Document V1EVxGQLY2y3mqokwnbY060o

Proven Results. /}R 6 _ 7 0 8 Analytical Report Fluorochemical Characterization of Water Samples Daikin America, Inc. Exygen Research Laboratory Report No. L34865 Testing Laboratory Exygen Research 3058 Research Drive State College, PA 16801 R e q u e s te r Neal Waddell Daikin America, Inc. 905 State Docks Road (35601) PO Box 2252 Decatur, AL 35609 (256) 306-5000 CT3 T~P0* TO -p -a - O ~o p i ~--(Or r; ~xs rX ro PAGE 10 F 4 J^3 035058 Research Drive > r^ k s tSataite College, PA 16801, USA VT: 800.281.3219 F: 814.272.1019 exygen.com 1 Introduction Results are reported for the analysis of water samples received by Centre Analytical Laboratories, Inc. (dba Exygen Research) (Exygen) from Daikin America, Inc.. This report presents results assigned to Exygen Research study number L34865. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) was requested for all samples. A total of 5 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 Perfluoroctanoic Acid Acronym PFOA 2 Sam ple R eceipt The samples were submitted in individual plastic containers, cooled with wet ice. Samples were collected on 7/13/03 and 7/15/03 and were received on 7/16/03. Chaln-of-custody information is presented in Attachment C. Field and laboratory spikes of these fluorochemicals have shown stability for periods greater than 90 days. Samples were analyzed within 30 days of collection. 4 Methods - A nalytical and Preparatory 4.1 LC/MS/MS 4.1.1 Sample Preparation for LC/MS/MS Analysis Water 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 transferred to a C i8 SPE cartridge. The cartridge was eluted with 40% methanol: water. The eluate was discarded. The cartridge was then eluted with 100% methanol. A 5 mL portion of methanol was collected for analysis by LC/MS/MS. This treatment resulted in an eight-fold concentration of the samples prior to analysis. PAGE2OF4 000005 4.1.2 Sample Analysis by LC/MS/MS 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 7/23/03, 8/1/03, and 8/12/03. Samples were analyzed on 7/26/03,7/30/03,8/2/03, and 8/12/03. Raw analytical data can be found in Attachment D. 5.1 Calibration A 6-point calibration curve was analyzed at the beginning of the analytical sequence and throughout the run for the compounds of interest. The calibration points were prepared at 25, 50, 100, 250, 500, and 1000 ng/L (ppt), as perfluorooctanoic acid (PFOA). 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 >.0.992 (r2 > 0.985). Calibration standards for MS/MS analysis were prepared using the same SPE procedure used for samples. For the results reported here, calibration criteria were met. 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 method. 5.4 Matrix Spikes Matrix spikes were prepared for samples #2 Utilities DSN001 and #4 Unidyne DSN006 at levels approximating the sample concentrations. The matrix spike recoveries were within the acceptable range of 70 -1 3 0 % . Matrix spike recoveries are given in Attachment B. 5.5 Duplicates Samples #2 Utilities DSN001 and #4 Unidyne DSN006 were analyzed in duplicate. Results are given along with the sample results in Attachment A. 5.6 Laboratory Control Samples Milliq water was spiked with PFOA at 50 and 500 ng/L. with each extraction set. All laboratory control samples showed recoveries between 70 and 130%. PAGE3 OF4 000006 6 Data Sum m ary | Please see Attachment A for a detailed listing of the analytical results. All results are reported in (ng/mL) parts per billion as PFOA. 1 1 1 !! 01 il 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 Attachm ents ? || o 8.1 Attachment A: Results 8.2 Attachment B: Matrix Spike Recoveries 8.3 Attachment C: Chain of Custody 8.4 Attachment D: LC/MS/MS Raw Analytical Data 9 Signatures Paul Connolly, Team Leader-LCMS Other Lab Members Contributing to Data Karen Smith Date PAGE4 OF4 000007 f] nI i j ; i.s n n p it <1 V,, II 0 Hpm I1 Summary of PFOA in Samples Analyte Found (ng/mL) Sample ID______________________ PFOA________ #1 Utilities Field Blank #2 Utilities DSN001 1.11 677 \ #2 Utilities DSN001* #3 Unidyne Field Blank . #4 Unidyne DSN006 700 ND 153 #4 Unidyne DSN006* 163 #5 Control 116 *Laboratory Duplicate ND = N ot detected = R esponse betw een 0 and 0.025 ng/m L. 000008 '^ ^ ^3 0 5 8 Research Drive M m u ta te College, PA 16801, USA mF:800.281.3219 814.272.1019 exygen.com Proven Results. n Recovery Summary for PFOA in W ater PFOA W-1 U Sample Amount Amt Found Amount Spiked in Sample Recovered Recovery Description (ng/mL) (ng/mL) (ng/mL) (%) in. < #2 Utilities DSN001 500 ng/m L Spike 500 677 1210 107 f"! t j #4 Unidyne DSN006 250 ng/m L Spike 250 153 371 87 ir 1 Ii I4 H ij n MM| fc i n ^n-j 11 000009 in _ ^^3 0 5 8 Research Drive -# m S ta te College, PA 16801, USA r-* 800.281.3219 u I F : 814.272.1019 exygen.com 000010 CHAIN OF CUSTODY/ANALYSIS REQUEST FO RM Exygen Research Sample Receiving 3117 Research D rive S tate C ollege, PA 16801, USA T: 814.231.8032 9 F: 814.231.1580 exygenresearch.com Page / of / PROJECT INFORMATION Client (name & address) : Project Manager (Name & E-mail Address): / h * Y/*\<tr 'OQ , .jTrtC . 9 o r A U s /PA. ( 3~6ot ) p.0- &0< /Iglco s , A l Z 'T /o q Phone: ( 2 ir ) 3 o 6 - 5 ~ o o o /J/jQI J&cJcA / / toacJdfJi</L d iti fan -a n Grcci. co/n Project Name: Fax: R O .#: P 0 3 O 2 . 2 S 3 0 T~ Sampler: / ( / W U )*. d e J t /s A u L 5 /i0^ ' 7T Quotation # : Please fill out this form com pletely to ensure correct analysis and proper handling of your samples. ANALYSES REQUESTED SAMPLE ANALYSISExyLIMS# Client Sample Identification Collection Collection Date Time Q O Qo . E uo L v& G jr- ( ^ /~ic. Aink. 7~-o3 i C 5 0 y c U m E E z 2 , I-k/,4z.s SA/ o / 7 -/f- > 2 O S H Q y J n c -r-3 3. ffc U ik 09 /o y . L .J n ^ L /SAQO, 7 /T -0 3 O ^ /jT y L i i C f - r s . G t o / T -/T -0 ? O Y Z O Specify Matrix Comments s a X. X X X LAB USE ONLY CHAIN OF CUSTODY Relinquished by , Date Time /Y e a / i a .A tL l/^ y % A t^ y 7 -/r-o 3 7 * ------------- OTHER INFORMATION 0 3 C l] c : i L i;i el Cooler ID # / / c m ,a f L Received j i y ------------------------- Uz' Cooler Temp. (C) /,% -- Date, . 07// Yd Time /ejo ' ">#3; LAB USE ONLY PROJECT REQUIREMENTS Results Deadline: Laboratory Report Options: HH Sample results only 0 Add case narrative Add quality control summary 1 I Add calibration summary I I Add raw data Other ^* cz: c. IV , 3~C|~ - - ii 3058 Research Drive Phone: 800-281-3219 t State College, PA 16801 Fax: 814-272-10 9 Laboratory Sample Log-in Sheet (Environmental} 4 ' hi Complete upon sam ple receipt: Client and/or Project Name Z X k A n d /h -e ^ U c t . M e . Method of Walk-in Pick-up UPS ^CJ-FedEx- A ir Borne Delivery Tracking#: "2 C -70 C. y y Other (explain) F*. Chain of Custody Custody Seals: Brpresent, & O^nfSctJo broken (explain) absent Chaipjof-Custody Record: P present * absent Temperature Thermometer ID: CO2 - / 7 Samples Received: Preservation Cooler ID: Cooler temD: / - C ppiice n Cooler ID: Cooler ID: . Cooler temD: Cooler temp: C C J ^ln ice melt with ice pack r= Cooler ID: Cooler temD: C none Explanation Completed by Slanature: / " , Date fTimek 7 / /0> i c 7 / c y * Complte durinei sample loo-in: LIMS Log-in # Physical Condition Samples intact? ' - . - / J3*?es No (explain) -, . . v' Chain of Custody Samples received agree with COC record? ^ p -Y e s No (explain) Analysis Request Analysis request clear? Preservation Sample containers appropriate? #m Chemical preservation appropriate? Samples received within holding time? Sample volume/mass adequate? n t ; Explanation p s fe s No (explain) Yes No (explain) Yes No (explain) Yes No (explain) Yes No (explain) . Completed by Slanature: / / -- ----- - " -Bate: ,, y^ ^ ^ ' Complete followina resolution o f anv nonconformances: Client Contacted Yes Client: No Resolution Date (Time): ' Completed by Slanature: Date: Lab Sx Log-in Sheet -Ex 11 -5-01/0 O O O O ll LOGIN CHAIN OF CUSTODY REPORT (InOl) Jul 16 2003, 11:37 am P Login Number: L34865 Account: 3027 DAIKIN AMERICA, INC. Laboratory Sample Number Client :S:3'-mpX<'-Nfimber- Collect Receive Due Date Date PR Date fPr- 4 L34865-1 #1 UTILITIES FIELD BLANK 13-JUL-03 16-JUL-03 SAMPLES KEPT IN D0000539. L34865-2 #2 UTILITIES DSN001 15-JUL-03 16-JUL-03 L34865-3 #3 UNIDYNE FIELD BLANK 15-JUL-03 16-JUL-03 L34865-4 #4 UNIDYNE DSN006 15-JUL-03 16-JUL-03 L34865-5 #5 CONTROL 15-JUL-03 16-JUL-03 n f***! h j. i Page 1 Signature : Date : n 000012 000013 I7S7T f \ -- + So FedEx. Express i- '''"T- ? J nuHdj FdE* T ric k in g Number a3B5Bb.7D,llm3 V . DBK /'V- ;vr . -o -/ :7 i 1 F r o m c alio^nchariebe reenmraveiMsr Recipient's recort UJ ce y Sende Name! 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VQO Z *rT ` 1: L 1: L. 1 C.  i- - f "*1 J 1""*! . 1. fV n n i n f: r-* t 1 i. , r* P* Vi ' l, Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L34865 PFOA 413-> 369 NA RAW DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Volume: Final .Volume: 50ng/L 15 pL Water 40.0 mL 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 072303B Karen Risha LC/MS/MS Unit # 6 07/23/03 07/26/03 Exygen ID XC072303-0 XC072303-1 XC072303-2 XC072303-3 XC072303-4 XC072303-5 XC072303-6 Methanol Wash 0106020 Control 0106020 Spk A 0106020 SpkB L34865-2 Spk C XC072303-1 XC072303-2 XC072303-3 L34865-1 L34865-3 L34865-5 L34865-2 L34865-2 Rep L34865-4 XC072303-4 XC072303-5 XC072303-6 Sponsor ID - - NA NA NA #2, Utilities DSN001 __ #1, Utilities Field Blank #3, Unidyne Field Blank #5, Control #2, Utilities DSN001 #2, Utilities DSN001 #4, Unidyne DSN006 - - Sample Code c CS CS CS CS CS CS c c LCS LCS LF CS CS CS s s s s s s CS CS CS Run No. 072303B-501 072303B-502 072303B-503 072303B-504 072303B-505 072303B-506 072303B-507 072303B-508 072303B-509 072303B-510 072303B-511 072303B-512 072303B-513 072303B-514 072303B-515 072303B-516 072303B-517 072303B-518 072303B-519 072303B-520 072303B-521 072303B-522 072303B-523 072303B-524 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 1 1 1 1 1 1 - Peak Area 0 11914 22914 40286 101512 188471 372884 0 0 21453 180550 43939908 23062 22445 37342 422250 0 21427832 45139376 43781912 20768144 105514 173609 315949 x 100 PFOA Found (ng/L) - ND 39.7 503 * `* ND * * * * - - - Amount PFOA Added (ng/L) - 50 500 500 - - Recovery (%) - - -79 101 - ^- -'- Standard C urve: Linear (1/x weighted) Intercept = 7808.01 Slope = 343.430 Coef.OfDet. = 0.986965 CS = Calibration standard C = Control sample S = Sample LF asLab 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 *Sample requires dilution. See data set 072303BR. Spreadsheet prepared by: t 000014 LOGIN CHAIN OF CUSTODY REPORT (InOl) JLf* Jul 16 2003, 11:37 am L o g in N u m b e r: L 3 4 8 6 5 A c c o u n t: 3 0 2 7 D A IK IN A M E R IC A , IN C . Laboratory; : -L;:: XL; Client S:airri3!li ;; ;,v' Collet.b,..;'Reeeiye L34865-1 #1 UTILITIES FIELD BLANK 13-JUL-03 16-JUL-03 SAMPLES KEPT IN D00539. L34865-2 #2 UTILITIES DSNG01 15-JUL-03 16-JUL-03 L 3 4 S 6 5 :-3; #3 UNIDYNE FIELD BLANK 15-JUL-03 16-JU L - 03 #4 UNIDYNE DSN006 .15-JUL-03 16-JUL-03 L34865-5 #5 CONTROL 1S-JUL-03 16-JUL-03 Page 1 S ig n a tu r e : D a te : 000015 '1 n T ir i : t i im 13 : ; n T il ; : : i CHAIN O F CUSTODY/ANALYSIS REQUEST FORM RESEARCH PROJECT INFORMATION Exygen Research Sample Receiving 3117 Research Drive State College, PA 16801, USA T 814.231.8032 F: 814.231.15) exygenresearcli.com Page / .of_Z_ ANALYSES REQUESTED Client (name & address): _____ t t i h * . JZ hc. 9or rfoU s (iS T o i) Po- ort z r * /leca-s. AL ? <rQtj Phone: (,2S i ) 3 o 6 - 5 "o o o Fax: " ' Sampler: A /e .*/ L a d e J l /s h s L Project Manager (Name & E-mail Address): _____ A/a/ hJoeJeA / / __________________ _____ iv a a ld d l& c U i k -arnesito . pai Project Name: ROO..#: ! PP O 3 0 2 . Z 3 3 Q Quotation # Please fill out this form completely to ensure correct analysis and proper handling of your samples. SAMPLE ANALYSIS o a ExyLIM&P C lient Sample Id e n tifica tio n Collection Collection Date Time O uo L 3 `/e>c,s~-( * / j tSA/sde * f i t t t S L d 7-/3-Q5 M 1 M s / L 3 W ,r- c lu c r-i L ? n c .m tZ , tA M 'L s SAlOl (MdvKK. fh f h tk . / / A. A . j/ - . - 7-ir-cB Q 2 y y 9/Q Qtf/s~ y C . J U *1 1 C -t(t /s a I T d p o y Q9Z.Q o |i c3 Oc Z U Specify Matrix I hJaJts Com m ents I X X LAB USE ONLY CHJMN OF CUSTODY Relinquished by , . A /es*L * /f . D ate Tim e 7 -/r- > 3 OTHER INFORMATION C ooler ID # /y 'Ic ^ a o f t C ooler Temp. (C) /, - Receivedjy : T- ` Date, Time ':i,` i.T c/j lei ?e/e ^ -- . ' . :- - j: l, 1!' "'T* V: LAB USE ONLY - _ '-^v^ PROJECT REQUIREMENTS Results Deadline: Laboratory Report Options: 0 Sample results only 0 Add case narrative 0 Add quality control summary 0 Add calibration summary 0 Add raw data 0 Other REV. 302 000016 Exwen W F ^ /& e E A R C H 3058 Research Drive State College, PA 16801 Complete upon sample receipt: Phone: 800-281-3219 Fax: 814-272-1019 Chain of Custody Temperature Presentation Q Air Borne Other (explain) Custody Seals: ____ _ -B-pfesent, & Q-ftflacf/D broken (explain) absent ______________ Thermometer ID: Cooler ID: <r~* A. Cooler ID :_________________ Cooler ID :_________________ Cooler temp:/ C Cooler temp: _______ C Cooler temp: _______ C ChaipjsfCustody Record: tfp re s e n t * absent Samples Received: OppSce EsIn ice melt 'O with ice pack Qnone Physical Condition Chain of Custody Analysis Request Preservation Explanation Samples intact? Samples received agree with COC record? Analysis request dear? Sample containers appropriate? 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I Credit Ca-d f ] Cash/Cteck- It iS r if* t l j .V ^OurfaMttyhlitdW tlttllOPm ilessyiH utPdwealHghetm iii See the FedEx p n ^ e Ctwfe fat detaUs 8 ReleaseSignatura j*tomanverteHre.ivi*rt>!jf'hr>.-hrwumtve 1*9198846114 By tillin g you th o rite us to tfe tar this shipment without obtaining(signature and 93r w to nfemnify end hold us harmless h<rn any resulting clirrre S te W S ^ * ** * ? *' Ill I Rev Ibm71*fLirt4177OT*T>lin+-7tXI' G0fet(WM iw l % ,0 APlaigrnt#bo1t5to0m45o4tRAoltbvR.i/IOPOouchhero. o h* 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 SAMPLE TRANSFER SHEET Protocol Number: NA Exygen Study Number: L34865 Karen Risha 07/21/03 1035 Requested By (Printed Name/Date/Time) Samples removed from: Samples removed from: > lk - Samples transferred to the custody of Box# Box# Samples received from custodian; Samples moved to Samples removed from V - c f Samples returned to P (JO fl 7A Shelf# Shelf# Sample Custodian Initials/Date/Time Z Pd a 7 M 1/03 \\\z u Laboratory Personnel Initials/Date/Time f f /C - '7 / ^ / o3 Sample Custodian Initials/Date/Time 000019 n n RESEARCH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number: L34865 Matrix: Water Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No, 3 ` p Tim e__ 0 8 2 5 Date 7 / ^ / 0 3 Initials /? ! ..I CLIENT SAMPLE ID EXYGEN ID NUMBER VOLUM E (mL) FO RTIFICATION (ng) na na na #2, Utilities DSN001 #1, Utilities Field Blank 0106020 Control 0106020 Spk A 0106020 Spk B L34865-2 Spk C L34865-1 40.0 - 40.0 2.0 40.0 20.0 40.0 ' 20.0 40.0 #2, Utilities DSN001 #2, Utilities DSN001 L34865-2 L34865-2 Rep 40.0 40.0 _ _ #3, Unidyne Field Blank L34865-3 40.0 _ #4, Unidyne DSN006 L34865-4 40.0 _ #5, Control L34865-5 40.0 - - - -_ - - __ - -_ - - __ n - -' - - -_ __ - - __ - - -_ - - -- p"n Spiking Solution Used Volume Used for Spiking Initial/Date 0106020 Spk A F061803-5 (10 ng/mL) 200 pL (200 pL micropipet) 1i t /< n l2 3 ^ 0106020 Spk B F061803-4 (100 ng/mL) 200 pL (200 pL micropipet) \ b L /m in io ' L34865-2 Spk C F061803-4 (100 ng/mL) 200 pL (200 pL micropipet) t i u n ib(> > i - - _ 0 . - - __ '- _ - - -- All samples were measured: Time O O P Date 7i /j2^-Aj c/ 3 Initials C JSS After measuring samples were returned to refrigerator No. 3 2 Time 3 5 0 ________ Date llZ ? ,jo 3 Initials rE 5 Com m ents: 200 pL of 250 mg/mL sodium thiosulfate 5added to all samples before spiking. Initials/Date: OEbJ Analysis Summary: Data Set: 0723655 Data Set: C r7 2 3 6 3 & e. Data S et:______ ' Initials/Date: Initials/Date: Initials/Date: . 7l2Slb *' P ~! Set extracon/analysis data verified b y :______QOQ Date: July 26, 2001/6 .... 1 ; : : : i 1 1n Phone: 814-272-1039 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L34865 MATRIX: Water METHOD: f ANALYTES: PFOA PROTOCOL NUMBER: NA Client ID na na na #2, Utilities DSN001 #1, Utilities Field Blank #2, Utilities DSN001 #2, Utilities DSN001 #3, Unidyne Field Blank #4, Unidyne DSN006 #5, Control _ Exygen ID 0106020 Control 0106020 Spk A 0106020 Spk B L34865-2 Spk C L34865-1 L34865-2 L34865-2 Rep L34865-3 L34865-4 L34865-5 - STEP 1 >1 - STEP 2 / \ - Dilutions (mL/mL) -- -' - - -- - - - STEP 3 Dilutions (mL/mL) -- -- STEP 4 - - S> V 'y* oV w o >/ * 0-Vl.O \ / \/ --- Reagents/ Materials Methanol C18 SPE Type I Water _ . - Initials/Date - Lot# 43111310 \M 5 I1 2 ] NA - - M m & k& _ - -- - -- - _ . - - -- - --- - - _ - -- - -- - - - - - -- - -- - - - - - -- - --- - - - - -- - -- - - - - - -- - -- - - - - - -- - --- HPLC - - -- - -- - Methanol 4306131^ - - -- - - - - Ammonium Acetate - - -- - - - - Type I water NA - - ifr *lnitials/Date . S72S a 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. -- ra s la 3 IL * Q s m & m z . p iA c e h v im , fob Iter 1WJCTUNTIL07^03 -- Initials/Date tPIEg-O 97{25|3B0T t>7|2 Initials and date under each step indicates the personnel that performed this step. g ) b f 5 l; o o o 5 ^ * 1 $$ Method of Analysis for the Determination of Perfluorooctane sulfonate (PFOS), Perfluorooctane sulfonylamide (PFOSA), and Perfluorooctanoate (POAA) in Water COMMENTS: Final extracts stored in refrigerator 3 2 - Initials: wl July 19,2001/4 000021 PREPARATION OF EXTRACTED CALIBRATION STANDARDS Exygen STUDY NO* LS'iGS' Protocol No.: None Method No.: 01M-008-046* Exygen Study No.: NA Analytes: PFOA Matrix: Type I WaterA Sample Vol: 40 mL Sponsor Sample ID NA Exygen Sample ID 0106020 Sample Description Type I WaterA Fort. Solution ID - Fort Soin. Cone. (hg/mL) - Fort Volume (uL) - Micropipet used (PL) Fort. Level foot) - Final Solution ID #** XC072303-0 Reagents/ Materials Methanol Lot# 4 3 U931S NA 0106020 Type I WaterA F061803-5 10 100 200 25 XC072303-1 C18 SPE W S liz B * NA 0106020 Type I WaterA F061803-5 10 200 200 50 XC072303-2 Type I Water NA NA 0106020 Type I WaterA F061803-5 10 400 200 100 XC072303-3 - - NA 0106020 Type I WaterA F061803-4 100 100 200 250 XC072303-4 - - NA 0106020 Type I WaterA F061803-4 100 200 200 500 XC072303-5 NA 0106020 Type I WaterA F061803-4 100 400 200 1000 XC072303-6 - .- - - o NA 0106020 Type I WaterA F061803-7 -- - - - 100 200 250 XC072303-7 --- - Initials/Date: 3 Vertical arrows in a column indicate identical values. **This must be a unique number. Use this system: Extracted Calibration Soln ID #: XCMMDDYY-0,1,2,3. etc. Samples removed from r<^ngeratop)/ freezer # 3 2 - Time: 0 & 2 S 40 mL of each sample measured using a mT. graduated cylinder. After measuring, samples returned to j^Tngerafpr / freezer # Time: /.3 h Samples fortified: Initials/Date: / m l& jb z Initials/Date: C i3 ^ / 112^-.63 Initials/Date: / 'll2 Initials/Date: 0 = & / 1 TWfS IS AN EXACT COPY OF ^O R IG IN A L DOCUMENT" BY -- q v - ----- date 07120 SPE clean-up: Initials/Date: ZzjZ Final volume adjusted to 5 mL: Initials/Date: C k /~&ij 2 .^,/a, Extracts placed in refrigerator # *?2- Initials/Date: CE& /'? STANDARD EXPIRATION DATE: 8/6/03 Onmments: AThis type I water has been filtered through a hypercarb filter * Method of Analysis for the Determination of Ammonium Perfluorooctanoate (APFO) in Water. 000022 July 10, 2001/0 ''I II Masslynx - Sample List Sample List: C:\M ASSLYNX\Fluorochem icals.PRO\Sam pleDB\072303B D alkin.SPL Printed: Fri Jul 25 14:33:11 2003 Vial File Name LIMS ID Client ID Sample Description Matrix 1 1 072303B-501 ____ 2 2 072303B-502 -- 3 3 072303B-503 -- 4 4 072303B-504 -- 5 5 072303B-505 -- 6 6 072303B-506 -- 7 7 072303B-507 -- 8 92 072303B-508 -- 9 11 072303B-509 -- 10 12 072303B-510 -- 11 13 072303B-511 -- 12 14 072303B-512 -- 13 2 072303B-513 -- 14 3 072303B-514 -- 15 4 072303B-515 -- 16 15 072303B-516 -- 17 16 072303B-517 -- 18 17 072303B-518 -- 19 18 072303B-519 -- 20 19 072303B-520 -- 21 20 072303B-521 -- 22 5 072303B-522 -- 23 6 072303B-523 -- 24 7 072303B-524 -- ____ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- XC072303-0, 0 ng/L standard XC 072303-1,2 5 ng/L standard X C 072303-2,50 ng/L standard X C 072303-3,100 ng/L standard XC072303-4, 250 ng/L standard XC072303-5, 500 ng/L standard X C 072303-6,1000 ng/L standard Methanol W ash 0106020 Contrai 0106020 S p kA , 50 ng/L 0106020 Spk B, 500 ng/L L34865-2 Spk C, 500 ng/L XC072303-1,2 5 ng/L standard XC072303-2, 50 ng/L standard X C 072303-3,100 ng/L standard L34865-1 L34865-3 L34865-5 L34865-2 L34865-2 Rep L34865-4 X C 072303-4,250 ng/L standard XC072303-5, 500 ng/L standard X C 072303-6,1000 ng/L standard -- -- -- -- -- -- ~ 000023 1 T3 T 1 n r:i H xyg e n STUDY N O . L 5 H 8 6 S i !m Page 1 1 1PaSe Position: ( , ) ': n Sample Type Cone (ng/L) ConcB ConcC Test ID DF MS Method B la n k S ta n d a rd S ta n d a rd S ta n d a rd S ta n d a rd S ta n d a rd S ta n d a rd B la n k B la n k QC QC QC S ta n d a rd S ta n d a rd S ta n d a rd A n a ly te A n a ly te A n a ly te A n a ly te A n a ly te A n a ly te S ta n d a rd S ta n d a rd S ta n d a rd 0 25 50 100 250 500 1000 -- -- 50 500 500 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 -- --0 ----0 ---- ---- 0 0 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA 1 PFOA -"T7^ -"I-TM> *1 M asslynx - Sam ple L is t Sample List: C:\M ASSLYNX\Fluorocl Printed: Fri Jul 25 14:33:11 2003 icals. PRO\SampleDB\072303B D aikin.SPL f f lz s lo ^ _______________________ HPLC M ethod MS Tune F ile In j.V o lu m e 1 Fluorochem s Fluorochem s 15 2 Fluorochem s Fluorochem s 15 3 Fluorochem s Fluorochem s 15 4 Fluorochem s Fluorochem s 15 5 Fluorochem s Fluorochem s 15 6 Fluorochem s Fluorochem s 15 7 Fluorochem s Fluorochem s 15 8 Fluorochem s Fluorochem s 15 9 Fluorochem s Fluorochem s 15 10 Fluorochem s Fluorochem s 15 11 Fluorochem s Fluorochem s 15 12 Fluorochem s Fluorochem s 15 13 Fluorochem s Fluorochem s 15 14 Fluorochem s Fluorochem s 15 15 Fluorochem s Fluorochem s 15 16 Fluorochem s Fluorochem s 15 17 Fluorochem s Fluorochem s 15 18 Fluorochem s Fluorochem s 15 19 Fluorochem s Fluorochem s 15 20 Fluorochem s Fluorochem s 15 21 Fluorochem s Fluorochem s 15 22 Fluorochem s Fluorochem s 15 23 Fluorochem s Fluorochem s 15 24 Fluorochem s Fluorochem s 15 000024 Exygen study no. Page 2 Page Position: (2 ,1 ) n LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol N o : N A Exveen Study No: L34865 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #6) &j f; Computer: COMPAQ Professional Workstation AP200 Software: n lt - 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 M HP Autosampler HP Column Oven I HPLC Column: Genesis C-8, 5 cm x 2.1 mm i.d. x 4 p (Exygen ID: 74A) I I (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase ( A ) : 2 mM Ammonium Acetate in Type I Water f : 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 NO TE: The next 3 pages are com puter generated printouts from the m asslynx softw are program . T he pages contain the instrum ent settings used for th e analysis o f th is data set. A ll Handwritten Peak ID 's by: lO b I! Pi Ij n rt IT"! t t t! 000025 Scanning Method Report Method: C :\MASSLYNX\FLUOROCHEMICALS. PRO\ACQUDB\PFOA Last Modified: Wed Mar 26 16:31:10 2003 Printed Fri Jul 25 14:34:46 2003 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 ) 1 413.00 369.00 0.20 10 10 Page 1 000026 Method Report Method File: r*! Last Modified Printed C :\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\Fluorochems Friday, July 25, 2003 14:31:55 Friday, July 25, 2003 14:34:55 Page 1 HP1100 LC Pump Initial Conditions Solvents 60.0 40.0 0 .0 0 .0 P? Flow (ml/min) jr j Stop Time (mins) ' Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) i Oven Temperature Right(C) 0.300 14.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable i. The gradient Timetable contains 9 entries which are : Time pi**.4 0.00 0.40 1.00 7.00 7.50 n 9.00 V, 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 ns 0.00 a 0.05 i? o . io 7.95 8.00 p*) Column Switch Contactl Off Off Off On Off Off Off Off Off Off Off Off Contact2 Off Off Off On Off Off w HP1100 Autosampler Initial Conditions pm Draw Speed I5 ' Eject Speed (/nl/min) Draw Position (mm) Stop Time (mins) n Injection Volume (il) Vial Number 200.0 200 0.50 14.00 15.0 2 Contact3 Off Off Off Off On Off Contact4 Off Off Off Off Off Off 000027 tJ Tuning Method Report Method: C :\MASSLYNX\FLUOROCHEMICALS .PRO\ACQUDB\FLUOROCHEMS Printed: Fri Jul 25 14:35:25 2003 03 Page 1 P"**, ! Dau 499.00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. I '! t j Pressures Analyser Vacuum f"? Gas Cell Set Rdbk 3.00 20 0 .0 0 .0 0 .0 100 300 -2.93 -21 100 299 Rdbk OFF 3.4e-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 15 2 14.0 14.0 2.0 650 12 14 16 -648 Rdbk 131.0 755.7 )i 000028 r\. Ii Quantify Calibration Report Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, Analyst:K.Risha Page 1 Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\072303B Daikin Last modified: Sat Jul 26 15:58:52 2003 Printed: Sat Jul 26 16:00:33 2003 Exygen Research, 3058 Research Drive, State College, PA 16801 000029 Quantify Sample Report Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, Analyst:K.Risha Rage 1 Sample List: Last modified: Method: Last modified: Job code: Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\072303B Daikin Sat Jul 26 15:53:34 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\\^C80 oUJnly 072503 Sat Jul 26 15:54:50 2003 '* InHiate , nnto I Sat Jul 26 16:00:35 2003 o.,Jt *31 To ()1 2 r W ^ fi'.5 2 t Name: 072303B-501 Text: 1: C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000030 rt Quantify Sample Report Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, Analyst:K.Risha Rage 2 l*"j, Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303B Daikin Last modified: Sat Jul 26 15:53:34 2003 j Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 f*1 Job Code: . ' " Printed: Sat Jul 26 16:00:35 2003 1 I Name: 072303B-502 ' Text : f? i*- : t MM; ; t* ,' Exygen Research, 3058 Research Drive, State College, PA 16801 - \ 000031 Quantify Sanale Report Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, Analyst:K.Risha Page 3 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\072303B Daikin Last modified: Sat Jul 26 15:53:34 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 Job Code: Printed: Sat Jul 26 16:00:35 2003 t f \/ Harne: 072303B-503 Text: 1 : C8 Acid XC072303-2, 50 ng/L standard 072303B-503 Sm (Mn, 2x2) 4n n _ H%: i r n - ' 1I '1'1 11' 'r ' "I.11 ,|,"T11111 11' 1' 1.00 2.00 3 .0 0 5.03 229141 I 1 1..MI.1."1...r.T...i.., 111i-i-.-t--|--r-j ! 1 11111 4.00 5 .0 0 6.00 26-UI-2003 06:36:24 LC/MS/MS #6 MRM of 1 Channel ES413 >369 1,57e5 A re a I 1 1 ' ' 1Tim e 7.00 8.00 r*>* yS I s: i. iV { A r; Exygen Research, 3058 Research Drive, State College, PA 16801 i 000032 i Quantify Sample Report Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, Analyst:K.Risha Page 4 ^ Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303B Daikin ,i Last modified: Sat Jul 26 15:53:34 2003 ' ) Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 (f? Job Code: Printed: Sat Jul 26 16:00:35 2003 { , Name: 072303B-504 Text: 1: C8 Acid n i '< t... i, iI--J I' i- . rs Exygen Research, 3058 Research Drive, State College, PA 16801 000033 li ! i Quantify Sample Report Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, Analyst:K.Risha Page 5 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\072303B Daikin '( ' Last modified: Sat <Jul 26 15:53:34 2003 't Method: P:\Data\LCMSMS6\Masslynx\Fludfochemicals.PRO\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 Job Code: Printed: Sat Jul 26 16:00:35 2003 Name: 072303B-505 Text: 1: C8 Acid XC072303-4, 250 ng/L standard f*T 072303B-505 Sm (Mn, 2x2) I <1 100n %~ 5.02 101512 26-JUI-2003 07:07:51 LC/MS/MS #6 MRM of 1 Channel ES413 >369 6.60e5 Area 0: i ' ' ' T '1"'1i i |T n i | m 1.00 2.00 3.00 4.00 6.00 T -n-r-r 7.00 T-n Time 8.00 T< t il \' & t- i P. Exygen Research, 3058 Research Drive, State College, PA 16801 000034 I 4 r* t ; Quantify Sample Report Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, Analyst:K.Risha Page 6 ^ Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303B Daikin f ; Last modified: Sat Jul 26 15:53:34 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\C8 only 072503 Last modified: Sat <Tul 26 15:54:50 2003 Job Code : Printed: Sat Jul 26 16:00:35 2003 * ? Name: 072303B-506 t * Text: 1 : C8 Acid XC072303-5, 500 ng/L standard dg/t 072303B-506 Sm (Mn, 2x2) 100q P? %: 26-Jul-2003 07:23:32 LC/MS/MS #6 MRM of 1 Channel ES5.04 413 > 3 6 9 1.33e6 Area fT 0 ` I I I | *1 ` 1 I I 1.00 I 'I I "I '"T" ' I I I I ; > , , , I . 2.00 3.00 4.00 5.00 6.00 |. -ir T.-| r-r^ i i'i.i"T-r jT i m e 7.00 8.00 t! i >' *i Hi ii Exygen Research, 3058 Research Drive, State College, PA 16801 *00035 n et ; Quantify Sample Report Study No.:L34865, Set N o . :072303B, Ext.Date:07/23/03, Analyst:K.Risha Page 7 ^ Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\072303B Daikin | , Last modified: Sat Jul 26 15:53:34 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 f"', Job Code: Printed: Sat JUl 26 16:00:35 2003 Name: 072303B-507 k Text: 1: C8 Acid i. (. ii I: t; j 1 ft Exygen Research, 3058 Research Drive, State College, PA 16801 000036 pi t : f* ^- r Quantify Sanale Report Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, Analyst:K.Risha ' Page 8 - f * \ Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303B Daikin i Last modified: Sat Jul 26 15:53:34 2003 ' - Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 r - Job Code: t Printed: Sat Jhl 26 16:00:35 2003 _- - I Name: 072303B-508 Text: I i< ij r i k 'j #2Ss Exygen Research, 3058 Research Drive, State College, PA 16801 i 000037 n f *I i Quantify Sanale Report Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, AnalystsK.Risha Rage 9 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\072303B Daikin Last modified: Sat Jul 26 15:53:34 2003 Method: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 f****"' Job Code: Printed: Sat Jhl 26 16:00:35 2003 Name: 072303B-509 Text: /f; sf -A IJ i f* : I- f i 'I *- Exygen Research, 3058 Research Drive, State College, PA 16801 000038 ' 1 Quantify Sample Report Study No.:L34865# Set No.:072303B, Ext.Date:07/23/03, AnalysttK.Risha Pa r * * Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\072303B Daikin I j Last modified: Sat Jul 26 15:53:34 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 jH Job Code: " Printed: Sat Jul 26 16:00:35 2003 Name: 072303B-510 Text: fi jBL r* A I? * \ Exygen Research, 3058 Research Drive, State College, PA 16801 000039 n p Quantify Sample Report Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, Analyst:K.Risha Page 11 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochexnicals.PR0\SampleDB\072303B Daikin i Last modified: Sat Jul 26 15:53:34 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 n Job Code: Printed: Sat Jul 26 16:00:35 2003 Name: 072303B-511 Text: n 1: C8 Acid 0106020 Spk B, 500 ng/L 072303B-511 Sm (Mn, 2x2) 100-1 iir*>, %- n 1.00 2.00 /C 3.00 5.02 180550 26-Jul-2003 08:42:20 LC/MS/MS #6 MRM o f 1 Channel ES413 >369 1.25e6 Area 4.00 T ` 111I 5.00 6.00 7.00 Time 8.00 i I; frs- Il LV fn- - Exygen Research, 3058 Research Drive, State College, PA 16801 f* ;- 000040 r~ h ' r-> , .- : 4 Quantify Sample Report * Study No.:L34865, Set N o . :072303B, Ext.Date:07/23/03, Analyst :K.Risha Page 12 ^ Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\072303B Daikin | Last modified: Sat Jul 26 15:53:34 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 e""', Job Code: 'V Printed: Sat Jul 26 16:00:35 2003 f , Name: 072303B-512 Text: n 1: C8 Acid 4* h iJ I*14"*' \ t * Ii tj I4 n fs fe > H T i: ti FI ' ' ' ' ' Exygen Research, 3058 Research Drive, State College, PA 16801 r: 000041 ..... n Quantify Sample Report Study No.:L34865, Set No.:072303B, Ext.Date07/23/03, AnalystK.Risha Page 13 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SainpleDB\072303B Daikin I J Last modified: Sat Jul 26 15:53:34 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 J o b Code: TV Printed: Sat JUl 26 16:00:35 2003 n I i Name: 072303B-513 Text : i! Ei i t' I t 1; n Exygen Research, 3058 Research Drive, State College, PA 16801 H -- -, " 000042 t ' ' . n . Quantify Sample Report Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, Analyst:K.Risha Page 14 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303B Daikin < ' Last modified: Sat Jul 26 15:53:34 2003 \ ' Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 f * , Job Code: Printed: Sat Jul 26 16:00:35 2003 ; i Name: 072303B-514 Text : i n I: &i i. Exygen Research, 3058 Research Drive, State College, PA 16801 000043 f--l Quantify Sample Report t Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, Analyst:K.Risha Page 15 /H Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303B Daikin ] ! Last modified: Sat Jul 26 15:53:34 2003 1 Method: P:\Data\LCMSMS6\Masslynx\Pluorochemicals.PRO\MethDB\C8 only072503 Last modified: Sat Jul 26 15:54:50 2003 rI* -; Job Code: Printed: Sat Jul 26 16:00:35 2003 r*- l ; Name: 072303B-515 Text: ft* #L 1i '' n r^ 1; n* r~* k -i .. . i. hi i ` Exygen Research, 3058 Research Drive, State College, PA 16801 000044 Quantify Sample Report Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, Analyst :K.Risha Page 16 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\072303B Daikin Last modified: Sat Jul 26 15:53:34 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 Job Code: Printed: Sat Jul 26 16:00:35 2003 Name: 072303B-516 Text: 1: C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000045 Quantify Sample Report Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, Analyst:K.Risha Rage 17 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303B Daikin Last modified: Sat Jul 26 15:53:34 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\C8 only 072503 Last modified: Sat JUl 26 15:54:50 2003 Job Code: Printed: Sat Jul 26 16:00:35 2003 Name: 072303B-517 Text: 1: C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000046 f~> | ; Quantify sample Report ' ' Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, Analyst:K.Risha Rage 18 /~v Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\072303B Daikin ; 1 Last modified: Sat Jul 26 15:53:34 2003 1 Method: P:\Data\LCMSMS6\Masslynx\Pluorochemicals.PRO\MethDB\C8 only072503 Last modified: Sat Jul 26 15:54:50 2003 Job Code: *' Printed: Sat Jul 26 16:00:35 2003 -r-- >: Name: 072303B-518 Text : n rr h * i. : Exygen Research, 3058 Research Drive, State College, PA 16801 000047 Quantify Sample Report Study No.:L34865, Set No.:072303B, Ext.Date;07/23/03, Analyst:K.Risha Page 19 -- k Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303B Daikin j I Last modified: Sat Jul 26 15:53:34 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 r- Job Code: Printed: Sat JUl 26 16:00:35 2003 Name: 072303B-519 Text: 1: C8 Acid L34865-2 072303B-519 Sm (Mn, 2x2) 10CH 5.06 145139376 26-JUI-2003 10:48:25 LC/MS/MS #6 MRM of 1 Channel ES 413 >369 1.34e8 Area n t* ' ...r - p " ' I-r-pr I" Time 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 n i> n f-i' r-r fI r", n Exygen Research, 3058 Research Drive, State College, PA 16801 000048 Quantify Sample Report Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, Analyst:K.Risha Page 20 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\072303B Daikin Last modified: Sat Jul 26 15:53:34 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethPB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 Job Code: Printed: Sat Jul 26 16:00:35 2003 Name: 072303B-520 Text: 1 : C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000049 Quantify Sample Report Study No.:L34865, Set No.:072303B# Ext.Date:07/23/03, Analyst:K.Risha Rage 21 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303B Daikin Last modified: Sat Jul 26 15:53:34 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 Job Code: Printed: Sat Jul 26 16:00:35 2003 Name: 072303B-521 Text: 1: C8 Acid L34865-4 072303B-521 Sm (Mn, 2x2) 100-1 %- 5.02 20768144 26-UI-2003 11:20:00 LC/MS/MS #6 MRM of 1 Channel ES413 >369 1.19e8 Area (> 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 000050 r*. f: Quantify Sample Report Study Nb.:L34865, Set No.:072303b , Ext.Date:07/23/03, Analyst:K.Risha Rage 22 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303B Daikin t Last modified: Sat Jul 26 15:53:34 2003 ' Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 r~ Job Code: Printed: Sat Jul 26 16:00:35 2003 Name: 072303B-522 Text: I: < n h j jr1 ! fD f) Exygen Research, 3058 Research Drive, State College, PA 16801 000051 Quantify Sample Report Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, Analyst:K.Risha Rage 23 , Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SaiqpleDB\072303B Daikin Last modified: Sat Jul 26 15:53:34 2003 * Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 ,-- Job Code: Printed: Sat Jl 26 16:00:35 2003 Name: 072303B-523 Text: f-1 1: C8 Acid XC072303-5, 500 ng/L standard 072303B-523 Sm (Mn, 2x2) 100-1 5.03 173609 26-Jul-2003 11:51:35 LC/MS/MS #6 MRM of 1 Channel ES413 >369 1.12e6 Area 0 - frr 1.00 r -i--j-TT I " r p " r 1r-T | 2.00 3.00 1r y -i' 7.00 i Time 8.00 r n Exygen Research, 3058 Research Drive, State College, PA 16801 0000S2 Quantify Sample Report Study No.:L34865, Set No.:072303B, Ext.Date:07/23/03, Analyst:K.Risha Page 24 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303B Daikin Last modified: Sat Jul 26 15:53:34 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Sat Jul 26 15:54:50 2003 Job Code: Printed: Sat Jul 26 16:00:35 2003 Mame: 072303B-524 Text: 1: C8 Acid X C 072303-6,1000 ng/L standard 072303B-524 Sm (Mn, 2x2) 100n 5.01 315949~ k %: 1 . 7- r r T"i--r t t -| ' 1 ' 11 1 ' i > 1 1 1 n 1.00 2.00 3.00 1 111i 1 4.00 ...i i 5.00 26-JUI-2003 12:07:19 LC/MS/MS #6 MRM of 1 Channel ES413 >369 2.03e6 Area ' 1 1 i ` 1 * i 6.00 7.00 -r-i-i Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000053 n trt1 i F` ' i . - * f' ftf Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L34865 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: 072303BR Karen Risha LC/MS/MS Unit # 6 07/23/03 07/30/03 Exygen ID XC072303-0 XC072303-1 XC072303-2 XC072303-3 XC072303-4 XC072303-5 XC072303-6 L3486S-2 Spk C L34865-1 L34865-5 XC072303-1 XC072303-2 XC072303-3 L34865-2 L34865-2 Rep L34865-4 XC072303-4 XC072303-5 XC072303-6 Sponsor ID - #2, Utilities DSN001 #1, Utilities Field Blank #5, Control - #2, Utilities DSN001 #2, Utilities DSN001 #4, Unidyne DSN006 - - Sample Code c CS CS CS CS CS CS LF S S CS CS CS s s s CS CS CS Run No. 072303BR-701 072303BR-702 072303BR-703 072303BR-704 072303BR-705 072303BR-706 072303BR-707 072303BR-708 072303BR-709 072303BR-710 072303BR-711 072303BR-712 072303BR-713 072303BR-7I4 072303BR-715 072303BR-716 072303BR-717 072303BR-718 072303BR-719 PFOA Found (ng/L) = (peak area - intercept) / slope x DF Recovery (%) = [PFOA found (ng/L)-PFQA 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 10000 10 1000 10000 10000 1000 - - x 100 Peak Area 0 10741 19266 39308 84528 162064 320382 19393 36857 38359 8910 17062 31571 18321 19111 38261 80672 143502 293121 PFOA Found (ng/L) - 541000 1110 116000 506000^ 532000 * 116000 - - Amount PFOA Added (ng/L) 500 - - Recovery (%) - 7000A * - " Standard Curve ; Linear (1/x weighted) Intercept - 2846.40 Slope = 305.706 Coef. O f Det. = 0.995086 CS = Calibration standard C Control sample S = Sample LF = Lab fortified sample FF = Field fortified sample LCS = Laboratory Control Spike CK = Check Standard ND ss Not detected = Response between 0 and LOD NQ = Not quantifiable = Response between LOD and LOQ ASample residue significantly exceeds spiking level; therefore, an accurate recovery cannot be calculated. See data set 080103B for re-extraction at a higher level. + i_P , SetcUW s ti c6 i2o%AM fc--*fvv. Spreadsheet prepared by:_.j t j j / oe>[e>i|3> Itk- ' H i' i f! 000054 ' t i ;t j :i n ~tti i " ii M asslynx - Sample List Sample List: C:\MASSLYNX\Fluoroche nicals.PRO\SampleDB\072303BR Daikin.SPL ' t>l|3t)|i)^Printed: Wed Jul 30 13:25:18 2003 _________ Vial File Name LIMS ID C lient ID Sample D escription 1 1 072303BR-701 -- 2 2 072303BR-702 -- 3 3 072303BR-703 -- 4 4 072303BR-704 -- 5 5 072303BR-705 -- 6 6 072303BR-706 -- 7 7 072303BR-707 -- 8 11 072303BR-708 -- 9 12 072303BR-709 -- 10 13 072303BR-710 -- 11 2 072303BR-711 -- 12 3 072303BR-712 13 4 072303BR-713 -- 14 14 072303BR-714 -- 15 15 072303BR-715 -- 16 16 072303BR-716 -- 17 5 072303BR-717 -- 18 6 072303BR-718 -- 19 7 072303BR-719 -- XC072303-0, 0 ng/L standard XC072303-1,25 ng/L standard XC072303-2,50 ng/L standard XC072303-3, 100 ng/L standard XC072303-4, 250 ng/L standard XC072303-5, 500 ng/L standard X C 072303-6,1000 ng/L standard L34865-2 Spk C, 500 ng/L, DF=10( L34865-1, DF=10 L34865-5, DF=1000 XC072303-1, 25 ng/L standard XC072303-2, 50 ng/L standard XC072303-3, 100 ng/L standard L34865-2, DF=10000 L34865-2 Rep, DF=10000 L34865-4, DF=1000 XC072303-4, 250 ng/L standard XC072303-5, 500 ng/L standard XC072303-6, 1000 ng/L standard ooooss Exygen studyno. L3-I&S Page 1 Page Position: ( 1 , 1 ) M atrix S am ple Type Cone (ng/L) C one B C one C T e st ID DF MS Method -- Blank 0 Standard 25 -- Standard 50 -- Standard 100 -- Standard 250 -- Standard 500 -- Standard 1000 -- QC 500 -- Analyte -- -- Analyte -- -- Standard 25 -- Standard 50 -- Standard 100 -- Analyte -- -- Analyte -- -- Analyte -- -- 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 1 1 1 1 1 1 1 10000 10 1000 1 1 1 10000 10000 1000 1 1 1 PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA i ''in :;n 1 M asslynx - Sample List Sample List: C:\MASSLYNX\Fluorochei iicals.PRO\SampleDB\072303BR Daikln.SPL Printed: Wed Jul 30 13:25:18 2003 I HPLC Method MS Tune File Inj.Volum e 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 000056 : i ""'i *-j i iti m Exygenstudy no. ni Page 2 Page Position: (2,1 ) n i` LC/MS/MS SYSTEM AND OPERATING CONDITIONS n Sponsor Protocol No: NA i\ Exveen Study No: L34865 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 r~> HPLC Equipment: Hewlett Packard (HP) Series 1100 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) (JONESCHROMATOGRAPHY: Part No. FK5962E) fni>r '' Mobile Phase (A) : Mobile Phase (B) : 2 mM Ammonium Acetate in Type I Water Methanol Analyst: Karen Risha I : Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 n t , NO TE: The next 3 pages are com puter generated printouts from n the m asslynx softw are program . T he pages contain the instrum ent settings used for th e analysis o f this data set. 31n A ll Handwritten Peak ID 's by: B1 0 r-' - - t! r~! t1 0000S7 Scanning Method Report Method: C :\MAS SLYNX\ FLUOROCHEMICALS.PRO\ACQUDB\PFOA Last Modified: Wed Mar 26 16:31:10 2003 Printed: Wed Jul 30 13:25:25 2003 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 ) 1 413.00 369.00 0.20 10 10 Page 1 000058 nr i Method Report Method File: fl Last Modified: c:\masslynx\fluorochemicals.pro\acgudb\fluorochems Wednesday, July 30, 2003 13:22:57 Page 1 60.0 40.0 0.0 0.0 H Flow (ml/min) [ ; Stop Time (mins) Min Pressure (bar) Max Pressure (bar) P Oven Temperature Left(C) b ' Oven Temperature Right(C) 0.300 14.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable is j The gradient Timetable contains 9 entries which are : Time r*i 0.00 0.40 1.00 7.00 7.50 9.00 9.50 13.50 14.00 r- 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 ii : 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 D% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 p The Timetable contains 6 entries which are : Time Initial 0.00 0.05 b 0.10 7.95 8.00 F" 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 HP1100 Autosampler Initial Conditions Draw Speed Ih- i Eject Speed (/xl/min) Draw Position (mm) Stop Time (mins) Injection Volume (/xl) Vial Number r' 200.0 200 0.50 14.00 15.0 7 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 Contact4 Off Off Off Off Off Off Pressure 400 400 400 400 400 400 400 400 400 I 000059 Tuning Method Report H Method: C :\MAS SLYNX\FLUOROCHEMICALS.PRO\ACQUDB\FLUOROCHEMS i.i r1 n Page 1 it i fi Dau 395.00 n SOURCE ( ESP- ) Capillary Cone n 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 -21 99 302 Pressures Analyser Vacuum Gas Cell I! fi n i, 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 Rdb 14.0 14.0 1.0 -2 12 15 14 2 16 14.0 ' 14.0 2.0 650 -64 Rdbk 128.5 758.6 000060 r"i j R Quantify Calibration Report : Study No.:L34865, Set No.:072303BR, Ext.Date:07/23/03, Analyst:K.Risha p r~! Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\CurveDB\072303BR Daikin Quantify Sample Report Study No.:L34865, Set No.s072303BR, Ext.Date:07/23/03, Analyst:K.Risha Page 1 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303BR Daikin Last modified: Thu Jul 31 13:46:17 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Thu Jul 31 13:48:53 2003 Job code: Initiate. Printed: Thu JU1 31 13:53:41 2003 Run* To 0 1 Z & t t R r .l\ n ' I Name: 072303BR-701 Text: n M t 1 jn n Exygen Research, 3058 Research Drive, State College, PA 16801 000062 Quantify Sample Report Study No.:L34865, Set No.:072303BR, Ext.Date:07/23/03, AnalystsK.Risha Rage 2 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303BR Daikin Last modified: Thu Jul 31 13:46:17 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Thu Jul 31 13:48:53 2003 Job Code: Printed: Thu Jul 31 13:53:41 2003 Name: 072303BR-702 Text: 1: C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000063 Quantify Sample Report Study No.:L34865, Set No.:072303BR, Ext.Date:07/23/03, Analyst:K.Risha Page 3 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\072303BR Daikin Last modified: Thu Jul 31 13:46:17 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Thu J1 31 13:48:53 2003 Job Code: Printed: Thu Jul 31 13:53:41 2003 Name: 072303BR-703 Text: 1 : C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000064 Quantify Sample Report Study No.:L34865, Set No.:072303BR, Ext.Date:07/23/03, Analyst:K.Risha Page 4 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\072303BR Daikin Last modified: Thu Jul 31 13:46:17 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Thu Jul 31 13:48:53 2003 Job Code: Printed: Thu Jul 31 13:53:41 2003 Marne: 072303BR-704 Text : 1: C8 Acid X C 072303-3,100 ng/L standard 072303BR-704 Sm (Mn, 2x2) 100-1 %- 5.02 3930 30-JU1-2003 14:57:42 LC/MS/MS #6 MRM of 1 Channel ES413 >369 2.57e5 Area 0 T ",-i ,t t --j1' -Ir*". .. I I I* 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 000065 j Quantify Sample Report : Study No.:L34865, Set No.:072303BR, Ext.Dates07/23/03, AnalystsK.Risha Page 5 /-- Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303BR Daikin ' 1 Last modified: Thu Jul 31 13:46:17 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only072503 Last modified: Thu Jul 31 13:48:53 2003 " Job Code: * Printed: Thu Jul 31 13:53:41 2003 Name: 072303BR-705 Text: i: i; is 5 fs . i n Exygen Research, 3058 Research Drive, State College, PA 16801 r** l' 000066 Quantify Sample Report Study No.:L34865, Set No.s072303BR, Ext.Date:07/23/03, Analyst:K.Risha Page 6 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303BR Daikin Last modified: Thu Jul 31 13:46:17 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Thu Jul 31 13:48:53 2003 Job Code: Printed: Thu Jul 31 13:53:41 2003 Name: 072303BR-706 Text: 1: C8 Acid XC072303-5, 500 ng/L standard 072303BR-706 Sm (Mn, 2x2) 10(h %- 30-UI-2003 15:29:04 LC/MS/MS #6 MRM of 1 Channel ES5.01 413 > 3 6 9 1.07e6 Area Q l- ,- r , - T - l - T - r - r - , | - T r I I" I I " I I T I T l I I I I I I I' I I - I 1.00 2.00 3.00 4.00 5.00 T|"| I I T im eV r - | " ' T-- r T T - ] " i I " I I I I I I I I 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000067 Quantify Sample Report Study No.:L34865, Set No.:072303BR, Ext.Date:07/23/03, Analyst:K.Risha Page 7 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303BR Daikin Last modified: Thu Jul 31 13:46:17 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Thu Jul 31 13:48:53 2003 Job Code: Printed: Thu Jul 31 13:53:41 2003 Name: 072303BR-707 Text: 1: C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000068 Quantify Sample Report Study No.:L34865, Set N o . :072303BR, Ext.Date:07/23/03, AnalystsK.Risha Page 8 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRQ\SampleDB\072303BR Daikin Last modified: Thu <Jul 31 13:46:17 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Thu Jul 31 13:48:53 2003 Job Code: Printed: Thu JUl 31 13:53:41 2003 Name: 072303BR-708 Text: 1: C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000069 I ' Quantify Sample Report " -J Study No.:L34865, Set No.:072303BR, Ext.Date:07/23/03, AnalystsK.Risha Page 9 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303BR Daikin ; Last modified: Thu Jul 31 13:46:17 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Thu <Jul 31 13:48:53 2003 Job Code: f- ' Printed: Thu Jul 31 13:53:41 2003 #*"! 1 Name: 072303BR-709 Text: n 1: C8 Acid is l{ r*? it ? Exygen Research, 3058 Research Drive, State College, PA 16801 000070 Quantify Sample Report Study No.:L34865, Set No.:072303BR, Ext.Date:07/23/03, Analyst:K.Risha Page 10 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\072303BR Daikin Last modified: Thu Jul 31 13:46:17 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Thu Jul 31 13:48:53 2003 Job Code: Printed: Thu Jul 31 13:53:41 2003 Name: 072303BR-710 Text: 1: C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000071 Quantify Sample Report Study No.:L34865, Set No.:072303BR, Ext.Date:07/23/03, Analyst:K.Risha Page 11 Sample List: F:\Data\LQ4SMS6\Masslynx\Fluorochemicals.PR0\SaxnpleDB\072303BR Daikin Last modified: Thu Jul 31 13:46:17 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorocheraicals.PRO\MethDB\C8 only 072503 Last modified: Thu Jul 31 13:48:53 2003 Job Code: Printed: Thu Jul 31 13:53:41 2003 Name: 072303BR-711 Text: 1: C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000072 Quantify Sample Report Study No.:L34865, Set No.:072303BR, Ext.Date:07/23/03, Analyst:K.Risha Page 12 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303BR Daikin Last modified: Thu Jul 31 13:46:17 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Thu Jul 31 13:48:53 2003 Job Code: Printed: Thu Jul 31 13:53:41 2003 Name: 072303BR-712 Text: 1: C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000073 ! ' Quantify Sample Report ` Study No.:L34865, Set No.:072303BR, Ext.Date:07/23/03, Analyst:K.Risha Page 13 f l Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303BR Daikin f Last modified: Thu Jul 31 13:46:17 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Thu JUl 31 13:48:53 2003 f*] Job Code: Printed: Thu Jul 31 13:53:41 2003 Name: 072303BR-713 Text: n i: Exygen Research, 3058 Research Drive, State College, PA 16801 000074 Quantify Sample Report Study No.:L34865, Set No.:072303BR, Ext.Date:07/23/03, Analyst:K. Ri sha Page 14 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\SampleDB\072303BR Daikin Last modified: Thu Jul 31 13:46:17 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Thu Jul 31 13:48:53 2003 Job Code: Printed: Thu Jul 31 13:53:41 2003 Name: 072303BR-714 Text: 1 : C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000075 I** , - ; 1 Quantify Sample Report Study No.:L34865, Set No.:072303BR, Ext.Date:07/23/03, Analyst:K.Risha Page 15 f8-' Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303BR Daikin i Last modified: Thu Jul 31 13:46:17 2003 Method: P:\Data\LOMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Thu Jul 31 13:48:53 2003 Tl Job Code: t>~ * 1 Printed: Thu Jul 31 13:53:41 2003 Name: 072303BR-715 Text: }i n ft <. n Exygen Research, 3058 Research Drive, State College, PA 16801 r~ . 000076 1. : Quantify Sample Report Study No.:L34865, Set N o . :072303BR, Ext-Date:07/23/03, Analyst:K.Risha Page 16 <r~? Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\072303BR Daikin * ; Last modified: Thu Jul 31 13:46:17 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Thu <Tul 31 13:48:53 2003 P Job Code: Printed: Thu Jul 31 13:53:41 2003 i ! ' Name: 072303BR-716 Text: ft j/*"* i & -i pp Exygen Research, 3058 Research Drive, State College, PA 16801 000077 n * I , Quantify Sample Report Study No.:L34865, Set No.:072303BR, Ext.Date:07/23/03, AnalystsK.Risha Page 17 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303BR Daikin I I Last modified: Thu Jul 31 13:46:17 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Thu Jul 31 13:48:53 2003 -*! Job Code : f: Printed: Thu Jul 31 13:53:41 2003 ,f1 t > Name: 072303BR-717 s Text : n t. r\ n l 'j Exygen Research, 3058 Research Drive, State College, PA 16801 000078 I i Quantify Sample Report Study No.:L34865, Set No.:072303BR, Ext.Date:07/23/03, Analyst:K.Risha Page 18 -* Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303BR Daikin f * Last modified: Thu Jul 31 13:46:17 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Thu Jul 31 13:48:53 2003 Job Code: Printed: Thu Jul 31 13:53:41 2003 f ! Name: 072303BR-718 " Text : n If 1: C8 Acid c - XC072303-5, 500 ng/L standard r 072303BR-718 Sm (Mn, 2x2) 100^ 5.06 1435021 I %: 1 n ..................1................... .... 1.11.i-i-i 111111 ,"r"r","TT ' 1111111 1.00 2.00 3.00 4.00 5.00 30-Jul-2003 18:38:14 LC/MS/MS #6 MRM of 1 Channel ES413 >369 1.02e6 Area ~Tr1'"'T 1111T ' ' ' ' I'11111 11111Time 6.00 7.00 8.00 ? fa.i ii i n I` n Exygen Research, 3058 Research Drive, State College, PA 16801 000079 jn . - . . i i Quantify Sample Report -. Study No.:L34865, Set No.s072303BR, Ext.Date:07/23/03, AnalystsK.Risha Page 19 f l Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\072303BR Daikin ; ' Last modified: Thu Jul 31 13:46:17 2003 Method: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\C8 only 072503 Last modified: Thu Jul 31 13:48:53 2003 n Job Code: t! ' ' Printed: Thu Jul 31 13:53:41 2003 r*- i i Name: 072303BR-719 Text: n n fk W f*m f- i n Exygen Research, 3058 Research Drive, State College, PA 16801 000080 rs 1n 1 !> ' ri tr -5; fi { \ *H if- r r-! tS H i Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L34865 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: 080103B Karen Risha LC/MS/MS Unit # 7 08/01/03 08/02/03 Exygen ID XC072303-0 XC072303-1 XC072303-2 XC072303-3 XC072303-4 XC072303-5 XC072303-6 Methanol Wash 0106020 Control 0106020 Spk A 0106020 SpkB L34865-2 Spk C L34865-4 Spk D L34865-4 L34865-4 Rep XC072303-1 ' XC072303-2 XC072303-3 XC072303-4 XC072303-5 XC072303-6 Sponsor ID NA NA NA #2, Utilities DSN001 #4, Unidyne DSN006 #4. Unidyne DSN006 #4, Unidyne DSN006 - - Sample Code C CS CS CS CS CS CS c c LCS LCS LF LF S S CS CS CS CS CS CS Run No. 080103B_301 080103B_302 080103BJ03 080103B_304 080103B_305 080103B_306 080103B_307 080103B_308 080103B_309 080103B_310 080103BJ311 080103B_312 080103BJ13 080103B_314 080103B_315 080103B_316 080103B_317 080103B_318 080103B_319 080103B_320 080103B_321 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 2000 1000 1000 1000 - - x 100 Peak Area 137 1796 3403 6549 16882 32700 64982 204 0 3237 32284 40009 24370 10122 10770 1874 3356 6719 16734 32855 65202 PFOA Found (ng/L) - ND 47.0 493 1220000 371000 153000 163000 - Amount PFOA Added (ng/L) - - 50 500 500000 250000 - Recovery (%) . - _ - 94 99 143*+ 87 - --- Standard Curve : Linear (1/x weighted) Intercept = 173.237 Slope = 65.1877 Coef. Of Det. = 0.999367 CS = Calibration standard C = Control sample S = Sample LF = Lab fortified sample FF = Field fortified sample LCS = Laboratory Control Spike *Sample was corrected using tbe data found in set 072303BR. +Unacceptable LF recovery. Sample and spike reextracted. See data set 081203A. CK = Check Standard ND = Not detected = Response between 0 and LOD NQ = Not quantifiable = Response between LOD and LOQ Spreadsheet prepared by:. '"i n 000081 3058 Research Drive Phone: 814-272-1039 H State College, P A 16801 Fax: 814-231-1580 SAMPLE TRANSFER SHEET Protocol Number: __________ NA__________ Exygen Study Number:_______ L34865 Exygen Sample # L34865-2 L34865-4 _ Sponsor Sample # #2, Utilities DSN001 #4, Unidyne DSN006 _ Exygen Sample # . Sponsor Sample # -- _ --_ _ __, -_ _ _ _ -- -- Karen Risha 08/01/03 0700 Requested By (Printed Name/Date/Time) Samples removed fro m :______ s" F Samples removed from: *-- Box#_______ ' ___________ Shelf# B ox# ------ Shelf# Samples transferred to the custody of Samples received from custodian; Samples m oved to Samples removed from Samples returned t o __ O O O & 9 Comments: ? / ' / * i a y s -o Sample Custodian Initials/Date/Time 32- 08I01I03 1& LaboratoiVPersonnel Initials/Date/Time /f/0 Sample Custodian Initials/Date/Time December 19,2002/6 000082 n n fh ; t- h n r! a jhs n r ~: 1 il RESEARCH 3058 Research Drive State Colleg- e, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number: L34865 Matrix: Water Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No. 3 2 - T im e_ ^g Q -- ..................................Date Q & f o i f ^ Initials CLIENT SAMPLE ID na na na #2, Utilities DSN001 #4, Unidyne DSN006 #4, Unidyne DSN006 #4, Unidyne DSN006 EXYGEN ID NUMBER 0106020 Control 0106020 Spk A 0106020 Spk B - L34865-2 Spk C L34865-4 Spk D (0 L34865-4 G> L34865-4 Rep 0 VOLUME (mL) 40.0 40.0 40.0 40.0 40.0 40.0 40.0 FORTIFICATION (ng) _ 2.0 20.0 20000.0 10000.0 - _ - -. - - -_ _- - - - - -- _- - - - - -- _- - - - - -_ - - -- - - -- - - -- - - -- - - -- 0106020 Spk A 0106020 Spk B L34865-2 Spk C L34865-4 Spk D - - - All samples were measured: Time Spiking Solution Used F061803-5 (10 ng/mL) F061803-4 (100 ng/mL) F061803-1 (100000 ng/mL) F061803-1 (100000 ng/mL) - - - Volume Used for Spiking 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 100 pL (200 pL micropipet) _ _ Tnitial/Date JQ k / Ib i 1er o| o : 01 p id b 01 b _ -- Initials. After measuring samples were returned to refrigerator No. 3 2 - Time / 3 0 Q _______ _ Date ____ Initials C om m ents : 200 pL o f 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date: (2QS~ Q&J&fj HOOkUof SNMPUE; U it BRoOrttT v>? To 4t> M L yUTH VifWER-TUeD M L Op t U M Si & m O GM T DP TO H O V L vaATM UAtCfc-fOS- ^ ^F 'IO O . PK.t(l\0B> Analysis Summary: D ata Set: 6I63.W ' Initials/Date: ._1 I _ AC- / 6 & M o 5 Data Set: ~________ Initials/Date: J / ~~ D ata Set:_____________ Initials/Date: ~~_____ / ~_____ Set extraction/analysis data verified by: & U . Date: July 26, 2001/6 000083 - r- 'ti 1 :i '!"'1 1 : 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L34865 MATRIX: Water METHOD: " ANALYTES: PFOA PROTOCOL NUMBER: NA Client ID na na na #2, Utilities DSN001 #4, Unidyne DSN006 #4, Unidyne DSN006 #4, Unidyne DSN006 - Exygen ID 0106020 Control 0106020 Spk A 0106020 SpkB L34865-2 Spk C L34865-4 Spk D L34865-4 L34865-4 Rep - - - - - STEP 1 \/ - - - STEP 2 1 Dilutions (mL/mL) -- - /icv' K o STEP 3 \ - \y - -- -- -- --- - --- - -- -- -- -- -- -- -- -- Dilutions (mL/mL) > - - - - STEP 4 *, - -- -- - - - Reagents/ Materials Methanol C18SPE Type I Water . _ _ . Initials/Date Lot# V05U2.&I NA - ] r- _ -_. -_-> --- HPLC Methanol 450673IM Ammonium Acetate Type I water - w *U & \ NA - *Initials/Date - f i f e C fclttfo 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. fa r* a)bP>7CCO^.C0(l(t& -- -- Initials/Date lc^T ^ *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: July 19,2001/4 000084 '1 ' 'I " T j^ I--- ' ~*?T ' J .~-r ^ -t r*^ MassLynx - Sample List Sample List: Signature: Printed: C:\MassLynx\008-apfo.pro\SampleDB\080103B Daikin.SPL By CENTRE\Karens (Karen Risha) At Friday, August 01, 2003 3:36:27 PM Reason Create Sample S equence. Friday, August 01, 2003 3:36:31 PM U3 Vial File Name LIMS ID C lie n t ID Sample Description 11 22 33 44 55 66 77 8 92 9 31 10 32 11 33 12 34 13 35 14 36 15 37 16 2 17 3 18 4 19 5 20 6 21 7 080103B 301 080103B 302 080103B 303 080103B 304 080103B 305 080103B 306 080103B 307 080103B 308 080103B 309 080103B 310 080103B 311 080103B 312 080103B 313 080103B 314 080103B 315 080103B 316 080103B 317 080103B 318 080103B 319 080103B 320 080103B 321 -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- __ XC072303-0, 0 ng/L Standard -- XC072303-1, 25 ng/L Standard -- XC072303-2, 50 ng/L Standard -- X C 072303-3,100 ng/L Standard -- XC072303-4, 250 ng/L Standard -- XC072303-5, 500 ng/L Standard -- X C 072303-6,1000 ng/L Standard -- Methanol Wash -- 0106020 Control -- 0106020 Spk A, 50 ng/L -- 0106020 Spk B, 500 ng/L -- L34865-2 Spk C, 500000 ng/L, DF=2000 -- L34865-4 Spk D, 100000 ng/L, DF=1000 -- L34865-4, DF=1000 -- L34865-4 Rep, DF=1000 -- XC072303-1, 25 ng/L Standard -- XC072303-2, 50 ng/L Standard -- XC072303-3, 100 ng/L Standard -- XC072303-4, 250 ng/L Standard -- XC072303-5, 500 ng/L Standard -- X C 072303-6,1000 ng/L Standard 000085 n ... i 1 ;::i 1 11 Exygenstudy no. Page 1 of 2 Page Position (1 ,1 ) M a trix S am ple T ype C one (ng/L) C one B C one C T e s t ID _____ Standard 0 _____ __ 0.000000 -- Standard 25 -- -- 0.000000 -- Standard 50 -- -- 0.000000 -- Standard 100 -- -- 0.000000 -- Standard 250 -- -- 0.000000 -- Standard 500 -- -- 0.000000 -- Standard 1000 -- -- 0.000000 -- Blank -- -- -- 0.000000 -- Blank -- -- -- 0.000000 -- QC 50 -- -- 0.000000 -- QC 500 -- -- 0.000000 -- QC 500000 -- -- 0.000000 -- QC 100000 -- -- 0.000000 -- Analyte -- -- -- 0.000000 -- Analyte -- -- -- 0.000000 -- Standard 25 -- -- 0.000000 -- Standard 50 -- -- 0.000000 -- Standard 100 -- -- 0.000000 -- Standard 250 -- -- 0.000000 -- Standard 500 -- -- 0.000000 - - - Standard 1000 -- -- 0.000000 1 '1 1 M assLynx - Sample List Sample List: Signature: Printed: C:\MassLynx\008-apfo.pro\SampleDB\080103B Daikin.SPL By CENTRE\Karens (Karen Risha) At Friday, August 01,2003 3:36:27 PM Reason Create Sample Sequence, Friday, August 01, 2003 3:36:31 PM DF MS Method HPLC Method MS Tune File Inj Volum e 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 2000.000000 1000.000000 1000.000000 1000.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA W ater W ater W ater W ater W ater W ater W ater W ater W ater W ater W ater W ater W ater W ater W ater W ater W ater W ater W ater W ater W ater 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 PFOA Tune 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 000086 1 ' ' 'J ]n ::z :ri Exygen SI NO L 3 S Page 2 of 2 Page Position (2 ,1 ) fl R k- - i' f; n n -. t; ; n P! Jr -i n P"' i; 1. n '' LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: N A E xvsen Study No: L34865 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #7) Computer: IBM IntelliStation M Pro Software: Windows XP Professional: Version 5.1: Service Pack 1 Micromass Limited: MassLynx 4.0 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: M A 10327) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) Mobile Phase (B) 2 mM Ammonium Acetate in Type I Water Methanol . . . 1A Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 P(j NOTE: The next 3 pages are computer generated printouts from the m asslynx software program . The pages contain the instrum ent settings used for the analysis of this data set. A ll Handwritten Peak ID's bv: ] > 3 000087 *n ' Experiment Report File: c:\masslynx\008-apfo.pro\acqudb\008 pfoa.exp n Signature: At f- By Wednesday, June 25,2003 13:45:18 CENTRE\Karens (Karen Risha) Reason Create Experiment File r I' Printed: Friday, August 01,2003 15:35:14 D3 Page 1 Name Default Experiment Creation Time Wed 25 Jun 2003 13:45:18 Instrument Identifier Version Number 1.0 Duration (min) 8.0 Calibration Filename C:\MassLynx\calibration.pro\ACQUDB\NalRbCs032603.cal n Solvent Delay Start 2 Solvent Delay End 2 H Solvent Delay Temperature 2 8.0 15.0 0.0 Solvent Delay Divert Valve Enabled 1 Number Of Functions 1 Function 1 : MRM of 413.00->369.00, Time 0.00 to 8.00, E s pi Type MRM Ion Mode ES- Parameter File c:\masslynx\default.pro\acqudb\defauit.ipr Inter Channel Delay (sec) t1 -i Span(Da) 0.1 0.0 Start Time (min) 0.0 n End Time (min) 8.0 Ch Prnt(Da) Dau(Da) Dwell(s) Cone(V) Coll(eV) Delay(s) 1 413.00 369.00 0.20 10.00 10.00 0.03 pi f i. n iF i' 000088 n Method Report Method Files jT Last Modified C :\MassLynx\008-apfo.pro\ACQUDB\Water Friday, August 01, 2003 15:33:54 Signature At Wednesday, June 25, 2003 13:47:06 By CENTRE\Karens (Karen Risha) Reason Create Inlet Method Printed: Friday, August 01, 2003 15:35:10 01 0 ^ HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 60.0 40.0 0.0 0.0 p Flow (ml/min) 1 Stop Time (mins) r - Min Pressure (bar) Max Pressure (bar) --1 Oven Temperature Left(C) j*j 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 A% 0.00 H 0.40 1 : 1.00 7.00 7.50 p 9.00 ! 9.50 ! 13.50 14.00 3 15.00 B% 60.0 60.0 10.0 10.0 0.0 0.0 60.0 60.0 60.0 60.0 C% 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 40.0 D% Flow (ml/min) Pressure 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0.400 0.0 0.0 0.400 0.0 0.0 0.400 0.0 0.0 0.300 0.0 0.0 0.300 HP1100 LC Pump External Event Timetable The Timetable contains 4 entries which are : 1; Time Column Switch Contactl Contact2 Initial Off Off Off P 0.00 Off Off Off 0.10 Off On On 8.00 Off Off Off Contact3 Off Off Off Off Contact4 Off Off Off Off k . HP1100 Autosampler Initial Conditions Draw Speed p-i Eject Speed (pl/min) I e Draw Position (mm) ; Stop Time (mins) Injection Volume(pi) ^ Vial Number I ] Thermostat On ; Thermostat Temperature(C) 200.0 200 0.10 15.00 15.0 1 12.0 t Page 1 400 400 400 400 400 400 400 400 400 400 000089 i Tune Parameters File: Signature: Printed: C:\MassLynx\008-apfo.PRO\ACQUDB\PFOA Tune.lPR At By Reason Wednesday, June 25, 2003 13:46:34 CENTREVKarens (Karen Risha) Create Tune File Friday, August 01,2003 15:35:19 Page 1 3G7 O 3G8 O 3C9 o Type Daughter Scan Source (ES-) Capillary (kV) Cone (V) Hex 1 (V) Aperture (V) Hex 2 (V) Source Temperature (C) Desolvation Temperature (C) Cone Gas Flow (L/Hr) Desolvation Gas Flow (L/Hr) Analyser LM 1 Resolution HM 1 Resolution Ion Energy 1 Entrance Collision Exit LM 2 Resolution HM 2 Resolution Ion Energy 2 Multiplier (V) Pressure Gauges Pirani Pressure(mbar) Penning Pressure(mbar) MUX Configuration Probe Start Mass 367 Settings 3.00 10 0.0 0.0 0.0 100 300 128 709 Settings 15.0 15.0 1.0 -2 10 2 15.0 15.0 2.2 700 3.24e-3 OFF Standard 370.0 371 O End Mass 372 Readbacks -2.93 -11 Set Mass 413 101 300 Readbacks 8 9 11 -696 000090 i 3Quantify Calibration Report ' Study No.: L34865, Data Set: 080103B, Ext.Date: 08/01/03, Analyst: K.Risha | Dataset; ! *Signature:. ; Printed: C:\Massl_ynx\Q08-apfo.pro\080103B Daikin.qld At Sunday, August 03, 2003 6:29:18 AM By CENTREVKarens (Karen Risha) Reason Process and review data set Sunday, August 03, 2003 6:30:24 AM Method: C:\MassLynx\008-apfo.PRO\MethDB\072403 PFOA.mdb 25 Jul 200315:26:26 P Calibration: 03 Aug 2003 06:25:49 M. '^ Compound name: PFOA r - Correlation coefficient: r = 0.999934, rA2 = 0.999867 f Calibration curve: 65.1877 * x + 173.237 1 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None Page 1 of 1 < Quantify Sample Report Study No.: L34865, Data Set: 080103B, Ext.Date: 08/01/03, Analyst: K.Risha P Dataset: C:\MassLynx\008-apfo.pro\080103BDaikin.qld l , Signature: At Sunday, August 03, 2003 6:29:18 AM By CENTRE\Karens (Karen Risha) p. Reason Process and review data set j. Printed:______Sunday, August 03, 2003 6:30:24 AM Initials. Date Run#H Method: C:\MassLynx\008-apfo.PRO\MethDB\072403 PFOA.mdb 25 Jul 2003 15:26:26 r * Calibration: 03 Aug 2003 06:25:49 M . ` Name: 080103B 301 Date: 02-Aug-2003 t- Time: 02:58:00 Description: XC072303-0, 0 ng/L Standard - PFOA * 08013B_301 Smooth(Mn,2x3) XC072303-0, 0 ng/L Standard PFOA 5.44 Page 1 of 21 ^ i_ T o _.Q8oloa.fi MRM of 1 channel,ES413 > 369 i n l: f \ : ... f"i h- . ......... ....... - - ... ............. Exy9en Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000092 r Quantify Sample Report Study No.: L34865, Data Set: 080103B, ExtDate: 08/01/03, Analyst: K.Risha Page 2 of 21 jP Dataset: C:\MassLynx\008-apfo.pro\080103BDaikin.qid ; Signature: At Sunday, August 03, 2003 6:29:18 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set P \ 1 Printed: ------ Sunday, August 03, 2003 6:30:24 AM :------ :-------------------------------------------- !-- -----------------;----- --------------- Name: 080103BJ302 P Date: 02-Aug-2003 E Time: 03:14:48 " Description: XC072303-1, 25 ng/L Standard T , pF0A L ' 080103B_302 Smooth(Mn,2x3) XC072303-1,2 5 ng/L Standard PFOA 5.46 1796 MRM of 1 channel,ES413 > 3 6 9 1.884e+004 %_ M ii 0.64 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 fy t/ fi n Exygen R esearch, 3 0 5 8 R esearch Drive, State College, P A 16801, D ata acquired on L C M S M S #7 000093 fwj_________________________________________________________________________________________________ i Quantify Sample Report 1 Study No.: L34865, Data Set 080103B, ExtDate: 08/01/03, Analyst: K.Risha Page 3 of 21 f " Dataset: f Signature: ^ k <_P_rin_te_d:;___' C:\MassLynx\008-apfo.pro\080103B Daikin.qld At Sunday, August 03, 2003 6:29:18 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Sunday, August 03, 2003 6:30:24 AM ____________ Name: 080103B_303 p 8Date: 02-Aug-2003 Time: 03:31:36 Description: XC072303-2, 50 ng/L Standard t PFOA * 080103B 303 Smooth(Mn,2x3) XC072303-2, 50 ng/L Standard fm 100 | PFOA 5.46 3403 MRM of 1 channel,ES413 > 369 3.138e+004 8.000.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50 t- in v.f iM * Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 i t - .. v 000094 r , --------------------------------------;------;----------------------- :----------------------------------------------------------------------- Quantify Sample Report ' Study No.: L34865, Data Set: 080103B, Ext.Date: 08/01/03, Analyst: K.Risha P Dataset: Signature: ^ Printed: C:\MassLynx\008-apfo.pro\080103B Daikin.qld At Sunday, August 03,2003 6:29:18 AM By CENTREVKarens (Karen Risha) Reason Process and review data set Sunday, August 03, 2003 6:30:24 AM _ Name: 080103B_304 r * Date: 02-Aug-2003 Time: 03:48:25 Description: XC072303-3,100 ng/L Standard PFOA 080103B_304 Smooth(Mn,2x3) XC072303-3,100 ng/L Standard PFOA 5.45 P a g e 4 of 21 MRM of 1 channel,ES413 > 369 #fr / - r I4 Exygen Research, 3058 R esearch Drive, State College, P A 16801, Data acquired on L C M S M S #7 000095 I Quantify Sample Report ` Study No.: L34865, Data Set: 080103B, Ext.Date: 08/01/03, Analyst: K.Risha P Dataset: , Signature: ^ i Printed: C:\MassLynx\008-apfo.pro\080103B Daikin.qld At Sunday, August 03, 2003 6:29:18 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Sunday, August 03, 2003 6:30:24 AM ^ Name: 080103B_305 p D a te : 02-Aug-2003 Time: 04:05:19 ' Description: XC072303-4, 250 ng/L Standard 1 PFOA : ' 0801Q3B_305 Smooth(Mn,2x3) XC072303-4, 250 ng/L Standard 100--1 PFOA 5.45 16882 Pa9e 5 of 21 MRM of 1 channel,ES4 1 3 > 369 1.488e+005 %- 0 WfT 0.50 T ' , , ,-| n n I i t , I I I I ixyi n 1.00 1.50 2.00 2.50 3.00 TT-pT i i p m - i Mi l -p i n-rn-TT- T=fT- m - r p - i n I , , n Jn n T[TTi 1 |Y, iT| n iV| i i f ip iT T |T T V rp r 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50 t t | min 8.00 r, fi t f- n ^ Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on ICMSMS#7 iV 0000^6 i Quantify Sample Report v Study No.: L34865, Data Set: 080103B, Ext.Date: 08/01/03, Analyst: K.Risha Page 6 of 21 H Dataset: C:\MassLynx\008-apfo.pro\080103B Daikin.qld Signature: At Sunday, August 03, 2003 6:29:18 AM By CENTRE\Karens (Karen Risha) ^ Reason Process and review data set : Printed: Sunday, August 03, 2003 6:30:24 AM i .------------------------------------------------------------------------------------------------- Name: 080103B_306 f"" Date: 02-Aug-2003 Time: 04:22:01 Description: XC072303-5,500 ng/L Standard k ,PFOA 080103B_306 Smooth(Mn,2x3) XC 072303-5,500 ng/L Standard PFOA 5.45 MRM of 1 channel,ES413 >369 if** i\ f*. 1 \ ^ Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 t! 000097 1 Quantify Sample Report i Study No.: L34865, Data Set: 080103B, Ext.Date: 08/01/03, Analyst: K.Risha n Dataset: ! 5Signature: ' , Printed: C:\MassLynx\008-apfo.pro\080103B Daikin.qld At Sunday, August 03, 2003 6:29:18 AM By CENTREVKarens (Karen Risha) Reason Process and review data set Sunday, August 03, 2003 6:30:24 AM Name: 080103B_307 H D a te : 02-Aug-2003 Time: 04:38:53 Description: XC072303-6,1000 ng/L Standard PFOA ? ` 080103B_307 Smooth(Mn,2x3) XC072303-6, 1000 ng/L Standard jw- 100-1 ' PFOA 5.45 64982 Pa9e 7 of 21 MRM of 1 channel,ES413 >369 5.561e+005 %n T VlT'1111 1111TT i l 11 1 1 1 1n 1 11 min 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50 8.00 *~i * . f* ' f- ' V iJ Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on L C M S M S #7 00009S  'Quantify Sample Report * 'Study No.: L34865, Data Set: 080103B, ExtDate: 08/01/03, Analyst: K.Risha HDataset: j Signature: " 'P rinted: C:\MassLynx\008-apfo.pro\080103B Daikin.qld At Sunday, August 03, 2003 6:29:18 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Sunday, August 03, 2003 6:30:24 AM Name: 080103B_308 r Date: 02-Aug-2003 . Time: 04:55:41 Description: Methanol Wash rrvjM f nsnm.iR 3 0 8 SmooHVMn.2x3i PFOA P age 8 of 21 MRM of 1 channel,ES- t Vr - , I t Exygen Research, 3 0 5 8 Research Drive, State College, PA 16801, D ata acquired on L C M S M S #7 000099 , ? 1 ;Quantify Sample Report 4 ' Study No.: L34865, Data Set: 080103B, ExtDate: 08/01/03, Analyst: K.Risha H Dataset: ` Signature: ^ , Printed: C:\MassLynx\008-apfo.pro\080103B Daikin.qld At Sunday, August 03, 2003 6:29:18 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Sunday, August 03, 2003 6:30:24 AM Name: 080103B 309 P Date: 02-Aug-2003 Time: 05:12:36 Description: 0106020 Control PFOA P ag e 9 of 21 * rs H Exygen R esearch, 30 58 R esearch Drive, State College, PA 16801, D ata acquired on L C M S M S #7 OOOIOO PiQuantify Sample Report * Study No.: L34865, Data Set: 080103B, ExtDate: 08/01/03, Analyst: K.Risha f" i Dataset: f Signature: ^ I Printed: C:\MassLynx\008-apfo.pro\080103B Daikin.qld At Sunday, August 03, 2003 6:29:18 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Sunday, August 03, 2003 6:30:24 AM Name: 080103B_310 F Date: 02-Aug-2003 - Time: 05:29:35 Description: 0106020 Spk A, 50 ng/L PFOA i 080103BJ310 Smooth(Mn,2x3) 0106020 Spk A, 50 ng/L 100- PFOA 5.45 3237 Page 10 of 21 MRM of 1 channel,ES4 1 3 > 369 3.534e+004 %_ 0.66 TTfi-r,i|Mn" ~ffrjTn`rpTTFfiTwfrT T"'T` 11'T1' 111 min 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50 8.00 n n s i H Exygen R esearch, 3058 R esearch Drive, State College, PA 16801, D ata acquired on L C M S M S #7 OOOlOl n -- ------- -- -- --- -------------------------------------I i Quantify Sample Report ` Study No.: L34865, Data Set: 080103B, Ext.Date: 08/01/03, Analyst: K.Risha H Dataset: Signature: ^ } i Printed: C:\MassLynx\008-apfo.pro\080103B Daikin.qld At Sunday, August 03,2003 6:29:18 AM By CENTREVKarens (Karen Risha) Reason Process and review data set Sunday, August 03, 2003 6:30:24 AM Name: 080103B_311 r Date: 02-Aug-2003 Time: 05:46:22 Description: 0106020 Spk B, 500 ng/L * PFOA t 080103B_311 Smooth(Mn,2x3) 0106020 Spk B, 500 ng/L 100 PFOA 5.45 32284 P a g e 11 of 21 MRM of 1 channel,ES413 > 369 2.828e+005 ' %- 0 " I I I " i .-rn y rrT i I I . I I 1 I H | ' I1 II 111 . | 11 . I I ' 1' 1I I ' ' . I 1 I| . ' - I | 11 | I 1 0.50 1.00 1.50 2.00 2.50 3.00 3.50 n | i 11 1 | 1 1 1 q .' i i i | n 11 p n q i rii i | i 1,i 4.00 4.50 5.00 5.50 6.00 I r ' I ' n l-| 1 1 1 1 1 1 ! I i i' n M| min 6.50 7.00 7.50 8.00 r~! ii j f& A , r n Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 o ... (" 000102 1*1_____ -__________________________________________________ t i Quantify Sample Report 4 Study No.: L34865, Data Set: 080103B, Ext.Date: 08/01/03, Analyst: K.Risha H Dataset: * Signature: ki ? _P_r_i_n_t_e_d__:___ C:\MassLynx\008-apfo.pro\080103B Daikin.qld At Sunday, August 03, 2003 6:29:18 AM By CENTREVKarens (Karen Risha) Reason Process and review data set Sunday, August 03, 2003 6:30:24 AM Name: 080103B_312 r Date: 02-Aug-2003 j Time: 06:03:19 Description: L34865-2 Spk C, 500000 ng/L, DF=2000 i PFOA * 080103B_312 Smooth(Mn,2x3) L34865-2 Spk C, 500000 ng/L, DF=2000 100- PFOA 5.45 40009 P a g e 12 of 21 MRM of 1 channel,ES4 1 3 > 369 2.468e+005 k %t 0 r*-' ri'n'Ti'v ,","i | n rr-| i r,T| i , nr, .Tp Mrr, n Ti f i I .. |"I , I i | I I I i p i i r| , iTrjTiTTyri 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 r p - n I fVi I I [ I I I I I I r u I ! I I . | min 6.50 7.00 7.50 8.00 n ii /f*. k; tI H t. i A *v--fra- !> f* Exygen R esearch, 30 58 Research Drive, State College, PA 16801, Data acquired on L C M S M S #7 000103 m ______ -- --------------- -- -- .--------------------------I Quantify Sample Report ' Study No.: L34865, Data Set: 080103B, Ext.Date: 08/01/03, Analyst: K.Risha H Dataset: C:\MassLynx\008-apfo.pro\080103B Daikin.qld k Signature: At Sunday, August 03,2003 6:29:18 AM By CENTRE\Karens (Karen Risha) ^ Reason Process and review data set t Printed: Sunday, August 03, 2003 6:30:24 AM k ---- ---------- ------------------------------- ;---------- Name: 080103B_313 r Date: 02-Aug-2003 j Time: 06:20:06 Description: L34865-4 Spk D, 100000 ng/L, DF=1000 P PFOA : 080103B_313 Smooth(Mn,2x3) L34865-4 Spk D, 100000 ng/L, DF=1000 PFOA 5.45 P ag e 13 of 21 MRM of 1 channel,ES413 > 369 t n r: {' r. i' * 'I Exygen R esearch, 3 0 5 8 R esearch Drive, State College, PA 16801, D ata acquired on L C M S M S #7 \ 000104 |~j______________ __________________________________________ \ i Quantify Sample Report ' Study No.: L34865, Data Set: 080103B, Ext.Date: 08/01/03, Analyst: K.Risha H Dataset: C:\MassLynx\008-apfo.pro\080103B Daikin.qld \ Signature: At Sunday, August 03, 2003 6:29:18 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set t : Printed: Sunday, August 03, 2003 6:30:24 AM - ______________________________________________________________________________________ Name: 080103B_314 P Date: 02-Aug-2003 ; Time: 06:36:54 Description: L34865-4, DF=1000 : PFOA l 080103B_314 Smooth(Mn,2x3) L34865-4, DF=1000 r-- 100- i- f %- PFOA 5.45 10122 P a g e 14 of 21 MRM of 1 channel,ES413 >369 8.630e+004 TTTTTrri. rtT-pTf rTTY'n-rTprrn"|-rrr T-r[-ri-n=p-mTrr min 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50 8.00 f k t Exygen R esearch, 3 0 5 8 R esearch Drive, S tate College, PA 16801, D ata acquired on L C M S M S #7 000105 m -------------- -- --- ---- ---------------- ----------------r \ Quantify Sample Report * Study No.: L34865, Data Set: 080103B, Ext.Date: 08/01/03, Analyst: K.Risha p , Dataset: , 1Signature: '' Printed: C:\MassLynx\008-apfo.pro\080103B Daikin.qld At Sunday, August 03, 2003 6:29:18 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Sunday, August 03, 2003 6:30:24 AM Name: 080103B_315 r Date: 02-Aug-2003 - Time: 06:53:47 Description: L34865-4 Rep, DF=1000 * PFOA 1 080103B_315 Smooth(Mn,2x3) L34865-4 Rep, DF=1000 100- PFOA 5.46 10770 P ag e 15 of 21 MRM of 1 channel,ES413 > 369 9.002e+004 %- TT-rpn-r 0.50 1.00 1.50 2.00 2.50 3.00 i q tt 3.50 4.00 4.50 11'',11 11'1," 11111, , r r l 1r l ' P 11 1 I r r i 1 I r i 'r i I r n ' TT l r , T i m i n 5.00 5.50 6.00 6.50 7.00 7.50 8.00 r-i ti r; f "*: 11 * f Exygen R esearch, 30 5 8 R esearch Drive, S tate College, PA 16801, D ata acquired on L C M S M S #7 000106 <______ _________ --______________ ___________ _______ - ---------------- ---- ------- f: Quantify Sample Report ' Study No.: L34865, Data Set: 080103B, ExtDate: 08/01/03, Analyst: K.Risha H Dataset: ^Signature: jpPrinted: C:\MassLynx\008-apfo.pro\080103B Daikin.qld At Sunday, August 0 3 ,2003 6:29:18 AM By CENTREVKarens (Karen Risha) Reason Process and review data set Sunday, August 03, 2003 6:30:24 AM Name: 080103B_316 (" Date: 02-Aug-2003 * Time: 07:10:46 Description: XC072303-1, 25 ng/L Standard ! PFOA i 080103B_316 Smooth(Mn,2x3) XC072303-1,25 ng/L Standard . 100- f*-. f! ' %_ PFOA 5.45 1874 P ag e 16 of 21 MRM of 1 channel,ES413 >369 1.948e+004 0.66 6.42 t, min 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50 8.00 r~> ^l *4 $: ir- [ p; f"i !* n i Exygen R esearch, 3058 R esearch Drive, S tate College, P A 16801, Data acquired on L C M S M S # 7 000107 I 'Quantify Sample Report 1 Study No.: L 34865, Data Set: 080103B , Ext.Date: 0 8 /01/03 , Analyst: K.Risha H Dataset: Signature: ^ f Printed: C:\MassLynx\008-apfo.pro\080103B Daikin.qld At Sunday, August 03, 2003 6:29:18 AM By CENTREVKarens (Karen Risha) Reason Process and review data set Sunday, August 03, 2003 6:30:24 AM Name: 080103B_317 T D ate: 02-Aug-2003 ' Time: 07:27:33 Description: XC072303-2, 50 ng/L Standard rH I PFOA 080103B_317 Smooth(Mn,2x3) XC072303-2, 50 ng/L Standard f-- 100-, PFOA 5.45 3356 P a g e 1 7 o f 21 MRM of 1 channel,ES413 >369 2.935e+004 %n h r~i $ ' : 0.65 min 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50 8.00 (Is. i n t! nS i m I. r-i Exygen R esearch, 3058 R esearch Drive, State College, PA 16801, Data acquired on L C M S M S #7 000108 'Quantify Sample Report Study No.: L 34865, D a ta Set: 080103B , E x tD ate : 08 /01/03, Analyst: K.Risha f l Dataset: E ' Signature: Printed: C:\MassLynx\008-apfo.pro\080103B Daikin.qld At Sunday, August 03, 2003 6:29:18 AM By CENTREVKarens (Karen Risha) Reason Process and review data set Sunday, August 03, 2003 6:30:24 AM Name: 080103B_318 {"'Date: 02-Aug-2003 Time: 07:44:23 Description: XC072303-3,100 ng/L Standard ! PFOA > 080103B_318 Smooth(Mn,2x3) X C 072303-3,100 ng/L Standard I--^ 100- PFOA 5.46 6719 IIM ' %- P a g e 18 o f 21 MRM of 1 channel,ES413 >369 5.997e+004 0.66 0.50 1.00 M [-rn-rp=PrT|-ri-rq-t=Tri'|Tm [iin!r,i 1.50 2.00 2.50 3.00 --- _ . T T T T T T r r n - T T T r n r i T r r r p r r T p T r r ^ f m j r r r r ^ j'-r-TT) r r r r j n - n j , I i f p I , , | T , i I , r , M j I I , , | . n I j i i M , m i n 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50 8.00 k. fi- - n *? n n i i k1 n f rn * Exygen R esearch, 3 0 5 8 R esearch Drive, State College, PA 16801, D ata acquired on L C M S M S #7 0109 I \Q uantify S am ple R eport ' Study No.: L34865, D a ta Set: 0 8 0 1 03B, Ext.Date: 08/01/03 , Analyst: K.Risha PI Dataset: ^ ^Signature: Printed: C:\MassLynx\008-apfo.pro\080103B Daikin.qld At Sunday, August 03, 2003 6:29:18 AM By CENTREMCarens (Karen Risha) Reason Process and review data set Sunday, August 03, 2003 6:30:24 AM Name: 080103B_319 F* Date: 02-Aug-2003 * Time: 08:01:14 Description: XC072303-4, 250 ng/L Standard r PFOA , 080103BJ319 Smooth(Mn,2x3) XC072303-4, 250 ng/L Standard I-- 100-- f**. l. I - % PFOA 5.46 16734 r1 /1 r- TTTTrr 0.50 r T-r r r r r - pT -rrp^-rrr-T -rr iy r r n ^ r r i Ty n -rr p tt r p - r 1.00 1.50 2.00 2.50 3.00 TT" 3.50 i - r p n i"j ,-n rp -r> T | ! n - r p r 4.00 4.50 5.00 P age 19 of 21 MRM of 1 channel,ES413 >369 1.457e+005 TiTTfrpp-rrrfrn-ipr^T-p-r t=H min 6.50 7.00 7.50 8.00 r . n t n ? ' <-- ! i Exygen Research, 3 0 5 8 R esearch Drive, State College, PA 16801, D a ta acquired on L C M S M S #7 OOOllO * Quantify Sample Report 1 ; Study No.: L34865, D ata Set: 0 8 0 1 03B, Ext.Date: 08/01/03 , Analyst: K.Risha f l Dataset: 5Signature: n Printed: C:\MassLynx\008-apfo.pro\080103B Daikin.qld At Sunday, August 03, 2003 6:29:18 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Sunday, August 03, 2003 6:30:24 AM Name: 0801Q3B_320 F" Date: 02-Aug-2003 ; Time: 08:18:03 Description: XC072303-5, 500 ng/L Standard | PFOA " ' 080103BJ320 Smooth(Mn,2x3) XC072303-5,500 ng/L Standard PFOA 5.45 P ag e 2 0 of 21 MRM of 1 channel,ES413 >369 r-~i rn Exygen R esearch, 30 58 R esearch Drive, State College, P A 16801, Data acquired on L C M S M S #7 OOOlll i .Quantify Sample Report Study No.: L34865, Data Set: 080103B, ExtDate: 08/01/03, Analyst: K.Risha PDataset: f Signature: ^ P Printed: C:\MassLynx\008-apfo.pro\080103B Daikin.qld At Sunday, August 03, 2003 6:29:18 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Sunday, August 03, 2003 6:30:24 AM Name: 080103B_321 r~ Date: 02-Aug-2003 ! Time: 08:35:01 Description: XC072303-6,1000 ng/L Standard PPFOA 1 080103B_321 Smooth(Mn,2x3) XC072303-6, 1000 ng/L Standard PFOA 5.45 Page 21 of 21 MRM of 1 channel,ES. 413 > 369 F** i4 ^----1 : m f1 &3 L1 Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on L C M S M S #7 i' 000112 f! i` 1 n t *; i1 n i: ; (T"' f*"* r"! Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L34865 PFOA 413-> 369 NA R A W 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: 081203A Karen Risha LC/MS/MS Unit # 7 08/12/03 08/12/03 Exygen ID XC080603-0 XC080603-1 XC080603-2 XC080603-3 XC080603-4 XC080603-5 XC080603-6 Methanol Wash 0106020 Control 0106020 Spk A 0106020 SpkB L34865-2 Spk C L34865-2 L34865-2 Rep XC080603-1 XC080603-2 XC080603-3 XC080603-4 XC080603-5 XC080603-6 Sponsor ID - - - - - NA NA NA #2, Utilities DSN001 #2, Utilities DSN001 #2, Utilities DSN001 - - - Sample Code C CS CS CS CS CS CS c c LCS LCS LF S S CS CS CS CS CS CS Run No. 081203A_101 081203A_102 081203A_103 08I203A_104 081203A_105 081203A_106 081203A_107 081203A_108 081203A_109 081203A_110 081203A_111 081203A_112 081203A_113 081203A_U4 081203A_115 081203A_116 081203A_117 081203A_118 081203A_119 081203A_120 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)-PFQA fonnd in control (ng/L)]_____ x 100 amount PFOA added (ng/L) Dilution Factor - - - 1 1 1 2000 1000 .1000 - - Peak Area 0 834 1719 3259 8499 16424 32522 0 0 1566 15928 20766 23176 23939 877 1874 3431 9073 17353 35979 PFOA Found (ng/L) - Amount PFOA Added (ng/L) - Recovery (%) - - - - - - - ND 45.2 465 1210000 677000 700000 - - 50 500 500000 - - 90 93 107 - -- - -- - --- --- --- Standard Curve : Linear ( 1/x weighted) Intercept = 22.2204 Slope = 34.1757 Coef. Of Det. = 0.997395 CS = Calibration standard C = Control sample S = Sample LF = Lab fortified sample FF = Field fortified sample LCS a=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: Il 14 n 000113 Exygen % / g ^ R E S E A 8.CH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number. L34865 Matrix: Water Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator N o .. 3 Z I i Time. M L Date_ & - LInitials CLIENT SAMPLE ID EXYGEN ID NUMBER VOLUME (mL) FORTIFICATION (ng) na 0106020 Control 40.0 - n na 0106020 Spk A 40.0 2.0 na 0106020 SpkB 40.0 20.0 #2, Utilities DSN001 L34865-2 SpkC 40.0 20000.0 #2, Utilities DSN001 L34865-2 40.0 - #2, Utilities DSN001 L34865-2 Rep 40.0 - - - -- - - -- _ _ -- - - -- - - -- - - -- i1 _ _ - -- -- _ - -- _ n (a. j _ - -- -- - - -- - -- - - -- 0106020 Spk A 0106020 SpkB L34865-2 SpkC _ _ Spiking Solution Used F061803-5 (10 ng/mL) F061803-4 (100 ng/mL) F 0 6 1803-1 (100000 ng/mL) .. - - -- All samples were measured: Time 1 3 5 0 _______ D ate. Volume Used for Spiking 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) - - - Initial/Date /c fP' / o f l i t b /obios - Initials After measuring samples were returned to refrigerator No. 3.2.____ Time H \ S D ate. H = -Initials. Comments: 200 pL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date: c ltilo ! Analysis Summary: Data Set: 0 8 l2 & A Data Set: --_______ n Data S et:__ H Set extraction/analysis data verified by: _ Initials/Date:. Initials/Date:. Initials/Date:. /08/ix|d3> Date: July 26, 2001/6 000114 "3 ' 1 :n ZI "'3 1 J RC H 3058 Research Drive State College, PA 16801 "3 .. 1 ::n :u Phone: 814-272-1039 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L34865 METHOD:. $$ PROTOCOL NUMBER: NA MATRIX: Water ANALYTES: PFOA Client ID na na na #2, Utilities DSN001 #2, Utilities DSN001 #2, Utilities DSN001 . Exygen ID 0106020 Control 0106020 Spk A 0106020 Spk B L34865-2 Spk C L34865-2 L34865-2 Rep . _ _ . . ,, . . _ . _ _ _ - STEP 1 STEP 2 Dilutions (mL/mL) - ~ STEP 3 Dilutions (mL/mL) -- < tfM o oP%x> T1 \ r % * x/ _- _- - -- - -- - -- __ - -- - .. - - __ - -- _- - __- - - _- - __ - _- - \ l___ - - - - - - ** - - - - - - - - - *lnitials/Date - obS 3 STEP 1: SPE column clean-up STEP 2: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP 3: LC/MS/MS analysis STEP 4: LC/MS/MS reanalysis. 0 8 Fl i f e -- STEP 4 - - - - Reagents/ Materials !yuT Lot# Methanol C18 SPE Type I Water D3I2&I NA Initials/Date - HPI.c u - - Methanol W 1 3 Ammonium Acetate Type I water V ^ / S 5 _____ NA - Initials/Date 0g> < > 3 ^Initials and date under each step indicates the personnel that performed this step. $$ 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: 63 M y 19,2001/4 000115 ifr--' J f T T ff 'l 1 ::1 ] ---- T ^ T jj -py "3 MassLynx - Sample List Sample List: Signature: Printed: C:\MassLynx\008-APF02.PRO\SampleDB\081203A.SPL By CENTRE\Karens (Karen Risha) At Tuesday, August 12, 2003 1:49:34 PM Reason Create Sample Sequence rid e t eTuesday, August 12, 2003 1:49:37 PM Vial File Name LIMS ID Client ID Sample Description 11 22 33 44 55 66 77 8 92 9 71 10 72 11 73 12 74 13 75 14 76 15 2 16 3 17 4 18 5 19 6 20 7 081203A 101 081203A 102 081203A 103 081203A 104 081203A 105 081203A 106 081203A 107 081203A 108 081203A 109 081203A 110 081203A 111 081203A 112 081203A 113 081203A 114 081203A 115 081203A 116 081203A 117 081203A 118 081203A 119 081203A 120 ___ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- XC080603-0, 0 ng/L Standard XC080603-1,25 ng/L Standard XC080603-2, 50 ng/L Standard XC080603-3,100 ng/L Standard XC080603-4, 250 ng/L Standard XC080603-5, 500 ng/L Standard XC080603-6,1000 ng/L Standard Methanol Wash 0106020 Control 0106020 Spk A, 50 ng/L 0106020 Spk B, 500 ng/L L34865-2 Spk C, 500000 ng/L, DF=2000 L34865-2, DF=1000 L34865-2 Rep, DF=1000 XC080603-1,25 ng/L Standard XC080603-2, 50 ng/L Standard XC080603-3, 100 ng/L Standard XC080603-4, 250 ng/L Standard XC080603-5, 500 ng/L Standard XC080603-6,1000 ng/L Standard 000116 Exygenstudyno.3H84S Page 1 of 2 Page Position (1,1) Matrix Sample Type Cone (ng/L) Cone B Cone C Test ID Analyte 0.000000 -- Standard 25 -- -- 0.000000 -- Standard 50 -- -- 0.000000 -- Standard 100 -- -- 0.000000 -- Standard 250 -- -- 0.000000 -- Standard 500 --- -- 0.000000 -- Standard 1000 -- 0.000000 -- Blank -- -- -- 0.000000 -- Blank -- -- -- 0.000000 -- QC 50 -- -- 0.000000 -- QC 500 -- -- 0.000000 -- QC 500000 -- 0.000000 -- Analyte ... -- -- 0.000000 -- Analyte -- -- -- 0.000000 -- Standard 25 -- -- 0.000000 -- Standard 50 -- -- 0.000000 -- Standard 100 -- -- 0.000000 -- Standard 250 -- -- 0.000000 -- Standard 500 -- -- 0.000000 -- Standard 1000 -- -- 0.000000 i i ::i 7 ' i ~ r :i t 'i r :i n MassLynx - Sample List Sample List: Signature: Printed: C:\MassLynx\008-APF02.PRO\SampleDB\081203A.SPL By CENTRE\Karens (Karen Risha) At Tuesday, August 12, 2003 1:49:34 PM Reason Create Sample Sequence Tuesday, August 12, 2003 1:49:37 PM i DF MS Method HPLC Method MS Tune File Inj Volume 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 2000.000000 1000.000000 1000.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 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 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 000117 Exygenstudyno. J crs6n!e^is- Page 2 of 2 Page Position (2 ,1 ) LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exvsen Study No: L34865 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #7) Computer: Software: IBM IntelliStation M Pro Windows XP Professional: Version 5.1: Service Pack 1 Micromass Limited: MassLynx 4.0 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Quat Pump HP V acuum Degasser HP Autosampler HP Column Oven HPLC Column: Genesis C-8, 5 cm x 2.1 mm i.d. x 4 p (Exygen ID: M A10327) (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 m asslynx software program. The pages contain the instrum ent settings used for the analysis of this data set. All Handwritten Peak ID's by 000118 Experiment Report File: c:\masslynx\008-apfo2.pro\acqudb\008 pfoa.exp Signature: At Thursday, August 07,2003 09:44:44 By CENTREVKarens (Karen Risha) Reason Create MS Method pi Printed: Tuesday, August 12, 2003 13:55:02 Page 1 0^ * Name Default Experiment Creation Time Thu 07 Aug 2003 09:44:44 Instrument Identifier Version Number 1.0 Duration (min) 8.0 Calibration Filename C:\MassLynx\calibration2.PRO\ACQUDB\NalRbCs081103.cal Solvent Delay Start 2 8.0 i ] Solvent Delay End 2 Solvent Delay Temperature 2 15.0 0.0 Solvent Delay Divert Valve Enabled 1 Number Of Functions 1 i Function 1 : MRM of 413.00->369.00, Time 0.00 to 8.00, ES- n y i Type MRM Ion Mode ES- Parameter File c:\masslynx\default.pro\acqudb\default.ipr n Inter Channel Delay (sec) 0.1 Span(Da) 0.0 Start Time (min) 0.0 f"*, End Time (min) 8.0 i Ch Prnt(Da) Dau(Da) Dwell(s) Cone(V) Coli(eV) Deiay(s) 1 413.00 369.00 0.20 10.00 10.00 0.03 f* I r' 000119 Method Report Method File: p"1 Last Modified: P' < . . - Signature: Printed: C :\Mas sLynx\008 -A?FC>2.PRO\ACQUDB\Water Tuesday, August 12, 2003 13:06:36 At Thursday, August 07, 2003 09:43:42 By CENTRE\Karens (Karen Risha) Reason Create inlet method Tuesday, August 12, 2003 13:55:06 Page 1 H HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 60.0 40.0 0.0 0.0 rr Flow (ml/min) i Stop Time (mins) ' Min Pressure (bar) Max Pressure (bar) pmm Oven Temperature Left(C) ) ; Oven Temperature Right(C) j1 HP1100 LC Pump Gradient Timetable 0.300 15.0 0 400 35.0 35.0 1 The gradient Timetable contains 10 entries which are : i Time A% B% C% D% Flow (ml/min) Pressure 0.00 60.0 40.0 0.0 0.0 0.300 n 0.40 60.0 40.0 0.0 0.0 0.300 tfc-4' 1.00 10.0 90.0 0.0 0.0 0.300 7.00 10.0 90.0 0.0 0.0 O'.300 7.50 0.0 100.0 0.0 0.0 0.300 ri i 9.00 9.50 0.0 60.0 100.0 40.0 0.0 0.0 0.0 0.400 0.0 0.400 13.50 60.0 40.0 0.0 0.0 0.400 14.00 60.0 40.0 0.0 0.0 0.300 r*! 15.00 60.0 40.0 0.0 0.0 0.300 HP1100 LC Pump External Event Timetable * ! The Timetable contains 4 entries which are L Time Column Switch Contactl Contact2 Initial Off Off Off 0.00 Off Off Off - . 0.10 t-. 8.00 Off On On Off Off Off Contact3 Off Off Off Off Contact4 Off Off Off Off n 1- : HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (1/min) t i Draw Position (mm) Stop Time (mins) Injection Volume(ul) Vial Number fe J* Thermostat Thermostat On Temperature(QC) 200.0 200 0.10 15.00 15.0 1 12.0 400 400 400 400 400 400 400 400 400 400 > n i. n ? 000120 fnj Tune Parameters File: C:\MassLynx\008-APFO2.PRO\ACQUDB\PFOA Tune.lPR nr ! Signature: At I ! By Thursday, August 07, 2003 09:48:23 CENTRE\Karens (Karen Risha) n Printed: Reason Create Tune File Tuesday, August 12, 2003 13:55:33 i! Page 1 i f"i j Type Daughter Scan l Source (ES-) Capillary (kV) 0 -Ll Cone (V) Hex 1 (V) Aperture (V) Hex 2 (V) n Source Temperature (C) i. Desolvation Temperature (C) Cone Gas Flow (L/Hr) Desolvation Gas Flow (L/Hr) P l i Analyser LM 1 Resolution n HM 1 Resolution t .* Ion Energy 1 Entrance Collision rnt. .* Exit b * LM 2 Resolution HM 2 Resolution Ion Energy 2 ri\ Multiplier (V) 1 Pressure Gauges f**. Pirani Pressure(mbar) ** Penning Pressure(mbar) MUX Configuration n Probe Start Mass 367 Settings 3.00 10 0.0 0.0 0.0 100 300 132 716 Settings 15.0 15.0 1.0 -2 10 2 15.0 15.0 2.0 700 3.35e-3 OFF Standard End Mass 372 Readbacks -2.94 -11 Set Mass 413 100 300 Readbacks 8 9 12 -696 000121 r_-------------------------------------------------------=,-------------------------------------------------------- ' Quantify Calibration Report Page 1 of 1 ' Study No.: L34865, Data Set: 081203A, ExtDate: 08/12/03, Analyst: K.Risha P Dataset: ; Signature: ` Printed: C:\MassLynx\008-APF02.PRO\081203A.qld At Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Method: C:\MassLynx\008-APFO2.PRO\MethDB\PFOA 080603.mdb 11 Aug 2003 07:33:46 ^C a lib ra tio n : 13 Aug 2003 07:28:11 Compound name: PFOA Correlation coefficient: r = 0.998697, rA2 = 0.997395 JHCalibration curve: 34.1757 * x + 22.2204 1 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None Quantify Sample Report Study No.: L 34865, Data Set: 081203A , Ext.Date: 0 8 /12/03 , Analyst: K.Risha 7* Dataset: , Signature: _ ' Printed: C:\MassLynx\008-APF02.PRO\081203A.qld At Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Initiais Date Method: C:\MassLynx\008-APF02.PRO\MethDB\PFOA080603.mdb 11 Aug 2003 07:33:46 Calibration: 13 Aug 2003 07:28:11 Name: 081203A_101 *_Date: 12-Aug-2003 5 Time: 17:12:40 v Description: XC080603-0, 0 ng/L Standard Page 1 of 20 n \t t< Exygen R esearch, 3058 R esearch Drive, State College, PA 16801, Data acquired on L C M S M S #7 000123 ; Q uantify Sam ple R eport * Study No.: L34865, Data Set: 081203A , Ext.Date: 08/12/03, Analyst: K.Risha f " Dataset: Signature: `' ^ l Printed: C:\MassLynx\008-APF02.PRO\081203Aqld At Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Name: 081203A_102 I" 'D ate: 12-Aug-2003 Time: 17:29:31 Description: XC080603-1, 25 ng/L Standard gum i PFOA 081203A_102 Smooth(Mn,2x3) XC080603-1, 25 ng/L Standard PFOA 5.36 Page 2 of 20 MRM of 1 channel,ES413 > 369 k1 t: jn- ti ;. Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LC M S M S #7 000124 ; Quantify Sample Report Study No.: L34865, D a ta Set: 08 12 03 A , E x tD a te : 0 8 /12/03 , Analyst: K.Risha PDataset: ` Signature: jpPrinted: C:\MassLynx\008-APF02.PRO\081203A.qld At Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Name: 081203AJ03 I Date: 12-Aug-2003 * Time: 17:46:17 Description: XC080603-2, 50 ng/L Standard PFOA 081203A 103 Smooth(Mn,2x3) XC080603-2, 50 ng/L Standard PFOA 5.35 Page 3 of 20 MRM of 1 channel,ES413 >369 1` * `I rr Exygen Research, 3 0 5 8 R esearch Drive, State College, PA 16801, D ata acquired on L C M S M S # 7 000125 [ , Quantify Sample Report Study No.: L34865, Data Set: 081203A, ExtDate: 08/12/03, Analyst: K.Risha P Dataset: Signature: ^ i Printed: C:\MassLynx\008-APF02.PRO\081203A.qld At Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Name: 081203A 104 f Date: 12-Aug-2003 I Time: 18:03:07 Description: XC80603-3,100 ng/L Standard f^PFOA 081203A 104 Smooth(Mn,2x3) XC080603-3, 100 ng/L Standard PFOA 5.36 Page 4 of 20 MRMof1channel,ES413 >369 t- t ' ! t, Exygen R esearch, 3 0 5 8 Research Drive, State College, PA 16801, D ata acquired on L C M S M S # 7 000126 F"""1' i Quantify Sample Report ! "Study No.: L34865, Data Set: 081203A, Ext.Date: 08/12/03, Analyst: K.Risha pDataset: P Signature: __ Printed: tj C:\MassLynx\008-APF02.PRO\081203A.q!d At Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Name: 081203AJ05 P Date: 12-Aug-2003 ; Time: 18:20:04 Description: XC080603-4, 250 ng/L Standard I PFOA 1 081203A_105 Smooth(Mn,2x3) XC080603-4, 250 ng/L Standard PFOA 5.36 Page 5 of 20 MRM of 1 channel,ES413 >369 . Ir i i; Exygen R esearch, 30 5 8 R esearch Drive, S tate College, PA 16801, D ata acquired on L C M S M S #7 000127 r>_:____________________ :_______ :______ ,_____________ :_______________ :_____ Quantify Sample Report Page 6 of 20 Study No.: L34865, Data Set: 081203A, Ext.Date: 08/12/03, Analyst: K.Risha P Dataset: Signature: ^ ! Printed: C:\MassLynx\008-APF02.PRO\081203A-qld At Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Name: 081203AJ06 P D ate: 12-Aug-2003 ! Time: 18:36:53 Description: XC080603-5, 500 ng/L Standard <***! ' I PFOA f 081203A J06 Smooth(Mn,2x3) XC080603-5, 500 ng/L Standard " ' 100- PPOA 5.36 16424 MRM of 1 channel,ES413 >369 1 ,404e+005 %- 0.50 1.00 1.50 2.00 2.50 3.00 n - r m i -f l H r p T M r i r u -n -n r | Tn -i-r n 'i. 3.50 4.00 4.50 5.00 t t< I t; Exygen Research, 30 58 R esearch Drive, State College, P A 16801, D ata acquired on L C M S M S #7 000128 H ______________________________________________________________ I Q uantify Sam ple R eport Study No.: L34865, D ata Set: 081203A , Ext.Date: 08 /12/03, Analyst: K.Risha i Dataset: ^ Signature: | Printed: C:\MassLynx\008-APF02. PRO\081203A.qld At Wednesday, August 13, 2003 7:28:37 AM By CENTREVKarens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Name: 081203A_107 r*Date: 12-Aug-2003 Time: 18:53:54 Description: XC080603-6,1000 ng/L Standard ; PFOA * 08120 3 A J 0 7 Smooth(Mn,2x3) XC080603-6,1000 ng/L Standard PFOA 5.36 Page 7 of 20 MRM of 1 channel,ES413 >369 ti tJ n 0% fbc* i 4 rn rt Exygen R esearch, 3 0 5 8 Research Drive, State College, PA 16801, Data acquired on L C M S M S #7 000129 j" .----------------------------------------------------------------------------------------:-------------h Quantify Sample Report Study No.: L34865, Data Set: 081203A, Ext. Date: 08/12/03, Analyst: K.Risha Dataset: ` Signature: f Printed: C:\MassLynx\008-APF02.PRO\081203A.qld At Wednesday, August 13, 2003 7:28:37 AM By CENTREVKarens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Name: 081203AJ08 f"`Date: 12-Aug-2003 Time: 19:10:44 Description: Methanol Wash PFOA 081203A J08 Smooth (Mn,2x3) Methanol Wash 1/ Page 8 of 20 MRM of 1 channel,ES413 >369 n nf s ^ Exygen R esearch, 30 5 8 R esearch Drive, State College, PA 16801, D ata acquired on L C M S M S # 7 000130 I Quantify Sample Report ' Study No.: L34865, D ata Set: 081203A , E xtD ate : 08 /12/03, Analyst: K.Risha " 'Dataset: f Signature: j Printed: C:\MassLynx\008-APF02.PRO\081203A.qld At Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Name: 081203A_109 ""Date: 12-Aug-2003 1 Time: 19:27:42 Description: 0106020 Control PFOA 081203A 109 Smooth(Mn,2x3) 0106020 Control 1/ Page 9 of 20 MRM of 1 channel,ES413 >369 ti nI' P # .i l> Exygen R esearch, 3 0 5 8 R esearch Drive, State College, PA 16801, D ata acquired on L C M S M S #7 000131 t ----------------------------------------------------------------------------------------------- ;------------------------------------- -------------------------- -------- ------ Quantify Sample Report Page 10 of 20 ' Study No.: L34865, Data Set: 081203A, Ext.Date: 08/12/03, Analyst: K.Risha T Dataset: f Signature: f^Printed: C:\MassLynx\008-APF02.PRO\081203A.qld At Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Name: 081203A_110 fD a te : 12-Aug-203 r Time: 19:44:45 Description: 0106020 Spk A, 50 ng/L pPFOA 081203A J10 Smooth(Mn,2x3) 0106020 Spk A, 50 ng/L PFOA 5.35 MRM of 1 channel,ES413 >369 t t n. Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 H. 000132 f Quantify Sample Report Study No.: L34865, D ata Set: 081203A , E x tD a te : 08/12/03, Analyst: K.Risha r * Dataset: * Signature: j>p' P'!_r_i_n_t_e_d_:___ C:\MassLynx\008-APF02.PRO\081203A.qld At Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Name: 081203A_111 PDate: 12-Aug-2003 k Time: 20:01:45 Description: 0106020 Spk B, 500 ng/L pPFOA L 081203A_111 Smooth(Mn,2x3) 0106020 Spk B, 500 ng/L PFOA 5.36 P a g e 11 o f 2 0 MRM of 1 channel,ES413 > 369 1.328e+005 --, "T-,......... , im - m , min 7.00 7.50 8.00 f f* i - I' p-i I1 f Exygen Research, 3 0 5 8 R esearch Drive, State College, PA 16801, D ata acquired on LC M S M S #7 000133 fc ------------ 1---------------------------------------------------------------------i Quantify Sample Report r Study No.: L34865, Data Set: 081203A, ExtDate: 08/12/03, Analyst: K.Risha f " Dataset: I Signature: --, ! Printed: C:\MassLynx\008-APF02.PRO\081203A.qld At ' Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Name: 081203AJ12 r*Date: 12-Aug-2003 j1 'Time: 20:18:42 Description: L34865-2 Spk C, 500000 ng/L, DF=2000 pPFOA i 081203A J12 Smooth(Mn,2x3) L34865-2 Spk C, 500000 ng/L, DF=2000 PFOA 5.35 Page 12 of 20 MRM of 1 channel,ES413 > 369 n ' fj n (; r* ! Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 I; i ' ' 000134 | Quantify Sample Report ' Study No.: L 3 48 65 , D ata Set: 081203A , E x tD a te : 0 8 /12/03 , Analyst: K.Risha f " Dataset: Signature: r 1_P_r_in_t_e_d: C:\Massl_ynx\008-APF02.PRO\081203A.qld At Wednesday, August 13, 2003 7:28:37 AM By CENTREVKarens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Name: 081203AJ13 Date: 12-Aug-2003 i Time: 20:35:34 Description: L34865-2, DF=1000 PFOA I 081203A 113 Smooth(Mn,2x3) L34865-2, DF=1000 PFOA 5.36 Page 13 of 20 MRM of 1 channel.ES413 >369 il -ii i Exygen Research, 3058 Research Drive, State College, P A 16801, Data acquired on L C M S M S #7 000135 ;J-' i ; Q uantify Sam ple R eport Study No.: L34865, Data Set: 081203A , Ext.Date: 08 /12/03 , Analyst: K.Risha r * Dataset: I Signature: * Printed: C:\MassLynx\008-APF02.PRO\081203A.qld At Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Wednesday, August 13,2003 7:29:16 AM Name: 081203A_114 r*D ate: 12-Aug-2003 f Time: 20:52:28 Description: L34865-2 Rep, DF=1000 PFOA 081203A 114 Smooth(Mn,2x3) L34865-2 Rep, DF=1000 ---- ---- ------------------------------------------ --- Page 14 of 20 PFOA 5.35 MRM of 1 channel,ES413 >369 I n i j ^f .i! ( Exygen R esearch, 30 5 8 Research Drive, S tate College, PA 16801, D ata acquired on L C M S M S # 7 000136 f*"1Q u a n tify S a m p le R e p o rt r Study No.: L34865, D ata Set: 081203A , Ext.Date: 0 8 /1 2 /0 3 , Analyst: K.Risha r Dataset: ^Signature: F" Printed: C:\MassLynx\008-APF02.PRO\081203A.qld At Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Name: 081203A_115 Date: 12-Aug-2003 Time: 21:09:21 Description: XC080603-1, 25 ng/L Standard r PFOA Page 15 of 20 n t' l i rn f: v. > n Ii? Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 n 000137 H "" -------------------------------------------------------------------------------------------------- Quantify Sample Report ' Study No.: L34865, Data Set: 081203A, Ext.Date: 08/12/03, Analyst: K.Risha r Dataset: \ Signature: ' f*Printed: C:\MassLynx\008-APF02.PRO\081203A.qld At Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Ristia) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Name: 081203A_116 r~ Date: 12-Aug-2003 t Time: 21:26:02 Description: XC080603-2, 50 ng/L Standard f~ PFOA f J081203A_116 Smooth(Mn,2x3) " XC080603-2, 50 ng/L Standard PFOA 5.37 Page 16 of 20 MRM of 1 channel,ES413 >369 t H t IIf I; m f1 Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 H. 000138 f Q uantify Sam ple R eport Study No.: L34865, D ata Set: 081203A , E xtD ate : 08/12/03, Analyst: K.Risha ["Dataset: Signature: : Printed: C:\MassLynx\008-APF02.PRO\081203A.qld At Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Name: 081203A_117 [""Date: 12-Aug-2003 I Time: 21:42:51 Description: XC080603-3,100 ng/L Standard P p FOA I 081203A 117 Smooth(Mn,2x3) X C 080603-3,100 ng/L Standard PFOA 5.36 Page 17 of 2 0 MRM of 1 channel, ES413 >369 n i fr *1 i: k P {' H I Exygen Research, 3 0 5 8 R esearch Drive, State College, PA 16801, D ata acquired on L C M S M S #7 000139 f Q uantify Sam ple R eport 1 Study No.: L34865, D a ta Set: 081203A , Ext-Date: 08/12/03, Analyst: K.Risha r Dataset: t Signature: f'Printed: C:\Massl_ynx\008-APF02.PRO\081203Aqld At Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM Name: 081203A_118 "Date: 12-Aug-2003 Time: 21:59:44 Description: XC080603-4, 250 ng/L Standard rP F O A i 081203A J18 Smooth(Mn,2x3) ' XC080603-4,250 ng/L Standard PFOA 5.35 P age 18 of 20 MRM of 1 channel,ES413 >369 t< i n Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 n .... 000140 / / / p i -------- ;-----------------;------------------------------------------------------------- ----- !------------ ^ j Q uantify Sam ple R eport ' Study No.: L34865, D ata Set: 081203A , Ext.Date: 08 /12/03, Analyst: K.Risha :------ :--------- :-- ------------------------ Page 19 of 20 r Dataset: C:\MassLynx\008-APF02.PRO\081203A.qld | Signature: At Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set r Printed: Wednesday, August 13, 2003 7:29:16 AM ft j ----------------------------------------------------- ------------------------------------------------ ------------------------------------------- :------------------------------- Name: 081203A_119 r Date: 12-Aug-2003 \ Time: 22:16:31 Description: XC080603-5, 500 ng/L Standard j PFOA [ 081203A J19 Smooth(Mn,2x3) XC080603-5,500 ng/L Standard PFOA 5.36 MRM of 1 channel,ES413 > 369 H ir""\ tfb n n Exygen Research,3058 Research Drive, State College, PA 16801, D ata acquired on L C M S M S #7 000141 Q uantify Sam ple R eport Study No.: L34865, D ata Set: 081203A , Ext.Date: 08 /12/03, Analyst: K.Risha r Dataset: : Signature: [Printed: C:\MassLynx\008-APF02.PRO\081203A.qld At Wednesday, August 13, 2003 7:28:37 AM By CENTRE\Karens (Karen Risha) Reason Process and review data set Wednesday, August 13, 2003 7:29:16 AM . Name: 081203A_120 [""Date: 12-Aug-2003 f Time: 22:33:33 Description: XC080603-6,1000 ng/L Standard MMRh ! PFOA I 081203A 120 Smooth(Mn,2x3) XC080603-6,1000 ng/L Standard PFOA 5.35 Page 20 of 20 MRM of 1 channel,ES413 > 369 P] 1 Ii I( w r Exygen R esearch, 3058 R esearch Drive, State College, P A 16801, Data acquired on L C M S M S #7 000142