sarc~le Voltmm: er ji Final Volume: 50 ppt 15 p.L Water 40.0 mL 5.0 mL sare ama Set No: fd prac Anal)st: Ere are Irtstrument Type: -- = Extraction Date: han Analyzed on: 03 1704A Karen Risha LC/MS/!VlS Unit # 6 03/17/04 03/18/04 -- w oe o>r arrte e oem eoa rEwR TEmd amwtem Exygen Sponsor Sample Run Std. Conc. Dilution Peak Analyte Found Amotmt Added Recovery. ID XC030504-0 ID Code No, (ppt) Factor Area (PrO (pVt) (%) CS 031704A-601 0 1384 XC0305~34-1 CS 031704A-602 25 5637 XC030504-2 CS 031704A-603 50 9780 XC030504-3 CS 031704A-604 100 19409 XC030504-4 CS 031704A-605 250 41045 XC030504-5 XC030504-6 CS 031704A-606 500 CS 031704A-607 1000 86735 151544 SCeommaant :: SSoemmaenn CoVomm R ow aAaa MethanolWash C OMTO4A-608 1 0106020 Control U 031704A-609 1 1243 ND 0106020 Spk A LCS 031704A-610 1 9223 48.8 50 98 0106020 Spk B na LCS 031704A-611 1 81477 524 500 105 XC030504-1 XC030504-2 we L1958-17 Spk C Unis L1958-5 Spk D Goat L1958-9 Spk E fra] L1958-13 SpkF L1958-1 Spk G evra XC030504-3 XC030504-4 TAY L1958-3 rolnfluent 3 cmon Comb Effluent 1/2 xPort 4A TaPort 4B lntluent 1/2 e--i_--ew Influent t/2 Low Spk CS 031704A-612 CS 031704A-613 SOME LF 031704A-615 bo ome LF 031704A-616 Booman LF 031704A-617 En LF 031704A-618 LF 031704A-619 & oma CS 031704A-620 CS 031704A-621 BGED FF 031704A-623 25 50 Ye Sb 1000 TE 100 Cm mn 100 lm om 100 100 wo me 100 250 Ck a 100 5205 8898 80237 30659 83217 87895 85567 17312 38557 24434 ee ww ow 516000 250000 188 mm 19000 10~O0 185 he em 53600 25000 161 moon 56600 25CO0 164 55100 10000 512 o we wT e 14900 10000 110 XC030504-5 CS 031704A-626 XC030504-6 Analyte Found (PP0 Reeovery (%) = = (peak rme aetsncCS a~ea - intercept) / slope x DF [allal~'te found ~ppt)-anal~'te found in eolltl'ol 031704A-627 (ppt)] r, 100 500 1000 79456 143391 Tere Standard Carve : Linear (1/x weighted) rTe n Intercept = 1811.49 amount added (PP0 Slope - 152.008 r-- 1 um re CS = Cal~rmion standard LF = Lab fo~fled sample Sony lr. C - Control san~le FF - Field fortified sample Lr Tes DoesComte. S = Sarc~ple LCS = Laboratory Control Spike CK = Check Standard A hombres nite ND - Not detected - Response between 0 and 25 ppt Ee Dacom NQ = Not quantifiable = Response between 25 ppt and LOQ (50 ppt) Seven cro si On Samples were corrected using the data found in set 030504A. snr Coef. OlDer. = 0.993757 $5 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTTT.EECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00225599 W_Mo1S30410 3M MN01539410 I I | ie Sponsor Study No: rosie Exygen gtady No: EaAnalyte: Et Ions Monitored: ESite: --_--oT3Exygen NA 9L1958 orn Perfluorooctanoic Acid 413 -> 369 7NA F---- RAWDATA REPORT dtm re . Limit ofQuanfitafion: uti tind Injection Volun~: f= iz or Matrix: Sore |S Sample Volun~: me gE == Final Volume: 50 ppt l 5 pL Water 40.0 mL 5.0 mL Set No: Analyst: lnslnanent Type: Exlxact]on Date: Analyzed on: ii_ete 031704A Karen Risha =LC/MS/MS Unit # 6 03/17/04 03/18/04 roao Sponsor Sample Rtm aSeewbh Cone. Dilution Peak 2WT Analyte Foand Amount Added ouw m Recovery ID XC030504-0 ID Code No. q3pt! Factor Area ~P9 ~vpO (~) CS 031704A-601 0 1296 XC030504-1 CS 031704A-602 25 7657 XC030504-2 CS 031704A-603 50 14896 XC030504-3 CS 031704A-604 100 27966 XC030504-4 CS 031704A-605 250 58208 XC030504-5 CS 031704A-606 500 119459 XC030504-6 UaEmMethanol Wash 0106020 ConUol 0106020 Spk A 0106020 Spk B XC030504-1 XC030504-2 Th L1958-17 Spk C DoeY L1958-5 Spk D 3ina na na ume Influent 3 o=< e Comb Effluent 1/2 CS 031704A-607 1000 236685 LgSogEmey cI o EomoW2:5 o8i C C LCS LCS 031704A-608 031704A-609 031704A~610 031704A-611 40977 1 1515 ND 1 14001 50.6 50 101 l 121791 511 500 102 CS 031704A-612 25 7709 CS 031704A-613 50 14377 EELS LF 031704A-615 I000 136155 0 IUD -CZhPE LF 031704A-616 100 30247 gen 572000 250000 lOg BmEmE?Z 12000 lOO00 119 L1958-1 Spk G lnfluent 1/2 MBhrmoowwmmiigyzn XC030504.3 XC030504.4 L1958-3 LI958-23 Infiuent 1/2 Low Spk Trip BlankHigh Spk LF 031704A-619 I00 70266 29100 10000 175 oLposEmS CTomLDom oom oom o2f CS 031704A-620 lO0 26988 CS 031704A-621 250 60720 FF 031704A-623 100 45237 18400 113000 68 FF 031704A-625 1000 26721 105000 100000 105 B a CE tA a Ea e) XC030504-5 XC030504-6 CS 031704A 626 CS 031704A-627 Analyte Found (ppt) - (peak area - intercept) / slope x DF Recovery (%) = [anal/t~ fotuld (ppt)-analyte found in control (ppt)] x 100 500 1000 120195 232929 Standard Cwve: Linear(l/xwighted) Intercept = 2135.08 amount added (ppt) gots CS = Cahbmtion standard f Sarn C = Control sample spies LF = L~b fortified sample Li r cg m, FF = Field forfilied sample E SE sussE oneriomyoon S- Sample LCS - LaboratoD" Control Spike CK = Cheek Standard ND = Not detected = Respomc between 0 and 25 ppt NQ = Not quantifiable - Response between 25 ppt and LOQ (50 ppt) ten ten Samples were corrected using the data fmmd in set 030504A. Slope = 234.327 Coe OlDer - 0.999637 ---- toll CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00226600 3M MN01539411 | | | ! RRAAWW DDAATTAA RREEPPOORRTT Spnsesuani 8 Umisrquein som sate aon Sponsor Study No: ' Eomsmne sss ce te BI Sa Raut Exygen Study1~o: Ae Fetes Vann I [= Analyte: rsbiint 8 Samevote. toms [rag Ions Monitored: = w Fe Som a a Site: NA L1958 PerBuerobutanesulfenate 299 -> 99 NA Limit of Quantitation: Injection Volume: Matrix: Sample Volume: Final Volume: 50 ppt 15 Water 40.0 mL 5.0 mL Set No: Analyst: Instrument Type; Exlraction Date: Analyzed on: 031704A Karen Risha LC/MS/MS Unit # 6 03/17/04 03/18/04 T Soy Sor Spe Bm W Coc Dim Tak Toms mAawd Rem Exygen > ry Cit 5 om mew dm on ow og ID ww &omaar T 2 XC030504-0 Sponsor ID Sample Code CS Run No. 031704A-601 Conc. Dilution Peak Factor Area o 0 Analyte Found (pin) Amount Added (,aFt) Recovery (%) `xcmoss2 XC030504-1 XC030504-2 : eae sw : - CS 031704A-602 25 0 CS 031704A-603 384 xcmosous XC030504-3 XC030504-4 : owes mL mC : : CS 031704A-604 lOO CS 031704A-605 25o 611 1589 XC030504-5 CS 031704A-606 500 3300 XC030504-6 C~ 031704A-607 5524 Methanol Wash C 031704A-608 0 0106020 Control o0sin 0106020 Spk A Ooanosas 0106020 Spk B XC030504-1 Seoces XC030504-2 misao L1958-1 Spk G oes XC030504-3 XC030504-4 pieL1958-3 frre] L1958-3 Lie: L1958-22 LisiL1958-23 cones XC030504.5 -a bt Influent 1/2 ities Influent 1/2 Low Spk hitless Influent I/2 Low Spk Tybwiitn Trip Blank Low Spk Tomo Trip BlankI-Iigh Spk C womens LCS IS mma LCS CS & oma CS Gobind LF omnes CS CS 7 aroma FF Bo arowss FF FB oloaer FF olokas FF & owes CS 031704A-609 031704A-610 031704A-611 031704A-612 031704A-613 031704A-619 031704A-620 031704A-621 031704A-622 031704A-623 031704A-624 031704A-625 031704A-626 0 ND 1 mo we 6 ow 281 39.0 50 C0 we wm wom 3262 553 500 25 0 mC 50 278 Cue do me wx 100 8001 137000 10000 Ww wo 1oo 657 250 1501 I lOO0 1042 170000 10000 we am low 10o 9328 10000 wom we leew 10o 522 8050 10000 wo us ow www IOO0 465 70700 100~00 0s wo 5o0 2945 78 111 949 1279 81 71 XC030504-6 CS 031704A-627 Tere Ga eo Analyte Found (ppt) = (peak area - intercept) / slope x DF Rey eeon gonce0d 10 Recovery (%) = [analyte lbund ~opt)-anal;cte found in control (13pt)] x 1 O0 sit amount added (ppt) 5 + thin nbn 15 te rpc CS = Calibration standard LF = Lab fortified sample = Commie 1 etre C = Control sample FF = Field fortified sample Sime LES eyCn $5 S = Sample LCS = Laboratory Control Spike CK - Check Standard dnRepent ND - Not detected - Response between 0 and 25 ppt NN qb Renbert 35 9 100 5000) NQ = Not quantifiable = Response between 25 ppt and LOQ (50 ppt) [ ---- Samples were corrected using the data found in set 030504A. aalueltSoneorvsa- 6soT7ma2ark9n ee 5816 Standard Curve : Linear (l/x weighted) Intereept = 54.7291 Slope = 5,80467 Coef. OfDet. - 0.993620 patacepepmesty LOB) of `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTTT,EECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00226611 IM_MNO1539412 3M MN01539412 | spmrsuye Sponsor Study No: Eos Exygen Study No: ee Analyte: Jere Ions Monilored: -Site: WoNA LEL195g J -- Perfluorhexane~ulfonate 399 -> 80 "NA RAWDATA REPORT RAW DATA REPORT Ltr inir Limit of Qaantitation: ee Injection Volume: jrMatrix: Sooper: Sample Vnlume: Fam Final Volume: Soe50 ppt io15 ~tL fiWater on 40.0 mL So5.0 mL sae Set Ne: oe Analyst: mete lnstrament Type: Brcoine Ex~'action Date: ---- Analy~ed on: oom 031704A jrKaren Risha LoS rs LC/MS/MS Unit # 6 om 03/17/04 ie 03/18/04 BuExygcn 5ID Tomo XC030504q) Sper Sponsor o2>ID Sok he Gm Dh fk Sarnp~ Ce Gm ter dm Code Emaar t CS Run No. 031704A-601 Conc. (ppt) 0 Dihfion Fac~r Peak 0 TGemw Analyte Found (ppt) iemAmount Added (PP9 Re"wmem Recovery (%) XC030504-1 CS 031704A-602 25 873 XC030504-2 CS 031704A-603 50 1918 XC030504-3 CS 031704A-604 100 3759 XC030504-4 CS 031704A-605 250 ~576 XC030504-5 CS 031704A-606 500 17829 XC030504-6 CS 031704A-607 1000 35559 onceamsmaan -3 iEs oains PPoomdse wwm wens Methanol Wash 0106020 Control 0106020 Spk A 0106020 Spk B C 031704A-608 na C 031704A-609 na LCS 031704A-610 na LCS 031704A-611 0 0 ND 1858 52.3 50 105 17060 484 500 97 XC030504 1 CS 031704A 612 25 906 XC030504-2 CS 031704A-613 50 1733 Lions XC030504-3 XC030504-4 L1958-3 Wien Influent 1/2 Low Spk BOA ote a0 we wm uw CS 031704A-620 100 3370 CS 031704A-621 250 8581 FF 031704A-623 lOO 5147 14600 10~00 100 XC030504-5 CS 031704Ao626 500 17277 XC030504-6 CS 031704A-627 Tor eS Analyte Found (ppt) - (peak alea intercept) / slope x DF Rev oyeot Ear nt co pe 00 Recovery (%) = [analyte found (ppt)-analyte found in eonlrol (ppt)] x 100 1000 35458 Saket DeTend Standard Carve : Linear (l/x weighted) nee341500 Intercept = 16.7342 amount added (PP0 Slope = 35.2308 5 = Catmmates 1 bb CS = Calibration standard LF = Lab fortified sample Coma 7 ova C = Control sample FF - Field fortified sample 5samp LSLabrtry Cont Ske S = Sample LCS = Laboratory Control Spike CK = Check Standard 0. tbR e eemen 2 ND = Not detected = Response between 0 and 25 ppt Nagar Fee bee 7 00 (O77) NQ = Not quantifiable = Response belween 25 ppt and LOQ (50 ppt) Conf. OfDet. = 0.999704 Somstibetrepay. 03) Sot rc ig eo rd CTSA Samples were corrected using ~e data fonnd in set 030504A. `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTTT,EECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00226622 IM_MNO1539413 3M MN01539413 i ' sprsute Sponsor Study ]qo: frente Exygen Study No: Analyte: int Ions Monilo*ed: =Site: 00NA L1958 wPerfluorooctanesulfonate 499 -> 99 NA RAW DATAREPORT RAW DATA REPORT Smads Limit of Quanfitafion: Int Injection Volume: Matrix: Savane Sample Volume: Tema Final Volume: So50 ppt Swoom15 ~tL Water 40.0 mL 5.0 mL savSet No: ae Analyst: Instrument Type: oom Extraction Date: fra Analyzed on: ann 031704A Kanaa Karen P,isha LCAMS,qV[S Unit # 6 ta 03/17/04 Se 03/18/04 Ee Exygen =ID XC030504-0 pe] XC030504-1 soSponsor wo:ID Sr Sample aCode CS CS ehe eGe m OMe Rk R Tm Run Conc. Dilution te Gm tee he mm No. (ppt) Factor 031704A-601 o 310 omar w o 031704A-602 25 440 Analyte Found (ppt) Amount Added (ppt) Ne"m w Recovery (%) XC030504-2 CS 031704A-603 50 900 XC030504-3 CS 031704A-604 IOO 1583 XC03050~M CS 031704A-605 250 3392 XC030504-5 CS 031704A-606 5o0 7489 XC030504-6 CS 031704A-607 1000 13775 Methanol Wash O106020 Control monn 0106020 Spk A mens 0106020 Spk B orn XC030504-1 fry XC030504-2 L1958-1 Spk G aana na na tt12 Inflaent 1/2 C 03 [ 704A-608 C 031704A-609 ws orones Ve moa ow LCS 031704A-610 iS man Vom wm om LCS 031704A-611 ome w CS 031704A-612 25 0 0 ND 659 34.9 7099 525 532 50 70 500 105 uo ones wo wn me ww we CS 031704A-613 50 777 LF 031704A-619 100 3927 28300 10000 149 XC030504-3 CS 031704A-620 100 1421 frLoessn XC030504-4 L1958-3 XC030504-5 Els lnfluent 1/2 Low Spk aFo oommwae ww wo FnAe mH w-e ow CS 031704A-621 250 3438 FF 031704A-623 100 3246 23200 10000 9g CS 031704A-626 50O 6406 XC030504-6 CS 031704A-627 C--O Analyte Found (ppt) - (peak area - intercept) / slope x DF a A oese Recovery (%) = [anal)Ce found ~pptkanal)ae found in conlrol (ppt)] x 100 iim So 1s amount added (PP0 1000 es =Comat srs 1 <u samp xtra om CS = Calibration standard LF = Lab fortified sample pit Feat C - Conuol sample FF - Held furdtied Si~IIlple Soom Te contre Sabir. lod S = Sample LCS = Laboratory Control Spike CK - Cheek Standard 0 = tek Rae en32 ND = Not detected = Response between 0 and 25 ppt NONvmitie-Rope 3 7 AL0Q 570 NQ - Not quantifiable = Response between 25 ppt and LOQ (50 PP0 Sipswecc i ordio Samples were corrected using the data found in set 030504A. 12885 Standard Curve : Linear (1/x weighted) Intercept = 200.030 Slope = 13.i525 Coef. Of DeL - 0.995843 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSTUUYBBIDJJIEAESCCTLTTRITTCOOT AACOPPURRROOTTT,EECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR-2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00226633 IM_MNOTS39414 3M MN01539414 ------ ee--e------------------------ E IY ootecanne Pon 16272109 3058 Research Drive CHE EE To shat State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 otras Chinof CustodyForicaton Sheet Internal Chain of Custody/Fortification Sheet bomsuigtonte, Las No wie Exygen Study Number: L1958 Matrix: Water SonSymi Sponsor StudyfProtocol No: N__A emma teiion scetemo fon eg 32 The samples listed below were removed from refrigerator No. Teas n- obilo nsf Time Date 0~]17]t~14 r~ia~s #l-ma TEr TT Ta T Ee CLIENT SAMPLE -- er-- -------- ---- na EXYGEN ID NUMBER 0106020 Control I VOLUME (mL) I 40.0 FORTIFICATIOI~" (ng) e omarT or[5 na 0106020 Spk A 40.0 2.0 e emaT TosTwo na 0106020 Spk B 40.0 20.0 eer T menmc T doo Toms | lnfluent 3 [Compemmenia| uiossssn | wo [aon | Comb Effluent 112 roman 1 riosmesie |wo| wo | Port 4A L1958-17 Spk C L1958-5 Spk D L1958-9 Spk E 40,0 40.0 40.0 I0000.0 400.0 1000.0 [me 1 wens a0| mec | Port 4B L1958-13 Spk F 40.0 1000.0 hein teisse ee eso] Influent 1/2 L1958-1 Spk G 40.0 400.0 omeitiea | bem Influent 1/2 Low Spk L1958-3 40.0 yy TST ---- Trip Blank Low Spike L ! 958-22 40.0 Trip Blank High Spike L1958-23 40.0 r Pe PS r SSEPS-- rT r rT r1 1 C 1 Er SBE ] 1-- ---- ---- rr r r C evaT Teton|] [--owvsn 0106020 gpk A 1pose oayat) [ooamr010s602a0 Spsk B TT roizooes io0ant) [meneTung oatmeer TE gil [Tussin LI958-17 Spk C 1rouoesuoncgm) [imstL1a958-s5 gpek D |vFo01o20m0e4-n7gomosyeiy L1958-9 Spk E isnT vers tomes {rw coy [0 lod L1958-13 Spk F F012004-7 iomisao rosisomer conmere | 5 03rd L1958-1 Spk G 200.1 optmiewsipes|EL rcai7bd |200, ootmore)| leonirlo | son cong menpess|PY valnlol |10. oostmenpimy| 0ial 1BY . All samples were measured: Toe Wz owe_03lizlod Time 11~ Date O~!lT]Oq Aer eso es ws metsgc 32. After measuring samples were returned to refrigerator No. TE Time I~.Ot) Date 0.,~! I]~O~ ~- is_ ANE, Initials wise ~itials Cranes oraat pse sie so 18Eloy Comments: ZOO p.L of 250 rag/alL sodittm thiosuffate was added to allsamples before spiking. Initials/Date: Ay Smear: Baouaaseseec_03VTONA --w--ai --e T E--en= odhe plol Analysis Summary: Data Set: Data Set: Data Set: Initials/Date: Initials/Date: / Initials/Date: ~ / ee dhtao Set extraction/analysis data verified by: ~ July~6, 2001/6 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00226644 aunotsasets 3M MN01539415 Exygen steers 3058 Research Drive -- Phone: 814-272-1039 mmoAMPtLdE EXTRACTIONmANaDrAVtAL YSIS TRACKING STcnn R E S E A R ( H State College, PA 16801 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L1958 METHOD: s~ PROTOCOL NUMBER: NA Client ID er T fmo rrrEeEerrS EmTrE ae To]] na Fe Hm] na Er ree ree s na Een HE] Influent 3 e EE pE e he r eee Comb Effluent 1/2 MATRL-'K: Water Exygen 1D 0106020 Cunlrol 0106020 Spk A 0106020 Spk B L1958-17 Spk C L1958-5 Spk D STEP 1 ANALYTES: CA~ C6, C7 & C8 Acids, CA, C6 & (3.8 sulfomtes STEP 2 Dilutions (mL/mL) ~'~ 'VtO STEP 3 Dilutions (mL/mL) ~ ~ ~ ~ STEP 4 ~ ~ -_ Reagents/ Materials Methanol c18 SeE Type 1 Water Port 4A L1958-9 Spk E o.\/| O - Port 4B Influent 1/2 Fra mem e He HHs s HP t~u~t 1/2 Lo,~ spk Trip Blank Lo'~. Spike E F t F t a F e e t r FF F F Trip Blank High Spike L1958-13 Spk F L1958-1 Spk G t,195s-3 L 195 g -22 LI95g-23 o. ~AO - 0"~/i0 , 0. ~tI 0 / - ~ Initials/Date - - HPLC rr min|yabisn | ee 1 emer Ta oolTrod uts] *Initials/Date STE SPE he oy tga7 -- 0% Ko, ho W Dowd B00 STEP l : SPE column clean-up (omitting 40% wash) R =R TD rae STEP 2: Final volume to 5 mL collected in 15 mL polypropolene tubes Ze STEP 3: LUtMS/MS analysis STEP 4: LC]MS/MS reanalysis. R S AE i T i nn *Initials and date under each st~ indicates the personnel that performed this step. $$ Method of Analysis for the Determination of Perfluer~oetane sulfonate (PFOS), Perfluorooctane sulfonylamide (PFOSA), and Perfluorooctmxoate (POAA) in Water comm COMMENTS: iFinlalceoxnlracclsssrtoerediinn reefriigergatoer 332n~. Iennit'isal.s: A/~/M1 IE/~ DDuatee: 03[12004 July 19, 2001/4 F i T ------ CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 swore 3M_MN01539416 11993399..00226655 CS Masslynx - Sample List FEES Sample List: C:\MASSLYNX\FluorocheF0i~a.ls.PRO\SampleDB\031704A CG ACSFM.SPL Pdnted: Thu Mar 18 08:01:22 2004~,~~.~0~)-,~- I ~,I Bogensor Exygen STUDY no.NO.L~ ER --Page 1 rot Page Position: (1, 1) Vial File Name AHS ChatS Sum ttn LIMS ID ClientlD Sample Description at St Gone a Gmc Te OF Matdx Sample Type Conc(ng/L) Conc B ConcC Test lD DF 1 1 031704A-601 ...... XC030504-0, 0 ng/L Standard -- Standard 0 ..... 0 d]o (MOmBm : o-C R IEE hiMvE.E I"EomEe Eak -= C=Z 331 2 2 031704A-602 ...... XC030504-1,25 ng/L Standard -- Standard 25 ..... 0 PIemEEC oC omemMsER CER oR OC Df 3 3 031704A--603 ..... XC030504-2, 50 ng/L Standard -- Standard 50 ..... 0 ITE: - DBmNEe CEE BZ OC ZI} i 4 4 031704A-604 ...... XC030504-3, 100 ng/L Standard -- Standard 100 ...... 0 5 5 031704A-605 ...... XC030504-4, 250 ng/L Standard -- Standard 250 ..... 0 IDM: - ei CEE 2 O:- - i | 6 6 031704A-606 ...... X030504-5, 500 ng/L Standard -- Standard 500 ..... 0 7 7 031704A-607 ...... XC030504-6, 1000 ng/L Standard -- Standard 1000 ...... 0 {SEE ir TE zz % 8 92 03170ZtA-608 ..... Methanol Wash -- Blank ....... 0 Wo 2 mAs = 9 41 031704A-609 ...... 10 42 031704A-610 ...... 0108020 Sok A.80 ng. 0106020 Control 0106020 Spk A, 50 ng/L = a -- Blank -- QC 0 - - ....... 0 50 ..... 0 Fim cE TE 0B Zz ii '11 43 03170~A-611 ...... 0106020 Spk B, 500 ng/L -- QC 500 ...... 0 IoElEEEE:C -- iEmmmiaanSE,e oCc "oEB.m FfP COC Z Dfi| 12 2 031704A-612 ...... XC030504-1,25 nglL Standard -- Standard 25 ...... 0 13 3 031704A-613 ...... XC030504-2, 50 ng/L Standard -- Standard 50 .... 0 FLEE: - SERRE B= Ew CZ 1 lw 14 44 031704A-614 ...... L1958-17 Spk C, 250000 ng/L, DF=10000 -- QC 250000 ..... 0 BoEEHT OC EBS FT BR oC CF 15 45 031704A-615 ...... L1958-17 Spl~ C, 250000 ng/L, DF=1000 -- QC 250000 ..... 0 Pagmmic - mEmmanhatc- fF OB Oo: - |B 16 46 031704A-616 ..... L1958-5 Spk D, 10000 ng/L, DF=100 -- QC 10000 ...... 0 ogmbi- - EHERERMER Cf &= oC - f B 17 47 031704A-817 .... L1958-9 Spk E, 25000 ng/L, DF=100 -- QC 25000 ...... 0 3 osamamc C umuasReny og om HE | 18 48 031704A-818 -- -- L1958-13Spk F, 25000 ng/L, DF=100 -- QC 25000 .... 0 19 49 031704A-619 .... L1958-1 SpkG, 10000 ng/L, DF=100 -- QC 10000 ..... 0 BHES oE ramE EECE- Sr AWERr ERT CAoE Bw 2 oEC ECf 20 4 031704A-620 .... XC030504-3, 100 ng/L Standard -- Standard 100 ..... 0 21 5 031704A-621 ..... XC030504-,4, 250 ng/L Standard -- Standard 250 ..... 0 FiEma- - EEE TEFL CZ) 22 50 031704A-622 ..... L1958-3, DF=1000 -- QC 10000 ..... 0 23 51 031704A-623 ..... L1958-3, DF=100 -- QC 10000 ..... 0 Fags. - Ew EE BEEBE 24 52 031704A-624 ...... L1958-22, DF=100 -- QC 10000 ..... 0 FEE EEE = SELB oof & 25 53 031704A-625 ..... L1958-23, DF=1000 -- QC 100000 ...... 0 ETSHS- B%en Bx ZZ} 26 6 031704A-626 ..... XC030504-5, 500 ng/L Standard -- Standard 500 ..... 0 27 7 031704A-627 ..... XC030504-6, 1000 nglL Standard -- Standard 1000 ..... 0 1 1 1 1 1 1 1 1 11 1 1 1 1 10000 1000 100 100 100 100 1 1 1000 100 100 1000 1 1 S CONFIDER NCTIaAL SUBJECOT Tr0 ASPoROTECTIVE GROER ENTERED HENNEPIN COUNTY CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 sumer 3M_MN01539417 11993399..00226666 bFsEET -- MoMasslynx Sengotn - Sample List Cots MS Method | Simm 1 C6 8 ACIDS C4 6 8 SULF | SE 2 C6 8 ACIDS C4 6 8 SULF 3 C6 8 ACIDS C4 6 8 SULF i sian 4 C6 8 ACIDS C4 6 8 SULF 5 C6 8 ACIDS C4 6 8 SULF {dimond 6 C6 8 ACIDS C4 6 8 SULF 7 C6 8 ACIDS CA 6 8 SULF 8 C6 8 ACIDS CA 6 8 SULF |i SSiiEEBSoeHHl 9 C6 8 ACIDS CA 6 8 SULF 10 C6 8 ACIDS CA 6 8 SULF j 1 iEE Sds 1t C6 8 ACIDS C4 6 8 SULF 12 C6 8 ACIDS CA 6 8 SULF GimEns '13 C6 8 ACIDS CA 6 8 SULF t4 C6 8 ACIDS CA 6 8 SULF i dimdii 15 C6 8 ACIDS CA 6 8 SULF giant 16 C6 8 ACIDS 0.4 6 8 SULF i sitmdity 17 C6 8 ACIDS C4 6 8 SULF 18 C6 8 ACIDS CA 6 8 SULF giomate 19 C6 8 ACIDS CA 6 8 SULF GgiiEEBmEdHn 20 C6 8 ACIDS CA 6 8 SULF E 21 C6 8 ACIDS CA 6 8 SULF i ooimEnE 22 C6 8 ACIDS CA 6 8 SULF 23 C6 8 ACIDS CA 6 8 SULF Poms 24 C6 8 ACIDS C4 6 8 SULF EEE 25 C6 8 ACIDS CA 6 8 SULF i Gil 26 C6 8 ACIDS CA 6 8 SULF 27 C6 8 ACIDS C4 6 8 SULF ns HPLC Method EE pros water a pfbs water pros water Bam pros water pros water Bm pfbs water pfbs water B= pfbs water BE pfbs water ptbs water Bam pfbs water E ptbs water om pfbs water pfbs water Bm pfbs water 2m pros water == pfbs water pros water EE pros water mmEm pros water pfbs water am pfbs water pros water am pfbs water Bx pfbs water 22 pros water pfbs water vere wre MS TuneFile Inj.Volume Re Fluorochems 15 Ei Fluorochems 15 Fluerochems 15 Amn Fluorochems 15 Fluorochems 15 Amn Flu~rochems 15 Fluerochems 15 Fluorochems 15 EmEdE Fluorochems 15 Fluorochems 15 EEEER Fluorochems 15 ) Fluerochems 15 Em Fluorochems 15 Fluorochems '15 Am Fluorochems 15 Em Fluorochems 15 Sm Fluorochems 15 Fluorochems 15 EE Fluorochems 15 EEEoRm Fluorochems 15 E Fluorochems 15 EEE Fluorochems 15 Fluorochems 15 mm Fluorochems 15 Em Fluorochems 15 EE Fluerochems 15 Fluorochems 15 xnsuo R ws TowznPage 2 Page Position: (2, 1) CONOR iE m 0NPROTECTSGRORR ENTERED EEF CTY CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 swmorsus 3M_MN01539418 11993399..00226677 LISS SYSTEM ANDOPERATING CONDITIONS I LC/MS/MS SYSTEM AND OPERATING CONDITIONS | SpSopnonssoorrPPrroottooccoollNNoo:: NNAA EExxvyegeennSSttuuddyyNNoo:: LL11995588 ' IInnssttrruummeennt:t: MMiiccrroommaassss QQuuaattttrroo UUllttiimmaa ((LLCC//MMSS//MMSS UUnniitt ##66)) | SORS---- Computer: COMPAQ Professional Workstation AP200 ata A Hoot MorsNTVen. Bl Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Mieromass Limited: MassLynx 3.4 Build 004 APLC Bt TerensrPaetrondes1) eis 100t vap der HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Bin Pump HP Vacuum Degasser HP Autosampler HP Column Oven PLCC Gi ems, Sem 1 id 4EoAn D MAES) HPLC Column: Genesis C-8, 5 cm x 2.1 mm i.d. x 4 ~t (Exygen ID: MA0012842) (JONESCHROMATOGRAPHY: Part No. FK5962E) Vltuaitly Ladue Mobile Phase (A)" oh: 1 Mobile Phase (B) : 2 mM Ammonium Acetate in Type I Water Aral KaKT rnaRiskes e i ln. U0 #0 Analyst: Karen Risha Exygen Research 3058 Regearch Drive, State College, PA 16801 PhPohonnee:: ((881144)) 227722--11003399 FFAAXX:: ((881144))223311--11558800 NNOOTTEE:: TTthhheeemnnaeesxxsttl33ynppxaaggseeossfatarwraeercceoopmmrppougutrteearrm.ggeennTeehrreaattpeeaddgeppsrriicnnottnootuuattissnfftrrhooemm the masslynx software program. The pages contain the iinnssttrruummeenntt -- sseettttiinnggss uusseedd ffoorr tthhee aannaallyyssiiss ooff delet tthhiiss ddaattaa sseett.. ' CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00226688 3M MN01539419 i | Scanning Method Report Page 1 Scanning M~thod Report Page 1 MoMLteathshotoddM::odified: CCT::u\\eMMAAMSSaSSrLLIY1NN6XX\\1F~5LL:UU0OO6RR:OO1C2CHHEE2MM0II0C8CAALLSS..PPRROO\VAACCQQUUDDBB\\CC6S 88 AACCIIDDSS CC44 66 88 SSUULFF Last Modified: Tue Mar 16 15:06:12 2004 PPrriinntteedd:: TThhua Mvaarr 1180 0088::0011::4459 22000044 2] 03yp) SSoollvveenntt DDeellaayy (( mmiinnss)) :: 00..0000 | AAFnnuaanllcootgigonCChhiaannnn1eell 44 G:: MUUnnouusfseed5d Mase Pairs (ESP-) Function : I MRM of 5 Mass Pairs ( ESP- ) SIIpnnattneerr ( CChhdaaannlnnteeollns DDee) llaayy ( ( Secs Secs |: ) : 000...000330 SESStntpadaarrnetTi(rTTeiiDnmaeel( toM((niMsnMsiinn) s)s:)) : : 0001...2000.00000 RERenepdpeeaaTttissmCeha: n(neMlinsPoz) en: t Daughter D111 u2e.l0l0 (Secs) Coll Energy (eV) Cone (V Channel Parent Daughter Dwell (Secs) Coll Energy (eV) Cone ( V ) 21 1 232910939.1.000000 29$6999..00.0000 000...222000 20400 I24n09 235: 34335119933910..00000000 8283066..9900..000000 0000...22220000 33I1500 525100O0 4 5 5 4445193390..000000 399699.9.0.00000 000...222000 3I5000 ii1000 | i V ' `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACPOPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00226699 IM_MNO1539420 3M MN01539420 fer. Method Report I Method File= NT. Last Modified~ | mae Printed: i h 3 ve ieeo e sesaves HPII00 LC Pump Initial Conditions AS TSS wane C:~MASSLYNX\FLUOROCHEMICALS.PRO\ACQDDB\pfbs water SETI Thursday, March 18, 2004 07:03=06 enTnevente s ov ere o3efed Thursday, March 18, 2004 08:02:05 --- Page 1 Solvents A% 90.0 B% i0.0 C% 0.0 D% 0.0 Flow (ml/min) 0.300 Stop Time (mins) 20.O Min Pressure (bar) 0 Max Pressure (bar) 40O Oven Temperature Left(C) 35.0 Oven Temperature Right(C) 35.0 ean seman ender Stange HPII00 LC Pump Gradient Timetable soe Fis SMe SH + asian ish 3 4 The gradient Timetable contains 8 entries which are : a y n Time A% B% C% 0.00 90.0 i0 0 0.0 2.00 90.0 i0 0 0.0 5.00 I0.0 90 0 0.0 9.00 I0.0 90 0 0.0 9.50 0.0 I00 0 0.0 14.00 0.0 I00 0 0.0 14.50 90.0 !0 0 0.0 i 35 50 Sestosen ovr sowie 20.00 90.0 I0 0 0.0 HPII00 LC Pump Exte[nal Event Timetable ame D% Flow 0 0 0 300 0 0 0 300 0 0 0 300 0 0 0 300 0 0 0 300 0 0 0 300 0 0 0 300 0 0 0 300 mee Pressure 40O 4OO 40O 40O 40O 40O 40O 40O rap come The Timetable contains 6 entries which are : Time Column Switch Contactl Contact2 Initial Off Off Off 0o00 Off On Off 0.05 Off Off Off 0.i0 Off Off On 11.90 Off Off Off 12.00 Off Off Off aio sssnmtos Ssk at Gomis HPII00 Autosampler Initial Conditions ho "we Draw Speed Eject Speed I~i/min) Beer vies Ss Draw Position (mm) Stop Time (mins) Injection Volume(@l) Be i Vial Number 200.0 200 0.00 20.00 15.0 92 sme Contact3 Off Off Off Off On Off sg Contact4 Off Off Off Off Off Off , CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00227700 3M MN01539421 I [RR -- Tuning Method Report Method: J ---------- Method: C:\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\FLUOROCHEMS [Rr --, var 30 08:02:20 2008 W A Printed: Thu Mar 18 08:02:28 2004 [ Page 1 [R rrANa AE re a CEE Coa enee n BREaEe Sd i pSa ata E iiR i COTES RE EEL T go 1UAiESEIEE Da= 2S99.T00rETTTTTEE Dau 299.00 sons (nse) SOURCE ( ESP- ) captizary Capillary arCone Senagote 1 Hexapole 1 iol Aperture 1 Heels 3 Hexapole 2 E SumSa re. Source Block Temp. se na Set soo 2 3.00 50h I0 &0.0 oe0.0 20.2 D8 100 I00 Rdbk -2.93 -ii i00 Desolvation Temp. 300 299 J-- Pressures snatyser acum Analyser Vacuum ooGas Cell sae Rdbk orsOFF es 2.8e-3 | i seatyaos Analyser aes 1 LM Res 1 whet HM Res 1 Hote IEnergy 1 fs Entrance . Collision Fo)Exit Hier 2 LM Res 2 Be? HM Res 2 Toneser 2 IEnergy 2 LG Multiplier -- Gas Flows cone cas Cone Gas Eenation Desolvation ser nan Set Rdbk 1014.0 1814.0 11.0 La -2 0B 30 PB 2 fo14.0 1:814.0 ht2.0 Hn 650 28 29 31 -648 sakRdbk 1206 129.6 ws 751.3 CCHEOONNNNFEIDFPEIINNTDCIAOELU-NN- TSSTUYUIBBDJJIAEESCCLTTTRTITOCOT AAGPOPRUROROTTT.EECNCTOTIIVV2EE7 -OO0RR1-DD1EE0RR.0E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00227711 Sw umotsssez2 3M MN01539422 1 adnTepinein hedge |QQuuS aannttiitfyy CCIaalliibbNrraattEiioonn NRReeeppooirstttrenn, mxt.Dater03/17/08,Amadystix. isha page 1 Page 1 CCSCaatallsuiiedbbyrrmaaoNttdoiii.oof=nniL=seId9:58,PPF:eil\S\DetWaDatraaNO\c.L19:aC0M\3S11LM37S1C0634H4\A1MA,5a7KssSlE2Eyxb0nt\4.xDW\aFatles~=os0r3io/cy1h7me/ma0i4\c,aFlAisn.PsaPRloROyOr\s\GtoCI=ucEKrV.vhAReeDiDRsBn\h\ia003c311a770l044sA CCGG AACCSFSM | Lbarismteemaordifioedt= FVrEiL Maarr 019 1112=13344=15078 22000048 Printed~ Fri Mar 19 12524=05 2004 [tos | ([CoomCmppooouunsnddoi1fTDnfeaatmecremm:ieCnCaeo6ntAiAo:tccni:daP0P9FR9HA3A757 | [(CCCRGRiaeoalsneeiibpfbesfroriacypantipteisoooenennnttyycocsLppufieuernDv::eseeaEE:rtxe,xt11rtem5eO5r2r2rimn.n.ia0a0alg0l0St:i8S8odEtn*xd,x:,xcA0lA++.or9rcee191ea883,a117W115e..74i4g90hting: 1x, Ais trans: Nono Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None po | 1.54e5- -- . |( a 1 1 | | | | | | | | - RReessppoonnssoer | 1| | | " | || | Or| , , ~ .... , , , ,-. , .... , .... , .... , .... ,ng/L { bo ao oho 6000 ho wooed 0.0 200.0 400.0 600.0 800.0 1000.0 BExayygoenn RReesseeaarrcchh,, 3300S588 RReesseaasrscchh DDrriivvee,, State State College, College, APA 16801 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00227722 _Motsaeezs 3M MN01539423 1 quantity cattbresion tapers - Quantify Calibration Report PRE 2-8 rs Study No.:L1958, Set No.=031?04A, Ext.Date=03/17/04, Analyst=K.Risha Page celtbrarions BY\DMCANLCHENSS asalyme\Pisorochenicale.FRO\CHONNITITON 5 ACS Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\031704A CG ACSFM Last modified= Fri Mar 19 Ii~34:57 2004 Printed: Fri Mar 19 12:24=05 2004 | [ommapmeCaaAGnEPRaOR Compound 2 name: C8 Acid PFOA [Goof eavon. 098657 Coefficient of Determination: 0.999637 Crancna 57 135.0 Calibration curve: 234.327 * x + 2135.08 Rosponsosm Extril i Area Response type: External Std, Area ' |CCuurrvvee ttyyppee:: LLiinneeaarr,, OOrriiggiinn:: EExxcclluuddee,, WWeiegighthitinngg:: 1l//xx,,AAxxiissttrraannss:: NNoonnee: [a2.37e5- vo | | :| | , | | | 1 |i I| | |RResepsopnonsse- ' 1| | | | Vo | yo | | 3) 3000 io oho 0~ 200.0 400.0 600.0 | Exygen Research, 3058 Research Drive, State College, PA 16801 soho 800.0 CHEONNNEFPIINDCOEU-NNTSTYUIBDJIAESCTLTRITCOTACPOURROTT.ECNTG.IV2E7-O0R1D1E0R.8E8N6T2ERED IN I CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00227733 | T0308|" 1000.0 su_wmoresoss 3M MN01539424 ! QQS uuaannttiiE tfyy cCaaS lliibbrraattiioonn RRMeeppioorrett n, mee.oatei03/a7/01, amatystin.nisha rage 3 Page 3 Study No.=LI958, Set No.=031704A, Ext.Date=03/17/04, Analyst=K.Risha Catibration: B.\DAa\LOIENSO\Masslyme\Pluozochenicals. PO\CUEvVaDB\I31T04A Calibration= P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\031704A rrp aad rHheEHon Last modified: Fri Mar 19 11:34=57 2004 CO CG AcSTE ACSFM Printed: Fri Mar 19 12:24:05 2004 | [Eompoumazname: ci Suon PE5S Compound 3 name: C4 Sulfonate PFBS (ConoftDeteerminnatton: 0.833620 (CCCaoalleiibfbfrriacatiteiiononnt occuufrrDvveee::te55r.m.880in04a46ti67o7*n*:xx0++.9559443..67722209911 Responseype:Extomalod, Area Response type: External Std, Area I CuCruvrveettyyppee:: LLiinneeaarr,, OOrriiggiinn:: EExxcclluuddee,, WWeeigihtingg:h1l//txx,,AiAxxinisstgtrraa:nnss:: NNoonnee | sass 5.86e3- to | '| yo 1 || | | | 1 | | | x | | | | | { 1 | | x | ||pre] | || "|i Response- || || | . | | | || | T | T a 0 0.0 200.0 400.0 600.0 800.0 Exyoun Research, 3058 Raseasch Delve, State College. PA 16803 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00227744 [ | 1000.0 aunotsasezs 3M MN01539425 ` Era nnn ras Quantify Calibration Report 0 SLR, sss ssa Study No.=LI958, Set No.=031?04A, Ext.Date=03/17/04, Analyst~K.Risha Page 4 A, Calibration= P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\031704A CG ACSFM Last modified= Fri Mar 19 11:34:57 2004 Printed: Fri Mar 19 12:24:05 2004 oun Frame: Sora PES Compound 4 name: C6 Sulfonate PFHS * Coefficisiententooff DDeetteerrmmininaattiioonn::00..999999770044 a er a2 Calibration curve: 35.2308 * x + 16.7342 rs Response type: External Std, Area 1 [EER cine vasa one | 35604 Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis tran8: None 3.56e4- i xo 1i | || | |1 ` || \ || 1 | Resorse Response || . | | .i | .1 4 t r | an | 0 ........, ....,....., ...., ...., ....,....., ...., .., , ng/L to %o Wo 0 %0 T0008" 0.0 200.0 400.0 ~00.0 800.0 1000.0 1 Exygen Research, 3058 Research Drive, State College, PA 16801 ETN LATTE ATRL ORR NeEneros ' CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 [pT 3M MN01539426 11993399..00227755 | ay Sesion BP Quantify CaZibration Report yA IE BE rs, sussaresenisnions meeipetitontrhe Study No.:L1958, Set No.:031704A, Ext.Date=03/17/04, Analyst=K.Risha REITs SIRR sSASI SI IMA 08 Calibration= P=\Data\LCMSMS6\Masslynx\Fluorochemlcals. PRO\CurveDB\031704A CG Last modified~ Yr Mar 19 ii~34~57 2004 Eoald EE Printed= Fri Mar 19 12:24:05 2004 mgasaneTr crs --r-- cs -- Compound 5 name: C8 Sulfonate PFOS ' Cooeeffffiicciieenntt ooff DDeetteerrmmininaattiioonn:: 00..999955884433 eR Calibration curve: 13.1525 * x + 200.030 eeprom Ses Response type: External Std, Area | CCuurrvveettyyppee:: LLiinneeaarr,, OOrriiggiinn:: EExxcclluuddee,, WWeiegighhtitinngg:: l1//xx,, AAxxiiss ttrraannss:: NNoonnee: votes 1.38e4- TT -- Page 5 ARTE ACSFM . 1 | | 1 | 1 |i |b 1 | |i 1 | i ' | : | | RReessppoonnssee- 1 | x || | vl] | || i . 1 .| | vl 1 co| | 0 . 4 0.0 %0 "ho 50 060 200.0 400.0 600.0 800.0 . Sr, aN E330 2528 Has Tek Sh TAR $n 0 Exygen Research, 3058 Research Drive, State College, PA 16801 '| GONFIDE-NSTUIBJAECLT TO APROTECTIVE ORDER ENTEREDIN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN NE COTY TRIE Soar N37 ure zeses HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00227766 | | 1 i , ng/L T0308" 1000.0 swmorsssezr 3M MN01539427 QqSutuuaadnnyttiiNffoyy. sS1aa1mm1pp5ll8ee, RReeSppatoorrttNo.:031704A, Ixt.Date:03/17/04, Analyst.K.Riska age 1 Page 1 Study No.:LI958, Set No.=031704A, Ext.Date:03/17/04, Analyst:K.Risha LSSaaasmmtpplleemodLLiiifssitt:e:d:PrPP\r:Dd\aDtMaaat\raL\CL2H5CSMMS1SM3S1S3\60M\1Ma3as3sssll2y0ym0ne8x\\PFlluucorroocchheenmiiccaallss..PPRROO\\SSaamppLlaeDDEBN\G03311770044AA CCOG AACCSSFFM NMoLJLLeaaaattsssbhthttooCdommmd:dooo:eddd:iiifffiiieeeddd::: TPTFPhrh1: iua\\DDMMMaaaataterrra\\LL131C869CHMSS0i0HMi99S:S::E36550\11\:M::a300a~s88s-ssl~~L2--y000n0y00x444\nFlxuo\roFchlemuicoalxs.o.oPPvRcReOO\h\,NMeeethhnODBiB\CCcioaottaGGrlroovsvee NNPPDDEESS 003311660044 Job Code : Srinted: Pri vax 19 12:24:08 2008 RBDor~noe ~EE'~1~Cm| TD m' e .~-~]. NTNaaommeat=: 003311770046A--660011 Text= 1:(Cc0s30Ar5ce0it4-de0,pPrF0HiAnng/L Standard XC030504-0, 0 ~ Stsndsrd 10P03311770044AA.-660011 Sm Sm (Mn, (Mn, 2x3) 2x3) | l~n~~ |% EE 1~88--MMaarr--22L00C00/44M00S88/::M1177S::22~1 MRM MRM of of 5LCCChh/aMann5nSne1e/lM3lssSEE2SS#6-9-6) 850 313 > 269 28r50e4a) 2.89e4 131838.68404 | Area | A | [' saae0 rR RAT 2 time { 200~ . 2.00 ~ . . 400. ~ , 4.00 , 500 80 1000 ~ .... ~ .... ~ .................... Time 6.00 8.00 10.00 2: ca acid prox [[XX:CC00C383005A50c04i4-d-00,P, F00OAnngg//hL SSttaannddaarrdd 1188--MMaarr--22L00C00I44M00S88/":M117S7::2#2116 (0317044601 Sm (Mn, 20) MRMof LCCh/aMnnSeIlMsSES#6.| I" 031704A-601 100 Sm (Mn, 2x3) MRM of 5 Channels ES- 4133>5330619] || 502 Arreeaa| | Tol! a -- ES || Id - | C0TT.... ah , .... , .... 2.00 ~ ake .... ~ .... 4.00 , ste .... , .... 6.00 , Tao .... ~ .... 8.00 , woe .... , .... , 10.00 .... Time 3X : :(CC0i4C 30Ss5uu00 4ll-ff0oo,nn3 aa0ttneeng0pP/FLrBSsS5tan0 darrdd40.0 ie-Ma18-rMar-22000400580:117742:211 XC030504-0, 0 ng/L Standard l031704A501 Sm (vn, 28) 1M8R-MMoafr-2LL0CCC0h/4MaMnS0nSI8e/l:MM1sSS7E:S2#-16I loo, 074 031704A-601 Sm (Mn, 2x3) MRM of 5 265250 Channels ES- [= | pd 299>99,3.58e3 | | lems 100~/~0.14 229@0 o37m6 4 453 sss essT7711P55 CB81iN1~l8aR4o0 P99R2255I99N'48991100"1168 me 11 64 | | oer . 655 " " 200 400 500 B00 1000 Time|J 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00227777 SW_MNO1S39428 3M MN01539428 gurizy supe rogers [ Quantify Sample Report BEL ETE Ee rsresn, me pevnsonsa/on, smaiponnsishe Study No.:LI958, Set No.:031704A, Ext.Date:03/17/04, Analyst:K.Risha Page 2 A -- Sample List: ph Eg Last modified: EE Bo raerochmtesi.Pcs on\csrove 1788 07168 Method: FEN Le Last modified: wrJob Code: P:\Data\LCMSMS6\Masslynx\~luorochemicals.PRO\SampleDB\031704A CG ACSFM Fri Mar 19 11:30:32 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031604 Thu Mar 18 09:51:08 2004 pratense var 1 1212000 208 Printed: Fri Mar 19 12:24:08 2004 p---- Name= 031704A-601 Text= csmomcenms X4XC:C0C0363005S50u04l4-f-0o0,n, a00tennggP//LFLHSSSttaannddaarrdd | JJon oncasso1 mun 220 100,014 031704A-601 Sm (Mn, 2x3) 1 00 ...0.14 1188--MMaarr--22000044 0088::1477::2211 LLCC//MMSS//MMSS ##66 Whoot rams 5. MRM of 5 66>60 Channels E8399 > 80 Tosh 8.52e3 | %- \ U | oh aman seae"Rum Te|| 0~'~''~ ''~ .... I .... , .... 2.00 4.00 258 maton og - 5: C8 Sulfonate PFOS XXCC003300550044--00,, 00 nngg//LL. SSttaannddaarrdd | [0317042.601 5m 223) MRM of 5 Channels ES- 031704A-601 Sm (Mn, 2x3) 9.81~ _..11"0~.__~'5-.5~6 .... , .... , .... , .... , .... , .... , .... Time 6.00 8.00 10.00 1188--MMaarr--22000044 0088::1177::2211 LLCClIMMSS/M/SM#S#6 MRM of 5 Channels ES- || : oar esoasivcesd 9.27 5.94e3 Area p | wd l e ee E rm e sh e ,,2,0.0... , ....40, 0.... , 60, 0 , 80, 0 , ..1..00, .0... , .... Tiimte) 2.00 4.00 6.00 8.00 10.00 Seren Research, 3048 Repose Brive, Sate Subieg, TA 1803 Exygen Research, 3058 Research Drive, State College, PA 16801 COENFIDEENTICALBSAUBJhECeT y10APSROETREGTvIoV5EoOROeER rENTERED IN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00227788 -- 3M MN01539429 smi ere rr J Quantify Sample Report SAT BIA ae puemts riot, esate iain Study No.=LI958, Set No.=031704A, Ext.Date=03/17/04, Analyst:K.Risha Page 3 re i TruPte err Sample List: Last modified: BEi tennant ons 201 Method= Last modified= oes Job Code= p:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\031704A CG ACSFM Fri Mar 19 11:30=32 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove ~TPDES 031604 Thu Mar iS 09=51:08 2004 Printed= Fri Mar 19 12:24:08 2004 -- Name= 031704A-602 =Text: Cecsiema i: C6 Acid PFHA (KC030504-1, 25 ngiL. Standard XC030504-1, 25 ng/L Standard |00331t770044An.-680022 Sm Sm (Mn, (Mn, 2:3) 2x3) P| F| -lI o/,~ |I a MAE 2.00 4.00 6.00 route smn 9 2:: 0C88 AAcciidd PPFFOOAA cure [x'XcoC30035005a0-41-,1, 2255 nngg//LL SSttaannddaarrdd | i031704A-602 Sm (Mn, 2x3) -- | eEeTrE 100) 2.00 4.00 6.00 a 7188--MMaarr--22000044 0088::3399::0044 bsoo8.60 LCL/CM/MSS/IMMSS##66 MRM of 5 Channels ES. | MRM of 5 Channels ES- = 313 > 269 56371~ 3A.5Ar8ereaa4) | MEYT A ne|] 8.00 10.00 99..0044 7657i 1188--MMaarr--22000044 0088::3399::0~1 in LC/MSlMS #~ Ss MRM of 5 Chan44n11e33ls5>3E38S69-9 E 4.65e4 IE ||me} 8.00 10.00 3X:(CCC0043300S55u004l4-f-1o1,n, a22t55e nnPggF/lBLLSSSttaannddaarrdd ; ; es (|o1704n602 5m vn, 22) 031704A-602 Sm (Mn, 2x3) op PEE 0.14 Io tr1.1e2 11.5s3i20, 250390 490 52650 69s 3.90 4.90 5.92 6.50 6.96 8 78s|) MRM of Channels ES- LCMSIMS 1188--MMaarr--22000044 0088::3399::0044] MRM of 5 Channels ES- 299 > 99r O [10180.787 ner | 1.34e3I 11.81 i o | ofLogg 22E e ze 202%ST R 09r 0%5%,7E LES MeIpeTe 2.00 4.00 6.00 8.00 10.00 Time seg Settee, 3430 wsbseh Som dan rene 8 4400 Exygen Research, 3058 Research Drive, State College, PA 16801 COS NFIDENTA IAL SUBJR ECTT0 API ROTECTIVTE OREDERIsENTERED CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00227799 sao 3M MN01539430 1 PT rr Quantify sample Report | BLE ET creas, we oveon/an/oe, sneipenin viene Study No.=LI958, Set No.:031704A, Ext.Date:03/17/04, Analyst=K.Risha Page 4 sample Tiss Feu apr assossenteeLe FRCNSRRSTOTTOM 5 CEE Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\031704A CG ACSFM rp ppg | MmLeeattshhtooddm:=odified: PPF:=ri\\DDaMatatara\\LL1CC9MMSS1HM1SS:6630\\:MM3aa2ssssll2yy0n0nx4x\\FFlluuoorroocchheenmiicaclasl.s.PPRROO\\NMMeetthhDDBB\\CCoottGGrroovvee NNPPDDEESS 003311650044 EE rea, Tae SEE Last modified: Thu Mar 18 09=51:08 2004 Le Job Code= 1 PrPirinntteedd:: PFrrii MMaarr 1199 1122:=2244::0088 22000044 I mNTaaemxxete:=s 031704A-602 IS | 4[XX:CCC0063300S55u00l4-f-1o1,n, a22t55e nnPggFl/HLLSSSttaannddaarrdd os1701n502 50m 263) 031704A-602 Sm (Mn, 2x3) o| 1188--MMaarr--22000044 0088::3399::00:4 {imams LC/MS/MS #6 oss NofSCM rmne5e. MRM of 5 Channels ES- 8.85 887733 - 39559..11>99e86330 A~a | | in ree am an w RA e 2.00 4.00 6.00 8.00 10.00 cosx sggazetmnemnge2r70s8 5: C8 Sulfonate PFOS ostroin02.i5.m 223 |XXCC003300550044--11,, 2255 nngg//LL SSttaannddaarrdd [ 031704A-602 Sm (Mn, 2x3) w1fi oz WR ofS Croemos5n. 494.201 1188--MMaarr--22000044 0088::3399::0044~ LLCC//MMSS/IMMSS ##66I MRM of 5 Channels ES-I 26063 499 > 99 2.80e3J Area Pen Drm LL rrrrr rrr Cp 22.0000 4040 .00 --~ Epps -- TE 6060 .00 880.000 10100.000 Exygen Research, 3058 Research Drive, State College, PA 16801 EE -- en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00228800 pr 3M MN01539431 ) Quantity sample Ropers res Quantify Sample Report I Ee nreen, me maters3/27/08, ansiyenik.Riehe Study No.:LI958, Set No.:031704A, Ext.Date=03/17/04, Analyst:K.Risha Page 5 Fr -- Sample List: Ea methane io Trrsb in Tos Last modified: | Emon ete\LOWbiS ans yaa Fluorochemicals.FRO\MethD\Cotarove NEDES 631604 Method: [RS de Last modified: eet Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\031704A CG ACSFM Fri Mar 19 11:30:32 2004 P:\Data\LCMSMS6\Massly~x\Fluorochemicals.PRO\Metb_DB\CotGrove NPDES 031604 Thu Mar 18 09:51:08 2004 | rrimeds vet ar 19 s2eaer0s 7000 Printed: Fri Mar 19 12:24:08 2004 ranar SriToRne Name: 031704A-603 Text: GT31o700A.603 Sm vn28) Li:icC6shActiad mPFe~nIA xXCC003300550044--22,, 5500 nnogl/Lt SSttaannddaarrdd 031704A-603 Sm (Mn, 2x3) . *1001 - Ea8.s5So9 9780i SE 1188--MMaarr--22000044 0099::0000::4466 LLCC//MMSS//MMSS ##66 MRMof Grannos E5- MRM of 5 Channels ESTi3o0 313 > 269 ares| Area) 6.02e4Area | o 0r~b ,,,,e .... r , .... , .e ... e, ...e. , ...r . , .e...e, .... , .... , .... , ....~TTiimmeo| 22..0000 44..0000 66..0000 88..0000 1100..0000 U 2:cs ned son I 2:C8 Acid PFOA XC030504-52,0 ng Standard 18-Mar-2004 09:00:4 XC030504-2, 50 nglL Standard ||o331%7044.603 Sm vn 2) o=c MRMof 5 ChanSnelvsofere5-ee 031704A-603 Sm (Mn, 2x3) 18-Mar-2004 09:00:4t~ LLCC/lMMSS//MMSS #~ 9.04 MRM of 5 Channels ES413 > 369 8.67e4 Area I = seme Time| 0-v,,''-~-/,', ,~ , i , ,~ .... i .... ~ ;,,,-i , , ,-~-~-, , . , LTTETTA eh sm eee) 2.00 4.00 6.00 8.00 , , , , ~ Time 10.00 B 3:C4 Sulfa onate PFBn S main [XG030504-2, 50nolL.Standard T6-Mar 2004 09:00:4 XC030504-2, 50 ng/L Standard o0r31708003 Sm n20) MRMof 5 Channels E5- 031704A-603 Sm (Mn, 2x3) 0 ey 1"'~ | rea vv~ %| eA mn Jt Ansineahndhn umnbut. L 22..0000 44..0000 A 66..0000 8.28 338844~ ---- 18-Mar-2004 09:00:46 LLCC//MMSS/IMMSS #6 MRM of 5 Channels ES299 > 99/ 225.522ee33| PASTA 88..0000 1100..0000 Time J Sargon Tesesceh, 3058 Research Drive, State College, PA 16903 Exygen Research, 3058 Research Drive, State College, PA 16801 CCHEOONNNNFEIDFPEIINNTDCIAOELU-NN- TSSTUYUIBBDJJIAEESCCTLTTRTITCOOT AAGPOPURRROOTT.TEECNCTOTIIVV2EE7 -OO0RR1-DD1EE0RR.0E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00228811 Sw umorssses 3M MN01539432 | QQSuuaaEnnttiiEffyy sSIaammppEllee RReeippeoorrteoamroun, sxe pates03/17/04, Anaiyssik.nisna rPaaggee 66 Study No. :L1958, Set No. :031704A, Ext.Date:03/17/04, Analys~:K.Risha [I LLSSaaaassmmttppllmmeeooddLLiiiiffssitti:e:edd::i\PFFeDr:\iai\tDDatMMa\aataLrca\C\LHL119S9CHHMSS11M1SR1:S\336N0\0\a1k:Ms3a3as3a2sLssyl212m0y0c00ny\44xF\alFul\ouroProoLcchhueenmoiiccxaalloas..cPPPRRhROOO\e\NSGaasaLmphpilDlaceRDD\EaBC\\o0l0t33r1s17o70v.04e4AANCCDGGEAACC0SS3FP1M604 LoMLeaabtsahttoCdmom:aoondd:iifeiieedd:= Thu Mar 30 03051108 2004 P:\Data\LCMSMS6\Massly~x\Fluorochemicals.PRO\MethDB\CotGrove Thu Mar 18 09:51:08 2004 NPDES 031604 Job Code: | pPrriinntteeads: eFrti Maarr 1139 11220:22040:0008 22000048 TaNamemeem:= C03311770044AA--560033 Text= 44: :Cc6o sSuurlffoonnaactee PpFoHmSs [[X1X0CC3001337000554008440--322,,S55m00(Mnnngg,//LL26SS3)ttaannddaarrdd 031704A-603 Sm (Mn, 2x3) oo 1188--MMaarr--22L00O00M44 S009I9::M00S00::#446~6 MRM of 5LCCh/aMnnSeIlMsSES#-~ MRM of 5 Channels ES- [10 as 36650 " 189.8168 39T91>00840 1 Areal 1.10e4 A~a *] iNSE tne | 22.0000 44.0000 86.0000 88.0000 1100.0000 J 5: co sulfonate pros 5:(CC0830S5u0l4-f2o,na5t0e nPgF/OLSStandard 18-Mar-2004 09:00: XC030504-2, 50 nglL Standard 18-Mar-2004 09:00:46 | 00033171074A0-6403ASS.mm6M(0Mn3n,, 2x3) 2x3) MRMof 5LLCCC/h/MMaSSn//nMMeSESlS#s-6 921 MRM of 5 4993>9 Channels ES- 9.21 499 > 99 | 900 "real 44.8811ee33)~ Area ||Lo TT ee abe eee eae ae se en Time Time 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReessesazrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166080011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00228822 _MNO1S39433 3M MN01539433 I | QQSuutaaunndtytiiNtfoyy.rSsLaaimm3ppSllsee, RReeSppeboorrttMo.:031704A, Ext.Date:03/17/04, AmalystiK.Risha rPeaggee 7 Study No.:LI958, Set No.:031704A, Ext.Date:03/17/04, Analyst=K.Risha | LMLSSaeaaastsmmthtppolldmeme:ooddLLiiiiffssiitte=e:dd:: PFFPrr:P1iii\\\DDMMDaaaaAttrxtaaa\\\LL11LC99CCHMHSS11SHM11MS:S:S33\6E00\N\=:MN33aaa23sssssl22i0y0sy00nm4l4xx\y\FFlmiuvoxorr\ooccThhelemaiuiccoaallrss..oPFPRRcROOO\h\\SKSeaeamEmnAppIlliBee\DcDCBEoa\\t0GlG331o1s77v00.e44AANPCCDGGESAACC0SS3FF1M604 MLoLeaabtsshttoCdmom=dooedd:iirfiieedd:: Thu Mar 18 09:51:08 2008 P=\Data\LCMSMS6\Massly~x\Fluorochemicals.PRO\MethDB\CotGrove Thu Mar 18 09:51:08 2004 NPDES 031604 Job Code= [Er Printed: et wax 15 12024108 2008 Fri Mar 19 12=24:08 2004 NNoammae:= 003311770044A--660044 Text= [1i::XCc0Ce6305aA0cc4ii-dd3,pPrF1iH0nA0 ngiL Standard SE XC030504-3, 100 ng/h Standard 031704S6m i04, 220) MRM of 5 Ghannol ES- 031704A-604 Sm (Mn, 2x3) 100]1i)1 /lO,~ 1889.5640000 19409~ 1188--MMaarr--22L00C00I44M00S99I::M22S22::3#3262 LC/MS/MS #6 MRM of 5 Channels ES- 3135 269 313 > 269 1.1265 1,12e5 Areal Ama | ~ 250 Orme 0-~;, , , , .... , .... , 4% .... , , ,-, 600 ..p.e.pp.er, .... ,,,, 800 RS T; ,-~-~, , 1000CT Time .... , .... ~Time | 2: C8 Acid pron 2.00 4.00 6.00 8.00 10.00 ESSSAZ, Wow 2: C8 Acid PFOA XC030504-3, 100 ng/L SSatanntdaarrds 1188--MMaarr--22L00C00I44M00S99I::2M22S2::33:2 0i03311770044A4-660044 Sm Sm (vn, (Mn, 263) 2x3) 504 M MRMoofR f 5LCCChha/MM nann4Sen3le/Msl>sS3EE6SS#-9-6 || 279.0048 4131>.r535e66a95 1.55e5Area L| TT , .T..e. e, .... , ....aw,, ,~ , , ....ew, .... , ....Bre,l o.2.7.9.66, ~....0,,0~,,, .... " TTiimnea 2.00 4.00 6.00 8.00 10.00 f3[X:vCC04s30e5S0ul4l-ft3o,nea1te0e0rPnFegB/SsL Standard XC030504-3, 100 ng/t Standard | 1000310371|0740A4-860044 Sm Sm (Mn, (Mn, 253) 2x3) I00~ " 5 T168--MMaarr--22L00C004M4 S009I9::M222S2::33:2 88a.3311 MRM MRM of of 5LCCChh/aMannnSn2e/elM9lssS9EE>SS#-9-6 29"940>09093 611 ] 4 00e3 || oI e L 200 400 2.00 4.00 -- 600 800 6.00 8.00 AL Time 1000 Time j 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR-2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00228833 IM_MNoTS343 3M MN01539434 -_-- | | gQSeuuudaaynnNett.iigfiyy5SS5aamm0ppll,ee RReeSppetoorrteMo.:031704A, Ext.Date:03/17/04, AnalystiK.Risha rage 8 Page 8 Study No.:LI958, Set No.:031704A, Ext.Date=03/17/04, Analyst:K.Risha LMLSSaaaaassmmtttpphllememerooddLLiiiiffssiitte:e:dd:: P PFPPrE:iLi\D\iNMaDaatrraa\\ tL1195aC~\S11DLM11S:1C363a 0H0\N:1MS3a3a23MsstssSLl22Ey0y00m0n\a44xxN\\PFaLl\suucosFrloL occyhhmeeCnmcii\caalFUlals..uPPBEoRRROOOrV\\oN MSSeacatmmhhppSDlelBeaa\DDCBiBo\\ct00G3a3z1\lo7TOv0sMe4.AAKFCCDGGESAACCS0SI3TV1E~604 MTLLeaaotssbhttocdmmo:ooddad:iiffiieedd:: Thu Nak 16 03:53:08 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Thu Mar 18 09:51:08 2004 NPDES 031604 Job Code: PPreiinntteead:: PFerti aMaxr 1195 11220:22441:0008 22000084 Names 0317042604 Name: 031704A-604 Tt Text: a:ce sutton pene 4:C6 Sulfonate PFHS [XXCC003300550044--33,, 110000 nngg//LL SSttaannddaarrdd osvr0in04 sm on 20 0317045604 Sm (Mn, 266) 100) 031704A-604 1 Sm (Mn, 2x3) i %1 a. 22.0000 44.0000 sicosufonaterros 5X:(CCC0083300S55u004l4-f-3o3,n, a11t00e00 PnnFggOllSLL SSttaannddaarrdd 1l" 1 f 031704A-604 Sm (Mn, 2x3) 1188--MMaarr--22000044 0099::2222::33221 LLCC//MMSS//MMSS #6 #.~ MRM of 5Chennels 5- MRM of 5 Channels ES-. 7 39>80 78.5897 39290>7e840! ea) 3759L 2.07e4Area rrp BreERTtie | .... , .... , .... , ;~ ........... .--7-, Time G00 800 000 6.00 8.00 10.00 uot Chamois 5. 18-Mar-2004 09:22:32 LOMSIMS#6 18-Mar-2004 09:22:32 LC/MSlMS #6i 991.199. MRM of 5 499> 99] Channels ES499 > 99 6a Bo7e3 8.97e3 "area Area |Io OTTTS T TN RAST A" Tim 200 400 500 800 100 Time 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00228844 _MNO1S39435 3M MN01539435 e --e ---------------- | | qQB uuaannttiiE ffyy SSaaE smpplloe RReeSppioorrttNe. oomroun, mxt.pater03/17/08, Anayssik.nisha aPaggee s9 Study No.=LI958, Set No.:031704A, Ext.Date:03/17/04, Analyst=K.Risha | GeLSSaaaatsmmshtppllomeemsooddLLiiiiffssiittee::dd:: P PPFF\rr:iiD\aDrNMtaaaetrr\a\L\LC1195CHMSSM11DM1S1S:1E363\A 00\NN:1Maa33asa23ssR sslLl22yyy00mm00nca44xx\\\FFPil\ uLuouorCrooL ocCchhheeenCmRiicCcaaaH lllsas..PPFSRRROOO\\KN SSAaAEnER~pDSlLEe\aDCnBoRS\t\0G03r31o1\7vTa00,44ANNECCDOGESAACCS03FS1M604 MTLLeoaatbsshttocdmmo=oocdda:tieftieedd=s Thu Nar 16 03151108 2008 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Thu Mar 18 09:51=08 2004 NPDES 031604 Job Code: | rence Pet wax 15 12024100 2008 Printed= Fri Mar 19 12:24:08 2004 NNpaamm=ees= 003311770044A2-660055 Text= ice rciamn XiX:CC00C363005A50c04i4-d-44,P, F22H55A00 nnggi/LL SSttaannddaarrdd 00p3311i770044A6-60055 Sm Sm (Mn, (Mn, 266) 2x3) ] 168--MMaarr--22L00C00I84M00S99I::M4444S::11#115 se MRM MRM of of 55LCCChh/aMannHnSneoe/lMlsssSEE2SS#0--06 4810.6405 2305 313 > 269 2.34e5 1 or * | Area || 0~'''', ....20, 0.... ~ ...."0, 0.... , ....50I 0.... , ....50, 0..A .. , ....w, ..o .. , .o ... ) Ttimme 2.00 4.00 6.00 8.00 10.00 Se atm-- TT |2X:(CCC0093300A55c00i44d--44,P, F22O55A00 nngg//LL SSttaannddaarrdd 1168--MMaarr--22L00O00M44 S00I99::M44S44::1#1116 -- (003311770044A2-660055 SSmm ((MMnn,, 22:x33)) 00 MMRRMMooff 5LCCChh/aMann"nSn1ee/l3Mlss>SEE3S#S0-06-| S290.048 32ce5 413 > 369 3.26e5 Area i | ob 200 a0 2.00 4.00 33X::C0Cc3t~05sS0uu4ll-ff4oo,nnaa2tt5ee0 PonFgrB/sSL Standard XC030504-4, 250 nglt Standard pJ0o3os11770044An-.60055 5m Sm (in, (Mn, 29)2x3) |i | he EE 200 400 2.00 4.00 | 500 B0058208~ c10r00 eme Tir Time }| 6.00 8.00 10.00 _ 6188--MMaarr--22L00o0044m00s99:M:44S44::1111 a3 RM MRM of of 55LCCChh/aMannnSn7ee/lMlss9SEES>S#--6 188.3019 29B9or>et9ae9l ee 5006.00 8008.00 1100.0000 EExxyyggeenn RReessseaarxcchh,, 33005586 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- TSSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV27EE-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00228855 _MNO1S39435 3M MN01539436 ' | qQSuutaaenndtytiiWtfeyy..SsLaaImmspp5ll8ee, RRSeeepproorsttNo.:031704A, Ext.Date:03/17/04, Anslyst:X.Risha PPaaggee 1i00 Study No.:LI958, Set No.:031704A, Ext.Date:03/17/04, Analyst:K.Risha LSSaaesmmtppllemeodLLiiiessitte::d:P:PP\r:Di\aDMtaatara\\LL1H9CSMH1SS1MS:S\36M0\a:Ms3as2slsyl2my0x0n4\x\PFlluuoosroocchheemmiiccaallss.PPRROO\\SSaAmEpplleeDDBB\\0O33117T0O4NA CCOG AACCSFSM [LLM= aeastshttodmm:ooddiitflieedd:: TPFPhr:1iu\\DDNMaaacatarra\\LL11C69CHMS0S1H3M1S1S:E53610\\:1MN30aa2s6sss2l2L0y000ny44x\nFlxuo\roFchlemuicoalrs.o.PPRRcOOV\hMMeeethhnODBBt\CCooottaGGrrloovvsee NNPPDDEESS 003311660044 JLaabstcmodoedsified= Thu Mar 18 09=51:08 2004 Job Code: I ePrrtinneteeads= Pet MMaarc 1199 1122::2244::0088 22000044 | aTNamometess: o0s3i1v7a0s4nA--6s0o5s Text: | 44[:X:CCc06o30Ss5uu0ll4ft4oo,nnaa2tr5ee0 PpnFgrH/sSL Standard XC030504-4, 250 nglh Standard "ol |1031704605 Sm (Mn, 253) bf | 031704A-605 Sm (Mn, 2x3) | | 1188--MMaarr--22L00C00M44 S00I99::M44S44::1111 #5 sss MM RMoofR f55LCCChha/MM annnSne`IeGlMalssnScEEeSSl#-o-6| a58.85 Cancel[9 W7vteea4l| 4.78e4 Area ] 200 400 600 800 1000 Time 2.00 4.00 6.00 8.00 10.00 55::6C8 Ssuullffoonnaattee pPFrOoSs i(XXCC003300550044--44,, 225500 nngg//LL SSttaannddaarrdd 1188-.MMaarr--22L00C00I44M00S99I::M4444S::1#1115 00313011077,10044A4-660055 $Smm ((MMnn,, 22xx33)) E99X.2211 MRM MRM of of 55LCCChh/aMannnSn4eIelMlss9S>EES99S#-9-6 4919.9>08949! i oa 3392L 1.90e4Area 1| ph20r 0 r00---- 600 ---- 800 --1-- 000 -- Tr|e 2.00 4.00 .... , .... , .... , .... , .... , .... , .... Time 6.00 8.00 10.00 EEAx~yyggeenn RReesseesasrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00228866 SW_MNO1839437 3M MN01539437 [ oI qQuuaannttiiftyy sSaammppllee RReHeppeoorrtot a0an, mxt.Daten03/17/08, Ansdyetix. isha rage 11 Page ii Study No.:LI958, Set No.:031704A, Ext.Date=03/l?/04, Analyst:K.Risha WU eSLLSeaatmmsv~htpelolememsoodLLdiiiifssttiti.:eedd: PFmEir:P\di\rDD\aMwaDtaetRsrraC\\aLL1\1C95CLHMOESH1TNM1SLS:SiME3a6S00\EH:iMWa33aans2sssss2yl2l0yy00mnm84xcX\\FF\lluuFocrrlooccuhheeommiirccaaollssc..PPBhRRROOOe\\MSSSnaammhippDllcBeeDD\aBEC\\ol0OG3Srs1Io7Tv.0Oe4NAANECCDGOESAACCSS0F3T1ME604 MLLTeaaotssnhttocdmom:dooeddriitfiieedd:: Tha Mar 16 03151108 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Thu Mar 18 09:51:08 2004 NPDES 031604 Job Code: 1 pPrriinntteedd:: FPrrii MMaarr 1199 1122::2244::0088 22000044 me Name: ona 031704A-606 T3.extc:e eid orn 1 ,XXC:C00c363005A5c00i44d5-5,P, F55H00A00nnggi/LLSSttaannddaarrdd , 031704A.506 Sm (Mn, 260) 031704A-606 Sm (Mn, 2x3) | | "i wns es oo _ 16.Mar-2004 10:05:57 ry 18-Mar-2004 10:05:51 LOMSIMS # LC/MS/MS #6 MRM of Channe>ls E2S0-0 MRM of 5 Channels ES- 8.60 313 > 269 4.8AAr3reeeaa5) | | 0-~,, , ~ 206 .... ~ .... ,, , 00,, .... ~ 500 .... , .... , ho .... , .... ~ Too .... , .... , .... TTiimme|e 2.00 4.00 6.00 8.00 10.00 | [22::KcocCso805An0ce4ia-d5,pPrF5oO0nA0 gi StandarI d _ SE 18-Mar-2004 10:05-:51 XC030504-5, 500 ng/L Standard | 00I3311770044A4-660086 Sm Sm (Mn, (Mn, 20) 2x3) 900 18-Mar-2004 10:05:51 LCIMSIMS LC/MS/MS #~ MRM of ChanpneilsrESe- MRMof5 Channels ES- Ti9o.0e4ss 413 > 369 65r50e5a, 6.56e5 \% | Area , ||Lof TT a0 3%) 50 1000 re Time|| Time 3: ct suionate 2b.0r0as 4.00 6.00 _ 8.00 10.00 . XC030504-5, 500 3:C4 Sulfonate XC030504-5, 500 ng/L PFBS ng/L SSttaannddaarrdd 1788--MMaarr--22L00C00M44 S110I0::M00S55::#55611 00o3311o7700448A.-660066 Sm Sm (Mn, (Mn, 23) 2x3) 831 MRM MRM ooff55LCCChh/aMannnSnTeeIloMlssoSE-5S%#--60| 8.31 299 > 99 . 1 0 pe | % 1.88e4 rea} Area ol' Op 260 p ao e500e 800IA 1000 Time Time j 2.00 4.00 6.00 8.00 10.00 i Exygen Research, 303 Reseach Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 1 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993309..00228877 m_Motsaoess 3M MN01539438 ' | qRQuuaaEnnttiiftyy sSaammppllee RReeRppeoo.rrctt on0en, mer.Date:03/17/00, amsdyscix. isha rage 12 Page 12 Study No.:LI958, Set No.=031704A, Ext.Date:03/l?/04, Analys~:K.Risha | MLSLSeaaaatssmmhttppollammeerooddLniiiiffssiitt:=eedd=:Pr7FPF\Er:D\)i\aDDtaNMaataate\rka\L\LCL11CH99CuSMEMS11MS1M1SE1S=E\336\0W0\H1=aMa33sas32sssls1yl22y00mym00nex44x\\\PFFllluuuccorrroooccchhheeemamiiicccaaalllsss...PPPRRROOO\\\MSSSAatEmhppDllRaeD\DECB\O\Ot03G3IE17?O00V44AANFCCDGOESAACCS0SF3I1M604 MLLGeaaotsnshttocdomm=sooeda:itfeiseedd:s Thu Nar 16 0315110 2008 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Thu Mar 18 09=51=08 2004 NPDES 031604 bo JaoetbatCeoadse= ret a 19 12124108 2008 Printed: Fri Mar 19 12:24=08 2004 Names 0317042606 Name: 031704A-606 Text= 44.: 0C66 SSoullfofnoatneaPPYtFHHeSE 0O31s704A.608 Sm (Mi, 263) |XXCC03300550044--55,, 50000 nngg//LL SSttaannddaarrdd i 031704A-606 Sm (Mn, 2x3) 1 -- -- - pa 1188--MMaarr--22000044 1100::0055::5511 LLCC//MMSS/lMMSS ##66 as MofR ChaM nne3l5s>ES0-0 8.87 17820 MRM of 5 Channels ES- 39999..77>44ee8404| `roaArea | 200 pr 500 2.00 4.00 6.00 55::(CcC0oB30Ss5uu0l4i-ft5oo,nnaa5tt0ee0 PpnFrgOoiSsL Standard _ XC030504-5, 500 ng/L Standard 003311770044AA--660066 SSmm ((MMnn,, 22xx33)) |fe?| * 200 a 500 2.00 4.00 6.00 008.00 _ i.794.8219 a6 8.00 000 Time | Time 10.00 18-Mar-2004 10:05:51 18-Mar-2004 10:05:51 LLCC//MMSS//MMSS #4 ees MMRRMM ooff 55 CChhaannnneellss EESS-4.034] 499 > 99 = 4.03e4 | 1000 or TTTiiimmmeee 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, FPAA 1166880011 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- TSSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV27EE-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00228888 _MNO1S39439 3M MN01539439 | QQuuaannttiiftyy sSaammppllee RReeppoorrtt. | Study Mo.:11958, Set No.:031704A, Ext.Date:03/17/04, Analyst:K.Risha PPaaggee 1133 LSSSaatasmumtppdllymeeoNdoLL.iiifss:ittL::e1d9:58,PPPri:i\\SDDetmaaatarNa\o\L.LC1:C9H0MS3S1K11MS71SE036\40\MA1Ma,3as3sssll2Ey0yxm0tnc4.x\D\FaFltlueuo:or0ro3oc/ch1he7em/mi0ic4ca,allsAs.n.aPRlRoyO\s\StSa:amKmp.plRleiesDDhBBa\O03311T7O0N4AA CCGO AACCST~H | MLTwLLeeaoaattsnsshntttoocdaommm:rtooomadd:iiitffiiseeeddd==s P TPFhr:ii\DIHMaaatrra\\L1196CMS01DM311S=53S10a\1H=M03aa82sstssl2120yv000Ena44ex\\FFll\uuoorrooLcchheenCmiiccaaHllss..PPERROO\\MNMeatthhSDOBB\\CCEoottGGrr\oovvee Thu Mar 18 09:51:08 2004 NNPPDDEESS 003311650044 Job Code: | primes ed war 19 12:20008 2008 Printed: Fri Mar 19 12:24=08 2004 | emer caradn-cor Name: 031704A-607 1: ce nia pen _ , Text= | iX[:XCC0C063300A550c04i4-d-66,P, F11H00A0000 nngg//LL SSttaannddaarrdd If00331177004A4-660077 Sm Sm (Mi, (Mn, 263) 2x3) |* s15e158.60 151544-~ --_ 1188--MMaarr--22L00O00M44 S11I00::M22S77::3344 RM MRM of of 55LCCChh/aMann3inSn1eae/3lMlsss>Se2E2S0#6d.969 ea 8.32e5 | Area 1 , ...2.0.,0, ,,, ....",0.... , ....50, 0.... , ....50, 0.... , ....00, 0.... , .... TTiimnee 2: conctap2r.00on oo 4.00 6.00 _ 8.00 _ 10.00 _ 2XX:CC00C338005A50c04i4-d-66,P, F11O00A0000 ng ng/L SSttaannddaarrdd 1188--MMaarr--22L00O00M44S11I00::M22S77::3#3464 LC/M$1MS #6 |oorroen07smn 20 MRMof Gramel 5. 100,1 031704A-607 Sm (Mn, 2x3) zsao9e.e0t4es MRM of 5 Channels ES- 4135 369 413 > 369 T3008 1.30e6 i ea *] 2366851 Area | - Time| 0~ .... , .... , .... , .... , .... , .... , .... Time LTT eT e aeTTTeeTakeTree 2.00 4.00 6.00 8.00 10.00 33[: X:sCCC0ut43l05Sf0uo4l-fn6oa,nat1t0ee00pPFnrBgSe/LsS_ta_nd_ar_d _ XC030504-6, 1000 ng/L Standard 10P3013o710740A4-660077 Sm Sm (Mn, (Mn, 263) 2x3) 1 *i SE saa8a.3t1 SE16-Mar-2008 10:27 1W8R-MIaorf-25LL0CCO0hl4aMMn1nSSe0/MlM:2sSS7E:S3#-~t] MRM of 5 2039075694 Channels ES299 > 99 3.07e4 | AAvreesa, | ob2e 00 r40 500 80B 0 e 1000 e iTimmTMee| 2.00 4.00 6.00 8.00 10.00 Exygen Resescch, 3050 Ressazch Drive, State College, PA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00228899 _MNO1S39440 3M MN01539440 I quantity sample napers rage 4 Quantify sample Report |B Ne ovmronn, mx patessa 17/00, amipec. isha Study No.=LI958, Set No.=031704A, Ext.Date:03/17/04, Analyst=K.Risha Page 14 Semis stato \oucs\cuuSE asm oroshanicnte BRO\SRmLSTR\O00 3 Aca Sample List: i, Last modified= LE orbstagstyi iscrochenical. 770etso8\cosczove NEBES 031604 Method: Frac Last modified= a Job Code: P:\Da~a\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\031704A CG ACSFM Fri Mar 19 11=30:32 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031604 Thu Mar 18 09=51:08 2004 ' PPrriinntteedd:: PFrrii MMaarr 1199 1122:=2244::0088 22000044 Name= 031704A-607 i: cs surtonce seus Text= 4:C6 Sulfonate PFHS [XXCC003300550044--66,, 11000000 nngg//LL SSttaannddaarrdd ; wy1003311770044AA--660077 SSmm ((MMnn,, 22xx33)) %- 7% we i 2.00 4.00 6.00 5:C8 Sulfonate PFOS ou 1701507 5m 0. 20 X(C0C30300550044--66,, 11000000 nngg/lLL SSttaannddaarrdd 031704A-607 Sm (Mn, 2x3) i| d E | * 1~! I 22.0000 "440.000 56.0000 =os8.86 eh A 8.00 _ ETeeEnse 1188--MMaarr--22000044 1100::2277::334, LC/MS/MS #5 MMRRMM ooff 55LCCChh/aMannnSnee/lMlssSEESS#--:' 399 > 80 1.93e5 Area Ww ~ 10.00 TTiimmee | 1188--MMaarr--22000044 1100::2277:3:3:4 LLCC/lMMS$//MMSS #6 Wet or 5 Cram 5. MRM of 5 Channels ES- oar Ts 9.21 499 > 99 Hs Foon 7.50e4~ Area| Area - - Te | 88.0000 13775~ 1100.0000 Time Exygen Research, 3058 Research Drive, State College, PA 16801 CORNEFRINDEERNNTICAOLUNSTUYBDIIESCTTRITCOTAPCROUORTTE.CNTOI.V2E7O-R01D0ER20E5NT2ERED CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00229900 au nissast 3M MN01539441 QSQiuuaaadnnyttiiNftoyy.sS1aa1mm1pp55ll0ee,RRee`SppaoocrrNtto.:031704, xt.Date:03/17/04, AnalystiK.Risha Sage 15 Page 15 Study No. :L1958, Set 1;o. :031704A, Ext.Date:03/17/04, Analyst=K.Risha NLSLSaaaaatssmmhttppolldmmee:ooddLLiiiiffssiitt.:eedd:s PFPPFr1r=:ii\\DD\MaNataatDarraa\\LL11tC99CHMaSS1iH\1MiS1S:L336\00\CK1:Ma33Ha3a2sIss1l22My00ym00nSx44xG\\lF\ulcuKornroocschhesenlmiicycaaalmllaasx...\SPPRRRPOOO\\l\SSAauaEmmLoppDllxEee\oDBCB\co\0t0h3G31re17o70nv04a4iAANFCCDGGESAACCSS0F3T1MH604 MLLTeaaotsbshttocdmmo;oodddaiitfiieedd:: Thu Nar 16 09:53108 2004 P:\Data\LCMSMS6\Masslyrnc\Fluorochemicals.PRO\MethDB\CotGrove Thu Mar 18 09:51=08 2004 NPDES 031604 Job Code: PPrriinntteedd:: PFreid Mvaarr 1199 1122::2244::0088 22000084 NsTaoamtmess= 0317042608 031704A-608 Text= ivM:ootCch6asnAeoctlidaWraPseFHhaA Methanol Wash o00u3311770044A7-660088 Sm Sm (Mn, (Mn, 2x5) 2x3) " |,100! . 85011811.688088 oo 1188--MMaarr--22000044 1100::4499::1188 MRM MRM of of 55LLCCCCh/h/aMaMnnS3nSn1/e/elM3Mlss5SS2EE#S6S#-69-6 313 > 269 \/ Areal 11..1199ee44| A~a | ho rsmero rarer | 200 4% 600 2.00 4.00 6.00 a2:iCc8 oAcnicd iPFwOAeon MMeetthhaannooll WWaasshh |003311770044AA--660088 SSmm ((MMnn,, 22xx33)) 10 | * {1 lL o T oe 2.00 Tak4.0e0 r ee 6.00 33: :Cc4a Ssuullffoonnaattee oPFrBaSs 800 1000 MN Tim|a Time 8.00 10.00 99.004 aeis}asrr wi}ee_ pr"hres|| 8.00 1188--MMaarr--22000044 w 10:49e :18 LLCC//MMSS//MMSS #~ MMRRMMooff 55 CChhaannnneellss EESS-- | CCanancceell23xx| 2.26e5 Area 10.00 ,, ,- TTiimmee | I[MMeetthhaannooll WWaasshh 003311770044AA--660088 SSmm ((MMnn,, 22xx33)) |[[lo R2R RI ONAN ar tora 0I16k \208230 { 0.16 11.1186 11 80232 305 AN 8.62 PONS 6.84 7.98. 1188--MMaarr--22000044 T10o:t4e9:18 LLCC//MMSS//MMSS #6t MMRRMM ooff 55 CChhaannnneellss EESS-- I .... 1U.lZ. 41 11.64 299 > 99 1.05e3 200 E 4% E600 2.00 4.00 6.00 800 -- 1050 8.00 10.00 Time EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00229911 SW_MNo1S39442 3M MN01539442 I | QgBuuaeInnttiiLftyyIsSuEasmgpltee RneEappoorrtteostromn, we.pater03/47/04, Amalpetik nie rage 36 Page 16 | arSSSLaaatismmumgtppdllyoRmeeoNdoLLi.iif=ssrittL:e=Id9:58,PPFrr=i\\SeeDDMtatMateArNa\\o\LL.L1OC=9CWH0MBB3S1NU1M1SS7:SeE036W40\aA:Ma,g3ags2selsyiyE2m0yxa0enta4.x\D\PaFiitlvueuoo:orr0roo3occ/chh1hee7enm/mii0icc4ce,alalsls.Asn.PaPRlRRyOOGs\\tNSS:aREKmaA.ppDRllSieesD\ShBCBa\o\0tI3GS1ET7oO0vN4eAANPCCDOGESAACC6S3FS1M604 een ssattios Method: Last modified= Hamas Se operon Sion P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Thu Mar 18 09:51:08 2004 NPDES 031604 Job Code: ! PPrriinntteedd=: FPrrii MMaarr 1199 1122::2244::0088 22000044 oe Name= 031704A-608 Text= : C6 Sulfonate PFHS MMeetthhaannooll W Waasshh |astroin608 sm in, 2) 031704A-608 Sm (Mn, 2x3) h1( om0.20 Woe | 147178 2.41 Io1 ol 3%2.00 5: co outtonace bros 5: C8 Sulfonate PFOS da TN0RoW%Lo;Ef10hs ee0l85s.| 580 amsos_szneTY 4.22 5.01 5.69 6.71 7.52 1188--MMaarr--22000044 J10s:4d9o:1d8 LLCC//MMSS/IMMSS #6 ~ MRM of 5 Channels ES- ~1~ 10.54 399 > 80 orn, NW, ~ 10 08/~ 11 04 1 13e3 8.58 ~--/ \ 1 '~' ' WA A 9.77>,../ kJ vv\_ ~'~ ~ \ ":a oooo 4.00 6.00 we i e Tos e Tie 8.00 10.00 Time MMeetthhaannooll WWaasshh ' cot70AA608 Sm 250) 031704A-608 Sm (Mn, 2x3) i a | 014,068 100-~.!4 0i.68 ree o/oI vx..--~.~ (50243 2.I|~|8 _ _ wo g42370 .4..6~3 1188--MMaarr--22000044 1100::4499:1:11 8 Lcmsms I, LClMS/MS #6 MRMof 5 Gram5. MRM of 5 Channels ES- a BBO we i)A 17 AAC~A\ 6.63 ~ .23 Can, 10.00 499 > 99 11;~1611 79 872 sm [missles] V | ~5.-59o . / ~7,~06..7'~60..8 "b~ O 38 ir a5 a5 r Tos Tin | 0I .... , .... , .... ~ .... ,, 2.00 4.00 ,, ,, 6.00 , .... ~ .... ~ .... , .... Time 8.00 10.00 Savion Reseach, 3058 Reseuzeh Drive, State College, FA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 CHOENNFNIEDPEINNTCIAOLUN- TSYUBDJIESCTTRTICOTACPOURROTT.ECNTG.IV2E7-O0R1D1E0R.8E8N6T2ERED IN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00229922 su_wmoresosss 3M MN01539443 | | QSQuueaEnnttiiEfsyy ESSaammppEllee RReeeepp.oorrttconr70an, met.pate:03/17/04, Amatyaeix. isha PPaaggee 1177 | aGSLSSaaaatcnsmmuttppdhllymmeoeooNddoLLii.iizfss:iittL::eeIdd9=:58B,PPFirr=\\di\SDDDeaaMwtattaataarrNa\\o\uL.3L1O:99COU0MM3S3EiS13MiE71:S\03364M00\iAa:1Mn,s33ag2s2ssLsyl12E20my0xy00ctni84.x\\D\TFaFihtluueuoo:orx0roo3occ/chh1hee7emn/mii0icc4ca,aalsls.As.n.aPFPlRRRyOOOs\\\tSaN:ameKmpL.plARlaDieDBsDBChB\oa\0t03a31r17o700v44eAANFCCDGOESAACCS03FS1M604 MGTLeaaotsnhttocdmmo:oodddaiitfiieedd:: Th Mar 36 03153108 2904 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Thu Mar 18 09:51=08 2004 NPDES 031604 | eJoibnCeodse: ved ar 19 12024008 2008 Printed: Fri Mar 19 12=24=08 2004 rama: 031700A-609 | TNTeaexmxtte:== 031704A-609 3: ce reid ven I: C6 Acid PFHA [00110066002200 CCoonnttrrooll 091704A.608 Sm (Mn, 2) 031704A-609 Sm (Mn, 2x3) 110( 0+ || | _ 20 3: co ncid zron 2.00 2: C8 Acid PFOA 00110066002200 CCoonnttrrooll 00;33171074A0-64093SS.mm6((M0Mn8n,, 2:3) 2x3) 00 Tae88.6611 ne" ho --~ 5% 00 4.00 6.00 8.00 asts9.02 1515 oo 1188--MMaarr--22000044 1111::1111::00(0 LCMSIMS LCIMS/MS #6 Rof 5CM hannel E5- MRM of 5 Channels ES- 331133 >> 226699) ried \ 1.1vAelreea4al| 1000 al| 10.00 Time 1188--MMaarr--22000044 1111::1111::0000 LLCC//MMSS//MMSS ##66 MRMof 5 Chanel ES. | MRM of 5 Channels ESe300 413 > 369 ol 1.4Av1ereeaa4l CLT a em l>%oA se eee 3. ci sulfonace ore 2.00 4.00 6.00 3:C4 Sulfonate PFBS oo 5568.00 on fos10.00 "| ~\Ve Time jo - mit TT fe | * 2RoeRz am\t "38a 20 n AN VN 00110066002200 CCoonnttrrooll fCancelox ispining x3) 1| K ogiR1m 20s on 809 6 ors 1188--MMaarr--22000044 1111::1111::00 LCMSIMS LCIMS/MS #6 W2I 3V9 ANoR fSAChAM 2am5el>50 8.35 MRM of 5 Channels ES- 9.23 9.56 10.60 299 > 99 11.52 1.05e3 260 at 550 860 050 Time .... ~ .... = .... ~ .... ~ .... ~ .... ~ .... Time 6.00 8.00 10.00 Exygen Research, 3038 Research Drive, State College, FA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRR\-DD1EE0RR-2E6E3NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00229933 _Motsaoses 3M MN01539444 | TE rns Quantify Sample Report ie TPN Study No.~LI958, Set No.:031704A, Ext.Date:03/l?/04, Analyst:K.Risha Page 18 BE -- Sample List: p=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\031704A CG ACSFM Last modified: Fri Mar 19 11=30=32 2004 EE aEE Method: p~\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031604 NEL LaSt modified= Thu Mar 18 09:51:08 2004 Job Code: : PPrriinntteedd:: PFrrii MMaarr 1199 1122::2244=:0088 22000044 io Name: 031704A-609 Text= : C6 Sulfonate PFHS 0106520 Gontrl 0106020 Control cst704n500 5m in, 229) 031704A-609 Sm (Mn, 2x3) f or , ,--,,-, | C2RD amawn ,uu~ 00.1144 R0080aeTgeom nsmn To Mar2008 TTT 18-Mar-2004 11:11:00 LLCC//MMSS//MMSS #6 WCho anna 5. [ MRM of 5 Channels ES- 20% psooso 1\ a nt 9230270) d/ 11.83.399 > 80 827~ 8989531002'277 10A,~R56T10.7V7^1A 943 TONY i | 8 27 8.98 | o e er To We w a T e e | | 0" '''' r .... , .... I .... r .... , .... , .... , .... , .... , .... , .... I .... TTiimme|e 2.00 4.00 6.00 8.00 10.00 [0011: 00C6680022S00uClCofnootnnratrtooell PFOS J!Joes1704n809 5m 4. 259) 031704A-609 Sm (Mn. 2x3) || 10R0-~oie es on smseeew J 30 iw ~0~,...w ---- 2.00 4.00 5% .,..,, ,,.-,,, 6.00 1188--MMaarr--22000044 1111::1111::0000] Lomsin7s6 LC/MSlMS #6 WMC of Ge rolS5l. I MRM of 5 Channels ES- // 10.48 499 set sar tom] ("ou{W ~V 9.27 1006~"1.-,~,--/ 0"66A 1/1.44 >09091 991 IT) ,.,,,, 8.00 0, , 10.00 | Time Exygen Research, 3058 Research Drive, State College, PA 16801 GFEOANNEFRIICDOUE-NNTSYUTBDJIIESCATTRITC0TAPCROOUTRETCNTGI.V2E7OGRunOiEoR26E8N0T3ERED CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00229944 swossouss 3M MN01539445 1 | QQSuueaaanlnyttiitfNyyERsSaaemmnppll,ee RReeEppRoosrNteo. oa1r0n, mae.Daces03/17/08, Analystik.misha rage 19 Page 19 | aLSSSEaathtasmsuhntppdellynmemesoNodoLLbi.iiif=sslittLe=e.Ind9:=58,PFFPFer:Dii\SiDeRbMtaEaat\arrNao\\D.L1L1=95CC0MsE3S1SN1M1Sic7S=#036s40\MaAt:Ma,3aon2\sssylE2oUmy0xo0ntk4Oe.xD\aF\KtlueuFo:oEr0r1o3ocM/cuh1he7eEso/mt0icr\4ca,alolMsAs.cn.aaPFRhlRROyOOseNWs\StaSnsh:atoKmhi.ppDLLRlpceie\DysDGIahBo\a\mtOl0G331sse1To70v0.0\e4AAICCDOGESAACCS0F3E1M604 TMLeeatnshttoedmm:eoeddiitfiiaedd=s The War To a9ietio6 2551 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Thu Mar 18 09=51:08 2004 NPDES 031604 Job Code: } PPrriinntteedd:= FFrrii MMaarr 1199 1122:=2244=:0088 22000044 Name: 0317043610 Name= 031704A-610 1: ce nce vous } Text~ i0[:0110C06660022A00cSiSdppkkPAFAH,,A5500 nnggi/LL. l0;3o137014A7-60140 rS5mm6((1iMn0n,, 220) 2x3) [TM |" 1188--MMaarr--22000044 1111::3322:4:,455] LLCC//MMSS//MMSS ##66 sso MRMof 5 ChanSnaesl 2560. | 8.60 MRM of 5 Channels ES313 > 269 5223 Seeead 5.62e4 g22~~~ Area [ES onion .... ~ .... i .... i .... i .... ~ .... i .... i ................ 256 i a abo i050 2.00 4.00 6.00 8.00 10.00 Time 2. ca acia pron 200:1100C6680022A00cSiSdppkkPAFAO,,A5500 nngg//LL. |1 7046150m (230) i5g0or MRM of 5Gran`>nsro3oe05lae0- 031704A-610 Sm (Mn, 2x3) 9.04 ~400~ 1188--MMaarr--22000044 1111::3322::44!5 LLCC/lMMSS//MMSS #6 MRM of 5 Channels ES413 > 369 8.29e4 Area % [> 2 rrr Tene || .... , .... , .... , .... , .... , .... , .... , ............ , .... Time 200 1) soo eno how 2.00 4.00 6.00 8.00 10.00 3:C4 Sulfonate PFBS 100110066002200SSppkkAA,, 5500 nngg//LL. 03;311770044AA.-661100 5m Sm bn,(Mn, 20)2x3) l1w00~ { 206 | orem 2.00 ox8.29 281 ~ Am A , a5 o% 550 4.00 6.00 8.00 1188--MMaarr--22000044 1111::3322::44!5 LLCC//MMSS//MMSS #6 MRMof 5 ChanneEl5s- MRM of 5 Channels ES299-59 29229..00>22ee9339| reeA~a AS AN"en i 0 10.00 TTiimmee Exygen Research, 3058 Reseach Drive, State College, TA 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00229955 auotssseds 3M MN01539446 I guatiey suis neport rage 20 Quantify Sample Report |B II TR en onto, mee.pateraa/a7/04, maipston.niena Study No.=LI958, Set No.:031704A, Ext.Date:03/17/04, Analyst:K.Risha Page 20 fumple Lists Er\SuCaE aA rrFsorochemioALs SRNSRTELACINOSETOAR C6 ACEP Sample List: Eo patton Ieee pearo Last modified: | a LobisWassyaaPhuorochenicals. PRO\NetRBB\Gotzove NPDES 031604 Method: Tart meatcioa, Tut I oviet ae Bot Last modified: EP Job Code= P:\Da~a\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\031704A CG ACSFM Fri Mar 19 11:30:32 2004 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031604 Thu Mar 18 09=51=08 2004 | Pprriinntteedd:: FPrrii MMaarr 1199 1122::2244::0088 22000044 [Rp---- Name= 031704A-610 Text= 4: co suitonsce pens 4:C6 Sulfonate PFHS {ro020 SpkA. Song 10106020 Spk A, 50 ng/L sitro 10m n,2:0) 031704A-610 Sm (Mn, 2x3) |= ass fMaRwMaofr05LG0h4ean1meT1l:oso3s2#5s4e.i68} 8.85 ha p~e 1858~ 18-Mar-2004 11:32:45~ LC/MSlMS #6! MRM of 5 Channels ES-[ 399 > 80 1.10e4 . 2% prs oo e woo e ooo | 2.00 2 on sortenses orcs _ 5: C8 Sulfonate PFOS 0106020Spk A.50ngiL TT ew 0106020 Spk A, 50 nglL Iastroatno sm un, 225) Riof 5Chamel 5. 031704A-610 Sm (Mn, 2x3) oe on 550 I100~1 4.00 | %-- ee -- --3-- 6 --pr-- y --5-- 0 --55-- 0 -- ~ fr-- ) -- y 2.00 4.00 6.00 6.00 8.00 L 10.00 . Area] 9.21~ 655091 18-Mar-2004 11:32:4! LLCC//MMSS//MMSS MRM of 5 Channels ES- 499 > 99 33..8888e33 Area 8.00 10.00 Bergen Research, 3050 Research Drive, Sate College, PA 16001 E~ygen Research, 3058 Research Drive, State College, PA 16801 CHEONNNEFPIINDCOEU-NNTSTYUIBDJIAESCTLTRITCOTACPOURROTT.ECNTG.IV2E7-O0R1D1E0.R8E8N6T2ERED IN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00229966 su_woresoss 3M MN01539447 , avant sete sapere rao Quantify Sample Report + SERIE ine snes ssn Study No.:L~958, Set No.=031704A, Ext.Date:03/17/04, Analyst=K.Risha Page 21 LT SL 2 SAE RAH $5 Sample List= Last modified= etoe t iueroshenicab.roWettom ovGrove REDRS GTIS08 Method= Last modified= Lm Job Code= P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\031704A CG ACSFM Fri Mar 19 11=30=32 2004 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031604 Thu Mar 18 09=51:08 2004 Printed= Fri Mar 19 12:24=08 2004 Name= 031704A-611 1. co reid om Text= : C6 Acid PFHA [00110066002200 SSppkk BB,, 550000 nngg//LL. os70tns11sm vn 26) 031704A-611 Sm (Mn, 2x3} J;]100; %1 =88.5599 _ 1188--MMaarr--22000044 1111::5544::3312 Loma7sa LC/MS/MS # Rot Som MRM of 5 Channels ES- I ow 331133>> 226699I y= 4.42e5! | 1 HT em ae Te 2.00 or BET. 2: C8 Acid PFOA 4.00 6.00 8.00 10.00 feosran11 5m in 2) 00110066002200 SSppkk BB,, 550000 nngg//LL. ii 031704A-611 Sm (Mn, 2x3) 2o9.o0sr4 VR of Cra o3 etsa 1188--MMaarr--22000044 1111::5544::3322 LLCC//MMSS//MMSS #6 MRM of 5 Channels ES413 > 369 |= | 6.7AA0rreeea5a bL y HTT eT TR as t 0~ ' ' '~I ' ' ' ' I ' ' ~ ' I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ~ ' ; ' ' ' ' I ' ' ' ' 1 ' ' ' ' 2.00 4.00 6.00 8.00 10.00 Time Time 3: C~ Sulfonate PFBS 00110066002200 SSppkk BB,, 550000 nngg//Lh. o||fsro7m0un11 5m vn 26) 031704A-611 Sm (Mn, 2x3) 1188--MMaarr--22000044 1111::5544::32 Lomas LC/MS/MS #6 Ve or Cre 5. MRM of 5 Channels ES- on mes 8.29 299 > 99 = HL 1.87e4 reArea A Toe ew awe | 2.00 4.00 6.00 8.00 10.00 Time Scroen sesearch, 958 seseese seive, Suave Celieqe, TA T6362 Exygen Research, 3058 Research Drive, State College, PA 16801 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00229977 3M MN01539448 ' | QQSuutaaundntytiitfNyyo.rssLaa1mm5pp5ll8ee,RReeSppetoorrttNo.:031704A, Ext.Date:03/17/04, Asalystik.Risha Page 22 Page 22 Study No.=LI958, Set No.=031704A, Ext.Date:03/17/04, Analyst:K.Risha | LMLSSeaaaatssmmhttppolldmemesooddLLiiiifessilttee=:ddr:PrPFF$\1re:D\ld\aDDcMaMaaaat~rr\aa\L\L1CL195CSCMHH1S1SS1M1EI1:S\S336M00\aM1:Msa53ass32slssy2Ll2m0y0yx0m0n\44xxP\\PlFiuluouorororocochchheeennmiticccaaalllsss...PPPRRROOO\V\GMSseamEmpApLDlaEeD\DBCB\o\0t03G31r17o70v04e4AANCPCDGGESAACCSS0F3T1MH604 MoLLeaabtsshttoCdmom:dooeddriiffiieedd:= Thu Mar 18 09:51:08 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Thu Mar 18 09:51:08 2004 NPDES 031604 Job Code: | etneas Pet waz 19 12024108 2008 Printed: Fri Mar 19 12:24:08 2004 | pNaemmee~s o03o17u0n4Ae-n61s1 Text~ 24(:0:1Cc06s802sS0uuilStfpooknnaaBtt,ee5Pb0Fe0HnSsng/L 0106020 Spk B, 500 ng/L 00f331o177o0044A4-661111 Sm Sm (Mn, (Mn, 23)2x3) |a 1780.8840 _ 18-Mar-2004 11:54:32 1M8R-MMaorf-25LL0CCC0hI/4aMMn1nSSo1IIlM:Ms5SS4E:S3##-265 MRM of 5 Chann33e999l9s.>1>E6S880-004 Area 9.18e4 Area | * 250 200 600 850 10.00 TTiimmee|J 2.00 4.00 6.00 8.00 10.00 550:1:C0Co680s2uS0ullfSfoponknaaBtt,ee 5Pp0Fr0OosSnglL T6-Mar-2004hi 0106020 Spk B, 500 ng/L 0317044811 Sm (Mn, 2:3) 1M8R-MMaorf-25LL0GCC0hI/4aMMn1nSSo1I/lM:Ms5SS4E:S3-2#6 1031704A-611 Sm (Mn, 2x3) 79a.019%9 MRM of 5 Channels ES- 4938906045) 499 > 99 rea 70991 3.80e41Area | epee Time | , .... , .... ~ .... , .... , .... , .... , .... , .... ~,, ,~,,, .... Time 260 4% 850 800 1000 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR-2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00229988 IM_MNoTS3449 3M MN01539449 I quatity sump sapere J Quantify Sample Report | SEL IE ER siren, enoeveneasin/on, esipeniateta Study No.=LI958, Set No.:031704A, Ext.Date~03/l?/04, Analyst=K.Risha Page 23 A Sample List= Last modified= TE EN Method: Lest modified= wm Job Code: P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\031704A CG ACSFM Fri Mar 19 11=30:32 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031604 Thu Mar 18 09=51=08 2004 i PPrriinntteedd:: Pri MMaarr 1199 1122=:2244::0088 22000044 ~ame= 031704A-612 [a Text= A. i: C6 Acid PFHA | Hovso8nasi.osaneda.rd Tar2004 TE XC030504-1, 25 ng/L Standard ;trons smn, 2) MonetEaa, 031704A-612 Sm (Mn, 2x3) ss Te | 55822.50o955~ 18-Mar-2004 12:16:15 LLCC/lMMSS//MMSS #~ MRM of 5 Channels ES- 31333.>.222776e449] i| ~~ pos| 1'o/~_ [|I rere -re 0..I ,~,,,~q-~,,, , Hs ew ew iw J 2.00 4.00 6.00 8.00 10.00 poser EE : c8 Acid PFOA Casasodt,25 ng Sandard Mar 2004 27 XC030504-1, 25 ng/L Standard o:snosnezsm on, 239 HRo1ot3 Chas 5, 031704A-612 Sm (Mn, 2x3) Boix Headd | 9.04 7709~ 18-Mar-2004 12:16:15 LLCC//MMSS//MMSS #6 MRM of 5 Channels ES- ea 413 > 369 4.69e4 || ow | 1(i/1~ /~ { 0r. ,-7-~.. ~. , , i ,"--~.. i ,''-~' ....... , .... , EmEEr--rarrrrrrry .... , .... , .... , .... , , . . lTimi,e 22..0000 ~ 44..0000 66..0000 88..0000 1100..0000 : c4 sulfonate PFBS X(CC003300550044--11,, 2255 nngg//LL SSttaannddaarrdd concsnm 0h 22) Uot3Ct harl 5. 031704A-612 Sm (Mn, 2x3) " | +R om Ra a SRE vn era J005U0111A0 98N5ue | 100-~ lo?45 147 339077338 500528 640 |/ I8w.2y7 /~ / A 9.06 LCMSIMS 1188--MMaarr--22000044 1122::1166:1:1:5 LC/MS/MS #6 T5163 MRM of 5 Channels ES229999>>9999) 1.51e3 9 71 1080 10.85 nes aE a ewe | eo eet 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00229999 3M MN01539450 I | qSQuuaaannttiiEftyy sSTaammppEllee RseEepgEoorrNtte. oatraen, mer.pate03/17/08, analyst. isha Pnaaggee 2244 [I p SLSSaaatsmmutppdllyr meeoNdoLLi.iifss:tittL.:eId9:58B,PF.7r:\i\\SDDeoaMetacaatearNat\o\aL.L1r O:9C\0MML3SS11uM1G7S:\Gp 036W40\aA:Msa,3aas2slg ssylE2mby0x\0ntyF4.xlD\nuaFtolaesu:oo\0rc3ohF/ce1hnu7ei/mco0ie4crl,aslo.Asn.FcFaPRRlRhOOyO\Ws\eStSaa:ansKmpR.piLRlEeiecDDsDBChBa\oa\Ot0l3a31c1a7o70v0.4e4AAOCCDGaESAACCS0F3S1M604 a Het eatte: Method: Last modified= Thu Har So obiitior 3004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Thu Mar 18 09=51=08 2004 NPDES 031604 | JeoetbnsCeoadse: red war 19 3202408 2004 Printed: Fri Mar 19 12:24:08 2004 sna: o33700A-622 Name= 031704A-612 Lore Text= 4: cs sustonate prs 4:C6 Sulfonate PFHS i X[XCC003300550044--11,, 2255 nngg/lLL SSttaannddaarrdd Lo |03170458m v1n2, 230) 031704A-612 Sm (Mn, 2x3) i" MofRCraM nn9el>6ES8-0 8.84 w S~ou 906-~ 1188--MMaarr--22000044 1122::1166::11!5 LLCC//MMSS/lMMSS #6 MRM of 5 Channels ES399 > 80 5.69e3 Area 1001 e 35 PE) I) r 00 BR i000 Tn 0/"~.'-~ ,..---, . 2.00 .,, .... , .... , .... , .... , .... ~ .... ~ .... ~ .... , .... Time 4.00 6.00 8.00 10.00 5. co sulfonate pros 5: C8 Sulfonate PFOS (C030504-215, nolL Standard T6.Mar-2004 12:16:15 XC030504-1, 25 ng/L Standard i("03170S4m6(142, 223) EIS MRM of 5 hann5aS5ee55ad0- 031704A-612 Sm (Mn, 2x3) 18-Mar-2004 12:16:15 LLCC//MMSS//MMSS ##66 MRM of 5 Channels ES- 9.19 499 > 99 3.13e3 A~a % | | --e A || ol 355 in 5b ab 050 me 2.00 4.00 6.00 8.00 10.00 Time | I Sxygen Reseacch, 2058 Research Drive, State Collage, PA 16001 E~ygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00330000 aW_Notsssst 3M MN01539451 | | QqSuiuuaalnnyttWiiotfyy.1SS1aa3mmp5pll0ee,RReSeapproorrttNo.:031704A, Ext.Date:03/17/04, Amalyst:k.Risha rage 33 Study No.=LI958, Set No.:031704A, Ext.Date:03/l?/04, Analyst=K.Risha | MLSTSaaeaacsmrmhtptpollammeerooddLLiiiiffssiitt:ee:dd:= 5PFPP7rr:r\ii\\DDDaMMaataattarraa\\\LLL11CC95CHMoSS11HM11SSS=1E633\\00NM=1a3a3Ms2s3asa1l21y05sn00yx48\aFmlluo\yrocmFhexmui\cccaaaolll?sss...ruPB5RRRooOOO\\\rSMScaAamoEmpAhplDcleBeD\eDhBCBo\\t0emIG3Lr1nTos7Ov0iNe4AANPCCDGOESAACCS0F3P1M604 LMLSeaaotssnhttocdmmo=oodddaitflieedd:: Thu Nar 16 09:51:08 2008 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Thu Mar 18 09=51:08 2004 NPDES 031604 [QJrob--Co,de: Pei war 19 12024108 2008 Printed: Mar 19 12:24:08 2004 | Nmaemmee=s 0o3317700u4A--661133 Text= i[1::XC0Cco6305Ar0cc4ia-d2,PoF5He0AngiL Standard XC030504-2, 50 ng/L Standard 003311r77o0044A7-661133 Sim Sm (bn, (Mn, 233) 2x3) 1 1168--MMaarr--22L00O00I44M11S22I::M33S88::0#0262 880 MMRRMM ooff C5LCChh/aM an3nSn1/enM 3ls5eS2El65S#.0-6 a8n.o60s 3135.>r320e60a94 | | 1~i/1 8898~ 5.30e4Area CeEeep EEArr TE Tie | 01~,,, ~ .... , .... , .... , .... ~ .... , .... , .... r .... ~ .... , .... Time 200 400 500 800 1000 2.00 4.00 6.00 8.00 10.00 2: co acia pro _ SE 2:C8 Acid PFOA [xXcCo0s3o0s50044--22,, 5500 nngg//LL SSttaannddaarrdd I N 902 wLe CIM1SI3M>S369 031704A-613 Sm (Mn, 2x3) 1188--MMaarr--22000044 1122::3388::00:2 LC/MSIMS #6 9.02 MRM of 5 Channels ES413 > 369 ||| 18377 saepa, Area 200 350 2.00 4.00 [33(::XCCc04o30Ss5uu0li4f-t2oo,nnaa5tt0ee nPpgFr/BeLSsStandard XC030504-2, 50 nglL Standard 003311770044A7-661133 SSmm ((MMnn,, 233) 2x3) | 600 800 1000 TT"iimmee 6.00 8.00 10.00 882.22s99 . 278 ~ 1188--MMaarr--22L00C004M4 S11I22::M33S88::02 AMRRMM ooff 5LhCCha/MannSne2Ie0Msls9S>EE9SS#9--6) 29119.48r>04ee93a39) Area [I SSISSV NES a 100-~ 22.0000 Tab4.0'0 "eb6.0"0 S-- Tebow 8.00 10.00 J Time ESxxyyggeenn RReessesaarrcchh,, 32005586 RReesseeasrccchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166860011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00330011 SW_MNo1S39452 3M MN01539452 ) | QSQeuuaaalnnyttiiNtfeyy. SsiaaTmm3pp5lleee, RReSepeproorrttNo.:031704n, Ext.Dates03/17/04, AnalystiX.Risha Page 26 Page Study No. :L1958, Set No.:03IT04A, Ext.Date:03/17/04, Analyst:K.Risha [I LSSaeasmm?ppllmeeodLLiiifssitt:=ed: Last modified: PPPPFEr\=rLi\b\DsNMatDaatefraa\\Lt1L1C9e9CHM\ES11ML1M1S1S:CE336H00\H1:MSa33an32MsssSl2L2E00yy00n\44xWi\Faelsu\osrFlocylhmeumeic\carFllso.uEcPPcRROhOOr)\\oeSMSaaacnztmhppilleBaecnADDEGBia\\OOc0l3G3a11oaTl7vO0.s4e4A.ANECCDGOESAACCS0IA3~T1f604 MLoLeaantsshttocdomm=nooeadsiitfiieedd:= Tha Nar 16 03151108 2004 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Metb_DB\CotGrove Thu Mar 18 09=51=08 2004 NPDES 031604 Job Code= 1 ecinteas Pet ar 19 12134008 2008 Printed= Fri Mar 19 12:24=08 2004 N[ Taemxet~sp031-- 704A-- -613 Text~ 4: ce surtonate prus 4:C6 Sulfonate PFHS XXCC003300550044--22,, 5500 nngg//LL. SSttaannddaarrdd 031704513 Sm (Mn, 263) 031704A-613 Sm (Mn, 2x3) 10( 739 888.855 |{ % | 200 2.00 55: :cC8o Ssuullftoonnaattee pPFrOoSs E an E 500 E 800 4.00 6.00 8.00 _ X(CC003300550044--22,, 5500 nngg//LL SSttaannddaarrdd *00;3311770044A8-561133 5m Sm (4m, (Mn, 263) 2x3) sts || kg9.19 RE T 200 T aboI T50T0R 530 2.00 4.00 6.00 8.00 1188--MMaarr--22000044 1122::3388::0022 LLComIMsSiImMsSi#g6 MRMof 5 Channais 5- MRM of 5 Channels ES339999 >>8800 10104] 1.01e4 ee Ama | S 00 TE TTimee| 10.00 1188--MMaarr-.22000044 1122::3388::00:~ LLCC//MMSS//MMSS: #(1 MRM of 5 Channels ES. MRM of 5 Channels ES"409550) 499 > 99 peo 4.62e3 rea)|Area ..0~0 TH-i_m-HeI 10.00 ESxxyyggeenn RReesseeaarscchh,, 13005588 RReessesasrzcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PTAA 1166800011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00330022 _MNO1S30453 3M MN01539453 ' J -- Quantify Sample Report rage 37 Sample List: PY\DRA\LCHBUSE WasimPiuorochenicale FO\SanpleDR\GSLTONA CO ACER Study No.=LI958, Set No.:031704A, Ext.Date~03/17/04, Analyst=K.Risha Sample List= P:\Data\LCMSMS6\Masslynx\Pluorochemicals. PRO\SampleDB\031704A CG ACSFM Ea e sattion Mame Se mean iT I MeMLetatshhtooddm::odified= PPF:r=i\\DDaMatatara\\LL1C9CMMSS1HM1SS:E36\0\:MM3a2sasls2y0s0n4xl\Fylunorxo\chFemlicualos.r.PPoRROOc\\MMheeLtehhDDnBBi\\CCcoottaGGrrloovvsee IN~PPDDEESS 003311660044 Last modified: Thu Mar 18 09=51:08 2004 Job Code: 1 PPrriinntteedd:= FFrrii MMaarr 1199 1122::2244=:0088 22000044 Name= 031704A-614 1. cs seta pn Text= I: C6 Acid PFHA Cf|f ost701n81asm vin, 2) I [LL11995588-1177 SSppkk CC,, 225500000000 nngg/lLh,, DDFF==1I00000000 031704A-614 Sm (Mn, 23) |[= . 1188--MMaarr--22000044 1122::5599::4444 Lemans #5 LC/MS/MS #6 sso MRMof 5 Ghrerelsd5. 8.59 o721 MRM of 5 Channels ES313 > 269 55..8855ee44. poeA~a 25 dimpmrepy pprrossrr------w9_e o721j~ eTon Ti Tite Time 2: co etd pron 2.00 4.00 6.00 8.00 10.00 2: C8 Acid PFOA LL11995588--1177 SSppkk CC,, 225500000000 nngg//LL,, DDFF==1100000000 o2otr0snsa smn, 2:0) WofR5 aI rmel 5: 031704A-614 Sm (Mn, 2x3) | seoss S`ryea | Io N pr) Te a 5a ar 0 oc | 2.00 4.00 6.00 9.04 8.00 1188--MMaarr--22000044 1122::5599::44 LLCC//MMSS//MMSS #6 MRM of 5 Channels ES413 > 369 9.59e4 | Area 10.00 Time 3:C4 Sulfonate PFBS 1L9195588--1177 SSppkk CC,, 225500000000 nngg//Lh,, DDFF==1100000000 astro sta sm (in 2) MRMofSLCehamreoenlss5. 031704A-614 Sm (Mn, 2x3) | 6 30063 | 1 1188--MMaarr--22000044 1122::5599::44 LC/MS/MS #6 MRMof5 Channels ES- 882.299. 229999>> 9999 3.66e3 |IK -- Bo we r rr rr yer TTimie | | 250 io Py am oo 2.00 4.00 6.00 8.00 10.00 Sargon Research, 3038 Research Drive, State College, PA 16001 Exygen Research, 3058 Research Drive, State College, PA 16801 CHEONNNEFPIINDCOEU-NNTSTYUIBDJIAESCTLTRITCOTACPOURROTT.ECNTG.IV2E7-O0R1D1E0.R8E8N6T2ERED IN CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00330033 su_wmoresosss 3M MN01539454 1 Quantity Sample Report rage 20 Quantify Sample Report | Ie TR Ne onmnomn, awe.Date103/27/08, anaiyesik. niet Study No.:LI958, Set No.:031704A, Ext.Date:03/17/04, Analys~=K.Risha Page 28 Sample List. p.\Data\LOME\Masslyme\FiuPoRrO\oSacmhpLeaiDIc\3e1l7s0. CO ACS Sample List= P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\031704A CG ACSFM pry erga 1 MeMLetatshhtooddm:=odified= PPF:r=\i\DDaMatatara\\LL1C9CUMSS1MM1SS=6360\\M=Ma3as2sssl2ly00ny4x\nFlxuo\roFchlemuicoalrs..oPPRRcOO\\hMMeeetthhnODBBi\\CCcoottaGGrrloovvsee NNPPDDEESS 003311660044 Eastmattied: Tha Har 1b 03 otis 1501 Last modified= Thu Mar 18 09=51=08 2004 Ey Job Code= 1 PPrriinntteedd:= PFrrii MMaarr 1199 1122:=2244=:0088 22000044 [ToR m O Name= 031704A-614 T4:extc=e suasonase pens 4:C6 Sulfonate PFHS [L11098588-1177 SSppkk CC,, 225500000000 nngg//LL,, DDFF==1100000000 TMJi|0o3a1r770044Aa.-661144 sm Sm vin, (Mn, 210) 2x3) [a0e0]i % a80u.0840 0 _ 1188--MMaarr--22000044 1122::5599::4444~ Lams#6 LCIMS/MS #6 MRM of 5 Channole 5- MRM of 5 Channels ESrie) 399 > 80 50163 6.01e~ eaArea 25 xs a0 abo i050 0"J-~'-' , ' ,,, .... , .... t .... ~ .... , .... , .... , ............ , .... Time 2.00 4.00 6.00 8.00 10.00 5. cs sultonase pros {5L1:19C955888--S11u77lfSSoppnkkatCCe,, 22P55FO00S000000 nngg//Lh,, DDFF==1100000000 1188--MMaarr--22000044 1122::5599:2:44 0033311770044A2-661144 Sm Sm (Mn, (Mn, 23)2x3) 1'1 || % = ree Ol .... , .... , .... , .... ,,, 200 a 2.00 4.00 a1 MofR 5GhaM nn1ol5s5555-9 9,19 & eeda 521~ LLCC//MMSS//MMSS #6 MRM of 5 Channels ES499 > 90 8.38e3 Area rT ~ Timo| , .... , .... i .... , .... , .... Time 1m a0 oo ] 6.00 8.00 10.00 Exygun Ressacch, 3038 Resoasch Drive, State Collage. Th 14801 Exygen Research, 3058 Research Drive, State College, PA 16801 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00330044 aunotsasess 3M MN01539455 ' | QQBuuaaynntteiit.yy sST aammpplleeT RReeppoorrNtte. 10nm704n, met.Date:a/17/04, Amsdystix. isha age 20 Page 29 Study No.:LI958, Set No.:031704A, Ext.Date:03/l?/04, Analyst:K.R~sha | MLSLSeaaaatssmmhttppollammeerooddLLiiiiffsstiit:e:edd=: pP PFrr=Pii\DiWM\ aaa\trraD\D 1L1a99CtMS11aa 1M11:S\336L00\M1=t MCa33a3s2sHss1Sa l22y00yMn00nx44xO\\ \FSFll\uucL oMrroaoccshC hesenmiliccH cyaaallmlsss..cS .PPP\RRROPOO\H \NlSSSAauEmmHopS pDLlNree\DDoCE BBoc\At0IhG31r\ 1e7o70nv04e4iAAKECCDGOESAACCS0SF3F~1604 oMLLeaabtsahttocdomm=cooadd:iiftiioedd:: Thu Mar 16 03153108 2004 P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethD~\CotGrove Thu Mar 18 09=51=08 2004 NPDES 031604 Job Code= PPrriinntteedd:= Prt vas 19 12124100 2008 Fri Mar 19 12=24:08 2004 uNpasrmeeer= 0317048615 031704A-615 Text= LI1::19Cc56s8-An1ci7iadSpPokFrHCmA, 250000 ng/L, DF=1000 L1958-17 Spk C, 250000 ng/L, DF=1000 00:3311770044AA-661155 Sm Sm (Mn, (Mn, 263) 2x3) | | 1 v | * 200 a0 650 2.00 4.00 6.00 22L::19c8Ca858-As1ce7itdaSpPpkFroOCnA, 250000 ng/L, DF=1000 [1B0317044651m5 (n, 29) |!L1958-17 Spk C, 250000 031704A-615 Sm (Mn, 2x3) ng/h, DF=1000 {| J 1T8o-Mararz-2oL00o0s4m11s33m:72S11:2288 aso HR MRM LC/MS/MS #6 fs Cr3 om 2650 of 5 Channels ES- su8a.5s9 "apzoess 313 > 269 4.42e5 Area | . ime | 00 50 8.00 10.00 Time 1188--MMaarr-.22L000O044M1BS3Ma:2S1r:2z8 90s MMRRMMooff 55LCCChh/aMannHnSnee/laMlssSEE3SS#6-6-9 1398.10845 41377.>.4`4030e6e6a559l) Area |L200 400 0/q ' ' '~"T" ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' 2.00 4.00 3: cs suitonate seas 3: C~ Sulfonate PFBS [L1858-17 Spk C, 250000 ngiL, DF=1000 L1958-17 Spk C, 250000 ng/L, DF=I000 |! 0:317044615 5m (Mn, 29) 031704A-615 Sm (Mn, 2x3) [I ' 600 ' ' I ' ' 6.00 ' - ' I ' ' ' ' ] .... I ' ' ' ' I .... ~ .... 800 t00 | 8.00 10.00 Time = ie 1168--MMaarr--22L00e0044ms113i3::M2211s::22181 820 MRMof MRM of 55LCCChh/aMannnSn2e/el6Mlss9S>EES#5S-691/| 8.29 299 > 99 `ra, ! { th20e 0 ea0 2.00 4.00 500 . 00 rr 1-- 000 --. TIJ12, e41 6.00 8.00 10.00 ESxxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCo~lllleeggee,, PPAA 1166880013 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- TSSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV27EE-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00330055 _MNO1S39455 3M MN01539456 QQSuutaaunndttyiiffNyoy.1SSLaa1mm3pp5ll8ee, RReeSppeootrrttNo.1031704A, Ext.Date:03/17/04, Analyst:k.Risha Study No.=LI958, Set No.=031704A, Ext.Date=03/17/04, Analyst:K.Risha PPaaggee 3300 LSSaaasmmtppllmeeodLLiiifssitt:=ed: PPrP=ii\\DMDaaatrtaa\\L1L9CCMHS1SM1M1SS36G0\\1MM3aa3ssssl2l0yy0nm4xe\\FFlluuoorroocchheemniiccaallss..PPRROO\\SSaammpplleaDDBB\\003311770044AA CCGO AACCSFTM MeMLLeatatsshhttooddmm:=ooddiiffiieedd:= TPPFr=ihi\\DDMMaaeattrara\\UL11C09CHMSS01HM91SS:=53610\\:=M03Ma82sasl22sy0000ns84x\lFylunorxoc\heFmlicualos..rPPRoROOc\\MNhettehhDDnBB\\iCCcoottaGrrloovvsee NNPPDDEESS 003311660044 3JL5oab5stCCmooddoeed=rified= Thu Mar 18 09=51=08 2004 PPrriinntteedd:= FPrei MMaarx 1199 1122=22441=0088 22000044 NNaammee=: 003311770044AA--661155 Text= 4[: L: 1C9C6658-sS1uu7llffSoopnnkaattCee, p2PF5rH0sS000 ngiL, DF=1000 ! L1958-17 Spk C, 250000 nglL, DF=1000 |0o13s1r77004eAa-s61155 Sm Sm (un, (Mn, 223) 2x3) % 1188--MMaarr--22L00C00/44M11S33/::2M211S::228 sas MMRRMMooff 5LCCChh/aMannnSn3eeI9lMl9ssS>EESS#8-0-6) 748.84 39449.88A>0r0e0e8a440) Area i 22.0000 440.000. [55:L:18cC5o88-sS1uu7llffSoopnnkaattCee, 2PPF5rOo0sS000 ng/L, DF=1000 L1958-17 Spk C, 250000 ng/t, DF=1000 0317044615 Sm (Mn, 263) pl031704A-615 Sm (Mn, 2x3) | 66.0000 _ 88.0000 n -- a99.11389 1100.0000 rem Time 18-RMaPr-2004 13:21:28 1M8R-MMaorf-25LL0CCC0h/I4aMMn1nSSe3/IlM:M2sSS1E:S#2-68 MRM of 5 Chann44e992l99s2>>E6S0999-49) ee 2.28e4 Area r---------------- Ta , .... , .... , .... ~ .... , .... , .... , .... , .... , .... , .... , .... -Time 200 200 500 800 1000 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00330066 IM_MNO1539457 3M MN01539457 QQSuutaaunndttyiiffNyoy.1sSLaa1mm9pp5ll8ee, RReeSppeootrrtNto.:031706, Ext.Date:03/17/04, AnalystiK.Risha Page 31 Page 31 Study No.:LI958, Set No.:031704A, Ext.Date=03/17/04, Analyst:K.Risha HoLSLSaaatasmsmhtptpollmdmeeo:oddLLiiiifssfittie:=edd:: FPPPrr1=Pid\\iDD\NMaaDaattararat\\aLL11\C99CLHMCSS11HHM11SE=1SHE336S00\\E:1MN\33aaM23ssassslL22s00yyl00nny44xxm\\xFF\lliuuuoorororoccohhceehnmeiimcciaacllassl.sPP.RRPOOR\\OSN\aGSmCapLplDLeBaD\DBCB\o\0tO3G31r17oT0vO4eANNCPCDOGESAACCSS0TF3H1M604 aMLLeaabtsshttocdomm=dooedd:iiffiieedd:= Thu Her 16 09:51:08 2004 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Thu Mar 18 09=51:08 2004 NPDES 031604 Job Code: Printed: Printed: eFrdi MMaarx 1195 1122:=2244::0088 22000048 Name= 031704A-616 Text= [1:1: 1CC96s58AA5cciiSddpkpPeFDHm,AA0000 ngiL, DF=100 L1958-5 Spk D, 10000 rig/L, DF=100 p|0o3o17a041A-67160sS4mm1v(Mn6n,, 223) 2x3) | 1188--MMaarr--22L00C00I44M11S33I::M44S33::1#1454 850 MMRRMMooff 55LCCChh/aMann3nSn1ee/3lMl>ssS25#6.06 088.5590 31311>.77r525e06ea595 Area tleBe Ting 200 400 600 2.00 4.00 6.00 22L::19CC58o8-AR5ceitSdapkpPrFDOo,An10000 ngiL, DF=100 L1958-5 Spk D, 10000 ng/L, DF=100 00133010170740A4-64166S1Smm6 (Mn, (Mn, 23) 2x3) |* 800 8.00 0992.0047 10.00 10.00 Time 1188--MMaarr--22L00C00I44M11S33I::4M43S3:1:.14 M MRMoofR f55LCCGhhlaM Mann1nSno3/elMl>ssSEE3SS#6--96 4131.>7r32e66a59] 1.72e5Area ~ rr e T20r 04 6r 00 80 .... ~ .... , .... , ~-',,,, .... ,,,, ",, .... ,,30,-2~4-7,,~, 2.00 4.00 6.00 8.00 33[:L:1C9C4358-Ss5uullSffpooknnaaDtt,ee10FPF0aB0sS0 ngiL, DF=100 1L1958-5 Spk D, 10000 ng/h, DF=100 p10o3013710740A4-6A1.66SS1mm6 (Mn, (Mn, 2:3) 2x3) 829 | 1' ' 178.8289 * tn Time ,~-~,, ;,,,, .... ~Time 1000 10.00 1168--MMaarr--22L00C00I44M11S33I::M44S33::14 MMRRMMooff 5LCCChh/aMannnSn2eIe9lMl9ss>SEESS#9-6-| 29999..1A1>r99ee96a393l Area ; | ohm ee ime | 0.--~-:.~~ .,, ,,~, ,, , .... , .... , .... ~ .... , .... , .... , | 200 400 600 800 1000 J 2.00 4.00 6.00 8.00 10.00 ~-Time EExxyyggoenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHGEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00330077 IM_MNO1S39458 3M MN01539458 GSQuueaasnrttiiTfthyy.ESsaamcpp5liee e0ReppoosrNtto. aa704n, Ext.Date:03/21/08, AmalyatiR.Risha sage 52 Page 32 SpoLSSaaatrsmmutppdallymeeoNdoLLi.iifs:sittLe::Id9:585,FP:r:\i\SpDDeaaMtatcatEraNa\o\\L.L1r L:9CO0MHE3SIN1M1S7:Se E03640\WWA=Ma,a3as2ssssblyE2yy0xm0ntte4x.\D\FFaFhtlLueuo:or0ruo3oc/coh1h7ee/szm0ii4cco,aallssAsn.BFahPRRlROOyO\e\s\SHtSasa:amKKmpI.pi1DRlaBieDc\sDRChB\aoa\Is0SG3l1r17o70ev04e4AASUCCDGOESAACCS03FS1M604 MLCSeaatsrahttotdmm:oaedaiifciieadd: Thu ker 10 03es1i0 000 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Co~Grove Thu Mar 18 09:51:08 2004 IqPDES 031604 JboribntCeoddie: ved ar 19 12034100 2008 Printed: Fri Mar 19 12:24:08 2004 Nsmaummtes= o3704n-628 031704A-616 4T41:e:9xC5tc6=o6.sS5uutlStfpooknnaa,ctee10PseF0iH0sS0 ngiL, DF=100 . 78-Mar-2004 13:43: cat70iA816 Sm vn 20) L1958-5 Spk D, 10000 ng/h, DF=100 031704A-616 Sm (Mn, 2x3) on 18-Mar-2004 13:43:14 Less LCIMSlMS #6 MRM of 5 Cramn2e5l8555-0 MRMof5 Channels ES- " 85 8.84 a 20204 399 > 80 2.02e4 Area | .tl po) r ko e oh ho Be 0 te 0-~ ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' ] ' ' ' Time 2.00 4.00 6.00 5. co sultomste pros 5:C8 Sulfonate PFOS 1956.5 Spk , 10000 ng, DF=100 L1958-5 Spk D, 10000 ng/L, DF=100 1n7s1 0885.m on, 2) 031704A-616 Sm (Mn, 23) 8.00 m9.Ma1s9 18-Mar-2004 13:43:14 18-Mar-2004 13:43:14 LCMSIS #6 LC/MS/MS #6 MRM 0 5 Cramol 5- MRM of 5 Channels ESre 499 > 99 Toren 7.62e3 eaAma L| o 200 a0 I emo 800 e 1000e TTiimmee|| 2.00 4.00 6.00 8.00 10.00 Sygen Ressazch, 2058 Raseazch Drive, State College, TA 6001 Exygen Research, 3058 Research Drive, State College, PA 16801 CCHEOONNNNFEIDFPEIINNTDCIAOELU-NN- TSSTUYUIBBDJJIAEESCCTLTTRTITCOOT AAGPOPURRROOTT.TEECNCTOTIIVV2EE7 -OO0RR1-DD1EE0RR.0E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00330088 Sw umotsssdso 3M MN01539459 PR ------ J Quantify Sample Report Study No.=LI958, Set No.=031704A, Ext.Date:03/17/04, Analyst:K.Risha Page 33 Spiess oneEssros chas laa 7RO mp r BITOR 3 ACO Sample List= Li, heen Last modified= Eo E 2sseseL chmicnt.roaston\carve 36 3360 Method= FES he or Last modified= en Job Code= P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\031704A CG ACSFM Frl Mar 19 11=30=32 2004 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove NPDES 031604 Thu Mar 18 09=51=08 2004 Printed= Fri Mar 19 12=24=08 2004 Name= 031704A-617 Text= np : C6 Acid PFHA Lioss SpE. 25000 ml, F< L1958-9 Spk E, 25000 ng/L, DF=100 icarasnet?smn 0) 031704A-617 Sm (Mn, 2x3) 1100~| % mm 2.00 2 25 rte zon - 2: C8 Acid PFOA 4.00 se TWeeCarrBoURArT0e5E0a.2 8.58 er sr 18-Mar-2004 14:05:0~ LLCC//MMSS/IMMSS ##~6 MRM of 5 Channels ES- / 31344..>55424e6e955! Area ae awe | ....6.00'.... ' ....88.3002'.1.7.~. ' ....10.00'~'.., .... TTimmee | 1LL11995588--99 SSppkk EE,, 2255000000 nngg/lLL,, DDFF==110000 lstrosnatr smn 229) uaa scram Ea. | to031704A-617 Sm (Mn, 2x3) aris ses] | 1188--MMaarr--22000044 1144::0055::00:2 LLCC/lMMSS//MMSS #~ 902 413> 369 9.02 MRM of 5 Channels ES413 > 369 4.13e5 ArAe~aal | : Tne | 0-.-~, , , ,~ .... .... , .... , .... , .... , .... , .... , .... , .... , .... , .... maw ew aw hw 2.00 4.00 6.00 8.00 10.00 | T me j 3:C4 Sulfonate PFBS losrounstr mn 21 LL11995588--99 SSppkk EE,, 2255000000 nngg/lLL,, DDFF==110000 031704A-617 Sm (Mn, 2x3) l11000 882.299 8992217-~ 1188--MMaarr--22000044 1144::0055::00:2 LLCC//MMSS/lMMSS #6 Ura Cras 5. MRM of 5 Channels ES229999 >> 9999| 44..6677e644 elArea | am eh ane Time J 0" 2.00 4.00 6.00 8.00 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00330099 3M MN01539460 | | SQQtuuuaadnnyttiiNffgyy.iSSLaaImmoppsllsee, RReSepepotorrttNo.:031706A, Ext.Date:03/17/04, Analyst:K.Risha PPaaggee 3344 Study No.=LI958, Set No.=031704A, Ext.Date=03/17/04, Analyst=K.Risha LSSaaasmmtppllmeeodLLiiifssitt:=ed: FPeP=di\D\MaDataart\aL\1C9LMCSM1MS1SN163S\0\M1Ma3a3ssssll2y0yn0nx4x\\FPlluuoorroocchheemaiiccaallss..PPRROO\\SSaammpplleeDDBB\\003311770044AA CCOG AACCSSFPM | MMLLeeaettsshhttooddmm:=ooddiiffiieedd=: PTPF1r=h\i\DDaMMataatarra\\LL1109CMCS01M91S:S=53610\\::MM03aa82sssslI22y0y00n0n84xx\\FFluloruocohemricoalcs..PhPRROOe\\MNneetthhiDDBBc\\CCooattdGlrroosvvee ~NTPPDDEESS 003311660044 LJJoeabsbtCComoddoeed::ified= Thu Mar 18 09=51~08 2004 | Pprriinntteedd=: FPerti MMaaxr 1199 1122=22441:0088 22000044 NNaammea=: 003311770044A--661177 Text= 44: :CC66 sSuullffoonnaattee PpFrHsS [LL11995588--99 SSppkk EE,, 2255000000 nngg//Lh,, DDFF==110000 00o331o71047A-06147S4Smm6(1(MMn7n,, 22xx33)) 00 * 1188--MMaarr--22L00C00/44M11S44I::0M05S5::00:2 so8at.86s51 M MRMoofR f 55LCCChhaIMM annnSne33Iel9M5ls9s90>S0E>E80S9S#84-0-60, 9161 5.0AAr6reeeaa4) Time 01 ' ' ' ' I ' = ' ' I ' ' ' ' ] ' ' ' ' I ' ' ' ' I ' ' ' ' 1 ' ' ' ~ I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' L 200 450 600 800 1000 2.00 4.00 6.00 8.00 10.00 Time 5: Co sulfonate pros I 5: C8 Sulfonate PFOS 1858-9 Spk E, 25000 nglL, DF=100 18-Mar-2004 14:05:0: [L1958-9 Spk E, 25000 ng/L, DF=100 | 0Pt3170446S1m7 (Mn, 2x3) 919 MRMof 5LCChIaMnnS4eIl9Ms9SE5S.9 031704A-617 Sm (Mn, 2x3) 18-Mar-2004 14:05:02 LC/MS/MS #6 9.19 MRM of 5 Channels ES499 > 99 | Ey 20A6reda]) | 3854L 2.10e4Area !lo a Time , .... , .... , .... ~ .... , .... , .... , .... , .... , .... , .... , .... -Time 200 400 6.00 800 1000 i 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACPOPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00331100 IM_MND1539461 3M MN01539461 QQSutuauandntytiiNffoyy.1sS1aa1mm3pp5ll6ee, RReeSppeootrrtNto.:031704A, E<t.Date:03/17/04, Analystik.Riska Page 35 Page 35 Study No.:LI958, Set No.:031704A, Ext.Date:03/17/04, Analyst:K.Risha SLSeaamsmptpllemeodLLiiifsstti::ed: FPrP=ii\\DNDaaatrtaa\\L1L9CCMHS1SM1MS1S63E\0\M1Ma3as2sssl2ll0yr0mn8ex\\FFlluucozroocchheemmiiccaallss..PPRROO\\SSsaEmpplleeDDEB\\G0I311170044AA CCOG AACCSFSM NMLLoeaattsshhttooadmmr=ooddiiffiieedd;: PTFPrrh=i\u\DDNaMaaLatarra\\L1L1C69CHMSS01MM91S:S=E53630\M:=Ma03as82sss1l22y00ym00nx44x\\FFiluucorroocchheenmiiccaallss.PFRROO\\MNeStEhEDDBI\\CCoottGGrroovvee bKTEPDDEESS 003311660044 Fob codar Last modified; Job Code= Thu Mar 18 09;51;08 2004 PPrriiantteedds= PFreit dMaarr 1195 1122:022441=0088 22000084 NNaammea=: 003211770040A8--651288 Text= i1:: cCs6 eActiad pPFrHA 1L9195588--1133 SSppk FF,, 2255000000 nngg//LL,, DDFF==110000 00"331177004A4-661188 Sm Sm (Mn, (Mn, 2:3) 2x3) | { | "1 1168--MMaarr--22L00C00I44M11S44I::M226S6::#5533 858 MRM MRM of of 55LCGChh/aMann3nSno3e/lM5lssS2EE6SS#0--6 s788.5085 31346>A22r6e65a9)l || 4.82e5Area ....20, 0.... , ....a0, .... , ....60, 0.... , 500 ....87, 8.9.5.~. ~ ....10,00..- .. , .... TTiimmee | 2.00 4.00 6.00 8.00 10.00 22: :CC83 AAcciidd PpFroOnA (~L11995588--1133 SSppkk FF,, 2255000000 nriggi/LL,, DDFF==110000 | 1188--MMaarr-.22L00C00I44M11S44I::M22S665:5:3 [0043311770044AA.-661188 5m Sm (Mn, (Mn, 29) 2x3) 902 RM MRM of of 55LCCChh/aMann4nSn1e/e3lMlssSEE3SS6#-9-6) 793.0225 41340>736659] | en 4.07e5 Area || % || i Timo L 22.0000 44..0000 86..0000 88.0000 1100..0000 Time 33::Cc4s sSuullffoonnaattee PpFrBaSs [LL11995586--1133 SSppkk FF,, 2255000000 nnggl/LL,, DDFF=110000 1188--MMaarr--22L00O0044MS11I44::M22S66::553 00p3311770044A4-661188 5m Sm (in, (Mn, 2)2x3) 82 MRM MRM of of 5LCCChh/aMannnSn2eIe9lMlss9S>EESS#9--6 || Te8.2s9 29449.00A>00r0ee9a449l Area 100-~ v - Time ui17 ;-; T~; TT ; ~T7 TT~ TT7 ~- T ;-~ , I .... I ' ' ' I .... I ' ' ' ' I ' ' ' ' I .... I -- .... Time 200 a0 600 800 1000 2.00 4.00 6.00 8.00 10.00 BEexyyggeenn RReessecaarzcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, 7PAA 1166880011 `CHGEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 9193309..00331111 SW_MNo1S39462 3M MN01539462 i qQSuutaaunndttyiitfHyyo.SSiaa1mm5pp5ll8ee, RReeSppeootrrtNto.:031704, Ext.Date:03/17/04, Analyst:k.Risha rPaaggee 3366 Study No.=LI958, Set No.:031704A, Ext.Date:03/17/04, Analyst:K.Risha SLSaaamsmptpllemeodLLiiifssitte:=d: FPrP=ii\\DNDaaatrtaa\\L19LCCMHS1SM1K1S3S60E\1\M3Ma7assssi20ly0yn4mxx\\Flluuoorroocchheemmiiccaallss..PPRROO\\SSaamspplleeDDBB\\0033117T0044AA CCOG AACCSSTFHM NoMLLeatatsshhttooddmm::ooddiiffiieedd:: TPPFh:r\ui\pDaMMateatarra\\LL11C6C9UMSS01HM19SS=:E635\01\M::Ma30as28sssll22yy00n00nx44x\\FFlluuoorroocchheenmticcaallss.PPRROO\\MKeS~EhhDDBB\\CCoottGGrroovvae PIqDPEDESS 003311660044 Jab codes Last modified; Job Code: Thu Mar 18 09=51:08 2004 PPrriinntteedd:: eFrti dMaarr 1199 1122:=2244::0088 22000044 uNammee:= 003311770044Ar--661288 Text= 44[: L:1CC96s58-Ss1uu3llffSoopnnkaattFee, 2pP5Fe0HnSs00 ng/L, DF=100 L1958-13 Spk F, 25000 nglL, DF=100 00;3311770044A6-61188 sm Sm (vn, (Mn, 213) 2x3) | |" T1A8M-Maarr2-2L00C04I4M14S42I:M62S6.:5533 835 MRM MRM of of 5LCCChh/aMannnSn3ee/lMlss9>SEE9S8#S0-6 887.4835 399 > 80 47r9e0a4 4.79e4 Area 20 400 600 2.00 4.00 6.00 551::9C5C868-sS1uu3llffSoopnnkaattFee, 2PF5FO0OSS00 ng/L, DF=100 L1958-13 Spk F, 25000 rig/L, DF=100 [00'n3311770044A4-661188 Sm Sm (Mn, (Mn, 23) 2x3) 11 | * | 800 8.00 59.622007 1000 Time Time 10.00 1188--MMaarr--22L00C00I44MS114I4:M:22S66:::55:3 MRMof MRM of 55LCCChhlaMannnSn4ee/lM9lss9SEE9SS#9--6 4919.8>20949] || Area 1.92e4Area , .... , .... , .... , .... , .... , .... , .... ~ ...3.46, 7.~... , .... , .... Time Le 200 4% 500 800 1000 TM 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSTUUYBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00331122 IM_MNO1539463 3M MN01539463 1 | gQSuutaaunndttyiitfNyyo.:sSiaa1mm5pp5ll8ee, RReeSppetoorrttNo.:031704A, Ext.Date:03/17/04, Analystik.Risha PPaaggee 3377 Study No.=LI958, Set No.:031704A, Ext.Date:03/17/04, Analyst:K.Risha LSSaaasmmtppllemeodLLkiiessitte::d: PPrP:i:\\DMDaaa~rcaa\\L1L5CCMH1SE1MM:SS36E0\\:MM3aa2ssssl2ly0y0nn4xx\\FPlluuoorroocchheamsiiccaallss..PPRROO\\SGasmspplleeDDBB\\003311770044AA CCGO AACCSTFHM | MLMLeeaattsshhttooddmm::ooddiiffiieedd:: PFPTir=h\iu\DDaNMataa~arra\\LL11C96CUMS0S1H3M1S:S=E53610\\=:MM30aa25ssss2ll20yy000nn44x~\\FFlluuoorroocchheenmticcaallss..PFRROO\VMNeetthhDDBB\\CCoottGGzroovvee KNFPPDDEESS 003311660044 ab Code: Last modified= Job Code= Thu Mar 18 09:51=08 2004 | ertnteas Printed: Prt Frl MMaarr 1199 11220:2344=10088 22000044 I NHraaemmeas=: 003311770044AA--661199 Text~ 2i[::L19CC5668-AA1cciiSddpPEVGEH,AA10000 ng/L, DF=100 L1958-1 Spk G, 10000 ng/L, DF=100 001331177040A4-A61:96SS1mm9 (Mn, (Mn, 233) 2x3) |* o 200 400 600 2.00 4.00 6.00 2[:L: 19CC5o88-Aa1cciiSddppPrFGoO,nA10000 ng/L, DF=100 L1958-1 Spk G, 10000 ng/L, DF=100 03170445S1m9 (Mn, 233) 031704A-619 Sm (Mn, 2x3) | * as88s.55e88r 500 8.00 7990.020262 6 1188--MMaarr--22L00C00/44M11S44/::M4488S::4#0 MRMof MRM of 5LCCChh/aMann3nSn1ee/3lMl>ssSEE2S6S#0--6) 313`4,>47r732e3e6a559 Area | 1000 Time Time 10.00 1188--MMaarr--22L00C00I44M11S44I::M44S88::4#4060 MRMof MRM of 55LCCChh/aMann4nSn1eeIl3Mlss>SEE3SS6#.9-6) 413 > 369 3.A8o6a5l 3.86e5 Area | 22.0000 44.0000 3: ca sulfonate prs [LL:1199C55488--S11ulSSfppokknaGGt,,e11P00F00B00S00 nngg//LL,, DDFF==110000 I00B3311770044AA-:61189 Sm Sm (Mn, (Mn, 23) 2x3) | | *% 600 800 h100e 0 e TTiimmee 6.00 8.00 10.00 ea 1168--MMaarr--22L00C00I44M11S44I::4M488S::41~ 827 MMRRMM ooff 55LCCChhlaMannnSn2e/el9Mlss9S>EESS5--9 ad8.o27 29493>50949 4.35e4 Area 22.0000 44.0000 660.000. 88.0000 1100.0000 Time | EExxyyggeenn RReesseeaarrcchh,, 33005588 RReessesaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166680011 `CHGEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00331133 IM_MNOTS39464 3M MN01539464 | | SGQtuuuaadnnyttiiNffoyy..SsLaaImm5pp5llsee, RReSepeptoorrttNo.:031704A, Ext.Date:03/17/04, Analyst:k.Risha PPaaggee 3388 Study No.=LI958, Set No.:031704A, Ext.Date=03/17/04, Analyst=K.Risha TSSaaasmmkppllmeeodLLiiifssitte=:d: PPrB=d:\\DDwaaattraa\\1LL9CCMHS1S1MH:SS36E0\\:MM3aa3ssssl2l0yy0nn4xx\\FFlluuoorroocchheemmiiccaallss..PPRROO\\SSaAmRpplLeeDDBB\\0O33117T0O44AA CCOG AACCSFSM | NMLLeaoatssthtteoddmm:=ooddiiffiieedd=: 7TPF:hr=\ui\DDaMNataatarra\\C1L169CHMES10N1M5::SG356\03\:=MK13a02sasl22s00y00ns44xl\Fylunorxoc\hFemlicualos.rPPoRROOc\\MNheSteHhDDnBB\\iCCocottaGGrrloovvsee NB~PPDDEESS 003311660044 on" codes Last modified= Job Code= Thu Mar 18 09=51=08 2004 | sPcriinntteead:: ed Max 19 12024108 2004 Fri Mar 19 12=24=08 2004 | mNeammees: o03a1r7o0e4aA--e6i1s9 Text= | [44L::1C9c56e8-sS1uuilStfpooknnaaGtt,ee1pP0F0rH0sS0 ngiL, DF=100 L1958-1 Spk G, 10000 ng/L, DF=100 oop 003311770044A4-661199 Sm Sm (Mn, (Mn, 23) 23) [ar i |* 10~ oo i8u.s8s5 pr 1188--MMaarr--22L00O004M4 S11I44::M44S88::4#4060 MMRRMM ooff 55LCCChhlaMannnSne9eIlM0lss5SEESS#8--60 399 > 80 `ron 4.79e4Area | oes 1 i .... , ....20, 0.... , .... 5, 0.... , ....60, 0.... ~ 8845~ ....50, 0.... , ....10,:0~0,, ,, .... TTiimmee 2.00 4.00 6.00 8.00 10.00 55[:L:1C9c85o8-sS1uullpffkoonnaaGtt,ee1pP0Fr0Oo0Ss0 ng/L, DF=100 _ 18-Mar-2004 14:}48: |0L1391587-10S4p8kSm6G(,1M1n90,002603)ng/L, DF=100 1M8R-MMoafr-2LL0CCC0hI/4MaM1SnS4I/nM:M4eSS8El:S4#s-06 10s 0; 031704A-619 Sm (Mn, 2x3) se99.22r00 MRM of 5 Channels ES- 929.>169049) 499 > 99 2.16e4 " Area |g ~ Time 0I" ' ' ' ' I .... I .... I .... I .... I .... I .... I .... I .... I .... I ' ' ~-"~' I , 200 400 600 800 1000 2.00 4.00 6.00 8.00 10.00 ' ' ' Time ' | | | EBxxyyggeenn RReesssesarrcchh,, 33005580 RReesseeaaxrcchh DDrriivvee,, OSttaattee CCoolllleeggee,, BPAA 1166880011 1 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00331144 SW_MNo1S39465 3M MN01539465 | | QQSuuiaalnantytiitfweyy. sSTaaLmmip5p8ll0ee,RReeSpperoorrttNe.1031704n, xt Dates0d/17/04, Analystix.Risha PPaaggee 3399 Study No.=LI958, Set No.=03IT04A, Ext.Date=03/17/04, Analyst:K.Risha | eLYSSaaatassmmhttppolldmeme:ooddLLiiiiffssitti:esedd:: PFi7P1r:ii\i\\DDDHMaaaaatttrraaa\\\LL11LC99CCHMSSH11HM11HS:S1SE336\00\VM:1Maa33ass23ssssLll22yyy09nm00nxx44x\\\PPFLlluuuooozrroooccchhheeeaamiiicccaaalllsss...PPFRRROOO\\\NSSSaaEmzRppDlLDea\DDCBBo\\t00a33F11o770v04e4AADCCEOGSAACCS0F3S1M604 LTMLaeoatssnhttocdmom=odoeda:itfeiseodd:= Tho Har 16 03051100 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Cot~rove Thu Mar 18 09=51=08 2004 NPDES 031604 | states Job Code= Printed= ret wax 19 12:24:08 2004 Fri Mar 19 12:24:08 2004 | aNammae:= o03311770044An--662200 Text= [1:X: C02C66305aA0cc4ii-dd3,pPFe1Hn0An0 nglL Standard XC030504-3, 100 ng/L Standard Lo.003311770044A4-662200 Sm Sm (Mn, (Mn, 255) 2x3) he!{ 1168--MMaarr--22L00O00M44 S11I55::M110S0::3#3464~ ss MRM MRM of of 55LCCChh/aMann3Snn1e/eM3lls>S2EES6#S.06~ 78.60 313 > 269 10`1ar0e5a 1.01e5i Area! EE 200 00 500 500 R 1000e Time | 2: 8 eta pron 2.00 4.00 x2:C03C805A0c4i-d3,PF1O0A0 ngiL Standard 6.00 8.00 10.00 In 16-Mar-20P 04 15:10:34 XC030504-3, 100 ng/L Standard 100030137,10740A4-862200 5m Sm (4n, (Mn, 233) 2x3) 1M8R-MMaorf-25LL0CCO0hlM4aMnS1nSIe5/lM:M1sSS0E:S3##.~66| 90 MRM of 5 Ha Channels 30ES- | 2090.0848 413 > 369 15"1h5r 1.51e5 | *1001 ~ | /l 200 Pr) 600 85026988~ 00 TTiimTMmee 3: cs suitonate 2s.0e0as 4.00 6.00 8.00 10.00 XC030504-3, 100 3: C~ Sulfonate !XC030504-3, 100 nglL PFBS ng/L SSttaannddaarrdd 116a--MMaarr--22000044 1155::1100::34 "[ 003311770044A8-62200 5m Sm (Mn(Mn, 23)2x3) 820. MMRRMM ooff 55LLCCCChhI/MaaMnnSSn2eI/eM0llMsS>SEE0S#S9-6| | &8.29 29493">0r09e39a | Area | o een ........20, 0.... , ....40, 0.... , ....50, 0.... , ....80, 0.... R , ....10,00.A ... , ...N . TTiimme|e 2.00 4.00 6.00 8.00 10.00 EExxyyggeonn RReesseeaarrcchh,, 33005580 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, P7AA 1166800013 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2E7E-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00331155 _MNO1S39465 3M MN01539466 I some es re po Quantify Sample Report ET Study No.=LI958, Set No.=031704A, Ext.Date:03/17/04, Analyst:K.Risha Page 40 rete ---------------- roc ee Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\031704A CG ACSFM I MMLeeattshhtooddm::odified: PPF+:r\i\DDaMatatara\\LL1CC9UMMSS1MH1SS:6630\\:MM3a2sasl2sy00ns4x\lFylunorxoc\heFmlicualos..rPPRoROOc\\MMhetthehDDnBB\\iCCocottaGGrrloovvsee NNPPDDEESS 003311660044 E HEE Rn Last modified: Thu Mar 18 09:51:08 2004 Job Code: I PPrriinntteedd:: FPrril MMaarr 1199 1122::2244::0088 22000044 Name= 031704A-620 Text= : C6 Sulfonate PFHS SRT XC030504-3, 100 ng/L Standard CProma meer 031704A-620 Sm (Mn, 2x3) a... 18-Mar-2004 15:10:34 i LC/MS/MS #6 =we ess5s MRM of 5 Channels ES- ClI a| MA 1(o/1 2.00 ee vn 5:C8 Sulfonate PFOS aaa Tana 4.00 6.00 8.85 399 > 80 1A.rA88e~eaa4) A 3370~ 8.00 Time 10.00 . ~ momen XXCC003300550044--33,, 110000 nngg//LL SSttaannddaarrdd 031704A-620 Sm (Mn, 2x3) wr 1188--MMaarr--22000044 1155::1100::34 LLCC/lMMSS//MMSS #6 MRM of 5 Channels ES- 9.19 1421 [ 7| re ee Te Te hg eg 2.00 4.00 6.00 8.00 -- 10.00 499 > 99 88..0088e33 Area Time ov eee, 3458 seer eve Ste tin 8 6 Exygen Research, 3058 Research Drive, State College, PA 16801 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00331166 3M MN01539467 1 Qquuaannttiiffyy SSaammppllee RReeppoorrtt PPaaggee 4411 | SSttuuddyy WNoo..::LLI1955588,, SSeett NNoo..::003311770044AA,, EExxtt..DDaattee::0033//1177//0044,, AAnnaallyysstt=:KX..RRiisshhaa SLSaaamsmptpllemeodLLiiifssitte::d: P7r:Pi\:\DNDaaatrtaa\\L1L9CCMH1SS1MH:SS36S0\\:MM3aa7ssssl2ly0y0nm4xx\\FPlluuoorroocchheemmiiccaallss..PPRROO\\SSaAmmpplleeDDBB\\0O3I1L7T0ON4MA CCGG AACCSSFFM | NMLLaeaittsnhhttoomdamo:roddiiftiieedd:: 7TPF3hr:\ai\DDaMNataatarra\\LL11C9C6HMIS01KM31S1S:S56330\H:1Ma30as28sssl2l2y00y0n0n44xx\\FFlluuoorroocchheenmiiccaallss..PPRROO\\MNeEtAhDDBB\\CCoottGGrroovvee NNPPDDEESS 003311660044 Gab coder Last modified: Job Code: Thu Mar 18 0%:51=08 2004 I Pprriinntteeda:: PFrrii MMaarx 1199 1122:=2244::0088 22000044 | NTaammtees: o0331177004nA--e62211 Text: | i[1::XC0Cc6o305Ar0cc4ii-ad4,PpF2rH5aA0ngiLStandard XC030504-4, 250 ng/L Standard i 00|3311770044AA.-662211 Sm Sm (Mn, (Mn, 223) 2x3) po as88s.55s097 1188--MMaarr--22L00O0044M11S55M::33S22::117 MRM MRM of of 55LCCChh/aMann3nSnee/lMl1>ssS2EE36SS#-9-6 3132>2r12e66a59 2.21e5Area 111/1 38557~ 200 400 600 500 ..................... i-~ 1000 ......... Time 2.00 4.00 6.00 8.00 10.00 (22:X:CC0c83o05aA0cc4ti-da4,PprF2oO5nA0 ngL Standard 18-Mar-2004 15:32:1 XC030504-4, 250 nglh Standard 00o3311y7700447A.-662211 Sm Sm (Mn, (Mn, 263) 2x3) 1M8R-MMaorf-25LL0CCO0h/4MaMnS1nSeI5/lM:Ms3SS2E:S1#-76 904 MRM of 5 413 Channels 3E6S0- e97.0240 41333>3.3r333e0e6a559l, |= | Area ~ | o0 ~,, ,~-, 200 .... , .... , 450 .... ~ .... ~ 650 .... ~ .... , 800 .... ~ .... ~ 1000 .... , .... ~ .... Time Tim~ 2.00 4.00 6.00 8.00 10.00 3: ct sultanate prs 3[;XC(023405S0u4l-fo4,na2t5e0 PnFgB/SL Standard 18-Mar-2004 15:32:47 XC030504-4, 250 nglL Standard 031704A.621 Sm (Mn, 223) 1M8R-MMoafr-25LL0CCC0h//4aMMn1nSSe5//lM:M3sSS2E:S1##.676I |i 031704A-621 Sm (Mn, 2x3) 8288.28 5011501-~ MRM of 5 Channels ES- / 2%9>99 299 > 99 93L5e03y 9.33e3 |% Area ES a 200 400 500 EE500 i 1000 in i, 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReessseaaxrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEEASCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00331177 SW_MNO1839468 3M MN01539468 | | QSQuutaaunndttyiiffNyyo.iSSLaa1mm3pp5ll8ee, RReeSppeootrrttNo.:031704A, Ext.Date:03/17/04, Analystik.Risha aPaggee 4422 Study No. :L1958, Set No. :031704A, Ext.Date:03/17/04, Analyst:K.Risha LSSaaasmmtppllemeodLLiiiessltte=:d: PPr:Pi\iD\MaDatarat\aL1\9CLMM1SS1MH:SS36\0\M:Ma3as2sssll2y0ym0nx4x\\PFlluuoozroocchheemmiiccaallss..PPRROO\\SSAaSmPpLleeDDEBA\O0I311T70044AA CCOG AACCSFSM | MLMLeeaattsshhttooddmm::ooddiifiieedd:: TPFPhr=riu\D\NMaDaa~rraa\tL1169CaM\0S1M13L:S1C3650\H1:M13Sa02sMslS22y00600n44x\\aFlsusorloychnexmi\cPalLs.u.PFoRROzO\\oMNecStChhDDeDB\n\CCiootctdGarrolovvsee ~N-PPDDEESS 003311660044 ab coder Lest modified= Job Code: Thu Mar 18 09=51=08 2004 | rPriinntteeads= PFrrii MMaarr 1195 1122:=3244::0088 22000044 | Naammees= 0o3v1r7o0s4nA--e6n2s1 Text= 44::CC66 sSuulltfoonnaattee pPrFiHsS | [XxCC003300550044-44,, 225500 nngg/lLLSSttaannddaarrdd vo 003311770044A4-662211 SSmm ((MMnn,, 226x33)) | no * 1188--MMaarr--22L00C00I44M11S55I::M3322S::11 ? sa MMRRMM ooff 5LCCChh/aaMnnnSn3oe/lMlss0>SEESS68-0-) as8.e84 39449.77r>88e0ea844l0 Area | || 200 400 630 800 2.00 4.00 6.00 8.00 | 55[:X:CCC08o30sS5uu0ll4fo4on,naa2tt5ee0 PpnFrgOo/sSL Standard I XC030504-4, 250 ng/L Standard p{r003311770044A2-662211 Sm Sm Mn, (Mn, 223) 2x3) 921 | si9.s21s [I | . 200 400 600 800 2.00 4.00 6.00 8.00 1- 000 Tine | Time 10.00 1188--MMaarr--22L00C00/44M11S55I::3M322S::11.7 MMRRMM ooff 5LCCChh/aMannnSne9e/lMl9ssS>EESS#9--6 499 > 99 1.e90a04 1.90e4 Area | 1000 Time | Time 10.00 0 | | | | Exygen Resessch, 3056 Research Drive, State College, 7A 16801 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSTUUYBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00331188 IM_MNO1539469 3M MN01539469 | | gSQtuuuaadnnyetiiNtfoyy.:sSLaa1mm5pp5ll3ee, RneSepepotorrtNto.:031704R, Bxt.Date:03/17/04, Analysti.Risha PPaaggee 4433 Study No.:L1958, Set No.:031704A, Ext.Date:03/l?/04, Analyst=K.Risha SSSa~aammtppllemeodLLiiifssitte::d:PrFP\r:Di\aDcaaatr\aL\C1LH9CSMHS1SM1E1S\36M0\a1Ms3as3slsyl2n0yx0n\4xF\iFulouroorcohcehneimciaclasl.s.PFRROO\NSGaRmEpplLeeDDBB\\0O331T?0044AA CCOG AACCSSFFM I 0eLMLLbeaaatt"sssnhtttoocadommms=doooedddriiiffeiiieeeddd==: Thu var 16 09:53:00 2004 PPF:r=\i\DDaMatatara\\LL1C9CUMSS1NM1SS:S63\0\M:Ma3as2sssll2y0yn0nx4x\\FFlluuoorroocchheexmilccaallss..PPRROO\\MMOeLtEhDDEB\\CCoottGGrroovvee Thu Mar 18 09=51=08 2004 hN-PPDDEESS 003311660044 | sJeoibntCeoadse= Pri Mar 19 22:20108 2004 Printed= Fri Mar 19 12:24=08 2004 | eNammeer= o03s1u7o0a4nA--e6z2z2 | 1I[::18cCe658AA3cciiDadF=PpF1eH0nA00 L1958-3, DF=1000 1 10[033011707h0044AA.-662222 5m Sm (Mn, (Mn, 2)2x3) 1001 388850.6070 3807-~ 18-Mar-2008 15:54: 1M8R-MMoafr-25LL0CCC0h/M4aMnS1nS/a5/iM:M5sSS4E:S0#.46 MRM of 5 313i5a26d0 Channels ES313 > 269 rea) 2.43e4 Area ro ~ 1 Say~ ~,~~ N e e e "qm , , , ~ .... ~ .... ~ .... ~ .... ~ .... i , 1 ew 30 500 80 1000 2.00 4.00 6.00 , , ~ .... ~ .... ~ .... r .... lime 8.00 10.00 2: co ncia pron ~ | [2LL:1199C55888--A33c,,iDDdFF=P=F11O00A0000 1188--MMaarr--22L00C00I44M11S55:I:5M54S4::0#0464 LC/MSIMS #6 317048.022 Sm in, 269) MRMor 5 Chemels 5- | 031704A-622 Sm (Mn, 2x3) 1|0% i7100~ c2ose 13o>sAe3r6de9]a 9.04 MRM of 5 Channels ES413 > 369 3.65e4 Area FYN 0 r re Time . 22.0000 44.0000 66.3000 88.0000 33L:1:9Cc54o8-3sS,uullDffFoo=nnaa1tt0ee00ePFrBeSs ` L1958-3, DF=1000 0033e1177y0044A4-662222 Sm Sm (Mn, (Mn, 2)2x3) 828 ' 1, :i 028.29 ' || % NN | Te2.00m aw4.00 e6.d0d0 eo 8.00 foc 10.00 Time 188--MMaarr2-2L000C044M11S55M::55S44::004 MRM MRM of of 55LCCChh/aMannnSn2e/elM6lss9SEE0SS#9--6 299 > 99 55r00a3 5.50e3 Area tie t10o.00oo el Time I Rxygen Research, 3058 Research Drive, State College, BA 16901 Exygen Research, 3058 Research Drive, State College, PA 16801 | `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00331199 SW_MNO1839470 3M MN01539470 I EE as po Quantify sample Report | BL SE Te cntrans, on Deserov27/00, nmsyasen Riana Study No. :L1958, Set No. :031704A, Ext.Date:03/17/04, Analyst:K.Risha Page 44 FTI LNessere ATI 50 APR Sample List= P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\031704A CG ACSFM | MsLeeattshntooddm::odified= PPF:r=i\\DDMaatatara\\LL1C9CMMSS1MM1SS=636\0\M=Ma3as2sssll2yy0n0nx4x\\FFlluuoorroocchheemmiiccaallss..PPRROO\\MMeetthhDDBB\\CCoottGGrroovvee NNPPDDEESS 003311660044 EUS on Bait Last modified= Thu Mar 18 09=51:08 2004 Be Job Code: | eter eet wae 20 sero sun Printed= Fri Mar 19 12=24=08 2004 DPName= 031704A-622 Text= 4:C6 Sulfonate PFHS CB passa i LL11995588--33,, DDFF==11000000 1 031704A-622 Sm (Mn, 2x3) i Ce or Ec we 8.87 = 539 1188--MMaarr--22000044 1155::5544:(:04 LLCCIIMMSSI/MMSS #6 MRM of 5 Channels ES399 > 80 33..3333ee33| Area i Wak ab awe | ori ~~ en "rAaNre Ti | Time 2.00 4.00 6.00 8.00 10.00 5:08: S C8 u Sulfl onaf te PPo PFOOSSnate ------ [LL11995588--33,, DDFF==1lO00000 [ A ; " Ra ro%a ryELoe=2ed 031704A-622 Sm (Mn, 23) 1188--MMaarr--22000044 1155::5544::0044 LLCC//MMSS//MMSS ##66 MRM of 5 Channels ES- 9.21 499 > 99 2.22e3 Area Time 2.00 4.00 6.00 8.00 10.00 ` I es i reel testes eaFeceed I Exygen Research, 3058 Research Drive, State College, PA 16801 CONFIDENTIAL SURMEECTTT0 ATPROETEGe E OROET R ENTERED I I CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00332200 worsen 3M MN01539471 1 QQuuaannttiiftyy Ssaammppllee RReeppoorrtt PPaaggee 45. | SSttuuddyy Noo..::LL11995588,, SSeett NNoo..::003311770044AA,, EExxtt..DDaattee.:.0033//1177//0044,, AAnnaallyysstt::KK..RRiisshhaa LSSaaasmmtppllmeeodLLiiifssitt::ed: PPrP:i:\\DDMaaattraa\\L1LC9CMMS1S1MN:SS36E0\\:MM3aa2ssssl2ly0yn0n4xx\\FFlluuoorroocchheemniiccaallss..PPRROO\\SSaammpplleeDDBB\\003311770044AA CCGG AACCSSFTMM | MLwLeeaattsshnttooadmmr:ooddiitfiieedd:: TPPFhr:+ui\\DDMMaaeattrraa\\L11L98CCMHS01SM91SS:=636501\\::MM30a28sasl22sy0000ns44x\lFylunorxoc\heFmlicualos..rPPRRoOO\c\MMhSeLtehhODmBB\\iCCcoottaGGrrloovvsee NNPPDDEESS 003311660044 oLJoahbstCC~ooddoeed:=ified: Thu Mar 18 09:51:08 2004 | Pprriinntceead:: Ferti MMaarr 1199 1122:=2244:=0088 22000044 | TdNaeemmxete=:: o033a1770004aA--662233 Text= 1i:: Cc6o nAcciida PpFeHnA | L[11995588--33, DDFF==110000 (0317044623 Sm (Mn, 263) 031704A-623 Sm (Mn, 2x3) I |1 A 1188--MMaarr--22L00C00I44M11S66I::M1155S::447 MRM of 5LCChIaMnnSe/lMsSES#-6 2880.4663004 MRM of 5 1.405) Chan33n11e33ls>>E226S69-9) "veal 2443~__ 1.40eSArea | oB hm ee I 200 ",1 I .... 2.00 I 4.00 .... I .... 4.00 I 6.00 .... I .... 6.00 I 8.00 .... I .... 8.00 I 1000 .... I .... 10.00 I'' ,-~ Time 2: co Acid pron 2: C8 Acid PFOA | [L19583, DF=100 18-Mar-200416:15:47 L1958-3, DF=100 a i 0317044623 Sm (Mn, 263) r9e04s MRM of LCChIaMn1nSe3Il2M>s.S4E35S#60-956 031704A-623 Sm (Mn, 2x3) 18-Mar-2004 16:15:47 LC/MS/MS #6 9.04 MRM of 5 Channels ES413 > 369 2.45e5 | ea | * Area . h e r200 400 60n 0 800 1000 TTiimmee 2.00 4.00 6.00 8.00 10.00 3: : CC44 Ssuullffoonnaattee pPFrBeSs o [LL11995588--33,, DDFF==110000 1188--MMaarr--22L00C00I44M11S66I::M11S55::447 | (00033101770044A4-662233 Sm Sm (Mn, (Mn, 263) 2x3) 831 MRM MRM of of 55LCCChhIaMannnSn2ee/lM0lss9SEE9SS#0--6 o83.3218 29499>76949 Area) 4.97e4 A~a Vd % - Time 0" .... ~ .... ~ .... , .... , ........ ~ .... , .... ~ .... ~ .... , \ 200 400 600 800 1000 2.00 4.00 6.00 8.00 10.00 , .... Time | EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 t `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACPOPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00332211 IM_MNO1539472 3M MN01539472 1 |S Qquuannstiitfyy sSaammppllee RReegpoorrNete commons, extmate.03/17/04, Asaiyatix.ntsna sage 46 Page 46 Up LSSSn aaatssmutppdllyr meeoNdoLLi.iifss:tittLe::Id9:58,PFFPr:.oi\S\RDeDEeMtaRataCrrNaa\o\\Lp.L1U:9CO0MCM3S1S11MS7\:S0W3640a\WA:Msa,3ass2sLssylE2ym0yxme0ntH\4.x\PD\FlaF1utluoeuos:os0oro3coc/chh1hae7esn/mii0ic4cca,aalsls.As.n.aPFPlRRRyOOOs\\\tSSW:aaSKmsC.ppHRlLDeieEDsD\BhIC\a\o03t31E17o70v04e4AAICCDOGESAACcS0EF3KM1604 TE MLeeatnshttondmB:oodaisftiinegd:: Th Mar 1 a8isks08 2054 P:\Da~a\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\CotGrove Thu Mar 18 09:51:08 2004 B-PDES 031604 Job Code= ' PPrriinntteedd:: FFrril MMaarr 1199 1122::2244::0088 22000044 | peNammeeer= orouneas 031704A-623 T4:extc=o suitonace pes 4:C6 Sulfonate PFHS I 1L9159858--33,, DDFF==110000 f1003o311770044A.-662253 Sm Sm (tn, (Mn, 220) 2x3) a 1188--MMaarr--22000044 1166::1155::4477 LLCC//MMSS//MMSS #6 ser MofR5 ChM annea65ES0- 8.87 MRM of 5 Channels ES399 > 80 Siar SE2.84e4 reaArea | oerrprp ! 0! .... 22.0000 44.0000 66..0000 5. co sulfonate pros : C8 Sulfonate PFOS | [L1958.3, DF=100 L1958-3, DF=100 |0;3a1s70t47A-06243n5S.mm6(2uMn3n., 22x93) 1 la 88.0000 0219.21 3246 rpm Ying| 1100..0- 000 - - Time 6-Mar-2004 16:15:47 18-Mar-2004 16:15:47 LLCC//MMSS//MMSS ##66 MRM of 5 Channa E5- MRM of 5 Channels ES55500 49119..77>000e9449. ea|| Area 20 in 50 a0 i060 | " re -------- TTimee 2.00 4.00 6.00 8.00 10.00 | Exyoan Research, 3058 Ressaseh Drive, State College, FA 14803 Exygen Research, 3058 Research Drive, State College, PA 16801 i `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NTSSTUYUBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT.TEECNCTGT.IIVV2EE7-OOGRRu-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00332222 auotsasers 3M MN01539473 I comer seme vee re Quantify Sample Report | EIR en, mses iin, metres site Study No. :L1958, Set No. :031704A, Ext.Date:03/17/04, Analyst=K.Risha Page 47 BA, Sample List= P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SaunpleDB\031704A CG ACSFM fis pen, pesos Last modified= Fri Mar 19 11:30:32 2004 1 iiwrmmtmmssvimemtsrs7ni Method= P=\Data\LCMSMS6\Massly~x\Fluorochemicals.PRO\MethDB\ConGrove ~rPDES 031504 BeE erien tian dian es Last modified= Thu Mar 18 0%:51=08 2004 Job Code= Printed= Fri Mar 19 12=24:08 2004 I NmTaaemxxeet=s= 031704A-624 I: C6 Acid PFHA A 1 L19159588--2222,, DDFF==110000 031704A-624 Sm (Mn, 2x3) I TM 100, |i I| i TET | = 2.00 4.00 88.6600 1166334411-~ Wot 1188--MMaarr--22000044 1166::3377::331(~ LLCC/IMMSS//MMSS #6 MRM of 5 Channels ES- 33131 >>2263699) 99..8844ee44| Areal 1 6.00 - 8.00 10.00 Tim|e 2:C8 Acid PFOA aos3170472 Sm vn,23) [LL11995588--2222,, DDFF==110000 031704A-624 Sm (Mn, 2x3) ass9.04 26432 MRMof 5 Cha= moi5s-| 1188-.MMaarr--22000044 L16T:37:30 LLCC/IMMSS//MMSS #6 MRM of 5 Channels ES413 > 369 11..5500e855 Area lero A EEE | | 0I~-' ' '/~, .... , .... , .... , .... , .... I .... , .... , .... , .... , .... , ' "-~ Time 2.00 4.00 6.00 8.00 10.00 : C4 Sulfonate PFBS I5L11995588--2222,, DDFF==110000 | c:oroontze mom 228 031704A-624 Sm (Mn, 2x3) 10o0r~ er 220.000 a4.0 00 660.000 u2o8.29 522 i : 88.0000 1188--MMaarr--22000044 1166::3377::30 ian LClMS/MS #6 it MRM of 5 Channels ES- we 299 > 99 23.72e3 7Area 0100.000 Tne [| Time | FR. Exygen Research, 3058 Research Drive, State College, PA 16801 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00332233 3M MN01539474 I rT Jn Quantify Sample Report | BEIT, een, me meteesriron, smsipson sin Study No.:LI958, Set No.:031704A, Ext.Date:03/17/04, Analyst:K.Risha Page 48 pire Sr TOV eae esse RAS RASAS 3 A557 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\031704A CG ACSFM mL, prem: I MMLeeattshhtooddm::odified: PFPr:1i\\DDMaatatara\\LL1CC9MMSS1MM1SS:6E3\\0MM:aa3ss2ssll2yy0nn0xx4\\FFll~u1oorroocchheenmiiccaallss..PPRROO\\MMeetthhDDBB\\CCoottGGrroovvee IN~PPDDEESS 003311660044 ER rea, Bh ESS Last modified: Thu Mar 18 09:51:08 2004 Ee Job Code: Printed: Fri Mar 19 12:24:08 2004 I NTTaeemxxett=~: 031704A-624 : C6 Sulfonate PFHS i 1LL1199588--2222,, DDFF==110000 str0sn524 5m in. 23) 031704A-624 Sm (Mn, 2x3) C[ e| fm obTRiee 2.00 4.00 6.00 028.87 ah RA 8.00 1188--MMaarr--22000044 1166::3377::33(0 LLCC//MMSS//MMSS #6 Wea rg 2 MRM of 5 Channels ESeSso)n 399 > 80 2.02e4 erArea ae10.00 Time 5:C8 Sulfonate PFOS LL11995588--2222,, DDFF==110000 oner;o aze sme,2) 031704A-624 Sm (Mn, 2x3) 1188--MMaarr--22000044 1166::3377::3300 LLCC//MMSS//MMSS##66 I" wr ws 9.19 MRM of 5 Channels ES499 > 99 = 55 8.83e3 oiArea I FEAMMANASYAMANE A MARAE SAMEC 2.00 4.00 6.00 8.00 10.00 Time E~ygen Research, 3058 Research Drive, State College, PA 16801 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00332244 3M MN01539475 I J -- JS | SQStutuaudndyytiNNfooy..::SLLa1Im99p55l88e,, ReSSpeetotrNtNoo..::003311770044AA,, EBxxtt..DDaattee:=0033//1177//0044,, AAnnaallyysstt=:KK..RRiisshhaa Page 49 A -- Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\SampleDB\031704A CG ACSFM fat esti ty I MeMLetatshhtooddm:=odified= P?Fr=3i\\DDaMatataar\\LL1CC9MMSS1HM1SS:663\\0M:Ma3s2asls2y0sn0x4l\Fylunorxoc\heFmlicualos..rPPoRROOc\\MMheettehhDDnBBi\\CCcoottaGGrrloovvsee NNPPDDEESS 003311660044 Fra INE Last modified: Thu Mar 18 09:51:08 2004 BaJob Code: I PPrriinntteedd=: PFrrii MMaarr 1199 1122::2244::0088 22000044 Name: 031T04A-625 B=Text= tei: C6 Acid PFHA o 0517040525 5m in 23) I |1L11995588--223, DF=1000 031704A-625 Sm (Mn, 2x3) |= | 1001%1 TE 2.00 4.00 I ee6.00 os MRS Crmoee2e6.) t8e.5o923 1188--MMaarr--22000044 1166::5599::1:13 LLCC//MMSS//MMSS #6 MRM of 5 Channels ES- 3131.>0276659) 16923L 1.01Areae5 | = ee ww 8.00 10.00 Time. 2: C8 Acid PFOA Por T LL11995S8S--2233,, DDFF==11000000 031704A-625 Sm (Mn, 2x3) i[ 1001%t oor9.0~ 26721 26721~ 1188--MMaarr--22000044 1166::5599::1133 LLCC//MMSS//MMSS #6 oS Crm MRM of 5 Channels ESgs 413 > 369 1.51e5| ed 1 .SAreea5l PIMPMSNA "MAMA AIRS 01=-, ,,~ .., ., ., ., .,,...., ..,.~ ...,....,,.. , ~-, : .., ... ," ....,.... " Time 2.00 4.00 6.00 8.00 10.00 3:C4 Sulfonate PFBS LL11995588--2233,, DDFF==11000000 |003311770044AA--662255 SSmm ((MMnn,, 22xx33)) :| 11'0~'0~ vv~ t 8.229 448655~ I es 1188--MMaarr--22000044 1166::5599::11:3 LLCC//MMSS/lMMSS #6 MMRRMM ooff 55 CChhaannnneellss EESS-- 2 2999>>99999 33..3333e33, Area To ae ew rae k m We . i 2.00 4.00 a 6.00 8.00 AINAAre, 10.00 Time TAI reer Serre A A TD Exygen Research, 3058 Research Drive, State College, PA 16801 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00332255 3M MN01539476 ' SQQtuuuaadnnyttiiNffoyy.1sSLaa1mm3pp5ll8ee, RRSeeepptoorrttNo.:031704A, Ext.Date:03/17/04, AnalystiX.Risha Psaaggee 5500 Study No.:LI958, Set No.:031704A, Ext.Date:03/l?/04, Analys~:K.Risha LSSaaasnmt~pllmeeodLLiiifssitte=:d: PFPe=di\D\MaDatarat\aL1\9CLMC1SM1MS:SS36\0\M:Ma3as2sssl2ly0yn0nx4x\\FFlluuoorroocchheemniiccaallss..PPRROO\\SSaampplleeDDBB\\003311770044AA CCOG AACCSSTFMM | MMLLeeaattsshhttooddmm:=ooddiicfiioedd:: T:PFhr\=iu\DDaMMataatarra\\L1L1C89CHMIS01N9M1S:S:E53610\\:=M03Ka82sasl22s00y00ns44x\1Flyuonroxc\helmiucaolsr..PPoRROOc\\MhMeeeEthhaDDBBi\\CCcoottaGGrrloovvse~ NNPPDDEESS 003311660044 0LJaobsbtCCmoododeda=:ified= Thu Mar 18 09=51:08 2004 PPrriinntteedd:: eFrdi MMaaxr 1199 1122::2244:=0088 22000044 NTNeaaxmmteas=: 003311770044aA--662255 Text= 44: :CC6o Ssuullffoonnaattee pPFrHiSs L[L11995588--2233,, DDFF==11000000 11003017044625 Sm (Mn, 263) | 1188--MMaarr--22L00C00I44M11S66I::M55S99::#11~53 888 MRM of 5 Chann3ol9s>E8S-0 Ey 1.r9e8a0l4 *] oberg RL O]T~ r~ T :~ 200 ;T- 7 2.00 :~ , , 400 .... , .... 4.00 , 6.00 .... ~ .... 6.00 , 800 .... , .... 8.00 , 1000 ...... 10.00 -7~ ] ~TT 7- Time J 55::CC8s Ssuullffoonnaattee pPFrOoSs [LL11995588.-2233,, DDFF==11000000 1188--MMaarr--22L00C00I44M11S66I::M55S99::1133 (0317044625 Sm (Mn, 263) MRM of LCCh/aMnnSe/lMsSES- 031704A-625 Sm (Mn, 2x3) MRM of 5 Channels ES- |e 521 105559 | `real | 1492.261 49779..88>116e9339] Area SE -- TE Te 200 450 60800 10/00 Time 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEAESCCTLTTRTITCOOT AACPOPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00332266 IM_MNO1539477 3M MN01539477 | | QSQtuuuaadnnyttiiNffoyy.isSLaa1mm9ppSllAee, RReeSpeptoorrtNto.:031704A, Ext.Date:03/17/04, Analystik.Risha Page 52 Page 51 Study No.:LI958, Set No.:031704A, Ext.Date:03/17/04, Analyst:K.Risha LSSaeasrmtppllmeeodLLiiifssitt::ed:PrFP\r:Di\aDNtaaatr\a\L1LC9CHMSS1SM1G1S\36M0\a1Ms3as2slsyl2m0yx0n\4xF\lFulouroroocchheenmiicceallss..PPRROO\\SSAammppLleeDDRB\\003311770044AA CCGG AACCSFSM | MMLLeeaattsshhttooddmm:sooddiiffiieedd:= PPTFrrh:\iu\DDaNMataatarar\\LL11CC69HMSS01HM51SS::653\\10MM:=aa03ss82ss1l22yy00nn00xx44\\FFlluuoorroocchheenmiiccaallss. PPRROO\\MNeGtEhHDDBE\\CCoottGGrroovvee K~YEPDDEESS 003311660044 Fob codes Last modified: Job Code: Thu Mar 18 09:51:08 2004 I Poreitnntteeda:s FPrrii MMaarr 1199 1122=02244=10088 22000048 NNaammae:= 003311770044AA--652266 Text= 11: :Cc6s Aaccitda PrFHmA X[XCC003300550044--55,, 550000 nngg//LL SSttaannddaarrdd 10.03311770044AA-:662266 Sm Sm (Mn, (Mn, 253) 2x3) || = 1188--MMaarr--22L00C00/44M11S77/::M2200S::556 87805.460505 MRM MRM of of 55LCCChh/aMann1nSne3e/lMl>ssSEE2SS6#-0-6] 313 >th26e9s rea 4.44e5 Area o 200 00 500 500 1000 Time 2.00 4.00 6.00 8.00 10.00 22:: cCo8 AAcciidd PpFroOAA (XXCC003300550044--55,, 550000 nngg//LL SSttaannddaarrdd 1188--MMaarr--22L00C00I44M11S77I::M22S00::5#5666 00o3311r77y0044A4-662266 Sm Sm (Mn, (Mn, 253) 2x3) 12950.0011485 MRMof MRM of 55LCCChh/aMann4nSn1ee/l3Mlss5$3EES6S#-0-6 Goto 413 > 369 1 iO01 rea 1201851 6.64e5Area 22.0000 44.0000 33.. cCa4 sSuullffoonnaattee PpFrBsS 'XXCC003300550044--55,, 550000 nngg//LL SSttaannddaarrdd 00:3311770044AA:-662266 Sm Sm (Mn, (Mn, 2:3) 2x3) ' Time .... , .... , .... , .... , .... , .... , .... Time 500 800 00 6.00 8.00 10.00 a8.31 204529451 1188--MMaarr--22L00C00/44M11S77/::2M20S0:5:#15~66 MRM MRM of of 55LGCChh/aMannSne2/el9Mlss9S>EESS3--9 291965>0949) 1.65e4 Area (I RE PR ~ L_ rr Ti ime .... ~ .... ~ .... ~ .... ~ .... ~ .... ~ .... ~ .... , .... ~ .... ~ .... ~ .... Time 200 400, 600 800 1000 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReessesaarzcchh DDrriivvee,, SSttaattee CCoolllleeggee,, P7AA 1166880011 `CHGEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00332277 SW_MNO1839478 3M MN01539478 QQSutuauandntytiiNftoyy.1sSLaa1mm3pp5ll8ee, RReeSppetoorrttNo.1031704A, Ext.Date:03/17/04, Analyst:k.Risha Study No.:LI958, Set No.:031704A, Ext.Date:03/17/04, Analyst:K.Risha aPaggee 5522 LSSaaasmmtppllemeodLLiiifssitt:e:d: PPr:Pdi\\DMDaaatrtaa\\L1L9CCMHS1SM1MS:S36S0\\:MM3aa2ssssl2l0yy0nm4xx\\FPlluuocrroocchheemniiccaallss..P7RROO\\SSaamxpplleaDDBB\\003311770044AA CCGG AACCSFTM MMLLeeaattsshhttooddmm::ooddiiffiieedd:: TFPPhr:riu\\DDMMaaaattrraa\\LL119C6CHMSS10NM13ES::636501\M::Ma30as28sssl2y2y00n00nx84x\\FFlluucorroocchheenmticcaallss..PPRROO\\MNeetthhDDBI\\CCoottGGrroovvee NNPEDDEESS 003311660044 JLJooabbstCComoddoeedr=ified: Thu Mar 18 09=51:08 2004 PPrriinntteedd:: FPreii MMaarr 1199 1122:02244:10088 22000044 NNaammse:: 003311770044A--662266 Text: 44::Cc6o sSuullffoonnaattee PpFrHsS XXCC003300550044--55,, 550000 nngg/LL SSttaannddaarrdd 00"3311770044A4-662266 Sm Sm (Mn, (Mn, 263) 2x3) i % 1188--MMaarr--22L00C00I44M11S77I::M22S00:56 885 MMRRMM ooff 5LCCChhIaMannnSn3e/elM9lssS2EE8SS#--06| 187.28157 39p9 r> 8o0 rea) 9.29e4 Ama | Io 200 400 600 800 1000 Time| Time 2.00 4.00 6.00 8.00 10.00 55: :CC83 Ssuullffoonnaattee P2FPOOSS _ X(CC003300550044--55,, 550000 nngg//LL SSttaannddaarrdd 1188--MMaarr-.22L00C00I44M11S77I::2M200S::556 |os1708A528 5m (vn. 22) 031704A-626 Sm (Mn, 2x3) 921 MMRRMMooff 55LCCChh/aMannnSn'e/elMl4ss>SE9ESgS#9o.-6) | 69i.021s 49339.44">7a7r6e9e449a Iw 64061 | Area [1 | | - Tine L ....20~ 0.... , ....40~ 0.... , ....60, 0.... , ....80, 0.... , ....10-/T0-0~,,,, ,-,, ,Time 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReesseeaarrcchh,, 33005588 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOCNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIDJJIEEASCCTLTTRTITCOOT AACPOPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00332288 IM_MNO1539470 3M MN01539479 QQSutuauandntytiNffoyy. sS1aa1mm5pp5ll8ee, RReeSpptoorrtNto.:031704A, Ext.Date:03/17/04, Analyst:X.Riska sPaaggee 5533 Study No...LI958, Set No. :031704A, Ext.Date:03/l?/04, Analyst:K.Risha LSSauasrmtppllmeeodLLiiifsstti::ed:PiPP\r:Di\aDtNaaat\raL\CL19HCSMMS1SM1:SS36\0\M:Ma3as3sssll2y0ym0ne4x\\FFlluuccrroocchheenmiiccaallss.PPRROO\\SSaamxppllseDDEB\\003311770044AA CCOG AACCSSFFM NaaMLLLeaacab~ssshhtttomocadommo:=doodeddiriitffiiieeeddd:== TPPFrhr=\ui\DDaNMataaterra\\LL11C69CHMOS01NM91SS4=665330\\1=Ma03as62sssl2L2y0000ny44x\Fnluxoro\chP~milccaaullss..cPPRRrOO\\MoSeCthchDDBBh\\CCeoottaGnzrooivvee Thu Mar 18 09=51=08 2004 NNPPDDEESS 003311660044 Job Code= PPrriinntteedd:: PFertl Mwaarr 1195 1122=02244:10088 22000044 NNaammee=: 003311770044AA--662277 Text= iX1::C0Cc3o605Aa0cc4ti-ad6,PpFr1Hi0An00 ng/L Standard XC030504-6, 1000 ngfL Standard I00s331177004A4-662277 Sm Sm (Mn, (Mn, 2:3) 2x3) |th] || | 200 40: 0 2.00 4.00 22:cCa8pAcciidanPFeOoAr [XXCC003300550044--66,, 11000000 nngg//LL SSttaannddaarrdd 1031704527 Sm (Mn, 29) 031704A-627 Sm (Mn, 2x3) Js| ||% | 0 200 300 2.00 4.00 33::(CCc04i30sS5u0u4ll-ff6oo,nnaa1tt0ee00PoFrnBgsS/L Standard XC030504-6, 1000 ng/L Standard 0317048627 Sm (bn, 223) || 031704A-627 Sm (Mn, 2x3) ' |w |1 _ 650 ; 6.00 600 6.00 = 58.5599 850 8.00 oo 1188--MMaarr--22000044 1177::4422::4433 MRMof MRM of 55LLCGCChIhlaMaMnn3SnSna3Ie/iM5Mlss2SSEE#0SS#06--6)| 31377.>.9A622r2e6e059a5 Area |i 1000 Time| Time 10.00 _ 1188--MMaarr--22L00O0044M11S77:M:44S22::44:3 RMof 5LGChlaMnnSa/iMsSES#-6 MRM of 5 Channels ES- sos po 2092.0948 1.2606, 413 > 369 1.28e6 ves|| Area To 800 1000 8.00 10.00 Time 118S--MMaarr--22L00O00M44 S117I7::M44S22::#436 5s88.31t16 MRM MRM of of 5LCCChh/aMannnSn22ele90lMSl9ss9oS>rE>E9eSS#9l.0-96]| rea y 3.27e4 Ar~a | | Bol lrr2r00rrr~ 4--00------ ----6-- 00---- ----.--800ar_y1000ree Tine 2.00 4.00 6.00 8.00 10.00 EExxyyggeenn RReessesaarzcchh,, 33005598 RReesseeaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSUTUYBBIJDJIEAESCCTLTTRTITCOOT AACPOPURRROOTT.TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00332299 SW_MNO1839480 3M MN01539480 ' | QQSuutaaundnyttiiNffoyy.iSSLaa1mm3pp5ll6ee, RRSeeepptoorrttNo.:031704A, Ext.Date:03/17/04, Analystik.Rishe PPaaggee 5544 Study No.=LI958, Set No.=031704A, Ext.Date=03/17/04, Analyst:K.Risha LSSaaasmmtppllmeeodLLiiifssitte::d:P:PP\r=Di\aDtNaaat\raL\CL1HC5MSS1M1MS:SS36\0\M:Ma3as3sssll2yy0nn0x4x\\PFlluucosroocchheeamiiccaallss.PPRROO\\SSaanmpplleeDDEB\\O0I311T70044AA CCOG AACCSFSM | MMLLeeaattsshhttooddmm::ooddiiffiieedd=: PTFPhrr=ul\\DDNaMaetatasra\\LL11C9C6HMSS01HM91S1S:G53603\\M=1Ma30as28sssly22y000n0n44x\xFl\uoFrolchuemoicralos.PPcRROOh\\KMeSeLtnhhDDiBBA\CcCootatGGrlroovsvee NNEPDDEESS 003311660044 6b coder Last modified= Job Code= Thu Mar 18 09=51:08 2004 PPrriinntteedd:: FFerid MMaaxr 1199 11220=22441=0088 22000044 NNaammea=: 003311770044AA--662277 Text= [44:X:CC0C63605sS0uu4ll-ft6oo,nnaa1~t0ee00pPrFnHigSs/L Standard {XC030504-6, 1000 nglL Standard 00;3311770044A7-662277 SSmm ((MMnn,, 225x33)) |I wl 3a58s4.85s68' 18-Mar-2004 17:42:43 1M8R-MMaorf-2LL0CCC0h//4aMMn1nSSe7/Il:M4Ms2SSE:4S##3.661L MRM of 5 Channels ES- 301.988905 399 > 80 Area 1.89e5' Area: io: 22.0000 44.0000 56..0000 88.0000 1100..0000 TTiimmee | 55X:C:0cC3o805sS0uu4ll-ff6oo,nnaa1tt0ee00PpFrnOogSs/L Standard 18-Mar-2004 Ta XC030504-6, 1000 ng/L Standard i003311770044A4-662277 Sm Sm (Mn, (Mn, 23) 2x3) M1R8-MMoafr-2LL0CCC0hI/a4MMnn1SSe7I/lM:Ms4SS2E:S#4-63| 921 MRM of 5 499590) Channels ES- || TM 192.82815 49669..8`>83r3ee9a694li | 200 aw 650 550 : 1000 Timo Time 2.00 4.00 6.00 8.00 10.00 EExxyyggeeun RReesseeaarrcchh,, 33005588 RReessceaarrcchh DDrriivvee,, SSttaattee CCoolllleeggee,, PPAA 1166880011 `CHEOGNNONFEINDPEIFNNITCIDAOLEU-N-NSTSTUUYBBIDJJIAEESCCTLTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRV-DD1EE0RR.2E6E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00333300 3M_MNo1539481 3M MN01539481 MMeettaallss FFIINNAALL RREEPPOORRTT EEVVEENNTT 22 EE0044--00112266 FFeebbrruuaarryy 2255,, 22000044 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 1939.0331 3M MN01539482 North Shore Analytical, Inc. MoDRkLbaR 027m1o3ri7389 MDH ~b # 027-13%389 WDN~ Lab # 3990 DSa12nMial TrSo5n51iho Su 1 FFenin(319) eissss Analytical Report Glens: MAdC:otTeogmeBuntei C1o0t7a45gemnGorvoavtei,oMnNa,55B0l1d6g 145 Cogage Grove, MH 5501 Phone: 6514582072 ~hone: 651 o458o20~2 Fox on438259 Fa~: 651~58~2596 sample rDrF Fednlok a1 " F}eld BtapN .... 8094 Fin ss ~ E~'ueut g095 Date Repos 34104 Sengletfntions ChainSoampfletd t.y: 3M0A89M By: TMGMAM FMG ero: EPA 1651 Method: EPA 1631 ET seid smyssvus | igotr cos owes vee ol < 0,5 fo anv aso 1;{0 2125/7004 3/3120C~4 2125/2004 ..... 31312004 ....... taint meeps agen i sovevied ~w level mereu, resalt~ are reagent Nank o~cted. idps Reviewed By [HY x Reviewed By: ~ ; 1you have ay questions egading is port, plas cal 218) T4658 you ~ave a~y ques~-m~s regarding tgi~ re~or~, please call (218) 72%4658. Sens Ena gH Lina hrsensen CLhinediacCahlriEsnteg~isnee~er CCHEOONNNNFEIDFPEIINNTDCIAOELU-NN- TSSTUYUIBBDJJIAEESCCTLTTRTITCOOT AAGPOPRUROROTTT.EECNCTOTIIVV2EE7 -OO0RR1-DD1EE0RR.0E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00333322 Sw uotsssdss 3M MN01539483 ANnoalryttihcaSl,hoInrce, NootNa 5LLa2sb 79# 10517135809 Vc%NR Lab # 399(117190 2Vi TrFighvSoaes1 5612 Mi l|er Tr~lNHi~way. Suite Do ut1,8)n T34386158 Phone: (2I 8) 729-4658 Te)Aves Fa.,< (218~ 729-4659 Analytical Report Clen: SnMnCoTraogmeBGarues Co0t7a4g6enGorvoavtei,oMnNRa5B30l1d6. 143 Pons 6514582032 Phoebe: 65 t -45g-2032 Fac 681.438.2596 bax: 651-45 g-2596 Dit Repaid: 3403 Date ReDorle4:3/4/04 Sample npormaton: ChanpoflCuestidBsy:: 3M0A89M TTMG Meo: BPA 1631 Mek~od: E~A 1631 sped Ream Field Blmqk Phoe3 Elune o Phase "~ Element TeV or. wm 0s 8092 893 Ss 8{)93 < ~:5 < ~L5 SpeDue mee 2125/20~4 vas 2 g2512004 bmeDme iMtDoyL vow 31312004 oaws od 313/20(}4 Lovie meeny emseientgo Hank crete EowJeve~ mer~ur.~ resales are reagcmt b{a~k corrected, Vnroc Soin U0 Reviewed By: (~ o o~- _ Fou eve any ions gain i por, pese call G13) 29465, have any questi~as rega~Oing Nis rep~, please call (2I 8) 7294658 fe Halos Linda Christensen Li~da Cbrislvr:sen Chemical Engineer CONFIDE-NSTUIBJAECLTTO APROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00333333 sas S3MH.MMNNa0r1s5s39484 Nort Shore Amgen. ET ---- Rama Ct C/iem}~ame TT 3M Cottage G-ore I a sora mass TT B d,a. 14s Enviror:me~ Lab; 10746 ~sovat on Road ~ 65!-768-2032 i ~ PCOT lhIO 2. |ERO [EROS -((FudDF PedalIOOOTWwWeR[xTT GNA Tiowtew Very ET EeEIR SSI A VI [TSX08) 777 ES RNER PI SR 7S | 0 I EESRa NL OL NEL EL mE Ct rar mmm iam omaha IE GS------------ EET 1 Fell BS Besoin io MoO XT TYLATorii Shp,| Rel pees (C11[POFcRa [0 NOCITwal XTT7407] 1 rr ri4 ---- 1 ke] PE T e H etEee -------- JE eeFore d Fempepore ee~feee meres) elAtteo poste ieeeteeterJenemies isin) RB sco goer.coercoerce oreoFroemergormromeforoioeJemmeri eremiorems a. i 1 CE PateI 7 Feigao | owe|Tow | Gegun Te HA PRNIIROO-- (CQ EE |Da | ew Come] TRA IooD |apne | ol ------------]-------- TT ERRTE----eeerieeeirmeslaemrrrseearlrereeseberrolrm eerrrea) Sum sep CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 3M_MN01539485 11993399..00333344 Method: WWTP Scan Method: WWTP Scan RReessulutlt:: CCGG WWWWTTPP CCaarrbboonn SSttuuddyy EEvveenntt 22 E0404--00112266 sh 20683 cCaailinb Astass7e As 188.979 a4xk ai s5kk 1 ( em (cps) ((cecppmss)) 7 pd 7 I)0.000Cali Eqns Licnco,onnCcca((mcmggIln/LtL)) 11.00C0 00.0000Cali Eqns Lincc,oonnCcca((cmmggrIL/tL)) 11.000( ' Corr Coeff: 0.356734 Calib Eq'n: Li~, Ca~c l~t Corr Coeff: 0999734 2 Corr Coeff 0.999637 Calib Eq'n: Li~, Catc Corr Coeff: Be 313107 Comests 3wM 1 6622kk g ((cecppmss)) _ ((cecppmss)) 7 0~.).0000CGCoaarllriibGoEEeqqfn'tns:: LL0ii.~ncc%9,oo5nn5Cc6c~a(0(lcmcm0ggIln/LtL)) 11..00C0 00..0000CGCoaarllriibGEEoqqen'nls: LL0iic.~nc%3o,o5nCn9Cc7caa(0(lmcmc4ag~IlR/tLLt)) 11.000( 3C3 azes Corr Coeff: 4Coarse Corr Coeff: 0o~99704 6611kk A 75k 75k ps om em ((cecppmss)) ((cecppmss)) pd 00GCoarleiCEoqsnts; Lic8nco,5on5nCc7cai6(mcm0agIln/LtL)) 5 11.000~ . 00.0000GCCoaarlleiibCEEoqsqnt'ns;: L0Li#c.nc~8o,,o3nCn5Cc6caa(3(lmcmc9gghIln/~LtL)) Corr Coeff: 0.999639 PPaaggee 11 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- TSSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV27EE-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00333355 11.000( WWiinnLLaabbs322 _MNO1S39485 3M MN01539486 Method: WWTP Scan Method: WWTP Scan RReessulutlt:: CCGG W WWWTTPP CCaarrbboonn SSttuuddyy EEvveennt2t2 EE0044--00112266 zo cCaailinb Po 220353 Pb 220.353 a4s5kk "1 1144Kk 1 (c(ceppmss)) ((ceeppmss)) pe I)0.000Cali Eqns Licnco,onnCcca((mcmggIln/LtL)) : Corr Coeff: 0.355570 Calib Eq'n: Li~, Ca~c Corr Coeff: 0999578 S7e 196.025 ks 4k 11 00 00.0000Cali Eqns Lincc,oonnCcca((cmmggrIL/tL)) 11.000( . Corr Coeff, 0.95841 Calib Eq'n: Li~, Catc Corr Coeff: Z8 amaest Zn 213.857 1 100226k pd ((ceppmss)) ~ ((cecppmss)) y 0i~.000Gali Eqns Lincc,oonCncca((cmmggIn/itL)) 1.00 00.000Gali Eqns Lincc,oonCncca((cmmggI/tlL)) 101.0( . Corr Goeft: 0.955620 Calib Eq'n: Li~% Caic Corr Coeff: 0.999620 0 Corr Goel 0.359755 Calib Eq'n: Li~% Calc ~r~t Corr Coeff: 0.999755 10 PPaaggee 22 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- TSSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV27EE-OOCVRR-DD1EE0RR28EE8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00333366 WWiinnLLaabbs322 _MNO1S39487 3M MN01539487 fre or mr Em mE Sample ID Sdn a 0.Sppm be TE re Sr erat 0.Sppm fe en TEE mm in 83 0.8ppm frm edn SEE mm mm om 0.Sppm EE. SE mm EE 3 0.Sppm fe hE man SEE EE 93 0.Sppm EE. EE EW EE Ea 0.Sppm frm dE an sme mm mE 93 0.8ppm fem ean DR mm Emm lo 0.Sppm fm a i men E EmmAEEm EW BI 0.Sppm boos JdeBEem EneaEnnR aun on we RE ThEm E ME mEmELEEE a ESE MP-04-181 E TE adEEhi ey alnn SE E EEr hEEi E C E mEEmnTtEEE EE=O=E aMPp-04e-1s83 ose EbiTLFE EEashmeEaBmmEegee]ennnnnbra ow im foSSS SHHmRemEemmiEr mHBmemsEmE mmENei mEE:rREEEOB=wnREn MP-04-184 hr, oZ aTAbviReEaa E memma EeeenannnR mESESSEHHREEnERhEESE emEsmmEumnmmmzmMeWEeEEEE EZEOS=BRRER MP-04-185 EE dsvZf E E EaE vEEiaaEEEl l a y y Emea2EEE. nnns3E Lo SPMWSGSTHS[ mMeERaEEuEEEeEEERmEEeEaguagEmmoBE= HaESsmmmr mmmRmEmmLmELIE En2EESoUaNiEMRam%3am=E3=EEnEiERB =2oI3oo8oBom MP-04-185 MS Date 3/1/2004 3/1/2004 3/1/2004 3/1/2004 3/1/2004 3/1/2004 3/1/2004 3/1/2004 3/1/2004 311/2004 311/2004 3/1/2004 3/1/2004 311/2004 3/1/2004 311/2004 3/1/2004 3/1/2004 311/2004 SVI004 3/1/2004 3/1/2004 3/1/2004 3/1/2004 3/1/2004 aos 311/2004 3/1/2004 311/2004 3/1/2004 3/1/2004 311/2004 311/2004 311/2004 3/1/2004 3/1/2004 311/2004 311/2004 3/1/2004 311/2004 3/1/2004 311/2004 311/2004 311/2004 3/1/2004 311/2004 3/1/2004 311/2004 3/1/2004 311/2004 311/2004 3Jl/2004 311/2004 311/2004 3/1/2004 311/2004 3/1/2004 3/1/2004 311/2004 3/1/2004 311/2004 Time 12:40:44 PM 12:40:44 PM 12:40:44 PM 12:40:44 PM 12:40:44 PM 12:40:44 PM 12:40:44 PM 12:40:44 PM 12:40:44 PM 12:40:44 PM 12:45:11 PM 12:45:11 PM 12:45:11 PM 12:45:11 PM 12:45:11 PM 12:45:11 PM 12:45:11 PM 12:45:11 PM 12:45:11 PM 124038PW 12:45:11 PM 12:49:35 PM 12:49:35 PM 12:49:35 PM 12:49:35 PM 11122z::44a99p::33a55sePPMMm 12:49:35 PM 12:49:35 PM 12:49:35 PM 12:49:35 PM 12:54:00 PM 12:54:00 PM 12:54:00 PM 12:54:00 PM 12:54:00 PM 12:54:00 PM 12:54:00 PM 12:54:00 PM 12:54:00 PM 12:54:00 PM 12:58:26 PM 12:56:26 PM 12:58:26 PM 12:58:26 PM 12:56:26 PM 12:58:26 PM 12:56:26 PM 12:56:26 PM 12:58:26 PM 12:58:26 PM 1:02:51 PM 1:02:51 PM 1:02:51 PM 1:02:51 PM 1:02:51 PM 1:02:51 PM 1:02:51 PM 1:02:51 PM 1:02:51 PM Sample ID Initial Sample Wt Field BIk 0.614 MInfPPhRasIe 1Z12 00.86225 Inf Phase 1i2 r 0.721 Port A Unit 1 0.722 PortA Unit 1 MDL 3.26 33.220 2.77 2.77 2.77 Analyte Name Sb 206.836 As 188.979 Be 313.107 Co 228.615 Cd 228.802 Cr 267.716 Ni 231.604 Pb 220.353 Se 196.026 Zn 213.857 Sb 208.836 A~ 188.979 Be 313.107 Co 228.616 Cd 228.802 Cr 267.716 Ni 231.604 Pb 220.353 Se 196 026 20083 Zn 213.857 Sb 206.836 As 188.979 Be 313.107 Co 228.616 Cogn Cd 228.802 Cr 267.716 Ni 231.604 Pb 220.353 Se 196.026 Zn 213.857 Sb 206.836 As 188.979 Be 313.107 Co 228.616 Cd 228.802 Cr 267.716 Ni 231.604 Pb 220.353 Se 196.026 Zn 213.857 Sb 206.836 As 188.979 Be 313.107 Co 228.616 Cd 228.802 Cr 267.716 Ni 231.604 Pb 220.353 Se 196.026 Zn 213.857 Sb 206.836 As 188.979 Be 313.107 Co 228.616 Cd 228.802 Cr 267.716 Ni 231.604 Pb 220.353 Se 196.026 Reported Conc Calib (Calib) Units 0.834 mglL 0.834 mglL 0.863 mg/L 0.863 mglL 0.859 mglL 0.861 mglL 0.862 mg/L 0.868 mglL 0.834 mg/L 0.86 mglL 0.009 mglL 0.007 mg/L 0.001 mg/L 0.003 mglL 0.004 mg/L 0.005 mg/L 0.006 mglL 0.007 mglL 0 002 mg/L 001 mpl 0.007 mglL 0.011 mglL 0.002 mglL 0.001 mglL 0.003 mglL g00..o0000o46smmmeggtllLL 0.006 mglL 0.005 mg/L 0.008 mglL 0.005 mglL 0.008 mg/L 0.001 mglL 0.001 mg/L 0.004 mg/L 0.004 mg/L 0.005 mglL 0.006 mglL 0.005 mglL 0.004 mglL 0.009 mg/L 0.01 mg/L 0.003 mg/L 0.001 mg/L 0.004 mg/L 0.004 mglL 0.005 mglL 0.006 mg/L 0.005 mglL 0.011 mg/L 0.006 mg/L 0.797 mglL 0.803 mglL 0.818 mglL 0.801 mglL 0.77 mglL 0.821 mg/L 0.85 mglL 0.846 mglL 0.898 mglL Reported Conc (Samp) 0.834 0.834 0.863 0.863 0.859 0.861 0.862 0.868 0.834 0.86 N D N D N D ND N D N D N D N D N D NNNODD N D N D ND NNNODD N D N D N D N D N D N D N D ND N D N D N D N D N D N D N D N D N D ND N D N D N D N D N D N D 55.2 55.61 56.64 55.44 53.33 56.89 58.87 58.59 62.19 Samp Units rng/L rng/L rng/L rng/L mg/L rng/L rng/L rng/L rng/L rn~i/L mg/kg mg/kg rng/kg mglkg rng/kg rng/kg rng/kg rng/kg rng/kg ah rng/kg mg/kg rng/kg rng/kg mg/kg moh rng/kg rng/kg mg/kg rng/kg rng/kg rng/kg rng/kg rng/kg mg/kg rnglkg rng/kg rng/kg mg/kg rng/kg mg/kg rng/kg rng/kg rng/kg mg/kg mg/kg rng/kg rng/kg rng/kg rng/kg mg/kg rng/kg rng/kg rng/kg rng/kg rng/kg rng/kg rng/kg rng/kg mg/kg rng/kg QC Recovery 1 O4.23 1 O4.28 107.86 107.65 107.35 107.66 107.76 108.47 104.27 107.51 80% 60% 82% 80% 77% 82% 85% 65% 9O% 311/2004 1:02:51 PM Zn 213.857 1.116 mg/L 77.3 rng/kg 112% en CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00333377 3M MN01539488 Sample ID bs M P-04-195 brane MP-04-186 ad MP-04-187 be MP-04-186 fo0.8ppm [uMpPo-0s4t-1a8s9 Date Time Sample ID TE TTmT ete 3/1/2004 EEE SEER = 3/1/2004 iE oe iSEr Egmair = 3/1/2004 a 3/1/2004 i3 ) EER a ow EE EME 3/1/2004 mrs 3/1/2004 Ii=E oa EEE 3/1/2004 5 ge my = 3/1/2004 Wa HthEe EmEiEe =3 3/1/2004 Lea j5E mami om 311/2004 i 311/2004 iE Fi 3/1/2004 HE Emi = 3/1/2004 iE oe of 311/2004 1:07:24 PM 1:07:24 PM 1:07:24 PM 1:07:24 PM 1:07:24 PM Lab BIk 1:07:24 PM 1:07:24 PM 1:07:24 PM 1:07:24 PM 1:07:24 PM 1:11:51 PM 1:11:51 PM 1:11:51 PM 1:11:51 PM Initial Sample Wt 0.723 PE DERase ow SHE EE EW 311/2004 3/1/2004 Pi=E EoEa TR 2 311/2004 iE on gieE EEmRmEi =ou 3/1/2004 3/1/2004 Taos 311/2004 Pros eam 3/1/2004 3/1/2004 iE om i 2: = 3/1/2004 3/1/2004 1:11:51 PM Por~A Unit 1 D 1:11:51 PM 1:11:51 PM 1:11:51 PM 1:11:51 PM TTS TEP 1:11:51 PM 1:16:18 PM 1:18:18 PM 1:16:18 PM 1:16:18 PM 0.647 as BE ERE = aos 3/1/2004 iE EE 3/1/2004 11v::11i66i ::1188 PPe MM POoe Rrt BB UUm nNit T1 00.8685 i) Hr ERE oT 3/1/2004 1:16:18 PM gE ERE = 3/1/2004 1:16:18 PM i= ae iE SEE = 3/1/2004 1:16:18 PM a Seat 3/1/2004 1:16:18 PM 3/1/2004 1:20:45 PM iIE= =a ats 3/1/2004 1:20:45 PM 5a tBhEr mEmRrE == 3/1/2004 1:20:45 PM 3/1/2004 1:20:45 PM iI3=52oB3eoas ow SEEhE mEmmrEEE 3/1/2004 3/1/2004 iE ok HHEE EERmEi 3/1/2004 iE iE Emi =om 3/1/2004 3/1/2004 3/1/2004 Em HE ae Ee oO 311/2004 I= =m ir mm En Ee 3/1/2004 52% BE En Em 3/1/2004 3/1/2004 322200 gE Em ERE 3/1/2004 3/1/2004 1:20:45 PM Port B Unit 1 D 1:20:45 PM 1:20:45 PM 1:20:45 PM 1:20:45 PM 1:20:45 PM 1:25:13 PM 1:25:13 PM 1:25:13 PM 1:25:13 PM 1:25:13 PM 1:25:13 PM 0.767 i5E o2mE [ELEE EE E EL R OE 3/1/2004 1:25:13 PM MDL 2.77 3.09 33.008 2.54 Analyte Name Sb 206.836 As 186.979 Be 313.107 CO 228.615 C,d 228.802 Cr 267.716 Ni 231.604 Pb 220.353 Se 196.026 Zn 213.857 Sb 206.836 A~ 188.979 Be 313.107 CO 228.616 Cd 228.802 Cr 267.716 Ni 231.604 Pb 220.353 Se 196 026 520083 En 213.857 Sb 206.836 As 188.979 Be 313.107 Co 228.616 Cagis Cd 228.802 Cr 267.716 Ni 231.604 Pb 220.353 Se 196.026 7n 213.857 Sb 206.836 As 188.979 Be 313.107 Co 228.616 Cd 228.802 Cr 267.716 Ni 231.604 Pb 220.353 Se 196.026 Zn 213.857 Sb 206.836 As 188.979 Be 313.107 Co 228.616 Cd 228.802 Cr 267.716 Ni 231.604 Reported Conc Calib (Calib) Units 0.005 mg/L 0.002 rng/L 0.001 mg/L 0.004 mg/L 0.005 mg/L 0.005 mg/L 0.006 mg/L 0.003 mg/L 0.011 mg/L 0.004 m~/L 0.009 mg/L 0.005 mg/L 0.001 mg/L 0.004 mg/L 0.004 mg/L 0.005 mg/L 0.005 mg/L 0.005 mg/L 0 004 mg/L 00% mot 0.004 mg/L 0.006 mg/L 0.005 mg/L 0.001 mg/L 0.004 mg/L osmal 0.004 mg/L 0.005 mg/L 0.006 mg/L 0.005 mg/L 0.004 mg/L 0.005 mg/L 0.012 mg/L 0.004 mg/L 0.001 mg/L 0.003 mg/L 0.005 0.005 0.005 0.005 0.011 0.005 0.834 0.833 0.853 0.859 0.857 0.861 mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L 0.859 mg/L Reported Conc (Samp) N D ND ND ND N D N D N D N D ND N D N D ND ND ND Samp Llnits mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg rng/kg mg/kg rng/kg rn~/k~ mg/kg mg/kg mg/kg mg/kg ND rng/kg ND mgikg ND rng/kg N D mg/kg N D mg/kg NOND ND oh rng/kg mg/kg ND mg/kg ND rng/kg ND mg/kg NNNDDO moh rng/kg mg/kg ND mg/kg ND mg/kg ND rng/kg ND mg/kg N D rng/kg ND mg/kg ND mg/kg ND mg/kg ND rng/kg N D mg/kg N D mg/kg N D rng/kg ND mg/kg N D mg/kg 0.834 rng/L 0.833 mg/L 0.853 mg/L 0.859 mg/L 0.857 rng/L 0.861 rng/L 0.859 rng/L QC Recovery 104.20 104.06 106.59 107.42 107.12 107.58 107.32 3/1/2004 3/1/2004 3Jl/2004 LEeEnEd 311/2004 I= oa 3/1/2004 iE3/1/2004 52a 2004 3/1/2004 3/1/2004 3/1/2004 iimE o=an 3/1/2004 5iE2EaE 3/1/2004 1:25:13 PM 1:25:13 PM 1:25:13 PM 1:29:41 PM 1:29:41 PM 1:29:41 PM 1:29:41 PM 11 :29:42 1 PPMM0 pPoy4 rtAyU1 anity4 1:29:41 PM 1:29:41 PM 1:29:41 PM rBSHENEtheEoEeEeEnEEEaEeEnRaRWEiEE: =e==z=A3y w0.o63n7 a 3.14 Pb 220.353 Se 196.026 Zn 213.857 Sb 206.836 As 188.979 Be 313.107 EME CO 228.616 Cd 228.802 Cr 267.716 Ni 231.604 Pb 220.353 0.856 mg/L 0.828 mg/L 0.857 mg/L 0.009 mg/L 0.001 mg/L 0.002 mg/L Sibiet 0.004 mg/L 0.004 mg/L 0.005 mg/L 0.005 mg/L 0.005 mg/L 0.856 mg/L 0.828 mg/L 0.857 mg/L N D rng/kg ND mg/kg ND mg/kg WO moh ND mg/kg ND mg/kg ND mg/kg ND mg/kg N D rng/kg 107.04 103.45 107.17 3/1/2004 1:29:41 PM Se 196.026 0.003 mg/L ND mg/kg 3/1/2004 1:29:41 PM Zn 213.857 0.004 mg/L ND mg/kg coEniebentL surscer oAa prorcceeoReosRsEvTERED CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00333388 mors 3M MN01539489 Sample ID boo MP-04-190 for MP-04-191 [MuPr-0a4t-1e92 bon MP-04-193 bs MP-04-193 MS MP-04-182 A ay gy Date Time Sample ID TTEET A a a 3/1/2004 ion SE Ent om 3/1/2004 ZH fT he r omy ozw 3/1/2004 311/2004 1:34:09 PM 1:34:09 PM 1:34:09 PM 1:34:09 PM Initial Sample Wt = oBRo m BER re ew gFoEnigEmmaErroMOWH 3/1/2004 3/1/2004 iE Em 311/2004 iE aE me Emi ow 3/1/2004 Em PHhEn EEmar o3m 3/1/2004 i515 E14 311/2004 Te311/2004 uE Smemommmr a 3/1/2004 =n 3/1/2004 z= BE pRB 311/2004 1:34:09 PM 1:34:09 PM 1:34:09 PM 1:34:09 PM 1:34:09 PM 1:34:09 PM 1:38:39 PM 1:38:39 PM 1:38:39 PM 1:38:39 PM Port A Unit 4 D 0.748 HE Ean ow we SEEOIBELE 311/2004 311/2004 imE = a Emi 3 3/1/2004 om mmsmEr mr w=m 3/1/2004 1:38:39 PM 1:38:39 PM 1:38:39 PM 1:38:39 PM Port B Unit 4 0.788 MDL 2.67 2.54 Analyte Name Sb 206.836 As 188.979 Be 313.107 Co 228.615 Cd 226.802 Cr 267.716 Ni 231.604 Pb 220.353 Se 196.026 Zn 213.857 Sb 206.836 As 188.979 Be 313.107 Co 226.618 Cd 228.802 Cr 267.716 Ni 231.604 Pb 220.353 Reported Conc Calib (Calib) Units 0.009 mg/L -0.001 mg/L 0.002 mg/L 0.004 mg/L 0.005 mglL 0.005 mg/L 0.005 mglL 0.004 mg/L 0.008 mglL 0.004 mllL 0.008 mglL 0 mg/L 0.001 mg/L 0.004 mglL 0.005 mg/L 0.005 mg/L 0.005 mglL 0.004 mg/L Reported Conc (Samp) N D ND ND ND ND N D N D N D ND N D N D ND ND ND ND N D N D N D Samp Llnits mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg ml/k] mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg QC Recovery 3/1/2004 311/2004 T Siac m Tce 3/1/2004 3/1/2004 EE 3/1/2004 3/1/2004 TE 312006 3/1/2004 3/1/2004 z iE o 3/1/2004 3/1/2004 iE3/1/2004 dea 3/1/2004 3/1/2004 inmnm 3/1/2004 3/1/2004 iE3/1/2004 i1E Rn ow 311/2004 iE3/1/2004 Zs 3/1/2004 3/1/2004 = iE3/1/2004 . 208 3/1/2004 3/1/2004 izE = am 3/1/2004 22 3/1/2004 Si BER 311/2004 iE am 3/1/2004 nm 3/1/2004 = 3/1/2004 3/1/2004 3/1/2004 Z= 3Jl/2004 H2om-72 311/2004 I=311/2004 311/2004 m= EER, 3/1/2004 Zw 3/1/2004 3/1/2004 iE Emmm 311/2004 is am 3/1/2004 iE ER 3/1/2004 1:38:39 PM 1:38:39 PM 1:43:08 PM 1:43:08 PM 1:43:08 PM 1:43:08 PM vasosew 1:43:08 PM 1:43:08 PM 1:43:08 PM 1:43:08 PM 1:43:08 PM 1:43:08 PM 1:47:37 PM 1:47:37 PM 1:47:37 PM 1:47:37 PM PPoTrt BB UUMnitA4CD 1:47:37 PM Combined Elf 1:47:37 PM 1:47:37 PM 1:47:37 PM 1:47:37 PM 1520P7M 1:47:37 PM 1:52:07 PM 1:52:07 PM 1:52:07 PM 1:52:07 PM 1:52:07 PM Combined Eff 1:52:07 PM 1:52:07 PM 1:52:07 PM 1:52:07 PM 1:52:07 PM 1:56:37 PM 1:56:37 PM 1:58:37 PM 1:56:37 PM 1:58:37 PM Field BIk Dup 1:56:37 PM 1:56:37 PM 1:58:37 PM 1:58:37 PM 00.86223 33.221 3.25 on0.615 3.25 0.72 2.78 Se 196 026 ames Zn 213.657 Ft Sb 208.836 As 188.979 Fc IE Be 313.107 Co 228.618 for = Gogig Cd 228.802 Cr 267.716 de Emr om Ni 231.604 mE Emr ow Pb 220.353 iE Em Ea Se 196.026 5513 Zn 213.857 Sb 206.836 arm As 188.979 smhuEnm: oBu Be 313.107 n Co 228.616 ghmE mEmME: oH Cd 228.802 Cr 267.716 dBee EEMmEr ow Ni 231.604 oo Pb 220.353 ME Emi om Se 196.026 EI ee Mail rEa 268% Zn 213.857 Sb 206.836 As 166.979 IE oEm ousm ozR Be 313.107 am ES AEE Co 228.618 5 IZ 1 Cd 228.802 Cr 267.716 $HIe EEmmoInm oooB Ni 231.604 Pb 220.353 Se 198.026 Imag EEE Zn 213.857 if Zaa8 Sb 206.836 Sfehmm EEmmmmiy o=:o AS 166.979 Be 313.107 Im Ear om Co 228.616 aTemn EEaE:E SomE Cd 228.802 Cr 267.716 Prac = Ni 231.604 iI ms EEmamIry E3= Pb 220.353 0 013 mg/L OmRmeL 0.006 mg/L 0.009 mg/L 0 mg/L 0.001 mg/L 0.004 mg/L oosmat 0.005 mg/L 0.005 mg/L 0.005 mg/L 0.004 mg/L 0.014 mg/L 0.005 mg/L 0.005 mg/L -0.009 mg/L 0.002 mg/L 0.003 mg/L 0.005 mg/L 0.004 mg/L 0.004 mg/L -0.001 mg/L 0.011 mg/L 099mol 0.002 mg/L 0.909 mg/L 0.695 mg/L 0.956 mg/L 0.942 mg/L 0.924 mg/L 0.966 mg/L 1.002 mg/L 1.014 mg/L 0.796 mg/L 1.326 m@/L 0.011 mg/L 0.003 mg/L 0.001 mg/L 0.004 mg/L 0.004 mg/L 0.005 mg/L 0.006 mglL 0.007 mglL ND mg/kg NoN D N D mag mg/kg mg/kg ND mg/kg ND mg/kg ND mg/kg NNNODD a mg/kg mg/kg N D mg/kg N D mg/kg ND mg/kg N D mg/kg N D mg/kg ND mg/kg ND mg/kg ND mg/kg ND mg/kg N D mg/kg N D mg/kg N D mg/kg ND mg/kg N D 77338.888mmmoggv//kkegg 72.73 mg/kg 77.74 mg/kg 76.61 mg/kg 75.1 mg/kg 78.51 mg/kg 81.46 mg/kg 62.41 mg/kg 64.73 mg/kg 107.8 m@/k@ N D mg/kg ND mg/kg ND mg/kg ND mg/kg ND mg/kg N D mg/kg N D mg/kg N D mg/kg n91l% 90% 96% 94% 92% 97% 100% 101% 80% 133% Se 196.026 0.006 mg/L ND mg/kg 3/1/2004 1:58:37 PM Zn 213.857 0.005 mglL N D mg/kg EER CERT 0 5 rs CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00333399 3M MN01539490 frre Sample ID bow MP-04-197 fon MP-04-194 0.Sppm hoe MP-04-196 MP-04-198 bo0.8ppm Initial or me es Boe Date Time Sample ID Sample TI Wt TE Ee 3/1/2004 2:01:00 PM 3/1/2004 2:01:00 PM 3/1/2004 2:01:00 PM 2 311/2004 2:01:00 PM BimE BaeER ow 3/1/2004 3/1/2004 2:01:00 PM 2:01:00 PM 100 ppm Stanc 0.706 i= E ae 3/1/2004 2:01:00 PM 3/1/2004 2:01:00 PM iE ae 3/1/2004 2:01:00 PM E iE m 311/2004 2:01:00 PM EEE 311/2004 2:05:31 PM 3/1/2004 2:05:31 PM I= Ee 3/1/2004 2:05:31 PM Zz3/1/2004 2:05:31 PM 3/1/2004 HE Elen owe 3/1/2004 2:05:31 PM Combined Eff I 2:05:31 PM 0.801 Z iE a Em 3/1/2004 2:05:31 PM = 3/1/2004 2:05:31 PM MDL 2.83 2.50 po Bm am a Analyte Name A Srl a Ek R Sb 206.836 As 188.979 Be 313.107 Yo IZ EB Co 228.615 Em Em EE Cd 226.802 IE I= 7 Cr 267.716 BFZe EEmx mmmm IoBd Ni 231.604 ihn Ew nm Pb 220.353 B Se 196.026 PEE E En 5W5E 8 Zn 213.857 Sb 206.836 fEemERnn:y ooua As 188.979 Be 313.107 GEER om Co 228.615 Cd 228.802 SEE IEEE Cr 267.716 a Emi 3 Ni 231.604 mBsE EEmMrE woHm Pb 220.353 Reported Conc Calib (Calib) Units 1.254 mg/L 1.229 mg/L 1.254 mg/L 1.274 mg/L 1.254 mglL 1.286 mg/L 1.326 mg/L 1.301 mg/L 1.219 mg/L 1.429 mllL 0.012 mg/L 0.007 mg/L 0.002 mglL 0.004 mglL 0.005 mg/L 0.005 mglL 0.006 mg/L 0.005 mg/L Reported Conc Samp (Samp) Units 88.82 rng/kg 87.05 rng/kg 88.83 mg/kg 90.21 mg/kg 68.83 r~lg/kg 91.09 mg/kg 93.91 rng/kg 92.13 mg/kg 86.31 rng/kg 101.2 ND mg/kg ND rng/kg ND rng/kg ND mg/kg ND mg/kg ND mg/kg ND mg/kg ND rng/kg QC Recovery 89% 87% 89% 9O% 89% 91% 94% 92% 86% 101% 3/1/2004 3/1/2004 Zn eer 3/1/2004 = Ee EERE=v 3/1/2004 3/1/2004 3/1/2004 Zo Bar wai od oH 312004 3/1/2004 z= GE ame = oF 3/1/2004 3/1/2004 3/1/2004 I= pu EE EEE ZOE 3/1/2004 311/2004 Sis Sze Swe comet No mo 3/1/2004 io-n arm 311/2004 iE fohEaenmi E8E 3/1/2004 3/1/2004 Bae z EEE es win SRE 3 311/2004 iE gm mm: oH 3/1/2004 Ze dBee mBMmEr woom 3/1/2004 zm SI 3/1/2004 3/1/2004 311/2004 Eoaen aAa RaT 3/1/2004 ion EE EE Oo 3/1/2004 2 EE iE om mB 3/1/2004 Gi EER. am ES ESSE OB 311/2004 iE gam Em Um B 3/1/2004 ay Fr Ew um 3 3/1/2004 3/1/2004 =u He EW SEE 3/1/2004 3/1/2004 IiLz= a I ESe-nmimiaE--auoamem--1n 3/1/2004 2:05:31 PM 2:05:31 PM 2:09:56 PM 2:09:56 PM 2:09:56 PM 2:09:56 PM 2093P6M 2:09:56 PM 2:09:56 PM 2:09:56 PM 2:09:56 PM 2:09:56 PM 2:09:56 PM 2:14:23 PM 2:14:23 PM 2:14:23 PM 2:14:23 PM 2:14:23 PM 2:14:23 PM 2:14:23 PM 2:14:23 PM 2:14:23 PM 2:14:23 PM 2:18:48 PM 2:15:46 PM 2:18:48 PM 2:18:48 PM 2:18:48 PM 2:18:48 PM Lab BIk Dup 100 ppm Stanc 2:18:48 PM 2:18:48 PM 2:18:48 PM 2:18:48 PM 0.591 0.641 2.69 3.12 Se 196 026 Zn 213.657 8b 206.836 As 188.979 Be 313.107 Co 228.618 cane Cd 228.802 Cr 267.716 Ni 231.604 Pb 220.353 Se 196.026 Zn 213.857 Sb 206.836 As 188.979 Be 313.107 Co 228.616 Cd 228.802 Cr 267.716 Ni 231.604 Pb 220.353 Se 196.026 Zn 213.857 Sb 206.836 As 166.979 Be 313.107 Co 228.618 Cd 228.802 Cr 267.716 Ni 231.604 Pb 220.353 Se 196.026 Zn 213.857 0 01 mglL 0.005 mglL 0.797 mg/L 0.797 mg/L 0.834 mg/L 0.821 mg/L omzmeL 0.82 mg/L 0.622 mglL 0.819 mg/L 0.824 mg/L 0.796 mg/L 0.821 mglL 0.007 mg/L 0 mglL 0.001 mg/L 0.004 mg/L 0.004 mglL 0.005 mglL 0.006 mg/L 0.003 mg/L 0.008 mg/L 0.005 mglL 1.163 mglL 1.142 mg/L 1.176 mg/L 1.185 mglL 1.169 mg/L 1.199 mglL 1.239 mg/L 1.206 mg/L 1.133 mg/L 1.331 m~lL ND mg/kg ND rng/kg ND mg/L ND rng/L ND rng/L ND mg/L NO ot ND rng/L ND mg/L ND rng/L ND rng/L ND rng/L ND rng/L ND rng/kg ND rng/kg ND mg/kg ND rng/kg ND rng/kg ND rng/kg ND mg/kg ND rng/kg ND mg/kg ND mg/kg 90.73 rng/kg 69.05 rng/kg 91.71 rng/kg 92.42 rnglkg 91.17 rng/kg 93.5 rng/kg 96.61 rng/kg 94.07 mg/kg 88.39 mg/kg 103.8 99.57 99.58 104.19 102.61 12271 102.45 102.71 102.41 102.96 99.54 102.64 91% 89% 92% 92% 91% 94% 97% 94% 88% 104% 3/1/2004 3/1/2004 3/1/2004 IBi=m oEEmR 311/2004 Zn 3/1/2004 2:23:20 PM 2:23:20 PM 2:23:20 PM 2:23:20 PM 2:23:20 PM Sb 206.836 As 166.979 Be 313.107 E ShiEmEm Co 228.615 Ten Wm Cd 228.802 O.791 0.784 0.817 0.808 0.81 mglL mg/L mg/L mglL mg/L 0.791 rng/L 0.784 rng/L 0.817 mg/L mmma 0.808 rng/L om 0.81 rng/L 98.8 EEtd9603 102.17 101.04 101.23 3/1/2004 2:23:20 PM Cr 267.716 0.812 mglL 0.812 rng/L 101.49 HE311/2004 3/1/2004 3/1/2004 3/1/2004 2:23:20 PM 2:23:20 PM 2:23:20 PM 2:23:20 PM I Ni 231.604 Pb 220.353 Se 196.026 Zn 213.857 0.81 mglL 0.809 mg/L 0.782 mg/L 0.81 mg/L 0.61 rng/L 0.609 mg/L 0.782 rng/L 0.81 rng/L 101.27 101.07 97.75 101.22 EER CERT 0 5 rs CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00334400 3M MN01539491 Method: WWTP scan cab Calib Result: Method: Result: CG WWTP Carbon WWTP Scan CG WWTP Carbon SSttuuddyy EEvveenntt 22 EE0044.-00112268 NNoonn-DDiiggeesstt Sha0sa3 Astasars As 188.979 ~ a 4 2k 3k peem (cps) . ops)em (cps) dd 0~..o0o0 coconncc((mmggi/LL)) 11..00C0 ali Eqn: Li, Gale nt alib Eqn: Lin, Gale nt Calib Eq'n: Li~, Ca~ ~t B' estar Gore Col: 0.857535 2Comes Gore Col; 0.555186 Corr Coeff: 0.997935 00..0000 ccoonncc((mmggi/LL)) 11..00(0 Calib Eq'n: Li~, Catc Corr Coeff: 0o999195 m ~ an 1 2M 38k Leem (cps) Leem (cps) ~~ 06..0000 ccoonncc((mmggi/LL)) 1.00 alib Eqn: Lin, Gale nt alib Eqn: Lin, Gale nt Calib Eq'n: Li~% Caic 3azzesn ore Cost; 0.836503 .pe or Cost; 0.8350 Corr Coeff: 0998903 00..0000 `ccoonncc((mmggi/LL)) 11.000( Calib Eq'n: Li~% Calc ~nt Corr Coeff: 0o99909 so an J 40k 47k oepm ms) _ ~~ (cps) eempms) ~ ~~ (cps) 06..0000 ccoonncc((mmggi/LL)) alib Eqn: Li, Gale It Calib Eq'n: L#~0 talc ~r~t s Gort Got:0.356015 Corr Coeff: 0o99~0t 8 100 . 00..0000 ccoonncci(mmogl/LL)) alib Eqn: Lin, Gale Int Calib Eq'n: L#~, Calc h~t Gort Gout 0.338522 Corr Coeff: 0o998922 PPaaggee 11 `CHCEOONNNNFFEIIDPDEIENNNTTCIIAOALLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT.IIVV2EE7-OOCRRU-DD1EE0RR.2E8E8NN6TT2EERREEDD IN IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00334411 11.000( WWiinntLaabbs3z2 u_mnotssais 3M MN01539492 Method: WWTP Scan cCaalliibb Result: Method: Result: WGCGW G TWWPWWSTTcPPanCCaarrbboonn SSttuuddyy EEvveenntt 2 2 EE0044--00112266 NNoonn--DDiiggeesstt Ni 231.604 PPbb 222200..335533 2277kk > 88k ((cecppmss)) . ((cecppmss)) > i/, rd 0.00Calib Eq'n: Licnco,onnCcac(l(mmcggIln/LtL)) 11.00 00..0000Calib Eq'n: Licnco,onnCcac(l(mmcagIln/LtL)) 11.000( CCCooarrlrirbCCoEoeqef'ffnf::: 0L0.i~99,998C893a33~00c lnt CCCooarrlrirbCCoEoeqef'fnff::: 0L0o.i~99,99C7777a44tc77 lnt 577 196.026 238 0213857 Zn 213.857 *2k ~ 6655kk A ((ceppmss)) 7 ((cecppmss)) . 0~.).0000Calib Eqn: Licnco,onnCcac(l(mmcggIln/LtL)) 1.00 00..0000Calib Eqn: Licnco,onnCcac(l(mmcagIln/LtL)) 11.000( CCoarlribCoEeqf'fn:: L0i.~%99C90a5ic5 ~nt CCoarlribCEoqe'n:: L0i.~%999C0a8l1c ~r~t 5 Corr Coeff: 0.999055 10 Corr Coeff: 0.~99061 10 PPaaggee 22 CCHOEONNNFNFIEIDDPEEINNNTTICIAAOLLUN-- STSUUYBBDJJIEESCCTTTRITTCOOT AACOPPURRROOTT,TEECNCTOT,IIVV2EE7-OOCRRV-DD1EE0RR-2E8E8NN6TT2EERREEDD IINN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00334422 WWiinnLLaabb3322 33MM_MMNNO011553399449933 fee Sample ID en0.8ppm . F[ieeled Blank epad Influent 1/2 ad Port 1A ..Port 1B oyPo y tycmee e Date Time 3/1/2004 2:31:38 PM a PmhoR amm 3/1/2004 2:31:36 PM Concentration m J Bn m Ee Analyte Be, E0BEo Name Sb 206.836 a EmRuEmm a32 As 188.979 Reported Conc Calib (Calib) Units 0.744 mg/L 0.743 mg/L QC Recovery 93.04 92.87 3/1/2004 3/1/2004 EE BER wo EEE HE 3/1/2004 momo EE bm 2 3/1/2004 3/1/2004 Immamm Emdoommo2 3/1/2004 mom Tum oO 3/1/2004 3/1/2004 iS8ELE ESE.ee 3/1/2004 iam EEE 3/1/2004 3/1/2004 Z mamo. mmEE oz 3/1/2004 312004 3/1/2004 nm gz 3/1/2004 En sz 3/1/2004 3/1/2004 T EEEE i tenzd 3/1/2004 3/1/2004 re re 3/1/2004 Wim = 3/1/2004 3/1/2004 mam tmmE 3/1/2004 EE HEE BEER 2 W204 3/1/2004 mum git 2 3/1/2004 myn Ezz 3/1/2004 3/1/2004 Hee 3/1/2004 3/1/2004 iEaen r=2 3/1/2004 mas IEE 3/1/2004 3/1/2004 3/1/2004 mam. EEE ize 3/1/2004 3/1/2004 mmaarr EEEzE z2 3/1/2004 mE Nz 3/1/2004 2:31:38 PM 2:31:38 PM 2:31:38 PM 2:31:38 PM 2:31:38 PM 2:31:38 PM 2:31:38 PM 2:31:36 PM 2:36:06 PM 2:36:08 PM 2:36:08 PM 2:36:08 PM 23606 PM 2:36:08 PM 2:36:08 PM 2:36:08 PM 2:36:08 PM 2:36:08 PM 2:36:06 PM 2:40:36 PM 2:40:36 PM 2:40:36 PM 2:40:36 PM 24036 PM 2:40:36 PM 2:40:36 PM 2:40:36 PM 2:40:36 PM 2:40:36 PM 2:40:36 PM 2:45:01 PM 2:45:01 PM 2:45:01 PM 2:45:01 PM zasorem 2:45:01 PM 2:45:01 PM 2:45:01 PM 2:45:01 PM Be 313.107 Co 228.616 100% Cd 228.802 Cr 287.716 Ni 231.604 Pb 220.353 Se 196.026 Zn 213.857 Sb206.636 ND As 188.979 ND Be 313.107 ND Co 228.616 ND 1000%% oasis Cd 228.802 Cr267.716 NNNDDD Ni 231.604 ND Pb220.353 ND Se 196.026 ND Zn 213.857 ND Sb206.836 ND As 188.979 ND Be 313.107 ND Co 228.616 ND 1o00%% case Cd 228.802 Cr267.716 WNNDDD Ni 231.604 ND Pb220.353 ND Se 196.026 ND Zn 213.857 ND Sb206.836 ND As 188.979 ND Be313.107 ND Co 228.616 ND "Gras 100% Cd 228.802 Cr267.716 wNNDDo Ni 231.604 ND Pb220.353 ND 0.779 mgtL 0.773 mgJL 0.774 mgJL 0.775 mg/L 0.774 mg/L 0.772 mg/L 0.742 mg/L 0.775 mg/L mg/L mg/L mg/L mg/L mpl mg/L mg/L mgJL mg~L mg/L mg/L mg/L mg/L mg/L mg/L mmmoggl//LL. mg~L mg/L mg/L m~/L mg/L mg/L mg/L mg/L mol mg/L mg/L mg/L mg/L 97.33 96.64 96.69 96.82 96.73 96.48 92.81 96.91 3/1/2004 3/1/2004 San ZR Soom to mo 3/1/2004 L mam f HEE 3/1/2004 mum HEE oz 3/1/2004 ZS. ge 3/1/2004 3/1/2004 ImEuEmE ooew ZEEEEEE 22 3/1/2004 3/1/2004 mam EEE 2 3/1/2004 mEuEmn E TEsz 3/1/2004 2:45:01 PM 2:45:01 PM 2:49:26 PM 2:49:26 PM 2:49:26 PM 2:49:26 PM 2:49:26 PM 2:49:26 PM 2:49:26 PM 2:49:26 PM 2:49:26 PM 100% Se 196.026 ND Zn213857 ND 8b206.636 ND As 188.979 ND Be 313.107 ND Co 228.616 ND Cd 228.802 ND Cr287.716 ND Ni 231.604 ND Pb220.353 ND Se 196.026 ND mg~L mg/L mg/L mg/L mg/L mgtL mg/L mg/L mg/L mg~L mg/L 3/1/2004 2:49:26 PM Zn 213.857 ND mg/L SRS SORT ay CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00334433 3M MN01539494 Sample ID foePort 4A .[pPoerte4=B i: Combined Eft 1/2 eeLab Blank .-0.8ppm Tutt ma re Date Time Tre 3/1/2004 2:53:51 PM mIEaEmE tfmhEER o2 3/1/2004 2:53:51 PM Concentration Analyte Name Sb206.836 As 188.979 Reported Conc (Calib) ND ND Calib Units mg/L mg/L QC Recovery 3/1/2004 2:53:51 PM Be 313.107 ND mg/L 3/1/2004 3/1/2004 SEIheEsEEdEoEm OvMt GEdEiiElEe m2t 3/1/2004 3/1/2004 Ea EEE oR 3/1/2004 EC LE 3/1/2004 3/1/2004 S EEE as 3/1/2004 IEE mmo 3/1/2004 Eas EER 2 3/1/2004 EEEm Eshe oA 3/1/2004 32004 3/1/2004 ia oe osEER oR 3/1/2004 pam mm om 3/1/2004 mas HERB 3/1/2004 DEE seen of 3/1/2004 3/1/2004 PER 3/1/2004 Imm mmm 3 3/1/2004 EEE EEE RB 3/1/2004 EEE EEE 2 3/1/2004 Em SEER OB 3/1/2004 EEE EEE OB 3/1/2004 EE mR on 3/1/2004 pom RRR oR 3/1/2004 (ALR ow DRE 3/1/2004 IEEE oe ERLE 3/1/2004 mE ov BEET en ow 3/1/2004 Eas Comme AmB 3/1/2004 IE IER ER 3/1/2004 EEE gE ER OB 3/1/2004 IEEE EE am 8 3/1/2004 EEE EI SEB 3/1/2004 EEEEE EmeoaEnm 8om 3/1/2004 2:53:51 PM 2:53:51 PM 2:53:51 PM 2:53:51 PM 2:53:51 PM 2:53:51 PM 2:53:51 PM 2:56:17 PM 2:58:17 PM 2:58:17 PM 2:58:17 PM 25817 PM 2:58:17 PM 2:58:17 PM 2:58:17 PM 2:58:17 PM 2:58:17 PM 2:56:17 PM 3:02:44 PM 3:02:44 PM 3:02:44 PM 3:02:44 PM 3:02:44 PM 3:02:44 PM 3:02:44 PM 3:02:44 PM 3:02:44 PM 3:02:44 PM 3:07:11 PM 3:07:11 PM 3:07:11 PM 3:07:11 PM 3:07:11 PM 3:07:11 PM 3:07:11 PM 100% 1000%% 100% Co 228.616 ND Cd 228.802 ND Cr257.716 ND Ni 231.604 ND Pb220.353 ND Se 196.026 ND Zn 213.857 ND Sb206.636 ND As 188.979 ND Be 313.107 ND Co 228.616 ND Grate Cd 228.802 Cr257.716 NNNDDO Ni 231.604 ND Pb220.353 ND Se 196.026 ND Zn 213.857 ND Sb 206.836 ND As 188.979 ND Be 313.107 ND Co 228.616 ND Cd 228.802 ND Cr267.716 ND Ni 231.604 ND Pb 220.353 ND Se 196.026 ND Zn 213.857 ND Sb 206.836 As 188.979 Be 313.107 Co 228.616 Cd 228.802 Cr267.716 Ni 231.604 mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mpl mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L 1.055 mg/L 1.131 mg/L 1.133 mg/L 1.008 mg/L 1.05 mg/L 1.036 mg/L 1.071 mg/L 106% 113% 113% 101% 105% 104% 107% 3/1/2004 3/1/2004 3/1/2004 EaYs Y 3/1/2004 IE ns mE = 3/1/2004 Ens EER OB 3/1/2004 GEER EmEE oN 3/1/2004 ium om SEE om 3/1/2004 EEE EEE 2 3/1/2004 ina aE 2 3/1/2004 EEE EEE oR 3/1/2004 Imasy sERR 3/1/2004 AR py 3/1/2004 I i 3/1/2004 IEEE me an 2 3/1/2004 EEE IEE ERB 3/1/2004 mn Eno 3/1/2004 EEE we SEE ER 3/1/2004 IER ovosEE Bm i 3/1/2004 3/1/2004 EIEEEEE 2EdE EaED oBo 3/1/2004 EEE EEE Em EH 3/1/2004 3/1/2004 3:07:11 PM 3:07:11 PM 3:07:11 PM 3:11:45 PM 3:11:45 PM 3:11:45 PM 3:11:45 PM 3:11:45 PM 3:11:45 PM 3:11:45 PM 3:11:45 PM 3:11:45 PM 3:11:45 PM 3:16:23 PM 3:16:23 PM 3:16:23 PM 3:16:23 PM 3:16:23 PM 3:16:23 PM 3:16:23 PM 3:16:23 PM 3:16:23 PM 3:16:23 PM 100% 100% Pb220.353 Se 196.026 Zn 213 857 8b206.636 ND As188.979 ND Be313.107 ND Co 228.616 ND Cd 228.802 ND Cr287.716 ND Ni 231.604 ND Pb220.353 ND Se 196.026 ND Zn213.857 ND Sb 206.836 As 188.979 Be 313.107 Co 228.616 Cd 228.802 Cr287.716 Ni 231.604 Pb 220.353 Se 196.026 Zn 213.857 1.041 mg/L 1.193 mg/L 1 542 mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L 0.696 0.691 0.715 0.702 mg/L mg/L mg/L mg/L mg/L 0.704 mg/L 0.701 mg/L 0.702 mg/L 0.704 mg/L 0.694 mg/L 0.705 mg/L 104% 119% 154% 87.04 86.38 89.39 67.80 87.97 87.60 87.74 87.98 86.77 88.14 CONFIDENTIAL - SUBJECT TO A PROTECTIVE ORDER ENTERED IN HENNEPIN COUNTY DISTRICT COURT, NO. 27-CV-10-28862 11993399..00334444 3M MN01539495