Document G5xNJ7JKQ70Er3G8nmexr85jY

V-- I V U J ^ U I U l . Proven Results. M M G _ I79 Analytical Report H if I Fluorochemical Characterization of Water and Sludge Samples Daikin America, Inc. Exygen Research Laboratory Report No. L35195 Testing Laboratory Exygen Research 3058 Research Drive State College, PA 16801 11 Requester tGo? Randy Roussel Daikin America, Inc. PO Box 2252 - x"O O-o?r0n ro -- -3 0 ---trn n Decatur, AL 35609 --z0x xO cp-, <->o F3 "J rtk I i 000143 3058 Research Drive State College, PA 16801, USA PAGE 800.281.3219 F: 814.272.1019 exygen.com 1 In tr o d u c tio n Results are reported for the analysis of surface water and sediment samples received by Exygen Research (Exygen) from Daikin America. The Exygen study number assigned to the project is L35195. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC /M S/M S) was requested for all samples. A total of 2 samples were received for analysis. The samples were prepared and analyzed by LC /M S/M S for the following list of fluorochemicals: T able 1: T arget Analysis Comoound Nam e Perfluorooctanoic Acid Acronvm C 8 Acid (PFOA) The analytical methods used were originally developed for groundwater samples and were validated by Exygen. The validation protocol and results are on file with Exygen. T h e methods w ere adapted for the sludge samples. Sludge sam ple methods have not been fully validated at this time. The samples were submitted in plastic containers. All samples were cooled to 4C from time of collection to receipt at Exygen Research. Sam ples w ere stored at 4C from receipt at Exygen Research until analysis. Samples w ere collected on 9/25/03. Chain-of-custody information is presented in Attachment C. -:,r: Field and laboratory spikes of these fluorochemicals have shown stability for periods greater than 90 days. Samples w ere analyzed within 30 days of receipt. Methods -Analytical and Preparatory , iv! '.- 4.1 4.1 .1 LC/MS/MS S a m p le P re p a ra tio n fo r L C /M S /M S A n a ly s is W ater samples were initially treated with 2 00 uL of 250 mg/L sodium thiosulfate solution to remove residual chlorine. Solid phase extraction (SPE) was used to prepare the samples for LC/M S/M S analysis. A forty-milliliter portion of sample was used for analysis. T h e samples were transferred to a C i8 SPE cartridge. T h e cartridge was eluted with 5 m L of 100% methanol. This treatm ent resulted in an eight-fold concentration of the diluted sam ples prior to analysis. PAGE2 OF5 000144 V Sludge samples w ere first extracted into methanol (5 grams of sludge to 5 ml_ of methanol). % f i' T h e methanol extract was diluted to forty-milliliters and treated in the sam e manner as the w ater sam ples, using SPE. 4 .1 .2 S a m p le A n a ly s is b y L C /M S /M S l/ In HPLC, an aliquot of extract is injected and passed through a liquid-phase chromatographic column. Based on the affinity of the analyte for the stationary phase in the column relative to the liquid mobile phase, the analyte is retained for a characteristic amount of time. Following H PLC separation, ES/M S provides a rapid and accurate m eans for analyzing a wide range of organic compounds, including fluorochemicals. Electrospray is generally operated at relatively mild temperatures; molecules are ionized, fragm ented, and detected, ions characteristic of known fluorochemicals are observed and quantitated against standards. A Hewlett-Packard H P 1100 H PLC system coupled to a Micromass Ultima M S /M S was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SR M ). Sam ples extractions and analyses were performed on 10/2/03 and 10/3/03. Exact dates for extraction and analysis of each sample batch are given in the raw data. Raw ,! analytical data is provided in Attachments D and E. ..... 5 Ana : ;;; :. IV-; : -i ... mm 5.1 Calibration n A 7-point calibration curve was analyzed at the beginning and end of the analytical sequence i for the compounds of interest. The calibration points were prepared at 0, 2 5, 50, 100, 250, 500, and 1000 ng/L (ppt) for LC/M S/M S analysis. The instrument response versus the concentration was plotted for each point. Using linear regression with 1/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determination (r2) w ere determined. A calibration curve is acceptable if r > 0 .9 8 5 (r2 > 0.970). p*m I 'f Calibration standards are prepared using the sam e SPE procedure used for samples. l, Calibration check standards were analyzed periodically (every three to five sam ple injections) throughout the analysis sequence. Compliance is obtained if the standard analyte concentrations are within +/-20% of the actual value. All calibration criteria were m et for this analysis. X; I , 5.2 Blanks Extraction blanks were prepared and analyzed with every extraction batch of samples. The extraction blanks should not have any target analytes present at or above the concentration of i the low-level calibration standard. For these samples, the extraction blanks w ere compliant. Instrument blanks in the form of clean methanol solvent w ere also analyzed after every highlevel calibration standard, and after known high-level samples. Again, the blanks should not have any target analytes present at or above the low-level calibration standard. For the samples presented here the instrument blanks are compliant. P 5.3 Surrogates Surrogate spikes are not a component of the LC /M S/M S analytical methods. #1 PAGE3 O F5 000145 5.4 Matrix Spikes Matrix spikes w ere prepared for each sample. Matrix spike recoveries are given in Attachment B. For sludge samples, recovery is calculated from the amount present in the sam ple extract. 5.5 Duplicates Laboratory duplicates w ere performed for each sample. The duplicate results are included with the sam ple results in Attachment A. Laboratory Control Samples For LC /M S/M S analyses, Milliq w ater was spiked with all compounds with each extraction set. All recoveries for all compounds were between 70-130% in each LCS. Results are given along with the raw data in Attachment D. 6 Data Summary Please see Attachment A for a detailed listing of the analytical results. Results are reported in parts per million (ppm) (ug/mL) for the water samples. Sludge samples are also reported in units of parts per million (ppm) (ug/g). Sludge results are reported on a dry-weight basis. Sam ples are disposed of one month after the report is issued unless otherwise specified. All electronic data is archived on retrievable m edia and hard copy reports are stored in data folders maintained by Exygen. 8.1 Attachment A: Results 8.2 Attachment B: Matrix Spike Recoveries 8.3 Attachment C: Chain of Custody 8.4 Attachment D: R aw Analytical D ata (W ater Samples) 8.5 Attachment E: Raw Analytical Data (Sludge Samples) PAGE4 OF5 000146 / John M. Flaherty, Vice President O ther Lab M em bers Contributing to Data K aren R isha Date PAGE5 OF5 000147 #. * _ Analytical ^ ?] Report 1' '/ Proven Results. Summary of PFOA in Sludge and Water Samples r*r A n a ly te F o u n d (p g /g ) S a m p le ID PF0A A D A I-092503-N W -01 , DAI-0925Q3-NW-01 * 9.37 9.31 f**: A n a ly te F o u n d (p g /m L ) u S a m p le ID PFO A DAI-092503-NW -02 DI-092503-NW -02* 1.01 0.997 ! i ' Laboratory Duplicate ) j ADry-weight basis /T i Li t -j !l 1 000148 ^ ^ 3 0 5 8 Research Drive - # m S t a t e College, PA 16801, USA ^kT: 814.272.1039 m F : 814.231.1580 exygen.com STANDARD TERMS AND CONDITIONS Services provided by Exygen Research are lim ited to th e terms and conditions stated herein, unless otherw ise agreed to in a form al contract. ' CONFIDENTIALITY-- Oxygen Research ("Exygen," "us," or "w e") maintains the strictest confidentiality in all of our client interactions. If a signed confidentiality agreement is required, we will provide one. If a regulatory or legal body subpoenas information, the client will be notified promptly. 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ACCEPTANCE OF PURCHASE ORDER--This Purchase Order becomes a binding agreement, subject to the specific terms and conditions stated herein, upon Exygen's commencement of work. 000149 Recovery Summary for PFOA in Sludge and Water S am p le D escrip tio n D A I-092503-N W -01 500 ng/mL Spike Am ount S p iked (ng/m L) PFOA Amt Found Am ount in S am p le R ec o ve red R eco very (ng/m L) (ng /m L ) (% ) 500 549 985 87 D A I- 92503-N W -02 500 rig/mL Spike 500 1010 1530 104 f #1 n I} Ii jrS i n A 000150 i3058 Research Drive State College, PA 16801, USA ^ L t : 800.281.3219 m F: 814.272.1019 exygen.com 000151 CHAIN OF CUSTODY/ANALYSIS REQUEST FORM Exygen Research Sample Receiving 3117 Research Drive State College, PA 16801, USA T: 814.231.8032 * F: 814.231.1580 exygenresearch.com JP a g e ___ [ _ o f PROJECT INFORMATION ANALYSES REQUESTED | Client (name & address): L)QtKt*\ X p //c .Zv'/c' A O . A fA A l~ 3 5 ~ Phone: (L.5~) 3 o 6 ~ T& oo Fax: Yz t I ) 3o6 - T V 3 Z Sampler: aA o / A ja d d e S / 3& i-s 'o 6Z- Project Manager (Name.& E-mail Address): /^smc/-/ /cMS 5<2- / / ro u ss^ f^ dcu'kn '-ewe/VCo'. C o r i Project Name: RO. # : / / > 0 3 0 2 .-Z. 3 3 0 Quotation # : ftj Please fill out this form completely to ensure correct analysis and proper handling of your samples. SAM PLE ANALYSIS ExyLIMS# Client Sample Identification A /- a v is o s - A /d - o 1 / r / j r - J - AA I- O -A/U) ~ O Z. Collection Collection Date Time O&30 q-2f-c& n.R/<r 0) 'o ^ '<> oa _ua>g.<Ed UXmJ E uo 3 cO Z U Specify Matrix A/udaC* udA r Comments VA AJ 0 VN .K ____ : LAB USE ONLY CHAIN O F C U S T O D Y R elin q u ish e d by D a te T im e 0 9 /S ' R ece ived b y i D a te It/3 T im e /* / OTHER INFORMATION 0 * A CL i. LAB USE ONLY c-o yio iA d e w %. - c i ....... i l i: : . 9-Zi-O * 9-25^ 0 5 z% z . 00010 Q ooo __ -- PROJECT REQUIREMENTS Results Deadline: Laboratory Report Options: Q Sample results only Q Add case narrative Add quality control summary ED Add calibration summary CD Add raw data O ther__________________ uCL c: " I 3-0] LC 1 Frofii Thisortionran be renxn^ forRecipient's records. sDat fm FedExTracking Number fiM 0 B 3 b 7 7 fl3 FedExPriorityOvernightj Ne business morning / f l FedExStandard Overnight 1-- 1 N w busmess afternoon t. E -f O 2 2 "-iosr: C5 ` -O v.i ' :.0 ' A IK jM A M E R IC A ft\i( H Si.,-. Address 9 0 5 S T A T E DOCKS RD & -- ;----------------------- - Ku cptCy D E C A T/ p U2 YourInternal Billing Reference MlA l , d i " A~ , y 3 To s r t it M i , K , ; m . Im I A m Company Address ,,^)j * ,/ j ' h A W, To'NOLOD'"aatFt eFeddEExxllooccaattiioonn,,pprriinfcFFedExaddresk-- 1 * Address ( V> I City ; -, u . . i. '.t- -, i ; fl4 D B 3 f l b l Bione ' 3 Q o ~ - d Q 0 0 ^ j Q~Fgd20ay ' r p ] FedBcExpressSaver / ' -, ` i - Secondbusmessday -- Third business day y* , 5 tj -- ; Fcii&Envelone Jale not ava'^able.Mmgnurn charge: One-pound rate 1 , < : 4b ExpressFreight Service I ;n fed&d1DayFreight* [--i FedEx2DayFreight , '-- i Next business day , ^ 1-- I Second busmess day. Stata / .i JU AL, y S Oept/Rcw/Surta/Room I * Callfor Confirmation: ) 5 Packaging A y 1 -j g g M L r yj Fed Envelope* FedExPak* includes FedEx Sinafl Pk, FedEx" ______ large Pak,andFedE>tSturdyPak - i m - i u 6 SpecialHandling : InudfrfedExaddre'. r t SATURDAY Devety LU AvsiableonfyforFedcFrterity OvemightandFedEx2Day toselectZIPcodes HOLDW eeikkdd rrijyy \ |_( NaottaFvaeidiaEblxofcrJ,iCcif.tfiJoh ' . FedExFntqfnght Doesthisshpmentcontamdangerousgoods? I Oneboxmustbechecked. -----A---___ . iO LD fdtFeds' 'Ayadabtt. '* FedExPrior * aftJftdEx" select locai I No r [--j Yes ! n Tes . : , j per attached 1 Lu -_Ji Samhippppeerr'ss..DDeeclaration Sh-p*rpors D----c--la-r-a--o-d--n---S----,-----n.wo.t.re.q,vu'iurr^^dj I I 0:ytee I-- I Dry Ice,9,11^1845_____ Dangerous Goods including P ry/cekannofo sNpptfin F e d a packaging. I I CargoA' We cannotdeliver. P.0, boxes or P.O.ZJPcodes, , 7 Payment Billto; ~ I . ~EnterFe-^ AcciNo.orCreditCardNo.below.--- --- fS fesecta LJ^cipient Q Third Party Crediti, I will bg M e d DepURoor/Suite/Room j State ZIP' ) l/A > ) 7 7 fi3 TotalPackages I: To'talWeight ja .^tTnrAebilSyistinyterfloSIOOufttsssyoudeclareaNahervalve.SeetheME*SmicoSuiteto .8 Release Signatura [0 i/erwr,whomattainssywura. . 1_ j.,.. ' IS.": , 1 ^0 ^4 3 3 5 6 7 2 8 L _ ________ i M U, andagtefltoindBmnifyandUjhcFJIddUeslvhearrtmhilsessshifprommenatnwyirtehsouulttionbgtcalianiimngs.asignature'-mmv.mEY- ^F*RevDaufl.PartilSieiOS.oi^joojfedx.pBiNTajiNuA ----- "> ------, -- _* r~ a if) H O O O BEST COPY AVAILABLt i . .. -.Sii 1.. --, 1: . t : l i :: t. c i:: c_: 1 : , i,. n n f; f*r n rL < - n f. I > ! - 1 Exveen %/ research 3 0 5 8 R e s e a rc h O riv e S ta te C o lle g e , P A 16801 P h o n e : 8 0 0 -2 8 1 -3 2 1 9 F a x: 8 1 4 -2 7 2 -1 0 1 9 L a b o ra to ry S a m p le L o g -in S h e e t (E n v iro n m e n ta l) Complete upon sample receipt: Client and/or Project Name Method of Delivery O Walk-in Tracking#: Pick-up UPS S 'iC ' 1 .'{<?&/ ~7 ,,B'FedEx . Air Borne Other (explain) Chain of Custody Temperature Preservation Custojjy-Seals: ___ Bfiresent, & -Eflntact / broken (explain) absent Thermometer ID: Cooler ID: Cooler ID: Cooler ID: Cooler ID: a .i `f }e Cooler temD: Cooler temD: Cooler temD: Cooler temD: -S'- ~7 C C C C ChairpeftJustody Record: Bpresent absent Samples Received: B-effige Q tn lc e melt with ice pack none Explanation Completed by Slanature: __ Date (Time): 9 / * * - Q /* *& J / 'H Complete during sample log-in: LIMS Log-in # . -S r/tr Physical Condition Samples intact? ^P-Yes No (explain) Chain of Custody Samples received agree with COC record? CJ-Yes No (explain) Analysis Request Analysis request clear? EKfes No (explain) Preservation Sample containers appropriate? Yes No (explain) Chemical preservation appropriate? Yes No (explain) Samples received within holding time? Yes No (explain) Sample volume/mass adequate? Yes No (explain) Explanation Completed by Signature: --- " Date: Complete following resolution of any nonconformances: Client Contacted Yes Client: No Resolution 9 /j- Q /y / / j i ? Date (Time!: Completed by Signature: Lab Sx Log-in Sheet -Ex Date: O01S3 LOGIN CHAIN OF CUSTODY REPORT (InOl) Sep 29 2003, 11:50 am Login Number: L35195 Account: 3027 DAIKIN AMERICA, INC. Laboratory' ::!: :!: Client 'Collect:; "Receive . Due' Sa'ftip.I:.Numb%; i : Sample ..Number'!.: ; Date'- , :Dat PR Date L35195-1 DAI -092503-NW-01 25-SEP-03 29-SEP-03 ANALYZE BOTH SAMPLES FOR PFOA ANALYSIS. BOTH SAMPLES ARE STORED IN D000053 9. SLUDGE S PERC SOLID H o l d :06-OCT-03 D0000539 L35195-2: D A I - 0 9 2 5 0 3 - N W - 02 25-SEP-03 2 9 -SEP-03 Page 1 Signature : Date : 000154 Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L35195 PFOA 413->369 NA RAW DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Volume: Final Volume: 50 ng/L 15 pL Water 40.0 mL 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 100203A Karen Risha LC/MS/MS Unit # 7 10/02/03 10/02/03 Exygen ED XC092303-0 XC092303-1 XC092303-2 XC092303-3 XC092303-4 XC092303-5 XC092303-6 Methanol Wash 0106020 Control 0106020 Spfc A 0106020 SphB L35195-2 SpkC L 3 5 195-2 L35195-2Rep XC092303-1 XC092303-2 XC092303-3 XC092303-4 XC092303-5 XC092303-6 Sponsor ID - - - NA NA NA DAI-092503-NW-02 DAI-092503-NW-02 DAI-092503-NW-02 - - Sample Code c CS CS CS CS CS CS c c LCS LCS LF S S CS CS CS CS CS CS Run No. 100203A-1001 100203A-1002 100203A-1003 100203A-1004 100203A-1005 100203A-1006 100203A-1007 100203A -1008 100203A-1009 100203A-1010 100203A -1011 100203A-1012 100203A-1013 100203A-1014 100203A-1015 100203A-1016 100203A-1017 100203A-1018 100203A-1019 100203A -1020 Std. Cone. (ng/L) 0 25 50 100 250 500 1000 - - - - - - - 25 50 100 250 500 1000 PFOA Found (ng/L) = (peak area - intercept) / slope x DF Recovery (%) = [PFOA found (ng/L)-PFOA found in control (ng/L)]_____ x 100 amount PFOA added (ng/L) . ,, Dilution Factor - - 1 1 1 1 1 1 - - Peak Area 1450 4745 8495 16858 40221 85297 169611 0 0 8554 84522 29737922 28953448 28219348 33379 12881 18501 41713 86403 167355 PFOA Found (ng/L) - - Amount PFOA Added (ng/L) - - Recovery (%) - --- --- --- --- --- --- ND - - 43.7 50 87 499 500 100 A 500 - * -- * -- --- *-- --- --- -- - --- Standard Curve : Linear (1/x weighted) Intercept = 1259.89 Slope = 166.855 Coef. Of Det. = 0.999212 CS = Calibration standard C = Control sample S = Sample LF = Lab fortified sample FF s= Field fortified sample LCS Laboratory Control Spike ASample requires a higher spiking level. See data set 100903A. Sample requires dilution. See data set 100903A. CK = Check Standard ND sc Not detected = Response between 0 and LOD NQ = Not quantifiable = Response between LOD and LOQ Spreadsheet prepared by: 000155 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 r"'; Internal Chain of Custody/Fortification Sheet fi Exygen Study Number: L35195 Matrix: Water Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No. q 2- Time (M-fO Date 10 02- 03 i tInitials, CLIENT SAMPLE ID EXYGEN ID NUMBER VOLUME (mL) FORTIFICATION (ng) na 0106020 Control 40.0 na 0106020 Spk A 40.0 na 0106020 Spk B 40.0 r DAI-092503-NW-02 L35195-2 Spk C 40.0 DAI-092503-NW-02 L35195-2 40.0 - 2.0 20.0 20.0 - DAI-092503-NW-02 L35195-2 Rep 40.0 - _ - -- - t - - -- -- tt - - -- -- *i _ - - -- -- -- /H I _ _ - - -- - _ - -- -- - - -- - - -- 0106020 Spk A 0106020 Spk B L35195-2 SpkC _ Spiking Solution Used F092203-5 (10 ng/mL) F092203-4 (100 ng/mL) F092203-4 (100 ng/mL) _ Volume Used for Spiking 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) - Riitial/Date xC- / idoe-e* /iofoz/ ^ /lojciiS D -' _ _ II - _ , - ---- All samples were measured: ., Time l\5 I Date l0\Q2-]E0 Initials After measuring samples were returned to refrigerator No. , r " > Time \ 5 D 0 Date [0 __ Initials. Comments: 200 |JL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/D ate:. Analysis Summary: Data Set: 1 0 0 2 0 ^ Data Set: \ C C f \ t > k Data Set: --_____ i Set extraction/analysis data verified by: Is Initials/Date:. Initials/Date:. Initials/Date:. /to / (Q\cR j 5 Date: JP /f/t July 26, 2001/6 000156 '3 n 3 :n 3 I 3058 Research Drive C H State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L35195 MATRIX: Water METHOD: $$ ANALYTES: PFOA PROTOCOL NUMBER: NA Client ID na na na DAI-092503-NW-02 DAI-092503-NW-02 DAI-092503-NW-02 Exygen ID 0106020 Control 0106020 Spk A 0106020 Spk B L35195-2 Spk C L35195-2 L35195-2 Rep . _ _ ._ _ . . _ . . . _ _ STEP 1 \r ~ _ _ _ . _ _ _ _ . .. . _ |- STEP 2 V _ - _ _ - - _ A Dilutions (mL/mL) _ - - STEP 3 Dilutions (mL/mL) STEP 4 -- - \ ^V lj /iD -- A L _ --- --- --- --- --- -- - --- --- --- --- --- --- --- --- --- --- . loo , - 1- Reagents/ Materials Methanol C18SPE TypeI Water Lot# 4 2 ,1 3 ^ -^ 2 0 \*}2>U2->1 NA Initials/Date . & ib\2> c3 -- -- -- - HPLc - Methanol 43lfcft32fc> Ammonium Acetate Type I water - NA tj^\o\02_[o3 *Initials/D ate - 1*2 h - IDcBj e 0 3 \ m c2> In itia ls/D a te 000157 STEP 2: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP 3: LC/MS/MS analysis STEP 4: LC/MS/MS reanalysis. Initials and date under each step indicates the personnel that performed this step. $$ Method of Analysis for the Determination of Perfluorooctane sulfonate (PFOS), Perfluorooctane sulfonylamide (PFOSA), and Perfluorooctanoate (POAA) m Water COMMENTS: Final extracts stored in refrigerator Initials: Date: __10|h?-)o3_ July 19,2001/4 *J S' ' S- : > '| "f T ' 1 -T ' ' "" "j 'j Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochems.PRO\SampleDB\100203A Daikin.spl Printed: Thu Oct 02 15:00:15 2003 Vial File Name LIMS ID Client ID Sample Description 1 1 100203A-1001 -- 2 2 100203A-1002 -- 3 3 100203A-1003 -- 4 4 100203A-1004 -- 5 5 100203A-1005 -- 6 6 100203A-1006 -- 7 7 100203A-1007 -- 8 92 100203A-1008 -- 9 11 100203A-1009 -- 10 12 100203A-1010 -- 11 13 100203A-1011 -- 12 14 100203A-1012 -- 13 15 100203A-1013 -- 14 16 100203A-1014 -- 15 2 100203A-1015 -- 16 3 100203A-1016 -- 17 4 100203A-1017 -- 18 5 100203A-1018 -- 19 6 100203A-1019 -- 20 7 100203A-1020 -- XC092303-0, 0 ng/L standard XC092303-1, 25 ng/L standard XC092303-2, 50 ng/L standard XC092303-3,100 ng/L standard XC092303-4,250 ng/L standard XC092303-5, 500 ng/L standard XC092303-6,1000 ng/L standard Methanol Wash 0106020 Control 0106020 Spk A, 50 ng/L 0106020 Spk B, 500 ng/L L35195-2 Spk C, 500 ng/L L35195-2 L35195-2 Rep XC092303-1, 25 ng/L standard XC092303-2, 50 ng/L standard XC092303-3,100 ng/L standard XC092303-4, 250 ng/L standard XC092303-5, 500 ng/L standard XC092303-6,1000 ng/L standard 000158 Exygen STUDY N O . L 3 5 S . Page 1 Page Position: ( 1, 1) Matrix Sample Type Cone (ng/L) Cone B Cone C Test ID DF MS Method ___ Blank 0 -- Standard 25 -- Standard 50 -- Standard 100 -- Standard 250 -- Standard 500 -- Standard 1000 -- Blank -- -- Blank -- -- QC 50 QC 500 QC 500 -- Analyte -- -- Analyte -- -- Standard 25 -- Standard 50 -- Standard 100 -- Standard 250 -- Standard 500 -- Standard 1000 0___ ___ 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- ----0 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA i -;: t :::i i z i :" : i :i Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochems.PRO\SampleDB\100203A Daikin.spl Printed: ThuOct 02 15:00:15 2003 \ 0 u l L o HPLC Method MS Tune File Inj Volume (pL) 1 water PFOATune 15 2 water PFOATune 15 3 water PFOA Tune 15 4 water PFOATune 15 5 water PFOATune 15 6 water PFOATune 15 7 water PFOA Tune 15 8 water PFOA Tune 15 9 water PFOATune 15 10 water PFOATune 15 11 water PFOATune 15 12 water PFOATune 15 13 water PFOATune 15 14 water PFOA Tune 15 15 water PFOATune 15 16 water PFOATune 15 17 water PFOATune 15 18 water PFOATune 15 19 water PFOATune 15 20 water PFOATune 15 6S T000 i :i n Exygen STUDY N O . ,, L 3 5 i% . Page 2 Page Position: (2,1 ) n LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: N A Exygen Study No: L35195 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #7) n Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT : Version 4 Build 1381 : Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 f""! HP Quat Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Genesis C-8, 5 cm x 2.1 mm i.d. x 4 p (Exygen ID:MA10327) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) : 2 mM Ammonium Acetate in Type I Water r ; Mobile Phase (B) : Methanol 05 r Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 *\ * ! NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the I instrument settings used for the analysis of this data set. A ll Handwritten Peak ID's by: P : m fe' i L- f? L! fc- ( t' 1 000160 Scanning Method Report Method: C :\MASSLYNX\FLUOROCHEMS.PRO\ACQUDB\008 PFOA Last Modified: Thu Oct 02 14:56:38 2003 Printed: Thu Oct 02 15:04:11 2003 Solvent Delay ( mins ) : 0.00 Function : 1 M R M of 1 Mass Pair ( ESP- ) Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Time { Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 8.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 413.00 369.00 0.20 10 10 Page 1 000181 Method Report Method File: Last Modified Printed C :\MASSLYNX\FLORt)CHEMS.PRO\ACQUDB\water Thursday, October 02, 2003 14:57:31 Thursday, October 02, 2003 15:05:03 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 60.0 40.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 15.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 10 entries which are : Time 0.00 0.40 1.00 7.00 7.50 9.00 9.50 13.50 14.00 15.00 A% 60.0 60.0 10.0 10.0 0.0 0.0 60.0 60.0 60.0 60.0 B% 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 40.0 C% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 0.300 HP1100 LC Pump External Event Timetable The Timetable contains 4 entries which are : Time Initial 0.00 0.10 8.00 Column Switch Off Off Off Off Contactl Off On Off Off Contact2 Off Off On Off Contact3 Off Off Off Off Contact4 Off Off Off Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (/il/min) Draw Position (mm) Stop Time (mins) Injection Volume ( i l ) Vial Number 200.0 200 0.10 15.00 15.0 16 Page 1 Pressure 400 400 400 400 400 400 400 400 400 400 000162 Tuning Method Report Method: C :\MASSLYNX\FLUOROCHEMS .PRO\ACQUDB\PFOA TUNE Printed: Thu Oct 02 15:04:16 2003 mp? Page 1 Dau 413.00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 10 0.0 0.0 0.0 100 300 -2.93 -10 98 300 Pressures Analyser Vacuum Gas Cell Rdbk OFF 3.9e--3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set RdJ 14.0 14.0 1.0 -2 10 2 14.0 14.0 2.0 700 8 9 11 -6 Rdbk 128.5 711.7 000163 Quantify Calibration Report Study No.:L35195, Set No.:100203A, Ext.Date:10/02/03, Analyst:K.Risha Page 1 Exygen Research, 3058 Research Drive, State College, PA 16801 000164 f ; Quantify Sample Report Study No.:L35195, Set N o . :100203A, Ext.Date:10/02/03, Analyst:K.Risha Page 1 H Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203A Daikin f Last modified: Fri Oct 03 12:51:11 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 fl Job Code: Initials : Printed: Fri Oct 03 12:56:03 2003 D a t e u B H _ ______________________ iQhSPQ h 'l(O I To 10b->t&h'IMP f Name: 100203A-101 Text: n 1 : PFOA i rmm>i m n b- * Exygen Research, 3058 Research Drive, State College, PA 16801 000165 Quantify Sample Report Study No.:L35195, Set No.:100203A, Ext.Date:10/02/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203A Daikin Last modified: Fri Oct 03 12:51:11 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 12:56:03 2003 Page 2 Name: 100203A-1002 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000166 f' **-1 Quantify Sample Report ' Study No.:L35195, Set No.:100203A, Ext.Date:10/02/03, Analyst:K.Risha f S a m p l e List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203A Daikin ; Last modified: Fri Oct 03 12:51:11 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 P Job Code: Printed: Fri Oct 03 12:56:03 2003 Name: 100203A-1003 Text: P ? .5 V- ; n I! n FF r*i it t t Exygen Research, 3058 Research Drive, State College, PA 16801 000167 1 j Quantify Sample Report t Study No.:L35195, Set No.:100203A, Ext.Date:10/02/03, Analyst:K.Risha f-' Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SaxnpleDB\100203ADaikin l ' Last modified: Fri Oct 03 12:51:11 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 P Job Code: j- - Printed: Fri Oct 03 12:56:03 2003 Page 4 Name: 100203A-1004 Text: 1 : PF0A XCOi2303-3,100 ng/L standard 1002(33A -1 0 0 4 Sm (M n , 2x2) 100 %: 02-0ct-2003 17:13:35 LC/MS/MS #7 5 .1 9 M RM of 1 Channel ES413 > 3 6 9 1 .72e5 A rea ' j; : t: t K u - H -ri .. . . r 1 -t --1 ' 1 1 1 1 1 I f 1 ' > > J < 1 > 1 1 < , 1 I j < < < > 1 .0 0 2 .0 0 3 .00 1 1 1 11 " '1 I 11 1 1 I 1111 4 .0 0 5 .0 0 ' ' 1 1.1 1 I 1 1 1 1 i 1 1 1 i 1111 1 1 1 6 .0 0 7 .0 0 1 1 1 1im e 8 .00 fr ' l; i p6i i; Exygen Research, 3058 Research Drive, State College, PA 16801 000168 fi *' Quantify Sample Report Study No.:L35195, Set No.:100203A, Ext.Date:10/02/03, Analyst:K.Risha Page 5 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203A Daikin Last modified: Fri Oct 03 12:51:11 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 12:56:03 2003 n i: t* Name: 100203A-1005 Text: r " ! 1 : PFOA___________________________________________________________________________________ XC092303-4, 250 ng/L standard 02-0ct-2003 17:30:22 LC/MS/MS #7 Ik 10 0 2 0 3 A -1 005 S m (M n , 2 x 2 ) MRM of 1 Channel ES " 413 >369 4 .1 9e5 l Area t1 1 .0 0 2 .0 0 ________ 3XX)________ 4 .0 0 5 .0 0 i 1 1 1 1 I 1 1 I I I 1 I t"t I 1 1 6 .0 0 7 .0 0 11 1 1 I Tim e 8 .0 0 r FT FT i? 1 n fi f - m, {: rTM r] Exygen Research, 3058 Research Drive, State College, PA 16801 000169 i Quantify Sample Report Study No.:Ii35195, Set No.:100203A, Ext.Date:10/02/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100203A Daikin Last modified: Fri Oct 03 12:51:11 2003 Method: P :\Data\LCMSMS7 \Masslynx\Fluorochems. PRO\MethDB \PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 12:56:03 2003 Rage 6 Name: 100203A-1006 Text: i 'r h- -i r"! Exygen Research/ 3058 Research Drive, State College, PA 16801 000170 Quantify Sample Report Study No..-L35195, Set No.:100203A, Ext.Date:10/02/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203A Daikin Last modified: Fri Oct 03 12:51:11 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 &S*>1 Job Code: Printed: Fri Oct 03 12:56:03 2003 Page 7 Name: 100203A-1007 Text : 1 : PFOA XC092303-6,1000 ng/L standard 1 00203A -1007 Sm (M n, 2x2) 100n #s* is i 5.23 169611 02-0ct-2003 18:03:53 LC/MS/MS #7 M RM of 1 Channel ES413 >369 1 .74e6 A rea -rr-T -r-r T-- I I " ' i ' J --: 1 j-- I-- i-- n --]-- t t " 1.00 2.00 'I 3 .00 4 .00 5 .0 0 TTTTTTT 6.00 7 .0 0 i T im e 8.00 - :! M I1 mm, l Exygen Research, 3058 Research Drive, State College, PA 16801 00017| Quantify Sample Report Study No.:L35195, Set No.:100203A, Ext.Date:10/02/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100203A Daikin Fri Oct 03 12:51:11 2003 P :\Data\LCMSMS7 \Masslynx\Fluorochems. PRO \MethDB \PFOA 100203 Fri Oct 03 12:53:47 2003 Printed: Fri Oct 03 12:56:03 2003 Page 8 Name: 100203A-1008 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000172 Quantify Sample Report Study No.:Ii35195, Set No.:100203a , Ext.Date:10/02/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203A Daikin Last modified: Fri Oct 03 12:51:11 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 12:56:03 2003 Name: 100203A-1009 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000173 : * Quantify Sample Report { Study No.:L35195, Set No.:100203A, Ext.Date:10/02/03, Analyst:K.Risha Rage 10 I*! Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100203A Daikin t Last modified: Fri Oct 03 12:51:11 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 J o b Code: Printed: Fri Oct 03 12:56:03 2003 Name: 100203A-1010 Text: H 1 : PFOA \: *J ^ Exygen Research, 3058 Research Drive, State College, PA 16801 000174 rn r .. I ; Quantify Sample Report - - ' Study No.:L35195, Set No.:100203A, Ext.Date:10/02/03, AnalystrK.Risha Page 11 f* Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100203A Daikin : Last modified: Fri Oct 03 12:51:11 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 H Job Code: ll J Printed: Fri Oct 03 12:56:03 2003 Name: 100203A-1011 Text: n t M. Exygen Research, 3058 Research Drive, State College, PA 16801 ; 000175 FF t' i Quantify Sample Report ' Study No.:L35195, Set No.:100203A, Ext.Date:10/02/03, Analyst:K.Risha Page 12 f t Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203A Daikin i i Last modified: Fri Oct 03 12:51:11 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PEO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 jp Job Code: h- - -- Printed: Fri Oct 03 12:56:03 2003 Name: 100203A-1012 Text: I- . ** P' i- ? * ll i Exygen Research, 3058 Research Drive, State College, PA 16801 000176 Quantify Sample Report Study No.:L35195, Set No.:100203A, Ext.Date:10/02/03, Analyst:K.Risha Page 13 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100203A Daikin Fri Oct 03 12:51:11 2003 P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Fri Oct 03 12:53:47 2003 Printed: Fri Oct 03 12:56:03 2003 Name: 100203A-1013 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000177 Quantify Sample Report Study No.s 1.35195/ Set No.:100203A# Ext.Date:10/02/03, Analyst:K.Risha Rage 14 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100203A Daikin Last modified: Fri Oct 03 12:51:11 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 job Code: Printed: Fri Oct 03 12:56:03 2003 Name: 100203A-1014 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000178 Quantify Sample Report Study No.:L35195, Set No.:100203A, Ext.Date:10/02/03, Analyst:K.Risha Page 15 " Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203A Daikin t- Last modified: Fri Oct 03 12:51:11 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 P : job Code: Printed: Fri Oct 03 12:56:03 2003 t1 t Marne: 100203A-1015 Text: I n jfm \ I ? Exygen Research, 3058 Research Drive, State College, PA 16801 000179 Quantify Sample Report Study No.:L35195, Set No.:100203A, Ext.Date:10/02/03, Analyst:K.Risha Page 16 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100203A Daikin Last modified: Fri Oct 03 12:51:11 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 12:56:03 2003 Marne: 100203A-1016 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000180 Quantify Sample Report Study No.:L35195, Set No.:100203A, Ext.Date:10/02/03, Analyst:K.Risha Page 17 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203A Daikin Last modified: Fri Oct 03 12:51:11 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 n Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 12:56:03 2003 t\ t- . Name: 100203A-1017 Text: 1 : PFOA XC092303-3,100 ng/L standard 10 0203A -10 1 7 Sm (M n, 2x2) 100- %" 02-0ct-2003 20:51:34 LC/MS/MS #7 5.24 M RM of 1 Channel ES413 > 3 6 9 1 .99e5 Area t 1 0 : ^ r ' i 'rT^~r'i 1 1 I" ' ' m 111 rT r"' 1"n.1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 r ri I I i i , T im e, - t I - I I r r r r i - r m 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 l: I! f \, A Exygen Research, 3058 Research Drive, State College, PA 16801 H 000181 Quantify Sample Report Study No.SL35195, Set No.s100203A, Ext.Date:10/02/03, Analyst:K.Risha Page 18 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203A Daikin Last modified: Fri Oct 03 12:51:11 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 12:56:03 2003 Name: 100203A-1018 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000182 Quantify Sample Report Study No.:L35195, Set Nd.:100203A, Ext.Date:10702/03, Analyst:K.Risha Page 19 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100203A Daikin Last modified: Fri Oct 03 12:51:11 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 12:56:03 2003 Name: 100203A-1019 Text: 1 : PFOA XC092303-5, 500 ng/L standard 100203A -1019 Sm (Mn, 2x2) 100-1 %~ 02-0ct-2003 21:25:20 LC/MS/MS #7 5.24 M RM of 1 Channel ES413 >369 8.92e5 Area Q r~i I--r II I I I J I I r i ] I I 11I j I 'I I I j rT'r r~j-ri 1.00 2 .0 0 3.00 T -r 4.00 5.00 6.00 I"i i I I n I I"H ' I Tim e 7 .0 0 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000183 Quantify Saiqple Report Study No.:L35195, Set No.:100203A, Ext.Date:10/02/03, Analyst:K.Risha Page 20 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100203A Daikin Last modified: Fri Oct 03 12:51:11 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 12:56:03 2003 Name: 100203A-1020 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000184 Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L35195 PFOA 413 -> 369 NA RAW DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Volume: Final Volume: 50 ng/L 15 pL Water 40.0 mL 5.0 mL Set No.Analyst: Instrument Type: Extraction Date: Analyzed on: 100903A Karen Risha LC/MS/MS Unit # 7 10/09/03 10/09/03 Exygen ID XC100703-0 XC100703-1 XC100703-2 XC100703-3 XC100703-4 XC100703-5 XC100703-6 Methanol Wash 0106020 Control 0106020 Spk A 0106020 Spk B L35195-2 Spk C L35195-2 L35195-2 Rep XC100703-1 XC100703-2 XC100703-3 XC100703-4 XC100703-5 XC100703-6 Sponsor ID NA NA NA DAI-092503-NW-02 DAI-092503-NW-02 DAI-092503-NW-02 - - Sample Code c CS CS CS CS CS CS c c LCS LCS LF S s CS CS CS CS CS CS Run No. 100903A-2001 100903A-2002 100903A-2003 100903A-2004 100903A-2005 100903A-2006 100903A-2007 100903A-2008 100903A-2009 100903A-2010 100903A-2011 100903A-2012 100903A-2013 100903A-2014 100903A-2015 100903A-2016 100903A-2017 100903A-2018 100903A-2019 100903A-2020 PFOA Found (ng/L) = (peak area - intercept) / slope x DF Recovery {% ) = fPFOA found (ng/L)-PFOA found in control (ng/L)] amount PFOA added (ng/L) Std. Cone. (ng/L) 0 25 50 100 250 500 1000 25 50 100 250 500 1000 Dilution Factor - - - - 1 1 1 10000 10000 10000 - - x 100 Peak Area 1319 5416 9442 17769 41378 89375 173528 0 0 12156 93093 27318 18384 18123 5414 9766 18655 42172 89046 169898 PFOA Found (ng/L) - - ND 64.9 538 1530000 1010000 997000 - Amount PFOA Added (ng/L) _ . . . . - 50 500 500000 - Recovery (%) . . - . - . 130 108 104 - --- Standard Curve : Linear (1/x weighted) Intercept = 1045.97 Slope = 171.248 Coef. Of Det. = 0.999288 CS = Calibration standard C = Control sample S = Sample * LF = Lab fortified sample FF = Field fortified sample LCS = Laboratory Control Spike CK = Check Standard ND = Not detected = Response between 0 and LOD NQ - Not quantifiable = Response between LOD and LOQ Spreadsheet prepared by:. 000185 F*1 f! tA VT RESEARCH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet |f t Exygen Study Number: L35195 Matrix: Water Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No. _____ m r* Time _____ Date 10 1Cf\ 10 3 Initials, CLIENT SAMPLE ID EXYGEN ID NUMBER VOLUME (mL) FORTIFICATION (ng) na 0106020 Control 40.0 _ na 0106020 Spk A 40.0 2.0 na 0106020 SpkB 40.0 20.0 D A I-092503-N W -02 L35195-2 Spk C 40.0 20000.0 n - - -_ - -- - - __ - - -- - -- r", i ! r - - -- -_ - -_ - - -- `- - - - - - -- - -- - - -_ - - -_ - t - - -- -- Fl Spiking Solution Used Volume Used for Spiking Ipitial/Date k ! 0106020 Spk A F092203-5 (10 ng/mL) 200 pL (200 pL micropipet) 0106020 SpkB F092203-4 (100 ng/mL) 200 pL (200 pL micropipet) /M e 2 F; L35195-2SpkC F092203-1 (100000 ng/mL) 200 pL (200 pL micropipet) /|o i- : -- _ -- __ r-' - - __ -- -- All samples were measured: .. * Time CR\f~)______ Date l O y ^ l ^ Initials After measuring samples were returned to refrigerator No. Time_ \\0 ? Date Initials i Comments: 200 pL Of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date::: ^ L H > M o3 Analysis Summary: Data S et:. IlH f j t f f A Data Set: ^ _______ Data Set: _______ Initials/Date: TInniittiifalllcs//TDiaaft-efv: Initials/Date: rjv / "* v/ / Set extraction/analysis data verified by: P i. Date: July 26, 2001/1 '1 1 'Z 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L35195 MATRIX: Water METHOD: ANALYTES: PFOA PROTOCOL NUMBER: NA Client ID na na na DAI-092503-NW-02 - Exygen ID 0106020 Control 0106020 Spk A 0106020 SpkB L35195-2 SpkC - STEP 1 I - STEP 2 s! - - - -- - - -- - - -- - - -- - - -- _ - -- - - -- - - -- _ - -- - - -- - - -- - - -- _ - -- - - -- - - -- - - -- _ - -- - *Initials/Date - JE - lo p lc s . STEP 1: SPE column clean-up STEP 2: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP 3: LC/MS/MS analysis STEP 4: LC/MS/MS reanalysis. Dilutions (mL/mL) -- - o b l STEP 3 \! . - ib lS fe Dilutions (mL/mL) - - STEP 4 - - - - Reagents/ Materials Methanol C18 SPE TypeI Water Lot# 43I& 32-O U oziM SE NA -- -- -- -- - Initials/Dale - - J'1 m o c f{o s 0 -- -- -- -- -- -- -- HPLC Methanol Ammonium Acetate Type Xwater - NA Initials/Date *Initials and date under each step indicates the personnel that performed this step. $$ Method of Analysis for the Determination of Perfluorooctane sulfonate (PFOS), Perfluorooctane sulfonylamide (PFOSA), and Perfluorooctanoate (POAA) in Water COMMENTS: Final extracts stored in refrigerator. Initials: Date: iDjCftlcB July 19, 2001/4 000187 i n Tl ri -n i rr r in Masslynx - Sam ple List Sample List: C:\MASSLYNX\Fluoroche:irnis.PRO\\SSaammpplleDB\100903A Daikin.spl Printed: Thu Oct 09 13:17:06 2003 Vial File Name LIMS ID Client ID Sample Description 1 1 100903A-2001 -- 2 2 100903A-2002 -- 3 3 100903A-2003 -- 4 4 100903A-2004 -- 5 5 100903A-2005 -- 6 6 100903A-2006 -- 7 7 100903A-2007 -- 8 92 100903A-2008 -- 9 11 100903A-2009 -- 10 12 100903A-2010 -- 11 13 100903A-2011 -- 12 14 100903A-2012 -- 13 15 100903A-2013 -- 14 16 100903A-2014 -- 15 2 100903A-2015 -- 16 3 100903A-2016 -- 17 4 100903A-2017 -- 18 5 100903A-2018 -- 19 6 100903A-2019 -- 20 7 100903A-2020 -- XC100703-0, 0 ng/L standard XC100703-1, 25 ng/L standard XC100703-2, 50 ng/L standard XC100703-3,100 ng/L standard XC100703-4,250 ng/L standard XC100703-5, 500 ng/L standard XC100703-6,1000 ng/L standard Methanol Wash 0106020 Control 0106020 Spk A, 50 ng/L 0106020 Spk B, 500 ng/L L35195-2 Spk C, 500000 ng/L, DF; L35195-2, DF=10000 L35195-2 Rep, DF=10000 XC100703-1, 25 ng/L standard XC100703-2, 50 ng/L standard XC100703-3,100 ng/L standard XC100703-4, 250 ng/L standard XC100703-5,500 ng/L standard XC100703-6,1000 ng/L standard 000188 ExygenstudyNO. J r 0^13 Page 1 Page Position: (1,1) Matrix Sample Type Cone (ng/L) Cone B Cone C Test ID DF _____ Blank 0 __ __ 0 -- Standard 25 0-- -- -- Standard 50 0-- -- -- Standard 100 0-- -- -- Standard 250 0-- -- -- Standard 500 0-- -- ------ Standard 1000 0-- -- -- Blank -- 0-- -- Blank -- 0-- -- -- QC 50 0-- -- -- QC 500 0-- -- -- QC 500000 -- -- 0 -- Analyte -- 0-- -- -- Analyte -- 0-- -- -- Standard 25 0-- -- -- Standard 50 --0 -- Standard 100 0-- -- -- Standard 250 0------- _____ -- Standard 500 --0 -- Standard 1000 0-- -- 1 1 1 1 1 1 1 1 1 1 1 10000 10000 10000 1 1 1 1 1 1 11 Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochen is.PRO\SampleDB\100903A Daikin.spl Printed: Thu Oct 09 13:17:06 2003 ______ _______________ ; MS Method HPLC Method MS Tune File Inj Volume (yL) 1 008 PFOA 2 008 PFOA 3 008 PFOA 4 008 PFOA 5 008 PFOA 6 008 PFOA 7 008 PFOA 8 008 PFOA 9 008 PFOA 10 008 PFOA 11 008 PFOA 12 008 PFOA 13 008 PFOA 14 008 PFOA 15 008 PFOA 16 008 PFOA 17 008 PFOA 18 008 PFOA 19 008 PFOA 20 008 PFOA water water water water water water water water water water water water water water water water water water water water PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 000189 issGT Exygen STUDY N O . Page 2 Page Position: (2,1 ) n ? LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: N A Exygen Study No: L35195 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #7) n t1 Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 P HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Quat Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Genesis C -8 ,5 cm x 2.1 mm i.d. x 4 p (Exygen ID:MA10327) (JONESCHROMATOGRAPHY: Part No. FK5962E) n .5 Mobile Phase (A) : 2 mM Ammonium Acetate in Type I Water Mobile Phase (B) : Methanol .03 f. Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. A ll Handwritten Peak ID 's by: \0 03 u< 1. : r? 000190 n Scanning Method Report Method: C:\MASSLYNX\FLUOROCHEMS.PRO\ACQUDB\OO8 PFOA Last Modified: Thu Oct 02 14:56:38 2003 Printed: Thu Oct 09 13:16:18 2003 F Solvent Delay ( mins ) : 0.00 ^ J p fo /03 Function : 1 M R M of 1 Mass Pair ( ESP- ) Inter Channel Delay Span ( Daltons ) : Start Time ( Mins ) End Time ( Mins ) : Repeats : Channel Parent Secs ) Daughter 0.03 0.00 0.00 8.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 413.00 369.00 0.20 10 10 F* Page 1 m 1: ***1 l.J f'*! Yi 000191 Method Report Page 1 Method File: Last Modified: C:\MASSLYNX\FLUOROCHEMS.PRO\ACQUDB\water Thursday, October 09, 2003 13:14:21 Printed: Thursday, October 09, 2003 13:16:24 ^ I oM o3 HP1100 LC Pump Initial Conditions Solvents A% <T> B% C% D% 60.0 40.0 0.0 0.0 Flow (ml/min) t .1 Stop Time (mins) fc- -v Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 15.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable ft-.1 The gradient Timetable contains 10 entries which are ; Time 0.00 i ' 0.40 i ; 1.00 7.00 7.50 (I' 9.00 9.50 13.50 14.00 f t 15.00 A% 60.0 60.0 10.0 10.0 0.0 0.0 60.0 60.0 60.0 60.0 B% 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 40.0 - HP1100 LC Pump External Event Timetable C% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 D% Flow Pressure 0.0 0.300 400 0.0 0.300 400 0.0 0.300 400 0.0 0.300 400 0.0 0.300 400 0.0 0.400 400 0.0 0.400 400 0.0 0.400 400 0.0 0.300 400 0.0 0.300 400 The Timetable contains 4 entries which are : *j Time Initial M 0.00 l A 0.10 8.00 Column Switch Contactl Off Off Off On Off Off Off Off <Contact2 Off Off On Off Contact3 Off Off Off Off Contact4 Off Off Off Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (/xl/min) r i : Draw Position (mm) Stop Time (mins) Injection Volume (/xl) Vial Number 200.0 200 0.10 15.00 15.0 16 f- 000192 Tuning Method Report Method: C :\MASSLYNX\FLUOROCHEMS. PRO\ACQUDB\PFOA TUNE Printed: Thu Oct 09 13:16:30 2003 k Mo1o[1p3 Page 1 SOURCE ( ESP - ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 10 0.0 0.0 0.0 100 300 -2.93 -10 99 304 Pressures Analyser Vacuum Gas Cell Rdbk OFF 3 . l e - 3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation I* Set Rdbk 14.0 14.0 1.0 -2 10 2 14.0 14.0 2.0 700 8 9 11 -696 Rdbk 129.9 719.0 000193 Quantify Calibration Report Study No.:L35195, Set No.:100903A, Ext.Date:10/09/03, Analyst:K.Risha Calibration: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\CurveDB\100903A Daikin Page 1 Exygen Research, 3058 Research Drive, State College, PA 16801 000194 Quantify Sample Report Study No.:L35195, Set No.:100903A, Ext.Datesl0/09/03, Analyst:K.Risha Page 1 Sample List: Last modified: Method: Last modified: Job Code: Printed: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903A Daikin Fri Oct 10 07:25:26 2003 P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Fri Oct 03 12:53:47 2003 I Fri Oct 10 07:30:15 2003 Initials. D a te _ |q 3o o i q . Run#l \-2Q O \ To EE3; i Z J S P Name: 100903A-2001 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000195 Quantify Sample Report Study No.:L35195, Set No.:100903A, Ext.Date:10/09/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903A Daikin Last modified: Fri Oct 10 07:25:26 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 10 07:30:15 2003 Page 2 Name: 100903A-2002 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000196 Quantify Sample Report Study No.:L35195, Set No.:100903A, Ext.Date:10/09/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903A Daikin Last modified: Fri Oct 10 07:25:26 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 10 07:30:15 2003 Page 3 Name: 100903A-2003 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000197 f"*' n f t Quantify Sample Report : Study No.:L35195, Set No.:100903A, Ext.Date:10/09/03, Analyst:K.Risha C " Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903A Daikin Last modified: Fri Oct 10 07:25:26 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 ^ Last modified: Fri Oct 03 12:53:47 2003 ; Job Code: Printed: Fri Oct 10 07:30:15 2003 Page 4 Name: 100903A-2004 Text: 1 : PFOA XC100703-3,100 ng/L standard ` 10 0 9 0 3 A -2 0 0 4 Sm (M n , 2x2) 100-j i %: n o: L r r T .r .r ...r. 1.00 , ....................... 2 .0 0 3.00 5.18 1 7 7 6 9 "] 4 .0 0 { 5.00 09-0ct-2003 15:07:44 LC/MS/MS #7 M RM of 1 Channel ES413 > 3 6 9 1.71e5 Area 'n ' "T"'1" '-'-I ' .! ' ' i T im e 6.00 7.00 8.00 fi * ; I, ti ,' rr Exygen Research, 3058 Research Drive, State College, PA 16801 000198 n Quantify Sample Report Study No.:L35195, Set No.:100903A, Ext.Date:10/09/03, Analyst:K.Risha Page 5 fl Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903A Daikin I `i Last modified: Fri Oct 10 07:25:26 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 _ Last modified: Fri Oct 03 12:53:47 2003 i ; Job Code: t; - Printed: Fri Oct 10 07:30:15 2003 4S" ___________________________________________________________________________ _ __ Name: 100903A-2005 Text: n 1 : PFOA X C 1 0 0 7 0 3 -4 , 2 5 0 n g /L s ta n d a rd t : 100903A -2005 S m (Mn, 2x2) [ 100n i: % : 5-20 413781 1 0 9 -0 c t-2 0 0 3 15:24:31 L C /M S /M S # 7 MRM of 1 Channel ES- 413 >369 4 .0 1e5 Area fn- A ik Jh O 1 iS~"l '"!] 1 r ) 1 | 1 j i TT 1 . I 'T 1 j "T""i '1 T "] " 1 '!' 1 1 "1 '1 1 1 ' 1' { 1 ' 1' 1 1 | 1i 11i 1' *. H '1'"f i 1 1.00 2.00 3 .00 4 .00 5 .00 6.00 i:-'~rTT7 -- 'M -p -rrrH Tim e 7.00 8.00 fs ii r i1 *** Exygen Research, 3058 Research Drive, State College, PA 16801 f\ . i: ' 000199 Quantify Sample Report Study No.:L35195, Set No.:100903A, Ext.Date:10/09/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903A Daikin Last modified: Fri Oct 10 07:25:26 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 10 07:30:15 2003 Page 6 Marne: 100903A-2006 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000200 Quantify Sample Report Study No.:I<35195, Set No.:100903A, Ext.Date:10/09/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903A Daikin Last modified: Fri Oct 10 07:25:26 2003 Method: P :\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 10 07:30:15 2003 Page 7 Name: 100903A-2007 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000201 n Quantify Sanale Report Study No.:L35195, Set No.:100903A, Ext.Date:10/09/03, Analyst-.K.Risha 1 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903A Daikin 4 Last modified: Fri Oct 10 07:25:26 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 10 07:30:15 2003 Page 8 Harne: 100903A-2008 Text: IT 1 : PFOA j*---Ii l ' n k % I ' f1 iH r""f Exygen Research, 3058 Research Drive, State College, PA 16801 000202 Quantify Sample Report Study No.:L35195, Set N o . :100903A, Ext.Date:10/09/03, Analyst:K.Risha Sample L i s t : P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903A Daikin Last modified: Fri Oct 10 07:25:26 2003 Method: P :\Data\LCMSMS7 \Masslynx\Fluorochems. PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 10 07:30:15 2003 Page 9 Name: 100903A-2009 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000203 Quantify Sample Report Study No. :L35195, Set No. :100903A, Ext.Date:10/09/03, Analyst:K.Risha Rage 10 rr-5a Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903A Daikin Last modified: Fri Oct 10 07:25:26 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 10 07:30:15 2003 II Name: 100903A-2010 Text: ii l: Research, 3058 Research Drive, f a t-. 000204  Quantify Sandle Report ; Study No.sL35195, Set No.:100903A, Ext.Dates 10/09/03, AnalystsK.Risha f* Sample Lists Ps\Data\LCMSMS7\Masslynx\Fluorochems,PRO\SampleDB\100903A Daikin Last modifieds Fri Oct 10 07:25:26 2003 T ' Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 {T5 Job Codes f? Printed: Fri Oct 10 07:30:15 2003 Rage 11 f f Names 100903A-2011 Text s ! f-- i t4 Li f. fc * * iJ H t1 rj k Exygen Research, 3058 Research Drive, State College, PA 16801 n 000205 *I > Quantify Sample Report Study No.:L35195, Set No.:100903A, Ext.Date:10/09/03, Analyst:K.Risha Page 12 P* Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903A Daikin i- Last modified: Fri Oct 10 07:25:26 2003 ` Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 H Job Code: I- Printed: Fri Oct 10 07:30:15 2003 < -------------------------------------------- ts Name: 100903A-2012 Text: r* 1 : PFOA k* ft i sI t- 4 n Exygen Research, 3058 Research Drive, State College, PA 16801 000206 f Quantify Sample Report Study No.:L35195, Set No.:100903A, Ext.Date:10/09/03, Analyst:K.Risha Page 13 Sample List: P:\Data\LOMSMS7\Masslynx\FTuorochems.PR0\SampleDB\100903A Daikin Last modified: Fri Oct 10 07:25:26 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 10 07:30:15 2003 t > t Name: 100903A-2013 Text: j 1 : PFOA L35195-2, DF=10000 e-> . 100903A -2013 Sm (Mn, 2x2) E 10Ch 5.24 183841 09-0ct-2003 17:38:23 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.56e5 Area %: o - f'. 1 1 * i ~1 1 1 .................. | 1.00 2.00 . . r-'T-[" ' ' ' I 1 ' ` ' I ' ' ' 1I ' 1 ' r 1'' ' i . -t-.-i", i ' <n .' . 1 . .-r-n Tim e 3.00 4.00 5.00 6.00 7.00 8.00 n* I n i' r --> Exygen Research, 3058 Research Drive, State College, PA 16801 000207 I > Quantify Sample Report ' Study No.:L35195, Set No.:100903A, Ext.Date:10/09/03, Analyst:K.Risha Page 14 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903A Daikin : Last modified: Fri Oct 10 07:25:26 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 fl Job Code : k- Printed: Fri Oct 10 07:30:15 2003 Name: 100903A-2014 Text: 1 : PFOA L35195-2 Rep, DF=10000 , . 1 0 0 9 0 3 A -2 0 1 4 S m (M n, 2x2) 1OOn n k; %~ 5.24 181231 0: t'i iT=rrr-i=rT-,itt r r r i i i"i i t i i 1.00 2.00 3 .0 0 A 1111111` ` 11i 111M 1 4.00 5.00 09-0ct-2003 17:55:06 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.64e5 Area .' 11 j i i i t t t i t t i i i i I i i i i-i Tim e 6.00 7 .0 0 8.00 Jr.- ' r'f: ; ti .n Exygen Research, 3058 Research Drive, State College, PA 16801 000208 pM* Quantify Sample Report Study No.:L35195, Set No.:100903A, Ext.Date:10/09/03, Analyst:K.Risha Page 15 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903A Daikin Last modified: Fri Oct 10 07:25:26 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: i Printed: Fri Oct 10 07:30:15 2003 rs Name: 100903A-2015 Text: 1 : PFOA t p-- ` r I- : Exygen Research, 3058 Research Drive, State College, PA 16801 000209 Quantify Sample Report Study No.:L35195, Set No.:100903A, Ext.Date:10/09/03, Analyst:K.Risha Page 16 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903A Daikin Last modified: Fri Oct 10 07:25:26 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 10 07:30:15 2003 Name: 100903A-2016 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000210 n t: , Quantify Sample Report '< Study No.:L35195, Set No.:100903A, Ext.Date:10/09/03, Analyst:K.Risha Page 17 f' Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903A Daikin t Last modified: Fri Oct 10 07:25:26 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 ET? Job Code: Printed: Fri Oct 10 07:30:15 2003 t" 1 ' ' Name: 100903A-2017 Text : 1 : PFOA XC100703-3,100 ng/L standard 100903A-2017 Sm (Mn, 2x2) 100n %- 5.24 18655 09-0ct-2003 18:45:22 LC/MS/MS #7 M R M of 1 Channel E S 413 > 3 6 9 2.13e5 Area Kr 1.00 2.00 I" j '| I..I.I' 3.00 4.00 5.00 6.00 7.00 Tim e 8.00 f' r"*"- P k t} n n i1 p - Exygen Research, 3058 Research Drive, State College, PA 16801 000211 Quantify Sample Report Study No.:L35195, Set No.:100903A, Ext.Date:10/09/03, Analyst:K.Risha Page 18 r"' Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903A Daikin 1 Last modified: Fri Oct 10 07:25:26 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 f-- job Code: Printed: Fri Oct 10 07:30:15 2003 Name: 100903A-2018 Text: 1 : PFOA n Ii! : Exygen Research, 3058 Research Drive, State College, PA 16801 000212 fr* Quantify Sample Report Study No.:L35195, Set No.:100903A, Ext.Date:10/09/03, Analyst:K.Risha Page 19 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903A Daikin Fri Oct 10 07:25:26 2003 P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Fri Oct 03 12:53:47 2003 Printed: Fri Oct 10 07:30:15 2003 Name: 100903A-2019 Text: 1: PFOA XC100703-5, 500 ng/L standard r"*!i 100903A -2019 S m (Mn, 2x2) r* i* ' 100: _ %: 5.23 89046 09-0ct-2003 19:18:49 LC/MS/MS #7 MRM of 1 Channel ES413 >369 9.09e5 Area o : ,,'T 1 " 1.00 !- I ' " 'I" r I ! I I I I I " 2.00 3.00 4.00 5.00 I I I I i I r -r-r r t 11"T i "t p 6.00 7.00 Tim e 8.00 prTn i' *. * n r ti. . V- Exygen Research, 3058 Research Drive, State College, PA 16801 J0 1 3 ; Quantify Sandle Report Study No.:L35195, Set No.:100903A, Ext.Date:10/09/03, AnalysttK.Risha Page 20 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903A Daikin Last modified: Fri Oct 10 07:25:26 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 n Job Code: Printed: Fri Oct 10 07:30:15 2003 IFF ' Name: 100903A-2020 Text: 1 : PFOA XC100703-6,1000 ng/L standard 100903A -2020 Sm (Mn, 2x2) : s 1 0 0 n 1 hT i /c r 5.23 169898 09-0ct-2003 19:35:46 LC/MS/MS #7 M R M of 1 Channel ES413 > 369 1.69e6 Area n (y n . 1.00 ~ r"i T ~ r \ \ i~'T'T-r-T 2.00 3.00 4.00 5.00 6.00 7.00 Tim e 8.00 IF**, I4 r", Exygen Research, 3058 Research Drive, State College, PA 16801 000214 Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L3S19S PFOA 413 -> 369 NA R A W DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Weight*. Final Volume: 50 ppt 15pL Soil 5.0 g 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 100203B Karen Risha LC/MS/MS Unit #7 10/02/03 10/02-03/03 Exygen ID XC092303-0 XC092303-1 XC092303-2 XC092303-3 XC092303-4 XC092303-5 XC092303-6 Methanol Wash Reagent Blank Reagent Spk A Reagent Spk B L35195-1 SpfcC L35195-1 L35195-1 Rep XC092303-1 XC092303-2 XC092303-3 XC092303-4 XC092303-5 XC092303-6 Sponsor ID - '- - NA NA NA DAI-092503-NW-01 DAI-092503-NW-01 DAI-092503-NW-01 - - - - Sample Code c CS CS CS CS CS CS c c LCS LCS LF s s CS CS CS CS CS CS Run No. 100203B-2001 100203B-2002 10023B-2003 10203B-2004 100203B-2005 100203B-2006 100203B-2007 100203B-2008 100203B-2009 100203B-2010 100203B-2011 100203B-2012 100203B-2013 100203B-2014 100203B-2015 100203B-2016 10023B-2017 100203B-2018 100203B-2019 100203B-2020 Analyte Found (ppt) = (peak area - intercept) / slope x DF Recovery (%) = [analyte found (ppt)-analyte found in control (ppt)] x 100 amount added (ppt) Std. Cone. (PPt) 0 25 50 100 250 500 1000 - - 25 50 100 250 500 1000 Dilution Factor - - 1 I 1 1 1 1 - - - Peak Area 920 5013 9278 17316 39809 84547 168445 0 0 8819 86088 28826504 28145108 28103830 31817 12566 19576 41926 87122 169386 Analyte Found (ppo ND 43.4 507 A # * - Amount Added (ppo 50 500 500 - - - - Recovery m 87 101 - - - - Analyte Found (ppb) - - - - -- -- Standard Curve: Linear (1/x weighted) Intercept = 1588.19 Slope = 166.671 Coef. Of Det. = 0.999178 Total Solids (%> - - 46.94 46.94 - - Analyte Found (ppb) = [analyte found (ppt) x volume extracted (0.04 L)] / sample weight (5 g) Analyte Found (ppb) dry weight = analyte found (ppb) x (100% / total solids (%)) CS = Calibration standard C = Control sample S = Sample LF = Lab fortified sample FF = Field fortified sample LCS = Laboratory Control Spike CK = Check Standard ND = Not detected = Response between 0 and 25 ppt NQ = Not quantifiable = Response between 25 ppt and LOQ(50 ppt) ASample requires higher spiking level. See data set 100903B. Sample requires dilution. See data set 100903B. Spreadsheet prepared by:. Analyte Found (ppb) Dry Weight - - - - - 000215 fl 3058 Research Drive Phone: 814-272-1039 H State College, PA 16801 Fax: 814-231-1580 SAMPLE TRANSFER SHEET Protocol Number: __________ N A __________ Exygen Study Number. L35195 Exygen Sample # Sponsor Sample # Exygen Sample # Sponsor Sample # fe 1 ti L 35195-1 DAI-092503-NW-01 L 35195-2 DAI-092503-NW-02 _ -_ -- -_ -- -_ f _- - - --- - - _' -- -- -- -- t i Karen R ishal0/01/03 1500 Requested By (Printed Name/Date/Time) tn Samples removed from:_____ ___________________ Box#______ ----_________ Shelf# Samples removed from: ' Box# --- Shelf# Samples transferred to the custody of <? f f " Sample Custodian Initials/Date/Time r* Samples received from custodian; Samples moved to Samples removed from_________ Samples returned to ______________f l* ? Labrate Personnel Initials/Date/Time " Sample Custodian Initials/Date/Time fs 000216 " 3 a l ;:j s h ' :.i 1 ' * ' '1 w:;::i3ror;^G4.r:i m Analysis: Solids Title: Data I ! I `1 r I ` Ire p C "' ' j3 -0 c " 7 1 Analyst Initials Date and Time Data Aquired (ctrl+t) shz shz 13-O ct-03 16:49 13-Oct-03 16:49 shz 14-Oct-03 08:48 CAL ID CLIENT ID MATRIX PAN ID PAN WEIGHT (g) SAMPLE +PAN (g) W G 46472-1 W G46472-2 L35195-1 L35212-1 L35228-1 L35247-5 L35259-2 MB P E R C SO LID | SOLID UP: L35195- PERO SOLID | SOLID 1-092503-NV P E R C SO LID | SOLID SS9-29 P E R C SOLID | SOLID SHOT P E R C S O LID | SOLID DSSD206 P E R C SOLID | SOLID ALE POND P ER C SO LID | SOLID 1 2 4 5 6 7 8 1.2685 1.2671 1.2695 1.2718 1.2688 1.268 1.2697 1.2685 25.881 24.2526 17.6671 14.1902 24.2113 22.4373 DRIED SAMPLE + PAN (g) IGNITED SAMPLE +PAN (9) 1.2684 12.9117 12.0587 14.5221 13.7454 17.786 16.8762 "/.S olids or % TVS or % Ash 0 47.3 46.94 80.81 96.55 71.99 73.72 _________________i 000217 Print Date: 14-Oct-03 ----------- -- -------------------- Page 1 of 1  Ai.,,.7" i:S h .Z l - -1 Xo-W'O'b Item r| iwo;::iroLin v G ,r 72 rri Analysis: Solids Title: Comments ;t i :r3>ate:>rec ;:ioct-;7 ;i ' z i Comment About 20 g of each sample was weighed in aluminum weighing dishes using balance 9 (IN0000288). Samples were placed into oven 2 (IN0000062) at 1700 for over night, (temperture In 104C) Samples were removed from oven at 0830 and cool in desiccators 6 and weighed using balance 9 (IN0000288).(temperture out 104oC) 0218 Print Date: 14-Oct-03 Page 1 of 1 > A,.;;ishi -i 10 ~ l Y - 2 1 1 i :!:T w o:::iroL ^ !lvG C rr2 ;' T3 Analysis: Solids Title: QC Workgroup LAB ID Matrix QC ID DF PERC SOLID WG46472-1 SOLID MB 1.00 0.00 TV 0.00 Q>5xMDL WG46472-2 SOLID DUP: L35195-1 TV RPD(%) Q+/-5% 1.00 1.00 u 47.30 46.94 0.76 m ^^rbater^iarecr'ioctr::! "1:3 000219 Print Date: 14-Oct-03 Page 1 of 1 v .:" i :* "i '. ' i .T: i r :.T w o ..:iro C :)vG<z:n'2 \0'^ ~ 63 Analysis: Solids Title: Send .t : ::^ate:::iaref:rioct-: i r z i ID Result Product Matrix DF MDLxDF CRDLxDF Flags Time Collect L35195-1 46.94 PERC SOLID SOLID 1 0.01 0 25-Sep-03 08:30 L35212-1 80.81 PERC SOLID SOLID 1 0.01 0 29-Sep-03 13:00 L35228-1 96.55 PERO SOLID SOLID 1 0.01 0 02-0ct-03 16:30 L35247-5 71.99 PERC SOLID SOLID 1 0.01 0 08-0ct-03 10:00 L35259-2 73.72 PERC SOLID SOLID 1 0.01 0 09-0ct-03 11:02 Time Run 13-Oct-03 11:58 13-Oct-03 11:58 13-Oct-03 11:58 13-Oct-03 11:58 13-0ct-03 11:58 Client ID DA1-092503-NW-01 SS9-29 SHOT DSSD206 HUNTSDALE POND BOTTOM 000220 Print Date: 14-Oct-03 Page 1 of 1 1 S\ Z 3 /H ^ Item n :iwc::nroC-^vG::>2 n j j Date " ]>are' 5-Oct' | Analysis: Solids Title: Comments Comment About 20 g of each sample was weighed in aluminum weighing dishes using balance 9 (IN0000288). Samples were placed into oven 2 (IN0000062) at 1700 for over night, (temperture in 104C) 00 221 Print Date: 13-Oct-03 Page 1 of 1 ' * - 1 -yy?- *- yr'-v' % 1 A...., A SHL......J -- ,,J A'>V O i .} t i :::i vciiGro; /g^ i ::r> .:::) Analysis: Solids Title: Data Analyst Initials Date and Time Data Aquired (ctrl+t) shz shz 13-O ct-03 16:49 1 3 -0 c t-0 3 16:49 33-0 <;:: r : n 000222 P rin t Date: 13-Oct-03 Page 1 of 1 n n 3058 Research Drive Phone: 814-272-1039 it R E S E A R C H State Colle-ge, PA 16801 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number: L35195 Matrix: Sludge Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No. FI T im e___ Q H 'P ii &Initials CLIENT SAMPLE ID EXYGEN ID NUMBER W EIG H T (g) FO R T IFIC A T IO N (ng) na Reagent Blank . na Reagent Spk A 2.0 na Reagent Spk B _ 20.0 DAI-092503-NW-01 L35195-1 SpkC DAI-092503-NW-01 L35195-1 DAI-092503-NW-01 L35195-1 Rep H ^ - - -- 5.0 5.0 5.0 _ _ 20.0 _ . _ - fi - - '- - - __ - __ -_ _ __ __ _ __ _ __ _ __ -_ _- _ - -- Spiking Solution Used Volume Used for Spiking friitial/Date Reagent Spk A F092203-5 (10 ng/mL) 200 |xL (200 pL micropipet) / io\ozfo- i- ' Reagent Spk B F092203-4 (100 ng/mL) 200 pL (200 pL micropipet) * tr /XOlfizb L35195-1 Spk C - F092203-4 (100 ng/mL) 200 pL (200 pL micropipet) M /iDfcZi1Qf------------ ------- - ------ --------- ----- - _ - _ __ -- All samples were weighed on balance No. Time ______ Date jO | 03-1^ Initials - - After weighing samples were returned to refrigerator No. 3 - Thne---- LSCO______ D ate__ [ 0 | o 24d?7 Initials. *: cj07-103 , Com m ents: 200 pL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date: Analysis Summary: Data Set: 1 0 0 2 D 3 & Initials/Date: n Data Set: 1n o i0 * > & " Initials/Date: Data Set:_____ H I______ Initials/Date: Set extraction/analysis data verified by: o Date; July 26, 2001/1 000223 1 3 \ I1 1 ' 3058 Research Drive Phone: 814-272-1039 C H State College, P A 16801 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L35195 METHOD: ExM-023-014 $$ MATRIX: Sludge ANALYTES: PFOA PROTOCOL NUMBER: NA Client ID na na Exygen ID Reagent Blank Reagent Spk A STEP STEP STEP 12 3 na DAI-092503-NW-01 DAI-092503-NW-01 DAI-092503-NW-01 - *lnitials/D ate Reagent Spk B L35195-1 Spk C L35195-1 L35195-1 Rep - - - - - - - J \/ --- \Y - - --- --------------------- CJ-L1jL. VI L 5 f t >|C>[C2|6 STEP1: Add5mLof methanol and shake by hand f o r - 1 minute STEP 2: Bring up to 40 mL with hypercarb filtered type I water STEP 3: Centrifuge for 10 minutes a t -3000 rpm , .. STEP 4: FHtei tlliuugfrgiass aermfec...SAMPLE ^AUlCh. STEP 5: SPE column clean up U STEP 6: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP 7: LC/MS/MS analysis STEP 8: LC/MS/MS reanalysis. STEP STEP STEP 456 \/ \ ----- --- - -------------------- it! 3 * c* L A i____ Dilutions (mL/mL) - - ' ~ - - - - - - - - - STEP 7 Dilutions (mL/mL) *- STEP 8 - - \ 1 V La1___ -- --- - -- --- - -- --- - -. -- _ - -- -- - --- - -- - -- 4% j: 'o p t (pfcf-=\O fiO O Reagents/ Materials Methanol C18 SPE Type I Water - - . _ _ - Initials/Date - . . _ - Lot# 43132320 NA _ _ ^ ID 6 2 3 U- _ _ HPLC Methanol 43U>&524 Ammonium Acetate Type I water - Initials/D ate NA ------ ----------- initials and date under each step indicates the personnel that performed this step. $$ Method of Analysis for the Determination of Perfluorooctanesulfonate (PFOS) and Pentadecafluorooctanoic Acid (PFOA) in Soil COMMENTS: Final extracts stored in refrigerator Initials: Date: 1d M o3 July 19, 2001/4 000224 "1 i 1 Mass lynx - Sample List Sample List: C:\MASSLYNX\Fluorochleemiss..KPKRUOV\Sbai mpleDB\100203B Daikin.spl Printed: Thu Oct 02 15:03:53 2003 ^ I Q l Z k l ___________________ Vial File Name LIMS ID Client ID Sample Description 1 1 100203B-2001 -- 2 2 100203B-2002 -- 3 3 100203B-2003 -- 4 4 100203B-2004 -- 5 5 100203B-2005 -- 6 6 100203B-2006 -- 7 7 100203B-2007 -- 8 92 100203B-2008 -- 9 21 100203B-2009 -- 10 22 100203B-2010 -- 11 23 100203B-2011 -- 12 24 100203B-2012 -- 13 25 100203B-2013 -- 14 26 100203B-2014 -- 15 2 100203B-2015 -- 16 3 100203B-2016 -- 17 4 100203B-2017 -- 18 5 100203B-2018 -- 19 6 100203B-2019 -- 20 7 100203B-2020 -- XC092303-0, 0 ng/L standard XC092303-1, 25 ng/L standard XC092303-2, 50 ng/L standard XC092303-3,100 ng/L standard XC092303-4,250 ng/L standard XC092303-5, 500 ng/L standard XC092303-6,1000 ng/L standard Methanol Wash Reagent Blank Reagent Spk A, 50 ng/L Reagent Spk B, 500 ng/L L35195-1 Spk C, 500 ng/L L35195-1 L35195-1 Rep XC092303-1, 25 ng/L standard XC092303-2, 50 ng/L standard XC092303-3,100 ng/L standard XC092303-4,250 ng/L standard XC092303-5, 500 ng/L standard XC092303-6,1000 ng/L standard 000225 Exygen STUDY N O . L 3 S ftr Page 1 Page Position: (1,1) Matrix Sample Type Cone (ng/L) Cone B Cone C Test ID DF MS Method -- Blank 0 -- Standard 25 -- Standard 50 -- Standard 100 -- Standard 250 -- Standard 500 -- Standard 1000 -- Blank -- -- Blank -- -- QC 50 -- QC 500 -- QC 500 -- Analyte -- -- Analyte -- -- Standard 25 -- Standard 50 -- Standard 100 -- Standard 250 -- Standard 500 -- Standard 1000 -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA I m m "::i i r : i r : i ; : i ::'"i Masslynx - Sample List Sample List: C:\MASSLYNX\Fluoroche3irnss..PPRKOO\\Sbampl!eLDB\100203B Daikin.spl Printed: Thu Oct 02 15:03:53 2003 \ i0(02-103> HPLC Method MS Tune File inj Volume (pL) 1 water PFOA Tune 15 2 water PFOATune 15 3 water PFOA Tune 15 4 water PFOATune 15 5 water PFOATune 15 6 water PFOATune 15 7 water PFOATune 15 8 water PFOA Tune 15 9 water PFOA Tune 15 10 water PFOATune 15 11 water PFOATune 15 12 water PFOATune 15 13 water PFOATune 15 14 water PFOATune 15 15 water PFOATune 15 16 water PFOATune 15 17 water PFOATune 15 18 water PFOA Tune 15 19 water PFOATune 15 20 water PFOATune 15 9ZZ000 Exygen study n o . c s s n s * Page 2 Page Position: (2,1) n LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: N A Exygen Study No: L35195 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #7) r*! * Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 Ip -1 HP Quat Pump HP Vacuimi Degasser HP Autosampler HP Column Oven HPLC Column: Genesis C-8, 5 cm x 2.1 mm i.d. x 4 jr (Exygen ID:MA10327) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) Mobile Phase (B) : 2 mM Ammonium Acetate in Type I Water Methanol Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. A ll Handwritten P eak ID 's by:_ n I. Lt-J; 000227 n Scanning Method Report r-s Method: C:\MASSLYNX\FLUOROCHEMS.PRO\ACQUDB\OO8 PFOA ; Last Modified: Thu Oct 02 14:56:38 2003 Printed: t- : Thu Oct 02 15:04:11 2003 Solvent Delay ( mins ) 0.00 0:2 . 0 3 r"* Function : 1 M R M of 1 Mass Pair ( ESP- ) ' Inter Channel Delay i( Secs ) : 0.03 n Span ( Daltons ) : Start Time ( Mins ) : t : End Time ( Mins ) : 0.00 0.00 8.00 Repeats : 1 Channel Parent Daughter Dwell (Secs) Coll Energy (eV) P ?' ' 1 413.00 369.00 0.20 10 Cone 10 t - n #> -* Page 1 .r-* ;lt : p <1 *4 t ; 000228 ;r^ r' ------------* Method Report Method File: Last Modified: C:\MASSLYNX\FLUOROCHEMS.PRO\ACQUDB\water Thursday, October 02, 2003 14:57:31 Page 1 Printed: n HP1100 LC Pump Initial Conditions Thursday, October 02, 2003 15:05:03 mmv3 Solvents n A% B% C% D% 60.0 40.0 0.0 0.0 p Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) C~j Oven Temperature Left(C) f ' Oven Temperature Right(C) 0.300 15.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable t gradient Timetable contains 10 entries which are : t Time A% B% C% D% 0.00 60.0 40.0 0.0 0.0 * ! 0.40 60.0 40.0 0.0 0.0 1.00 10.0 90.0 0.0 0.0 7.00 10.0 90.0 0.0 0.0 7.50 0.0 100.0 0.0 0.0 9.00 0.0 100.0 0.0 0.0 9.50 60.0 40.0 0.0 0.0 13.50 60.0 40.0 0.0 0.0 14.00 60.0 40.0 0.0 0.0 15.00 60.0 40.0 0.0 0.0 t Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 0.300 Pressure 400 400 400 400 400 400 400 400 400 400 HP1100 LC Pump External Event Timetable j The Timetable contains 4 entries which are : Time Initial 0.00 0.10 8.00 Column Switch Contactl Off Off Off On Off Off Off Off P""! HP1100 Autosampler Initial Conditions Contact2 Off Off On Off Contact3 Off Off Off Off Contact4 Off Off Off Off Draw Speed P Eject Speed (1/min) ' ( Draw Position (mm) Stop Time (mins) Injection Volume(/l) n Vial Number Vf :' 200.0 200 0.10 15.00 15.0 16 ' n i` r? f n Xt 000229 Tuning Method Report Method : C :\MASSLYNX\FLUOROCHEMS .PRO\ACQUDB\PFOA TUNE Page 1 Dau 413.00 SOURCE ( ESP- ) CapillaryCone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 10 0.0 0.0 0.0 100 300 -2.93 -10 98 300 Pressures Analyser Vacuum Gas Cell Rdbk OFF 3.9e-3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set Rd 14.0 14.0 1.0 -2 10 2 14.0 14.0 2.0 700 8 9 11 -6 Rdbk 128.5 711.7 000230 Quantify Calibration Report Study No. :L35195, Set No. -.100203B, Ext .Date; 10/02/03, Analyst sK.Risha Calibration: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\CurveDB\100203B Daikin Last modified: Fri Oct 03 13:38:26 2003 Printed: Fri Oct 03 13:39:45 2003 Page 1 Exygen Research, 3058 Research Drive, State College, PA 16801 000231 bi Quantify Saiqple Report Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, Analyst:K.Risha Rage 1 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203B Daikin 3 Last modified: Fri Oct 03 13:37:02 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 13:39:46 2003 In itia ls .__ J i= - Ruim&giaxn To locfra&afi Name: 100203B-2001 Text: v< f H fe" - n f^ f' jH"1 Exygen Research, 3058 Research Drive, State College, PA 16801 000232 ri fr1 ; Quantify Sample Report ` Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, Analyst:K.Risha r** Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203B Daikin ' Last modified: Fri Oct 03 13:37:02 2003 1 Method: P:\Data\LOMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 P" Job Code: S Printed: Fri Oct 03 13:39:46 2003 Page 2 I Name: 100203B-2002 Text: i l 1: PFOA R l, r ? i f` L ..- f Exygen Research, 3058 Research Drive, State College, PA 16801 000233 pi in I 1 Quantify Sample Report Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, Analyst:K.Risha Sample List; P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203B Daikin I Last modified; Fri Oct 03 13;37;02 2003 ! Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 H Job Code : )J- ' - Printed; Fri Oct 03 13:39:46 2003 s;i ^ ` Name: 100203B-2003 Text: r ' 1 : PFOA Page 3 *'S it 1 P"| p .1 j n i; i !n 4 Exygen Research, 3058 Research Drive, State College, PA 16801 n 000234 V Quantify Sample Report Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, Analyst:K.Risha Page 4 f*! Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203B Daikin i Last modified: Fri Oct 03 13:37:02 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 13:39:46 2003 c*i Name: 100203B-2004 Text: FF 1 : PFOA XC092303-3,100 ng/L standard 100203B -2004 Sm (Mn, 2x2) 100-1 5.24 17316 02-0ct-2003 23:06:15 LC/MS/MS #7 M R M of 1 Channel ES413 >369 1.89e5 Area 0-^ I1I1 1.00 2.00 1 3.00 4.00 I1111i I I I1I I I 5 .0 0 6.00 7.00 Tim e 8.00 kn * y***. -s , si Exygen Research, 3058 Research Drive, State College, PA 16801 000235 Quantify Sample Report Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, Analyst:K.Risha jC*1! Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203B Daikin t ; Last modified: Fri Oct 03 13:37:02 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 13:39:46 2003 Rage 5 t ! Name: 100203B-2005 Text : 1 : PFOA ?i Exygen Research, 3058 Research Drive, State College, PA 16801 000236 Quantify Sample Report Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100203B Daikin Last modified: Fri Oct 03 13:37:02 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 13:39:46 2003 Rage 6 Name: 100203B-2006 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000237 Quantify Sanale Report Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203B Daikin Fri Oct 03 13:37:02 2003 P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Fri Oct 03 12:53:47 2003 Printed: Fri Oct 03 13:39:46 2003 Page 7 t ' Name: 100203B-2007 Text: 1: PFOA XC092303-6,1000 ng/L standard jpe f. ; 10 0 2 0 3 B -2 0 0 7 S m (Mn, 2 x 2 ) 100-1 5.24 168445 02-0ct-2003 23:56:35 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1 .79e6 Area O-J-f T-n Time 1.00 2.00 3 .00 4.00 5.00 6.00 7 .00 8.00 *- Exygen Research, 3058 Research Drive, State College, PA 16801 000238 f Quantify Sample Report Study No.:L35195, Set N o . :100203B, xt.Date:10/02/03, Analyst:K.Risha 0* Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100203B Daikin f ; Last modified: Fri Oct 03 13:37:02 2003 - - Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 H Job Code: ` v Printed: Fri Oct 03 13:39:46 2003 FT Marne: 100203B-2008 Text: 1 : PFOA Page 8 5| 1*1 5- ' L- ! Exygen Research, 3058 Research Drive, State College, PA 16801 000239 fi I*'"* i ! Quantify Sample Report Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, Analyst:K.Risha f* Sample L i s t : P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203B Daikin l i Last modified: Fri Oct 03 13:37:02 2003 * ` Method: P :\Data\LCMSMS7 \Masslynx\Fluorochems. PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 f~* Job Code: Printed: Fri Oct 03 13:39:46 2003 Rage 9 8 Name: 100203B-2009 Text : 1 : PFOA r? i1 r* * --* hi l.j Exygen Research, 3058 Research Drive, State College, PA 16801 000240 pi t: 4 Quantify Sample Report Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, Analyst:K.Risha Page 10 f*85 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100203B Daikin r Last modified: Fri Oct 03 13:37:02 2003 ^ ' Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 f-> Job Code: Printed: Fri Oct 03 13:39:46 2003 Name: 100203B-2010 Text: T' LJ I -- Exygen Research, 3058 Research Drive, State College, PA 16801 000241 jh i Quantify Sample Report Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, Analyst sK.Risha Rage 11 f* Sample Lists P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203B Daikin : Last modified: Fri Oct 03 13:37:02 2003 f Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 f ; Job Code: Printed: Fri Oct 03 13:39:46 2003 Name: 100203B-2011 Text: 1 : PFOA R' l ./ ' jl , ; %< n f Exygen Research, 3058 Research Drive, State College, PA 16801 000242 t ' Quantify Sample Report * Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, Analyst:K.Risha Page 12 f Sample List: P:\Data\LCMSMS7\Masslynx\FluorocheirLS.PRO\SampleDB\100203B Daikin 1 j Last modified: Fri Oct 03 13:37:02 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Bast modified: Fri Oct 03 12:53:47 2003 jH Job C o d e : Printed: Fri Oct 03 13:39:46 2003 r1 ; Name: 100203B-2012 Text: fc i } t- H ! n Exygen Research, 3058 Research Drive, State College, PA 16801 000243 Quantify Sample Report Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, Analyst:K.Risha Page 13 jf"; Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203B Daikin | ; Last modified: Fri Oct 03 13:37:02 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 H Job Code: Printed: Fri Oct 03 13:39:46 2003 Name: 100203B-2013 Text: 1 : PFOA L35195-1 100203B-2013 Sm (Mn, 2x2) 100-1 * %- 0 ` '''I ' 1 I I ' 1 1 I I 1 ' I ' 1 1 I I 1 1 ` ` 1.00 2 .0 0 3.00 5.27 4.00 5.00 03-0ct-2003 01:37:25 LC/MS/MS #7 M RM of 1 Channel ES413 > 3 6 9 1,34e8 Area 6.00 ' ' ' 1 M 1 11h "111 Tim e 7.00 8.00 n Jr . " n Exygen Research, 3058 Research Drive, State College, PA 16801 000244 Quantify Sample Report Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, Analyst:K.Risha Page 14 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203B Daikin Last modified: Fri Oct 03 13:37:02 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 13:39:46 2003 Name: 100203B-2014 Text: 1 : PFOA L35195-1 Rep 100203B-2014 Sm (M n , 2x2) 100n %- 5.25 28103830 03-0ct-2003 01:54:09 LC/MS/MS #7 M RM of 1 Channel ES413 > 3 69 1.34e8 Area 0 '''I<' 1I1" 1.00 '"np"' i j - 'f - r "!" \ I ; r " ii "t I t t i I I i I I I I' 2.00 3.00 4.00 5.00 6.00 7.00 - h Tim e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000245 n 11 n . .. . . f Quantify Sample Report Page 15 ; Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, Analyst:K.Risha p Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203B Daikin Last modified: Fri Oct 03 13:37:02 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 n Job Code: i ` Printed: Fri Oct 03 13:39:46 2003*I r~ ' I Name: 100203B-2015 Text: ( > M' n '' '. r I Exygen Research, 3058 Research Drive, State College, PA 16801 n 000246 JT"1 f"1 ' I Quantify Sample Report * ; Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, Analyst:K.Risha Page 16 jH Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203B Daikin j. Last modified: Fri Oct 03 13:37:02 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 n Job Code: Printed: Fri Oct 03 13:39:46 2003 Name: 100203B-2016 Text: n n I5 Exygen Research, 3058 Research Drive, State College, PA 16801 000247 Quantify Sandle Report Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, Analyst:K.Risha Page 17 Sandle List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100203B Daikin Last modified: Fri Oct 03 13:37:02 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 13:39:46 2003 Name: 100203B-2017 Text: 1 : PFOA XC092303-3,100 ng/L standard 100203B-2017 Sm (Mn, 2x2) 10Ch %- "i iT Hi( y T " i'T T ' l i 1 1 1 1 1 1 1T 1V i T T '. , i , . 1 , 1.00 2.00 3.00 4.00 5.25 195761 { 5.00 03-0ct-2003 02:44:18 LC/MS/MS #7 M RM of 1 Channel ES413 >369 2.02e5 Area i T-TT. I-T-I-! f n - r r i T r~r . n~| Tim e 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000248 mm i ?/ (n: I Quantify Sample Report Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, AnalystsK.Risha Page 18 P I Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203B Daikin Last modified: Fri Oct 03 13:37:02 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 13:39:46 2003 i Name: 100203B-2018 Text: 1 : PFOA XC092303-4, 250 ng/L standard n 100203B -2018 Sm (Mn, 2x2) 100n nk < %- 5.24 41926 03-0ct-2003 03:01:14 LC/MS/MS #7 M RM of 1 Channel ES413 >369 4.36e5 Area 0^ 1.00 I I j "1 I I I I I T I--1" |....1 I I 1 I 2 .0 0 3.00 4.00 5.00 6.00 r-i"i`1 r-i-r-rt- T im e 7 .0 0 8.00 H I ks Exygen Research, 3058 Research Drive, State College, PA 16801 000249 Quantify Sample Report Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, Analyst:K.Risha Page 19 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203B Daikin Last modified: Fri Oct 03 13:37:02 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 13:39:46 2003 Name: 100203B-2019 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000250 Quantify Sample Report Study No.:L35195, Set No.:100203B, Ext.Date:10/02/03, AnalystsK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100203B Daikin Last modified: Fri Oct 03 13:37:02 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Fri Oct 03 13:39:46 2003 Page 20 Marne: 100203B-2020 Text : 1 : PFOA XC092303-6,1000 ng/L standard 100203B -2020 Sm (Mn, 2x2) 100~] %: 03-0ct-2003 03:34:50 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1 .66e6 Area r- j I I ) I j I ! 'I " I j I r i'-'T - p ' I" I I I I I I r | i 1.00 2.00 3.00 '' ' '"I1"1'"1 I I I I " I I Tim e 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000251 Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L35195 PFOA 413->369 NA R A W DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Weight: Final Volume: 50 ppt 15 pL Soil 5.0 g 5.0 tnL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 100903B Karen Risha LC/MS/MS Unit #7 10/09/03 10/07/03 Exygen ID XC100703-0 XC100703-1 XC100703-2 XC100703-3 XC100703-4 XC100703-5 XC100703-6 Methanol Wash Reagent Blank Reagent Spk A Reagent Spk B L35195-1 SpkC L35195-1 L35195-1 Rep XC100703-1 XC100703-2 XC100703-3 XC100703-4 XC100703-5 XC100703-6 Sponsor ID - - - - NA NA NA DAI-092503-NW-01 DAI-092503-NW-01 DAI-092503-NW-01 - - - Sample Code c CS CS CS CS CS CS C C LCS LCS LF s s CS CS CS CS CS CS Run No. 100903B-4001 100903B-4002 100903B-4003 100903B-4004 100903B-4005 100903B-4006 100903B-4007 100903B-4008 100903B-4009 100903B-4010 100903B-4011 100903B-4012 100903B-4013 100903B-4014 100903B-4015 100903B-4016 100903B-4017 100903B-401S 100903B-4019 100903B-4020 Analyte Found (ppt) = (peak area - intercept) / slope x DF Recovery (%) = [analyte found (ppt)-analyte found in control (ppt)] x 100 amount added (ppt) Std. Cone. (ppt) 0 25 50 100 250 500 1000 - - - - - - - 25 50 100 250 500 1000 Dilution Factor - - - - 1 1 1 10000 10000 10000 - - - Peak Area 1101 5000 9400 18429 40654 86873 167378 0 0 8332 89809 17625 10243 10183 5175 9421 19175 41227 88553 172811 Analyte Found (ppt) - Amount Added (ppt) - Recovery (%) - Analyte Found (ppb) - -- -- -- - - ---- ---- -- -- -- -- ND - -- 43.7 50 87 - 524 500 105 - 985000 500000 87 - 549000 - - 4400 546000 - - 4370 -- -- -- -- -- - - -- -- -- -- -- -- Standard Curve: Linear (1/x weighted) Intercept = 927.09 Slope = 169.602 Coef. OfDet. = 0.999069 Total Solids <%) - 46.94 46.94 - - Analyte Found (ppb) = [analyte found (ppt) x volume extracted (0.04 L)j / sample weight (5 g) Analyte Found (ppb) dry weight = analyte found (ppb) x (100% / total solids (%)) CS = Calibration standard C = Control sample S = Sample LF = Lab fortified sample FF = Field fortified sample LCS = Laboratory Control Spike CK = Check Standard ND = Not detected - Response between 0 and 25 ppt NQ = Not quantifiable = Response between 25 ppt and LOQ (50 ppt) Analyte Found (ppb) Dry Weight - 9370 9310 - - Spreadsheet prepared by:. 000252 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number: L35195 Matrix: Sludge Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No. 3 ^ Time OffiO0 ______ Date 10 O*'}) 0 3 ______ Initials_ CLIENT SAM PLE ID EXYGEN ID NUMBER W EIG H T (g) FO R T IFIC A T IO N (ng) na Reagent Blank _ : ' na Reagenl Spk A _ 2.0 na Reagent Spk B 20.0 n DAI-092503-NW-01 L35195-1 Spk C 5.0 20000.0 - -_ - - __ - - __ - - _ - _ __ -- _ - It : fr i - - __ __ - _ __ -_ fi< - __ _. _ _ _ __ - - -- Spiking Solution Used Volume Used for Spiking .Initial/Date n Reagent Spk A F092203-5 (10 ng/mL) 200 pL (200 pL micropipet) M r ' / idol 6 t: Reagent Spk B F092203-4 (100 ng/mL) 200 pL (200 pL micropipet) L35195-1 SpkC _ F092203-1 (100000 ng/mL) _ 200 pL (200 pL micropipet) _ U _' __ _ _ n- _ __ -- -- All samples were weighed on balance No. Time CR3>0______ Date 10 01 0 3 %Initials After weighing samples were returned to refrigerator No. ^ 2 - f, *i Time \ \ 0 Q Date l p |C ^ i 0 3 Initials & C o m m e n ts: 2 0 0 |JL o f 2 5 0 m g /m L s o d iu m th io s u lfa te w as a d d e d to a ll sa m p le s b e fo re s p ik in g . In itia ls /D a te :. -\&1c r 1d 3 Analysis Summary; DataSet: i 0 0 ^ 0 3 ^ n D ata Set: ~ l Data Set: Initials/Date: Initials/Date: Initials/Date: W : / |o |io te ~/ ~ /. Set extraction/analvsis data verified bv: O p ] f ^ Date: July 26, 2001/1 _ 000253 '`J ] r ^ i "1 1 CH 3058 Research D rive Phone: 814-272-1039 State College, P A 16801 F a x :814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L35195 MATRIX: Sludge METHOD: ExM-023-014 $$ ANALYTES: PFOA PROTOCOL NUMBER: NA Client ID Exygen ID STEP STEP STEP STEP STEP 12 3 4 5 na Reagent Blank na na -DAI-092503-NW-01 - Reagent Spk A Reagent Spk B -L35195-1 SpkC - >/ -- -- --- _-i --z _ j \J - --- -- \-L - --- - - --- - - - - - - - -- - - ---- - - ---- - - ---- - - ---- - - *Initials/Date - --- - --- --- --- &- 4 STEP 1: Add 5mL of methanol and shake by hand for ~1 minute STEP 2: Bring up to 40 mL with hypercarb filtered type I water STEP 3: Centrifuge for 10 minutes a t -3000 rpm ,. , . STEP 4: Filter through-glass acrodisc - SAMP<Xi<AMlEk. W y iq ^ l l<2> STEP 5: SPE column clean up STEP 6: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP 7: LC/MS/MS analysis STEP 8: LC/MS/MS reanalysis. - @3 - - STEP Dilutions STEP Dilutions STEP 6 (mL/mL) 7 (mL/mL) 8 --- - --- -- \ -V - V- -- -- -- --- -- --- -- --- - - - -- -- --- -- --- - --- - - - -- -- --- - - --- -- - -- -- --- -- --- -- --- -- l o f f i a sMe _z__ Reagents/ Materials Methanol C18 SPE TypeI Water . _ - _ - Initials/Date . . - Lot# to lto lo NA _ _ _ _ J H ilD '" 0 1 {ft 0 5 -_ -_ HPLC Methanol 4 5 1 U ttz io Ammonium Acetate -Type I water NA Initials/Date d lo f e *Initials and date under each step indicates the personnel that performed this step. $$ Method of Analysis for the Determination of Perfluorooctanesulfonate (PFOS) and Pentadecafluorooctanoic Acid (PFOA) in Soil COMMENTS: Final extracts stored in refrigerator Initials: t y - Date: July 19, 2001/4 000254 PREPARATION OF EXTRACTED CALIBRATION STANDARDS Protocol No.: None Method No.: 01M-008-046* Exygen Study No.: NA Analytes: PFOA Matrix: Type TWater* Sample Vol: 40 mT. Sponsor Sample ID NA Exygen Sample ID 0106020 Sample Description Type I WaterA Fort Solution ED - Fort. Soin. Cone. fns/mL) - Fort. Volume fuL) - Micropipet used (ML) Fort. Level (ppt) - Final Solution ID #** X C 100703-0 Reagents/ Materials Methanol Lot# 4 ^232-0 NA 0106020 Type I WaterA F092203-5 10 100 200 25 XC100703-1 C18 SPE U i3 \(? 7 B 2 - NA 0106020 Type I WaterA F092203-5 10 200 200 50 XC100703-2 Type I Water NA NA 0106020 Type I WaterA F092203-5 10 400 200 100 XC100703-3 _ _ NA 0106020 Type I WaterA F092203-4 100 100 200 250 X C 1 0 0 703-4 _ _ NA 0106020 Type I WaterA F092203-4 100 200 200 500 XC100703-5 - _ NA 0106020 Type I WaterA F092203-4 100 400 200 1000 XC100703-6 - - - - _- - - - - - - .- - Vertical arrows in a column indicate identical values. - --- - Initials/Date: d **This m ust be a unique number. Use this system: Extracted Calibration Soln ID #: XCM M DDYY-0,1,2,3. etc. Samples removed froig 'feMgeratfflVfreezer # 3 * 2 - Time: 0& 55~ Initials/Date: I jg | ot| o3 40 mL of each sample measured using a .J 2 L _ _mL graduated cylinder. After measuring, samples returned to fefiigerato^ / freezer # Time: Initials/Date:_ Initials/Date: 10)0-7/03 lolcnloa Samples fortified: Initials/Date: jh i s / j o k i l Q 3 SPE clean-up: Initials/Date: Final volume adjusted to 5 mL: Initials/Date: Extracts placed in refrigerator # Initials/Date: STANDARD EXPIRATION DATE: 10/21/03 Comments: AThis type I water has been filtered through a hypercarb filter * Method of Analysis for the Determination of Ammonium Perfluorooctanoate (APFO) in Water. 000255 July 10, 2001/0 in i n Masslynx - Sample List Sample List: C:\MASSLYNX\Fluoroche ns.PRO\SampleDB\100903B Daikin.spl Printed: Fri Oct 10 09:05:52 2003 \J Vial File Name LIMS ID Client ID Sample Description 1 1 100903B-4001 -- 2 2 100903B-4002 -- 3 3 100903B-4003 -- 4 4 100903B-4004 -- 5 5 100903B-4005 -- 6 6 100903B-4006 -- 7 7 100903B-4007 -- 8 92 100903B-4008 -- 9 21 100903B-4009 -- 10 22 100903B-4010 -- 11 23 100903B-4011 -- 12 24 100903B-4012 -- 13 25 100903B-4013 -- 14 26 100903B-4014 -- 15 2 100903B-4015 -- 16 3 100903B-4016 -- 17 4 100903B-4017 -- 18 5 100903B-4018 -- 19 6 100903B-4019 -- 20 7 100903B-4020 -- XC100703-0, 0 ng/L standard XC100703-1,25 ng/L standard XC100703-2, 50 ng/L standard XC100703-3,100 ng/L standard XC100703-4,250 n g /L s ta n d a r d XC100703-5, 500 ng/L standard XC100703-6,1000 ng/L standard Methanol Wash Reagent Blank Reagent Spk A, 50 ng/L Reagent Spk B, 500 ng/L L35195-1 Spk C, 500000 ng/L, DF; L35195-1, DF=10000 L35195-1 Rep, DF=10000 XC100703-1, 25 ng/L standard XC100703-2, 50 ng/L standard XC100703-3,100 ng/L standard XC100703-4, 250 ng/L standard XC100703-5, 500 ng/L standard XC100703-6, 1000 ng/L standard 000256 Exygenstudy no. Lefts' Page Position: ( 1, 1) Matrix Sample Type Cone (ng/L) Cone B Cone C Test ID DF ___ -- -- -- -- -- -- -- -- -- -- =10000 -- -- -- -- -- -- -- -- Blank Standard Standard Standard Standard Standard Standard Blank Blank QC QC QC Analyte Analyte Standard Standard Standard Standard Standard Standard 0 25 50 100 250 500 1000 -- -- 50 500 500000 -- -- 25 50 100 250 500 1000 -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- __ 0 --0 --0 --0 0 --0 --0 0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 1 1 1 1 1 1 1 1 1 1 1 10000 10000 10000 1 1 1 1 1 1 |'TPSrl*Rj :o Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochems.PRO\SampleDB\100903B Daikin.spl Printed: Fri Oct 10 09:05:52 2003 \h D ______________________ MS Method HPLC Method MS Tune File Inj Volume (pL) 1 008 PFOA 2 008 PFOA 3 008 PFOA 4 008 PFOA 5 008 PFOA 6 008 PFOA 7 008 PFOA 8 008 PFOA 9 008 PFOA 10 008 PFOA 11 008 PFOA 12 008 PFOA 13 008 PFOA 14 008 PFOA 15 008 PFOA 16 008 PFOA 17 008 PFOA 18 008 PFOA 19 008 PFOA 20 008 PFOA water water water water water water water water water water water water water water water water water water water water PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 000257 T Exygen STUDY N O . L 3 S - M S ih i ::t :i Page 2 Page Position: (2,1 ) t n LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: N A Exygen Study No: L35195 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #7) 4 Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 H Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Quat Pump HP Vacuum Degasser HP Autosampler HP Column Oven n HPLC Column: Genesis C-8, 5 cm x 2.1 mm i.d. x 4 (i (Exygen ID:MA10327) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) : 2 mM Ammonium Acetate in Type I Water Mobile Phase (B) : Methanol Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 n- NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. All Handwritten Peak ID 's by: N fn V1 ( n FT, t: ' f- F*""! Lj 000258 Scanning Method Report Method: C:\MASSLYNX\FLUOROCHEMS.PRO\ACQUDB\OO8 PFOA Last Modified: Thu Oct 02 14:56:38 2003 Printed: Fri Oct 10 09:06:00 2003 Solvent Delay ( mins ) : 0.00 Function M R M of 1 Mass Pair ( ESP- ) Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 8.00 1 Dwell (Secs) Coll Energy (eV) cone ( V ) k ii 1 413.00 369.00 0.20 10 10 Page 1 jpmq. 'L * 'I ' .fT fc \ I" fi ! fo 000259 Method Report Method File: P Last Modified Printed C :\MAS SLYM2\FLMS.PRO\ACQUDB\water Friday, October 10, 2003 01:35:39 Friday, October 10, 2003 09:06:06 f s HP1100 LC Pump Initial Conditions I -1 ' 1 Solvents A% B% C% D% 60.0 40.0 0.0 0.0 ; Flow (ml/min) ; ' StopTime (mins) *" " Min Pressure (bar) Max Pressure (bar) Pp Oven Temperature Left(C) Oven Temperature Right (C) 0.300 15.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable FT*. ^ " The gradient Timetable contains 10 entries which are : ti Time A% B% C% ,*** 0.00 60.0 40.0 0.0 ii. 0.40 60.0 40.0 0.0 ; 1.00 10.0 90.0 0.0 v 7.00 10.0 90.0 0.0 rilrf 97.-0500 0.0 0.0 100.0 100.0 0.0 0.0 i! 9.50 60.0 40.0 0.0 -!' 13.5 0 60.0 40.0 0.0 14.00 60.0 40.0 0.0 jp* 15.00 60.0 40.0 0.0 i f HP1100 LC Pump External Event Timetable D% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 ;, The Timetable contains 4 entries which are : Time pf. Initial 0.00 s', r, 0.10 8.00 Column Switch Contactl Off Off Off On Off Off Off Off Contact2 Off Off On Off . Contact3 Off Off Off Off . . ................................. - ! HP1100 Autosampler Initial Conditions Draw Speed pp. Eject Speed (pl/min) I Draw Position (mm) 1 i Stop Time (mins) Injection Volume (xl) Vial Number 200.0 200 0.10 15.00 15.0 16 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 0.300 Contact4 Off Off Off Off Page 1 Pressure 400 400 400 400 400 400 400 400 400 400 ?T- n 000260 Tuning Method Report Method: C :\MASSLYNX\FLUOROCHEMS .PRO\ACQUDB\PFOA TUNE Printed: Fri Oct 10 09:06:12 2003 Page 1 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 10 0.0 0.0 0.0 100 300 -2.93 -10 99 311 Pressures Analyser Vacuum Gas Cell Rdbk OFF 4 .Oe-3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set Rdbk 14.0 14.0 1.0 -2 10 2 14.0 14.0 2.0 700 8 9 11 -696 Rdbk 130.3 ' 723.4 000261 Quantify Calibration Report Study No. :L35195, Set No.:100903B, Ext .Date: 10/09/03, Analyst-.K.Risha Calibration: P :\Data\LCMSMS7\Masslynx\Fluorochems.PRO\CurveDB\100903B Daikin Last modified: Mon Oct 13 07:26:54 2003 Printed: Mon Oct 13 07:30:07 2003 Page 1 Exygen Research, 3058 Research Drive, State College, PA 16801 000262 Quantify Sample Report Study No.:L35195, Set Mo.:100903B, Ext.Date:10/09/03, Analyst:K. Risha Sample List: Last modified: Method: Last modified: Job Code: Printed: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903B Daikin Hon Oct 13 07:26:44 2003 P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Fri Oct 03 12:53:47 2003 M o n Oct 13 07:30:09 2003 In itia ls . D a te . R u n # \Q P X 5 P r^ 0 .L T o Page 1 Marne: 100903B-4001 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000263 Quantify Sample Report Study No.:L35195, Set No.:100903b , Ext.Date:10/09/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903B Daikin Last modified: H o n Oct 13 07:26:44 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: M o n Oct 13 07:30:09 2003 Page 2 Name: 100903B-4002 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000264 Quantify Sample Report Study No.:L35195, Set No.:100903B, Ext.Date:10/09/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903B Daikin Last modified: Mon Oct 13 07:26:44 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Mon Oct 13 07:30:09 2003 Page 3 Name: 100903B-4003 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000265 Quantify Sample Report Study No.:L35195, Set No.:100903B, Ext-Date:10/09/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903B Daikin Last modified: Mon Oct 13 07:26:44 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Mon Oct 13 07:30:09 2003 Rage 4 Name: 100903B-4004 Text : 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000266 Quantify Sample Report Study No.:L35195, Set No.:100903B, Ext.Date:10/09/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903B Daifcin Last modified: Mon Oct 13 07:26:44 2003 Method: P :\Data\LCMSMS7 \Masslynx\Fluorochems. PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Mon Oct 13 07:30:09 2003 Page 5 Name: 100903B-4005 Text: 1 : PFOA XC100703-4, 250 ng/L standard 100903B -4005 Sm (Mn, 2x2) 100- %: 5.20 _ 40654~| I 1 10-0ct-2003 11:03:30 LC/MS/MS #7 M RM of 1 Channel ES413 >369 3.97e5 Area 0 : /V,".,", . 1 1 11 11I lI r1 1 rf ~7' T-j `1 I1 I1 -II--rI--1I--rI rI' iI iI iI iI iI i1"1Ir -nn rnrTr rnr Tr vV |TT- iH-, T Hr- r 1 ,' , 1I ' ' ' MrTTTjTI iI"l1- n '~-rr 'i '' II 1 '' '1 1' !1 1 '' I I TIim e 1.00 2.00 3.00 4.00 5.00 6 .0 0 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000287 Quantify Sample Report Study No.:L35195, Set No.:100903B, Ext.Date:10/09/03, AnalystiK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903B Daikin Last modified: Mon Oct 13 07:26:44 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Mon Oct 13 07:30:09 2003 Page 6 Name: 100903B-4006 Text: 1 : PFOA XC100703-5, 500 ng/L standard 100903B-4006 Sm (Mn, 2x2) 100-) - %- 5.21 868731 1 1 10-0ct-2003 11:20:13 LC/MS/MS #7 M R M of 1 Channel ES413 >369 8.34e5 Area 0: 1f^v"! r-| I I I I I I--I fi Ji i --I--1 -j..r11 "T...1"1 --T""i--i--r-]--i--i--i--r i"V'T'T']--J--11T 1 1"11i`"T--|' 1^^^*** 11 1"1 1 T p T p r i r \ 1i"j'i \"'\ $ \ TimO 1.00 2.00 3^00________ 4 .0 0 5.00 6.00 7 .0 0 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000268 *' . Quantify Sample Report * - Study No.:L35195, Set No.:100903B, Ext.Dates 10/09/03, AnalystsK.Risha p Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903B Daikin I ! Last modified: M o n Oct 13 07:26:44 2003 1 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 p Job Code: Printed: M o n Oct 13 07:30:09 2003*1 Page 7 Marne: 100903B-4007 Text: 1 : PFOA XC100703-6,1000 ng/L standard 10 0903B -4007 Sm (M n, 2x2) 100n %: 10-0ct-2003 11:37:04 LC/MS/MS #7 M R M of 1 Channel ES413 > 3 69 1.56e6 Area # 0 rr-r i j t ' i i i | i i i t | i i i i |- r - i i-r~| i i i i |i i ' i 1.00 2.00 3.00 4.00 ' i t i i t I IT i i I i I i T im e 7 .0 0 8.00 f fn. .) Exygen Research, 3058 Research Drive, State College, PA 16801 p 000269 r-> f I Quantify Sample Report ` Study No. :L35195, Set No.:100903B, Ext.Date:10/09/03, Analyst:K.Risha r~>: Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903B Daikin f \ Last modified: Mon Oct 13 07:26:44 2003 i-j Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 f| Job C o d e : 1 Printed: Mon Oct 13 07:30:09 2003 I- ; * Name: 100903B-4008 Text: Rage 8 i| I! fA S i' l' IM fI n Exygen Research, 3058 Research Dr.ive, Stat1e, College, P A 16801 j -i 000270 in . - , ; Quantify Sample Report ' * Study No.:L35195, Set No.:100903B, Ext.Date:10/09/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903B Daikin Last modified: Mon Oct 13 07:26:44 2003 Method: P :\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 n Job Code: Printed: Mon Oct 13 07:30:09 2003 R - Name: 100903B-4009 Text : P 1 : PFOA Page 9 n ns. tI n t Exygen Research, 3058 Research Drive, State College, PA 16801 000271 Quantify Sample Report Study No.:L35195, Set No.:100903B, Ext.Date:10/09/03, Analyst:K.Risha Page 10 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903B Daikin f ' Last modified: Hon Oct 13 07:26:44 2003 ; Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 JH Job Code: r* Printed: M o n Oct 13 07:30:09 2003 r, ; , : ; Name: 100903B-4010 Text: 1 : PFOA - * 1I ; ! i r*. i r Exygen Research, 3058 Research Drive, State College, PA 16801 000272 ' n. i \ Quantify Sample Report 1 Study No. :L35195, Set No.:100903B, Ext.Date:10/09/03, Analyst:K.Risha Page 11 ^ Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903B Daikin J ! Last modified: M o n Oct 13 07:26:44 2003 5 ' Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 r 1 Job Code: * ,i - Printed: Mon Oct 13 07:30:09 2003 Marne: 100903B-4011 Text: 1 : PFOA n 11 it- ; Exygen Research, 3058 Research Drive, State College, PA 16801 000273 Quantify Sample Report Study No.:L35195, Set No.:100903B, Ext.Date:10/09/03, Analyst:K.Risha Page 12 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903B Daikin Last modified: Mon Oct 13 07:26:44 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Mon Oct 13 07:30:09 2003 Name: 100903B-4012 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000274 Quantify Sample Report Study No.:L35195, Set No.:100903B, Ext.Date:10/09/03, Analyst:K.Risha Page 13 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903B Daikin Last modified: Mon Oct 13 07:26:44 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Mon Oct 13 07:30:09 2003 Name: 100903B-4013 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000275 Quantify Sample Report Study No.:L35195, Set No.:100903B, Ext.Date:10/09/03, Analyst:K.Risha Page 14 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903B Daikin Last modified: Mon Oct 13 07:26:44 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Mon Oct 13 07:30:09 2003 Name: 100903B-4014 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000276 n I! H Quantify Sample Report ' 1 Study No.:L35195, Set No.:100903B, Ext.Date:10/09/03/ Analyst:K.Risha Page 15 n Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903B Daikin I Last modified: Mon Oct 13 07:26:44 2003 ' Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Fri Oct 03 12:53:47 2003 jT': Job Code : f: . Printed: Mon Oct 13 07:30:09 2003 n1 \ Name: 100903B-4015 Text: 1 : PFOA n n I; f! ; tr -' 1 jn - r-> f! Exygen Research, 3058 Research Drive, State College, PA 16801 000277 n t- I } Quantify Sanale Report f Study No.:L35195, Set No.:100903B, Ext.Date:10/09/03, Analyst:K.Risha Page 16 H Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903B Daikin l , Last modified: Mo n Oct 13 07:26:44 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 n Job Code: Printed: M o n Oct 13 07:30:09 2003 Name: 100903B-4016 Text: H *j. < t r " P ! * if f '" Exygen Research, 3058 Research Drive, State College, PA 16801 00027S *n. ? ' n f Quantify Sample Report r Study No-:L35195, Set No.:100903B, Ext.Date:10/09/03, Analyst:K.R i sha Page 17 m Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903B Daikin Last modified: Non Oct 13 07:26:44 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 jm Job Code: Printed: M o n Oct 13 07:30:09 2003 t ; Name: 100903B-4017 Text: 1 : PFOA n t H n jn Exygen Research, 3058 Research Drive, State College, PA 16801 000279 Quantify Sample Report Study No.:L35195, Set No.:100903B, Ext.Date:10/09/03, Analyst:K.Risha Page 18 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903B Daikin Last modified: Mon Oct 13 07:26:44 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Mon Oct 13 07:30:09 2003 Name: 100903B-4018 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000280 Quantify Sample Report Study No.:L35195, Set No.:100903B, Ext.Date:10/09/03, Analyst:K.Risha Page 19 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\100903B Daikin Last modified: Hon Oct 13 07:26:44 2003 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 Job Code: Printed: Mon Oct 13 07:30:09 2003 Name: 100903B-4019 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000281 n * ] Quantify Sample Report - Study No.:L35195, Set No.:100903B, Ext.Date:10/09/03, Analyst :K.Risha Page 20 pi Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\100903B Daikin || Last modified: M o n Oct 13 07:26:44 2003 ! Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Fri Oct 03 12:53:47 2003 f"l Job Code: h * Printed: M o n Oct 13 07:30:09 2003 n '' i Name: 100903B-4020 Text: : 1' ---------------------------- 1 : PFOA XC100703-6,1000 ng/L standard (T"! j 100903B -4020 Sm (Mn, 2x2) i 100~] !f" ; %: 10-0ct-2003 15:15:11 LC/MS/MS #7 M RM of 1 Channel ES413 > 3 69 1.64e6 Area k. ki 0 ~ ^ r'i I t I ) I"i I | r I I-1 ) I r n ..p t i i |"i u i | i 1.00 2.00 3.00 ~r~r"r~r~i.1y 1 1 I : I f r I I I I T im e 6 .0 0 7.00 8.00 n Ij fr * h: Exygen Research, 3058 Research Drive, State College, PA 16801 000282