Document 44D9Za9p9oD96xxrzDY581851

Proven Results. A R A 3 .& _ / 7 /4 n t. Analytical Report i- i Flyorochemicai Characterization of Water Samples n Daikin America, Inc. ti Exygen Research Laboratory Report No. L0001562 1 Testing Laboratory n Exygen Research , 3058 Research Drive State College, PA 16801 n Requester r-o tXTJ Randy Roussel 33 Daikin America, Inc. "O o p o PO "O m Ii PO Box 2252 r o --D\ rO-^ Decatur, AL 35609 T> "^ c O pn rc o o ro 000419 3058 Research Drive State College, PA 16801, USA PAGE f: 800.281.3219 F: 814.272.1019 exygen.com 1 Introduction T','': /< : Results are reported for the analysis of water samples received by Exygen Research (Exygen) from Daikin America. The Exygen study number assigned to the project is L0001562. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) was requested for all samples. A total of 2 samples were received for analysis. The samples were prepared and analyzed by LC/MS/MS for the following list of fluorochemicals: Table 1: Target Analysis Compound Name Perfluorooctanoic Acid Acronym C8 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. 2 Sample Receipt .. ... ; ^ The samples were submitted in plastic containers. All samples were cooled to 4C from time of collection to receipt at Exygen Research. Samples were stored at 4C from receipt at Exygen Research until analysis. Samples were collected on 1/2/04 and 1/6/04. Chain-of-custody information is presented in Attachment C. 3 Holding Times Field and laboratory spikes of these fluorochemicals have shown stability for periods greater than 90 days. Samples were analyzed within 30 days of receipt. 4 Methods - Analytical and Preparatory 4.1 LC/MS/MS 4.1.1 Sample Preparation for LC/MS/MS Analysis Samples were initially treated with 200 uL of 250 mg/L sodium thiosulfate solution to remove residual chlorine. Solid phase extraction (SPE) was used to prepare the samples for LC/MS/MS analysis. A forty-milliliter portion of sample was used for analysis. The samples were transferred to a C18 SPE cartridge. The cartridge was eluted with 5 mL of 100% methanol. This treatment resulted in an eight-fold concentration of the diluted samples prior to analysis. PAGE2 OF5 000420 4.1.2 Sample Analysis by LC/MS/MS 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 HPLC separation, ES/MS provides a rapid and accurate means for analyzing a wide range of organic compounds, including fluorochemicals. Electrospray is generally operated at relatively mild temperatures; molecules are ionized, fragmented, and detected. Ions characteristic of known fluorochemicals are observed and quantitated against standards. A Hewlett-Packard HP1100 HPLC system coupled to a Micromass Ultima MS/MS was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Samples were extracted on 1/8/04 and analyzed on 1/12/04 and 1/13/04. Raw analytical data is provided in Attachment D. 5 Analysis ' Y "YYY'' Y'Y'YKY '/V- YY- " '. 5.1 Calibration A 7-point calibration curve was analyzed at the beginning and end of the analytical sequence for the compounds of interest. The calibration points were prepared at 0, 25, 50, 100, 250, 500, and 1000 ng/L (ppt) for LC/MS/MS 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) were determined. A calibration curve is acceptable if r >.0.985 (r2> 0.970). Calibration standards are prepared using the same SPE procedure used for samples. Calibration check standards were analyzed periodically (every three to five sample injections) throughout the analysis sequence. Compliance is obtained if the standard analyte concentrations are within +/-20% of the actual value. All calibration criteria were met for this analysis. 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 the low-level calibration standard. For these samples, the extraction blanks were compliant. Instrument blanks in the form of clean methanol solvent were 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. 5.3 Surrogates Surrogate spikes are not a component of the LC/MS/MS analytical methods. 5.4 Matrix Spikes A matrix spike was prepared for sample DSN001. Matrix spike recoveries are given in Attachment B. PAGE3 OF5 0 0 0 4 2 1 5.5 Duplicates Sample DSN001 was analyzed in duplicate. The duplicate results are included with the sample results in Attachment A. 5.6 Laboratory Control Samples For LC/MS/MS analyses, Milliq water 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 units of parts per billion (ppb) (ng/mL). 7 Data/Samp/e Retention Samples are disposed of one month after the report is issued unless otherwise specified. All electronic data is archived on retrievable media and hard copy reports are stored in data folders maintained by Exygen. 8 Attachments 8.1 Attachment A: Results 8.2 Attachment B: Matrix Spike Recoveries 8.3 Attachment C: Chain of Custody 8.4 Attachment D: Raw Analytical Data PAG E4 OF5 000422 P *" f' i--- 9 Signatures if .tf " ^ l X c -- X L Paul Connolly, Team Leader - LC^|S #***> a L m fL U c C /J o h n M. Flaherty, Vice President f! t- ` Other Lab Members Contributing to Data * * Karen Risha 1i t i*** i U. J /QH Date /fa h Date #i f PAGE 5 OF5 000423 Analytical ^ p Ii Report I** Proven Results. *! Summary of PFOA in Water Samples n Sample ID DSN001 DSN001* Rinse Blank Analyte Found (ng/mL) PFOA 1260 1310 1-80 I! ` Laboratory Duplicate fft*"1\ v. ki n i? i. ; H i. VJ l Li f] LJ 000424 ^ L 0.3505e8 Research Drive ^ ^ L S tSatatte College, PA 16801, USA J: 814.272.1039 V -i F: 814.231.1580 exygen.com STANDARD T ER M S AND CONDITIONS Services provided by Exygen Research are limited to the terms and conditions stated herein, unless otherwise agreed to in a formal contract. CONFIDENTIALITY---Exygen 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. The client agrees not to use Exygen's name and/or data in any manner that might cause harm to Exygen's reputation or business. Approval must be obtained, in writing, before Exygen's name can be published in any way. 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ACCEPTANCE OF PURCHASE ORDER--Shis Purchase Order becomes a binding agreement, subject to the specific terms and conditions stated herein, upon Exygen's commencement o f work. 000425 Proven Results. t. Recovery Summary for PFOA in Water fmm PFOA Amount Amt Found Amount Sample Spiked in Sample Recovered Recovery Description (ng/mL) (ng/mL) (ng/mL) (%) n fi DSN001 500 ng/mL Spike 500 1260 1770 102 i] tI i\ I: :t tI r n h> n ii n H 000426 n X 3058 Research Drive State College, PA 16801, USA I I T. 800.281.3219 V F: 814.272.1019 exygen.com Phone: 814-272-1039 Fax: 814-231-1580 Login Group: L0001562 Togin m 1672 , Project: P0000449 Project Storage: ' Company Name: Daikin America Submitted By: Neal Waddell and Randy Roussel r - Login Type: Immediate Receipt of Samples i Started: T Date Start: Due Date: 01/07/2004 01/21/2004 P Received Date: 01/07/2004 i- Received By: ROBB, SHAWN Spread Sample: r~ Label: Project Title/Type: Analysis of PFOA in W ater / ROUTINE Exygen SD/Pl: RISHA, KAREN Login Notes: ' Conform Notes: Conform COC Sample: Conform COC: Conform Sample: Conform Request- Package , K0002161 Packages / Containers Mail Date / Condition Shipper /_ID 1/7/2004 10:18:42AM Package & Contents Uncompromised FEDEX 8402386190870215 Temp. Control/Temp. W et Ice 1.1 Container # 'C0018572 C0018613 Gross Weight 617.1 g 608.4 g pH Container Type 500 mi Clear Plastic 500 ml Clear Plastic Preservative NONE NONE Mfg. Lot 3232010 3232010 Miscellaneous Item Key None Description ICOC Direction / Handled By RECEIVED ROBB, SHAWN Mfg. ID 471382 471602 1 Sample ID L0001562-0001 rU O O 0 1562-0002 / Matrix LIQUID LIQUID Fraction Water Water Sample DSN001 RINSE BLANK Samples Date Sampled Date Received 01/06/2004 01/07/2004 01/02/2004 01/07/2004 Date Due 01/21/2004 01/21/2004 fr--i1/14/2004 Login, rpt Report Version: Dec 22 2003 10:44AM Page 1 of 2 000427 Instance: R0079793 R0079793 p 0 0 1 562-0001 C o n ta in e r C0018572 / 500 ml Clear Plastic / NONE f"! L0001562-0002 <--! Container l C0018613 / 500 ml Clear Plastic / NONE n * : t' P**, l- l Bottles Method Method r it * n ij m ^1/14/2004 ; ogin.rpt Report Version: Dec 22 2 0 0 3 10:44AM Page 2 of 2 000428 Instance: R0079793 R0079793 Number of Containers 000429 F RESEARCH PROJECT INFORMATION Client (name & address): flcrJk 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 Page___j_ of _l_ ANALYSES REQUESTED Project Manager (Name & E-mail Addre): _h?>Jac(f --A A / r -------------------- Project Name: Phone: (z 5 3 o A Too /Ao4 s jJ ^ y Fax: v y RO. #: / / >o 3 o ^ Z i 3 o Sampler: 77,J o / Quotation #: J/ Please fill out this form completely to ensure correct analysis and proper handling of your samples. 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Extraction Date: Analyzed on: 010804A Karen Risha LC/MS/MS Unit # 6 01/08/04 01/12-13/04 Exygen ED XC123003-0 XC123003-1 XC123003-2 XC123003-3 XC123003-4 XC123003-5 XC123003-6 Methanol Wash 0106020 Control L1562-2 0106020 Spk A 0106020 Spk B XC123003-1 XC123003-2 XC123003-3 L1562-1 SpkC L1562-1 L1562-1 Rep XC123003-4 XC123003-5 XC123003-6 Sponsor ED -' NA Rinse Blank NA NA - DSN001 DSN001 DSN001 - - Sample Code 'c CS CS CS CS CS CS C C C LCS LCS CS CS CS LF S 'S CS CS CS Run No. 010804A-501 010804A-502 010804A-503 010804A-504 010804A-S05 010804A-506 010804A-507 010804A-508 01804A-509 010804A-510 010804A-511 010804A-512 010804A-513 010804A-514 010804A-515 010804A-516 010804A-517 010804A-518 010804A-519 010804A-520 010804A-521 PFOA Found (ng/L) = (peak area - intercept) / slope x DF Recovery (%) = [PFOA 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 1 2000 2000 2000 - - x 100 Peak Area 589 10618 21734 43739 101002 203985 385342 1508 1161 629804 25626 206531 11980 23174 45056 342570 245894 254997 105210 200209 363438 PFOA Found (ng/L) - - ND * Amount PFOA Added (ng/L) - - - - - Recovery m - - - - -' - 58.9 530 1770000 1260000 1310000 - 50 500 - 500000 - 118 106 - 102 - --- Standard Curve : Linear (1/x weighted) Intercept = 2988.44 Slope = 384.319 Coef. OfDet. = 0.996236 CS = Calibration standard C = Control sample S =s Sample Sample requires dilution. See data set 010804AR. 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: F* 'j? 1 Hi i r 000431  !' ' n 3058 Research Drive Phone: 814-272-1039 ! I1 RESEARCH State College, PA 16801 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number: L1562 Matrix: Water Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No. .5 2 Time M O O_______ Date Oil CPi j AW Initials CjFJE CLIENT SAMPLE ID EXYGEN ID NUMBER VOLUM E (mL) FORTIFICATION (ng) na 0106020 Control 40.0 - na 0106020 Spk A 40.0 2.0 na 0106020 Spk B 40.0 20.0 DSN001 L1562-1 S pkC 40.0 20000.0 bli i DSN001 L1562-1 40.0 - DSN001 L1562-1 Rep 40.0 - Rinse Blank L I562-2 40.0 - _ - -- - - -- - fi _ - -- -- - - -- - - -- - - -- _ - -- _ Li . - - - - - -- -- - - -- - - -- 0106020 Spk A 0106020 Spk B L I562-1 SpkC _ _ _ Spiking Solution Used F120903-5 (10 ng/mL) F I20903-4 (100 ng/mL) F120903-1 (100000 ng/mL) - . _ -- All samples were measured: Time 1030________ Date Q\ r>Aj&4__ _ Volume Used for Spiking 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) - - - - Initial/Date Vbij /t>t t if b /Oil 'o - Ls - - - - Initials t! 1 000432 J "1 "ZI 1 3058 Research Drive State College, PA 16801 _1 Phone: 814-272-1039 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L1562 MATRIX: Water METHOD: ANALYTES: PFOA PROTOCOL NUMBER: NA Client ID na na na DSN001 DSN001 DSN001 Rinse Blank - ExygenID 0106020 Control 0106020 Spk A 0106020 Spk B L I562-1 Spk C L1562-1 L1562-1 Rep L1562-2 - STEP 1 \ 1/ - - STEP 2 \v - - - - -- - - -- - - -- - - -- - - -- - - -- - - -- - - -- - - -- - - -- - - -- - - -- - - -- *In itia ls/D a te O fe o r - Oijo&JoM oi f t M STEP1: 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) -- -- - - - STEP 3 Dilutions (mL/mL) - -- /-- { % /(0 - -- -- -- STEP 4 -- -- -- - - - - - Reagents/ Materials Methanol C18 SPE Type Water _ _ _ _ - In itia ls /D a te - Lot# V M IpT % . NA _ _ _ _ _ - o i lo H - --- - -_ . _ - --- _ _ - --- _ _ - --- _ _ - -- - _ _ - --- . _ - --- HPLC - --- Methanol - - - - AmmoniumAcetate \I 4 ^ - - - - Type I water NA ____r nL- - - - i'n'Kf i-2 0 0 0 OPh) 12lriM [) ^ & I o4 In itia ls/D a te o ilf c _ .. . KlLDTlhO'T \ . |_i , . (01 jlSjo4-! O 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 2>2- Initials: C&- Date: 01 DP,j&L July 19, 2001/4 000433 w-. 3 ail T y" 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 PREPARATION OF EXTRACTED CALIBRATION STANDARDS Exygen STUDYNO L15(?2~ I Protocol No.: None Exygen Study No.: NA Method No.: 01M-008-046* Analytes: PFOA Matrix: Type I WaterA Sample Vol: 40 mL Sponsor Sample ID NA NA Exygep Sample .ED 0106020 0106020 Sample Description Type I WaterA Type I WaterA' Fort. Solution ED - F 120903-5 Fort. Soin. Cone. (ng/mL) ' 10 Fort. Volume (uL) - 100 Micropipet used (uL) - 200 Fort. Level (ppt) - 25 Final Solution ED#** XC123003-0 XC123003-1 Reagents/ Materials Methanol C18 SPE Lot# 43308345 V tklB l NA 0106020 Type I WaterA F120903-5 ' 10 200 200 50 XC123003-2 Type I Water NA NA 0106020 Type I WaterA F 120903-5 10 400 200 100 XC123003-3 - - NA 0106020 Type I WaterA F120903-4 100 100 200 250 XC123003-4 - - NA 0106020 Type I WaterA F120903-4 100 200 200 500 XC 123003-5 - - NA 0106020 Type I WaterA F120903-4 100 400 200 1000 XC123003-6 NA 0106020 Type I WaterA F102703-2 100 100 200 250 XC123003-7 - r - - - - - - - - - Initials/Date: lz|3 o lo 3 > Vertical arrows in a column indicate identical values. **This must be a unique number. Use this system: Extracted Calibration Soln ID #: XCMMDDYY-0,1,2, Samples removed from (fefrigeratpr-y freezer # _ Time: 40 mL of each sample measured using a S O _mL graduated cylinder. After measuring, samples returned torefrigeratpf / freezer #. Samples fortified: SPE clean-up: Final volume adjusted to 5 mL: Extracts placed in refrigerator # 3 2 - Initials/Date:. P 1 l*|3c .03 Initials/Date:. tL / 12-30 D3 Initials/Date:. 'ttlr / Y2, Initials/Date: / I23DD3 Initials/Date:. Initials/Date:. Initials/Date: 12 . j3 0 l h 3 ' _ [2 - |3 o| o5 T H IS IS AN EXA C T C O P Y O F T H E O R IG IN A L DO CUM ENT." DATE--1 m l STANDARD EXPIRATION DATE: 1/13/04 C om m ents: AThis type I water has been filtered through a hypercarb filter * Method of Analysis for the Determination of Ammonium Perfluorooctanoate (APFO) in Water. July 10, 2001/0 000434 Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochemip ls.PRO\SampleDB\010804A Daikin Water.spl Printed: Mon Jan 12 13:38:25 2004 Vial File Name LIMS ID Client ID Sample Description 1 1 010804A-501 XC123003-0, 0 ng/L standard 2 2 010804A-502 -- -- XC123003-1,25 ng/L standard 3 3 010804A-503 -- -- XC123003-2, 50 ng/L standard 4 4 010804A-504 -- -- XC123003-3,100 ng/L standard 5 5 010804A-505 -- -- XC123003-4,250 ng/L standard 6 6 010804A-506 -- -- XC123003-5, 500 ng/L standard 7 7 010804A-507 -- -- XC123003-6,1000 ng/L standard 8 92 010804A-508 -- -- Methanol Wash 9 11 010804A-509 -- -- 0106020 Control 10 12 010804A-510 -- -- L1562-2 11 13 010804A-511 -- -- 0106020 Spk A, 50 ng/L 12 14 010804A-512 -- -- 0106020 Spk B, 500 ng/L 13 2 010804A-513 -- -- XC123003-1,25 ng/L standard 14 3 010804A-514 -- -- XC123003-2, 50 ng/L standard 15 4 010804A-515 -- -- XC123003-3,100 ng/L standard 16 15 010804A-516 -- -- L1562-1 Spk C, 500000 ng/L, DF=2000 17 16 010804A-517 -- -- L1562-1, DF=2000 18 17 010804A-518 -- -- L1562-1 Rep, DF=2000 19 5 010804A-519 -- _ _ XC123003-4, 250 ng/L standard 20 6 010804A-520 -- -- XC123003-5, 500 ng/L standard 21 7 010804A-521 -- -- XC123003-6,1000 ng/L standard 00043 tn '1 Exygen STUDY NO L - l ^ > Page 1 Page Position: (1,1) Matrix Sample Type Cone (ng/L) Cone B ConcC Test ID DF MS Method Blank 0 0___ ___ 1 PFOA -- Standard 25 -- -- 0 1 PFOA -- Standard 50 -- -- 0 1 PFOA -- Standard 100 -- -- 0 1 PFOA -- Standard 250 -- -- 0 1 PFOA -- Standard 500 -- -- 0 1 PFOA -- Standard 1000 -- -- 0 1 PFOA -- Blank -- -- -- 0 1 PFOA -- Blank -- -- -- 0 1 PFOA -- Analyte -- -- -- 0 1 PFOA -- QC 50 -- -- 0 1 PFOA -- QC 500 -- -- 0 1 PFOA -- Standard 25 -- -- 0 1 PFOA -- Standard 50 -- -- 0 1 PFOA -- Standard 100 -- -- 0 1 PFOA -- QC 500000 -- -- 0 2000 PFOA -- Analyte -- -- -- 0 2000 PFOA -- Analyte -- -- 0----- 2000 PFOA -- Standard 250 -- -- 0 1 PFOA -- Standard 500 -- -- 0 1 PFOA -- Standard 1000 -- -- 0 1 PFOA ) V ` 2> n :J i ::rri : r : i n Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochemicals.PF iCASamp Printed: Mon Jan 12 13:38:25 2004 Up Hi z IM HPLC Method MS Tune File Inj.Volijme 1 Fluorochems Fluorochems 15 2 Fluorochems Fluorochems 15 3 Fluorochems Fluorochems 15 4 Fluorochems Fluorochems 15 5 Fluorochems Fluorochems 15 6 Fluorochems Fluorochems 15 7 Fluorochems Fluorochems 15 8 Fluorochems Fluorochems 15 9 Fluorochems Fluorochems 15 10 Fluorochems Fluorochems 15 11 Fluorochems Fluorochems 15 12 Fluorochems Fluorochems 15 13 Fluorochems Fluorochems 15 14 Fluorochems Fluorochems 15 15 Fluorochems Fluorochems 15 16 Fluorochems Fluorochems 15 17 Fluorochems Fluorochems 15 18 Fluorochems Fluorochems 15 19 Fluorochems Fluorochems 15 20 Fluorochems Fluorochems 15 21 Fluorochems Fluorochems 15 ^0 0 0 Exygen study no . Page 2 Page Position: (2,1) LC/MS/MS SYSTEM AND OPERATING CONDITIONS 'I ! Sponsor Protocol No: NA Exygen Study No: L I562 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #6) 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 HP Bin Pump HP Vacuum Degasser S' J HP Autosampler HP Column Oven jf*- * HPLC Column: Genesis C-8, 5 cm x 2.1 mm i.d. x 4 p (Exygen ID: 74A) i . (JONESCHROMATOGRAPHY: Part No. FK5962E) f* Mobile Phase (A) 2 mM Ammonium Acetate in Type I Water Mobile Phase (B) Methanol t ^*t- Analyst: Karen Risha Exygen Research ife V 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 ' A J I' ' 000437 t . Scanning Method Report ^ Method: C :\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\ PFOA "fi Last Modified: Wed Mar 26 15:31:10 2003 I\ - Printed: Mon Jan 12 13:39:21 2004 I*. ____________________________________________________________________________ tLb\\\2\o Solvent Delay ( mins ) : 0.00 Analog Channel 4 : Unused j Function : 1 MRM of 1 Mass Pair ( ESP- ) Inter Channel Delay { Secs ) : j"*' Span ( Daltons ) : f Start Time ( Mins ) : v End Time ( Mins ) : Repeats : A Channel Parent Daughter j! 1 ' 1 413.00 369.00 0.03 0.00 0.00 8.00 1 Dwell 0.20 (Secs) Coll Energy (eV) 10 A Cone ( V ) 10 Page 1 ! !.. I r** }* f-*i. J \J if*** i 000438 Method Report Method File : Last Modified: Printed: C :\MASSLYNX\FLUOROCHEMICALS.PRO\ACQODB\Fluorochems Monday, January 12, 2004 13:38:45 Monday, January 12, 2004 13:39:30 Page 1 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 14.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 9 entries which are : Time 0.00 0.40 1.00 7.00 7.50 9.00 9.50 13.50 14.00 A% 60.0 60.0 10.0 10.0 0.0 0.0 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 C% 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 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 Pressure 400 400 400 400 400 400 400 400 400 HP1100 LC Pump External Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.10 7.95 8.00 Column Switch Contactl Off Off Off On Off Off Off Off Off Off Off Off Contact2 Off Off Off On Off Off Contact3 Off Off Off Off On Off Contact4 Off Off Off Off Off Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (/xl/min) Draw Position (mm) Stop Time (mins) Injection Volume (/l) Vial Number 200.0 200 0.50 14.00 15.0 7 000439 Tuning Method Report ^ Method: '! ! . Printed: C :\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\FLUOROCHEMS Mon Jan 12 13:39:50 2004 i- : i! Page 1 Dau 395.00 i--* SOURCE ( ESP- ) i\ ' Capillary Cone Hexapole 1 1 1 Aperture 1 ; Hexapole 2 Source Block Temp. Desolvation Temp. \- i ; Pressures Analyser Vacuum l : Gas Cell Set Rdbk 3.00 20 0.0 0.0 0.0 100 300 -2.93 -20 99 299 Rdbk OFF 3.5e- 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 15 2 14.0 14.0 2 .0 650 12 14 16 -647 Rdbk 127.7 755.7 fl i- ' 0 0 0 4 4 0 Quantify Calibration Report Study No.:L1562, Set No.:010804A, Ext.Date:01/08/04, Analyst:K.Risha Page 1 Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\010804A Daikin Water Last modified: Tue Jan 13 08:52:49 2004 Printed: Tue Jan 13 08:53:26 2004 Exygen Research, 3058 Research Drive, State College, PA 16801 _ 000441 Quantify Sample Report Study No.:L1562, Set No.:010804A, Ext.Date:01/08/04, Analyst:K.Risha Page 1 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804A Daikin Wate: Last modified: Tue Jan 13 08:48:53 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 i Job Code: Initials. - Printed: Tue Jan 13 08:53:27 2004 Run# * $ Name: 010804A-501 Text: l: . ti i. r4 ]**> t > l ' Exygen Research, 3058 Research Drive, State College, PA 16801 -f 000442 Quantify Sample Report Study No.:L1562, Set No.:010804A, Ext.Date:01/08/04, Analyst:K.Risha Page 2 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804A Daikin Watej Last modified: Tue Jan 13 08:48:53 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: Printed: Tue Jan 13 08:53:27 2004 Name: 010804A-502 Text: 1: C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000443 p i- < > Quantify Sample Report > Study N o . :1.1562, Set No.:010804A, Ext.Date:01/08/04, Analyst:K.Risha Rage 3 ^ Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804A Daifcin Waten I Last modified: Tue Jan 13 08:48:53 2004 k-J Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 p; Job Code: t- Printed: Tue Jan 13 08:53:27 2004 Name: 010804A-503 Text : 1: C8 Acid |i ; p t\ ' L -;- it 11 t i1 Exygen Research, 3058 Research Drive, State College, PA 16801 fM; . , . , - li ` 1 * ` 000444 ri Quantify Sample Report - ' : Study No.:L1562, Set No.:010804A, Ext.Date:01/08/04, Analyst:K. Ri sha Page 4 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804ADaikinWatej Last modified: Tue Jan 13 08:48:53 2004 i Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 p "- Job Code : 1' Printed: Tue Jan 13 08:53:27 2004 t' . ; Name: 010804A-504 Text : n f] fl '! i-l $U*-I\4, fi1 k %L n Exygen Research, 3058 Research Drive, State College, PA 16801 n i 000445 I : Quantify Sample Report * Study No.:L1562, Set No.:010804A, Ext.Date:01/08/04, Analyst:K.Risha Rage 5 1*. Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804A Daikin Wate: f Last modified: Tue Jan 13 08:48:53 2004 i J Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 pi Job Code: ?i }' Printed: Tue Jan 13 08:53:27 2004 Name: 010804A-505 Text: 1: C8 Acid XC123003-4, 250 ng/L standard n 010804A-505 Sm (Mn, 2x2) 1Ch n %: 12-Jan-2004 21:23:48 LC/MS/MS #6 MRM of 1 Channel ES5.31 413 > 36 9 6.01 e5 Area 1.00 2.00 3.00 i r "i !'"[ i.. |~i i'm| 4.00 5.00 'i '' 6.00 7.00 - r r i Time 8.00 i i, m rr ti n Exygen Research, 3058 Research Drive, State C ollege, PA 16801 *' i t\ 000446 Quantify Sample Report Study No.:L1562, Set No.:010804A, Ext.Date:01/08/04, Analyst:K.Risha Page 6 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804A Daikin Watea Last modified: Tue Jan 13 08:48:53 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 Job C o d e : Printed: Tue Jan 13 08:53:27 2004 Marne: 010804A-506 Text: 1: C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000447 n n. ' Quantify Sample Report " ' ' ' Study No. :I>1562, Set No.:010804A, Ext .Date s01/08/04, Analyst :K.Risha Page 7 f~ Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804A Daikin Wate: f Last modified: Tue Jan 13 08:48:53 2004 ; Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 r . Job Code: t: Printed: Tue Jan 13 08:53:27 2004 -- -------- -- -- I' A I : Name: 010804A-507 Text: -- ' "" -- -- -- -- ' M' rr ; I n fi n Exygen Research, 3058 Research Drive, State College, PA 16801 000448 n n 6 i Quantify Sanale Report ' ' J Study N o .:L15 62, Set No.:010804A, Ext.Date:01/08/04, Analyst:K.Risha Rage 8 f> Sample List: P:\Data\LCMSMS6\Masslynx\Fluoroohenvicals.PR0\SanipleDB\010804ADaikinWate3 I I Last modified: Tue Jan 13 08:48:53 2004 1 ' Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 fT Job Code : t3 Printed: Tue Jan 13 08:53:27 2004 r-', ; f Marne: 010804A-508 Text: ti ! FT- !: FT n, i Exygen Research, 3058 Research Drive, State College, PA 16801 000449 t --- bk--'*i n ; Quantify Sanale Report Study No. :L1562, Set No.:010804A, Ext.Date:01/08/04, Analyst-.K.Risha Page 9 f"] Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804A Daikin Wate: f ` Last modified: Tue Jan 13 08:48:53 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 P Job Code: Printed: Tue Jan 13 08:53:27 2004 Name: 010804A-509 Text : r '! /T"* i. rr *\ r*i~, hi f; 11! z--r> I ' \* Exygen Research, 3058 Research Drive, State College, PA 16801 000450 Quantify Sample Report Study No-:L1562, Set No.:010804A, Ext.Date:01/08/04, Analyst:K.Risha Page 10 f-- Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804A Daikin Wate: Last modified: Tue Jan 13 08:48:53 2004 L Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 P' Job Code: kt ' - Printed: Tue Jan 13 08:53:27 2004 Name: 010804A-510 Text: n 1: C8 Acid L1562-2 010804A-510 Sm (Mn, 2x2) 100n f; n i P I; %: 0 r i ' r "i | - r i I I | I i "I I I' I i I ' I ' [ i r 1.00 2.00 3.00 5.29 4.00 5.00 12-Jan-2004 22:42:24 LC/MS/MS #6 MRM of 1 Channel ES413 >369 3.95e6 Area i.r i .-H f-i h -ri r i Time 6.00 7.00 8.00 t- t\ I li tm 11; f l! fl - ' n t- 1 Exygen Research, 3058 Research Drive, State College, PA 16801 000451 Quantify Sample Report Study No.:L1562, Set No.:010804A, Ext.Date:01/08/04, Analyst:K.Risha Page 11 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804A Daikin Wate: Last modified: Tue Jan 13 08:48:53 2004 Method: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: Printed: Tue Jan 13 08:53:27 2004 Name: 010804A-511 Text: 1 : C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000452 P I-- Quantify Sample Report Study No.:L1562, Set No.:010804A, Ext.Date :01/08/04, Analyst:K. Ri sha Page 12 rr*.1 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804A Daikin Watej Last modified; Tue Jan 13 08:48:53 2004 Method: p:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 n Job Code: i; I; Printed: Tue Jan 13 08:53:27 2004 fi Name: 010804A-512 Text : H .t 1: C8 Acid s 0106020 Spk B, 500 ng/L 010804A-512 Sm (Mn, 2x2) 10Oi 5.31 206531 12-Jan-2004 23:13:43 LC/MS/MS #6 MRM of 1 Channel ES413 >369 1.31e6 Area 1.00 2.00 r ~ r T~ T *' I T ' 3.00 4.00 5.00 6.00 7.00 Time 8.00 P f\ - n i fT'*1, fH E li n* I Is fr I; n i . ' Exygen Research, 3058 Research Drive, State College, PA 16801 000453 Quantify Sample Report Study No.:L1562, Set No.:010804A, Ext.Date:01/08/04, Analyst:K.Risha Page 13 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804A Daikin Wates Last modified: Tue Jan 13 08:48:53 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: Printed: Tue Jan 13 08:53:27 2004 Name: 010804A-513 Text: 1: C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000454 n f Quantify Sample Report Study No.:L1562, Set No.:010804A, Ext.Date:01/08/04, Analyst:K.Risha Page 14 {*"! Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804A Daikin Wate] ; Last modified: Tue Jan 13 08:48:53 2004 I Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 p Job Code: ' Printed: Tue Jan 13 08:53:27 2004 ri II 1 Name: 010804A-514 Text: " ;~ , ': : ` 1: C8 Acid XC123003-2, 50 ng/L standard H 010804A-514 Sm (Mn, 2x2) 'f '! 100"! %: 12-Jan-2004 23:45:13 LC/MS/MS #6 5.30 MRM of 1 Channel ES413 >369 1,40e5 Area f1 0 P T 1.00 2.00 3.00 4.00 5.00 T 6.00 ^ Time 8.00 4 rnI, Exygen Research, 3058 Research Drive, State College, PA 16801 000455 n & a ri : Quantify Sample Report Study No.:L1562, Set No.:010804A, Ext.Date:01/08/04, Analyst:K.Risha Page 15 r* Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804A Daikin Wate: l Last modified: Tue Jan 13 08:48:53 2004 ! Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 ; Job Code: Printed: Tue Jan 13 08:53:27 2004 Name: 010804A-515 Text: frct p\ ;? ?!i m t\i I It n i" 1 n Exygen Research, 3058 Research Drive, State College, PA 16801 000456 r* I1 ri Quantify Sample Report Study No.:L1562, Set No.:010804A, Ext.Date:01/08/04, AnalystsK.Risha Page 16 r-, Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804A Daikin Wate: I Last modified: Tue Jan 13 08:48:53 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: : Printed: Tue Jan 13 08:53:27 2004 Name: 010804A-516 Text: 1 n H f n1 ** n Exygen Research, 3058 Research Drive, State College, PA 16801 000457 Quantify Sample Report Study No-:L1562, Set No.:010804A, Ext-Date:01/08/04, Analyst:K.Risha Page 17 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SamplePB\010804A Daikin Wate: Last modified: Tue Jan 13 08:48:53 2004 Method: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: Printed: Tue Jan 13 08:53:27 2004 Name: 010804A-517 Text: 1 : C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 0004S8 p* I Quantify Sanale Report * Study No.:L1562, Set No.:010804A, Ext.Date:01/08/04, Analyst:K.Risha Page 18 H Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804A Daikin Watea Last modified: Tue Jan 13 08:48:53 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 f-1 Job Code : 'i , Printed: Tue Jan 13 08:53:27 2004 P Name: 010804A-518 Text: P! 1: C8 Acid H h3 II l- n !I n I^ H 1 1f pi Exygen Research, 3058 Research Drive, State College, PA 16801 000459 n Quantify Sample Report I' Study No.:L1562, Set No.:010804A, Ext.Date:01/08/04, Analyst:K.Risha Page 19 m Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804A Daikin Wat^a j: Last modified: Tue Jan 13 08:48:53 2004 * Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: Printed: Tue Jan 13 08:53:27 2004 Name: 010804A-519 Text: t !! f&Ic- 1 I h! K1 r Li fi 3 n m t Exygen Research, 3058 Research Drive, State College, PA 16801 000460 Quantify Sample Report Study No-:L1562, Set No.:010804A, Ext.Date:01/08/04, Analyst:K.Risha Page 20 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804A Daikin Watei Last modified: Tue Jan 13 08:48:53 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: Printed: Tue Jan 13 08:53:27 2004 f ! Name: 010804A-520 Text: 1: C8 Acid I n * I r: t. : fi 1 n tj Exygen Research, 3058 Research Drive, State College, PA 16801 n 000461 H f Quantify Sanala Report t.< Study No.:L1562, Set No.:010804A, Ext.Date: 01/08/04, Analyst :K.Ri sha Page 21 r- Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804A Daikin wate: | : Last modified: Tue Jan 13 08:48:53 2004 -- Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 r* Job Code : I! ' Printed: Tue Jan 13 08:53:27 2004 Name: 010804A-521 '< Text : P 1 : C8 A c id i- XC123003-6,1000 ng/L standard n Cancel'x is printing'x2) 100-] 5.28 363438*1 1 13-Jan-2004 01:35:16 LC/MS/MS #6 MRM of 1 Channel ES413 > 3 6 9 2.02e6 Area % -_ 1 0J M Time% i T ' ,|,,,i" T i i i i i i I i , n i ` " ' " r * i " i iT T " 1" T " | 1-- 1 1 1v y 11 11 1-- t1-- j--1"11 11 11 11 11 j 11 11 11 11 | 11 11 11 11 | 11 1 n1-- i1-- | i1 i1 i1 i1 | i1-- i1-- 1i-- 1 1 1 1 1 *>T~'1 1 1 i 1 1' - '1" 1H 1' i - 1 .....1...............1......1......... .... 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 p ki i n. L,, t! pm f! M wm, X3 ' Exygen Research, 3058 Research Drive, State College, PA 16801 fi ., , v 000462 Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L1562 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: 010804AR Karen Risha LC/MS/MS Unit # 6 01/08/04 01/13/04 Exygen ID XC123003-0 XC123003-I XC123003-2 XC123003-3 XC123003-4 XC123003-5 XC123003-6 L1562-2 XC123003-3 XC123003-4 Sponsor ID - - - - - Rinse Blank - Sample Code c cs cs cs cs cs cs c cs cs Run No. 010804AR-601 010804AR-602 010804AR-603 010804AR-604 010804AR-605 010804AR-606 010804AR-607 010804AR-608 010804AR-609 010804AR-610 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 100 250 x: 100 Dilution Factor - - - 10 - Peak Area 1187 10885 19769 40736 97924 188771 360350 68911 42930 99388 PFOA Found (ng/L) Amount PFOA Added (ng/L) Recovery (%) --- ------- - - 1800 - - -. - - - Standard Curve : Linear (1/x weighted) Intercept = 2668.61 Slope 368.969 Coef. Of Det. = 0.998187 C$ = Calibration standard C = Control sample S = Sample LF =sLab 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: 000463 ~3 1 '3 Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochemicals.PRO\SampleDB\010804AR Daikin Water.SPL Printed: Tue Jan 13 16:21:38 2004 Exygen STUDY N O . JJ5L L 3 3 Page 1 Page Position: (1,1) Vial File Name LIMS ID 1 51 010804AR-601 -- 2 52 010804AR-602 -- 3 53 010804AR-603 -- 4 54 010804AR-604 -- 5 55 010804AR-605 -- 6 56 010804AR-606 -- 7 57 010804AR-607 -- 8 61 010804AR-608 -- 9 54 010804AR-609 -- 10 55 010804AR-610 -- -- -- -- -- -- -- -- -- -- -- ID Sample Description Matrix Sample Type Cone (ng/L) XC123003-0, 0 ng/L standard XC123003-1, 25 ng/L standard XC123003-2, 50 ng/L standard XC123003-3,100 ng/L standard XC123003-4, 250 ng/L standard XC123003-5, 500 ng/L standard XC123003-6, 1000 ng/L standard L1562-2, DF=10 XC123003-3,100 ng/L standard XC123003-4, 250 ng/L standard -- -- -- -- -- -- -- -- -- Blank Standard Standard Standard Standard Standard Standard Analyte Standard Standard 0 25 50 100 250 500 1000 -- 100 250 ... -- -- -- -- -- -- -- -- Cone C Test ID DF MS Method _0 --0 --0 --0 --0 --0 --0 --0 --0 --0 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 10 PFOA 1 PFOA 1 PFOA 000464 1 r^'l r: ::1 'fT l 1n i :!";i Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochemicals.PRO\SampleDB\010804AR Daikin Water.SPL Printed: Tue Jan 13 16:21:38 2004 ^ D ||i 3 | ql| _______________________________ HPLC Method MS Tune File Inj.Volume 1 Fluorochems Fluorochems 15 2 Fluorochems Fluorochems 15 3 Fluorochems Fluorochems 15 4 Fluorochems Fluorochems 15 5 Fluorochems Fluorochems 15 6 Fluorochems Fluorochems 15 7 Fluorochems Fluorochems 15 8 Fluorochems Fluorochems 15 9 Fluorochems Fluorochems 15 10 Fluorochems Fluorochems 15 000465 Exygen STUDYNO. J 0 >2 z. 1 Page 2 Page Position: (2,1) LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: L I562 Instrument: Computer: Micromass Quattro Ultima (LC/MS/MS Unit #6) 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 I? * HP Bin 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: 74A) L (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) : Mobile Phase (B) : 2 mM Ammonium Acetate in Type I Water Methanol Analyst: Karen Ristia 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:__________________ in 0 0 0 4 6 6 ti3 Scanning Method Report Method: C :\MASSLYNX\FLUOROCHEMICALS .PRO\ACQUDB\PFOA Last Modified: W e d Mar 26 15:31:10 2003 Printed: Tue Jan 13 16:21:46 2004 I Solvent Delay ( mins ) 0.00 Analog Channel 4 : Unused Function : 1 MRM 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 ) i; 413.00 369.00 0.20 10 10 n Rage 1 H r? tr* k'- 1 f. km. ki 'i ` p I, 000467 Method Report Method File: Last Modified: Printed C s\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\Fluorochems Tuesday, January 13, 2004 15:51:31 Tuesday, January 13, 2004 16:21:59 Page 1 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 14.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 9 entries which are : Time 0.00 0.40 1.00 7.00 7.50 9.00 9.50 13.50 14.00 A% 60.0 60.0 10.0 10.0 0.0 0.0 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 C% 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 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 Pressure 400 400 400 400 400 400 400 400 400 HP1100 LC Pump External Event Timetable The Timetable contains 6 entries which .are : Time Initial 0.00 0.05 0.10 7.95 8.00 Column Switch Contactl Off Off Off On Off Off Off Off Off Off Off Off Contact2 Off Off Off On Off Off - Contact3 Off Off Off Off On Off Contact4 Off Off Off Off Off Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (/xl/min) Draw Position (mm) Stop Time (mins) Injection Volume (/xl) Vial Number 200.0 200 0.50 14.00 15.0 7 000468 Tuning Method Report Method: C :\MASSLYNX\FLUOROCHEMICALS .PRO\ACQUDB\FLUOROCHEMS Printed: Tue Jan 13 16:22:15 2004 Page 1 n i; r f*. I .3 Dau 395.00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 20 0.0 0.0 0.0 100 300 -2.93 -11 99 299 Pressures Analyser Vacuum Gas Cell Rdbk OFF 3.3e- 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 PIT f '< IK Set R d 14.0 14.0 1.0 -2 15 2 14.0 14.0 2.0 650 8 9 11 - 698 Rdbk 131.4 754.2 000469 Quantify Calibration Report Study No.:Iil562, Set No.:010804AR, Ext.Date:01/08/04, Analyst:K.Risha Rage 1 Exygen Research, 3058 Research Drive, State College, PA 16801 rs - 00047 Quantify Sample Report Study No.:L1562, Set No.:010804AR, Ext.Date:01/08/04, Analyst:K.Risha Rage 1 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804AR Daikin Wati Last modified: Wed Jan 14 07:34:28 2004 Method: R: \Data\LCMSMS6\Masslynx\Fluorochemicals .PRO\MethDEL\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: Printed: Wed Jan 14 07:38:09 2004 Initials . Date Run# s s m s m .T b ,,g itfe ftiA ftrJ3 P Name: 010804AR-601 Text: 1: C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000471  Quantify Sample Report - Study No.:L1562, Set No.:010804AR, Ext.Date:01/08/04, Analyst:K.Risha Page 2 f' Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804AR Daikin Wat j Last modified: Wed Jan 14 07:34:28 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 H Job Code: t i Printed: Wed Jan 14 07:38:09 2004 n Name: 010804AR-602 Text : n ipmnm i m h' > r n if- n (l Exygen Research, 3058 Research Drive, State College, PA 16801 000472 r E . Quantify Sample Report Study No.:L1562, Set No.:010804AR, Ext.Date:01/08/04, Analyst:K.Risha Page 3 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804AR Daikin Wat i : Last modified: Wed Jan 14 07:34:28 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: it- Printed: Wed Jan 14 07:38:09 2004 Name: 010804AR-603 Text: 1: C8 Acid fc : t i! r I; r*^ f< I !* Exygen Research, 3058 Research Drive, State College, PA 16801 r? 000473 _ ; Quantify Sandle Report Study No.:L1562, Set No.:010804AR, Ext.Date:01/08/04, Analyst:K.Risha Page 4 j-- Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804AR Daikin Wat j , Last modified: Wed Jan 14 07:34:28 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: r1 Printed: Wed Jan 14 07:38:09 2004 i- Name: 010804AR-604 Text : 1: C8 Acid f XC123003-3,100 ng/L standard 010804AR-604 Sm (Mn, 2x2) 100i l %: 13-Jan-2004 18:01:42 LC/MS/MS #6 5.30 MRM of 1 Channel ES413 >369 2.64e5 Area fl 0 I |T-| I I I i-n-| .Ilf ' rn-prrrrpri-nyr "i" 111I11' Time 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 H \! F tI i.' Exygen Research, 3058 Research Drive, State College, PA 16801 000474 n B-:-I Quantify Sample Report Study No.:L1562, Set No.:010804AR, Ext.Date:01/08/04, Analyst:K.Risha Page 5 p -i Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804AR Daikin Wat t; Last modified: Wed Jan 14 07:34:28 2004 t Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 |H Job Code: * Printed: Wed Jan 14 07:38:09 2004 Name: 010804AR-605 Text: mt I 1: C8 Acid XC123003-4, 250 ng/L standard F"i { I 010804AR-605 Sm (Mn, 2x2) 100n *' (i! i % : 13-Jan-2004 18:17:27 LC/MS/MS #6 5.30 MRM of 1 Channel ES413 >369 5.92e5 Area 0 ' r r I I J I I I I I I 1H-yi r I ! I I I I I ! I I I I I I I I I I n i i | i i !< 1.00 2.00 3.00 4.00 5.00 6.00 7.00 -n Time 8.00 r. in tI* i t r*n * r* ii Exygen Research, 3058 Research Drive, State College, PA 16801 n 000475 n ri Quantify Sample Report Study No.:L1562, Set N o . :010804AR, Ext.Date :01/08/04, Analyst:K.Risha Page 6 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804AR Daikin Wat |; Last modified: Wed Jan 14 07:34:28 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 fTi Job Code: l\ ; " Printed: .. . Wed Jan 14 07:38:09 2004 . Name: 010804AR-606 Text: 1 : C8 Acid XC123003-5, 500 ng/L standard 010804AR-606 Sm (Mn, 2x2) i 100n f*1 %: 5.29 188771 I i o: ' ' - T 11 " I r r" I I I i t...I --t-- - 1 -, ........................... 1.00 2.00 3.00 1 1 --1' '1 1 1 1--]--! M i l 4.00 5.00 ir*i. I: 13-Jan-2004 18:33:15 LC/MS/MS #6 MRM of 1 Channel ES413 >369 1.09e6 Area r--r 1 ' ty ittt'i'' ri Time 6.00 7.00 8.00 . f-i i1 I n n iI I: Exygen Research, 3058 Research Drive, State College, RA 16801 n 000476 ht! ! Quantify Sample Report Study No.:L1562, Set No.:010804AR, Ext.Date:01/08/04, Analyst:K.Risha Page 7 P"i Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804AR Daikin Wat | Last modified: Wed Jan 14 07:34:28 2004 L Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: 1 Printed: Wed Jan 14 07:38:09 2004 Name: 010804AR-607 Text: i j""3 fj n tt n ti Exygen Research, 3058 Research Drive, State College, PA 16801 00047? fn : Quantify Sample Report . ^ Study No.:L1562, Set No.:010804AR, Ext.Date:01/08/04, Analyst:K.Risha Page 8 ps Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804AR Daikin Wat ; Last modified: Wed Jan 14 07:34:28 2004 " Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 FI Job Code: <irr `` Printed: Wed Jan 14 07:38:09 2004 Name: 010804AR-608 Text: H Ij tt > %r?! n II n Exygen Research, 3058 Research Drive, State College, PA 16801 000478 Quantify Sample Report Study No.:L1562, Set No.:010804AR, Ext.Date:01/08/04, Analyst :K.Ri sha Page 9 r- Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804AR Daikin Wat< Last modified: Wed Jan. 14 07:34:28 2004 fci Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 m Job Code: I::t ' Printed: Wed Jan 14 07:38:09 2004 I i Name: 010804AR-609 5 Text : EH r"*! I) fi n . ii Exygen Research, 3058 Research Drive, State College, PA 16801 000479 JH Quantify Sample Report Study No.:L1562, Set N o . :010804AR, Ext.Bate:01/08/04, Analyst:K.Risha Page 10 fn Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804AR Daikin Wat< I:i Last modified: Wed Jan 14 07:34:28 2004 L, Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: I' i ' ' ' ''' Printed: Wed Jan 14 07:38:09 2004 - r Name: 01804R-610 Text : IP n M Exygen Research, 3058 Research Drive, State College, PA 16801 000480