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& 3M ENVIRONMENTAL LABORATORY METHOD EXTRACTION OF POTASSIUM PERFLUOROOCTANESULFONATE OR OTHER FLUOROCHEMICAL COMPOUNDS FROM URINE FOR ANALYSIS USING HPLC- ELECTROSPRAY/MASS SPECTROMETRY/MASS SPECTROMETRY Method Number: ETS-8-96.0 Adoption Date: 7-28-44 Author: Lisa Clemen, Glenn Langenburg Revision Date: NA Approved By: \ 1] Ze Laboratory Mhnager Date 5/77 Lit hn Group Leader 28/95 Date on A Cloman Technical Reviewer Hara Date 10 SCOPE AND APPLICATION 11 oSrcooptehe:r Tfhliusormoecthehmoidcails fcoormtphoeuenxtdrsacftrioomnoufrpinoet.assium perfluorooctancsulfonate (PFOS) 12 Applicable compounds: Fluorochemicals or other fluorinated compounds. 13 Matrices: Human, rat, and monkey urine or other fluids as designated in the validation report. Word 695 ExtrEaTcoSft-Pi8FoO9Sn6f0om Urine 001045 Page tofis 2.0 SumMMARY OF METHOD 2.1 (ThPiFsOSm)etohroodthdeerscfrliuboersotchheempircoaclesdufrreomfourrienxet,raocrtiontgheproftlausisdsi,umuspienrgflaunorioooncptaainreisnuglfroenaagteent PanFdOSm,ethPyFlO-tSeAr,t-bPuFtOylSAetAh,erE(tVFIOBES)E.-OIHn,thMi5s5m6e,thMo5d7,0e,igphetrfflluuoorrooocchteamniocaatles (aPreOAexAt)ra,ctaendd: ssaurmrpolgeataensdttahnedaarndal(ysteee f3o.n0 pDaeifriniistpiaorntsi)t.ioAnend iionntopMaiIrBiEn.g reTahgeenMtIiBEadedxetdratcottiwsoremmlovofed maentdhpauntolo,nttoheannfiitlrteorgeedntehvraopuogrhatao0r.u2ntyilmdnryy.lonEafcilhteerxattratcatchiesdretoco3nsctcitpultaesdtiicns0y.r5inmgleoifnto glass autovials. 22 These sample method. extracts arc analyzed following method ETS-8-97.0 or other appropriate 3.0 DeFNITIONS 31 PFOS: perfluorooctanesulfonate (anionofpotassium salt) CF,,SO; 32 PFOSA: perfluorooctane sulfonylamide C,F,,SO,NH, 33 PFOSAA: perfluorooctanc sulfonylamido (ethyDacetate CF,,SO;N(CH,CH,)CH,CO; 34 EtFOSE-OH: 2(N-ethylperfluorooctane sulfonamido)-thyl alcohol CF,SO.N(CH,CH,)CH,CH,OH 35 MSS6: CF,SO,N(H)(CH,COOH) 36 MS70: CF,SO,N(CH,)CH,COOH 37 POAA: perfluorooctanoate C,F,,COO' 3.8 Sumogate standard THPFOS: 1H-1H-2H-2H perfluorooctane sulfonic acid, used as an intemal standard in this method. 4.0 WARNINGS AND CAUTIONS 41 Health and safety warnings 4.1.1 Use universal precautions, especially laboratory coats, goggles, and gloves when handling animal tissue, which may contain pathogens. 50 .0 Inve0 meeme0 nces0000000000 5.1 Athtatthmisaytibmee,pirteissenutnksuncohwnashcoownjtuhgeateexdtrfalcutioornocmheetmhicoadlsis(aefgf.eGcltuecdubryonpiodteesn)t.ialCoinntjeurgfaetreesnces may become deconjugated during reported resultsof target analytes. extraction or analysis resulting in a high bias for ExtractionEoTfS.P8FO.S960from Urine Page 20114 001046 6.0 EQuipMENT 6.1 aTchceepftoalblleo.wing equipment is used while performing this method. Equivalent equipment is 6.1.1 Vortex mixer, VWR, Vortex Genie 2 6.12 Centrifuge, Mistral 1000 or [EC 6.1.3 Shaker, Eberbach or VWR 6.1.4 Nitrogen evaporator, Organomation 6.1.5 Balance (0.100g) 7.0 SUPPLIES AND MATERIALS 71 Gloves 72 Eppendororf disposable pipettes 73 Nalgene bottles, capable ofholding 250 ml and 1 L 74 Volumetric flasks, glass, type A 7.5 L.CHEM vials, glass, 40 ml glass 7.6 Centrifuge tubes, polypropylene, 15 ml 77 Labels 7.8 Oxford Dispenser ~3.0 to 10.0 ml 79 Syringes, capable of measuring 2.5 kL to 50 uL 7.10 Graduated pipettes 7.11 Syringes, disposable plastic, 3 cc 7.12 Syringe filters, nylon, 0.2 um, 25 mm 713 Timer 7.14 Crimp cap autovials and caps 7.15 Crimpers Note: Prior to using glassware and bottles, rinse 3 times with methanol and 3 times with Milli-QTM water. Rinse glass syringes a minimum of9 times with methanol, 3 rinses from 3 separate vials. 8.0 REAGENTS AND STANDARDS 81 Type reagent grade water, Milli-QTM or equivalent; all water used in this method should beMilli-QTM water and may be provided by a Milli-Q TOC PlusTM system 82 Sodium hydroxide (NaOH), J.T Baker or equivalent 83 Tetrabutylammonium hydrogen sulfate(TBA), Kodak or equivalent 84 Sodium carbonate (N&,CO,), J.T. Baker or equivalent 85 Sodium bicarbonate (NaHCO), J.T. Baker or equivalent ExtractiEonToSf8P.F9OS60from Urine 001047 Page 3of 14 8.6 Methyl-T-Butyl Ether, Omnisolv, glass distilled or HPLC grade 87 Methanol, Omnisolv, glass distilled or HPLC grade 88 Urine frozen from supplier 89 Fluorochemical standards 89.1 PFOS (3M Specialty Chemical Division), molecular weight = 538 8.9.2 PFOSA (3M Specialty Chemical Division), molecular weight = 499 8.9.3 PFOSAA (3M Specialty Chemical Division), molecular weight = 585 8.9.4 EIFOSE-OH (3M Specialty Chemical Division), molecular weight = 570 8.9.5 M56 (3M Specialty Chemical Division), molecular weight = 557 8.9.6 MS70 (3M Specialty Chemical Division), molecular weight = 571 89.7 POAA (3M Specialty Chemical Division), molecular weight = 452 89.8 THPFOS (1-H,1-H, 2-H, 2-H C/F,,SO;H) molecular weight = 428 8.9.9 Other fluorochemicals, as appropriate. 810 Reagent preparation NOTE: Wprheepanraptrieopna,riadnjgulsatragcercovrodlinugmleys.than listed in reagent, standard, or surrogate 810.1 11000N0 msoldbieuamkehrydcroonxtaiidnei(nNga5O0H0)m:lWMeiilglih-QaTMpprwoaxtiemra,tmeliyx2u0n0tilgaNllaOsoHl.idsPoaruer: into a dissolved. Store ina 1 L Nalgene bole. 8102 N1aNOsHodsioluumtihoyndriontxoidae1(0N0amOH!)v:oluDmielturtiec1fl0NaskNaanOdHdil1u:t1e0.toMveoalsuumreeu1s0imnglMoifll1i0N QM water. Store in a 125 ml Nalgene bottle. 810.3 0o.f5TMBAteitnrtoabaut1 yLlavmomlounmeiturmihcycdornotgaeinnisnuglf5a0t0e (mTlBMAi)l:liW-QeTMighwaatpeprr.oAxdijmuastteltyo p16H9 10 NusaiOnHg ,apapddrosxliowmlaytbe4elc4yautsoe5t4hemlpHofc1h0anNgeNsaaObrHupt(lWyh).ileDialdudtientgotvhoe lluasmtemwlitohf Milli-QTM water. Store ina I L Nalgene bottle. 8.10.3.1 TneBeAderdequusiirnegs 1aNchNecakOpHrisoorltuotieoanc.h use to ensure pH = 10.0. Adjust as 8.10.4 0a.p2p5roMximsaotdeiluym2c6a.r5bonoaftseo/sdoiduimumcabribcoanrabtoena(tNea,buCfOfje)r(aNnad,2C1O.0/NgaoHfCsOo,d)i:umWeigh bicarbonate QM water. (NaHCO,) Storeina | iLntNoaalg1 eLnevoblotutmlee.tric flask and bring to volume with Milli- 8.11 Standards preparation 8.11.1 Prepare PFOS standards for the standard curve. 8.11.2 Pflrueopraorcehoetmhiecralflsutoarnodcahredmsiacrael asctcaendpatradbsl,e a(sfoarpeprxoapmrpilatee,.onMeulwtoirckoimnpgosnteanntdard solution containing 1.00 1.10 ppm EXFOSE-OH.) ppm PFOS, 1.02 ppm PFOSA, 0.987 ppm PFOSAA, and ExtractionoETfSP8F.O9S60from Urine Pagedof 14 001048 8.11.3 tWheeiagchtuaaplpwreoixgihmtatienltyhe10S0tamngdaordf PLoFgObSooikn.to a 100 ml volumetric flask and record 8.11.4 Bring to volume with methanol for a stock standardof approximately 1000 ppm (ug/ml). 8.115 aDpilpurtoexitmhaetsetloyck50soplpumt.ion with methanol for working standard 1 solution of 8.11.6 aDpiplruotxe.wo5r.0kipnpgm.standard 1 with methanol foar working standard 2 solution of 8.11.7 Dilute working standard approx. 0.50 ppm. 1 with methanol for a working standard 3 solution of 812 Surrogate stock standard preparation 8.12.1 CWJeFi,g;hSOap;pHrionxtiomaat5e0lyml50v-o6l0ummegtroifcsfulrarsokgaantde srteacnodradrtdhe1-aHc,t1u-alH,we2i-gHh,t.2-H, 8.12.2 Bring to volume with methanol for a surrogate stockofapproximately 1000-1200 ppm. 8.12.3 Prepare stock to aa s1u0mmoglavtoelwumoertkriincgfsltaasnkdaarndd. brTirnagnstfoevroalpupmreoxwiimtahtemleyth1amnolloffsourarrogate S`wtoarnkdianrgdsLtoagnbdaorodko.f100-120 ppm. Record the actual volume transferred in the 9.0 SAMPLE HANDLING 9.1 All samplesarereceived frozen and must be kept frozen until the extraction is performed. 92 Allow samples to thaw to room temperature prior to extraction. 100 QuaLITY ContRoL 10.1 Solvent Blanks, Method blanks and matrix blanks 10.1.1 An aliquot of 2.0 ml methanol is used as a solvent blank 10.1.2 Extract two 2.0 method blanks. ml aliquots ofMilli-QTM water following this procedure and use as 10.1.3 Extract blanks. two 2.0 mi aliquotsofthe See 11.1.4. urine following this procedure and use as matrix 102 Matrix spikes 10.2.1 Pthreepaacrceuraancdyoafntalhyezeexmtartarcitxiosnp.ike and matrix spike duplicate samples to determine 102.2 `Pmraetpraixrereccaecihvsepdiwkiethuseiancghassaammpplleesceth.osen by the analyst, usually the control 10.2.3 cEuxrpveec.teAdddciotnicoennatlrastpiioknesssmhaouyldbefailnlcilnudtehde maindd-mraanygefoalfltihnethieniltoawl-craalnigberaotfitohne initial calibration curve. ExtacEoTftSP8oF.On9S60from Urine 001049 Page Sof 14 10.2.4 Prepare one matrix spike and matrix spike duplicate per 40 samples, with a minimumof 2 matrix spikes per batch. 103 Continuing calibration verifications 10.3.1 Pinrietipaalrecacloibnrtaitniuoinngcucrvael.ibration verification samples to ensure the accuracyof the 103.2 Psraemppalrees,. atFoarmeixnaimmpulme,, ionfaescaomnptlienusientg=ca3l4i,brfaotuironchveecrkifsicaarteiponreppearregdroaunpdof 10 extracted. 10.3.3 Prepare each continuing prepare the initial curve. calibration verification from the same matrix used to 10.3.4 The expected concentrations will fal within the mid-range of the initial calibration curve. Additional spikes may be included that fal in the low-range of the initial calibration curve, This is necessaryifthe analyst must quantitate using tohnalny 5thpeplbo--w e1n0d00ofpptbh)e. calibration curve (for example, 5 ppb -- 100 ppb, rather 11.0 CALIBRATION AND STANDARDIZATION 111 Prepare matrix calibration standards 11.11Transfer 2.0 mlofurine to a 15 ml centrifuge tube. 11.12 Record each sample volume on the extraction sheet. 11.1.3 While preparing a totaloftwenty-two aliquots in 15 ml centrifuge tubes, mix or shake between aliquots. 11.1.4 Two 2.0 ml aliquots serve as matrix blanks. 11.1.5 Typically use the standard concentrationsandspiking amounts listed in Table 1, at the endofthis section, to spike, in duplicate, two standard curves, for2 total of twenty standards, two matrix blanks, and two method blanks 11.1.6 RraenfgeerstaonvdaltihdeatLiionneraerpCoarltiFbrAaCtTio-nTROaXn-g1e3(1L,CWR)20f6or7,calwihbircahtiloinstcsutrhveesw.orking 11.1.7 Use Attachment D as an aid in calculating the concentrationsof the working standards. See Section 13.0 to calculate actual concentrations of PFOS in calibration standards. 11.2 To each standard, blank, or continuing check, add appropriate amountofsurrogate `working standardforthe concentration to fall within the calibration curve range 10ppb 1500 ppb. 113 Extract spiked matrix standards following 12.6-12.16ofthis method. Use these standards to establish each initial curve on the mass spectrometer. ExtractionEoTfSP8FO9S60from Urine 001050 Page of 14 Table 1 Approximate spiking amounts for standards and spikes Using 2.0 ml ofmatrix Working standard WL | Approx. final conc. | Approx. final conc (approx. conc.) ofanalyte in matrix_| Of analyte in solvent Bk Bam | 1.25 ppb 5.00 ppb 0.500 ppm [10 | 0.500 ppm 26.0 .p50pppbb. 21500.p0 pppbb 3.00 ppm 50.0 ppb [00p 5.00m ppm. [10 | 2625.50pppbb 250 ppb S00ppm 50.0 ppm |5 I 2a0S0pppebb| 7S5000ppepbb 500ppm |10| 250ppb 1000 ppb 50.0 ppm. 375 ppb 1500 ppb 12.0 PROCEDURE 12.1 Owabttearibnatfrhozen samples and allow to thaw at room temperature or in a lukewarm 122 Vortex mix for 15 seconds, then transfer 2.0 ml or other appropriate volume to a 15 ml polypropylene centrifuge tube. 123 Retum unused samples tofreezerafter extraction amounts have been removed. 124 Record the initial volume on the sample weight/volume worksheet. . See Attachment D. `The original weight/volume worksheet s included in the study binder. 12.5 Label the tube with the study number, sample ID, date and analyst initials. See attached `worksheet for documenting the remaining steps. 12.6 Spike all samples, including blanks and standards, ready for extraction with surrogate Standard as described in 11.2. 127 Spike each matrix with the appropriate amountofstandard as described in 11.1, or Table Tin that section, for the calibration curve standards. Also prepare matrix spikes and continuing calibration standards. 128 Vsoarmtpelxesmifoxr t1h5essetcaonnddasr.d curve samples, matrix spike samples, and continuing calibration 129 Check to ensure the 0.5 M TBA reagent is at pH 10. I not, adjust accordingly. 1210 To cach sample, add 1 mi 0.5 M TBA and 2 ml of 0.25M sodium carbonate/sodium bicarbonate buffer. 12.11 Using an Oxford Dispenser, add 5 ml methyl-tert-butyl ether. 12.12 Cap each sample and put on the shaker at a settingof 300 rpm, for 20 minutes. ExtractionEoTfSP-F8O9S60from Urine 001051 Page of 14 12.13 Centrifuge for 20 to 25 minutes ata settingof 3500 rpm, or until layers are separated. 12.14. Labela fresh 15 ml centrifuge tube with the same information as in 12.5. 12.15 Remove 4.0 mlof the organic layer to this clean 15 mi centrifuge tube. 12.16 Put each sample on the analytical nitrogen evaporator until dry, approximately 30 to 60 minutes. 12.41 Add 0.5 mlofmethanol to cach centrifuge tube using a graduated pipette. Ifexcessive residue is present, add the methanol and allow the extract to sit for 30 minutes prior to vortexing 12.17 Vortex mix for 30 seconds 1218 Lmaatbreilx,thfeinaaultosovlivaelnwti,tehxttrhaecstitoundydantue,mbfelru,oraoncihmeamlicnaulmcboemrpoannedntgesn,deerxt,rsacatmipolnettyipem,epvoiianlt, file archive number, and analys(s) performing the extraction. 12.19 Attach a0.2 jum nylon mesh filter to a 3 ce syringe and transfer the sample to this syringe. Filter into a 1.5 mi glass autovial or low-volume autovial when necessary. 12.20 Cap and store extracts at room temperature or refrigerated at approximately 4 C until analysis. 12:21 Complete the extraction worksheet, attached to this document, and tape in the study notebook or include in study binder, as appropriate. 13.0DATAANALYSISANDCALCULATIONS 13.1 Calculations 13.1.1 Calculate actual concentrationsof PFOS, or other applicable fluorochemical, in calibration standards using the following equation: mi ofstandard x concentrationof standard (ug /ml) = ml of standard + mlof surrogate standard + initial matrix volume (al) Final Concentration (g/ml) ofPFOS in matrix 14.0 METHOD PERFORMANCE 14.1 TfohrespmeectihfiocdMdeDtLectainodn lliimmiitto(fMqDuLan)tiitsaatniaolny(teLaOnQd)mavtalruiexs s(pseeceifAitc.taRcehfmeerntto BM).DL report 142 The following quality control samples are extracted with each batch of samples to evaluate the quality of the extraction and analysis. 14.2.1 Method blanks and matrix blanks. 14.2.2 Matrix spike and matrix spike duplicate samples to determine accuracy and precisionofthe extraction. 14.2.3 iCnointitailncuailnigbrcaatliiobnractuirovne.check samples to determine the continued accuracy of the 143 Refer to section 14of ETS-8-97.0 for method performance criteria. ExtractiEonoTfSP8F.O9S60from Urine Page of 14 001052 15.0 POLLUTION PREVENTION AND WASTE MANAGEMENT 15.1 Halul motahnerasnadmmpolenkweaystseaimspdliespwoassetdeiins dnoinsipnofseecdtiionuisnfbeicothiaozuasrbdiowhaasztaercdonwtaasitneersc.ontainers, Flammable disposed in solvent broken gwlaasstsecoisntdaiisnpeorssedloicnatheidghinBtTheUlcaboonrtaationreyr.s. Used glass pipette waste is 16.0 RECORDS 16.1 nCootmepbloeotkeotrheinecxlturdaectiinonthweo3r-krsihnegesttautdtyabcihnedderto, tahsisapmpertophroida,tea.nd tape in the study 17.0 TABLES, DIAGRAMS, FLOWCHARTS, AND VALIDATION DATE 17.1 Attachment A, Extraction worksheet 172 Attachment B, MDL/LOQ values and summary 173 Attachment C, Calibration standard concentration worksheet 174 Attachment D, Sample weight/volume worksheet 18.0 REFERENCES 18.1 The validation report associated with this method is FACT-TOX-131, W2067. 19.0 AFFECTED DOCUMENTS 19.1 `ETCSo-m8p-o9u7n.d0s, in"AUnrailnyesiEsxotrfaPcottsaUsssiinugmHPPeLrCf-lEuloreocotcrtoasnpersaulyfMonaastse SorpeOctthreormFelturoyr/oMcahsesmical Spectrometry" 20.0 Revisions ReNvuimsbieorn Reason For Revision ReDvaitsieon ExtractiEonoTfSPF.O9S6f0romUrine 001053 Page 90f 14 Extraction Worksheet ETS-8-96.0 SMuadtryix7 SoApmporogxa.e Spdpm| apFpEr0M.o5pxo.m| apFpMr$pop.m | approFx.C$M0ppm| Commens BoWxha fiActual ppm| "sctal ppm| "cual ppm |'senal ppm DateSpiked Anlyst eo rr 7 -- w wo or -- -- r rr r r rr r r r r r rr r r ---- rr 7 fr] --r -- r--r --r r r1 r rT T ] r rr rr r 1 -- r -- rr 0r r T r rr rr r rT r --r T r r rr r r 7/1 f Ie i (a Lt, [Bak saw emewm= ml | ser [S Sikemmn ere] rma Doned0eec 1] `Cont. Cal. Verifications usedsamematrixas for sd curve. Auachment A EEox TfSF.8O.S96f0c omUne 004.054 Page 100114 MDL/LOQ values for human urine Linear Calibration Range (LCR) FOS [(ppb4 ) ||1(6 p4p7b)| 15 ppb 1500 ppb (in final MeOH extract) PFOSA 5205 ppppbb--- 11050000ppppbb((iinnffiinnaall MMeeOOHHeexxttrraacctt)) PFOSAA. EFOSE-OH 2255 ppppbb -- 11000000 ppppbb ((iinn ffiinnaall MMeeOOHH eexxttrraacctt)) M556 25 ppb - 1000ppb (in final MeOH extract) M570 25 ppb- 1000ppb (in final MeOH extract) d= not determined NOTE: to calculate MDL, LOQ, and LCR values in ug/miofurine divide the above values by 4. MthDesLe/mLatOrQicveaslwueesreinexrtatraacntdedmaonndkaenyaluryizneedwweirteh nthoet hstuamtiastnicuarlilnyedceuterrvmeisnteod.detTewromicnuerevqeusivinaleeancche.of Rareespaosnssuemsedinttohbeerastimainldarmotoritkheeyvawleureessdiemtielramritnoetdhefohruhmuamnanreusrpionnes.es, therefore, their MDL and LOQ Ifasuitable amountofclean, control matrix i available, samples will be evaluatedversus a curve extracted from urine originating from the same species as the specimens. Please see LOQ Summary and MDL study in FACT-TOX-131, W2067 for further information. Attachment B: MDL/LOQ Summary ETS.8.960 ExtacoftPoFOnS fromUrine 001055 Page 11 of 14 Compound: PFOS Prepared range of| LCR from curve| % Recovery Human Urine| standards (ppb) (ppb). Range (ng/ml) (ng/ml) RSD Range CE EC I `Compound: POAA Psrteapnadraerddrsa(npgpeb)of| LCR frreom)curve| % RReacnogveery fomtiemes[ | |n | |e w awae ea]]] (ng/ml) (ng/ml). qxua,dratic. 2.5--1p50p 0ppbb | 50ppb-- 1500ppb. 86-105 +-30% Attachment B: MDL/LOQ Summary ETS-8-96.0 001056 Page 120f 14 PArneaprydtaetes: Ton Pair StaSntdaanrddaCradrnvuem-bUerri:ne Equipment number: Sample mates: Methodirevision: BFlinaanlksNoluviednitdaenndiTeNr:: Box Number: TFaCrmgietxastndaalyptep: r05o00xpn.: SFFuCCrrmmoiigxxatssetddstaadpppparrpoopssr..o$$.000010pp0oppmo:m: SAcFctFouOanlSeconSdPceFeOoSmnAetroaPfSFtdStOciaSononAdeanArdss iEnIhOe SKEC Scone mixFORA Sdco SEucGone MSeEeWme|| AAmTt FimAiWvol 1 gm gm wpm gel wpm sper | oem 60.350000 0500 [|03[0.0050010 [ |000 55000 |0 |T0005550 001011||| 00449%9 0499 ||| 050505000]00[0| 5000.5500111||00 op0s0 i|06 2y02r--00775 s55||| [[[53C00o00[ ]] s [[ssswo ww[sr ssooorrr |ag[vams | sso00o] seo | [[0o0o0ts [--2z0o07m55| so |oms| zo $00 [385000 [SI SS0010 500 | 500 sor | S01 | #95 499 S00 | | S00 | son 50.4 | | ooo | 0.0075 | 2007s 20100 S00[Sor[4s suo | sor |aon | ota (CooT505001 | s1 or | #5500 Calculatedconceofnstatndarrdsantth siampolemnatsrix sox oo|isorss] FiPlRcOmoSnle C FiFnRalOcoSneAr PRFoiOnpSleeKolnAem FrEiWulOimoSnEe oFoFgaOlRm oAme FaWoSnc FnNiiSonm e a SSdecr hee aiAte Tzes mmer ew |= eis erat Sw Fina cone: I CEeCSt SJ JCJ J3 1 +n | oH S rwm eee me ts e a n ise e Ta Tnw eee]] [TFCaOleSulte|d PcoRncOeSntrat_iPonFRsaOoflSseAtaAndaErdisOinSmEethanFForOlatRexaAtvreac (0F5Wrioslasmneea vowluemen) : ot proll Surg | piAnedtTmi] E1C091E 00]B. Ssooo Soo Fa] [sC5iTe5--0501T]--SFien|oe E Eon oo O toute "iaw| L s L m owe5 (1500 1503 |15|0 is0 s | IEC IE AvschmensC: StandardCaleulionSheetExEoTft SP-F6O9S6o f0omUn rine 001057 Page 30114 Prep Date(s): Analyst(s): Sample Matrix: Method/Revision: `Target Analyte(s): Study Number: Equipment Number: Final Solvent & TN Number: Matrix Blank/Identifier: Box: tt Toitial We/Vol. mL (------ rr -- -- rrr 1] I -- [1] Er Summaryof method: Notes: `Atachment D: Weight'Volume Sheet ExacEoiTfSPo-O8n9S6f0om Une (014 058 Page 14of 14