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^Precise Research. \ Proven Results AR226-2501 Analytical Report Fluorochemical Characterization of Water Samples DuPont Washington Works Exygen Resareh Laboratory Report No. 008-046B {Revision 1) Testing Laboratory . Exygen Research, inc. 3058 Research Drive State College, PA 16801 Requester Michael D. Aucoin URS Corporation Barley M ill Plaza Bldg 27 Room 2121 Lancaster Pike and R t 141 W ilmington, DE: ,19805 RJZ032545 EID185019 T IntrodEciion " " Results are reported for the analysis of water samples received by Exygen Research (Centre Analytical Laboratories, Inc.) (Exygen) from DuPont Corporation. The Exygen study number assigned to the project is 008-046. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) was requested for all samples. A total of 11 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 Comoound Name Ammonium Perfluorooctanoate Acronvm APPO 2. SampPeRecefph . ; '- The samples were submitted in individual plastic containers, cooled with wet ice. Samples were collected on 10/11/01. Samples were received on 10/12/01. Chain-of-custody information is presented in Attachment C. 3, H oM tiff Times . The analytical method used was validated against a maximum holding time of 14 days in water samples. All samples were analyzed within 14 days of collection. 4 Methods - AnalyticalandSPrepmaforyh 4.1 LC/MS/MS 4.1.1 Sample Preparation for LC/MS/MS Analysis Water samples were initiatty 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,BSPE cartridge. The cartridge was eluted with 40% methanol: water. The eluate was discard!. The cartridge was then eluted with 100% methanol. A 5 mL portion cf methanol was collected for analysis by LC/MS/MS. This treatment resulted in an eightfold concentration of the samples prior to analysis. 4.13. Sample Analysis by LC/MS/MS In HPLC, an aliquot of extract is injected and passed through a liquid-phase chromatographic column. Based on the affinity of the analyte for the stationary phase in the column relative to PAGE2 OFS RJZ032546 EXD185020 the liquid mobile phase, the analyte is retained for a characteristic amount of time. Following HPLC separation, ES/MS provides a rapid and accurate means for analyzing a wide range of organic compounds, including fluorochemicals. Electrospray is generally operated at relatively mild temperatures; molecules are ionized, fragmented, and detected. Ions characteristic of known fluorochemicals are observed and quantitated against standards. A Hewlett-Packard HP1100 HPLC system coupled to a Micromass Ultima MS/MS was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Samples were extracted on 10/1T/01. Samples were analyzed by MS/MS between 10/17/01 and 10/19/01. Raw analytical data can be found in Attachment D. & Analysis. ' 5.1 Calibration A e-point calibration curve was analyzed at the beginning of the analytical sequence and throughout the run for the compounds of interest. The catenation points were prepared at Q, 50,100, 250, 500, and 1000 ng/L (ppt). 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 sam e SPE procedure used for samples. For the results reported here, calibration criteria were m et 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 to 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 every field sample at concentrations erf 500 ng/L. Matrix spike recoveries are given in Attachment B. All samples showed matrix spike recoveries between 70 and 130% .. 5.5 Duplicates All field samples were analyzed to duplicate. Results are given along with the sample results in Attachment A. PAGE3 OF5 RJZ032547 EID185021 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%. 5.7 Sample Related Comments There are no other sample related comments associated with this sample s e t 6- DalatSammatjjr- - , ., >.' . V -o. Please se e Attachment A for a detailed listing of the analytical results. All results are reported in (ng/L) parts per trillion. ? Wata/Smpl Retention- Samples are disposed of one month after the report is issued unless otherwise specified. All electronic data is archived on retrievable media and hard copy reports are stored In data folders maintained by Exygen. &- Attachments. 8.1 AttachmentA: Results 32 Attachment B: MatrixSpike Recoveries 8.3 Attachment C: Chain of Custody 8.4 Attachment D: LC/MS/MS Raw Analytical Data 8.5 Attachment E Standards Data PAGE4 OF5 RJZ032548 EID185022 Other Lab Members Contributing to Data Karen Smith PAOE50FS RJZ032549 EID185023 kPrecise Research. \ Proven Results. Exvhen Research Laboratory Report 0Q8-046B Revisioin 1 This revisin was performed to report results as ammonium perfluorooctanoate (APFO) to conform tb historical reporting practices. Additional quality control data was also added at the request o f DuPont. /'J o h n M. Flaherty Date exygen-com RJZ032550 EID185024 s i. i ! s RJZ032551 EID185025 Analytical ResultiuPant Washington Works DuPont Sample Identification APFO (ng/L) WWK-D-adg-1-Main \ WWK-D-Bldg-1-Main (laboratory duplicate) WWK-G-Bldg-1-Mali>2 \ WWK-G-Bldg-1-Main-2 (laboratory duplicate) WWK-G-We#-332 \ WWK-G-Wei-332 (laboratory duplicate) WWK-D-BMg-231 \ WWK-D-Bldg-231 (laboratory duplicate) WWK-D-BWa-293 \ WWK-D-BMg-293 (laboratory dupBcate) \ WWK-D-Lubeck-Offlca \ WWK-D-Lubeck-Office (laboratory duplicate) VWVK-G-LPWD-WeB-F \ WWK-G-LPWD-Well-F (laboratory duplicate) \ WWK-e-LPWD-Well-A ' WWK-G-LPWD-Well-A (laboratory duplicate) WWK-Q-LPWD-WbB-B WWK-G-LPWD-Wei-B (laboratory duplicate) WWK-K-FBLK-1 WWK-K-FBLK-2 507 463 471 463 493 469 450 459 423 390 621 605 288 264 684 581 .. 568 '.N D ND / / l 13 S 5 uS *7* 2JLO ss LimHof Detection (LOD) tor th e procedure is appoximately'7,5 ng/L lim it of Quantitaflon (LOQ) tor the procedure is 50 ng/L \ H D -Com pound not detected \ HQ - Compound delected a t a level betw een th e LOD and LOQ, R esult to not quantifiable. ND<LOD<HQ<LOQ y0t 7-/2. UH 8 3058 Research Drive State College, PA 16801, USA VJ : 814J27Z1039 Ft 814.231.1580 exygen.oom RJZ032552 EID185026 L \ B 5 i t sX 1> * ! ? !* I !I >5 i RJZ032553 EXD185027 Attachment B: LC/MS/MS Laboratory Spike Recovery Sam ple ID: | WWK-D-Bldg-1-Main | Spiked A m ount (ng/L): | 500 | Ip f Sample Concentration (ng/L) 487 Matrix Spike Result (ng/L) 844 Matrix Spike Result (% Recovery) 71.4 Criteria (Pass/Fail) PASS Lower Recovery Limit: 70 Upper Recovery Limit: 130 I Concentrations represent amounts present as the perfluorooctanoate anion. RJZ032554 EID185028 Attachment B: LC/MS/MS Laboratory Spike Recovery Sam ple ID: | WWK-G-Bldg-1-Main-21 Spiked Amount (ng/L): | 500 [ fPF Sample Concentration (ng/L) 453 Matrix Spike Result (ng/L) 901 Matrix Spike Result (% Recovery) 89.6 Criteria (Pass / Fail) PASS Lower Recovery Limit: | 70 | Upper Recovery Limit: I 130 I Concentrations represent amounts present a s the perfiuorooctanoate anion. RJZ032555 EID185029 Attachment B: LC/MS/MS Laboratory Spike Recovery Sam ple ID: | WWK-G-Well-332 | Spiked Amount (ng/L): | 500 | Ipfo Sample Concentration (ng/L) 479 Matrix Spike Result (ng/L) 909 Matrix Spike Result (% Recovery) 86.0 Criteria (Pass / Fail) PASS Lower Recovery Limit: | 70 | Upper Recovery Limit: | 130 | Concentrations represent amounts present a s the perfluorooctanoate anion. i RJZ032556 EID185030 Attachment B: LC/MS/MS Laboratory Spike Recovery Sam ple ID: 1 WWK-D-Bidg-231 | Spiked A m ount (ng/L): [ 500 | Ipf Sample Concentration (ng/L) 432 Matrix Spike Result (ng/L) 967 Matrix Spike Result (% Recovery) 107.0 Criteria (Pass / Fail) PASS Lower Recovery Limit: [ 70 | Upper Recovery Limit j 130 | Concentratbns represent amounts present as the perfluorooctanoate anion. RJZ032557 EID185031 Attachment B: LC/MS/MS Laboratory Spike Recovery Sam ple ID: | WWK-D-Bldg-293 | Spiked A m ount (ng/L): | 500 | fPF Sample Concentration (ng/L) 406 Matrix Spike Result (ng/L) 926 Matrix Spike Result {% Recovery) 104.0 Criteria (Pass / Fail) PASS Lower Recovery Limit 70 Upper Recovery Limit: 130 Concentrations represent amounts present as the perfluorooctanoate anion. RJZ032558 EID185032 Attachment B; LC/MS/MS Laboratory Spike Recovery Sam ple ID: I WWK-D-Lubeck Office | Spiked A m ount (ng/L): 1 500 1 |PFOA Sample Concentration (ng/L) 597 Matrix Spike Result (ng/L) . 1080 Matrix Spike Result (% Recovery) 96.6 Criteria (Pass / Fail) PASS Lower Recovery Limit I 70 | Upper Recovery Limit | 130 | Concentrations represent amounts present as the perfluorooctanoate anion. s< R JZ032559 EID185033 Attachment B: LC/MS/MS Laboratory Spike Recovery sa m p le ID: 1WWK-G-LPWD-Well F 1 Spiked A mount (ng/L): I 500 ~| Ip f Sample Concentration (ng/L) Matrix Spike Result (ng/L) Matrix Spike Result (% Recovery) Criteria (Pass / Fail) ; 277 715 87.6 PASS Lower Recovery Limit: | 70 | Upper Recovery Limit: I 130 | Concentrations represent amounts present a s the perfluorooctanoate anion. RJZ032560 EID185034 Attachment B: LC/MS/MS Laboratory Spike Recovery Sam ple ID: | WWK-G-LPWD-Well A | Spiked Am ount (ng/L): [ 500 | |PFOA Sample Concentration (ng/L) 675 Matrix Spike Result (ng/L) 1105 Matrix Spike Result {% Recovery) 86.0 Criteria (Pass/Fail) PASS Lower Recovery Limit: I 70 1 Upper Recovery Limit | 130 | Concentrations represent amounts present as the perfluorooctanoate anion. RJZ032561 EID185035 Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: I WWK-G-LPWD-WeH B I Spiked Amount (ng/L): | 500 I |_ _ ! Sample Concentration (ng/L) 558 Matrix Spike Result (ng/L) 979 Matrix Spike Result (% Recovery) 84.2 Criteria (Pass/Fail) PASS Lower Recovery Limit | 70 | Upper Recovery Limit | 130 | Concentrations represent amounts present as the perfiuorooctanoate anion. RJZ032562 EID185036 c t \ i ?- !i ? i . S- I < 1 RJZ032563 EID185037 1 B B S B 3 1 S i S S n w i 011271S wwk-D-Bldg-1-Maln 10-12-0110:30 WATER 0112720 0112721 WWK-G-Bldg-1- 10-12-01 10:30 Maln-2 WWK-G-Well-33Z 10-12-01 10:30 WATER WATER 0112722 WWK-D-Bldg-231 10-12-01 10:30 WATER 0112723 WWK-K-FBLK-1 10-12-01 10:30 WATER 0112724 WWK-K-FBLK-2 10-12-01 10:30 WATER 0112725 WWK-D-Bldg-293 10-12-01 io:so WATER 0112726 YVWK-D-Lubeck- 10-12-01 10:30 WATER 0112727 0112728 0112729 WWK-G-LPWDWell-F WWK-G-LPWDWell-A WWK-G-LPWDWell-B 10-12-01 10:30 10-12-01 10:30 10-12-01 10:30 . WATER WATER WATER Exygen Research SampleLoginReport StudyNumfaen 008*046 Protocol; NA John Flaherty John Flaherty John Flaherty John Flaherty John Flaherty John Flaherty John Flaherty John Flaherty John Flaherty John Flaherty John Flaherty LAWRENCE O 10-12-01 LAWRENCE O 10-12-01 LAWRENCE O 10-12-01 LAWRENCE 0 10-12-01 LAWRENCE O 10-12-01 LAWRENCE O 10-12-01 LAWRENCE 0 10-12-01 LAWRENCE 0 10-12-01 LAWRENCE O 10-12-01 LAWRENCE 0 10-12-01 LAWRENCE 0 10-12-01 a I COOLER e COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 COOLER 6 C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A C-WET ICE-A . 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S l-fefl' \Y * ' .f 3 To ' Redptetfi o^l^/yVt/lS \fv i pii ' S i J | 3 a . ^ 2 | , 1M<MUad*ata3tal - ~~\ j : 0buwilaitaitoBnfPtnMJafdatMtnf*o30na(! JUdwahUtedh MEaButta* rU-, HJMeatOa&FOLeMeDdUErStiMxysLtOyuborNfcdarsiYtlioKn BoraWtd(dkpcptaortiicwoaitkiIanet fieftiunl e-*sondili i HiialKMfeM *THU" f aTW 4 /U a v/Tit t 1 betiwve*lW6d**. < L \ ' & X ` `i a i ^tamiNsGowfeDtaiOykjip x * . 4 oe r i D ta,u 0 ...... . O CargoAircraftQnfy D *U n Jt. , ] * " * V ^ BWkt: t Mfcl*rWwWtf________ OMtkiRccIp. Payneni 2 S --.-.-.--,,-b(waiMKfrttte*acNanaiM,MCCnnCettC6MirtMii..Mt;w.------------J U~ A^setNNVa. . Reolpiei Q hird Forty CroditCerd CooWChoek M " H O H oe uoi ib. ciw ^ i J c i* -?i C # l i ' y ------^ i * .1 . * 3313 1103 lo ti Pactes** Total Weight . lottiOoeieiodWw' TettiCkvgee t 3, 50 i ____5 4 ____ tcw>yeerefa.M0tt>aflueMoyM<lortOTOhiB0wiicSn0w0B--* n t .ReleasoSignature f s isdsr^ Vfi&rl.' ' f CyMftWVUlUteiusUlitarttaDapnatfwifcfM*' uOHR_)uW,O>ew*MlUtIliUOfolHmmitoruM7MoVn#IlibMv>'VMi*U4I*MM*eMiIUHiWMSBhBealb.nNMe<t^itiIanMmetOwffenaU>dsdUSaaB*<Xu*.9-ecS-oo-Fr-rCoo-7MiI ,I " . ' 1I ,HS 1 ........1 RJZ032567 D i r ! ii ii RJZ032568 EID185042 Sponsor Study No: NA Exygen Study No: 008-046 Analyte: APFO Ions Monitored: 413->369 Site: NA RAW DATA REPORT Limit o f Quantitation: Injection Volume: M atrix: Sample Volume: Final Volume: 50 ng/L U pL Waier 40.0 mL 5.0 inL Set No: Analyst: Instrum ent Type: Extraction Dale: Analyzed on: 101701A Karen Risha LC/MS/MS Unit tf 7 10/17/01 10/19/01 Amount - Std. PFOA APFO PFOA Expgcn Sponsor Sanale: Run Cone. g 1 Peak Found Found Added Recovery m ID Code No. (n/L) Factor Area (ogA) ("BA) m XC101501-0 - CS 10I701A-101 0 - 1552 - - XC101501-1 - cs 1O17O1A-I02 50 - 42219 - - - - -* XC101501-2 - CS 101701A-103 100 - 78392 - - - - XC101501-3 - cs 101701A-104 250 - 172691 - - - - XC101501-4 - cs 101701A-105 500 - 345627 - - - '- XC101501-5 - cs 101701A-106 1000 - 652107 -- - XC101501-6 - CK 101701A-107 250 - 153082 - -- - A . Methanol Wash - c 1017O1A-1O8 - - 957 - -- 0106020 Control NA c 101701A-109 - i 758 NQ NQ - - 3 0106020 Spie A NA LCS 101701A-110 * i 37136 47.8 49.8 50 96 \ - 0106020 Spie B NA LCS 101701A-111 - i 294914 431 449 500 86 ** 0112719 SpkC WWK-D-Bldg-l-Main LF 101701A-112 - 2 288866 844 879 500 72 XC101501-1 - CS 101701A-I14 50 - 34578 " - * - 0112720 SpkD WWK-G-BId-l-Main-2 IF 101701A-115 - 2 308063 901 938 500 90 0112721 SpkE 0112722 Spk F WWK-G-Well-332 WWK-D-BIdg-231 LF 101701A-1I7 LF 101701A-119 - 2 310592 2 330016 909 967 946 500 1010 500 86 107 XC101501-2 - CS 10170LA-121 100 - 75043 - -* - 0112719 WWK-D-Bldg-1-M ain s 10170A-122 - 1 332218 487 507 * * 0112719 Dup WWK-D-Bldg-1-Main S 101701A-I23 - 1 304179 445 463 - - 0112720 WWK-G-BId-l-Main-2 s 101701A-124 - i 309519 453 471 - * 0112720 Dup WWK-G-BId-l-Main-2 s 1070IA-125 - 1 304209 445 463 - * 0112721 WWK-G-Well-332 s 101701A-I26 - I 326892 479 498 - - 0112721 Dup WWK-G-Well-332 s 101701A-127 - i 307712 450 469 - - -- XC101501-3 - c s 101701A-128 250 - 167243 - -- - 0112722 WWK-D-Bldg-231 s 101701A-129 - t 295520 432 450 * 0112722 Dup WWK-D-Bidg-23I S 101701A-130 i 301617 441 459 - - 0112723 WWK-K-FBUC-1 s 101701A-131 - 1 1232 NQ NQ - - 0112724 WWK-K-FBLK-2 s 101701A-132 - i 771 NQ NQ - - XC101501-4 - ^ CS 101701A-133 500 - 350957 - -- - XC101501-5 - CS 101701A-134 100 - 686516 - *- - i PFOA Found (ng/L)= (peak area - intercept)/ slope xD F J . Recovery (%) = PFOA found (np/L)-PFOA found in control (nft/L)j X100 amountPFOA added (ng/L) Standard Curve :: Linear (1/x weighted) Intercept - =49732 5 Slope : 672J37 1 ' APFO Found (ng/L) = PFOA found (ug/L) x (MW APFO (431)/ MW PFOA (414)) Coef. O fD e t25=0.998381 CS -- Calibration standard C -- Control sample S = Sample IP --Lab fortified sample FF = Field fortified sample LCS = Laboratory Control Spflce CK * Check Standard ND = Not detected NQ - Not quantifiable AvgResp. o f th e250 ppt Standards (area): 169967 Response o f the Check Standard (area): 153082 Percent Difference (%): 11.0 % difference acceptable if within 15% Spreadsheet prepared by. in d it e lo ! RJZ032569 EID185043 I I H w 0 H 00 R JZ 032570 ..,,4 A '.. -, I I -ii --*4 1 11 3058 Research Drive State College, P 16801 Phone: 814-272-1039 Fax: 814-231-1580 PREPARATION OF EXTRACTED CALIBRATION STANDARDS Protocol No.: None Method No.: Z Exygen Study No.: 008-046 Analytes: PFOA Matrix: Type I Water? . Sample Vol: IfijnL Sponsor Sample ID NA NA NA NA Exygen Sample ID 0106020 0106020 0106020 0106020 Sample Description Type I Water-1' Type I Water-' Type I Water* Type I Water* Fort. Solution ID F070901-3 F070901-3 F070901-2 Fort, Soin. Cone. 10 10 100 Fort. Volume (uLl . 200 400 100 Micropipet used fuL) - 200 200 200 Fort. Level (ppt) - 50 10 250 Final Solution ID#* XC101501-0 XC101501-1 XC101501-2 XC101501-3 Reagents/ Materials Methanol C18 SPE Type I Water - Lot# w llB i NA * NA 0106020 , Type I Water* F070901-2 100 200 200 500 XC101501-4 NA 0106020 Type I Water* F070901-2 100 400 200 1000 XC1015Q1-5 - - NA 0106020 Type I Water* FIO1501-2 100 100 200 25.0 XC101501-6 -- - - - - - - Initials/Date: 1 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/refrigerator) freezer# I & Time: 3 i<` Initials/Date: ^2. I fo/'d~!'l 40 mL of each sample measured using a S & mL graduated cylinder. Initials/Date: Va. / flirt* / After measuring, samples returned to(reingeratqj)/ freezer U. 18 Time: I H f* Initials/Date: j f r Samples fortified: SPE clean-up: Initials/Date: j A . / Id/tr / Initials/Date: J i . / lt{tsll Final volume adjusted to 5 mL: Extracts placed in refrigerator H, 15 Initials/Date: V i / t p / t r W Initials/Date: M - J ...lit lS t>l STANDARD EXPIRATION DATE: 10/29/01 C om m ents; *This type l water has been filtered through a hypercarb filter * Method of Analysis for the Determination of Pcrfluorooctanolc Acid (PFOA) in Water. July 10.2001/0 en RESEARCH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Internal Chain o f Custody/Fortiiication Sheet Exygen Study Number. 008-046 Matrix: Water Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No. 1o ~' Initials CLIENT SAMPLE ID na na na WWK-D-Bldg-l-Mam WWK-G-Bldg-1 -Main-2 WWK-G-Well 332 WWK-D-Bldg-231 WWK-D-Bldg-l-Majn WWK-D-Bldg-l-Main WWK-G-Bldg-l-Main-2 WWK-G-Bldg-I-Main-2 WWK-G-Well 332 WWK-G-Well 332 WWK-D-Bldg-231 WWK-D-Bldg-231 WWK-K-FBLK-l WWK-K-FBLK-2 . EXYGEN ID NUMBER 0106020 Control 0106020 Spk A 0106020 SpkB 0112719 SpkC 0112720 SpkD 0112721 SpkE 0112722 SpkF 0112719 0112719 Dup 0112720 0112720 Dup 0112721 0112721 Dup 0112722 0112722 Dup 0112723 ` 0112724 _ VOLUME (mL) I FORTIFICATION (ng) 40.0 - 40.0 2.0 40.0 20.0 40.0 20.0 40.0 20.0 40.0 20.0 40.0 . 20.0 40.0 - 40.0 - 40.0 - 40.0 - 40.0 - 40.0 - 40.0 - 40.0 - 40.0 - 40.0 - -- -- - `- Spiking Solution Used Volume Used for Spiking Initial/Date 0106020 SpkB 0112719 SpkC 0112720 SpkD 0112721 S pkE 0112722SpkF F070901-2 (100 np/m L) F07Q901-2 (100 og/m L) F070901-2 (100 ofi/mL) F070901-2 (100 ng/m L) F070901-2 HOP ng/m L) 200 pL (200 pL m icropipet) 200 pL (200 pL m icropipet) 200 pL (200 pL m icropipet) 200 pL (200 pL m icropipet) 200 pL (200 pL m icropipet) "T All samples were measured: Time Date t * ~ n ~ * I Initials After measuring samples were returned to refrigerator No. Time f I Date ; - H ~ - I 1I initials,__________ ... Y> / / //* ) Comments: 200 pLof250 mg/mLsodiumthiosulfate was addedto all samplesbeforespiking. lnituls/Date:--Af----------- ' Analysis Summary: Data Set: lt)\~ lb\ A Data Set: Data Set: Set extraction/analysis data verified by: f' ' Initials/Date: vi /lt ll8 lo l Initials/Date: /~ Initials/Date: Date: f i tJ /f/'f July 26,2001/6 RJZ032571 EID185045 I I i M H H 03 R JZ 032572 .4 3058 Research Drive State College, PA 16801 Phone:814-272-1039 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: 008-046 METHOD: K PROTOCOL NUMBER: HA MATRIX: Water ANALYTES: PPOA Client ID na na WWK-D-B!da-1-Main WWR-G-Bldn-1 -Maln-2 WWK-G-Well 332 WWK-D-Bldjt-231 WWK-D-Bldg-1-Main WWK-D-Bldg- 1-Main WWK-G-Bldg-1 -Maln-2 WWK-G-Bldg-1-Main-2 WWK-G-Wcll 332 WWK-G-Well 332 WWK-D-Bldjt-231 WWK-D-Blde-231 WWK-K-FBLK-1 WWK-K-FBLK-2 Exygen ID 0106020 Control 0106020 Spk A 0106020 SnkB 0112719 Spk C OU2720 SpkD 0112721 SpkE 0112722 Spk F 0112719 0112719 Dup 0112720 0112720Dup 0112721 0112721Dup 0112722 0112722 Dup 0112723 0112724 ,. _ * ln ilia ls /D a le STEP 1 STEP 2 37 -- ,,, - N/ . - A* 7 1 1* O '*! Dilutions (mL/mLJ - - O A /,,0 ! - -- -- -- *. STEP 3 Dilutions (mL/mLl - - -- - STEP 4 * - - - ----- W. ---- ---- ---- ---- ---- -- _ '/ -- -- - -- -- -- - Reagents/ Materials Lot# M ethanol CIS SPE T ype I Water ustiJ 6* NA - -- Jnitials/Dale " - i t io-n-'i -- -- HPLc - Methanol 4 lD 2 .q AmmoniumAcetate Type I water T U 7 > 4 l k -------- NA (} In itia ls /D a te ju a k L . STEP 1: SPE column clean-up STEP 2: Final volume to 5 mL collected in 15 mL potypropolene tubes STEP 3: LC/MS/MS analysis STEP 4: LC/MS/MS analysis. Initials and date under each step indicates the personnel that performed this step. $$ Method of Analysis for the Determination of Perfluorooclanoio Acid (PFOA) in Water Hinauf until lolKloi ^ |oll<||oj COMMENTS: Final extracts stored in refrigerator 1S ' Initials: Date: foj|~f(ol. July 19, 2001/4 1, :enE y g r e s e a r c h 3058 Research Drive State College, PA 16801 Phone:814-272-1039 F a x :814^231-1580 SAMPLE TRANSFER SHEET Protocol Number. P.rvpen Sample # 0112719 0112720 v / 0112721 0112722 0112723 0112724 0112725 S 0112726 0112727 0112728 NA Exyseo Study Number-------- * Sponsor Sample U Exygen Sample # VAVK-D-Bldg-1-Main ~ ^ WK-G-Bldg-l-Main 2 - / 0112729 _ WWK-G-Well-332v/ .- WWK-D-Bldg-231 ^ - WWK-K-FBLK-1 ' - WWK-K-FBLK-2 ^ - WWK-D-Bldg-293 S / WWK-D-Lubeclc-Office^ WWK-G-LPWD-Well-F- / WWK-G-LPWD-Well-A / _ _ - Sponsor Sample # WWK-G-LPWD-Well-B--/ ~ - Requested Location: R e frig 18^ \blglb\ _________ Requested By (Printed Name/Date) pies removed from: C -G pies removed from: pies removed from: pies removed fro m :____.___ iples moved to Box# f) j' ~ r ) n ..... Box# -- Box# -- Box# -- Shell Shelf# Shelf# Shell# t- / -------- Samples removed from Samples returned t o __ (Z-/T -C> Comments: V /a - P i____ Sample Custodian Initials/Date July 12,2001/4 RJZ032573 EID185047 j : '4 ' I i I I M asslynx - Sam ple List Sample List: C:\MASSLYNX\008-046.PRp\SampleDB\101701a.spl Printed: Thu Oct 16 13:50:03 2001 M j_________ Exygen STUDY N O . Page 1 Page Position: (1,1) Vial File Name LIMS ID Client ID Sample Description Matrix Sam ple Type Cone A C one B Cone C T est ID DF MS Method 11 22 33 44 55 66 77 8 92 9 11 10 12 11 13 12 14 13 15 14 2 15 16 16 17 17 18 16 19 19 20 20 21 21 3 22 22 23 23 24 24 25 25 26 26 27 . 27 2B 4 29 28 30 29 31 30 32 31 33 5 34 6 101701A-101 .., 101701 A-102 ... 101701A-103 ... 101701A-104 -- 101701A-105 -- 101701A-106 101701A-107 101701A-108 -- 101701A-109 -- 101701A-110 W 101701A-111 -- 101701A-112 101701 A-113 ... ' 101701A-114 101701A-115 -- 101701 A-116 -- 101701A-117. ""V 101701A-118 ... 101701 A-119 101701A-120 101701A-121 101701A-122 101701A-123 -- 101701A-124 101701A-125 101701A-126 101701A-127 101701A-128 ... -- -- -- 101701 A-129 101701A-130 ... 101701 A-131 101701A-132 101701A-133 -- _ 101701 A-134 -- -- ... ... -- ... ... -- -- -- -- -- ... -- -- ... -- ... -- ... -- -- -- -- -- ... ... -- ... XC101501-0, 0 ppt Standard XC101501-1, 50 ppt Standard XC101501-2,100 ppt Standard XC101501-3, 250 ppt Standard XC101501-4,500 ppl Standard XC101501-5,1000 ppt Standard XC101501-6, 250 ppt Check Standard Methanol Wash 0106020 Control 0106020 Spk A, 50 ppt 0106020 Spk B, 500 ppt 0112719 Spk C, 500 ppt, DF=2 0112719 Spk C, 500 ppt XC101501-1, 50 ppt Standard 0112720 Spk D, 500 ppt, DF=2 0112720 Spk D, 500 ppt 0112721 Spk E, 500 ppt, DF=2 0112721 Spk E, 500 ppt 0112722 Spk F. 500 ppt, DF=2 0112722 Spk F, 600 ppt XC1Q1501-2,100 ppt Standard 0112719 0112719 Dup 0112720 0112720 Dup 0112721 0112721 Dup XC101501-3, 250 ppt Standard 0112722 0112722 Dup 0112723 0112724 XC101501-4, 500 ppt Standard XC101501-S, 1000 ppl Standard ... ... ._.. ... ... ... ... .,.. ... ... ... ... ... J1. ... ... ... ... ... _ ... ... ... ... ... -- Standard Standard Standard Standard Standard Standard QC Blank Blank QC QC QC QC Standard QC QC QC QC QC QC Standard Analyte Analyte Analyte Analyte Analyte Analyte Standard Analyte Analyte Analyte Analyte Standard Standard 0 50 100 250 500 1000 250 ... 50 500 250 500 50 250 500 250 500 250 500 100 -- -- -- -- 250 _ -- -- -- 500 1000 -- -- ... _ ... ... _ ... ... ... ... ... ... -- -- " -- ... -- -- --* -- ... -- ... -- -- -- '_ -- ... -- -- ... -- ... -- ... -- -- ... -- ... --* -- -- '... ... -- O 0 0 0 0 0 0 0 0 0 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 2 PFOA 1 PFOA 1 PFOA 2 PFOA 1 PFOA 2 PFOA 1 PFOA 2 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 M H O H CO R JZ 032574 M H 0 00 O *. U5 W C| N O U) 10 w w HPLC Method MS Tune File Inj.Volume 1 WATER 2 WATER 3 WATER 4 WATER 5 WATER 6 WATER 7 WATER 8 WATER 9 WATER 10 WATER 11 WATER 12 WATER 13 WATER 14 WATER 15 WATER 16 WATER 17 WATER 18 WATER 19 WATER 20 WATER 21 WATER 22 WATER 23 WATER 24 WATER 25 WATER 26 WATER 27 , WATER 28 WATER 29 WATER 30 WATER 31 WATER 32 WATER 33 WATER 34 WATER Water Water Water Water Water Water Water Water Water Water Water . Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: 0S-046 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #$) 7 (Ite) \ | | q| o\ ELECTROSPRAY ION SOURCE: Capillary: 3.0 kV Hexapole 1:0 V Aperture 1:0 V Hexapole 2: 0 V Source Block Temp.: 100'C Desolvation Temo.: 300C ANALYZER: LM Res. 1:10.5 V H M R e sl: 10.5 V OEnergy 1:1.0 V Entrance: -2 V Exit: 2 V LMRes 2 : 13.0 V HMRes2:13.0 V IEnergy 2:2.0 V Multiplier: 650-V GAS FLOWS AND PRESSURE: Desolvation N2 Flow Rate: -650 L/hr Nebuliser Nz Flow Rate: --150 L/hr Gas Cell Pressure: -0.003 mbar Computer Software: COMPAQ Professional Workstation AP200 Microsoft WindowsNT: Version 4 Build 1381: Service Pack 5 Mieromas3 Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Binary Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Column Temperature: Mobile Phase (A ): Mobile Phase (B ): Genesis C -8,5 cm x 2.1 mm i.d. x 4 p (Exygen ID: 35A) (JONESCHROMATOGRAPHY: Part No. FK5962E) 35C 2 mM Ammonium Acetate in Type I Water Methanol Injected Volume: Ions monitored: Analyte PFOA Time (m ini %A 0.0 60.0 0.4 60.0 1.0 10.0 7.0 10.0 7.5 0.0 9.0 0.0 9 3 60.0 133 60.0 14.0 60.0 Total run time = 14 min 15 pL %B 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 Flow Rate (mL/minl 03 03 03 03 03 0.4 0.4 0.4 03 Parent ion Daughter ion Dwell (sees) Coll Energy feV) Cone (V) 413 369 0.2 10 50 Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 A ll Handwritten Peak ID's by: .0 m 3 t e s ARLM A S S IF PR1U7UT5 t b t o W ^ u je s a s s o l i t h is w & e. SYSTEM. AWbcAkl 6 E .I RJZ032576 EID185050 Tuning Method Report M ethod: C:\M ASSL7NX\008-046.ERO\ACQDDB\W AIER P rin te d : F ri Nov 09 0 9 :3 7 :0 1 2001 Page 1 0\ Dan 413.00 SOURCE C E S P - ) C a p illa ry Cone H exapole 1 A p ertu re 1 H exapole 2 S o u rc e B lo ck Temp. D e s o lv a tio n Temp. S e t Rrihk 3 .0 0 50 0 .0 0 .0 0 .0 100 300 -2 .9 3 -2 0 100 301 P ressu res A n a ly s e r Vacuum Gas C e ll Rdbk OFF 2 .6e-3 A n aly ser LM R e s 1 HM R e s 1 lE n erg y 1 E n tran ce C o llisio n E x it LM R e s 2 HM R e s 2 IE nergy 2 M u ltip lie r G as Flow s Cone Gas D eso lv atio n S e t RdJ 1 0 .5 1 0 .5 1 .0 -2 10 2 1 3 .0 1 3 .C 2 .0 550 8 9 11 -6 Rdbk 1 3 6 .5 6 6 0 .4 RJZ032577 EID185051 Scanning Method Report M ethod: C : \M A S S L IN X \0 0 8 -0 4 6 . PRO\ACQUDB\PFOA L a s t M o d ifie d : Mon O c t 15 1 2 :3 7 :2 6 2001 Printed: E r i Nov 09 0 9 :4 1 :2 6 2001 S o lv e n t D elay { m in3 ) : 1 .0 0 F u n ctio n : 1 MEM o f 1 M a s s P a i r ( E S P -- ) I n t e r C hannel D elay { S ecs ) : Span ( D alto n s ) : S t a r t Tim e ( M in s ) : E nd T im e j M ins ) : R ep eats : C hannel P a re n t D au g h ter 0 .0 3 0 .0 0 0 .0 0 8 .0 0 1 D w ell (S e cs) C o ll E nergy (eV) Cone 1 4 1 3 .0 0 3 6 9 .0 0 0 .2 0 10 50 Page 1 RJZ032578 EID185052 Method Report Method File: Last Modified: Printed: C :\MASSLYNX\ 008-046. PRO\ACQUDB \water Friday, November 09, 2001 09:38:47 Friday, November 09, 2001 09:42:01 HP1100 LC Bump Initial Conditions Solvents A% B% Ci D% 60.0 40.0 0.0 0.0 Flow (ml/min) Stop Time (mins) M i n Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) O v e n Temperature Right (C) 0.300 14.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 9 entries which are : Time 0.00 0.40 1.00 '7.00 7.50 9.00 9.50 13.50 14.00 A* so.o 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 HP1100 LC Pump External Event Timetable The Timetable contains 4 entries which are : Time Initial 0.00 0.10 8.00 Column Switch Off Off Off Off Contactl Off On Off Off Contact2 Off Off On Off Contact! Off Off Off Off Contact4 Off Off Off Off HP110Q Autosampler Initial Conditions Draw Speed Eject S p e e d (fxl/min) D r a w Position (nun) Stop Time (mins) Injection Volume(jtl) Vial Humber 200.0 200 0.10 14.00 15.0 6 Page 1 ol Pressure 400 400 400 400 400 400 400 400 400 RJZ032579 EID185053 '. P roven Results. In order to verify mass resolution, a calibration check is performed on the mass spectrometer using a Nal/Rb/Cs tuning solution. The tuning solution is infused onto the m ass spec using an infusion pump set to a flow rate o f 10 pL/min. An MS scan to rn 80 to 1380 amu is perfomed on both M SI and M S2. The calibration is considered acceptable if the follow ing 11 peaks are found w ithin 0.2 amu o f their known m asses on both M SI andM S2: 8 4 .9 ,1 3 2 .9 ,1 7 2 .8 , 3 2 2.7,472.6, 2 2 .5 ,7 7 2 .4 ,9 2 2 .3 ,1 0 7 2 2 ,1 2 2 2 .1 and 1372.0. If any o f the m asses are outside the 0.2 amu, then the instrument w ill be recalibrated and another calibration,check performed. The printouts from Hie calibration check can be found on the follow ing 2 pages. ,^^3,0305508 Research Drive YState College, PA 16801, USA ,T: 814.272.1039 F: 814.231.1580 i'xygenxorn 4 RJZ032580 EID185054 BoVw.-.^ tfj KCWAiQ - 4j ,j * . J > J * *' <! 1 'J ' " J I i '''' I wH aM CD 1 O cn CJ1 N o w tO Ul oe H J -4 ' 4 *'-">4 a - ** 1 C a lib ra tio n 'C h e ck o f NalRbCs09080'0 on MS2 u s in g N alR bC s tu n in g s o lu tio n CALCHKD91001-2 9 (0.569) Cn (Cen,2, 80.00, Ht); Sm (Mn, 2x2.00); Sb (1,40.00 ); Cm (1:17) 100-1 172.8 "1 11 -------------------------------------L C /M S /M S ~ # 7 ] , 10-Sep*2001 08:55:20 ) 0} MS2 ES+ 1 ' 1,04e8 132.9 %- T H IS IS AN EXACT COPY O F THE ORIGINAL DOCUMENT.* BY, - D A T E illd k i... Exygen study NO* M ' f i n 92.0 / 322.8 472,7 622.5 w H d H CD 190.8 / .232.9 234.8 340.8 772.4 922.3 1072.1 1221.9 1371.8 >'*-j'1-illesi 100 200 / 382.9 5 3 2 , r ,, f, 440.8 \556.6 690.5^06.5 i 11 ,. >l A- 4' 5 ' ' 6 70 ` 840.4,856.3 990.2 1134.0 . 17 y | | r r f i l I r i-rH-i*,.i TT'yi I1'*1111'"'-; '' '' 1".sSo 1000 1100 1200 1289.9 1300 I m/z R JZ 032582 Initial Calibration Curve Exygca Study No.: SetNo: Extraction Date: Analyzed on: 008-046 101701A 10/17/01 10/19/01 The first curveofthe dataset is used to detennmeperformance. A linear recession (with no weighting) is perforated using the fust six standards ofdie analytical inn.' The coefficient o f determination (R.Square) must be 0.915 nr greater. I f die set fails to meet Thisrequirement, the nut must be rejected and the samples reanalyzed. S tan d ard C oncentration E iy een lD X C 10150I-0 (ne/L ) 0 P eak A rea 1552 XC101501-1 XC101501-2 50 100 42219 78392 XC101501-3 XC101501-4 XC101501-5 250 500 1000 172691 345627 652107 C oefficient o f D eterm ination: 0.99916321 SUMMARY OUTPUT \\W R eg re ssio n S ta tistic i M ultiple R 0.99958152 R S quare 0.99916321 A djustedR S qua: 0.99895402 Standard E rror 7974.56702 O bservations_____________6 ANOYA ,__________ R egression ______ S S _________ i ________F S ig n ifica n ce F 1 3.03736E+11 3.04B +11 4776.1882 2.6265E-07 Residuai 4 254374876.7 63593719 ' T o t a l _______ _ 5 3.0399E +U ____________________________ __ I C o e ffic ie n ts S ta n d a r d E r r o r t S t a t P -v a lu e LowerL o v e r 9 5 % . U p p e r 9 5 % 9 X 0 % U p p er 9 5 .0 ^ In te rc e p t X V ariable 1 10229.6406 4406.260677 1 3 2 1615 0.0809931 -2004.12568 22463.4068 -2004.1257 22463.4068 648.005346 9.376437708 69.10997 2.627B-07 621.972127 674.038564 621.972127 674.038564 RJZ0325B3 EID185057 Quantify Calibration Report , S tudy N o.: 008-046, S a t No: 101701A, E x t. D ata: 10/1 7 /0 1 , A n aly st: K R isha Calibration: P:\Data\LCMSMS6\Ma33lynx\008-046.PRD\CurveDB\101701A Last modified: Pci Oct 19 16:30:35 2001 Printed: Fri Oct 19 16:33:11 2001 U Page 1 [01 RJZ032584 EID185058 Quantify Sample Report Study No.: 009-046, Sat No: 101701A, Ext. Date: 10/17/01, Analyst: K Risha Page 1 S am ple L i s t : P : \D ata\L C M S M S 6\M as3 lynx\008-046. P R O \S am plaD B \101701a L a s t m o d ified : E ri O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D a t a \ L C M S M S 6 \M a s s l y n x \ 0 0 8 -0 4 6 .P R O \M eth D B \1 0 1 6 0 1 PFOA. L a s t m o d ified : E ri O ct 19 1 6 :1 9 :2 6 2001 Job Code: Initials . Dale 10(1*1 lo i P rin te d : F r i O ct 19 1 6 :3 3 :1 3 2001 Run# i o n e IA -lo i To IQI70 (A -IS U Name: 101701A -101 le x t: Exygen Research RJZ032585 EID185059 Quantify Sample Report Study No.: 008-046, Sat No: 101701A, Ext. Date: 10/17/01, Analyst: KRisha Sample l i s t : P:\Data\LCMSMS6\Ma33lynx\008-046.PRO\SampleDB\101701a L a s t m o d ifie d : F r i O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D a ta \L C M S M S 6 \M a 3 sly ro c \0 0 8 -0 4 6 .P R O \M a th D B \1 0 1 6 0 1 PFOA L a st m o d ifie d : F r i O ct 19 1 6 :1 9 :2 6 2001 Job Code: Printed: F r i O ct 19 1 6 :3 3 :1 3 2001 Name: 101701A -102 le x t: Page 2 Exygan Research RJZ032586 EID185060 Quantify Sample Report Study Ko.: 008-046, Set No: 1D1701A, Ext. Date: 10/17/01, Analyst: K Rxsha S am ple L i s t : L a st m o d ified : M ethod: L a st m o d ified : Jo b Code: I? : \ D a t a \ L C M S M S 5 \ M a - 3 s l y n x \ 0 0 B - 0 4 6 . P R O \S a m p le D B \1 0 1 7 0 1 a F r i O ct 19 1 6 :2 5 :3 2 2001 ... p : \D ata\L C M SM S 5 \M a s s ly n x \0 0 8 - 0 4 6 . E R O \M etK D B \101601 PFOA F r i O ot 19 1 6 :1 9 :2 6 2001 P rin te d : fid- O c t 19 1 6 :3 3 :1 3 2001 N a m e : 1 0 1 7 0 1A--1 0 3 T ex t: Page 3 Exygen Research RJZ032587 EID185061 Quantify Sample Report Study No.: 008-046, Set No: 101701A, Ext. Data: 10/17/01, Analyst: K Risfca S am ple L i s t : E :\D ata\L C M S M S 6 \M asslynx\008-046.E R O \S am pleD B U 01701a L a st m o d ified : F ri O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D a ta \L C M S M S 6 \M a ss ly n x \0 0 8 ~ 0 4 6 .P R 0 \M a th D B \1 0 1 6 0 1 PFOA L a s t m o d ifie d : F r i O ct 19 1 6 :1 9 :2 6 2001 Job Code: P rin te d : F ri O ct 19 1 6 :3 3 :1 3 2001 N aue: 101701A -104 T ex t: Page 4 Exygen Research RJZ032588 EID185062 Q u a n tify S am ple R e p o rt . S tu d y N o .: 0 0 8 -0 4 6 , S e t No: 101701A , E x t. D a te : 1 0 /1 7 /0 1 , A n a ly s t: K R ish a S am ple L i s t : P :\D ata\L C M S M S 6\M a33lynx\008-046.P R O \S am pleD B \101701a L a st m o d ifie d : F ri O ct 19 1 6 :2 5 :3 2 2001 Method: B:\Data\LCMSMS6\MaS3lynx\008-046.PHa\MethDB\101601 PFOA L a st m o d ifie d : F ri O ot 19 1 6 :1 9 :2 6 2001 Job Code: P rin te d : F ri O ct 19 1 6 :3 3 :1 3 2001 Name: 101701A -1Q 5 T ex t: 1 Exygen Reseaxch RJZ032589 EID185063 Quantify Sample Report Study No. : 008-046, Set Ho: 101701A, Ext. Date: 10/17/01, Analyst: K Risha S am ple L i3 t : P :\D ata\L C M S M S 6\M a33lynx\00B -046.P R O \S am pleD B \101701a L a s t m o d ified : F ri O ot 19 1 6 :2 5 :3 2 2001 Method: P:\Data\LCMSMS5\Masslynx\008-046.FRO\MetiiDB\101601 PFOA L a st m o d ified : F ri O ct 19 1 6 :1 9 :2 6 2001 Job Code: P rin te d : F ri O ct 19 1 6 :3 3 :1 3 2001 Harne: 101701A -106 T ex t: Page 6 Exygen. Research RJZ032590 EID185064 Quantify Sample Report Study Ho: 008-046, Set Ho: 10171A, Ext. Date: 10/17/01, Analyst: K Risha S am ple l i s t : l a s t m o d ified : M ethod: l a s t m o d ified : Job Coda: V : \D ata\L G M S M S6\M as3lyxuc\00B -046. PR O \Sam pleD B \1017 0 1 a F r i O ct 19 1 6 :2 5 :3 2 2001 ,. P :\D a ta \L C M S M S 6 \M a ss ly n x \0 0 8 -0 4 6 .PR O \M ethD B \101601 PFOA F ri O ct 19 1 6 :1 9 :2 6 2001 P rin te d : F ri O ct 19 1 6 :3 3 :1 3 2001 Name: 101701A -107 T ex t: Page 7 I Exygen Research :j 1 RJZ032591 EID185065 Quantify Sample Report Study Ho.: 000-046, Set Ho: 1D1701A, Ext. Date: 10/17/01, Analyst: K Risha S am ple l i s t : P :\D ata\lC M S M S S \M asslynx\008-046.E R O \S am plaD B \101701a l a s t m o d ifie d : F r i O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D a ta \lC M S M S 6 \M a s 3 ly n x \0 0 a -0 4 6 .P E O \M e th D B \1 0 1 6 0 1 PFOA l a s t m o d ified : F r i O ct 19 1 6 :1 9 :2 6 2001 Job Code: P rin te d : F r i O ct 19 1 6 :3 3 :1 3 2001 Page 8 Ham a: 101701A -108T ex t: 1 ; PFOA Methanol Wash 101701A-108 Sm (Mn, 2x2} 100n 19-Oct-20Q1 09:19:43 LC/MS/MS #6 MRM of 1 Channel ESna >369 V 2.35e4 %- - n Time 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 RJZ032592 EID185066 Quantify Sample Report _ Study No.: 008-046, Set No: 101701A, Ext. Date: 10/17/01, Analyst: K Risha S am ple L i s t : P :\D ata\L C M S M S 6 \M asslynx\008-046.P R O \S asrpleD B \101701a L a st m o d ified : F ri O ct 19 1 6 :2 5 :3 2 2001 Method: P:\Data\LCMSMS6\Masslynx\008-046.PRO\MetbDB\101601 PEOA L a st m o d ified : F ri O ct 19 1 6 :1 9 :2 6 2001 Job Code: P Jited: F r i O ct 19 1 6 :3 3 :1 3 2001 Name: 101701A -109 T ex t: Page 9 Exygen Research RJZ032593 EID185067 Quantify Sample Report Study No.: 009-046, Set No: 101701A, Ext. Dato: 10/17/01, Analyst: K Risha S am p le L i s t : P :\D ata\lC M S M S 6 \M asslynx\Q 0S -046.P R Q \S am pleD B \1017Q la L a st m o d ifie d : E ri O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D a ta \L C M S M S 6 \M a ss ly n x \0 0 8 -0 4 6 .P R O \M a th D B \1 0 1 6 0 1 PFOA L a s t m o d ifie d : E ri O ct 19 1 6 :1 9 :2 6 2001 Job Code: P rin te d : F ri O ct 19 1 6 :3 3 :1 3 2001 Name: 101701A -110 T ex t: 1: PFOA Page 10 ti t o 4 u" ' va j r. .. y *- - i v+- n a Exygen Research RJZ032594 EID185068 Quantify Sample Report Study Ho.: 008-046, Set No: 101701A, Ext. Date: 10/17/01, Analyst: K Risha S am p le L i s t : P :\D ata\L C M S M S 6 \M asslyruc\008-046.P R O \S aspleD B \101701a m o d ified : F r i O ct 19 1 6 :2 5 :3 2 2001 , M ethod: P :\D a ta \L C M S M S 6 \M a a sly n x \O O 0 -O 4 6 .P R O \M a th D B \lO 1 6 O l PFOA L a s t m o d ified : F r i O ct 19 1 6 :1 9 :2 6 2001 Jo b Code: P rin te d : F r i O ct 19 1 6 :3 3 :1 3 2001 Page 11 Hamo: 101701A -111 T ex t: . Exygen Research RJZ032595 EID185069 Q u a n tify Sam ple R e p o rt S t u d y N o * : 0 0 8 - 0 4 6 , S o t N o t 1 0 1 7 0 1 A , Ext. Date: 10/17/01, Analyst: K Risha S am ple L i s t : P :\D ata\L C M S M S 6\M as3lyrtx\008-046.P R O \S am pleD B \101701a L a.s't m o d i f i a d : F iri O c t 19 1 6 ;2 5 :3 2 2 0 0 1 M ethod: P :\D a ta \l0 1 S M S 6 \M a s sly n x \Q 0 8 -0 4 6 .E R O \M a th D B \1 0 1 6 0 1 PFOA L a s t m o d ifie d : P ri O ct 19 1 6 :1 9 :2 6 2001 Job Code: P rin te d : F ri O ct 19 1 6 :3 3 :1 3 2001 am e: 101701A -112 T ex t: Page 12 Exygen Research RJZ032596 EID185070 Quantify Sample Report Study Ho.: 008-046, Set No: 101701A, Ext. Date: 10/17/01, Analyst: K Risha S am ple L i s t : P :\D ata\L C M S M S 6\M asslY nx\008-046.P R O \S am pleD B \101701a l a s t m o d ified : F ri O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D a ta \ia 4 S M S 6 \M a s s ly n x \0 0 8 -0 4 6 .P R O \M e th D B \1 0 1 6 0 1 PFOA l a s t m o d ified : F ri O ct 19 1 6 :1 9 :2 6 2001 Job Code: P rin te d : F ri O ct 19 1 6 :3 3 :1 3 2001 Page 13 N am e: 1Q 1701A -113 T ex t: 1 : PFOA_________ . 0112719 SpkC , 500 ppt -,101701A-113 Sm (Mn, 2X2) 100 19-0ct-2001 10:38:29 LC/MS/MS #6 yRM of 1 Channel ES5.10 413 > 3 6 9 3.91 e6 %- 0- I 1i " I 1....... 1"1' 1.00 2.00 3.00 4.00 RJZ032597 EID185071 Quantify Sample Report Study Ho.: 008-046, Sot Ho: 1Q1701A, Ext. Dato: 10/17/01, Analyst: K Risha S am ple L i s t : P :\0ata\L C M S M S 6\M asslynx\O O 8-O 46.P R O \S anipleD B \lO 17O la L a s t m o d ified : F ri O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D a ta \L C M S M S 6 \M a ssly n x \0 0 8 -0 4 6 .E R O \M e th D B \1 0 1 6 0 1 PFOA L a s t m o d ifie d : F ri O ct 19 1 6 :1 9 :2 6 2001 Job Code: P rin te d : F r i O ct 19 1 6 :3 3 :1 3 2001 Harne: 101701A -114 T ex t: Page 14 Exygen Research RJZ032598 EID185072 Q u a n tify S am ple R e p o rt S tu d y N o .: 0 0 8 - 0 4 6 , S e t N o: 101701A ., E x t. D a ta : 1 0 /1 7 /0 1 , A n a ly s t: K R is h a S am p le L i s t : P :\D ata\L C M S M S 6 \M asslynx\008-046.P R O \S am pleD B \101701a L a st m o d ifie d : F r i O ct 19 1 6 :2 5 :3 2 2001 ' M ethod: P :\D a ta \L C M S M S 6 \M a ssly n x \O O B -O 4 6 .P H 0 \M a th D B \lO 1 6 O l PFOA L a s t m o d ified : F r i O ct 19 1 6 :1 9 :2 6 2001 Jo b Code: ' P rin te d : F ri O ct 19 1 6 :3 3 :1 3 2001 Page 15 Name; 101701A -115 T ex t: 0112720 Spk D , 500 ppt, DF=2 101701A-115 S m (Mn, 2x2) 100-, 19-0ct-2001 11:09:54 LC/MS/MS #6 MRMof 1 Channel ES- 5.10 413 >369 2.26e6 %- 1 i 1.00 IIIIII zoo T-T-p-T3.00 4.00 5.00 16r.i0-i0' l I I l l I I J '" 7.00 Fi8=.n0T0ime Exygen Research RJZ032599 EID185073 Quantify Sample Report Study Ho.: 008-046, Set Ho: 1Q1701A, Ext. Date: 10/17/01, Analyst: K Risha S am ple L i s t : P :\D ata\L C M S M S 6\M asslynx\008-Q 46.P R O \S am pleD B \101701a L a s t m o d ifie d : Era. O c t 19 1 6 :2 5 :3 2 2001 M ethod: P : \D ata\L C M SM S S \M a ss l y n x \ 0 0 8 - 0 4 6 . PR 0\M e th D B \ 1 0 1 6 0 1 PFOA L a st-m o d ifie d : F r i O ct 19 1 6 :1 9 :2 6 2001 Job Code: P rin te d : F r i O ct 19 1 6 :3 3 :1 3 2001 Harne: 1017 0 1 A -1 1 6 T ex t: Page 16 Exygsn Research RJZ032600 EX D 185074 Quantify Sample Report Study No.: 008-046, Set No: 101701A, Ext. Date: 10/17/01, Analyst: K Risha o lirt: P :\D ata\L C M S M S6\M as3lynx\O O 0-O 46.E R O \S am pleD B \lO 17O la l a s t m o d ifie d : F ri O ct 19 1 6 :2 5 :3 2 2001 M ethod: P:\Data\LCMSMS6\Masslynx\008-046.PRO\MatbDB\101S01 PFOA last m o d i f i e d : F r i Oct 19 16:19:26 2001 Jo b Code: P rin te d : F r i O ct 19 1 6 :3 3 :1 3 2001 Page 17 N a m e : 1 0 1 7 0 1 A --1 1 7 T ex t: 1 : PFOA 0112721 Spk E, 500 ppt, DF=2 101701A-117 S m (Mn, 2x2) 100-1 5.13 ' I 19-0ct-2001 11:41:19 LC/M S/M S #6 MRM o f 1 Channel ES413 > 369 2.27e6 \ /<r 0-' III Ill '' -r , - r i 111 11 1n 11 1 1p -l 1-T--1 I 1 111 1 '"HI 111 n r Ti f 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research RJZ032601 EID185075 Quantify Sample Report Study Ho. : 008-046, Set No: 101701A, Ext. Date: 10/17/01, Analyst: K Rista S am ple L i 3 t : P :\D ata\3 X M S M S 6 \M assly n x \0 0 8 -0 4 6 .P R O \S aap leD B \1 0 1 7 0 1 a l a s t m o d ifie d : F r i O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D ata\L C M S M S 6\M hsslynx\O O 8-O 46.F R 0\M ethD B \lO 16O l PE0A L a s t m o d ifie d : F r i O ct 19 1 6 :1 9 :2 6 2001 Jo b Code: P rin te d : F r i O ct 19 1 6 :3 3 :1 3 2001 Page 18 Name: 101701A -118 T ex t: 1 : PFOA____________ 0112721 Spk E, 500 ppt 101701A-118 Sm (Mn, 2x2) 100-1 19-0ct-2001 11:57:04 LC/MS/MS #6 MRM of 1 Channel ES5.14 413 >369 4.80e6 %- 0 >i >` I '"> t ><>i '1' [ I I I I p -l ! I I I I ' I I 11 1) ` r- 7 T 1 r i '1 1 1 1 1 1 1 1 1 . j11"1 1 1 1 *. ri-i-| Time 1,00 2.00 3.00______ 4.00 5.00 6.00 7.00 8.00 Exygen Research RJZ032602 EID185076 Quantify Sample Report Study Ho.: 008-046, Set Ho: 101701A, Ext. Date: 10/17/01, Analyst: K Exsha S am ple l i s t : L a st m o d ified : M ethod: Last modified: Job Coda: P :V > ata\L C M S M S 6\hfasslynx\008-046.P K Q \3am pleD B \10r701a F r i O ct 19 1 6 :2 5 :3 2 2001 P : \ D a t a \ L C M S M S 6 \ M a s s l y n x \ 0 0 8 - 0 4 6 . P R D \M s th D B \1 0 1 6 0 1 PFGA. F r i O ct 19 1 6 :1 9 :2 6 2001 P rin te d : F ri O ct 19 1 6 :3 3 :1 3 2001 Paga 19 Harne: 101701A .-119 T ex t: 1 : PF0A 0112722 Spk F, 500 ppt, DF=2 101701A-119 Sm (Mn, 2x2) 100a 19-0ct-2001 12:12:51 LCiNIS/MS#6| MRM of 1 Channel ES'5.13 413 > 369 2.40e6 %- 1.00 2.00 T-r-ftr 3.00 I I j 1j I I I I r i-t-p 4.00 5.00 =I r n i p ) 'r i~t i . i {I I i 6.00 7,00 8.0i T0ime Exygen Research RJZ032603 EID185077 Quantify Sample Report Study No.: 008-046, Sat No: 101701A, Ext. Data: 10/17/01, Analyst: K Risha S am p le L i s t : P :\D ata\L C M S M S 6\M a3alynx\008-046.P R O \S am pleD B \101701a L a s t m o d ified : F r i O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D a ta \L C M S M S 6 \M a 3 S ly n x \0 0 8 -0 4 6 .P R O \M e tb D B \1 0 1 6 0 1 PFOA L a s t m o d ified : F ri O ct 19 1 6 :1 9 :2 6 2001 Jo b Code: P rin te d : F r i O ct 19 1 6 :3 3 :1 3 2001 Nam e: 101701A -120 T ex t: Page 20 Exygen Research RJZ0326O4 EID185078 Quantify Sample Report Study No.: 008-046, Set No: 101701A, Ext. Date: 10/17/01, Analyst: K Risha S am ple l i s t : P :\D ataV L C M S M S 6\M asslynx\00B -046.P R O \S am pleD B \101701a L a s t m o d ified : F ri O ct 19 1 6 :2 5 :3 2 2001 M ethod: p :\D ata\L C M S M S 6 \M a3 3 ly n x \O O 0 -O 4 6 .P R O \M eth D B \lO 1 6 O l PFOA L a s t m o d ified : F r i O ct 19 1 6 :1 9 :2 6 2001 Job Code: P rin te d : F r i O ct 19 1 6 :3 3 :1 3 2001 Name: 101701A -121 T ex t: Page 21 Exygen Research RJZ032605 EID185079 Q u a n tify S am ple R e p o rt S tu d y N o ,: 0 0 8 -0 4 6 , S o t N o: 101701A , E x t. D a ta : 1 0 /1 7 /0 1 , A n a ly s t: K R ish a S am ple L i s t : P :\D ata\L C M S M S 6\M a33lynx\008-046.E R O \S am pleD B \101701a l a s t m o d ified : F r i O ot 19 1 6 :2 5 :3 2 2001 -Method: P:\Data\XCMSMS6\Mas3lynx\00B-046.ERO\MethDB\101601 PFOA L a st m o d ified : F r i O ct 19 1 6 :1 9 :2 6 2001 Job Code: P rin te d : F r i O ct 19 1 6 :3 3 :1 3 2001 Name: 101701A -122 T ex t: Exygen Research RJZ032606 EID185080 Q u a n tify S am ple R e p o rt S tu d y N o .: 00 0 -0 4 6 , S e t N o: 101701A , E x t. D a te : 1 0 /1 7 /0 1 , A n a ly s t: K R ish a S am p le L i s t : P :\D ata\L C M S M S 6\M asslynx\O O 0-O 46.P R O \S am pleD B \lO 17O la L a s t m o d ifie d : F iri O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D a ta \X e M S M S 6 \M a 3 3 ly n x \Q Q 8 -0 4 6 .E R O \M e th D B \1 0 1 6 0 1 PFOA L a s t m o d ifie d : F r i O ct 19 1 6 :1 9 :2 6 2001 Job Code: P rin te d : F r i O ct 19 1 6 :3 3 :1 3 2001 Name: 101701A -123 T ex t: Exygen Research RJZ032607 EID185081 Quantify Sample Report Study Ho.: 008-046, Sot No: 101701A, Ext. Date: 10/17/01, Analyst: K Risha S am ple L i s t : P :\D ata\L C M S M S 6\M as3lynx\008-04S .P R O \S am pleD B \101701a L a st m o d ified : F r i O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D a ta \L C M S M S 6 \M a 3 3 ly n x \0 0 8 -0 4 S .P R O \M e th D B \1 0 1 6 0 1 PFOA L a st m o d ified : F ri O ct 19 1 6 :1 9 :2 6 2001 Job C oda: P rin te d : F ri O ct 19 1 6 :3 3 :1 3 2001 Mame: 101701A -124 T ex t: Page 24 Exygen Research. RJZ032608 EID185082 Quantify Sample Report Page 25 Study N o .: 008-046, Set No: 1017Q1A, Ext. Date: 10/17/01, Analyst: K Risha S am p le L i s t : P :\D ata\IX M S M S 6 \H as8 ly n x \0 0 8 -0 4 6 .P R 0 \S am p lo D B \1 0 1 7 0 1 a L a s t m o d ifie d : F r i O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D ata\L C M S M S 6\M asslynx\0Q 8-046.P R O \M etbD B \101601 PFOA l a s t m o d ified : F ri O ct 19 1 6 :1 9 :2 5 2001 Job Coda: P rin te d : F r i O c t 19. 1 6 :3 3 :1 3 2001 Nam e: 101701A -125 T ex t: Exygen Research RJZ032609 EID185083 Quantify Sample Report . Study No.: 008-046, Sot Ho: 101701A, Ext. Data: 10/17/01, Analyst: K Risha S am p le L i s t : P :\D ata\L C M S M S 6\14aa3lynx\008-046.P R O \S am pleD B \101701a L a s t m o d ified : F r i O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D a ta \L C M S M S 6 \M a s3 ly n x \0 0 8 -0 4 6 .P R O \M e th D B \1 0 1 6 0 1 PFOA L a s t m o d ified : F ri O ct 19 1 6 :1 9 :2 6 2001 Job Code: P rin te d : F r i O ct 19 1 6 :3 3 :1 3 2001 Name: 101701A -126 Text: Exygen Research RJZ032610 EID185084 Quantify Sample Report Study No.: 008-046, Set No: 101701A, Ext. Date: 10/17/01, Analyst: K Risha S am ple L i s t : P :\D ata\L C M S M S 6\M as3lynx\008-046.P R O \S am pleD B \101701a L a st m o d ifie d : F r i O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D a ta \L C M S M S 6 \M a 3 3 ly n x \0 0 8 -0 4 6 .P R O \M a th D B \1 0 1 6 0 1 PFOA L a s t m o d ifie d : F r i O ct 19 1 6 :1 9 :2 6 2001 Job Code: P rin te d : F r i O ct 19 1 6 :3 3 :1 3 2001 Page 27 Name: 101701A -127 T ex t: 1: PFOA 0112721 Dup 101701A-127 Sm (Mn, 2X2) 10Ch 19-Oct-2QQ1 14:18:49 LC/MS/MS #6 MRM of 1 Channel ES 5.16 413 >369 2.29e6 % ' 1 1 1 1 ' 1 ' i 1.00 2.00 T T-f^r- i ' ' 1 1 1 ' 11 1 1 1 11 ' "P 3.00 4.00 5.00 6.00 uiip Time 7.00 8.00 Exygea Research RJZ032611 EID185085 Quantify Sample Report Study No.: 008-046, Sat No: 1017Q1A, Ext. Data: 10/17/01, Analyst: K Risha S a a p lo L i s t : P :\D ata\L C M S M S 6\M a33lynx\008-046.P R Q \S am pleD B \101701a L a s t a o d if is d ; F c i O ct 19 16:2 5 * 3 2 2001 M ethod: P :\D a ta \L C M S M S 6 \M a 3 3 ly n x \0 0 8 -0 4 6 .PR O \M ethD B \101601 PFOA i a a t m o d ified : E ci O ct 10 1 6 :1 9 :2 6 2001 Job Coda: P rin te d : F ri O ct 19 1 6 :3 3 :1 3 2001 Name: 101701A -128. T ax t: Paga 28 Exygen Research RJZ032612 EID185086 Quantify Sample Report Study No.: 008-046, Set No: 101701A, Ext. Date: 10/17/01, Analyst: K Risha S am ple L i s t : P :\D ata\L C M S M S 6\M asslynx\O O 8-O 46.P R 0\S am pleD B \lO 17O la L a s t m o d ifie d : P ri O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D ata\L C M S M 3 6 \M as3 ly n x \0 0 8 -0 4 6 .P R O \M eth D B \1 0 1 6 0 1 PFOA l a s t m o d ified : F ri O ct 19 1 6 :1 9 :2 6 2001 Job Coda: P rin te d : F ri O ct 19 1 6 :3 3 :1 3 2001 Name: 101701A -129 T ex t: Rage 29 Exygen Research RJZ032613 EID185087 Quantify Sample Report Study No.: 008-046, Set No: 101701A, Ext. Date: 10/17/01, Analyst: K Rista S am ple L i s t : P :\D ata\L C M S M S 6\M a33lynx\008-046.P R O \S am pleD B \101701a l a s t m o d ifie d ; F t i O ct 19 l(> i2 5 :3 2 2001 . M ethod: P :\D a ta \L C M S M S 6 S M a 3 3 ly n x \0 0 8 -0 4 6 .P R O \M e th D B \1 0 1 6 0 1 PROA L a s t m o d ified : F ix O ct 19 1 6 :1 9 :2 6 2001 Jo b Code: P rin te d : F ri O ct 19 1 6 :3 3 :1 3 2001 N am e: 101701A -130 T ex t: Page 30 Exygen Research RJZ032614 EID185088 Quantify Sample Report Study No.: 008-046, Sat No: 101701A, Ext. Data: 10/17/01, Analyst: K Risha S am p le L i s t : P :\D ata\L C M S M S 6 \M a3 3 lynx\00B -046.P R O \S am pleD B \10n01a X ,ast m o d ifie d : F r i O c t 19 1 6 :2 5 :3 2 2001 M ethod: P :\D a ta \L C M S M S 6 \M a 3 sly n x \0 0 0 -0 4 6 . P R O \M athD B \101601 PFOA L a s t m o d ifie d : F r i O ct 19 1 6 :1 9 :2 6 2001 Job Coda: P rin te d : F r i O ct 19 1 6 :3 3 :1 3 2001 Name: 101701A -131 T ex t: Page 31 Exygerx Research RJZ032615 EID185089 Q u a n tif y S am ple R e p o rt S tu d y M o.: 0 0 3 -0 4 6 , S e t H o: 101701A , E x t. D a te : 1 0 /1 7 /0 1 , A n a ly s t: K R is h a S am p le L i s t : P :\D ata\iC M S M S 6 \M assly n x \0 0 3 -0 4 6 .P R O \S am p leD B \1 0 1 7 0 1 a L a st m o d ified : F ri O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D ata\L C M S M 3 6 \M a3 3 ly n x \0 0 8 -Q 4 S .P R O \M ath D B \1 0 1 6 0 1 PfOA L a s t m o d ified : F ri O ct 19 1 6 :1 9 :2 6 2001 Job Coda: P rin te d : F ri O ct 19 1 6 :3 3 :1 3 2001 H ane: 101701A -132 T ex t: Page 32 Exygen Research RJZ032616 EID185090 Quantify Sample Report Study No.: 008-046, Set No: 101701A, Ext. Date: 10/17/01, Analyst: K Risha S am ple L i s t : P :\D ata\L G M S M S 6\M assly m x\008-046.P R O \S am pleD B \101701a L a s t m o d ifie d : E ra O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D ata\L C M S M S 6 \M a 3 sly n x \0 0 8 -0 4 6 .P R O \M e th D B \1 0 1 6 0 1 PFOA L a s t m o d ified : F r i O ct 19 1 6 :1 9 :2 6 2001 Job Coda: P rin te d : F r i O ct 19 1 6 :3 3 :1 3 2001 N am e: 101701A .-133 T ex t: Pago 33 Exygen Research RJZ032617 EID185091 Quantify Sample Report Study No.: 008-046, Set No: 101701A, Ext. Date: 10/17/01, Analyst: K Risha S am p le L i s t : P :\D ata\L C M S M S 6\M a33lynx\008-046.P R O \S am pleD B \101701a L a st m o d ified : F ri O ct 19 1 6 :2 5 :3 2 2001 M ethod: P :\D ata\L C M S M S 6 \M ao sly n x \0 0 8 -0 4 6 .P R O \M eth D B \1 0 1 6 0 1 PFOA L a s t m o d ified : F ri O ct 19 1 6 :1 9 :2 6 2001 Job Coda; P rin te d : F ri O ct 19 1 6 :3 3 :1 3 2001 Name: 101701A -134 T ex t: 1 : PFOA Page 34 Exygon Research RJZ032618 EID185092 1 1 Hf ' ' *. 1 *~~3 ii 1 * 'T 3 '1 i y o n Sponsor Study No: NA Exygen Study No: 008-046 Analyte: AFFO Ions Monitored: 413 -> 369 Site: NA RAW DATA REPORT Limit o f Quantitation: Injection Volume: M atrix: Sample Volume: Final Volume: 59 ng/L 15 pL Water 40.0 mL 5.0 mL Set No: A nalyst Instrument Type: Extraction Date: Analyzed on: 101701B K ara Ridia LC/MS/MS Unit fi 7 10/17/01 10/18/01 Std. Exygcn Sponsor Sample Run Cone. Dilution Peak m ID Code No. (ng/L) Factor Area XCI01501-0 - CS 10170IB-201 0 - ND XC101501-1 - CS 101701B-202 50 - 2269 XC101501-2 - CS 101701B-203 100 - 4485 XE101501-3 - CS 101701B-204 250 - 9753 X C 101501-4 - CS 101701B-205 500 - 20662 XC101501-5 - CS 101701B-206 1000 - 40877 XC101501-6 MethanolWash ' 0106020Control NA CK 10170IB-207 250 . 9594 c 10170IB-208 - - ND c 101701B-209 - 1 ND 0106020 Spk A NA LCS 101701B-210 - 1 1896 0106020 SpkB NA LCS 101701B-211 - 19553 0112725Spk C WWK-D-Bldg-293 LF 101701B-213 - 35585 0112726SpkD WWK-D-Lubeck-Office LF 101701B-214 - 2 20859 XC10150M - CS 101701B-216 50 - 2212 0112727 SpkE WWK-G-LPWD-Wdl-F LF I01701B-218 - 1 27533 0112728SpkF WWK-G-LPWD-Well-A LF 101701B-2I9 - 2 21348 0112729Spk G WWK-G-LPWD-Well-B LF 10170IB-222 - 1 37615 XC101501-2 - CS I01701B-223 100 - 3863 0112725 WWK-D-Bldg-293 S 101701B-224 - 0112725Dup WWK-D-BIdg-293 s 10170IB-225 - 0112716 WWK-D-Lubeck-Ofifce s 1017OB-226 - 0112726Dup. WWK-D-Lubeck-OE&e s 10I701B-227 - 0112727 WWK-G-LFWD-Well-F s 101701B-228 - 0112727Dup WWK-G-LPWD-Well-F s I01701B-229 - I 15758 I 14574 1 23022 1 22433 1 10823 1 9954 XC101501-3 . - CS 101701B-230 250 - 8481 0112728 WWK-G-LPWD-WeB-A S I01701B-231 - 0112728Dup WWK-G-LPWD-Wcll-A s 101701B-232 - 0112729 WWK-G-LPWD-Weil-B s 10170IB-233 - 1 26028 1 25325 I 21537 0112729Dup WWK-G-LPWD-Wdl-B S 10171B-234 - 1 21074 XC101501-4 '- CS 10I70IB-235 500 18440 XC101501-5 - CS 101701B-236 1000 - 36595 PFOA Found (ng/L) = (peak area -intercept)/ slope xD F Recovery (%) = [PFOA found (ng/L)-PFOA found in control (ng/L)l xlOO amountPFOA added (ng/L) APFO Found (ng/L)= PFOA found (ng/L) x (MW APFO (431) / MW PFOA (414)) PFOA Found (ng/L) APFO Found (ng/L) Amount PFOA Added (ng/L) Recovery <%> - .- -_ - __ . . . -_ _. _ _ - >_ -- _ ND ND 42.5 44.2 50 506 526 500 926 964 500 1080 H20 500 - .- 85 101 104 97 . 715 1110 979 - 406 375 597 581 277 254 675 657 558 546 - 744 1150 1020 - 423 390 621 605 288 264 703 684 581 568 - 500 500 500 _ _ . . . . - 88 87 84 . _ , - - - -- - Standard Curve: Linear fl/xw eiehtofl Intercept = 276.530 Slope = 38.1239 Coef. O fDel. = 0.992303 C S -- Calibration standard C ~ Control sample S = Sample LF = Lab fortified sample FF = Field fortified sample LCS= Laboratory Control Spike CK = Check Standard ND = N ot detected N Q = Not quantifiable AvgResp. o f the250 ppt Standards (area): 9117 Response o fthe Check Standard (area): 9594 Percent Difference (% ): - 5 2 % difference acceptable i f within 15% Spreadsheet prepared by: RJZ032619 EID185093 Exygen % / (_ /R E SEARCH 3058 Research Drive State College, PA 16801 Phone:814-272-1039 Fax:814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number: 008-046 Matrix: Water Sponsor Study/Protocol No: NA ~ The samples listed below were removed from refrigerator No. *& Time Id- l o ______ Date t * - 11 ~ " I Initials CLIENT SAMPLE ID na EXYGEN ID NUMBER 0106020 Control VOLUME (mL) ! FORTIFICATION (ng) 40.0 - _ aa 0106020 Spk A 40.0 2.0 na 0106020 SpkB 40.0 20.0 WWK-D-Bldg-293 0112725 SpkC 40.0 20.0 WWK-D-Lubeck-Offiee 0112726 SpkD 40.0 20.0 WWK-G-LPWD-Well-F 0112727 SpkE 40.0 20.0 WWK-G-LPWD-Well-A 0112728 SpkF 403) 20.0 WWK-G-LPWD-Well-B 0112729 SpkG 40.0 20.0 WWK-D-Bldg-293 0112725 40.0 - WWK-D-Bldg-293 0112725Dup 40.0 - WWK-D-Lubeck-Office 0112726 40.0 - WWK-D-Lubeck-Oflice WWK-G-LPWD-Well-F 0112726 Dup 0112727 40.0 40.0 - -. WWK-G-LPWD-Well-F 0112727 Dup 40.0 - WWK-G-LPWD-Well-A 0112728 40.0 - WWK-G-LPWD-Well-A 0112728 Dup 40.0 - WWK-G-LPWD-Well-B. WWK-G-LPWD-Well-B 0112729 0112729Dup 40.0 40.0 ` ' - , - - - - -- i y S p ik in g S o lu tio n U sed V olum e U sed fo r S p ik in g In itia l/D a te 0106020 Spk A F070901-3 (10 ng/m L) 200 pL (200 pL m icropipet:) z A I l l 'l l i b i 0106020 SpkB F070901-2 (100 ng/m L) 200 |tL (200 pL m icropipet) / 0112725 SpkC F070901-2 (100 ng/m L) 200 pL (200 pL m icropipet) / JT 0112726 SpkD F 07090I-2 (100 ng/m L) 200 pL (200 pL m icropipet) / U 0112727 SpkE F070901-2 (100 ng/m L) 200 pL (200 pL m icropipet) / 0112728 SpkF 0112729 Spk O F070901-2 (100 ng/m L) F070901-2 (100 ng/m L) 200 pL (200 uL nucropipet) 200 pL (200 pL m icropipet) / vk / - All samples were measured: . Time l t<-14 p Date t 6 - 1 1 ~ l Initials After measuring samples were returned to refrigerator No. >o Time 11 ^.T______ Date te> - t y ~ 1 Initials Xz 2 Comments: 200 p L o f 250 mg/mL sodium thiosulfate was added to alt samples before spitting. Wtials/Dste: X u ' l n l ' l Analyse: Summary: DataSet: lO H O lR l 11 Data Set: -- Data Set: Initials/Date: Initials/Date: Initials/Date: p&L- / tollfelol 'J/ ! ~ ~/ ~ Set extraction/analvsis data verified bv: f lolfllol Date: Ml July 26,2001/6 RJZ032620 EID185094 RESEARCH 3058 Rsearch Drive State College, PA 16801 Phone: 814-272-1039 Fax:814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYOEN STUDY NUMBER: METHOD; $ PROTOCOL NUMBER: NA MATRIX: Water ANALYTES: PROA Client ID ExygenID na WWK-D-Bldg-293 WWK-D-Lubeck-Office WWK-G-LPWD-Well-F WWK-G-LPWD-Well-A WWK-G-LPWD-Weli-B WWK-D-Bldg-293 WWK-D-Bldg-293 WWK-D-Lubeck-Office WWK-D-Lubeck-Office WWK-G-LPWD-Well-F WWK-G-LPWD-Well-F WWK-G-LPWD-Well-A WWK-G-LPWD-Weli*A WWK-G-LPWD-Well-B WWK-G-LPWD-Well-B 0106020 Control 0106020 Sole A 0106020 SpkB 0112725 SpkC 0112726 SpkD 0112727 SpkE 0112728 Spk F 0112729 Spk G 0112725 0112725Dup 0112726 0112726Dup 0112727 0112727 Dup 0112728 0112728 Dup 0112729 0112729Dup *Initlals/Date . STEP 1 STEP 2 \r ~ V0-<ri \V Dilutions (mL/mL) 0,5/ l . O 1/ STEP 3 Dilutions (mL/mL) -- -- -- -- -- --, -- --. --_ -- $ t~ tolflol ! - fa -- - -- - STEP 4 -- -- - -- -- -- -- -- -- -- -- -- -- -- -- -- -- - -- Reagents/ Materials Methanol CIS SPE Type I Water Lot# q .|a L vu I i i b 6 z NA InitiaWDate XL 1 * -1 7 -* ! - HPLc Methanol Ammonium Acetate TypeI water -floZ s' 1A247G NA initials/Dat Mu STEP 1: SPE column clean-up STEP 2: Final volume to 5 mL collected in 15 mL polypropolenc tubes STEP 3: LC/MS/MS analysis STEP 4: LC/MS/MS reanalysis. ' Initials and date under each step indicates the personnel that performed this step. SS Method ofAnalysis for the Determination o f Perfluorooctanoic Acid (PFOA) in Water COMMENTS: Final extracts stored in refrigerator Iff Initials: Date: loll~lio 1 July 19, 2001/4 .V Masslynx - Sample List Sample Ust: C:\MASSLYNX\008-046,PRO\SampieeDB\1017 01B,SPL Printed: Thu Oct 18 07:07:13 2001 iM |M &[ i6 |o i Exygen STUDY NO- m f c A Page 1 Page Position: (1,1) Vial File Name UMS ID Client ID Sam ple Description Matrix Sam ple Type Cone (ppt) C one B C oncC T est ID DF MS Method i ; 1 1 101701B-201 2 2 101701B-202 -- 3 3 101701B-203 -- 4 4 101701B-204 ... 5 5 101701B-205 6 6 101701B-206 ... 7 7 101701B-207 ... 8 92 101701B-208 9 41 101701B-209 ... 10 42 101701B-210 11 43 101701B-211 12 44 101701B-212 ... 13 45 101701B-213 14 46 101701B-214 15 47 101701 B-215 ... 16 2 101701B-216 ... 17 48 101701B-217 18 49 1017018-218 19 50 101701B-219 20 51 101701B-220 21 52 101701B-221 22 53 101701B-222 23 3 101701B-223 24 54 101701B-224 25 55 101701B-225 26 56 101701B-226 27 57 101701B-227 -- 28 58 101701B-228 29 59 101701B-229 30 4 101701B-230 31 60 1017018-231 32 61 101701B-232 33 62 101701B-233 34 63 101701B-234 35 5 101701B-235 ... 36 6 101701B-236 -- ... ... _ ... _ ... _ ... -- ... __ - ... _ -- _ -- ... -- -- ... -- XC101501-0.0 ppt standard XC101501-1, 50 ppt standard XC101501-2,100 ppt standard XC101501-3,250 ppt standard XC101501-4,500 ppt standard XC101501-5,1000 ppt standard XC101501-6, 250 pptcheck standard Methanol Wash 0106020 Control 0106020 Spk A, 50 ppt 0106020 Spk B, 500 ppt 0112725 Spk C, 500 ppt, DF=2 0112725 Spk C, 500 ppt 0112726 Spk D, 500 ppt, DF=2 0112726 Spk D, 500 ppt XC101501-1,50 ppt standard 0112727 Spk E, 500 ppt, 0F=2 0112727 Spk E, 500 ppt 0112728 Spk F, 500 ppt, DF=2 0112728 Spk F, 500 ppt 0112729 Spk G, 500 ppt, DF=2 0112729 Spk G, 500 ppt XC101501-2,100 ppt standard 0112725 0112725 Dup 0112726 0112726 Dup 0112727 0112727 Dup XC101501-3,250 ppt standard 0112728 0112728 Dup 0112729 0112729 Dup XC101601-4, 500 ppt standard XC101501-5,1000 ppt standard --. ... -- -- -- -- -- -- ... -- -- -- -- -- -- -- -- -- -- -- -- -- -- ... -- -- -- -- Blank Standard Standard Standard Standard Standard QC Blank Blank QC QC QC QC QC QC Standard QC QC QC QC QC QC Standard Analyte Analyte Analyte Analyte Analyte Analyte Standard Analyte Analyte Analyte Analyte Standard Standard 0 50 100 250 500 1000 250 -- 50 500 250 500 250 500 50 250 500 250 500 250 500 100 -- -- -- I -- 250 I ~ -- 500 1000 ----0 1 PFOA ... 0 1 PFOA ----0 --0 1 PFOA 1 PFOA ----0 1 PFOA ----0 ----0 1 PFOA 1 PFOA ---- -- -- -- ... 0 0 0 0 1 PFOA 1 PFOA 1 PFOA 1 PFOA -- *-- 0 . 0 2 PFOA 1 PFOA ... 0 2 PFOA -- --0 1 PFOA -- 0 1 PFOA --* 0 2 PFOA ... -- 1 PFOA 0 2 PFOA -- 0 1 PFOA *-- -- 0 ... -- 0 --0 --0 2 PFOA 1 PFOA 1 PFOA 1 PFOA -- -- 0 1 PFOA *-- --* 0 0 1 PFOA 1 PFOA --0 1 PFOA -- . 0 -- 0 0 1 PFOA 1 PFOA 1 PFOA ----0 1 PFOA ** 0 1 PFOA 0 ,1 PFOA -- 0 1 PFOA "" 0 1 PFOA R JZ 0 32622 Mass lynx Sample List Sample List; C:\MASSLYNX\008-046.PRO\tSSaammppleleDDBB\\1100117701 B.SPL Printed: Thu Oct 18 07:07:13 2001 d' OA l t1 y O' l HPLC Method MS Tune File InJ Volume (pL) 1 water PFOA WATER 15 2 water PFOA WATER 15 3 water PFOA WATER 15 4 water PFOA WATER 15 5 water PFOA WATER 15 6 water PFOA WATER 15 7 water PFOA WATER 15 8 water PFOA WATER 15 9 water PFOA WATER 15 10 water PFOA WATER 15 11 - water PFOA WATER 15 12 water PFOA WATER 15 13 water PFOA WATER 15 14 water PFOA WATER 15 15 water PFOA WATER 15 16 water PFOA WATER 15 17 water PFOA WATER 15 18 water PFOA WATER 15 19 water PFOA WATER 15 20 water PFOA WATER 15 21 water PFOA WATER 15 22 water PFOA WATER 15 23 water PFOA WATER 15 24 water PFOA WATER 15 25 water PFOA WATER 15 26 water PFOA WATER 15 27. water PFOA WATER 15 28 water PFOA WATER 15 29 water PFOA WATER 15 30 water PFOA WATER 15 31 water PFOA WATER 15 32 water PFOA WATER 15 33 water PFOA WATER 15 34 water PFOA WATER 15 35 water PFOA WATER 15 36 water PFOA WATER 15 H 0D R JZ0 32623 I Exygen stu d y ooM b .. J Page 2 Page Position: (2,1) LC/M S/M S SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: 008-046 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #7) ELECTROSPRAY ION SOURCE: Capillary: 3.0 kV Hexapole 1:0 V Aperture 1: 0 V Hexapole 2: 0 V Source Block Temp.: 100C Desolvation Temp.: 300C ANALYZER: LMRes 1:10.5 V HMRes 1: 10.5 V Energy 1:1.0 V Entrance: -2 V Exit 2 V LMRes 2 : 13.0 V HMRes 2: 13.0 V Energy 2 : 2.0 V Multiplier: 700 V GAS FLOWS AND PRESSURE: Desolvation N2Flow Rate: -650 L/hr Nebuliser N* Flow Rate: ~150 L/hr Gas Cell Pressure: --0.003 mbar Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment Hewlett Packard (HP) Series 1100 HP Quat Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Column Temperature: Mobile Phase (A) : Mobile Phase (B ): Genesis C-8,5 cm x 2.1 mm i.d. x 4 p (Exygen ID: 37A) (JONESCHROMATOGRPHY: Part No. FK5962E) 35C 2 mM Ammonium Acetate in Type 1Water Methanol Injected Volume: Ions monitored . Analyte PFOA Time (min) %A 0.0 60.0 0.4 60.0 1.0 10.0 7.0 10.0 7.5 0.0 9.0 0.0 9.5 60.0 13.5 60.0 14.0 60.0 Total run time = 14 min 15 pL %B 40. 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 Flow Rate CmL/min) 0.3 0.3 03 03 03 0.4 0.4 0.4 03 Parent ion Daughter ion Dwell (secs) . Coll Energy (eV) Cone (V) 413 369 0,2 10 50 Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814)272-1039 FAX: (814) 231-1580 All Handwritten Peak-ED's by:_ wewest-tuiePronoms FmMueslsiaAm ,<m ) i b T v e ftH VALUES USOEb O^THI^ $. Kgu|(ol RJZ032624 EID185098 Scanning Method Report M ethod: C :\M A S S L 2 H X \0 0 8 -0 4 6 . PRO\ACQUDB\PK>A L a s t M o d ifie d : Mon O c t 15 1 2 :3 7 :2 6 2001 P rin te d : F r i Nov 09 0 9 :4 1 :2 6 2001 S o lv e n t D elay { m ine ) ; 1 .0 0 F u n ctio n : 1 MRM o f 1 M a s s P a i r { E S P -- ) I n te r C hannel D elay { Secs ) : Span ( D alto n s ) : S t a r t T im e { M in3 ) : E nd Tim e ( M in3 ) : R ep eats : C hannel P a re n t D aughter 0 .0 3 0 .0 0 0 .0 0 8 .0 0 1 D w ell (S e c s) C o ll E nergy (eV> C o n e ( V ) 1 4 1 3 .0 0 3 6 9 .0 0 0 .2 0 10 50 Paga 1 RJZ032625 E X D 185099 Method Report Method File: hast Modified: Printed: C i\MASSLTMC\008-046. PRO\ACQUDB\watar Friday, N o v e m b e r 09, 2001 09:38*47 Friday, Nove m b e r 09, 2001 09:42:01 HP1100 L C P im p I n i t i a l C o n d itio n s Solvents A% B% C% % .60.0 40.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C| Oven Temperature Right(C) 0.300 14.0 0 400 3S.0 35.0 HP1 1 0 0 LC Pump g r a d i e n t T i m e t a b l e The gradient Timetable contains 9 entries which are : Time 0.00 0.40 1.00 7.00 7.50 9.00 9.50 13.50 14.00 At 60.0 60.0 10.0 10.0 0.0 0.0 60.0 60.0 60.0 Bt 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 KP110O LC Pump External Event Timetable The Timetable contains 4 entries which are : Time Initial 0.00 0.10 8.00 Column Switch Off Off Off Off Contactl Off On Off Off Contact2 Off Off On Off Contact3 Off Off Off Off Contact4 Off Off Off Off HP1100 Autosampler Initial Conditiona Draw Speed Eject Speed (/il/min) Draw Position (mm) Stop Time (mins) Injection Volume(pi) Vial Number . 200.0 200 0.10 14.00 15.0 6 Paga 1 Pressure 400 400 400 400 400 400 400 400 400 RJZ032626 EID185100 In order to verify mass resolution, a calibration check is performed on the mass spectrometer using aN al/R b/C s tuning solution. The tuning solution is infused onto the mass spec using an infusion pump set to a flow rate o f 10 pL/m in. An MS scan from 80 to 1380 amu is perfomed on both MS 1 and M S2. The calibration is considered acceptable if the follow ing 11 peaks are found within 0.2 amu o f their known m asses on both M SI and MS2: 84.9, 132.9, 172.8, 3 2 2 .7 ,4 7 2 .6 ,6 2 2 .5 ,7 7 2 .4 , 922.3,1072.2,1222.1 and 1372.0. I f any o f the m asses are outside the 0.2 amu, then the instrument w ill b e recalibrated and another calibration,check performed. The printouts from the calibration check can be found on foe follow ing 2 pages. X -.3058 Research Drwe M m s tSalatte College, PA 16801, USA w J : 814.272.1039 F: 814.231.1580 ejcygen.com RJZ032627 EID185101 Calibration Check o f NalRbCs090800 on MS1 using NalRbCs tuning solution CALCHK091001-1 13 (0.611 ) Cn (Cen,2,80.00, Ht); Sm (Mn, 2x2.00); Sb (1,40.00 ); Cm (1:16) 100- 172.8 l#ll|o| l c /m s /m s #7| 10-Sep-2001 08:53:03 Scan ES+ 1.11e8 THIS IS AN EXACTCOPY OF THEORIGINAL DOCUMENT.* BY___fe__ riATF ( M o l Exygen study n o * 132.8 %- 322.8 472.7 M H 84.9 O / 190.8 CD 622.5 ^ 232,9 H O hO 772.4 922.2 87.0 C s5o100 234.8 / fi 4M W 4 * . 200 30 340.8 / 382.9 .390.8 400 532,7558.7 590.5,706.6 840.4 .856.4 Ir+ J l 6 " ' " 7 " ' " 8 " ' " 9 ' 1072.2 1222.1 1371,9 990.2 11402 1290.0 1f40i0*0' ' f 1. 1100 1200 ' ` " 3'00 ' i m/z RJZ032628 Calibration Check o f NaIRbCs090800 on MS2 using RbCs tuning solution CALCHK091001-2 9 (0.559) Cn (C e n ,2 ,80.00, Hi); Sm (Mn, 2x2.00); Sb (1,40.00); Cm (1:17) i m 172.8 LC7MS/MS #7 10-Sep-2001 08:55:20 MS2 ES+ 1.0468 132.9 %- T H IS IS AN EXACT COPY OF THE ORIGINAL DOCUMENT* BY------ J L ------ -DATE..iljftftlo / E x y g e n STUDY N O 0 $ ^ 92.0 / 322.8 472.7 622.5 190.8 / .232.9 772.4 922.3 lp 234.8 / 340.8 / ^82.9 532.7 440.8 556,6 690.5.706.5 -5W 640,4^856.3 990.2 -Mr* 1072.1 1134.0 1221.9 1289.9 71.8 m/z 100 200 3 S o 400 50 ' 6 '' 705 8..............90 1000 1100 1200 1300 il r' t:;. i. i t. i i t i Initial Calibration Curve Exygea Study No.: Set No: Extraction Date: A nilyzednm 008-046 10I701B 10/17/01 10/18/01 The first curve o f the data set 3med to determineperformance. A linear regression (with no weighting) is performed using the first six standards ofthe analytical run. The coefficient o f determination (R Square) must be 0.985 or greater. If die set fads to meet this requirement, the ran must be rejected and the samples reanalyzed Exyaen ID XC10I501-0 XC101501-1 XC101501-2 X C I0101-3 XC101501-4 XC101501-5 Standard C oncentration (nji/L ) 0 50 to o 250 500 1000 Peak A rea 0 2269 4485 9753 20662 40877 C oefficient ofD eteim ination: 0.99963071 SUMMARY OUTPUT R e g r e s s io n S ta tis tic s M ultiple R 0.99981534 R Square 0.99963071 A djusted R Squa: 0.99953839 Standard E rro r 333.267525 O bservations____________ 6 ANOVA R egression R esidual of S MS F S ig n ific a n c e F 1 1202591346 I.2E+09 10827.597 5.1147E-08 I 00 4 111067.2 5 1203035615 Intercept C o e ffic ie n ts S ta n d a r d E r r o r tS ta t 95.7073733" 184.143363 0.519744 40.7746083 0.391853524 104.0557 P -v a lu e L o w e r 9 5 % U p p e r 9 5 % L o w e r 9 5 .0 % U p p e r 9 5 .0 % 0.6306791 415.557624 606.972371 -415.55762 606.972371 5.I15E -08 39.6866462 41.8625703 39.6866462 41.8625703 RJZ03263O EID185104 Q u an tify C a lib ra tio n R ep o rt jt R iah a S tu d y N o .: 0 0 8 -0 4 6 , S e t No: 101701B , E x t. D a te : 1 0 /1 7 /0 1 , A n a ly s t. K ^ 3" a C a l i b r a t i o n : p:\Data\LCMSMS7 \Ma3 alynx\0 0 8 -0 4 6 .PRO\CurvaDB\1 0 1 7 0 1B m l a s t m o d ified : F c i O ct 19 0 7 :0 8 :1 0 2001 P rin ted : F r i O ct 19 07 :1 5 :1 4 2001 Page X RJZ032631 EID185105 Quantify Sample Report Study No.: 008-046, Set No: 101701B, Ext- Date: 10/17/01, Analyst: K Risha S am p le L i s t : P :\D ata\L C M S M S 7 \M asslynx\008-046.P R O \S am ploD B \101701b L a s t m o d ifio d i F r i O ct. 19 0 7 i0 7 :3 3 2001 M ethod: . P :\D a ta \L C M S M S 7 \M a 3 3 ly n x \0 0 8 -0 4 6 .P R 0 \M o th D B \1 0 1 6 0 1 PFOA L a st m odified: Wed Oct 17 07:42:45 2001 Jo b Code: P rin te d : F r i O ct 19 0 7 :1 5 :1 6 2001 Initiate______ DRuania#.,,~SSJg2|Ei I 2 qT Nama: 101701B -201 T ex t: Exygen Research RJZ032632 EID185106 Quantify Sampla Report Study No.: 008-046, Set No: 101701B, E x t . D a t e : 1 0 / 1 7 / 0 1 , A n a l y s t : K R i s h a S am p le L i s t : P :\D ata\L C M S M S 7\M asalynx\Q 08-046.E B O \S am pleD B V l01701b L a s t m o d ifie d : F r i O ct 19 0 7 :0 7 :3 3 2001 Method: P:\Data\LCMSMS7\Ma33lynx\008-046.PRO\MethDB\101601 PFOA h a s t m o d if ie d : W ed O c t 17 0 7 :4 2 :4 5 2001 Jo b Coda: P rin te d : F r i O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B -202 T ex t: Page 2 Exygen Research RJZ032633 EID185107 Quantify Sample Report Study No.: 008-046, Set Ho: 101701B, Ext. Data: 10/17/01, Analyst: K Ri3ha S am p le L i s t : P :\D ata\L C M S M S 7 \M asslynx\008-046.P R O \S am plaD B \101701b L a s t m o d ifie d : F r i O ct 19 0 7 :0 7 :3 3 2001 M ethod: P :\D a ta \L C M S M S 7 \M a s s ly n x \0 0 8 -0 4 6 .P R 0 \M eth D B \lQ 1 6 O l PFOA L a s t m o d if ie d : Wed O c t 17 0 7 :4 2 :4 5 20 0 1 Job Code: P rin te d : F r i O ct 19 0 7 :1 5 :1 6 2001 Harne: 1 0 1 7 0 1 B -2 0 3 T ex t: Page 3 Exygen Research RJZ032634 EID185108 Q u a n tif y Sam p ia R e p o rt S tu d y No. : 008-046, S e t No: 101701B, E x t. D a ta : 1 0 /1 7 /0 1 , A n a ly st: K R ish a S am p le l i s t : P :\D ata\L C M S M B 7 \M as3 ly n x \0 0 8 -0 4 6 . P R O \S am plaD B \l01701b L a s t m o d ifie d : F r i O ct 19 0 7 :0 7 :3 3 2001 M ethod: P :\D a ta \L C M S M S 7 \M asa ly n x \0 0 8 -0 4 6 .E R O \M eth D B \1 0 1 6 0 1 PFOA L a s t m o d if ie d : Wad O c t 17 0 7 :4 2 :4 5 2 0 0 1 Jo b Code: P rin te d : F r i O ct 19 0 7 :1 5 :1 5 2001 Sago 4 Name: 101701B -204 T ex t: 1 : PFOA ______ XC 101501-3,250 ppt standard 101701B-204 S m (Mn, 2x2) I-. 100a i 18-0ct-2001 09:42:43 LC/MS/MS #7 MRM of 1 Channel ES5.10 413 > 369 1.81e5 ii O ' | ' i ' i i-i--i"r i i i i 1 1 1 1 i 11l l r i 1 1 ' r `~ 2.00________3.00________ 4.00 i i - p - r n 1 1' n ' | - i- T i--f -| . i i t r . -r-] T im e 5,00_____ ago_____ 7 jg _____ 8.00 1. Exygen Research 1 RJZ032635 EID185109 Quantify Sample Report Study Ho.: 008-046, Set No: 101701B, Ext. Date: 10/17/01, Analyst: K Risha S am p le L i s t : P :\D ata\L C M S M S 7\M asslynx\008-046.P R O \S am plaD B \101701b L a s t m o d ified : F r i O ct 19 0 7 :0 7 :3 3 2001 M ethod: P :\D a ta \L C M S M S 7 \M assly iix \0 0 8 -0 4 6 .P R O \M eth D B \1 0 1 6 0 1 PFOA L a s t m o d if ie d : W ed O c t 17 0 7 :4 2 :4 5 2 0 0 1 Jo b Code: P rin te d : F r i O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B -205 T ex t: Page 5 Exygon Research RJZ032636 EID185110 Quantify Sample Report Study So.: 008-046, Set No: 101701B, Ext. Date: 10/17/01, Analyst: K Risha S am ple l i s t : P :\D ata\L C M S M S 7\M a3slynx\008-046.F R O \S am pleD B \101701b L ast: m o d ifie d : F r i O ct 19 0 7 :0 7 :3 3 2001 Method: P:\Data\LCMSMS7\Masslyiuc\008-046.PRO\MQthDB\101601 PFOA. L a s t m o d i f i e d : Wed O c t 17 0 7 :4 2 :4 5 2 0 0 1 Jo b Code: P rin te d : F ri O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B -206 T ex t: Paga 6 Exygen R esearch RJZ032637 EID185111 Quantify Sample Report Study No.: 008-046, Set No: 101701B, Ext. Date: 10/17/01, Analyst: K Risha S am ple L i s t : P :\D ata\L C M S M S 7\M a3S lynx\0Q 8-046.P R D \S am pleD B \101701b L a st m o d ified : F r i O ot 19 0 7 :0 7 :3 3 2001 M ethod: P :\D a ta \lC M S M S 7 \M a 3 3 ly n x \0 0 8 - 0 4 6 .P R O \M e th D B \1 0 1 6 0 1 PEOA L a s t m o d ifie d : Wed O c t 17 0 7 :4 2 :4 5 2 0 0 1 Job Code: P rin te d : F r i O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B -207 T ex t: 1 : PFOA Page 7 Exygen Research RJZ032638 EID185112 Quantify Sample Report Study No.: 008-046, Set No: 101701B, Ext. Date: 10/17/01, Analyst: K Risha Sample List: P:\Data\LCMSMS7\Ma33lynx\008-046.PRO\SampleDB\101701b L a st m o d ifie d : F r i O ct 19 0 7 :0 7 :3 3 2001 Method: P:\Data\LCMSMS7\Masslyux\OO8-O46.PR0\MethDB\lO16Ol PFOA L a s t m o d if ie d : W ed O c t 17 0 7 :4 2 :4 5 2 0 0 1 Job Code: P rin te d : F r i O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B -208 T ex t: Page 8 Exygen Research RJZ032639 EID185113 Quantify Sample Report: Study No.: 008-046, Set No: 101701B, Ext. Date: 10/17/01, Analyst: K Eisha S am ple L i s t : P :\D ata\L C M S M S 7 \M assly n x \0 0 8 -0 4 6 .PR O \S anpleD B \101701b L a s t m o d ifie d : F r i O ct 19 0 7 :0 7 :3 3 2001 M ethod: P :\D ataV L C M S M S 7 \M assly n x \0 0 8 -0 4 6 .P R O \M eth D B \1 0 1 6 0 1 PFOA L a s t m o d if ie d : Wed O c t 17 0 7 :4 2 :4 5 2 0 0 1 Job Coda: P rin te d : F r i O ot 19 0 7 :1 5 :1 6 2001 Name: 101701B -209 Hext: Page 9 Exygen Research RJZ032640 EID185114 Quantify Sample Report Study No.; 000-046,. Set No: 101701B, Ext. Date: 10/17/01, Analyst: K Risha S am ple L i s t : P :\D ata\liC M S M S 7\M asslynx\008~046.P R O \S am pleD B \101701b L a s t m o d ified : F r i O ct 19 0 7 :0 7 :3 3 2001 M ethod: P :\D a ta \L C M S M S 7 \M a s s ly n x \0 0 8 -0 4 6 .P R O \M e th D B \1 0 1 S 0 1 PFOA L a s t m o d i f i e d : Wed O c t 17 0 7 :4 2 :4 S 2 0 0 1 Job Code: . P rin ted : F r i O ct 19 0 7 :1 5 :1 5 2001 Name: 101701B -210 T ext: 1: PFOA Page 10 Exygen Research RJZ032641 EID185115 Quantify Sample Report Study No.: 008-046, Set No: 101701B, Ext. Date: 10/17/01, Analyst: K Risha Sample List: P:\Data\BCMSMS7\Masslynx\00 8-046. PRO\SampleDB\101701b Last modified: F r i Oct 19 07:07:33 2001 , . ,,,,,,,, Method: P:\Data\LCMSMS7\Ha3slynx\008-046.PRO\MethDB\101601 PFOA h a s t m o d if ie d : Wed O c t 17 0 7 :4 2 :4 5 2 0 0 1 Job Coda: P rin te d : F ri O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B -211 T ex t: Page 11 Exygen Research RJZ032642 EID185116 Quantify Sample Report Study Ho.: 0Q8~046, Set No: 101701B, Ext. Date: 10/17/01, Analyst: K Risha Sample List: P:\Data\LCMSMS7\Ma33lynx\008-046.PRO\SamploDB\101701b Last modified: F ri O at 19 0 7 :0 7 :3 3 2001 F:\Data\LCMSMS7\Mas3lynx\008-046.PRO\MetbDB\lQ16Ql PFOA Method: Last modified: Wad O a t 1 7 0 7 : 4 2 : 4 5 2 0 0 1 Job Code: P rin te d : F ri O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B -212 Text: Page 12 Exygon Research RJZ032643 f EID185117 Quantify Sample Report ,, Study No.: 008-046, Sat No: 101701B, Ext. Data: 10/17/01, Analyst: K Risha Sample list: P:\Data\LCMSMS7\Ma33lyxuc\008-046.PRO\SampleDB\101701b L a st m o d ified : F r i O ct 19 0 7 :0 7 :3 3 2001 Method: P:\Data\LCMSMS7\Ma3slynx\008-046.PRO\MathDB\101601 PFOA Lagt modified: Wed O c t 17 0 7 : 4 2 : 4 5 2 0 0 1 J o b Coda: P rin ted : E ri O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B -213 T ex t: Page 13 Exygen Research RJZ032644 EID185118 Quantify Sample Report Study No.: 008-046, Set No: 101701B, Ext. Data: 10/17/01, Analyst: K Risha Sample List: P:\Data\XXMSHS7\Masslynx\008-046.PRO\SampleDB\101701b L a st m o d ifie d : F r i O ct 19 0 7 :0 7 :3 3 2001 , . .. ... Method: P:\Data\LCMSMS7\Masslynx\008-046.PRO\MetbDB\101601 PFOA L a s t m o d ified : Nad O ct 17 0 7 :4 2 :4 5 2001 Job Coda: P rin te d : F ri O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B -214 T ex t: Paga 14 Exygon Research RJZ032645 EID185119 Quantify Sample Report Study No.: 00B-046, Sat No: 101701B, Ext. Data: 10/17/01, Analyst: K Risha S am p le L i s t : P:\D ata\L C M SM S7\M asslynx\O O 8-O 46.PR 0\S am pleD B U O 17O lb L a st m o d ified : F ri O ct 19 0 7 :0 7 :3 3 2001 . Method: P:\Data\LCMSMS7\Masslynx\008-046. PRD\MethDB\101S01 PFQA L a s t m o d if ie d : Wed O c t 17 0 7 :4 2 :4 5 2 0 0 1 Job Code: P rin te d : F ri O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B -215 Text: Page 15 Exygen Research RJZ032646 EID185120 Quantify Sample Report Study No.: 008-046, Sat No: 1017D1B, Ext. Data: 10/17/01, Analyst: K Risha S am ple l i s t : P :\D ata\lC M S M S 7\M a33lynx\008-046.P R O \S aspleD B \101701b l a s t m o d ified : F ri O ct 19 0 7 :0 7 :3 3 2001 M ethod: P :\D a ta \lC M S M S 7 S M a 3 3 ly n x \0 0 8 -0 4 6 .P R 0 \M o th D B \1 0 1 6 0 1 PFOA l a s t m o d if ie d : Wed O c t 17 0 7 :4 2 :4 5 2 0 0 1 Jo b Code: P rin te d : F ri O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B -216 T ex t: Pago 16 Exygen Research RJZ032647 EID185121 Quantify Sample Report Study Ho.: 008-046, Sat Ho: 101701B, Ext. Data: 10/17/01, Analyst: K Risha. S am ple L i s t : P :\D ata\L C M S M S7\M a3slynx\008-046.P R O \S am pleD B \101701b Last modified: Fri O c t 19 07:07:33 2001 Method: P:\Data\LCMSMS7\Ma3slynx\008-046.PHO\MethDB\101601 PFOA L a s t m o d if ie d : Wed O c t 17 0 7 :4 2 :4 5 2 0 0 1 Job Code: Printed: Fri Oct 19 07:15:16 2001 Pago 17 Hamo: 101701B -217 T ex t: 1 : PFOA 0112727 S pk E, 500 ppt, DF=2 101701B-217 Sm (Mn, 2x2) 100-1 18-0ct-2001 13:18:59 LC/M S/N IS #71 MRM of 1 Channel E S 5.10 413 > 369 2.16e5 %- I i i I i I ' i r ( T Time 0- 2.00 3.00 4.00 5.00 6.00 7.00 8.00 RJZ032648 EID185122 Quantify Sample Report ^ Study Ho.: 008-046, Sot No: 101701B, Ext. Data: 10/17/01, Analyst: K Riaha S am ple L i s t : P :\D ata\L C M S M S7\M a33lynx\008-046.P R O \Sam pleD B \101701b L a st m o d ified : Fxx O ct 19 0 7 :0 7 :3 3 2001 M ethod: P:\Data\LCMSMS7\Ma33lynx\008-046.PRO\MethDB\101601 EFOA L a s t m o d ifie d : Ned O ct 17 0 7 :4 2 :4 5 2001 Job Code: P rin te d : F r i O ct 19 0 7 :1 5 :1 $ 2001 Hams: 101701B -218 le x t: Page 18 Exygen Research RJZ032649 EID185123 Quantify Sample Report S tu d y N o .- 008 -0 4 6 , S o t No: 101701B , Ext. Data: 10/17/01, Analyst: KRisha Sam ple L is t : L a st m o d ified : M ethod: L a st m o d ified : Job Coda: P : \D ata\L C M S M S 7 \M assly n x \0 0 8 -0 4 6 . PRO \Sam plaD B \101701b F r i O ct 19 0 7 :0 7 :3 3 2001 P :\D a ta \L C M S M S 7 \M a 3 3 ly n x \0 0 8 -0 4 6 .P R O \M ath D B \1 0 1 6 O l PFQA Wed O c t 17 0 7 :4 2 :4 5 2 0 0 1 P rin te d : F ri O ct 19 0 7 :1 5 :1 6 2001 Paga 19 Name: 101701B -219 T ex t: Exygen Rasaarch RJZ032650 EID185124 Quantify Sampla Report Study Mo.: 008-046, Sot Mo: 101701B, Ext. Dato: 10/17/01, Analyst: K Eisha Sample List: P:\Data\LCMSMS7\biasslynx\008 - 0 4 6 . P R O \S a m p le D B \1 0 1 7 0 1 b Last modified: Fri Dot 19 07:07:33 2001 Method: P:\Data\LCMSMS7\Masslynx\008 - 0 4 S .P R O \M e th D B \1 0 1 6 0 1 PFOA Last modified: Med Oct 17 07:42:45 2001 Job Code: P rin ted : F ri O ct 19 0 7 :1 5 :1 6 2001 Harne: 1 0 1 7 0 1 B -2 2 0 T ext: Page 20 Exygen Research RJZ032651 EID185125 Quantify Sample Report Study No.: 008-046, Sat No: 101701B, Ext. Data: 10/17/01, Analyst: K Risha S am ple L i s t : P :\D ata\X C M S M S 7\M asslynx\008-046.P R O \S am pleD B \101701b L a s t m o d ified : F ri O ct 10 0 7 :0 7 :3 3 2001 M ethod: P:\Data\lCMSMS7\Mas3lynx\008-046.PRO\MethPB\101601 PFOA L a s t m o d if ie d : Wed O c t 17 0 7 :4 2 :4 5 2001 Job Code: P rin te d : F r i O ct 19 0 7 :1 5 :1 6 2001 Paga 21 Name: 101701B -221 T ex t: 1 : PFOA_____________ 0112729 Spk G, 500 ppt, DF=2 101701B-221 Sm (Mn, 2x2) 1 0 0 "i 18-0ct-2001 14:25:54 L c m s m s #7 MRM of 1 Channel E'S5.09 413 > 369 2.54e5 %- 0 -rn Time 2.00 3.00 4.00 5.00________ 6.00 7.00 8.00 RJZ032652 EX D 185126 Quantify Sample Report ... Study Ho.: 008-046, Sat Ho: 101701B, Ext. Data: 10/17/01, Analyst: K Kasha S a m p le L i s t : P:\Data\LQiSMS7\Ma3slynx\008-046.PRQ\SampleDB\101701b L a s t n o d i f i o d t Fed. O c t 19 07:07:33 2001 Method: P:\Data\LCMSMS7\Mas3lynx\008-046.PRO\MethDB\101601 PFOA L a s t m o d i f i e d : H a d O c t 17 07:42:45 2001 Job Coda: P rin te d : F ri O ct 19 0 7 :1 5 :1 6 2001 Hama: 1017Q 1B -222 fa x t: Paga 22 Exygan Research RJZ032653 EID185127 Q u a n tify Sam ple H o p o rt S t u d y N o . : 0 0 8 - 0 4 6 , S o t N o : 1 0 1 7 0 1 B , E x t . D a t o : 1 0 / 1 7 / 0 1 , Analyst: K Risha Sam ple L is t : P :\D ata\L C M S M S 7\M as3lynx\008-046.P R O \S am plaD B \101701b L a st m o d ified : F ri O ct 10 0 7 :0 7 :3 3 2001 ___ M ethod: P :\D a ta \L a iS M S 7 \M a s 3 ly m x \0 0 9 - 0 4 6 .F R O \M a th D B \1 0 1 6 0 1 PFOA L a s t m o d i f i e d : Wed O c t 17 0 7 :4 2 :4 5 2 0 0 1 Jo b Code: P rin te d : F ri O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B-223 T ex t: Pago 23 Exygon Research RJZ032654 EID185128 Quantify Sample Report Study No.: 008-046, Sot No: 101701B, Ext. Date: 10/17/01, Analyst: K Risha Sam ple L i s t : P :\D ata\L C M S M S 7\M asslynx\008-046.P R O \S am pleD B \101701b L a st m o d ified : F r i O ct 19 0 7 :0 7 :3 3 2001 M ethod: P :\D ata\L O iS M S 7\M asslynx\008-046.P R O \M ethD B \101601 PF0A L a s t m o d if ie d : Wed O c t 17 0 7 :4 2 :4 5 2001 Job Code: P rin ted : F r i O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B -224 T ex t: Page 24 Exygen Research RJZ032655 EID185129 Quantify Sample Report Study No.: 008-046, Set No: 101701B, Ext. Date: 10/17/01, Analyst: K Risha List: P:\Data\LCMSMS7\Masslynx\008-04S.PRO\SampleDB\101701b Last modified: Fri Ocl: 19 07:07:33 2001 Method: P:\Data\LCMSMS7\Ma33lynx\008-046.PRO\MethDB\101601 PFOA L a s t m o d if ie d : Wed O c t 17 0 7 :4 2 :4 5 2 0 0 1 Job Code: P rin ted : F ri O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B -225 T ex t: Paga 25 Exygen Research RJZ032656 EID185130 Quantify Sample Report Study No.: 008-046, Sat Ho: 101701B, Ext. Date: 10/17/01, Analyst: K Risha Sample list: P:\Data\LCMSMS7\Masslynx\008-046.PRO\SampleDB\101701b Last modified: F r i Oct. 19 07:07:33 2001 M ethod: P :\D a ta \L C M S M S 7 \M a s s ly n x \0 0 8 -0 4 6 .P R O \M e th D B \1 0 1 6 0 1 PFOA L a s t m o d if ie d : Wed O c t 17 0 7 :4 2 :4 5 2001 Jo b Coda: P rin te d : F r i O ct 19 07 :1 5 :1 6 2001 Harne: 101701B-226 T ex t: Pago 26 Exygen Research RJZ032657 EID185131 Quantify Sample Report Study Ho.: 008-046, Sat Ho: 101701B, Ext. Date: 10/17/01, Analyst: K Risha S am ple L i s t : P :\D ata\lC 24S M S 7\M as3lynx\008-046.P R O \S am pleD B \101701b l a s t m o d ified : F ri O ot 19 0 7 :0 7 :3 3 2001 M ethod: P :\D a ta \lC M S M S 7 \ M a 3 3 l y n x \ 0 0 8 - 0 4 6 . P R O \M a th D B \l0 1 6 0 1 PFOA. l a s t m o d ified : Hed O ct 17 0 7 :4 2 :4 5 2001 Jo b Code: P rin te d : F ri O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B-227 T ex t: Page 27 Exygen Research RJZ032658 EID185132 Quantify Sample Report Study No.: 008-046, Set Ho: 101701B, Ext. Date: 10/17/01, Analyst: K Riaha S am ple L is t : L a st m o d ified : M ethod: ' L a s t m o d ified : Jo b Coda: P :\D ata\L C M S M S7\fctasslynx\008-046.E R O \S am pleD B \101701b F x i O ct 19 0 7 :0 7 :3 3 2001 P:\Data\LCMSMS7\Ma33lynx\008-046.PRO\MathDB\101601 PFOA Wad O c t 17 0 7 :4 2 :4 5 2001 P rin te d : F r i O ct 19 0 7 :1 5 :1 6 2001 Hame: 10170 IB -228 T ex t: Page 28 Exygen Research RJZ032659 EID185133 Quantify Sample Report Study Ho.: 008-046, Sot Ho: 101701B, Ext. Data: 10/17/01, Analyst: K Kasha Sample X.X3t: P : \D ata\I.C M S M S 7 \M a a s l y n x \ 0 0 8 --0 4 6 .P R O \S a m p la D B \1 0 1 7 0 1 b last modified: F r i O o t 1 9 0 7 : 0 7 : 3 3 2 0 0 1 Method: P:\Data\LCMSMS7\Masslynx\008-04 6,PRO\MethDB\101601 PFOA l a s t m o d i f i e d : Wed O c t 17 07:42:45 2001 Job Code: P rin te d : E ri O ct 19 0 7 :1 5 :1 6 2001 Hama: 101701B -229 Text: Paga 29 Exygen Research RJZ032660 EID185134 Quantify Sampla Report Study No.: 008-046, Sot No: 101701B, Ext. Data: 10/17/01, Analyst: K Riaha S am ple L i s t : P :\D ata\L C M S M S 7\M as3lynx\009-045.P R O \S am pleD B \101701b L a st m o d ified : F ri O ct 19 0 7 :0 7 :3 3 2001 M ethod: P :\D a ta \L C M S M S 7 \M a s 3 ly n x \0 0 8 -0 4 6 .P R O \M a th D B \1 0 1 6 0 1 PFOA L a s t m o d if ie d : Wed O c t 17 0 7 :4 2 :4 5 2 0 0 1 Job Code: P rin te d : F ri O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B -230 te x t: Pago 30 . Exygen Research RJZ032661 EID185135 Quantify Sample Report study No.: 008-046, Sot No: 101701B, Ext. Dato: 10/17/01, Analyst: K Risha S am ple L is t: P :\D ata\L C M S M S7\M a33lynx\008-046.P R Q \Sam ploD B \101701b L a s t m o d ified : F r i O at 19 0 7 :0 7 :3 3 2001 M ethod: P :\D a ta \L C M S M S 7 \M a 3 s ly n x \0 0 8 -0 4 6 .P R 0 \M o th D B \1 0 1 6 0 1 PFOA L a s t m o d ifie d : Hod O ct 17 0 7 :4 2 :4 5 2001 Job Coda: P rin te d : F ri O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B-231 T ex t; Paga 31 Exygen Research RJZ032662 EID185136 Quantify Sample Report . Study No.: 008-046, Sat No: 101701B, Ext. Data: 10/17/01, Analyst: K Rxsha Sam ple L i a t : P:\D ata\L C M S M S7\H a33lY nx\008-04S .P R O \S am pleD B \101701b X*ast m o d i f i e d : F r i O c t 1 9 0 7 : 0 7 : 3 3 2 0 0 1 M ethod: P:\Data\LCMSMS7\Ma33lynx\008--046.PRO\MathDB\101601 PFOA L a3 t m o d i f i e d : Wed O c t 17 0 7 :4 2 :4 5 2 0 0 1 Job Code: P rin te d : F ri O ct 19 0 7 :1 5 :1 6 2001 Name: 1017Q 1B-232 T ex t: Paga 32 Exygen Research RJZ032663 EID185137 Quantify Sampia Raport Study No.: 008-046, Sat No: 101701B, E x t . D a t a : 1 0 / 1 7 / 0 1 , A n a l y s t : K R i s i l a Sample list: P:\Data\LCMSMS7\Masslynx\008-046.PRO\SampleDB\101701b l a s t m o d ifie d : F ri O ct 10 07 :0 7 :3 3 2001 M ethod: P :\D a ta \lC M S M S 7 \M a 3 3 ly n x \0 0 8 - 0 4 6 .P R 0 \M o th D B \1 0 1 6 0 1 PFQA l a s t m o d i f i e d : Wed O c t 17 0 7 :4 2 :4 5 2 0 0 1 Job Code: P rin te d : F r i O ct 19 0 7 :1 5 :1 6 2001 Hamo: 101701B -233 T ex t: Page 33 Exygen Research RJZ032664 EID185138 Quantify Sample Ropoirt Study Ho.: 008-046, Sot Ho: 101701B, Ext. Data: 10/17/01, Analyst: K Rxsha Sample List: P:\Data\LCMSMS7\Ma33lynx\008-046.ER0\SamploDB\101701b La3t m o d ified : F ri O ot 19 0 7 :0 7 :3 3 2001 Method: P:\Data\LCMSMS7XMa33lynx\008-046.PRO\MethDB\101601 PFOA h a s t m o d if ie d : Wed O c t 17 0 7 :4 2 :,4 5 2 0 0 1 Jo b Code: P rin te d : F ri O ct 19 0 7 :1 5 :1 6 2001 Hama: 101701B-234 T ex t: Pago 34 Exygon Research RJZ032665 EID185139 Quantify Sample Report Study No.: 008-046, Sot No: 101701B, Ext. Data: 10/17/01, Analyst: K Riaha S am ple L i s t : P :\D ata\L C M S M S 7\M as3lynx\008-046.P R O \S am pleD B \101701b L a s t m o d ifie d : F t i O ct 19 0 7 :0 7 :3 3 2001 M ethod: P :\D a ta \L C M S M S 7 \M a ssly n x \0 0 8 -0 4 6 .F R O \M e th D B \1 0 1 6 0 1 PFOA L a s t m o d if ie d : Wed O c t 17 0 7 :4 2 :4 5 2 0 0 1 Jo b Code: P rin te d : F ri O ct 19 0 7 :1 5 :1 6 2001 Name: 101701B -235 T ex t: Page 35 Exygen Research RJZ032666 EX D 185140 Quantify Sample Report Study Ho,: 008-046, Sat Ho: 101701B, Ext. Data: 10/17/01, Analyst: K Rxsha Sample list: P:\Data\LCMSMS7\Masslynx\008-046.PRO\SampleDB\101701b L a st m o d ifio d : F r i O ct 19 0 7 :0 7 :3 3 2001 Method: P:\Data\LCMSMS7\Masslynx\00a-046.PRO\MethDB\101601 PFOA L a s t m o d if ie d : Wed O c t 17 0 7 :4 2 :4 5 2 0 0 1 Job Coda: P rin te d : F ri O ct 19 0 7 :1 5 :1 6 2001 Hama: 101701B -236 T ext: Paga 36 Exygen Research RJZ032667 EID185141 EID 185142 RESEARCH Precise Research. Proven Results. The follow ing pages are exact copies o f information for the standards used in this study. PentadecafluorooCtanoic acid (Inventory 01-008-75), obtained from Aldrich (lot # 08316DO) was used to make a stock solution (BD # S070901-1) which in turn, was used to make intermediate solutions (ID #'s F 07090M , F070901-2 and F070901-3). These intermediate solutions are used to prepare extracted calibration standards, laboratory control sam ples, and matrix spike samples. PentadecafluorooCtanoic acid (Inventory #:01-008-092), obtained flora Fluorochem USA (lot # U14D) was used to make a stock solution (ID # S10150I-1) which in turn, was used to make intermediate solutions (ED#'sF 101501-l andF101501-2). These intermediate solutions are used to prepare the check standard, which is designed as an independent source verification o f the calibration standards. The information on the follow ing pages provides the exact sources, lot numbers, shipping information, expiration dates and storage conditions o f the neat standards. A lso included are the preparation o f stock standard and fortification solution forms. These pages show the exact details o f the preparation o f each o f the stock and fortification solutions, as w ell as their expiration dates and storage conditions. RJZ032669 EID185143 Centre Analytical Laboratories, Inc. 3040 R esearch D rive Stai* C o fo g a , P A 16801 Phon*: (814) 231-8032 F a (814) 231-1253 o r (814) 231-1500 ANALYTICAL TEST, CONTROL AND REFERENCE STANDARDS RECEIPT & INVENTORY LOG Substance: PF.KlTMsKAf(JOEOQCTAMo\C ftU h Page Centre Analytical Inventory Number: Q l-00ft"* T 5 Amount Received (g): Gross Weight Received (g): 3 4 . 31S~R 3 4 .5 ^ 4 2 . Date Received: 6 llo 5 lo l Condition Upon R eceipt Frozen-RefriaeratedHAmbient^ R eceived From: Al KP'HA (M EM _ Lot/Batch N o.:. D BSILK d Date Last Characterized 1. UA 2. ________ 3 . ____________ Expiration Date O t jo s l o Z :____ % Purity Initials/Date i Storage Location: .FE6E2ER. B A STftVMEKCAftiHEX4 3 Logged in By: f m l t l U k l A k i ) ----------------------- D ate:. 7 / 05I 0I Date OlhlM Initial Gross WL fa) 34.SA52- Amount Withdrawn fa) o.oio42. Gross WL After Withdrawal Balance ID (g )_____ 34.5-HT- . Me Purpose/CAL Initials I Study Number oo8-04t> JL- . Comments: wa6H ria e e fW t e c ^ iM a -|& 0i|[6{i>t Removed from Inventory Q Returned to Sponsor Log continued next page THIS tS AN EXACTCOPYOF THEORIGINALDOCUMENT.' BY------- kS^L. , DATE .J llffilo L . (Mals/Date) (Inittals/Date) 8 February2001/4 RJZ032670 EID185144 t?l H H oe tn Hfe w Cl U1 N 0 W N 01 J H - n a -.ch Uw*.Jcaiw w* Ant. Product Numbanl714BS Product N am eiPentadecafluoroctanoic acid, 96% Itad h utitM t'inittA iin^ Description/Prising Cert. o( Analysis Enter Lot No MSDS S fu m a Print Preview Bulk Quote Ask A Sdentisi S A L P H I O r _____________:___________________________ ^ __________________ CertifeateofAnalyss TEST Product Name Product Number CAS Number Formula Formula Weight APPEARANCE INFRARED SPECTRUM TITRATION GAS LIQUID CHROMATOGRAPHY TITRATION QUALITY CONTROL ACCEPTANCE DATE SPECIFICATION Pentadecalluorooctanoic acid, 96% 171466 335671 CF3(CF2)bC 0 2H 414.06 WHITE TO OFF-WHITE POWDER CONFORMS TO STRUCTURE AND STANDARD AS ILLUSTRATED 95.5% -104.5% (WITH NAOH) 95.5% (MINIMUM) 2 % H 20 (MAXIMUM) LOT {08316DO} RESULTS WHITE POWDER CONFORMS TO STRUCTURE AND STANDARD. 100.4% (WITH NAOH) 99.9% 1.48% H 20 (WITH 'KARL FISCHER' REAGENT) JUNE 2001 David S w essel, Supervisor Quality Control P?ii I o f i http://info.sial.com /cgi-bin/gx.cgi/A pplogic+C O fA Info.R eturnC O fA II 8/2/01 3058 Research Drive 5tate College, PA16801 Phone: 814-272-1039 Fax: 814-231-1580 ANALYTICAL TEST, CONTROL AND REFERENCE STANDARDS RECEIPT & INVENTORY LOG {^FlD60MCtM4lC.. Substance: PEHTAtCAPUJOR.OCrAVllCA o L OR Kf-IL CPFoM Page ____ Exygen Inventory Number: 0 1~~QQfe- __________________ ____________ _ Amount Received (g): _______ Gross Weight Received (g): IS. Date Received: |hl |x \p l Condition Upon Receipt: Frozen-Refriaerated^AmbienT) Received From :FUIiSgnCR.V\ U6A____ . Lot/Batch No.: U -l4 b _________ _ D ate Last C h a ra c te rize d 1. UUYNbtOtJ______ 2 . . ______________________ 3 . ________________ Expiration D ate .. IDlUloT- _________________ ____________ % Purity V S to ra g e Location: S t C A f c l R H -A.2- ( F E f . Initiais/Data L ogged In By: / vflHlM- A H - / _____________ _ Date: lojlT-lbl Standard Custodian Review: L r -- d i r / '. D ate: ifijl^jpl Date l|\S |bl ..U /tr t/--o t Initial Gross Wt. fa) Amount Withdrawn (g) O-OlOSI ____ Gross Wt. After Withdrawal (9) ' ' 15.0O3OO .___ Balance ID It Purpose/Exygen Initials Study Number fl B - tlt -M - "XrYJ<nW .U C e V Comm ents: Log continued next page T H IS IS AN EXACT COPY OF THE ORIGINAL DOCUMENT.' . BY------- ^ _____ DATE--./i[l$[Pt. O R em o v ed from In v e n to ry ________ ____________________ (inWals/Date) Q R etu rn e d to S p o n so r ____________________________ (initlais^Date) 15 August 2001/5 RJZ032674 EX D 185147 Centre Analytical Laboratories, Inc. 3048 Research Drive Phone: 814) 231-8032 Slate College, PA 16801 Facsimile: (014) 231-1253 Page. PREPARATION OF STOCK STANDARD SOLUTION Protocol Number: ____________________ CAL Study Number: 0C6 ~ O'fb - Compound: PfitThNR-A FLUnRftOGTftNOll AUh Lot Number: C tolL L o_________ Source: fM&RU-K Purity: ^ % Date Last Characterized: NA Date Standard Received: Q llostol_____ Storage Location: STANAMI CAftlriCT3 Compound Expiration Date: nll&sl 02- CAL Inventory #: l~~ ______ A calibration check must have been conducted with the balance on the day o fsample weighing. Balance Calibration , , ------------ p)$tn|<mo 1 Stock Solution Balance Number: Pf ft .. Net Wt. o f Substance: 0. 0 1b 4 2. _g Logbook page for calibration data: 4 Wt. Adjusted for Purity: b.OIOOO _g _ Solvent: taHAUOL Manufacturer: FWifqPiiiE Lot Number: MlO^-C____________ Final Volume: Concentration: lDD loO mL _jtg/m L Stock Solution F.xpiratinn D ate*: I02-. Stock Solution ID: S 0~70^6|- | Stock Soln ID #: SMMDDYY- i ,2,3,etc. * Assign a one year expiration date for ail stock solutions unless otherwise indicated bv sponsor. . Storage Conditions for Solution: Freezer Number '-- Refrigerator Number: f t Room Temperature: ; Indicate which of die above is applicable, and location. REMARKS: RJZ032677 EID185148 Centre Analytical Laboratories, Inc. ' 3048 Research Drive Stale College, PA 16801 Phone: (814) 231-8032 Facsimile: (814) 231-1253 P a g e ______ PREPARATION OF FORTIFICATION STANDARD SOLUTIONS Protocol N um ber:_________ Z ___________ CAL Study Number: 0 0 6 ' % Date Prepared: P llo ^ lo l______________ Expiration D a te* :___ O ^ M o ? -______ ' Assign a one year expiration date for all dilations unless otherwise indicated bv sponsor. Separate sheets should be usedfo rfortification standards and calibration standards. Dilution o f .. Initial Aliquot Diluted to Solvent Final Final solution Compound IDS (code no.) SofTool-1 FWloH ) Ftnolot-2 i' Conc. (pg/mL) loo I.D 6-1 volume (mL) 1.0 10. o lb.0 _ volume (n i) 100 loo too '- (or solvent number) lAtH __ 1__ f -- conc. (jig/mL) t .0 O. \ 0.01 - solution ID S'* . Ftrufloi-i Ft0*101-2 Fot<l-3 F- _-- - --. - F- __ - - --- - F- _ - -- - - -- F- - ---- - --F- If 2 or more standard solutions are combined to make a mixed standard solution, indicate with a bracket of the solutions used. Solvent 1: Uf.lRAvloL- - Manufacturer: Lot No.: HIO2^ -- Solvent 2 : ______ ~ _______ . Manufacturer: Lot No.: ____________ Solvents: ' ______ _ Manufacturer: ___________ Lot N o .:____________ ** This must be a unique number. Use this system: Fortification Soin ID #: FM M DDYY-l.2.3, etc. Storage Conditions for Solution: Freezer Number. - Refrigerator Number: t3 Room Temperature: Indicate which o f the above is applicable, and location._____________ REMARKS: Oi" Signature Date: o i y . p i February 1995/2 "THIS IS AN EXACT COPY OF THE ORIGINAL DOCUMENT.* B Y _ _ m = ____ DATE fllQ a P-L RJZ032678 EID185149 3058 Research Drive Phone: 814-272-1039 State College, PA16801 Fax: 814-231-1580 Page PREPARATION OF STOCK STANDARD SOLUTION Protocol Number: MA___________ __ Exygen Study Number: fl-0 % Compound: C h> ( T O Lot Number: ____ Source: RUbRMriEfrft Purity: `'H % Date Last Characterized: M h Date Standard Received: lpjlT-W l - Storage Location: $TfvNb- riAS:^ 2 . Compound Expiration Date: 1o|D -1& 2. _ Exygen Inventory # :. ____ A TM llhraHon check most have been conducted with the balance on the day o fsample weighing. Balance Calibration .Stock Solution Balance N um ber:_____ lb ________ Logbook page for 7calibration data: _______ N et Wt. o f Material: , .0 ,b l l___ g W t. Adjusted for Purity: ....ft*Pl0,g,O _g Solvent: A&TVMAoL-________ . Manufacturer RM SGE-UHS Lot Number l2t>2-__________ Final Volume:_____ ____________ mL Concentration:----------IgO--------------pg/mL ' Stock Solution Expiration Date* : ,6 T (H-loV Stock Solution ID: S IQISQl.zJ--- Stock Soin ID SMMDDYY-l,2,3,ctc. * Assign a one year expiration date for all stock solutions unless otherwise indicated by sponsor. Storage Conditions for Solution:________________ Freezer N um ber -- Refrigerator Number: l^> Room Temperature: Indicate which o fthe above is applicable, and location. REMARKS: Signature: Qj Date: ipbloi M y IS, 2001/4 t h i s i s a n e x a c t c o p y o f THE ORIGINAL DOCUMENT." RJZ032679 EID185150 3058 Research Drive Phone: 814-272-1039 State College, PA 16801 Fax: 814-231-1580 Page PREPARATION OF FORTIFICATION STANDARD SOLUTIONS ProtocolNumber: NK _______ _ BxygenStudyNumber: ^ ' 0 % DatePrepared: lbjl5lt?l_______ _ ExpirationDate*: _____ Assign a one year expiration date for all dilutions unless otherwise indicated by sponsor. Separate sheets should be usedforfortification standards and calibration standards. Dilution o f solution ID # Compound (code no.) Initial Cone. (PKfaL) Aliquot volume (tuL) Diluted to volume (mL) Solvent (or solvent number) Final cone. (UR/mL) Final solution ID #** 5 lD l5 D \-l f f k P io m b i-1 PFA IDO 1 .0 1 .0 ib .O -- l o o ___ 10 -- V ct)H N \tO iL -- 1 .0 o .\ ~ F1M 501-1 F 101501-2. F~ __ -- -- .-- ' ___ ---- -- -- -- -- -- -- F F F -- -- -- -- -- ---- ~~ F -- - - -- -- -- *'* F - If 2 or more standard solutions are combined to make a mixed standard solution, indicate the solutions used with a bracket Solvent 1: N\ETVlM4oL Manufacturer: Lot No.: -- 412& 2- ... Solvent 2: ________ Manufacturer: ~ LotN o .:------- Z -------- Solvent 3 : _____________ _ Manufacturer: __________Lot N o .:---------------- ** This m ust be a unique number. Use this system: Fortification Soin ID : FMMDDYY-1,2,}, etc. ' Storage Conditions for Solution:________________ Freezer Number: REMARKS: -- Refiigerator Number: B Room Temperature: Indicatewhich ofthe aboveis applicable, and location. ________ ' T H IS IS AN EXACT COPY O F THE ORIGINAL DOCUMENT.* BY -D A T E lljo B fo L RJZ032680 EID185151 Barley Mill Plaza. Building 27________ ________ Lancaster Pike & Routa 1________ ;________ Wilmington. PE 19805 R JZ 032681 E ID 18 5152