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Exyeen ^J ^_^RREESSEEAAFRCH^Lpr.e_d_s-"eRReseseeaarrcchh.. .\, Proven Results. AR226-2501 Analytical Report Ruorochemical Characterization of Water Samples DuPont Washington Works Exygen Research Laboratory Report No. 008-046 B (Revision 1) Testing Laboratory \ ExygBn Research, Inc. 3058 Research Drive . State College, PA 16801 Requester Michael D. Aucoin URS Corporation Bariey Mill Plaza Bldg27Room2121 Lancaster Pike and Rt 141 Wilmington, DB.19805 PAGE t OF 5 y w3' ^058 Research State College, Dri PA ve 16 8 0 1 , USA J: 800.2B1.3219 K8-t4.272.1019 exygen-com RJZ032545 EID185019 T fnfrocfifctioa! 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 liquidchromatography/ 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 Compound Name Ammonium Perfluorooctanoate Acronym APFO 2. Sampre-KeEeipK ; ;. The samples were submitted h Individual plastic conta'ners, cooled with wet ice. Samples were collected on 10/11/01. Samples were received on 10/12/01. Chain-of-custody informafon is presented in Attachment C. 3. SToMngTimes The analytical method used was validated against a maximum holding time of 14 days in water samples. Alt samples were analyzed within 14 days erfcollection. 4 IWsthods - AnalyfEsaTancKPreparafbry^ 4.1 4.1.1 LC/MS/MS Sample Preparation for LC/MS/MS Analysis Water samples were InitiaBytreated with 200 uL of 250 mg/L sodium thiosuBate solution to remove residual chlorine. Solid phase extraction (SPE) was used to prepare the samples for LC/MS/MS analysis. A forty-milliliterportionof sample was transfeired to a C)B SPE cartridge. The cartridge was eluted with 40% methanol: water. The eluate was discarded;. The cartridge was then eluted with 100% methanol. A 5 mL portion of methanot was collected for analysis by LC/MS/MS. This treatment resulted in an eight-fold 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 chromatographfc column. Based on the affinity of the analyte for the stationary phase v\ the column relative to PAGE20FS RJZ032546 EID185020 tha liquidmobile phase, ths anatyte is retained for a characteristic amount of time. Follow'ng HPLC separation. ES/MS provides a rapid and accurate means for analyzing a wide range of organic compounds, including fluorochemicals. Bectrospray 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 llffima MS/MS was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Samples were extracted on 10/17/01. Samples were analyzed by MS/MS between 10/17/01 andlO/19/01. Haw analytical data can be found m Attachment D. 5? JSnialysfs-- 5.1 Calibration A 6-point calibration curve was analyzed at the beginning of the analytical sequence and throughout the run for the compounds of interest. The caltoratlon points were prepared at p, 50,100, 250, 500, and 1000 ng/L (ppt). 'The instrument response versus the concentration was plotted for each point Using linear regression with 1A( weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determination (r2) were determined. A calibration curve is acceptable if r^O.992 (rS 0.985). Calibration standards for MS/MS analysis were prepared using the same SPE procedure used for samples. For the results reported here, calibration criteria were met 5.2 Blanks Extraction blanks were prepared and analyzed with every extraction batch of samples. The extraction blanks should not have any target analyles present at or above the concentration of the low-level calibration standard. For these samples, the extraction blanks were compliant Instrument blanks in the form of clean methanol solvent were also analyzed after every highlevel calibration standard, and after known high-level samples. Again, tha 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 tor every field sample at concentrations of 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 in duplicate. Resute are given along with the sample results in Attachment A. PAGE30F5 RJZ032547 EID185021 5.6 Laboratory Control Samples Milliqwater 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 set ~ 6f DafsSamma'iy ;,':'. '.;.... . .'i5-...^ Please see Attachment A for a detailed listingof the analytical results. All results are reported in (ng/L)parts pertrBlion. p Wata/Sampfe^ Retention- Samples are disposed of one month after the report fe issued unless otherwise specified- All electronic data is archived on retrievable media and hard copy reports are stored In data folders maintained by Exygen. Affacnmenfs. 8.1 AttachmentA: Results '-';-' ^ :" -. 8.2 Attachment B: Matrix Spike Recoveries 8.3 Attachment C: Chain of Custody 8.4 Attachment D: LC/MS/MS Raw Analytical Data 8.5 Attachment E Standards Data PAGE40F5 RJZ032548 EID185022 ^ -T'"?"' "C-^^ ^ z ^ ^ ^ ' r, Oporations Manager Kevin J Lloyd, Vfce President Other Lab Members Contributingto Data Karen Smith ^/^/y Date ^IS(0> Date PAGE50FS RJZ032549 EID185023 1 FLYW%TPPIT tekV^i S; (^RESEARCH' \ f Kl: UPredse Research. \ Prown Results. Bxygen Research Laboratory Report 008-046B Revision 1 This revision was performed to report results as ammonium perfhiorooctanoate (APFO) to conform to.historical reporting practices. Additional quality control data was also added at the request of DuPont. A.Date /^~^________^^___ a/, ft) /<fohnM. Haherty ,3058 Research Drive .Sate Cblfey. PA 16801, USA ,T: 800.281.3219 f-. 814.27Z1019 exygen.conn RJZ032550 EID185024 yyrjs^ RJZ032551 EID185025 RESEAR.CH kpredse R&earch. '-. Proven-R&ute. Repoil --Analyhcal,- Analytical ResuHs-fiuPont Washington Works DuPont Sample Identihcatlon WWK-D-Hdg-1-Main WWK-D-adg-1-Main (laboratoly dupMcate) WWK-<3-Hd!l-1-Maln-2 WWK-<3-Bdn-1-Mailv-2 (laboratHryAjplicato) WWK-<3-WB^332 WWK-G-WoH-332 (laboratoly dupi'cale) WWK-D-Hdg-231 WWK-D-Bldg-231 (labcratoiydupllcalB) WWK-D-BMB-293 WWK-D-Bldg-233 (laboratory duplicate) , WWK-D-lJibedc-OHIce WWK-D-Lttbeck-Offlce llabotatoly dupllcalBji WWK-Q-LPWD-WefrF WWK-0-LPWD-Well-Fffabotatoiy duplicate) "-. WWK-<3-LPWI>W9ll-A WWK-Q-LPWD-Well-A Qaboratotyduplicate) WWK-G4-PWt)-Well-B WWK-<3-UWO-WB-B (laboratoty dupncats) WWK-K-FBLK-1 WWK-K-FBLK-2 r^-a^. Bi K.."ccy-^y rw vy-l 507 463 U ^ i j c ^ ^ -Ju 3/i d ^ ^ ^ ' - / ^ ' ^ / e > t 471 / 463 49B 469 450 459 t-^t Z/of 423 390 621 ^ S5 60S --^ 288 -^" 264^ 703-^--" ^7 684 5B1 9.3<f .. 568 \ND ND ti3 (. 1^t9 ^ ^s) t'l T. C.^8 C.38 Llinit of Detection (LOD) tor tie procedure is appoxiniately"?^ ngrt. Uniil of QuanSlalion (LOO) for lha procedure is SO ng/L \ ND - Compound not detected NQ - Compound detected at a level between the LOO and LOO. ReauH b not quanaiable. ND<U3D<NQ<LOQ "-h... ADnve [e, PA 16801, US^ T: 814.272.1039 f: 814^31-1580 exygen-oom RJZ032552 EID185026 V- - B ^ RJZ032553 EID185027 Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: | WWK-D-Bldg-1-Main Spiked Amount (ng/L): | 500 IPFOA 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 Concentrations represent amounts present as the perfluorooctanoate anion. RJZ032554 EID185028 Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: | WWK-G-Bldg-1 -Main-21 Spiked Amount (ng/L): | 500 IPFOA Sample Concentration (ngA.) 453 Matrix Spike Result (ng/L) 901 Matrix Spike Result (% Recovery) 89,6 Criteria (Pass/Fail) PASS Lower Recovery Limit 70 Upper Recovery Limit: 130 Concentrations represent amounts present as the perfluorooctanoate anion. ~i RJZ032555 EID185029 Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: | WWK-G-Well-332 Spiked Amount (ng/L): | 500 |PFOA 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 as the perfluorooctanoate anion. RJZ032556 EID185030 Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: | WWK-D-Bldg-231 Spiked Amount (ng/L): | 500 |PFOA 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 130 Concentrations represent amounts present as the perfluorooctanoate anfon. RJZ032557 EID185031 Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: | WWK-D-Bldg-293 Spiked Amount (ng/L): | 500 IPFOA 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 Sample ID: | WWK-D-Lubeck Office Spiked Amount (ng/L): | 500" IPFOA Sample Concentration (ng/L) 597 Matrix Spike Result (ng/L) 1080 Matrix Spike Result (% Recovety) 96.6 Criteria (Pass/Fail) PASS Lower Recovery Limit 70 Upper Recovery Limit 130 Concentrations represent amounts present as ths perfluorooctanoate anion. RJZ032559 EID185033 Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: | WWK-G-LPWD-Well F Spiked Amount (ng/L): | 500 IPFOA Sample Concentration (ng/L) 277 Matrix Spike Result (ng/L) 715 Matrix Spike Result (% Recovery) 87.6 Criteria (Pass/Fail) PASS Lower Recovery Limit: 70 Upper Recovery Limit: 130 Concentrations represent amounts present as the perfluorooctanoate anion. RJZ032560 EID185034 Attachment B: LC/MS/MS Laboratory Spike Recovery r" Sample ID: | WWK-G-LPWD-Well A Spiked Amount (ng/L): | 500 IPFOA Sample Concentration (ng/L) 675 Matrix Spike Result (ng/L) 1105 Matrix Spike Result (% Recovery) 86.0 Criteria (Pass/Fail) PASS Lower Recovery Limit: 70 Upper Recovery Limit 130 Concentrations represent amounts present as the perfluorooctanoate anfan. RJZ032561 EID185035 Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: | WWK-6-LPWD-Wel B' Spiked Amount (ng/L): | 500 IPFOA 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 perfluorooctanoate anion. KJZ032562 EID185036 w-cww^ C :-:?&s'-; i- RJZ032563 EID185037 @!S ^SHSffiffi 011271B wwh-D-Bldg-1-Maln 0112720 0112721 WWK.G-Bldg.1Maln-2 WWK-Q-Well-a3Z 0112722 WWK-D-Bldg-231 0112723 WWK-K.FBLK-1 0112724 WWK-K-PBLK-2 0112725 WWK-D-Bldg-293 0112726 0112727 0112728 0112729 WWK-D-LubockOftice WWK.G-LPWD. We!l-F WWK-Q-LPWDWell-A WWK-G-LPWOWell-B 10-12-01 10:30 10-12-01 10:30 10-12-01 10:30 10-12-01 10:30 10-12-01 10:30 10-12-01 10:30 10-12-01 10:30 10-12-01 10:30 10.12-01 10:30 10-12-01 10:30 10-12-01 10:30 Exygen Research Sarnpla Login Report Study Number: Protocol; 008.046 NA a!a^iai%mi.w WATER WATEB WATER WATER WATER WATER WATER WATER . WATER WATER WATER S^MSMSip John Plaherty John plarwrty John Flaherty John Flaharty John Flaherty John Plaherty John Flaherty John Flaherty John Flaherty John Flaherty John Flaherty ^ggi!S;B%BBSM| lBSffiSg^E; LAWRENCE 0 COOLER e C- 10-12-01 IAWRENCE 0 COOLER 6 C- 10-12-01 LAWRENCE 0 COOLER 6 C- 10-12-01 LAWRENCE O COOLER 6 C- 10-12-01 LAWRENCE 0 COOLER 6 C- 10.12.01 LAWRENCE 0 COOLER 6 C- 10.12-01 LAWH6NCE 0 10-12.01 COOLER 6 . C- LAWRENCE 0 COOLER 6 C- 10-12-01 LAWRENCE 0 COOLER 6 C- 10-12-01 LAWRENCE 0 COOLER 6 C- 10-12-01 LAWRENCE 0 COOLER 6 C- 10-12-01 Verified By/Date: n ' ^ ^ ^^^11^??^, .^^ 3048 Research Drive State College, PA 16801 phone: (814) 231-8032 Fax; (814) 231-1253 Centre Analytical Laboratories, Inc Chain of Custody/Analysis Request Form - ~ Please fill out this form completely to ensure correct analysis and pr RJZ032566 EID185040 EID185041 RJZ032567 sby-^t-a r.:^}^*^ RJZ032568 EID185042 Sponsor Stndy No:l<A Exygen StndyNo: (M8-046 Analyte: t UTO Ions Monitored: ' 113-> 369 Site: ]1A RAW DATA REPORT IjmitofQuaatilQrioB: 1njecdon Volinrie: )kfatrix: <SampleVolume 1"asl Volume: 50ng(L li>fL Waia40.0 niL 5.0 BiL ( tetNo: 1analyst: ilUiliument'Type: iixtrBOioniDate: i\adyaAaa: IOI701A Karen Risha LC/MS/MS;Unit<7 10/17/01 10/19/01 Exygen T> XC101501-0 XC101501-1 XC101501-2 XC101501-3 XC101501-4 XC101501-5 XC101501-6 McthandWash 0106020 Coatrol 0106020 Spk A - 0106020 SpkB 0112719 SpkC XC101501-1 0112720 SpkD 0112721 SpkE 0112722 SpkF XC101S01-2 0112719 0112719 Dup 0112720 0112720 Dap 0112721 0112721Dnp XC101501-3 0112722 0112722 Dup 0112723 0112724 XC101501-4 XC10150I-5 Sponsor ID - - - - - - - - NA NA NA WWK-D-Bldg-1-Main - WWIC-O-BU-l-Main-Z WWK-O-WeB-332 WWK-D-Bldg-231 - WWK-D-Blilg-1-Main WWK-D-Bldg-1-Mam WWK-G-Bld-l-Main-2 WWK-G-BM-l-Min-2 WWK-O-WeB-332 WWK-G-WeU-332 - WWK-D-Bldg-231 WWK-D-Bldg-231 WWK-K-FBLK-1 WWK-K-FBLK-2 - - Sample Code CS CS CS CS CS CS CK C C LCS LCS LF CS IF LP IF CS S S S S S S CS S S S S CS CS Rim No. 101701A-101 101701A-102 101701A-103 101701A-104 101701A-105 101701A-106 101701A-107 101701A-108 101701A-109 101701A-110 101701A-111 101701A-112 101701A-I14 IOI70IA-115 101701A-1I7 101701A-119 101701A-121 101701A-122 101701A-123 101701A-124 101701A-125 101701A-126 101701A-127 101701A-128 101701A-129 101701A-130 101701A-131 101701A-132 101701A-133 I01701A-134 Std. Cone. W 0 Dilnlioa Factor - Peak Area 1552 50 - 42219 100 - 78392 250 - 172691 500 - 345627 1000 - 652107 250 - 153082 - - 957 - 1 75 - 1 37136 - 1 294914 - 2 288866 50 - 34578 - 2 308063 - 2 310592 - 2 330016 100 - 75043 - 1 332218 - 1 304179 - 1 309519 - 1 304209 - 1 326892 - 1 307712 250 - 167243 - 1 295520 - 1 301617 - 1 1232 - 1 771 500 - 350957 1000 - 686516 PFOA Found (ng/L) = fpeak area - intercept) / slope x DP Recovery (%)= [PFOA found (ngL)-PFOA (bund in control (ng(L)) amount PFOA added (ng/L) xlOO APPO Found (ngrt.) -PPOA feund (iig/L) x ^W APFO (431)/MW PFOA (414)) PFOA Found (>B/L) APFO Found (KR/Ll Anoint PFOA Addcil W Recovery Wl - - - - - - - . - - - - - - . - - . - - - - - - - - - - NQ NQ - - 47.8 49.8 50 96 431 449 500 86 844 879 500 72 - - - - 901 938 500 90 909 946 500 86 967 1010 500 107 - - - - 487 507 - - 445 463 - - 453 471 - - 445 463 - - 479 498 - - 450 469 - ^ - - - 432 450 - - 441 459 - - NQ NQ - - NQ NQ - - - - - - - - - - Standard Curve: Linear (1/x weiehted) Intercept = 497335 Slope- 672-537 CoetOrDet= 0.998381 CS " CalibratioD standard C s= Control sample S= Sample LP -- Lab fortified sample FF - Field fortified sample LCS "Laboratory Comrol Spike CK~ Check Standard ND = Not detected NQ - Not quantifiable AvgRcsp.ofIfae250pptStaiulards(ana): 169967 Responseof the Check Standard (area): 153082 Percent Difference (%): 11.0 % difference acceptable if withio 15% Spread^iect prepared by;. ^- / litooi RJZ032569 EID185043 ^^^^^ '. l r-.....,} M ..-4 I r'' 1 E x y e e n ^/ (^RERSEESAEARRCCH 3058 Research Drive State College, PA 16801 Phone: Fax:8 PREPARATION OF EXTRACTED CALIBRATION STANDARDS Protocol No.; None Method No.: Exygen Study No.: 008-046 Analytes; PEOA Matrix; Ty Sample Vol; 40 Sponsor Sample ID , NA NA NA Exygen Sample ID 0106020 0106020 0106020 Sample Description Type I Water" TypeIWater" . TypeIWater" Fort. Solution ID . P070901-3' F070901.3 Fort, Soln. Cone. diE/mL) - 10 10 Fort. Volume (uLI 200 400 Micropipet used (HU - 200 200 Fort. Level foot) 50 100 Final Solution ID#* XC101501-0 XC101501.1 XC101501-2 NA 0106020 TypeIWater" P070901-2 100 100 200 250 XC101501-3 NA 0106020 Type I Water" F070901-2 100 200 200 500 XC101501.4 NA 0106020 Type I Water" F070901-2 100 400 200 1000 XC101501-5 NA 0106020 . Type I Water" P101501-2 100 100 200 25.0 XC101501-6 - - - - - - . Vertical arrows in a column indicate identical values, **This must be a unique number. Use this system: Extracted Calibration So!n JD it: XCMMDDYY-0.1,2.3, etc, Samples removed fronicfefrigeratorf)reezer *' IS Time; /3^<' Initials/Date; X2- / ^"/^'/'l 40 mL of each sample measured using a S^ mL graduated cylinder. After measuring, samples returned to(refrigeratoj)/freezer # I 8 Time; I V're Initials/Date; Initials/Date; ^> / /"/tr/*/ )(! //"/'s'l'l Samples fortified: SPE clean-up; Final volume adjusted to 5 mL: Extracts placed in refrigerator # 15 Initials/Date; Initials/Date: Initials/Date; Initials/Date; Z./4 / /g/r/p/ yi. _/ nfiJ'f'! yz /IP I ifl<'I }M I jo!|sr{|p STANDARD EXPIRA Comments; '^This type I water has been filtered through a hypercarb Filter Mcihod uf Analysis for the Delcnninailon ofPerfluorooctanoic Acid (PFOA) in Waier. Exyeen TLf ^JRERSESEEAARRCH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax:814-231-1580 Internal Chain of Custody/Fortiiicatfon Sheet Bxygen StudyNumber. 008-046 Matrix: Water Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No. I 6 Time e^ (" Pate /->>-'> Initials yfc CLIENT SAMPLE ID EXYGEN ID NUMBER VOLUME (mL) FORTIFICATION (ng) na 0106020 Control 40.0 - na 0106020 Spk A 40.0 2.0 na WWK-D-BIdg-1-Mam 0106020 SpkB 0112719 Spk C 40-0 40.0 20.0 20.0 WWK-0-Bldg-l-Manr2 0112720 Spk D 40.0 20.0 WWK-G-WeU332 0112721 Spk E 40.0 20.0 WWK-D-Bldg-231 0112722 SpkP 40.0 20.0 WWK-D-Bldg-1-Main 0112719 40.0 . WWK-D-Bldg-1-Main 0112719Dup 40.0 - WWK-G-Bldg-l-Main-2 0112720 40.0 - WWK-G-Bldg-l-Main-2 0112720 Dup 40.0 - WWK-G-Well 332 0112721 40.0 - WWK-G-Well332 0112721 Dup 40.0 - WWK-D-Bldg-231 0112722 40.0 - WWK-D-Bldg-231 0112722 Dup 40.0 - WWK.-K-FBLK-1 0112723 40.0 - WWK.-K-FBLK-2 0112724 40.0 - - - . - - - - - ' - - - 0106020 SpfcA 0106020 Spk B 0112719 Spk C 0112720 Spk D 0112721 Spk B 0112722 Spk F Spiking Solution Used F070901-3 (10 ngftnL) F070901-2(100ng/inL) F07090]-2(100ng/mL) FD70901-2(100ng/niL) F070901-2(100Dg/mL) F07090I-2 (100 Dg/mL) Volume Used for Spiking 200 pL (200 tiLmicropipel) 200 (iL (2(10iiL micropipet) 200 (it (200 fiLinicropipet) 200 nL (200 (iL micropipet) 200 (iL (200 fiL micropipet) 200 )tL (200 liL nricropipet) All samples were measured: Time o 1 S'' - Date I ~ '1 Initials ^ After measuring.samples were returned to refrigerator No. _ Time f I " Date I " - <1 ~" t I 8- Initials J^ Comments: 20anL of 250 me/mLjodimnlhiosuUati: vms added to all samples before sparing. Initials/Dale ^i " Initial/Date -z^ tiffni'i / i i t '* * i ' Analysis SBBBinaly: Data Set: _llbOnnbtA\JA'is__ TD\a*ta SP^et.:. ---- Data Set: Set extraction/analysis data verified by: QfflI " fInaitiaallss^/DDate: ^ / it)U8|ol InMiti-a'lllsp//Dnaittoe.:. SL-I -- Initials/Date: Date: /6^f'f July 26,2001/6 RJZ032571 EID185045 f . .'i 3058 Research Drive State College, PA 16801 Phone:814 Fax:814 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYOEN STUDY NUMBER; 008-046 METHOD; PROTOCOL MATRIX: Basi ANALYTES; PFQA Client ID na na na WWK-D-Bldg.l.Main WWK.-O.Bldg. 1-Main-2 WWK-G.Well 332 WWK-D-Bldg-231 WWK-D-Bldg-1-Main WWK-D-Bldg-1-Main WWK-G-Bldg.1 -Main-2 WWK-Q-Bldg-1-Main-2 WWK-O-Wcll 332 WWK-G-Well 332 WWK-D-Bldg-231 WWK-D-Bldg-231 WWK-K-FBLK-I WWK-K-FBLK-2 . . . ^Initials/Date ExygwID 0105020 Control 0106020SpkA 0106020 SpkB 01127l$SpkC Ol!2720SpkD 0112721 SpkE 0112722 SpkF 0112719 0112719 Dup 0112720 0112720 Dup 0112721 0112721 Dup 0112722 0112722 Dup 0112723 0112724 . - - . STEP 1 STEP 2 \./ . - - M l-i'i-i ' ' . A (.n-'| STEP1; STEP 2; STEP 3; STEP 4; SPE column clean-up Final volume to 5 mL collected in LC/MS/MS analysis LC/MS/MS rcanalysis. 15 rnL polypropolene tubes Dilutions (mL/mL) - 0>"S/,0 w - STEP 3 Dilutions (mL/mL'l - ~ >- -- - STEP 4 - ^ ~ -- - Rea Ma Me C Typ - -, - -- . Inftia -- -. -- -- -- - -- -- -- ^- ^- -- -- ^. -- ^ -- \ -- -- M - . . - Ammon . . .. - Typ io|i?[oi . - - Jr^ft-5- ) 10r)e t>l - --- Initi (bSW"S fU^ bU {W^WW- oO I' W3W uMriL loU^loi^. |ol|'(|oj Inilials and dale under each step indicates (lie personnel that performed (Ilis step. $$ Meiliod of Analysis for the Deiennination orperfluoroocianoic Acid (PFOA) in Water COMMENTS: pinal extracts slored in refriiitrator i 5' Initials; P^LDale; f0|('7(0j "^\/ ("^RREESSEEAARRCH 3058 Research Drive State College. PA 16801 Phone: 814-272-1039 Fax:814-231-1580 SAMPLE TRANSFER SHEET Protocol Number. NA Exygen Study Number; 008-046 Erygen Sample ff 0112719 ^ 0112720^ 0112721 ^ 0112722 -^ 0112723 -^ 0112724-^' 0112725 -/ 0112726 ^ 0112727 .-/" 0112728 ^ Sponsor Sample ft ^ WWK-D-Bldg-l-Main ' ^ WWK-Q-Bldg-l-MaSn 2- WWK-G-Well-332v-^ WWK-D-Bldg-231 "^ ' WWK-K-FBLK-1 1-^ WWK-K-FBLK-2 ^ WWK-D-Bldg-293-^ / ft'WK.-D.Lubeck-Office^. / WWK-G-LPWD-Well-F/ "ftTiVK-G-LPWD-WeU-A^ Exygen Sample ff 0112729 <-^ Sponsor Sample # WWK-G-LPWD-Wdl-B^ - . - - - - - - - - - - Requested Location: iRvecfuriigg i1i8* ^te^ Ibtelbl Requested By (Printed Name/Date) Samples removed from: Samples removed from: Samples removed from: Samples removed from: C~^ ^- -- --- Samples moved to A ~ ' Samples removed &om Samples returned to ^/r ^-6 Comments: Box# 1} j " -^"7} Box# -- Box# -- Box# -- ShelS ShelBf ShelfS Shel C ] ----- --- ^ ^ ^-/S~-'/ Sample Custodian Initials/Date /i /6 -^6> -ot Sample Custodian Inilials/Date July 12,2001/4 RJZ032573 EID185047 Masslynx Sample 1.1st Sample List; C;\MASSLYNX\008-046.PRp\SampteDB\101701a.spl Printed: ThuOct 1813:50:03 2001 wQ i,,|ick|r,i Exygen STUDY NO. JW& Vtal 1 1 2 2 3 3 4 4 5 6 6 6 7 7 8 92 9 11 10 12 11 13 12 14 13 15 14 2 15 16 18 17 17 18 1B 19 19 20 20 21 21 3 22 22 23 23 24 24 25 25 25 26 27 . 27 2B 4 29 28 30 29 31 30 32 31 33 5 34 6 File Name LIMS ID 101701A-101 101701A-I02 101701A-103 101701A-104 101701A-105 101701A-106 101701A-107 101701A-108 101701A-109 101701A-110 101701A-111 101701A-112 101701A-113 101701A-114 101701A-115 101701A-11S 101701A-117. 101701A-11S 101701A-119 101701A-120 101701A-121 101701A-122 101701A-123 101701A-124 101701A-125 101701A-126 101701A-127 101701A-128 101701A-129 101701A-130 101701A-131 101701A-132 101701A-133 101701A-134 Client ID Sample Description 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 XC101S01-6, 250 ppl Check Standard Mathanol Wash 0106020 Control 0106020 Spk A, 50 ppt 0106020 Spk B, 500 ppt 0112719 Spk C, 500 ppt, DF=2 0112719 SpkC, 500 ppt XC101501-1, 50 ppt Standard 0112720 Spk D, 500 ppt, DF=2 0112720 Spk 0,500 ppt 0112721 Spk E, 500 ppt, DF=2 0112721 Spk E, 500 ppt 0112722 Spk P, 500 ppt, DF=2 0112722 Spk F, 500 ppt XC101501-2,100 ppl Standard 0112719 0112719 Dup 0112720 0112720 Dup 0112721 0112721 Dup XC101501-3, 250 ppt Standard 0112722 0112722 Dup 0112723 0112724 XC101S01-4, 500 ppt Standard XC101S01-S, 1000 ppl Standard Matrix Sample Type Standard Standard Standard Standard Standard Standard QC Blank Blank QC QC QC QC Standard QC QC QC QC QC QC Standard Analyte Analyte Analyta Analyta Analyte Analyte Standard Analyts Analyte Analyta Analyta Standard Standard Cone A 0 SO 100 250 500 1000 250 -- -- 60 500 250 500 50 250 600 250 500 250 500 100 -- -- --- --. -- -- 250 -- -- -- .,500 1000 Cone B Cone C 0> <M IB -- a. e- 0 0) ca CL 0| I Q w ^ UJ r^ |S_^0 ^ in>nioioio>oioioio>oio<oio>oin>oio>o 10 loinioul loioiomioioiftinioiolo 5 ? Of 1 ^ ^2 W" ^m t ^ s ^ g 3^ V E >> ~m a-S. y2, ai'i: E OTO- ^ i i l l l ^ l l i l l l l i l i l ^ i j l ^ i j i i l i l l l l i l a><i)(0(Ba>(330>Q}Q)53(I>a.00(0<3fl3ll)0<l>lDQ)<QClBlODQ)0- ie a: c: B: n: a: a: o: n: o: a: a: B: n: Q: n: n: n: n: a: n: o: n: a: a; n: a: a: [C tt: K n; n: n: lULULUUJUJ&UUJLULlJllJUIlUlUUJlJLlLUllJUJllJIJUUJUJUJLUUJtiJtJLJUIlUUJlULUUJUJ l^^^g^^^^^g^^^i^^Hm^^i^^ii^ ^r<^>^o>$^ei5$i?st:?5aRaRsas?iS5S?;s3S RJZ032575 EID185049 LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: 008-046 Instrument: Micromass Quattro Ultima (LC/MS/MS Unitft6)7(^)j^uto6|ol ELECTROSPRAY ION SOURCE: CapilIaiy:3.0kV Hexapole 1:0 V Aperture 1:OV Hexapole2:OV Source Block Temp.: 1OO'C Desolvatfon Temp.: 300C ANALYZER: LM Res, 1:10.5V HM Res 1:10.5V Energy 1:1.0 V Entrance:-2V Exit 2V LM Res 2:13.0V HM Res 2:13.0V IEnergy2:2.0V Multiplier: 650-V GAS FLOWS AND PRESSURE: Desolvation N2 Flow Rate: -650 L/hr Nebuliser N2 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 Micromasa Limited: MagsLynx3.4Build004 HPLC Equipment: HewlettPackard (HP) Series 1100 HP Binary Pump HP Vacuum Degasser BP Airtosampler 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 [i (Exygen ID: 35A) (JONESCHROMATOGRAFHY: Part No. FK5962E) 35C t mM Ammonium Acetate in Type I Water Memanol Injected Volume: Ions monitored: Analvte PFOA Time I'd:nn) 0.0 0.4 1.0 7.0 7.5 9.0 9J 13.5 14.0 Total run time = ISuL % A 60.0 60.0 10-0 10.0 0.0 0.0 60.0 60.0 60.0 14 min Parent ion 413 Daughter ion 369 %B 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 Dwell f sees) 02. Flow Rate (mL/min) 03 03 03 0.3 03 0.4 0.4 0.4 03 Coll Enerev feV) 10 Cone I 50 Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 A^ ' / All Hand-written Peak ID'S by: -i^\^ W "W. 3 Ete& AEbNtf&S^H^P. mTOJT5 FRoMT^E- SSs-ltM. r^bc^H 6 ^E'b to ?^, TQ\j6.?-\l^VALUESUSI^OU-iHtS t^ulG^tol RJZ032576 EID185050 Toning Method Report Method: C:\MASSLBCC\008-046.PRO\ACQODB\WA'rKR Printed: Fra. Hov 09 09;37;01 2001 Page I 4\\Wo\ Dau 413-00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture I Hexapole 2 Source Block Desolvation Temp. Temp. Pressuras Analyser Vacuum Gas Cell Set 3.00 50 0.0 0.0 0.0 100 300 Kdbk -2.93 -20 100 301 Edbk OFF 2.6e-3 Analyser LM Res I HM Res I lEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 lEnergy 2 Multiplier Gas Flows Cone Gas Desolnation Set Rdbk 10.5 10,5 1.0 -2 10 2 13.0 13.C 2.0 650 9 11 -644 Edbk 136.5 660.4 RJZ032577 EID185051 Scanning Method Hapor-b Method: last Modified: Ex-inted: C: \MftSSLT01X\ 008-04 6. PRO\ACQUDB\PFO& Mon Oct 15 12:37:26 2001 Eci Nov 09 09:41:26 2001 ^Wi Solvent Dalay ( mins ) ; 1.00 Elmction ; 1 MEM of I Mass Bair ( ESP- ) Inter Channel Delay ( Span ( Daltons ) : Start Time ( Mins ) : End Time ! Mins ) : Repeats : Channel Parent Sees ) : Daughter 0.03 0.00 0.00 8.00 1 Dwell (Sees) Coll Energy (eV) Cone ( V ) 1 413.00 369.00 0.20 10 50 Paga 1 RJZ032578 EID185052 Hathod Report Method Pile; Last Modified; Printed: C; \MASSI.THX\ 0 0 8 - 0 4 S . PRO\ACQOTB \water Friday, November 03. 2001 09:38:47 Friday, November 09, 2001 09:42;01 KP1100 LC Pump Initial Conditions Solvents At B Vt D% 60.0 40.0 0.0 0.0 Plow (inl/niin) Stop Time (mins) Win Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Rigbt(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 A BS C% Dt 0.00 60.0 40.0 0.0 0.0 0.40 60.0 40.0 0.0 0.0 1.00 10.0 90.0 0.0 0.0 '7.00 10.0 90.0 0.0 0.0 7-50 0.0 100-0 0-0 0.0 3.00 0.0 100.0 0.0 0.0 9.50 60.0 40.0 0.0 0.0 13.50 60.0 40.0 0.0 0.0 14.00 60.0 40.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 HP1100 IiC Pump External Event Timetable The Timetabia contains 4 entries which are : Time Initial 0.00 0.10 8.00 Column Switch Off Off Off Off Contacti Off On Off Off Contact2 Off Off On Off Contact3 Off Off Off Off Contact4 Off Off Off Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (pl/min) Draw Position (mm) Stop Time (mins) Injection Volume(^1) Vial Mmnber 200.0 200 0-10 14.00 15.0 6 Page 1 Pressure 400 400 400 400 400 400 400 400 400 RJZ032579 EID185053 Proven Results. In order to verify mass resolution, a calibration check is performed on the mass spectrometer using a NaI/Rb/Cs tuning solution. The tuning solution is infused onto the mass spec using an infusion pump set to a flow rate of 10 uL/min. An MS scan ftpm 80 to 1380 amu is perfbmed on both MS1 and MS2. TTie calibration is considered acceptable if the following 11 peaks are found within A 0.2 amu of then known masses on both MS1 and MS2: 84.9,132.9,172.8, 322.7,472.6,622.5,772.4,922.3,10722,1222.1 and 1372.0. If any of me masses are outside fhe 0.2 amu, then the instrument will be recalibrated and another calibration, check performed. The printouts from ttie calibration check can be found on the following 2 pages. ^MAi 58 Reseaith Drive ate Coflege,PA 16801, USA J: 814.272.1039 F: 814-231.1580 exyyn.oom RJZ032580 EID185054 l J rA;;w.,,j fc.-.. .^ i j 1.....4 ;.. ..j ' .j ', . < -/ j . i i " i ] i Calibration Check of NalRbCs090800 on MS1 using NalRbCs tuning solution tiM^^^lIlOp1 | 1 CALCHK091001-1 13 (0.811) Cn (Cen,2, 80.00, Ht); Sm (Mn, 2x2.00); Sb (1,40.00 ); Cm (1:16) y 100-, 172,8 "THIS IS AN EXACT TOEQRrGlNALDOC GiY----^----ftA- Exygen STUDY No 1 171 H 0 R 03 g " S g u M Vi <s 1-1 132.8 %- 322.8 472.7 84.9 / 180.8 / 232.9 67.0 / 340.8 Ll f 11I,,, , , ... i6o 234.8 / 382.9 | ,390.8 iiilln.ijiiL,,..,i,,,u,i ...j),i r, 260 36o 460 622.5 77 !-4 922^ 1'"07'--9 2- 532.7556.7 ^^A I . .l.l./.. '''"^b" 560 e6o S90.S.70S.6 " '866" 990.2 114 '"'96o ri 111 ii'l i"i i.', 1000 111,1111010l'l J V.n...^ t:., ..) (. . j -->,] t. .;..,) '. j !'--- '1 '""'i ' ; ) " -i ' 1. ; Calibr;ation Check of NalRbCs090800 o n MS2 using NalRbCs tuning solution CALCH K091001.2 9 (0.569) Gn (Cen,2, SO.OO, Ht); 8m (Mn, 2x2.00); Sb (1,40.00 ); Cm (1:17) 100 172.8 I^N)00i 1 ; 132.9 %- THIS (S AN EXACT THE ORIGINAL DOC BY. ^ DAT Exygen STUDY NO* ! PI H 0 H 03 S a ,1 u M (J1 00 i N , 92,0 y ^ 322.8 47 2,7 92.2.5 190,8 / -232.9 234.8 ( / 340:8 ^382.9 i JV f "^.e 0 440.8 690.5^06.5 'r'W "|"^"^..ii, li"i!^Ll,"i-ni,"nn".ir^r,l-"l- l".fl.-il r. i 11 i i i i i i i i i i i iI.1!!.'"1'1'!'"11''1!"1 ' " " 7 6 0 " " 10 o 260 s6o 460 560 eoo 77 2.4 B2 2.3 107^2,1 840.4,856.3 390.2 113 1| i i 11 800 fl 1'iir8l0i 0i i' '''"1'o'dd'11' !i i | i i 1100 i' Initial Calibration Curve Exygca Study No.: SctNo: Extraction Date Analyzed on: 008-046 101701A 10/17/01 10/19/01 The first curve of the data set ia used to determine perfbnnance. Alinearepessioii(withnovreightmE) is performed using the fust six standards of the analytical vm. The coefficient of <tetenninaft>a(R Square)must be 0.985 or greater. If Ihe set tails to meet this requirement, the ron must be (ejected and the samplesreanalyzed. ErygenID XCI01501-0 XC101501-1 XC101501-2 XC101501-3 XC101501-4 XC101501-5 Standard Concentration (ne/L) 0 50 100 250 500 1000 Peak Area 1552 42219 78392 172691 345627 652107 Coefficient of Determination: 0.99916321 SUMMARY oumn- Regression Statistics Multiple R 0.99958152 R Square 0.99916321 Adjusted R Squa: 0.99895402 Staadard Error Observations 7974.56702 6 \\^ ANOYA Regression Residual Total JL 1 4 5 ss us 3.03736E+H 3.04E+11 254374S76.7 63593719 3.0399E+11 F Hgmficance F 4776.1882 2.6265E-07 __________Coefficients Standard Error tStat Intercept 10229.6406 4406.260677 1321615 X Variable 1 648.005346 9J7643770S 69-10997 P-value Lower 95%. Upper 95%Lawer9S.<W Upper 95.0% 0.0809931 -20p4.l256 22463.4068 -2(104.1257 22463.4068 Z627E-07 621572127 674.038564 621.972127 674.038564 RJZ0325B3 EID185057 Quantify Calibration Report Study So.: 008-046, Set Ko: 1Q1701A, Bart.. Data: 1.0/17/01, Analyst: K Risha Page I Calibration: S : \Data\LCHSHS6\Ma3 alynxXO 08-04 6. I>RO\CirryeDB\1017 01A :Last modified: Eri. Oct 19 16:30:35 2001 Printad; Tri Oct 19 16:33:11 2001 M^ Exygen Kesearch RJZ032584 EID185058 Quantify Sample Report Study Ho.: 009-046, Sat No; 101701A, Ext. Date: 10/17/01, Analyst; K Risha Page 1 Sample List; P:\Data\K2'ISfclS6\Mas3lynx\008-046.PBO\SaaiipleDB\101701a Last aodi-fied.: Kci Oct 19 16:25:32 2001 Mathod: P:\Data\I.CMSl>IS6\Masslynx\008-OA5.PBO\MathDB\101601 EFOA last modified: Sri Oct 19 16:19:26 2001 Printed: Pri Oct 19 16:33:13 2001 g-rgrmsr Ruttf. To lot-TCi IfT^PQ Name: 101701A-101 2ext: 1: PFOA s" Exygen Research RJZ032585 EID185059 Quantify Sample Report Study Ho.: 008-046, Sat Ho: 101701&, Bxt. Date; 10/17/01, Analyst: K Risha Sample Id-st; last modified: Method; Last modified: Job Code: P:\Data\LaiSyS6\Maaslyrix\008-OA6.ERO\SaiiipleDB\10170la Fri Oct 19 16:25:32 2001 Pi\Data\LCMSMS6\tto3slynx\008-046.BRO\MathDB\l01601 PFOA Fri Oct 19 16:19:26 2001 Printed; Fri Oct 19 16:33:13 2001 Page 2 Hama: 101701A-102 Text: 1: PFOA |XC101501-1, 50 ppt Standard 101701A-102 Sm (Mn, 2x2) 10(h 19-0ct-2001 07:45:38 LC/MS/MS #6 MRM of 1 Channel ES- 5.12 413 > 369 3.20e5 1.00 2.00 3.00 4.00 5.00 6.00 7.00 Time 8.00 Exygen Rasearch RJZ032586 EID185060 Quantify Sample Report Study No.: 008-046, Set Ho; 101701A, Ext. Date: 10/17/01, Analyst: K Risha Sample list: Last modified: Method: Last modified: Job Code: E:\Data\IQlSMS6\Ma3slynx\008-04S.BKO\SaBDleDB\10170la Vsi Oct 19 16:25:32 2001 P:\Data\].CMSMS6\Ma3slynx\008-046.ERO\MethDB\101601 PFOA EriL Oct 19 16:19:26 2001 Printed; Eri. Oct 19 15:33:13 2001. Page 3 Hame: 101701A-103 text: 1: PFOA [XC101501-2,10ft p.j3t Standard 101701A-103 Sm (Mn, 2x2) 100^ _1_&-0ct-2001 08:01:17 LC/MS/MS #6 MRM of 1 Channel ES- 5.11 413 > 369 5.97e5 -i-^ Time 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Basearch RJZ032587 EID185061 Quantify Sample Report Study Ho.: 008-046, Set No: 101701A, Ext. Data: 10/17/01, Analyst: K Risha Sampla Iiist; Last modified: Method; Last modified: Job Code: P: \Data\LCMSyS6\tfeLaslynx\OOa-046. ERO\SaaiipleDB\101701a fri Oct 19 16:25:32 2001 P; \Data\:LCMSMS6\Ma.sslYDX\008-046 .PEO\MBthnB\l01601 PFOA Eri Oct 19 16:19:26 2001 Printed: Kci Oct 19 16:33:13 2001 Page 4 Hame: 101701A-104 Text: 1: PFOA XC1C31501-3,250 ppt Standard 1017C31A-1048m(Mn,2x2) 100-1 . ,,,- 19-0ct-2001 08:17:02 - - LG/MS/IVIS #6 MRM of I Channel ES413 > 369 1.34e6 %- 0- ' ' i ' 1 i ' ' ' 1 ' ' ' ' | ' ' ' ' 1 ' i ' 1 ' ' i i P' 1 ' i 1 i i ' i | '' ' ' ' 1 ' ' ''' ' ' ' < 1 ' i 1 i i ' ' 1 ' ' 1 ' ' ' 1 ' ' ' 1 >mns 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research RJZ032588 EID185062 Quantify Sample Report Study Ho.: 008-045, Sat Ho: 101701A, Ext. Date: 10/17/01, Analyst: K Kisba Sample List; Last modified: Method; last aodified: Job Code: E.t\Data\LCMSMS6^Iaa3l-yruc\008-046.P&0\SaaipleDB\101701a Eri Ocfe 19 16:25:32 2001 B:\Data\LCMSl'136\Ma3si-ynx\008-046.PBO\MethDB\101601 PTOA Fri Oct 19 16:19:26 2001 Erintad; Exi Oct 19 16:33:13 2001 Page 5 Hama: 101701A-105 Text: 1: PFOA XC101501-4, 500 ppt Standard 101701A-105 Sm (Mn;2x2) 10(h 19-0ct-2001 08:32:38 LC/MS/MS#6 MRM of 1 Channel ES- 5.10 413 > 369 2.71e6 )''''1.0i0'''' i''''2.0i'0'' i 3.00 4.00 5.00 6.00 7.00 -r-r-i Time 8.00 Exygen Research RJZ0325B9 EID185063 Quantify Sample Baport Study Ho.: 008-046, Set o: 101701A, Ext. Data: 10/17/01, Analyst: K Risha. Sattpla last: Last modified; Method: last modified: Job Coda; P:\Data\LCMSMS6\Masslynx\008-046.PRO\SaiapleDB\101701a I-ri Oct 19 16:23:32 2001 B:\Data\LCMSMS6\MaS3lyuc\008-046.EEO\MethDB\l01601 EFOA Eri Get 19 16:19:26 2001 Printed: Bri Ocfe 19 16:33:13 2001 Page 6 Mame: 101701A-106 2ext: 1: PFOA |XC101.501-5,100.0 ppt Standard. 101701A-106 Sn-i (Mn, 2x2) 10(h 19-0ct.2001 08:48:21 LC/MS/MS #6 MRM of 1 Channel ES- 5.09 413 > 369 5.09e6 i''' 0 'i 11' > 11' i' i' 111-111) 1111 p 111111 11 i'' 111' ' ^^TI i 11 > 1111 ^ 111111.111111111 Time ______UK)__ 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research RJZ032590 EID185064 Quantify Sample Ropoct Stady Ho.: OOB-04S, Set Mo: 101701A, Ext. Date: 10/17/01, Analyst: K Eisha Sample lASt: last modified: Method; lA3t modified: Job Code: B:\Data\XMSMS6\l>&S3lyiue\008-046.PRO\SaBipleDB\10l701a Eri Oct 19 16:25;32 2001 P:\Data\tCMSHS6\Maaslynx\008-046.PRO\MQthDB\101601 PEDA Eri Oct 19 16:19:26 2001 Printed: Eri Oct 19 16:33:13 2001 Page 7 Mane: 101701A-107 Text: 1: PFOA XC1C31501-6,250ppt<Check Stan dard 1017(D1A-107Sm(Mn,2x;2) 100-1 %- 0- 111'' ' >'''' >' i P-"i 1.00 2.00 3.00 4.00 I5.10 5.00 6.00 19-Oct-2001 09: 04: 00 LC;/MS/MS #6 MRMcof1 Chann elE?S- 413 >369 1.19 e6 7.00 ' '' Tim e '8.130 Exygen Research RJZ032591 EID185065 Quantify Sancpla Report Study o.: 008-04S, Sal: Ho: 101701A, Ext. Data: 10/17/01, Analyst: K Risha Sample List: I^st modified: Method: Iiast modified: Job Code: P:\Data\UMSMSS\Maaslyiut\008-046.ERO\SaaplaDB\l01701a Fri Oct 19 16:25;32 2001 P;\Data\LCMSHSS\te33lynx\OOa-046.EEO\MQthDB\101601 PFOA Eci Oct 19 16:19:26 2001 Printed: Fri Oct 19 16:33;13 2001 Hane: 101701A-108Text: 1: PFOA Page 8 Exygon Reseacch RJZ032592 EID185066 Quantify Sample Report Study Mo.: 008-046, Sat So: 101701A, Ext. Data: 10/17/01, Analyst: K Bisha Sample List: :Last modified: Method: last modified; Job Code: P:\Data\I,OISys6\ttesslymc\008-046.ERO\Sa3l(pleDB\101701a Tri Oct 19 16s25;32 2001 P:\Data\I.a'lSMS6\t!&sslyii)C\OOa-046.PRO\l'tetbDB\101601 EEOA Fri Oct 19 16:19:26 2001 rrinted: Fri Oct 19 16:33:13 2001 Page 9 Hame: 101701A-109 Text; 1; PFOA 0106020 Control 101701A-109 Sm (Mn. 2x2) 10(h 19-0ct-2001 09:35:23 LC/MS/MSSq MRM of 1 Channel ES-! 413>369| fAl A2.18e4; Time 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 7" Exygen Research RJZ032593 EID185067 Quantify Sample Report Study Ho.; 009-046, Set Mo: 101701A, Ext. Dato: 10/17/01, Analyst: K Risha Sample list: Last modified: Method: last modified: Job Code: P:\Data\I,CMSMS6\tfasslynx\008-04S.PBO\SampleDB\101701a Rci Oct 19 16:25:32 2001 P:\Data\LCMSMS6\Masslynx\008-046.PBD\MathDB\101S01 PJFOA Tvi Ocfc 19 16:19:26 2001 Printed: Fri Oct 19 16:33:13 2001 Page 10 Hame: 101701A-110 Text: 1: PFOA 0108020 Spk A, 50 ppt 1017C31A-110Sm(Mn,2x2) 10Ch 19-0ct-2001 09:51:10 LC/MS/WIS #6 MRM of 1 Channel ES- 0. 413 > 369 3.03e5 %- /V 0- ' '' r'l-r-rT-r-rTrTi-i-rr i l | 1 1 l l | l l l l [ l , . 1 |-i , , . | . . . . | .1 r . l , . . i . [ l l i . | l-.-. . | . l i . | , i . i |l-.-. -r| |BHt( 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 ? a, Exygen Research RJZ032594 EID185068 Quantify Sample Raport Study No.: 008-046, Set No; 101701A, Ext. Date: 10/17/01, Analyst; K Risha Sample List; last modified: tfetbod: last modifi-ed: Job Code; P:\Data\LaISMS6\Massl:yTO\OOB-046.PRO\SaiirpleDB\10170la. Fri Oct 19 16:25:32 2001 P:\Data\LCMSHS6\Ma3slynx\008-046.ER.O\MQthDB\10l601 PE-OA i-ri Oct 19 16:19:26 2001 Printed: Pri Oet 19 16:33:13 2001 Paga 11 name! 101701A-111 Text: 1; PFOA 0106 020 Spk B, 50)0ppt 1017(01A-11-tSm(Mn ,2x2) 100-1 19-0ct-2001 10:06:57' LC;/MS/MS #6 MRM of 1 Channel ES- 5.11 413 > 369 2.25e6 %- '''' . 0- i' '' t '' . i. i >. i. 11 1.00 2.00 3.00 ' i ' ' ' ' ' 4 . 0i0' ' ' ' i 5.00 i'' i'' ' i' ' '' i 6.00 ' i ii --r--iTime 7.00 8.00 a Bxygen Research RJZ032595 EID185069 Quantify Sample Report Study Ho-; 008-046, Set No; 101701A, Ext. Date: 10/17/01, Analyst: K Risha Sample lAat: Last modified; Method: last modified; Job Code; P:\Data\LCMaiS6\Masslyox\OOB-046.PRO\SampleDB\lonola Rci Oet 19 16;25:32 2001 P:\Data\LCMSMS6\tfa3slynjc\OOB-04S.ERO\MethDB\101601 PFOA Eei Oct 19 16:19:26 2001 Printed: Eci Oct 19 16:33:13 2001 Page 12 Same; 101'701A-112 Text: 1: PFOA 0112719 Spk C, 500 ppt, DF=2 101701A-1125m(Mn,2x2) 10(h 19-0ct-2001 10:22:37 LC/MS/MS #6| MRM of 1 Channel ES- 5.09 413 > 369 2-12e6 jTime 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Raseaech RJZ032596 EID185070 Quantify Sample Report Study Ho.: 009-046, Set No: 101701A, Ext. Date; 10/17/01, Analyst: K Bisha Sample Hat: last modified: Method: Last modified: Job Code: P:\Data\:LQlSyS6\^3SlYnx\008-046.:reO\SampleDB\101701a. fri Ont 19 15:25:32 2001 Ps\&ata\l.QffiHS6\Mas3lYn3c\008-046.PRO\MethDB\101601 PFOA. Rci Oct 19 16:19:26 2001 Printed: Fri Ont 19 16:33;13 2001 Page 13 Nae: 101701A-113 Text: i: proa 0112719SpkC,500ppt 1017CD1A-113 Sm (Mn, 2X2) 100-i 19-0ct-2001 10:38:29 LC/MS/MS #6 MRM of 1 Channel ES- 0, 413 > 369 3.91e6 %- 0- i 1 '' 111 '1 1'' " 1.00 i '' ''"i' '' 2.00 ' i' ' ' f''''' 3.00 i' ' '4' .0i '0' ' ' i' '' IJ ^ 5.0C) 11111111111111 111' 11) i 111 Time 6.00 7.00 8.00 s- - Exygen Research RJZ032597 EID185071 Quantify Sample Haport Study Ho.: 008-046, Set No: 1D1701A, Ext. Date: 10/17/01, Analyst: K Risha Sample .List; last modified: Method: last modified: Job Code: P:\Data\LCMSMS6\MasslyBX\OOB-046.BRO\SainpleDB\101701a Fri. Oct 19 16:25:32 2001 P:\Data\I^MSMSe\Masslynx\008-046.ERO\HethDB\101601 PPOA Fri Oct 19 16:19:26 2001 Printed.: Eri. Ocst 19 16:33:13 2001 Page 14 Name: 101701A-114 Text: Ir PFOA XC1C)1501-1,50 ppt Standard 1017C31A-114Sm(Mn.2x2) 100-1 19-0ct-2001 10:54:12 LC/MS/MS #6 MRM of I Channel ES- 5.C 413>369 2.79e5 %- 0- 11111' ''' i' 11' i'11 11' 11 11'" i [l\i 111 > i'' '' i''''' r ''' 1'''' >' ''' 1'' '' i'' '' >''''1 nine 1.00 2.00 3-00 4.00 5.00 6.00 7.00 8.00 Exygen Research RJZ032598 EID185072 Quantify Sample Report Study Ho.; 008-046, Sat Ho: 101701A, Bxt. Data: 10/17/01, Analyst: K Risha Sample List: Last modified; Method: Last modified; Job Code: P:\Data\:LCMSMS6\Masslynx\OOB-046.PRO\SanpleDB\101701a Fri Ocfe 19 16:25:32 2001 P:\Data\I01SMS6\ttei3Slynx\008-046.E'HO\ltethDB\101601 PTOA Fr-i Oet 19 15:19:26 2001 Printed: Rci Ocfc 19 16:33:13 2001 Page 15 Haxoa; 101701A-115 fext: I: PFOA 0112720 Spk D, 500 ppt, DF=2 101701A-115 Sm(Mn, 2x2) 10(h 19-0ct-2001 11:09:54| LC/MS/MS #6| MRM of 1 Channel ES- 5.10 413>369 2.26e6 111'''' r' -n-T-i iTime 1.00 ^.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Roseaxcli RJZ032599 EID185073 Quantify Sampla Report Study Ho.: 008-046, Set Mo; 101701A, Ext- Date: 10/17/01, Analyst: K Kisha Sample lAst: Last modified: Method: Last-modifiad: Job Code: P:\Data\I>aaSMS6\Ma33lyox\008-046.RO\SaiapleDB\101701a ITi Oct 1,9 16:25:32 2001 P:\Data\LOrfSMS6\t^alynx\008-046.PRO\tfefhDB\10160l PFOA Pri Oct 19 16:19:26 2001 Printed; Fri Oct 19 16:33:13 2001 Page 16 llama: 10n01A-116 Text: 1: PPOA 0112720 Spk__D_, _SO_O ppt 1017(!)1A-116Sm(Mn,2x2) 10(h 19-0ct-2001 11:25:36 LC/MS/MS m MRM of 1 Channel ES- 0. 413 > 369 4.38e6 %- 1.00 2.00 3.00 '' 4.00 5.i00 0- 1 ' 1 11 ' 1 1 1 1 ' 1 1 ' > ' 1 ' 1 ' 1 1 1 1 ' I'l ' 1''' ' ' 1 ' ' ' ' 1 ' ' ' ' "' 1 ' ' ' ' 1 '' 7.00 6.00 ' ' 1 ' ' ' ' 1 ' ' ' ' 1' ' ' ' 1 11IIC 8.00 Exygen Resea-rch RJZ032600 EID185074 Qaaa.tS.Ey Sanpio Report Study Ho-: 008-046, Set Mo: 101701A, Ext. Data: 10/17/01, Analyst; K Risha Sample lAst: last modified: Method: I,ast nodified: Job Code: Pi\Data\I>aaSMS6\Massl-ynx\008-046.ERO\SaapleDB\10170la Fri Oct 19 16:25;32 2001 P:\Data\I,CMSMS6\Masslynx\008-046.ERO\MaaiDB\10160l PE-OA Fri Oct 19 16:19:26 2001 Printed: Fri Oct 19 16:33:13 2001 Page 17 Hams: 101701A-117 Text: 1; PFOA 0112721 Spk E, 500 ppt, DF=2 101701A-117 Sm (Mn, 2x2) I 100^ 19-0ct-2001 11:41:13 LC/MS/MS #6| MRM of 1 Channel ES- 5.13 413 > 369 2-27e6 % ' 1.00 2.00 i" ' P" " i' ' ' " i 3.00 4.00 5.00 ' 6.00 7.00 i'' i Time 8.00 ~ Exygen Reseaxch RJZ032601 EID185075 Quantify Sample Report Study Ho. : 008-046, Set Ho: 101701A, Bart. Data; 10/17/01, Analyst; K Riaha Saaple List: X-ast modified: Method: Last modified; Job Code: P:\Data\LCMSMS6\Masslynx\008-046.ERO\SaapleDB\10l701a Fri Oct 19 16; 25:32 2001 P:\Data\LCMSMS6\Masslynx\OOe-046.PEO\MethDB\101601 OTOA B-ri Oct 19 16:19:26 2001 Printed; Fri Oct 19 16:33:13 2001 Page 18 Haaa: 101701A-11B Text: 1: PE-OA 0112721 Sp_k _E_, 5.0_0 ppt 1017 01A-118Sm(Mn,2x2) lOO-i 19-0ct-2001 11:57:04 LC/MS/MS #6 MRM of 1 Channel ES- Oi 413>369 4.80e6 %- i''' i''' 0- ' 11' ' 11' '' 11' i i' i' 1111 r i '' i' ' i' '' i' '' i* i"i' 1'' i '' 1.00 2-00 3.00 4.00 5.00 6.00 i;' 7.00 " i nine 8.00 ,. Exygen Research RJZ032602 EID185076 Quantify Sample Rapor-fc Study Ho.; 009-046, Set Ho: 101701A, Ext. Date; 10/17/01, Analyst; K Ei.eha Sample list.: Last nodified: Method: Last Modified: Job Coda: P:\Data\I<MSMS6\tfasslymc\008-046.EEU3\3aiiipleDB\101701a Fri Oct 19 16:25:32 2001 P:\Data\ICMSMS6\Masslynx\008-Oa6.ERO\MathDB\101601 PE-OA Pri Oct 19 16:19:26 2001 Feinted; Fri Oct 19 16:33:13 2001 Paga 19 Hame: 101701A--L19 Text: 1; PFOA . 0112722 Spk F, 500 ppt, DF=2 I101701A-119 Sm (Mn, 2x2) 10(h 19-0ct-2001 12:12:51) LCfMS/Ms sq MRM of 1 Channel ES-i "5.13 413 > 369] 2.40e6l 0 (. ' i 11 i . 111 i. 111.11.. i . 1-1'' ' i' i " i " ' ' i^"" i " '' 1 " " 1'' ' 1' ' ' ' ' TI"'6 1.00 2.00 3-00 4.00 5.00____6.00____7.00____8.00 Exygen Research RJZ032603 EID185077 Quan-tify Sample Report Steady No-; 008-046, Sat No; 101701A, Ext. Data: 10/17/01, Analyst: K Risha Sample Li3t; Last aodified: fcfethod: last modified: .Tob Code: P:\Data\LCMSMS6\Ma33lynx\008-046.PRO\SampleDB\101701a Fti Oct 19 16:25:32 2001 P:\DataVLCMSMS6\Masslyn3C\ 008-046. PBO\MBthDB\101601 PFOA E^i Oct 19 16;19:26 2001 Printed: Tsi Oct 19 16:33:13 2001 Page 20 Hane; 101701A-120 Text: 1; PFO& 0112722 SpkF, 500 ppt 101701A-120 Sm (Mn, 2x2) 100^ 19-0ct-2001 12:28:43 LC/MS/MS #6 MRM of 1 Channel ES- 5.14 413 > 369 4.87e6 n i U I 1I I I I 1.00 2.00 3.00 4.00 7.00 -t-nTime 8.00 Exygen Research RJZ032604 EID185078 ~1 1 Quantify Sample Repoxt Page 21 Study No.: 008-046, Sat No: 101701A, Ext. Data: 10/17/01, Analyst: K Risha Sample Liat.: Last modified; Mathod: Last Modified: Job Coda: P:\Data\ICMSMS6\Ma33lynx\OOa-046.ERO\SamplBDB\10l701a Fri Oct 19 16:25;32 2001 P:\Data\IK31SMS6\Ma33lynx\OOB-046.ERO\MethDB\101601 PFOA Fri Oct 19 16;19;26 2001 Printed: Fri Ocfe 19 16;33;13 2001 Naaa: 101701A-121 Tax-ti 1; PFOA XC101501-2,100 ppt Standard 1017 01A-121Sm(Mn.2x2) 10Ch 19-0ct-2001 12:44:21 LC/MS/MS #6 MRM of 1 Channel ES- 5-' 413 > 369 5.96e5 %- rr 0- yr-r i r ri i I-}-T i i [--'- r I-' r i i-j i i i i ^i^l i -1 ) i 1.00 2.00 3.00 l-p"T"i'T|' 1 r~i'~i~^i^I-i j i^i-T-i^-T^r) i-n-i r | i T-T" ) i T-T i ) lIfllU 4.00 5.00 6.00 7.00 8.00 1J a g D 1 Exygen Eesearch ;'-^i RJZ032605 EID185079 Quantify Sample Report Study Mo,: 008-046, Sat No; 101701A, Ext. Data! 10/17/01, Analyst: K Risha Sample lAat: Last Modified: Method: Last modifisd; Job Code: P:\Data\LCMSMS6\Ma3Slynx\OOB-046.ERO\SampieDB\101701a Fri Oct 19 16:25:32 2001 P:\DataVLCMSMS6\Masslynx\OOB-046.PEb\MathDB\101601 PFOA E'ra. Oct 19 16:19:26 2001 Printed: Fri Oct 19 16:33:13 2001 Sage 22 Haae; 101701A-122 Text; 1; PFOA 0112719 101701A-122Sm(Mn,2x2) 100-1 19-0ct-2001 13;00:0ffl LC/MS/MS #6| MRM of 1 Channel ES-1 5.15 413 > 369 2.51e6 1.00 2.00 3.00 4.00 5.00 11 n 111111111111... 11 Time 6.00 7.00 8.00 Exygen Rasea-cch RJZ032606 EID185080 Quantify Sample Report Study Ho.: 008-046, Set Ho: 101701A, Ext. Date: 10/17/01, Analyst: K Risha Sample List: Last modified; Mathodt r.a3t modified: Job Code: P:\Data\I,CMSMS6\tfa3sly[uc\OOe-046.PRO\SaiiipleDB\10l701a Fei Oct 19 16:25:32 2001 P;\Data\ICMSMS6\lfaa3lyiix\OOB-046.BRO\MethDB\10l601 PTOA Fri Oct 19 15:1:9:26 2001 Printed: Fri. Oct 19 16:33;13 2001 Pago 23 name: 101701A-123 react: 1: PFOA 0112719 Dup 1101701A-S1m23(Mn, 2x2) 10(h 19-0ct-2001 13:15:40 LC/MS/MS #6 MRM of 1 Channel ES- 5.15 413 > 369! 2.27e6| a 1.00 2.00 3.00 4.00 5.00 6.00 7.00 i=j Time 8.00 11 y Exygen Research RJZ032607 EID185081 J Quantify Sample Report Study Ho.; 008-046, Set Ho: 101701A, Exfc. Data; 10/17/01, Analyst; K Bxsha Sample I-ist: last modified: Mathod: last modified; Job Code; P;\Data\LCMSMS6\Mas3lynx\008-046.PRO\Sa)apleDB\101701a Tri Oct 19 16:25:32 2001 P:\Data\LCMSMS6\Ma33lynx\008-046-l?RO\ltethDB\10l601 PrOA Fri Oct 19 16:19:26 2001 Printed: Fri Oct 19 16:33:13 2001 Paga 24 Hame; 101701A-124 rext; 1; PFOA 0112720 101701A-124 Sm (Mn, 2x2) 10(h 19-0ct-2001 13:31:2^ LC/MS/MS #6| MRM of 1 Channel ES- 5.15 413 > 369 2.39e6 :1 1.00 2.00 3.00 4.00 5.00 6.00 111111 ^ ' 11 Time 7.00 8.00 a Exygen Research RJZ032608 EID185082 <2uantiy Sample Rapor-t Study No.: 008-046, Set No: 101701A, Ext. Data: 10/17/01, Analyst: K Riaha Sanpla List: I.ast modified: Mathod: Last modified: Job Coda: P:\Data\I>CMSMS6\Ma3slynx\008-046.ERO\Sa.BpleDB\101701a .FBI Oct 19 16:25;32 2001 P:\Data\lCMSMS6\MasBlynx\008-046.PRO\fctBaiDB\101601 PFOA Fri Oct 19 16:19:25 2001 Printed: E'ci Oct 19. 16:33:13 2001 paga 25 Haae: 101701A-125 Text: 1; PFOA m 12720 Dup 101701A-125 Sm (Mn, 2x2) 10Ch 19.0ct-20Q1 13:47:10 LC/MS/M8 #6 MRM of 1 Channel ES- 5.15 413 > 369 2.23e6 1.00 2.00 -ri 3.00 4.00 5.00 6.00 7.00 ''=) Time 8.00 Exygen Research RJZ032609 EID185083 Quantify Sample Report Study Ho.; 008-046, Set No; 101701A, Ext. Data: 10/17/01, Analyst; K Risha Sample List; last modified: Mathod; last modified: Job Code: P:\Data\I,CMSMS6\lfasalynx\008-046.PRO\SampleDB\101701a Bri. Oct 19 16; 25:32 2001 P:\DataVLCMSMS6\Masalyn3c\008-046.ERO\M6thDB\101601 PFOA Ssi Oct 19 16; 19:26 2001 Printed: Fri. Oct 19 16:33:13 2001 Page 26 Name; 101701A-12S Text.; 1: PE-OA 0112721 101701A-126 Sm (Mn, 2x2) 10(h 19-0ct-200l 14;03:05 LC/MS/MS #6 MRM of 1 Channel ES- 5.15 413>369 2.45e6l 111111...11 Time 1.00 2.00 3.00 4.00 5.00 6.00 7.00 B.QQ Exygen Research RJZ032610 EID185084 1 Quantify Sample Raport Study Ho.: 008-046, Sat No: 101701A, Ext. Date: 10/17/01, Analyst; K Risha Sangpla List; P;\Data\lCMSMS6\Mas3lynx\008-046.PIU3\Sa3iipleDB\10noia Last modified: Pri Oct 19 16:25:32 2001 Hethod: Pi\Data\LCMSyS6\Ma33lynx\008-046.PRO\MathDB\101601 PFOA I Last modified: Fri Oct 19 16:19:26 2001 Job Code: Printad; Eci Oct 19 16;33:13 2001 Eaga 27 Haina: 101701A-127 'Eext; i;: proa 0112721 Dup 101701A-127 Sm (Mn. 2X2) 10Ch 19-0ct-2001 14:18:49 LC/MS/MS#6 MRM of 1 Channel ES- 5.16 413>369 2.29e6 1.00 2.00 3.00 4.00 5.00 y nTime 8.00 1 Exygen Research d RJZ032611 EID185085 ~1 Quantify Sample Report Study-No.; 008-046, Sot No; 101701A, Ext. Date; 10/17/01, Analyst; K Risha Page 28 Saaple Id-at; P:\Data\lCMSMS6\Ma33lyTOC\008-046.ETO\SampleDB\.10170la Last modified: Fri Ctet 19 16:25:32 2001 Method; P:\DatAlCMSMS6\Masslynx\008-046.PR.O\ttethDB\101601 PTQA. I^st nodified; rri Oct 19 1S:19;26 2001 '] Job Codoa: Printed: Fri Oct 19 16;33:13 2001 '1 Haaos 101701A-128. Text: 1: PFOA XC101501-^, 250 ppt Standard 1017C01A-128 Sm (Mn, 2x2) 100-j 19-0ct-2001 14:34:39 LC/MS/MS #6 MRM of 1 Channel ES- Ot! 413 > 369 1.35e6 %- 0- 1.00 2.00 3.00 4-00 5-00 6.00 7.00 8.00 Exygen Research RJZ032612 EID185086 ^ ~1 1 -1 1 3 Quantify Sanpla Report Study Ho.; 008--046, Set Mo: 101701A, Ext. Date: 10/17/01, Analyst: K Bisha Sample list: teat modified; Method: last modifiod: Job Coda: P:\Data\LCMSMS6\Maa3lymc\008-046.PKO\SaaipleDB\l01701a Frx Oct 19 16:25:32 2001 Ps\Data\IiCMSM36\Mas3lynx\009-046.ERO\ttethDB\101601 PFOA Fri Oct 19 16;19;26 2001 Printed: Fri Oct 19 16:33:13 2001 Pago 29 Nane: 101701A-129 Teoct: 1: PFOA 0112722 1017C31A-129 Sm (Mn, 2x2) 10(h 19-0ct-2001 14:50:22 LC/MS/MS ^6 MRM of 1 Channel ES- |5.15 413 > 369 2.18e6 n %ii 0- 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Q Exygen Research RJZ032613 EID185087 " "1 Quantify Sample Report Page 30 Study No.: 008-046, Set Mo: 101701A, Ext. Data: 10/17/01, Analyst: K Riaba Sample List: P:\Data\LCMSMS6\Mas3lyroc\008-046.ERO\SampleDB\101701a last modified: Fri. Oct 19 l6i25:32 2001 Method: Pi\Data\I.CMSM36\Ma33lyr>x\008-046.SRO\MethDB\101601 PfOA I^st Modified: Rci Oct 19 16!l9;26 2001 "5. Job Code: Printed: fri Oct 19 16t33:13 2001 -"1 Name: 101701A-130 Text: 1: PFOA 0112722 Dup 101701A-130Sm(Mn,2x2) 1 10(h 19-0ct-2001 15:06:07 LC/MS/MS #^ MRM of 1 Channel ES- 5.15 413 > 369 2;25e6 ;1 % 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00__ n 3.- Exygen Research RJZ032614 EID185088 ~^ Quantify Sample Report Page 31 Study No.: 008-046, Sat No; 101701A, Ext. Data: 10/17/01, Analyst: K Risha Sample List: Last modified: Method: laat modified: Job Coda: P;\Data\IMSMS6\Ma33lyiuc\OOB-046.PRO\SampleDB\lOn01a B-rx Ocb 19 16:25; 32 2001 P;\Data\IiCMSl!lS6\Ma33lynx\ 008-04 6. PRO\HethDB\101601 PFOA Fri Oot 19 16:19:26 2001 Printed; B-ri Oct 19 16:33:13 2001 Nane: 101701A-131 Text: 1: PFOA 1 0 n Exygen Research RJZ032615 EID185089 ~ -9 Quantify Sample Raport Page 32 Study Ho,: 008-046, Set Ho: 101701A, Ext. Data: 10/17/01, Analyst: K Kisha Sampla Iiist: Last Bodified: Method; Last Modified; Job Coda; P:\Data\I.CMSMS6\Mas3lyox\008-046.EKO\SanipleDB\101701a Fri Oct 19 16:25;32 2001 P:\Data\I,CMa^6\Ma33lynx\008-046.PRO\ltethDB\101601 PFOA Fri Oct 19 16:19:26 2001 Printed; Fri Oct 19 16:33:13 2001 Haixe: 101701A-132 Text; 1: PE-OA 0112724 1 101701A-132 Sm(Mn, 2x2) W-t '1 .?1 1 19-0ct-2001 15:37:29 LC/MS/MS #6| MRM of 1 Channel ES413 > 369 A 1-47e4 Time 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 n Bxygen Research V..I RJZ032616 EID185090 Quantify Sample Report Study Ho.: 008-046, Set tta: 101701A, Ext. Date: 10/17/01, Analyst: K Risha Sample List; Last modified: Msthod: Last Modified: Job Coda: P:\Data\I>CMSMS6\Masslynx\OOa-046.PRO\Sainpl6DB\lOnoia E'ri Oct 19 16:25:32 2001 P!\Data\LCMSHS6\Ma3alYnx\008--046.PRO\MethDB\101601 PFOA Fri Oct 19 1S:19:26 2001 Printed: B-ri. Oct 19 16:33:13 2001 Page 33 Haae: 101701A-133 Text: 1: PFOA XC101501-4,500 ppt Standard 1017(01A-133Sm(Mn,2x2) 1(Xh 19-0ct-2001 15:53:18 LC/MS/MS #6 MRM of 1 Channel ES- 0.' 413 > 369 2.81 e6 %- 0- 111' t ' ' 1 . i 0 0 ' ' ' i''''2.0> 0''' i'''3' .0r0'' '' i ' ' '4' .0i0' ' ' ' i''''5.010'^' '~i ''6' .0i0'''' i''''7.0> 0i''' i " i iiiiic 8.00 Exygen Research RJZ032617 EID185091 -^ Quantify Sanpla Report Study-No.: 008-046, Set Ho: 101701A, Ext. Date: 10/17/01, Analyst: K Risha Page 34 Sample Iiiat: Pt\nata\I,CMSMS6\bfa3slyiuc\008-046.PRO\SaiBpleDB\10170la 'Last modified: Fri Oct 19 16:25:32 2001 Method: P:\Da.ta\I.CMSMS6\Maaslynx\008-046.PRO\MethDB\101601 PFOA Iiasfc modified: Fci Ocfc 19 16:19:26 2001 "I Job Coda; Printed: Fri Oct 19 16:33:13 2001 Hana: 101701A-134 Text: 1: PFOA XC10M501-5,1000 ppt Standard 1 1017C31A-134 Sm (Mn, 2x2) 100-1 19-0ct-2001 16:09:06 LC/MS/MS #6 MRM of 1 Channel ES- 5.1 413 > 369 5.40e6 %- iiiii 0- > 11111 i.,.,c., ri i i-i 11. r'-'-'-i 1.00 2.00 i-ri-i-i-i-'-T-'-rr' 111111 i i'^"' 1111 11111 1 11 111 (i 11 1111111 i nuts 3.00 4.00 5.00 6.00 7.00 8.00 y 1 n Exygen Kesearch >.j RJZ032618 EID185092 Sponsor Study Noel1A. Exygcn Study No: ()0g-046 AaaSytK tons Monitored: ^UTO <113-> 369 Site: 1>rA RAW DATA REPORT Limit of Quantilation: Ini'ection Volume: Matrix: Sample Volume: Final Volume: 50ag/L 15 uL Water 40.0 niL 5.0 mL 4Set Ho: i oatyA- }tetninioitlypc Jattraction D'ate: Janalyzed on 101701B Kajcn Rishii LOMS/MS Unit #7 10/17/01 10/18/01 Amount Std. PFOA APFO PFOA Exygcn ID XC101501-0 Sponsor ID Sample Cone CS Rim No. 101701B-201 Cone. (ngfl.) 0 Dilulioa Factor Peak Area ND Found W Found ("S^ - Added (og/L) Recovery (%) - XC10150M CS 101701B-2C2 50 2269 - - - . XC101501-2 CS 101701B-203 100 4485 - - - . XC101501-3 CS 101701B-204 250 975? - - - - XC101501-4 CS 101701B-205 500 206S2 - - - - XC101501-5 ~? XC101501-6 CS 101701B-206 lOOtt 40S77 - - - - CK 101701B.207 250 9594 - - - - MctnanolWasa C 10170IB-208 ND - - - - 0106020 Control NA C 101701B-209 - 1 ND ND ND - - -^ 0106020 Spk A NA LCS 101701B-210 - 1 1896 42.5 44-2 50 85 0106020 SpkB MA LCS 101701B-2U - ! 19553 506 526 500 101 0112725 SpfcC WWK-D-BMg-293 LF 101701B-213 - 1 35585 926 964 500 104 0112726 SpkD WWR-n-Lubedc-Office LF 101701B-214 - 2 20859 1080 1120 500 97 XC101501-1 CS 101701B-216. 50 2212 - . - - 0112727 SpkE WWK-G-LPWD-Wdl-F LF I0170IB-218 - 1 27533 715 744 500 88 0112728 SpkF WWK-G-LPWD-WeB-A LF 101701B-219 - 2 21348 1110 1150 500 87 0112729 SpkG WWK-G-LPWD-Well-B LF 101701B-222 - 1 37615 979 1020 500 84 XC101501-2 CS I01701B-223 100 3863 - - - - 0112725 WWK-D-Bldg-293 S 101701B-224 - t 15758 406 423 - - 0112725 Dup WWK-D-Blae-293 S 101701B-225 - 1 14574 375 390 - - 0112726 WWK-D-Lubecfc-Ofifce S 10170IB-226 - 1 23022 597 621 - - 011272$ Dup. WWK-D-Lubedc-Oflice S 101701B-227 - 1 22433 581 605 - - 0112727 WWK-G-LPWD-WeB-F S 101701B-222 - 1 10&23 277 1SS - - 0112727 Dap WWK-0-LPWD-Well-F S 101701B-229 - 1 9934 254 264 - - XC101501-3 . CS 101701B-230 250 M81 - - - - 0112728 WWK-G-LPWD-WeB-A S 101701B-231 - 1 26028 675 703 . - 0112728 Dttp WWK-G-LPWD-Wcll-A S 10170IB-232 - 1 25325 657 684 - - 0112729 WWK-G-LPWD-Well-B S 101701B-233 - I 21537 558 581 - - 0112729 Dup WWK-G-LPWD-Wdl-B S 101701B-234 - 1 21074 546 56S . - XC1D1501-4 CS 101701B-235 500 1M40 - - - - XC101501-5 CS 101701B-236 1000 36595 - - - - PFOAFonnd(ng/L) " (peak.tea- intercept)/ slope x DF Recovery (%)= PTOA&Bnd(ng^)-PFOAfomdiBcoBtro!(ngtt.)] amount PFOA added (ng/L) xlOO APFO Foiunl (ngflL)= PFOA found (0{/L} x (MW APFO (431)/ MW PFOA (414)) Standard Curw: Linear Cl/xwciehlcdl Intercept = 276.530 Slope 38.123? Cosf. Of Del." 0.992303 CS = Calibration standard C ' Control sample S Sample LF "lab fortified sample FF = Field fortified sample LCS!- Laboratory Control Spike CK = Checic Sundtrd W)= Mot detected NQ Mot quantifiable AvgRcsp. of the 250 ppt Standards (area): 9117 Response of Ihe Check Standard (area): 9594 Spreadabcet prepared by.: 1^1\\\f^\ i! Percent Difference (%): -53. % diHereact acceptableif within 15% '~l RJZ032619 EID185093 Exyeen TL/ (.JRERSESEEAARRCH 3058 Research Drive State College, PA 16801 Phone:814-272-1039 Fax:814-231-1580 Exygen Study Number. Sponsor Study/Protocol No: Internal Chain of Custody/Fortification Sheet 008-046 Matrix: Water NA - I" t-i~\-"\ The samples listed below were removed from refrigerator No. ___"__ Time IH- Date Initials ,/2^ CLIENT SAMPLE ID EXYGEN ID NUMBER VOLUME (mL) FORTIFICATION (ng) na 0106020 Control 40.0 - na 0106020 Spk A 40.0 2.0 na 0106020 SpkB 40.0 20.0 WWK-D-Bldg-293 0112725 Spk C 40.0 20.0 WWK-D-Lubeck-Office 0112726 Spk D 40.0 20.0 WWK-G-LPWD-Well-P 0112727 Spk E 40.0 20.0 WWK-G-LPWD-Welt-A 0112728 Spk F 40 JO 20.0 WWK-G-LPWD-Well-B 0112729 Spk 0 40.0 20.0 WWK-D-Bldg-293 0112725 40.0 . WWK-D-Bldg-293 0112725 Dup 40.0 - WWK-D-Lubeck-Office 0112726 40.0 . WWK-D-JLubedc-Oflice 0112726 Dup 40.0 - WWK-G-LPWD-Well-F 0112727 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. 0112729 40.0 . WWK-G-LPWD-WeB-B 0112729 Dup 40.0 - - - - 0106020 Spk A Spiking Solution Used F07090I-3 (10 ng/mL) Volume Used for Spilling 200 uL (200 pL micropipet) Initial/Dale %4 iiii/n{'l 0106020 SpkB F070901-2 (100 Dg/mL) 200 |iL (200 (iL micropipet) 1 I] 0112725 Spk C 0112726 SpkD F07090l-2(100BgtaL) 200 |iL (200 ul, micropipet) 1 F07090I-2(100ng/mL) 200 (iL (200 fiL nucropipet) 1 0112727 Spk E F070901-2 (100 ng/mL) 200 pL (200 pL mieropipel) 1 0112728 Spk F 0112729 Spk 0 F070901-2 (100 ng/mL) F070901-2 (100 ng/mL) 200 )iL (200 uL micropipel) 200 fL (200 [tL micropipct) 1 V { -i/ - 1 All samples were measured: Time I'rt0 Date I"- 11 -"} Initials ^ IS After measuring samples were returned to refrig.eratorNo. ^ Time t'T'+jT Date li - ^~> r Initials V -.,, t^nl'f Comments: 200(iLof250ing/ioil. sodium Ihiosullate was Mkisi to all sampla before ipBdng. li[itirisyDtte: jft- IJ Analysis Summary; Data Set: 1011OlB Data Set: Data Set: -- Initial s/Date: Initials/Date: Initials/Date: ^ -yto|lblo| i/ f ~ i ~ ^ d llfth] Set extraction/analysis data v erifted by: (Mrif Date: ikl} July 26,2001/6 RJZ032620 EID185094 3058 Research Drive State College, PA 16801 Phone; Fax:8 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYOEN STUDY NUMBER: 008-046 . METHOD; $ PROTO MATRIX; \Vater ANALYTES; PTOA Client ID Exygen ID STEP STEP Dilutions STEP Dilutions STEP ] 2 (roL/mL) 3 (mL/mL) 4 na na na WWK-D.BldE-293 WWK-D-Lubeelc-Oflice WWK-G-LPWD-Well-P 0106020 Control 0106020SpkA 0106020 Spit B Oll2725SpkC 0112726 SpkD 0112727 SpkE ,. w ^A.o -- . -- ^^ ~ -. - --. -. -- ^. ,-- -- WWK-G.LPWD-WcU-A WWK-Q.LPWD-Wcll-B WWK-D-Bldg-293 WWK-D-Bldg-293 0112728 SpkP 0112729 SpkG 0112725 Oil 2725 Dup ^ --. ^/ -- .^, -- - - ^ -- ^B. I WWK-D-Lubeck-Offioe, WWK-D-Lubsck-Office WWK-0-LPWD-Well-P WWK-G-LPWD-Well-F 0112726 0112726 Dup 0112727 0112727 Dup .- ~ -- -- -. -. -- - .-- --- ~ . WWK.G-LPWD.Well-A 0112728 WWK-G-.LPWD-Well.-A 0112728 Dup WWK-0-LPWD-Well-B 0112729 WWK-0-LPWD.Wcll-B 0112729 Dup \ v -~. --. , . v\ -- -- -- -- ~ -- -- ^ --. Aj . InHlats/Date . . . . - S ^l-l1-| K^-n--i ,t,o,-|^|^.f.ol fri -- -- STEP 1: STEP 2: STEP 3; STEP 4: SPE column clean-up Final volume to 5 mL collected in LC/MS/MS analysis LC/MS/MS reanalysis. 15 nL polypropolene tubes Initials and date under each step indicaies the personnel that performed this step. SS Method of Analysis for the Determination ofPerfluorooctanoic Acid (PFOA) in Water COMMENTS; Final extracts stored in refrigerator ^5" Initials: t^- Date; loUlio Masslynx Sample List Sample List: C;\MASSLYNX\008-046,PRO\SampleDB\101701B.SPL Printed; Thu Oct 18 07;07;13 2001 i/)/) ID IPifftI Exygen STUDY NO- rrffl^k? Vial File Name LIMS ID Client ID Sample Description Matrix Sample Type Cone (ppt) Cone B 1 1 101701B-201 2 2 101701 B-202 3 3 101701B-203 4 4 101701B-204 5 5 101701 B-205 6 6 101701B-206 7 7 101701 B-207 8 92 101701B-208 9 41 101701B-209 10 42 101701B-210 11 43 101701 B-211 12 44 101701B-212 13 45 101701 B-213 14 46 101701B-214 15 47 101701 B-21S 18 2 101701B-216 17 48 101701B-217 18 49 1U1701B-218 19 50 101701B-219 20 51 1017018-220 21 52 101701B-221 22 53 101701B-222 23 3 101701B-223 24 54 101701B-224 25 55 101701B-225 26 S8 101701B-228 27 57 101701B-227 23 58 101701B-228 29 59 101701B-229 30 4 101701B-230 31 SO 1017018-231 32 61 101701B-232 33 62 101701B.233 34 63 101701 S-234 35 5 101701B-235 3S 6 101701B-236 XC101501-0,0 ppt standard XC101501.1, 50 ppt standard XC101501-2.100 pptstandard XC101501-3,250 ppt standard XC101501-4,500 pptstandard XC101501-5,1000 pptstandard XC101501-6,250 ppt check standard Methanol Wash 0106020 Control 0106020 Spk A, 50 ppt 0106020 Spk B, 500 ppt 0112725 Spk C, 500 ppt, DF2 0112725 Spk 0,500 ppt 0112726 Spk D, 500 ppt, DF=2 0112726 Spk 0,500 ppt XC1015Q1-1,50 ppt standard 0112727 Spk E, 500 ppt, OF=2 0112727 Spk E, 500 ppt 0112728 Spk P, 500 ppt, DP=2 0112728 Spk F, 500 ppt 0112729 Spk G, 500 ppt, DF=2 0112729 Spk G, 500 ppt XC101501-2,100 pptstandard 0112725 0112725 Dup 0112726 0112726 Dup 0112727 0112727 Dup XC101501-3,250 ppt standard 0112728 0112728 Dup 0112729 0112729 Dup XC101501-4, 500 pptstandard 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 Analyta Analyte Analyte Analyta Analyta Standard Analyte Analyte Analyte Analyte Standard Standard 0 SO 100 250 500 1000 250 -- -- 50 500 250 500 250 500 50 250 500 250 500 250 500 100 -- -- -- -- -- .-- 250 -- -- ,.- -- 500 1000 Masslynx Sample List Sample List: C:\MASSLYNX\008-046.PROlSampl9DB\101701B,SPL Printed: Thu Oct 18 07:07:13 2001 nV ,JioJr,| _______________________ P ^0-lOlr'-'lP' HPLC Method MS Tune File Inj Volume (pL) 1 water PPOA WATER 15 2 water PFOA WATER 15 . 3 water PPOA WATER 15 4 water PFOA WATER 15 5 water PFOA WATER 15 6 water PPOA WATER 15 7 water PFOA WATER 15 8 water PPOA 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 PPOA WATER 1S 15 water PPOA WATER 15 16 water PPOA 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 PPOA WATER 15 23 water PFOA WATER 15 24 water PFOA WATER 15 25 water PPOA WATER 15 26 water PPOA WATER 15 27, water PPOA WATER 15 28 water PPOA WATER 15 29 water PFOA WATER 15 30 water PFOA WATER 15 31 water PFOA WATER 15 32 water PPOA WATER 15 33 water PFOA WATER 15 34 water PFOA WATER 1S 35 water PFOA WATER 15 36 water PPOA WATER 15 Exygen STUDY ^0, OO& PA^/tb/ LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: 008-046 Instrument; Micromass Quattro Ultima (LC/MS/MS Unit VJ) ELECTROSPRAY ION SOURCE; Capillary: 3.0 kV Hexapole 2: 0 V I Hexapole 1:0 V Aperture 1: 0 V Source Block Temp.: 100C Desotvation Temp.: 300C ANALYZER: LM Res 1:10.5V HM Rest: 10.5V IEnergyl:LOV Entrance: -2 V Exite2V LM Res 2:13.0V HM Res 2: 13.0V Energy 2; 2.0V Multiplier: 700V GAS FLOWS AND PRESSURE: Desolvation N; Flow Rate: -650 L/hr Nebuliser Ni 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 (i (Exygen ID: 37A) (JONESCHROMATOGRAPHY: Part No. FK5962E) 35C 2 mM Ammonium Acetate in Type I Water Methanol Injected Volume: Ions monitored:. . Analvte 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 ==14min 15 uL %B 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 Parent ion 413 Dauehter ion 369 Dwell fsecs) 0,2 Flow Rate fmL/min) 0.3 0.3 0.3 03 0.3 0.4 0.4 0.4 03 Coll Enerev (eV) 10 Cone< 50 Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814)272-1039 FAX: (814) 231-1580 All Handwritten Peak-CD's by:_ 'Of ^'^'S?3^/^ ^W PiWUTS F^^^SBA ^CAO ^US^bTOV^HVftLOE.SUS^ OMTHI^ 9^. ^tl|oq(o( RJZ032624 EID185098 Scanning Mathod Report page 1 Mathod: Laat Modified: C;\MASSLTMX\008-046.EBO\ACQUDB\PEOA Mbn Oct 15 12:37:26 2001 Printed; Fri HOT 09 09:4l;26 2001 Sol-yant Delay { aina ) ; 1.00 ^u^ Fmiation : 1. MEM of 1 teas Pair ( ESP- ) Inter Channal. Delay ( Sees ) : 0.03 Span ( Daltons ) : 0.00 Start Time ( Mina ) : 0.00 t End Time ( dins ) : 8.00 Repeats : 1 Channel Parent Daughter Dwell (Sees) Coll Energy (eV) Cone ( V i... 1 413.00 369.00 0.20 10 50 EID185099 RJZ032625 Method Report Method rile-. Last Modified; Printed; C i \M&S3IiTOX\008- 046. PKO\ACQDI)B\waCar Friday, Novembar 09,2001 09:3Bi47 Friday, Mtovenibar 09. 3001 09i42:01 HP1100 IiC Pimp Initial Conditions Solvents A Bt C D 60.0 40.0 0.0 0.0 Plow (iHl/inin) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature LeftC'C} Oven Temperature Bight CO 0.300 14.0 0 400 35.0 35.0 HPllOO LC Pump Gradient Timetable The gradient Timetable contalna 9 entries which are : Time A Bt C D 0.00 60.0 40.0 0.0 0.0 0.40 60.0 40.0 0.0 0.0 1.00 10.0 90-0 0.0 0.0 7.00 10.0 90.0 0.0 0.0 7.50 0.0 100.0 0.0 0.0 9.00 0.0 100.0 0.0 0.0 9.50 60.0 40.0 0.0 0.0 13.50 60.0 40.0 0.0 0.0 14.00 60.0 40.0 0.0 0.0 Plow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 Paga 1 i|oih- Pressure 400 400 400 400 400 400 400 400 400 HnlOO LC Plimp Bxtemal Svont Timetable The Timetable contains 4 entries which are ; Time Initial 0.00 0.10 8.00 Column Switch Off Off Off Off Contacti Off On Off Off Contacts Off Off On Off Contact3 Off Off Oft Off Contact4 Off Off Off Off HPllOO Autosampler Tnltial Conditions Draw Speed Eject Speed (fll/min) Draw Position (mm) Stop Time (Bins) Injection Volume(^1) Vial Number 200.0 200 0.10 14.00 15.0 6 EID185100 RJZ032626 E x y e e n C^RERESSEEAARRCH ^ /ifc^Precdise Research. ". Proven Results. In order to verify mass resolution, a calibration check is performed on the mass spectrometer using aNaI/Rb/Cs tuning solution. The tuning solution is infused onto the mass spec using an infusion pump set to a flow rate of 10 uL/min. An MSscan&om80tol380amuisperfomedonbothMSl andMS2. The calibration is considered acceptable if the following 11 peaks are found within 0.2 anro oftheir known masses on both MS1 and MS2: 84.9,132.9,172.8, 322.7,472.6,622.5,772.4, 922.3,1072.2,1222.1 and 1372.0. If any of the masses are outside the 0.2 amu, then the instrument will be recalibrated and another calibration, check performed. The printouts from the calibration check can be found on me following 2 pages. ^._i8 Research Dwe ^SlateCDtegs, PA 16801, USA J: 814.272.1039 F: 814.231.1580 exygen.com RJZ032627 EID185101 ^ll&lol Calibration Check of NalRbCsOSOSOO on M$1 using NalRbCs tuning solution I CALCHK091001 -1 13 (0.811) Cn (Cen,2, 80.00, Mt); Sm (Mn, 2x2.00); Sb (1,40.00); Cm (1:16) 100. 172-8 THIS IS AN EXACT COPY OF M TOEORpNAL DOCUMENT.* ey W- DATC Exygen ssuw NO o^h% 132.8 322.8 472.7 64.9 / 190.8 / 232,9 187.0 V %MM 200 340.8 F-8 / 3S2.9 I^|I^.^.J,(L [ -390.8 622.5 772.4 322.2 1072.2 1 532.7S56.7 ^ 560 '' 666 690.S706.8 ^WQA 766' 866' 906 990.2 1000 1140.2 1100 ^^^1 1 ! 1 M H 0 -' 03 U1 h* 0 U 1-1 M 0 W . M 01 ' M 0 Calibration Check Of NalRbGs090800 on MS2 using NalRbCs tuning solution CALCHK091001-2 8 (0.569) Cn (Cen,2,80.00, H.t); Sm (Mn, 2x2.00); Sb (1,40.0M); Cm (1:17) 100-, 172.8 Mil0^.W./,W! OI } 132,9 %- THIS IS AN EXACT COP BY----^ THE ORIGINAL DOCUM nA-re \\ Sygen sru&Y NO ^ 92.0 ' / ^ 322.8 190.8 / .232.9 234.8 / Jj tejllll ..iiAiiii.i l,ji,-i. .. -i. 0 2 10 300 472.7 622.5 772.4 922.3 (340.8 -382.9 1.. 1,.440-8 532\5.75.6,.,6. 690.5J08.5 840,4^56.3 1072-1 990.2 1134.0 400 5'66 ' ' " 666' ""700"'1' 866" '"'s6o "'"ib'ob''' '1'1'o'd '' i Initial Calibration Curve ExygcaStuiyNo.: Set No: Extraction Date Anilyzcdnn: 008-046 101701B 10/17/1)1 10/18/01 The fua curve of the d^^iamed to determine perfbtmaiice. A linear regression(with no weightirig)is performed uAig the first six staadnrifa of the analyticalpin. The coefficient of itaetniination(R Square)niust be 0.935 or greater- Iflhcsct failltomert this requirement,tile nm must be rejectedand the samplesreanalyzed. Exygen ID XC101501-0 XC101501-1 XC101501-2 XCI01I01-3 XC1015C1-4 XCI01501-5 Standard Concentratioa (ns/U 0 50 100 250 500 1000 Peak Area 0 2269 4485 9753 20662 40877 Coefficient ofDetennination: 0.99963071 SUMMARY OUTPUT Regression Statistics Multiple R 0.99981534 R Square 0.99963071 Adjusted RSqua 0.99953839 Standard Error 333.267525 Observations_______6 ANOVA Regression Residual Total 'f SS MS F SignificanceF I 1202591346 I.2E+09 10827.597 5.U47E-08 4 4442685724 111067.2 5 1203035615 Intercept X Variable I Coefficients StamiardError tStal 95.7073733 184.143363 0.519744 40.7746083 0.391853524 104.0557 P-vaiue 0.6306791 5.115E-08 Lower 95% 415.557624 39.6866462 Upper 95% Lower 95.0% Upper 95.0% 606.972371 -415.55762 606.972371 41.8625703 39.6866462 41.8625703 EID185104 RJZ032630 Page 1 Quantify Calibration Report Study No.: 008-046, Sot Ho: 101701B, Sxte. Data: 10/17/01, Analyst: K Risha P:\Dat&\ICMSMS7\Masalynx\008-046.BRO\Cuxv^DB\101701B l^lo(l^(o| Calibration: tast aodifiad: Fca. Oct 19 07:08210 2001 u Printed: Fci Oct 19 07:15:14 2001 Exygen Roflaarch EID185105 RJZ032631 Quantify Saapla Report Study Ho.: 008-046, Sat Ho: 101701B, Ext- Data: 10/17/01, Analyst: K Biaha Eaga 1 Sample List: P!\Data\LCHEHS7\yasalyiuc\008-046.PRO\SaiBplQDB\101701b Last modified: Fri Oct 19 07:07:33 2001 Method: .P:\Data\I,Q.ISMS7\Mas3lynx\008-046.PM>\MathDB\l01601 PEOA Last aodifiad: Wed Oct 17 07:42; 45 2001 Job Coda: Printed; Fri Oct 19 07:15:16 2001 ,iA Inlfah _ Pria 1^| T!gKPg-._________"_" Run* 101y_ S-2.01 Thi&l'M-'j!^' ITaaa; 101701B-201 Text: 1: PFOft Sxygen Research RJZ032632 EID185106 Quantify Sampla Report Study Ho.; 008-046, Sat Ho: 101701B, Ext. Data: 10/17/01, Analyst: K Risha Sample List: Last modified: Mathod: Last modified: Job Coda: P:\Data.\IMSMS7\Masalynx\OOa-046.ERO\Sa3BpleDB\101701b E-ri. Oct 19 07:07:33 2001 P:\Data\I,caiSMS7\Ma33lyD3C\008-046.E-XlO\MatbDB\101601 PFOA Wed Oct 17 07:42:45 2001 Printed; Fra. Oct 19 07:15:16 2001 Eaga 2 Hamas 101701B-202 Toxt: 1: PFOA XC1C}1501-1,50 ppt standard 1017(01B-202Sm(Mn,2x2) 10(h 18-0ct-2001 09:09:23 LG/MS/MS #7 MRM of 1 Channel ES- 5- '9 413 > 369 4.20e4 %- 0- -r-i i^r fr r i-i"i~i i i i i . ,i-rTi1 2.00 3.00 i^r |-i j > i p i i <-i-|f-r7-~r7TTT~~F'~~.-r|'r i 4.00 5.00 6.00 r .-| ... i | .. 7.00 i i ) . . . . 8 . i 0 , 0 n u c Exygen Research RJZ032633 EID185107 Quantify Sample Report Study No.: 008-046, Set Ho; 101701B, Ext. Data: 10/17/01, Analyst: K Risha Sample List: Last modified: Method: last modified: Job Code; P:\Date\lCMSMS7\l&sslynx\008-046.PRO\SampleDB\101701b Fri Oct 19 07:07:33 2001 P;\Data\:LCMSMS7\Ma3slynx\008-046.PKB\MathDB\101601 PFOA Wed Oct 17 07:12:45 2001 Printed: Frx Oct 19 07:15:16 2001 Bags 3 Hame: 101701B-203 Text: 1: PFOA XC101501-2,100 ppt standard 1017CD1B-203Sm(Mn,2x2) 100-i 18-0ct-2001 09:26:05 LC/MS/MS #7 MRM of I Channel ES- 5. 0 413 > 369 8.23e4 %- 0- 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research RJZ032634 EID185108 Quantify Sample Report Study No.: 008-046, Set Ho: 101701B, Ext. Data; 10/17/01, Analyst: K Riaha Sample list: Last modified; Method; I,aot modified: Job Code: P:\Data\KMSMS7\Mas3Xyax\008-046.ERO\SaBplaDB\101701t> Pri Oct 19 07:07:33 2001 P:\Data\LCMSMS7\Maaalynx\008-046.PRO\HethDB\101601 PEOA Wod Oct 17 07; 42; 45 2001 Brintad: Fri Oct 19 07;15;16 2001 Pago 4 Same,: 101701B-204 2'ext: i: proa XC101501 -3.250 ppt standard 1017C01B-204 Sm (Mn, 2x2) 100-i 1 B-Oct-2001 09:42:43 LC/MS/MS #7 MRM of 1 Channel ES- 5. 0 413 > 369 1.81e5 %- 0- 2.00 3.00 4.00 ^ 5.0C) 11111 ri i-i. 6.00 j"i |iiii7.0p0-i .,(... ri Time 8.00 Exygen Raaoarch RJZ032635 EID185109 Quantify Sample Report Study Ho.: 008-046, Sat No; 101701B, Ext. Date: 10/17/01, Analyst: K Kiaba Sample List: Last aodified: Method: Last aodified; Job Code: P:\Data\:Ua.lSMS7\Masslynx\008-046.PRO\SaapleDB\101701b Fri Oc1: 19 07:07:33 2001 P:\Data\I.CMSMS7\Ma33lyBx\OOB-046.PaO\MathDB\10160l PB13A Wed Oct 17 07:42;45 2001 Printed: E'ri Oct 19 07:15:16 2001 Page 5 Nona: 101701B-205 Text; 1: PE-OA XC101501-4,500 ppt standard 1017C31B-205 Sm (Mn, 2x2) 100-1 18-0ct-2001 09:59:21 LC/MS/MS #7 MRM of 1 Channel ES- 5.1 0 413>369 3.76e5 %- 0- i i i i 1i . i i 1i i . i 2.00 1. i i . ) , , 3.00 . . ) 1-, ,. i i i , 4.00 . , i . i i . |T'' 5.0C) i''' i 6.00 '' i ''''7.0i 0' ' '"r'' i "iTime 8.00 Exygon Research RJ-Z032636 EID185110 Quantify Sample Report Study No.: 008-046, Set No: 101701B, Ext. Date; 10/17/01, Analyst: K Risha Sample list: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS7\Ma3slynx\008-046.PBO\SaitipleDB\101.701b Fri Oct 19 07:07:33 2001 P:\Data\I^aiSMS7\tesalyiw\OOB-046.:PIU3\MQtAiDB\l01601 PEOA. Wed Oct 17 07:42:45 2001 Printed; Exi Oct 19 07:15:16 2001 Page 6 Name: 101701B-206 Text: 1: PFOA XC1C)1501-5,1000 ppt standard 1017 01B-2068m(Mn,2x2) 100-i 18-Oct-ZOOI 10:15:56 LC/M5/M5#7 OJ >9 MRM of 1 Channel ES413 > 369 7.35e5 %- 0- 2.00 3.00 (1 4.00 5.00 6.00 7.00 8.00lime 1 1 1 1 | 1 1 1 1 1 1 1 1 1 ( . . 1 1 ( 1 1 1 , 11 1( 1 1 1 1 j 1 ! 11| . . . | , . . . ]. , . . | 1, 1 1 | 1 . . . ( . . 1 . ] Exygen Research R.7Z032637 EID185111 Quantify Sample Report Study No.: 008-046, Set Ho: 101701B, Ext. Date; 10/17/01. Analyst: K Higha Santpla List: lAst modified: Mathod: last modified; Job Code: P:\Data\lCMSMS7\Ma3alynx\008-Od6.PRO\SsmpleDB\101701b Fri Oct 19 07:07:33 2001 P:\Data\I,CMSMS7\l-faS3lyTLic\008-046.PBO\MQthDB\101601 PFOA Wed Oct 17 07:42:45 2001 Printed: E-ri Oct 19 07:15:16 2001 Page 7 Kama: 101701B-207 Text: 1: PFOA XC1C)1501-6,250 ppt check standard 1017C31B-207Sni(Mn,2x2) 100-1 5. 0 18-0ct-2001 10:32:34 LC/MS/MS #7 MRM of 1 Channel ES- 413>369 1.74e5 %- 0- ?i^ i ' > i i ' i i i i i 11 i - i i Time 2.00 3.00 4.00 5.0(0 6.00 7.00 8.00 Bxygen Research RJZ032638 EID185112 Quantify Sample Report Study No.: 008-046, Set No: 101701B, Bxt. Data; 10/17/01, Analyst: K Risha Sample List: Last modified: Method: Last modified: Job Coda: P:\Data\I,CMSMS7\Ma3alynx\008-046.EBO\aapleDB\101701b Pri Oot 19 07 .07; 33 2001 P;\Data\LCMSMS7\Mas3lyiuc\008-OA6.ESO\MathDB\101601 PFOA Wed Oct 17 07:42:45 2001 Printed; Fri Oct 19 07;15:16 2001 NaTO: 101701B-208 Text: 1: PFOA Page 8 Exygen Research RJZ032639 EID185113 Quantify Sample Report Study Ho.: 009-046, Set Ho: 101701B, Ext. Date: 10/17/01, Analyst: K Bisha Sample List; last modified: Mathod: laat laodified: Job Coda: P:\Data\LCMSMS7\Has3lynx\008-046.PaO\SanpleDB\101701b fri Oc-t 19 07:07:33 2001 P;\DataUaiSH37\Ma3slynx\008-046.?RO\MathDB\l01601 PFOA Wed Oct 17 07; 42; 45 2001 Printed; FBI Oat 19 07;15:16 2001 Page 9 Mame: 101701B-209 text: 1: PFOA 0106020 Control 18-0ct-2001 11:05:47 LC/MS/MS #7 MRM of 1 Channel ES- 7.10 ^y, 413 > 369 1.77e3 2.00 3.00 4.00 5.00 6.00 7.00 iTime 8.00 Exygen Research RJZ032640 EID185114 Quantify Sample Haport Study No.; 008-046,. Set Ho; 101701B, Ext. Data: 10/17/01, Analyst: K Riaha Sample list: Last modified: Mathod: taat jaodified: Job Code; P:\Data\LCMSMS7\Masslynx\008-046.PKO\Sa]BpleDB\10170lb fri Oct. 19 07;07;33 2001 P:\Dat.a\LCMBMS7\Mas3lyn3c\008-046.ERO\MathDB\101601 CTOA Wed Oct. 17 07:42:45 2001 Printed: Fri Oct 19 07:15:16 2001 Page 10 Hama: 101701B-210 Text: 1: PFOA 0106020SpkA,50ppt 1017C31B-210Sm(Mn,2x2) 100i 18-0ct-2001 11:22:24 LC/MS/MS #7 MRM of 1 Channel ES- 5. 0 . 413 > 369 3.21 e4 %- 0- hprT-^^-^-i-^-^-)--r-i-^^-F^(l^^-^}'T1v;^^('l7".^"('>'T^ r'pT-, ,..-? ,,,.(., , , , ,..,..^,.,.^,,11, . , i | . . . . i Dine 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research RJZ032641 EID185115 Quantify Saapla Report Study Mo.: 008-046, Set No: 101701B, Ext- Date: 10/17/01, Analyst; K Risha Sample IAat: I^st modified: Method: Last modified; Job Coda: P:\Data\I^MSMS7\Ma33lynx\008-046.I>RO\SaaipleDB\101701b Fri Oct 19 07:07:33 2001 P:\Data\LCMSMS7\Ma33lyiuc\008-046.PRO\MethDB\101601 PFOA Wed Oct 17 07:42:45 2001 Printed: Fri Oct 19 07:15:16 2001 Page 11 Haine; 101701B-211 Text: 1; PPOA 0106020 Spk B, 500 ppt 1017(01B-211Sm(Mn,2x2) 10(h 18-0ct-2001 11:39:01 LC/MS/MS #7 MRM of 1 Channel ES- 5- 1 413>369 3.49e5 %- 0- 2.00 3.00 4.00 'i 5.0C3 i i i i ' . i 6.00 i 11 i 11 ' 7.00 ' i ' '' i Time 8.00 Exygan Research RJZ032642 EID185116 Quantify Sample Report Study Ho.; 009-046, Sat No: 101701B, Ext. Data: 10/17/01, Analyst: K Ri-sha Sample List: Last modified: Mathod: Last modified: Job Code; P:\Data\LCMSMS7\Mag3lyTOC\008-046.PRO\SanploDB\101701b E-ri Oct 19 07:07:33 2001 E:\Data\La4SMS7\Ma33lyn3;\008-046.PBO\MethDB\101601 PE'OA Wad Oct 17 07:42:45 2001 Printed: Fri. Oct 19 07:15:16 2001 Pago 12 Name: 101701B-212 Text; 1: PFOA 0112725 SpkC, 500 ppt, DF=2 1017C31B-212Sm(Mn,2x2) 100-i IB-Oct-2001 11:55:39 LC/MS/MS #7 MRM of 1 Channel ES- 5* 1 413 > 369 2.88e5 1 i %- 0- '' ' 1 ' 1 1 ' 1 1 1 ' 1 1 1 < ' 1 ' ^ ^ ' ' 1 ' ' ' 1 ' '----'"T-- ' ; 1 ' ' ' ' 1 ' ' ' 1 ""1C 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygon Research RJZ032643 EID185117 Quantify Sample Report Study Mo.: 008-046, Sat Ho: 101701B, Ext. Data: 10/17/01, Analyst: K Biaha Sample Iiiat: Last modified: Method: last modified: Job Coda; P: \Data\:LCMSMS7\Ma3slyiuc\008-04 6. PBO\SanipleDB\101701b Eci Oct 19 07:07:33 2001 P:\Data\LCMSMS7\Ma33lyiUt\OOe-046.FRO\MethDB\l0160l PFOA. Wed Oct n 07:42:45 2001 Printed: ?ri Oct 19 07;15:16 2001 Page 13 Hana; 101701B-213 Text: 1: PFOA 0112725 SpkC, 500 ppt 1017 01B-213 Sm (Mn. 2x2) 10Ch 18-0ct-2001 12:12:15 LC/MSJMS #7 MRM of 1 Channel ES- 5. 1 413 > 369 6.07e5 %- 0- 2.00 3.00 4.00 5.00 6.00 7.00 8.001"'"- ' ' i ' ' i ' i ' i ' i i i ' i ' ' ' 1' ' ' ' i ' ' ' i ' ' ' i ' ' i ' ' ' i ' ' ' i Exygon Research RJZ032644 EID185118 Quantify Sample Report Study Ho.: 008-046, Sot Ho: 1Q1701B, Ext. Data: 10/17/01, Analyst: K Risha Sample List: Last modified: Method: Last modified: Job Codo: P;\Data\LCMSHS7\Magalynx\008-04.6.PBO\SaaipleDB\101701b Pri Oct 19 07:07;33 2001 P;\Data\LCMSMS7\Mas3lynx\008-04S.PB.O\MethDB\101601 PFOA Wed Oct 17 07:42:45 2001 Printed: E-ri Oct 19 07:15:16 2001 Paga 14 Kama: 101701B-214 Toxt; 1; PFOA 0112726 Spk D, 500 ppt, DF=2 1017{01B-214Sm(Mn,2x2) 100-1 18-0ct-2001 12:28:51 LC/MS/MS #7 MRM of 1 Channel ES- 5. 1 413>369 3.18e5 %- 0- - ' ' i ''2,.'0--0 i ' ' i' 3.00 ' ' i ' ' ' i' ' 4.00 ' , ' i' t 1 ' i"i 1 ' 5.00 ' ' 1' ' 6.00 ' 1' ' ' ' t' ' 7.00 ' ' 1 ' ' ' i iiin^ 8.00 Exygan Research RJZ032645 EID185119 Quantify Sample Report Study Ho.: 008-046, Sat Ho: 101701B, Ext. Date: 10/17/01, Analyst: K Kisha Sample List: Last modified: itethod: Last modified: Job Code: P:\Data\M4SMS7\Ma33lynx\008-046.PRO\SaiirpleDB\101701b Fri Oct 19 07;07;33 2001 P:\Data\I^MSl.lS7\Ma33lymc\009-046.PBO\MathDB\101601 PFOA Wed Oct 17 07:42:45 2001 Printed: Ezi Oct 19 07;15:l6 2001 Page 15 Hama; 101701B-215 Text: I: PE-OA 0112726 Spk D, 500 ppt 1017C318-215 Sm(Mn. 2x2) 100-i ----------- 5. 1 18-0ct-2001 12:45:31 LC/MS/MS #7 MRM of 1 Channel ES- 413>369 7.1 le5 %- 0 - 1 1 1 1 | 1 1 1 1 | 1 l | 1 1 | ' 1 | 1' ^ ' ' 1 ' 1 t ' ' 1 ' ' ' t ' ' ' 1 ' ' 1 ' 1 11111C 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygan Rogoarch RJZ032646 EID185120 Quantify Sampla Report Study No.; 008-046, Sat No: 101701B, Ext. Data: 10/17/01, Analyst: K Riaba Sample List: Last modified; Method: Last modified: Job Coda: B:\Data\I.OMSyS7^1a33lynx\008-046.ERO\SaanpleDB\101701b E-ri Oct 19 07:07:33 2001 P:\Data\LCMStffi7\lfa3slynx\008-046.ERO\MethDB\lOl601 PFOA Wed Oct 17 07:42:45 2001 Printed; Eci Oct 19 07:15:16 2001 Baga 16 Name: 101701B-216 'Eaxt: 1: PFOA XC101501-1,50 ppt standard 1017(01B-216Sm(Mn.2x2) 100^ 18-0ct-2001 13:02:14 LC/MS/MS #7. MRM of 1 Channel ES- 5. 0 413 >369 3.93e4 I %- i - fp 0- '-T-i-t-Ti'-r-i i . 2.00 < (-!'T-?T-r !~i-f-i-[''-'' t^'^ ' 3.00 4.00 ' i "''i ' r ' ' 5.00 i i 6.00 ' i ' i' 7.00 ' i' ' i ii""- 8.00 Eacygen Rasaarch RJZ032647 EID185121 Quantify Sample Report Study Ho.: 008-046, Sat Ho; 103.7013, Ext. Data: 10/17/01, Analyst: K Rxsha. Sajnpla list: Last nodifiod: Method: Last modified: Job Coda: P:\nata\IAlSMS7\te33Xynx\008-046.PHO\SaaplaOB\101701b fri. Oct 19 07:07:33 2001 P:\Data\LCMSMS7\Ite.33lyruc\009-046.PBO\MQthDB\10l601 PEOA Wed Oct 17 07:42;45 2001 Printed: rri Oct 19 07!l5:16 2001 Paga 17 Hane: 101701B-217 'Eext: 1; PE-OA 0112727 Spk E, 500 ppt, DF=2 1017C31B-217Sm(Mn.2x2) 10(h 18-0ct-2001 13:18:59 LC/MS/MS#7 MRM of 1 Channel ES- 5. 0 413 > 369 2.16e5 %- 0- r' 2.00 ' ' i " ' i ' i t . ' i ( 3.00 ri 6.00 7.00 4.00 5.0(B i 1111 i 11 > i 111 i 11 i 11 n 11-. i 11 Time 8.00 Bxygen Bagoarch RJZ032648 EID185122 Quantify Sampla Report Study Ho.; 008-046, Sot No: 101701B, Ext. Data: 1.0/17/01, Analyst: K Kiaha Sample List: Last modifiod: Method: Last modified: Job Coda: P:\Data\LCMSMS7\Ma33lynA008-046.PRO\SampleDB\1.01701b Exi Oct 19 07:07:33 2001 P:\Data\lCMSMS7\Ma33lynx\008-046.PRO\MethDB\10l601. EFOA Wed Oct 1.7 07:42:45 2001 Printed: E'ri Oct 19 07:15:16 2001 Page 1B name: 101701B-21B rext: I: PFOA 0112727 Spk E, 500 ppt 1017C01B-218Sm(Mn.2x2) lOO-i 18-0ct-2001 13:35:43) LC/MS/MS #7 MRM of 1 Channel ES- 5. 0 413>369 4.66e5 %- 0- i 1 ' i' '' i i ' ' i ' 2.00 3.00 ' ' i ' ' i' ' 4.00 ' i' ' ' i' '' 5.00 ' i ' ' ' ' i' ----i' 6.00 i' ' ' '-- 7.00 i''' i i in 8.00 <= ! Exygen Raaaarch RJZ032649 EID185123 Quantify Saapla Roport Study Ho.: 008-046, Set Wo: 101701B, Sxt. Data: 10/17/01, Analyst: K Bisha Sample IAst; Last modified; Method: last modifiad: Job Coda: E:\Data\I.CMSMS7\Mag3lynx\008-046.PM\SaiapleDB\l01701b Eri Oct 19 07:07:33 2001 B:\Data\LCMSMS7\Ha33lynx\OOa-046.PRO\t'lQtbDB\10l601 BTOA Wed Oct 17 07:42:45 2001 Printed: Rci Oct 19 07:15:16 2001 Paga 19 Mama: 101701B-219 Text: 1: PPOA 0112728 SpkF, 500 ppt, DP=2 1017C01B-219Sm(Mn,2x2) 100-i 18-0ct-2001 13:52:27) LC/MS/MS #71 MRM of 1 Channel ES- 0 413>369 3.15e5 %- 0- | 1 1 | 1 f 1 1 , 11 1 ' ' ' k^~-- -- --1 -- -- --' --'--,1------ --' --' --1 .,1.,,,'..-- i.-- --1 .'---'...'i..--' ..1....' 'f m ,,,,,^1 Ti"m1Ca 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Rasaarch RJZ032650 EID185124 Quantify Saaipio Report Study Ho.: 008-046, Set Ko; 101701B, Ext. Data: 10/17/01, Analyst: K Kisha Sample List: last modified: Mathod: Last modified: Job Code; P;\Data\lCMMS7\]!fa3slynx\OOa-046.EBiO\SaaipleDB\l01701b E-rx Oct 19 07:07:33 2001 P;\Data\IiCMSMS7\Mas3lyn.x\OOe-04S.PRO\M6thDB\10l601 PE"OA. Wed Oct 17 07:42:45 2001 Printed; E-ri Oct 19 07:15; 16 2001 Page 20 Hame; 101701B-220 Taxt: 1: PFOA 0112728 SpkF, 500 ppt 1017C31B-220Sm(Mn,2x2) 100-| 18-OCI-2001 14:09:15 LC/MS/MS #7 MRM of 1 Channel ES- 5.1 0 413>369 7.18e5 %- 2.00 3.00 4.00 5.00 1--......--q6--.00. .--......7--.0--0,, 8.0T0ima 0- 1 1 1 ' ) ' 1 ' | ' ' ' 1 | ' 1 1 1 1 1 1 1 ' 1 1 ' | ' ' ' 1 ' ' ' 1' '1 ' ' 1 ' 1 ' t 1 '. '. ' 1 1 ' ' 1 ' , ' ' , .--.' ' , . ,---"--"I, 11110 Exygan Raanarch RJZ032651 EID185125 Quantify Sampla Report Study No.: 008-046, Sat Ho: 101701B, Ext. Data: 10/17/01, Analyst: K Risha Sample List: Last modified: Method: Last modified: Job Coda: P:\DataUCMSMS7\Mas3lynx\OOa-046.PRO\SajBipleDB\101701b Fzri. Oct 19 07:07:33 2001 P:\nata\I,CMSMS7\Ma33lynx\008-046.PRO\MathDB\l01601 EFOA Wed Octe 17 07:42:45 2001 Printed: fri. Oct 19 07;15:16 2001 Paga 21 Name: 101701B-221 Text.; 1: PFOA 0112729 Spk G. 500 ppt. DF=2 1017(31B-221 Sm (Mn, 2x2) 100-1 18-0ct-2001 14:25:54| LC/MS/MS #71 3.1 19 MRM of 1 Channel ES413 > 369 2.54e5 %- 0- -,----, ,,...2..00 , ..... .,.----, 3.00 i, ,.4.;.0,0.,,1 ...,5|.0(0 i i i ii ' i ' ii i 6.00 i i i i , 'i'i 7.00 ' ' i ' ' ' iTime 8.00 Exygon Research RJZ032652 EID185126 Quantify Sample Report. Study Ho.: 008-046, Sat Ho: 101701B, Ext. Date: 10/17/01, Analyst: K Kisha. Sample Iiiat: Laat ntodxfiod: Method: Last modified: Job Code: P!\Data\IMSHS7\HaS3lynx\008-046.PRO\SaiBplQDB\101701b ETi Oct 19 07:07:33 2001 E;\Data\tCMSHS7\Ma33lynx\008-046.PRO\HathDB\101601 PfOA Wed Oct 17 07:42:45 2001 Printed: Fri Ocfc 19 07:15:16 2001 Page 22 Saw. 101701B-222 Text: I: PFOA______ 0112729 SpR G, 500 ppt 1017(D1B-222Sm(Mn.2x2) 10(h 18-0ct-2001 14:42:32 LC/MS/MS #7; MRM of 1 Channel ES-I '9 413 > 369] , 6.32e5l %i 0- l 1 ' 1 ' l 1 ' | ' l ' 1 1 ' 1 1 1 1 1 '------' | ' '' ' 1 ' ' 1 ' < . ' ' I ' 1 1 1 ' 1 ' 1 1 ' ' 1 1 ' ' ' ' 1 ' ' 1 ' 1 ' ' ' ' 1 11111C' 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Zxygon Resoarch RJZ032653 EID185127 Quantify Saapio Baport Study Ho.; 008-046, Sot No: 101701B, Sxt. Data: 10/17/01, Analyst; K Risha Sample List: Last mockLCied: Hethod: Last modified: Job Coda: P:\Data\LCMSMS7\MaBslynx\OOa-046.PRO\SamplaDB\101701b Fri Oct 19 07:07:33 2001 Pi\Data\I.CMSMS7\Maa3lyTMc\OOa-046.PE.O\MathDB\101601. PFOA Wed Oct 17 07:42:45 2001 Pri-ntod: Rci Oct 19 07:15:16 2001 Page 23 (Tana: 101701B-223 Text: 1: PFOA XC101501-2,100 ppt standard 1017C}1B-223Sm(Mn,2x2) 100-1 18-0ct-2001 14:59:13 LC/IVIS/MS #7 MRM of 1 Channel ES- 5.' 9 413>369 6.95e4 %- - 0- 2.00 3.00 4.00 5.00 6.00 7.00 8,00 Exygon Rasoarch RJZ032654 EID185128 Quantify Sample Baport Study Mo.: 008-016, Set Ho: 101701B, Bxt. Date: 10/17/01, Analyst: K Rl-aha Sample List: Last modified: Hethod: Last nodified: Job Code: P;\Data\LCMSMS7\Mas3lynx\008-046.PRO\SanipleDB\101701b Fri Oct 19 07:07:33 2001 P:\Data\I.CMSMS'7\Mag3lynx\008-046.PRO\MothDB\101601 PFOA Wed Oct 17 07:42:45 2001 Printed! Fri Oct 19 07:15:16 2001 Pago 24 Maine; 101701B-224 Text: 1; PFOA 0112725 1017C31B-224Sm(Mn,2x2) 10(h 18-0ct-2001 15:15:48 LCyMS/MS #7l MRM of-1 Channel ES- 5. '9 413 > 369 2-62e5 %- 0- i i i i i i i i i . i i . i i i i'--r-^Time 2.00 3.00 4.00 5.0(0 6.00 7.00 8.00 Exygen Research RJ2032655 EID185129 Quantify Sample Report Study Ho.: 008-046, Set Ho: 1017013, Sxt. Date; 10/17/01, Analyst: K Kiaha Sampla lAst: Last modified: Mothod: Last modified: Job Code: P:\Data\LCMSMS7\Mas3lyiix\008-046.PRO\SaiiipleDB\101701t> Fri. Oct 19 07:07:33 2001 P:\Data\LCMSMS7\lfa33lynx\008-046.ERO\MathCB\l01601. PE-OA Wed Oct 17 07:42:45 2001 Printed: Fri Oct 19 07:15:16 2001 Page 25 Name: 101701B-225 Text; 1: PFOA 0112725 Dup 1017(01B-225 Sm (Mn, 2x2) 100n 18-0ct-2001 15:32:27 LC/MS/MS #7 MRM of 1 Channel ES- 5. 1 413 > 369 2.38e5 %- i' r 7.00 ' Time 2.00 3.00 i'i 4,00 G- 1-,--. . , . .-. . ) . . , . i . . . . i . . i , . . 1 1 . 1 . . 1 1 1 . .-v 1i 5.0C) i ' i i ' 6.00 i' '' ' i B-00 Exygan Research RJZ032656 EID185130 Quantify Sampla Bepoxt Steady Mo.; 008-046, Sat Ho; 101701B, Ext. Date: 10/17/01, Analyst: K Riaha Saapla I>i3t: I^at modified: Method! Last. aodified: Job Coda: fri P:\Data\I>CMSyS7\Maa3lynx\008-046.PI!0\SaiapleDB\10170rb Oct. 19 07:07:33 2001 P;\Data\ACMSHS7\Ma33lynx\008-046.PBO\MathDB\101601 PTOA ffed Oct 17 07:42:45 2001 Printsd: Fri Oct 19 07:15:16 2001 Paga 26 Naaa: 101701B-226 Text: 1: PE-OA 0112726 1017(01B-226Sm(Mn.2x2) 10(h 18-0ct-2001 15:49:11 LC/MS/MS #7 MRM of 1 Channel ES- o. '8 413 > 369 3.65e5 %- 0- ' i 1 i' ''2.i00'' i ' ' i 3.00 ' i ' 4 -0i'0' ' ' > ' ' ' 5 . i 0 0 ' ' ' i '' 11' 6.00 ' i ' '' 7' .0.'0 ' ' ' i i i"" 8.00 Exygon Raaearch RJZ032657 EID185131 Quantify Sample Raport Study Ho.: 008-046, Sat Vto: 101701B, Ext- Data: 10/17/01, Analyst: K Bisba. fri Sample List: P:\Data\LCHSMS7\Ma3glynx\008-046.:PRO\SaiiiplaOB\101701b last aodifiad: Oct 19 07:07:33 2001 Method: P;\Data\I.CHSMS7\Ma33l2Tnjc\008-046.PRO\MathD'B\10l601 EE-OA lA3t modifxad: Wed Oet 17 07:42:45 2001 Job Coda: Printed; Eri. Oet 19 07;15:16 2001 Pago 27 Naae: 101701B-227 Text: 1; PE-OA 0112726 Dup 1017C31B-227Sm(Mn.2x2) 100-i 18-0ct-2001 16:05:55) LC/MS/MS #7, MRM of I Channel ES- o> 08 413 > 369 3.57e5 %- 3.00 4.00 5.0 6,00 .i i' 7.00 8.00 0- 2.00 .--i 0 Time ' 1 ' i i i i i i i . i . i i i i i i i i ' ' ' i ' ' 1 L! i ' i i i ' i Exygen Boaearch RJZ032658 EID185132 Quantify Sanpla Roport Study No.: 008-046, Set; Ho: 1(117013, Ext. Date: 10/17/01, Analyst: K Riaha Sanpla List: last nodifiad: " Method; last modified: Job Coda: P:\Data\:LCMSMS7\tfasslyiw\008-046-BTO\SainpleDB\l01701b Fri Oct. 19 07:07:33 2001 P;\Daka\LCMSHS7\lfa33lynx\008-046.PBO\MathDB\10ie01 BeOA Wed Oct 17 07:42:45 2001 Printad; Eri Oct 19 07:15:16 2001 Pago 28 Hame; 10170 IB-228 Taxt: I: PFOA 0112727 1017(31B-228 Sm (Mn, 2x2) 100-1 18-0ct-2001 16:22:38: LC/MS/MS#7 MRM of 1 Channel ES-; 3. 413 > 369. 1.74e5S t i %- iTime' 0- ' ' i ' ' i ' ' i ' ' . i i '' ' 2.00 3.00 4.00 5.0(0 6.00 7.00 8.00 Exygon Rosoarch RJZ032659 EID1B5133 Quantify Sampin Kaport Study Ho.: 008-046, Sot Ho: 101701B, Sxt. Data; 10/17/01, Analyst: K Risna Sample list: lA3t modified; Matbod: I-aat iaodiied: Job Coda: P:\Data\I.CMSM37\te33lynx\008-046.BEO\SaBplaDB\101701b Fri Oct 19 07:07:33 2001 P:\Data\IMSMS7\tfa33lyiut\008-046.PRO\MathDB\l0160t PFOA Wed Oct 17 07:42:45 2001 Printed: E'ri Oct 19 07:15:16 2001 Paga 29 Kama: 101701B-229 Text: 1: PFOA 0112727 Dup 1017(MB-229 Sm (Mn. 2x2) 100-1 18-0ct-2001 16:39:20) LC/MS/MS #7! MRM of I Channel ES-1 M 413>3691 1.57e5j 1 : %- i. 0- r r .-i , , >, 11.-,, i. i . . i i i i i . -1 iTims 2.00 3.00 4.00 5.0 0 6.00 7.00 8.00 Exygon Ragaasch RJZ032660 EID185134 Quantify Sampio Koport Study No.; 008-046, Sat Mo: 101701B, Ert. Data: 10/17/01, Analyst: K Riaha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\IMSMS7\Ma33lynx\OOa-046.PBO\SampleDB\1017Qlb fri Oct 19 07:07:33 2001 P:\Data.\LCMSMS7\Mas3lynx\008-046.PRO\MothDB\101601 PFOA Wed Oct 17 07:42:45 2001 Printed: Fri Oct 19 07:15:16 2001 Pago 30 Kama; 101701B-230 text: 1; PFOA XC101501-3,250 ppt standard 1017(31B-230Sm(Mn.2x2) 10Ch 18-0ct-2001 16:56:01 LC/MS/MS #7 MRM of I Channel ES- 5.' 8 413 > 369 1.48e5 %- (^ r. i. i. 2.00 4.00 3.00 5.0 0- I- r----.-r-r-.-- . . , . . . 1 l . . l l-l--------. . | l l . l 1 T-. t-r-, 1 . l 1 1 |-|T 0 i 11 1 111 1--. i i 6.00 7.00 >, . iTime 8.00 Exygan Rasaarch RJZ032661 EID185135 Quantify Sampio Ropoart: Study Ho.: 008-046, Set Ho; 101701B, 2xt. Date: 1.0/17/01, Analyst: K Risha Sample List: Laat. modified: Mothod: Last modified: Job Code: P:\Data\lQ'lSMS7\Ma33lynx\008-046.EBO\SampleDB\101701b fri Oct 19 07:07:33 2001 P:\Data\LCMSMS7\lto3slyox\008-04S.PRO\HethDB\10160l EE'OA Wed Oct 17 07:42:45 2001 Printad: Exi Oct 19 07:15:16 2001 Page 31 Kama; 101701B-231 Text; 1: PFOA. 0112728 1017C31B-231 Sm (Mn. 2x2) 100-i 18-0ct-2001 17:12:36 LC/MS/MS #7 MRM of 1 Channel ES- 5. )a 413 > 369 4.07e5 %- 0- 2.00 3.00i--' 4.00 5.{00 6.00 7-00 8.00iiinc ' ' ' l ' ' ' ' i-- ' i ' ' l i ' i ' ' ' l' ' ' ' ' ' ' l '--' ' l ' ' ' ' l ' ' ' l ' i ^ '-1 Exygon BBsaarch RJZ032662 EID185136 Quantify Saapla Report Study Ho.: 008-046, Sat No: 1017013, Ext. Data: 10/17/01, Analyst.: K Risha Sample List: Last modifiod: Method; Lagt nodiflad: Job Code: P;\Data\:LCMSHS7\Ma33lynx\008-046.ERO\SaiBpleDB\10l701b Fri Oct 19 07:07:33 2001 P;\Data\I.afflHS7\Ma33lynx\008-046.ERO\MethDB\101601 PFOA Wed Oct 17 07:42:45 2001 Printed.; Kci Oct 19 07:15:16 2001 Page 32 Nama: 101701B-232 'text: 1: PFOA 0112728 Dup 1017(D1B-232 5m (Mn. 2x2) 10(h 18-0ct-2001 17:29:18 LC/MS/MS #7 5. >7 MRM of 1 Channel ES413 > 369 4.02e5 %- 0- ' i' i '' ' i ' ' i - 2.00 3.00 1i' '' i'' 4.00 ' ' i ' ' '' i 5.0 0 i ' 11 r< 6.00 ' i' ' ' 7'.,00 i >' ' ' iTime 8.00 Exygen Rasearch RJZ032663 EID185137 Quantify Sanpla Rnport Study No.: 008-046, Sal: Ho; 101701B, Ext. Data: 10/17/01, Analyst: K Risha. Sanpla List: Last. modified; Method: last modified; Job Coda: P:\Data\KMSHS7\Ma33lyox\008-046.PKO\SaB.pleDB\10170Ib B-ri Oct 19 07:07;33 2001 P:\Data\LCMSMS7\fclaa3lynx\008-046.PRO\MethDB\10l60l PFOA Wed Oct 17 07:42:45 2001 Printed; Erf. Ocfc 19 07;15:16 2001 Page 33 HaMe: 101701B-233 rext: 1; PFOA 0112 729 1017(01B-233Sm(Mn.2x2) 100-1 18-0ct-2001 17:45:53 LC/MS/MS #7 3, 17 MRM of 1 Channel ES413 > 369 3.33e5 %- 0- ' ' , ' 1 ' ' , 1 ' 1 1 1' 1 1' 11 , ' ' i ~' ' ' ( '''---- 1 ' ' ' 1 ' ' 1 > 1 1111C 2.00 3,00 4.00 5.00 6.00 7-00 8.00 Exygen Rasaarch RJZ032664 EID185138 Quantify Sampla Report Study Ho.: 008-046, Sat Ho; 101701B, Ext. Data: 10/17/01, Analyst: K Bxaba Sample List: Iist modi.f3.ed; Method; I>a3t aodified: Job Coda; P:\Data\lCMSMS7\,Ma33lynx\OOa-046.PB.O\SainploDB\l01701b Fri Oct 19 07; 07; 33 2001 P:\Data\I.CMSMS7SMas3lyn3c\OOB-046.BEO\MothDB\101601 PFO& Wed Oct 17 07;42;.45 2001 Printed: Fci Oct 19 07:15:16 2001 Pago 34 Name: 101701B-234 Taxt: I: PFOA 0112729 Dup 1017C)1B-234Sm(Mn.2x2) lOO-i 18-0ct-2001 18:02:34 LC/MS/MS #7 MRM of 1 Channel ES- 5J 8 413>369 3.36e5 / %- 0- ' ' ' ' i ' ' ' t 2.00 ' i ' t --- 3.00 i 'i ' 4.00 ' . ' ' '' i 1 5.0(0 ' ' 1 ' * *I ' 6.00 ' ' ' I ' * l "I ' ' 7.00 ' ' ' ' t 1 llllc 8.00 Exygnn Raaaarch RJZ032665 EID185139 Quantify Saapla Raport Study No.: 008-046, Sot Ho: 101701B, Ext. Dato: 10/17/01, Analyst: K Riaha Sampla List: Laat modifiod: Method: Laat modified: Job Code; P:\Bata\IySHS7\Mas3lynx\OOB-046.PRO\SaBpXeDB\101701b Eci Oct 1,9 07:07 33 2001 P: \Data\LCMSMS7\Massl.ynx\008-OA6. PK3\MethDB\101601 PFOA Wed Oct 17 07:42:45 2001 Printed; Fri Oct 19 07:15:16 2001 Pago 35 Hama: 101701B-235 Text: 1: PE-OA XC1C)1501-4, 500 ppt standard 1017C01B-235Sm(Mn,2x2) 10(h 18-0ct-2001 18:19:15 LC/MS/MS #7 MRM of 1 Channel ES- 3j 38 413 > 369 3.21e5 %- 0- ' ' ' ' 1 - ' ' 1 ' ' ' ' 1 > 1------'" 1 i i i ' 1 3.00 4.00''>'----'-T 6.00 2.00 liiire '' ' ' 1 ' '' ' ' 1 ' ' ' ' 1 ' ' ' ' i ' ' ' ' 1 ' " -- 5.00 7.00 B.OO Exygen Kosaarch RJZ032666 EID185140 Quantify Sample Roport Study Ho.: 008-046, Sat Ho: 101701B, Bxt. Data: 10/17/01, Analyst: K Riaha Sample :Liat: Last modified; Mathod: I^sfc nodi-fied: Job Coda: P:\Data\lQISMS7\Ma3alynx\008-046.PRO\3aiiipl.eDB\101701b Fri. Oct 19 07:07:33 2001 P:\Data\LQlSMS7\Ma33lynx\008-046.PKO\MathDB\101601 PFOA Wed Oak 17 07:42:45 2001 Printed: Pri Oct 19 07:15:16 2001 Paga 36 Mama: 101701B-236 Toxt: 1: PFOA XC101S01-5.1000 ppt standard 1017 01B-236Sm(Mn.2x2) lOO-i IB-Oct-2001 18:35:54 LC/MS/MS #7 MRM of 1 Channel ES- 5. ^ 413 > 369 6.37e5 %- 0- 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen R3tiarch RJZ032667 EID185141 899zeoz.ra Zt'Tssxaia i l ^ ^"-^"Ss'^i Ex^y/ een C^'1"6'^ RESEARCH m.k. Precise Research. --. Proven Results. The following pages are exact copies of 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 (ED # S070901-1) which in turn, was used to make intermediate solutions (TOTs F070901-1, F070901-2 and F070901-3). These intermediate solutions 'are used to prepare extracted calibration standards, laboratory control samples, and matrix spike samples. Pentadecafluorooctanoic acid (Inventory #:01-008-092), obtained from Fluorochem USA (lot # U14D) was used to make a stock solution (ID # S101501-1) which in turn, was , usedtomakemtermediatesolutions(ID#'sFl(>1501-landF101501-2). These intermediate solutions are used to prepare the check standard, which is designed as an independent source verification of.the calibration standards. The information on the following pages provides the exact sources, lot numbers, shipping information, expiration dates and storage conditions of the neat standards. Also included are the preparation of stock standard and fortification solution forms. These pages show the exact details of the preparation of each of the stock and fortification solutions, as well as their expiration dates and storage conditions. 4^i>itf^ Research Drive -- ^StateCollege,PA 16601, USA J: 814.272.1039 F: 814.231.1580 exygeiuxini EID185143 RJZ032669 Centre Analytical Laboratories. 3018 RiiaaanA Drtv PlIOTO: (8141 231-B032 Inc. Staf CoBooa. PA 16B01 Fax: (814) 231-1253 01 (814) 231-15a<> ANALYTICAL TEST, CONTROL AND REFERENCE STANDARDS RECEIPT & INVENTORY LOG Substance: PaATM^TLOEOOCTAUp\C AaK Page Centre Analytical Inventory Number. Amount Received (g): fi^ Ctl-OOft-IS 0 Gross Weight Received (g): ^LSMil.S^42. Date Received: tntoslol Condtlon Upon Receipt Ffozen-Refrigerated-^n^fenO Received Frnm! ftl-^^fU frip^ Lot/Batch No.: OaSlbtsP Date Last Characterized 1. UA 2. 3. ________ Exoirallon Date {n{(K\GZ. % Purity %1o Soituoriaaygae iununuaalninunn:- jFEfcESERBftSiMrtAgkaBlMETAS .i*^.t-- KJI Logged In By. Q/^ fl^O Date: Initials/Date ^Mfosfcl (nioshi Date inhiM Initial GrossWt (g) S^sSa. Amount Withdrawn (9) o.oiot?. Gross Wt After Withdrawal (g) ^.Wit- Balance ID V Purpose/CAL Study Number OOQ-O^b Initials ^ Comments: lDEt6nrM1e^<lffi^^t^6ect6(^llAle-^ D Removed froni Inventory D Returned to Sponsor D Log continued next page THIS tS AN EXACT COPY OF THEORIGINAL DOCUMENT.' m K|g nA-rc Ijj^lot (inittab/Oala) (inlBals/Dala) 8 Fabtuary 2001/4 RJZ032670 EID185144 ,s 10 - 0) o a . 2 SI 0 l ^ 3 8 0 ^ 5CQ a C: i5 .2 "t5^B ^ >-- a 0 . %<s 0 k|j|jj ?>* u t5 ^ u SMM Ml H ^j lif ^^M a w 11 5? $ p 1 O? S CC a: a UJ 0- UJ i-^ Q .5) E (0 |g r* 0 0 cc ss 5 0. 0 0 1|11 ^ g S. s^< 1(M11 P? (- 0 0 m 1-W 3 i 3 ocow 0} T:U. Q ^ 5? EC tO 111 0 UlQ o' |^ " 0 | ctf &F 0 a. S 0 ?" h* 5 ?3 "5 ^d i 7 S" I ?^ o e I8 Q ^ i$ , P 0 'tg5 1 |1| fe< tSl2 a) T3 0^ 3 "~ o- ? S a (o <- ff S t= u0 - u? Eg I11 as." + 3: 5 ? s s? 3 x t0 3 Z S T 2. 0 S? .? ". c? S S CM a z *,- 1 S-1 1- n. ^ ^3 "| z c i 5 i 3 n. U <B a. m "S'3 <o ic ; ^itt00 THIS IS AN EXACT COPY OF THE ORIGINAL DOGUMEMT." BY-_-A__DATEjiteL RJZ032671 EID185145 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax:814-231-1580 ANALYTICAL TEST, CONTROL AND REFERENCE STANDARDS RECEIPT & INVENTORY LOG I^iU)6a6flCWlai6. Substance: PEHTAMKAmjOROOCrWoVCto^OK- ^ CPFoM Page _l__ Exygen Inventory Number: 0 \ - QOB- Cfl'2.__________________ Amount Received (g): ^5____ Gross Weight Received (g): IS-^ll Date Received: )ftJP^Ol Condition Upon Receipt: Frozen-Refrigerated^Ambfen^) Received FrQm:^^^^^^ \f&f\ Lot/Batch No.: U-l4b______ Date Last Characterized i. uu^bu3u~ 23. ..__________ Expiration Date , loialD^-' ________ % Purity ^n^ _______ Initials/Date . ^11 w. i"N~ oi - Storage Location: MMtJ-R'bfMJHtJ ^2. (.VS. \) ^^W/\!U' Logged In BE^y: lf/^!W^W^!U'_________ -^y^U.j:/^-^ ... >,, , ^>^/ry- Standard C ustodian Review/^uli-. ^v ( Gross Wt Date: Mlol2lZ-|bt)l > Ds^:IC^OI Date Initial Amount After Balance Purpose/Exygen GrossWt. Withdrawn Withdrawal ID (g) (g) (9) - Study Number lohsfbl tS-62ol4- 0.01051 15.60300 Ife Oo8-o^ H/ot/ot^,^!^ ---- ----- ^ TA^^W>e.u Initials ^ C-6- Comments: D Removed from Inventory D Returned to Sponsor D Log continued next page THIS IS AN EXACT COPY OF THE OBIGIMAL DOCUMENT." BY ^ njrc ^|ftfi|f)l (initials/Date) (Initials/Date) 15 August 2001/5 RJZ032674 EID185147 Centre Analytical Laboratories, Inc. 3048 Research Drive Slate College, PA 16801 Phone: (814) 231-8032 Facsimile: (814) 231-1253 Page PREPARATION OF STOCK STANDARD SOLUTION Protocol Number: CAL Study Number: 006-0%- C-^rre->(rW)@^-lll'5H Compound: PEUTW-CftO .HnRf>nC.T^Ol6 ftC-lh Lot Number: 6B?>I^O Source: >W\m Purity: th Date Standard Received: ollostol % Date Last Characterized: _|4l Storage Location: STAML^ CAftlblCT A3 Compound Expiration Date: mlbSJOi- CAL lnventoiy #: .01- 006-15 A calibration check must have been conducted with ihe balance on the day of sample weighing. Balance Calibration Stock Solution Balance Number: Logbook page for calibration data: T Net Wt. of Substance: .0.0104-2. g Wt. Adjusted for Purity: 6-btOOO g Solvent: teriftHOL. Manufacturer: EtASa'E^tE Lot Number: UwS Fmal Volume:, lt)D Concentration: 160 _mL _u.g/mL Stock Solution Expiration Date* WfA\02, S0^6|- Stock Solution ID: ------------------ Stock Solo ID #: SMMDDYY-1,23,etc. * Assign a one year expiration date for all stock solutions unless otherwise indicated bv sponsor. Freezer Number: Storage Conditions for Solution: "" Refrigerator Number: ^ Room Temperature: ~ Indicate which of die above is applicable,and location. REMARKS: Signature: r\fffiS^lM\ .Dote: 0'J^JOS Novembers, 1996/3 THIS IS AN EXACT COPY OF THE ORIGINAL DOCUMENT.' BY ___g__DATE-JlMN- RJZ032677 EID185148 Centre Analytical laboratories. Inc. 3048 DriveStale Research Phone; (814) 231-8032 College. PA 16801 Facsimile: (814) 231-1253 Page. PREPARATION OF FORTIFICATION STANDARD SOLUTIONS Protocol Number:_____r______ Date Prepared: Dllo^Ol CAL Study Number: 006 "0% Expiration Date*: 02|&^\Vt- *Assign a one year expiration date for all dilutions unless otherwise indicated bv sponsor. Separate sheets should lie wed for fortification standards and calibration standards. Dilution of solution IDS Compound (code no.) . Initial Cone. WmL) Aliquot volume (mL) Diluted to volume (mL) Solvent (or solvent number) Pina) conc. (|iS/inL) Final solution IDff" 60-Mol-l loo - A ^ FWtot-1 l.D Fo-lo^ol-3. 6. 1 -t-- -~ -- - -^ -- -- - - 1.0 10.0 Ib.O -- - - - 100 100 100 -- -- - lA<ort ^ r -- -- - 1.0 O.I 0.01 ~ - - Fo^ol-l F070101-2 Fo-TO^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: >Am<JoL. . Manufacturer: SW^MCE Lot No.: 41t)2S' Solvent!: ___~ Solvent 3: Manufacturer: ~~ Manufacturer: Lot No-: Lot No.: ** This must be a miqve number. Use this system: Fortification Soln ID If: FiWDDYY-f.2.3, etc. Storage Conditions for Solution: Freezer Number. - Refrigerator Number: 13 Room Temperature: Indicate whicb of the above is applicable,and location. REMARKS: (3>^llio5lo\ Signature: (J^M^^ Date: QllfiQ/.QI February 1995/2 THIS IS AN EXACT COPY OF THE ORIGINAL DOCUMENT.' BY___X----OATE-iiNL RJZ032678 EID185149 'iP^ni" '""A^ c H 3058 Research Drive state collee^ p^16801 Phone: 814-272-1039 Fax: 814-231-1580 Page. PREPARATION OF STOCKSTANDARD SOLUTION Protocol Number: NA_______. Exygen StudyNumber: 066-0% tteN Compound:T^^R.UbR.OCQM^ fC^ tfw) Lot Number: -N5^ U.l4b Source: rl-U^DCriEM Purity: ^l u9\ Date Standard Received: . i >D|l2-jO\ % Date Last Characterized: ^A Storage Location: iSTM^.^AB-H.1 S. Compound Expiration Date: l&(t'2-lP2- Exygen&iventorYtf: O^-OtB'-O^ A calibration check must have been conducted with the balance on the day of sample -weighing, BDalIanc-e rCia^liinb,r^a*t;i--on. Stock Solution Balance Number Logbook page for calibration data: ib_____ /_____ Net Wt of Material: 6.btD3| g Wt Adjusted for Purity: 0>t>i000 g Solvent: hErak^OL-_____ Manufacturer E-MSaE^CJS Lot Number: 4t2.KZ-______ Final Volume: Concentration: ^0_____mL 100_____ug/mL Stoivcak. Suuotluu.Ltii.ounii Expiration Date*: ^l.^.. L1l--o',T'^-"' Stock Solution ID: S IQISOl - 1 --,,,,---- -- -- ... - - -- __ _ ^.-,.,- r_._______ ^ StockSolaIDS: SMMDDYY-l^.etc. * Assign a one year expiration date for all stock solutions unless otherwise indicated by sponsor. Freezer Number: Storage Conditions for Solution:_________ "' Refrigerator Number: & Room Temperature: Indicate which ofthe above is applicable,and location. REMARKS: Signature: Q/N^ Date: w lp|l5lol July 1?, 2001/4 THIS IS AN EXACT COPY OF THE ORIGINAL DOCUMENT.' WH nA-reAN- RJZ032679 EID185150 Exysen ^/ (^RERSEESEAARRCH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Page. PREPARATION OF FORTIFICATION STANDARD SOLUTIONS Protocol Number: N^_______ Bxygen StudyNumber: i^B-o^L Date Prepared: lb|lslt?l_______ Expiration Date*: O^kz____ *Assign a one year expiration date &r all dilutions unless otherwise 'indicated by sponsor. Separate sheets should be usedforfortification standarck and calibration sttmdwds.____ Dilution of solution E> 6tol5M-l PU)t'7t)\-l Compound (code no.) m PRA Initial Cons. (>lgfaL) 100 l.O ^. -, -> ^^ --. -- -- -- -- Aliquot volume (n>L) 1.0 lb.0 --. -- -- ---- ---- Diluted to voluma (inL) loo loo -- -- ^ -- -- Solvent (or solvent number) NW l^.ori -- -~ -- -- -- Final cone. (|ig/mL) 1,0 O.I -- -- ,-- -- ----~ Final solution ID** F101501-1 FlOlSOl-Z F ~ F - F -- p -- 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: NteTUM^oL Manufacturer: &^SQE^CLotNo.: 4120-2. Solvent!: ___^_____ Manufacturer: Solvents: Manufacturer: '" LotNo.: LotNo.: ** This must be a unique number. Use this system: Fortification Soln ID : FUMDDYY-1,2.3, etc. Freezer Number:. REMARKS: Storage Conditions for Solution: Refrigerator Number: 13 Room Temperature: Indicate which of the above is applicable,and location. Signature.: ( y ^ ^ . Date: KfelDt My 16,2001/3 THIS IS AN EXACT COPY OF ^ - THE ORIGINAL DOCUMENT.' RY nATF |OB|D| RJZ032680 EID185151 Barley Mitt Plaza. Building 27_____:_____Lancaster Pike & Routs 1*1_____;_____WBmington. DE W805 RJZ0326B1 EID185152