Document 5k6a11VXo1v6NNJQxwVN5eo8R

DownloadViewSend us a messageRandom document
Precise Research. Proven Results. J tfk dunefltS Analytical Report Fluorochem ical Characterization of Filter Samples Particle Size D istribution Study 3/04 Exygen Research Laboratory Report No. L0002178 Testing Laboratory Exygen Research 3058 Research Drive State College, PA 16801 Requester Michael D. Aucoin URS Corporation Barley Mill Plaza Bldg 27 Room 1260 Lancaster Pike and Rt 141 Wilmington, D 19805 PeVra3 CD PAGE 10F 5 1 Introduction ---------Results are -reported for the analysis of filterr samples received by Centre Analytical Laboratories, Inc. (dba Exygen Research) (Exygen) from DuPont Corporation. This report presents results assigned to Exygen Research study number L0002178. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) was requested for all samples. A total of 29 samples were received for analysis. The samples were prepared and analyzed by LC/MS/MS for the following list of fluorochemicals: Table 1: Target Analysis Compound Name Perfluorooctanoic Acid Acronym PFOA 2 Sample Receipt The samples were submitted in individual plastic containers, at ambient temperature. Samples were collected on 3/25/04 and 3/26/04 and were received on 3/27/04. Chain-of-custody information is presented in Attachment C. 3 Holding Times The analytical method used was validated against a maximum holding time of 14 days in water samples. There are no validated holding times for filter papers. All samples were analyzed within 14 days of collection. 4 Methods - Analytical and Preparatory 4.1 LC/MS/MS 4.1.1 Sample Preparation for LC/MS/MS Analysis PFOA was extracted from the filter by shaking overnight with 40 mL of reagent grade water. The water was removed from the sample by filtration and transferred to a 50 mL centrifuge tube for subsequent cleanup and concentration of the extract. Solid phase extraction (SPE) was used to prepare the samples for LC/MS/MS analysis. The entire 40 mL extract was transferred to a C18 SPE cartridge. The cartridge was eluted with 40% methanol: water. The eluate was discarded. The cartridge was then eluted with 100% methanol. A 5 mL portion of methanol was collected for analysis by LC/MS/MS. This treatment resulted in an eight-fold concentration of the samples prior to analysis. PAGE2 OF5 000578 4.1.2 Sample Analysis by LC/MS/MS A Hewlett-Packard HP1100 HPLC system coupled to a Micromass Ultima MS/MS was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Samples were extracted on 4/3/04 and analyzed between 4/4/04 and 4/7/04. Raw analytical data can be found in Attachment D. 5 Analysis 5.1 C alibration A 6-point calibration curve was analyzed at the beginning of the analytical sequence and throughout the run for the compounds of interest. The calibration points were prepared at 25, 50, 100, 250, 500, and 1000 ng/L (ppt), as perfluorooctanoic acid (PFOA). The instrument response versus the concentration was plotted for each point. Using linear regression with 1/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determination (r2) were determined. A calibration curve is acceptable if r >.0.992 (r2 > 0.985). Calibration standards for MS/MS analysis were prepared using the same SPE procedure used for samples. For the results reported here, calibration criteria were met. 5.2 Blanks Extraction blanks were prepared and analyzed with every extraction batch of samples. The extraction blanks should not have any target analytes present at or above the concentration of the low-level calibration standard. For these samples, the extraction blanks were compliant. Instrument blanks in the form of clean methanol solvent were also analyzed after every highlevel calibration standard, and after known high-level samples. Again, the blanks should not have any target analytes present at or above the low-level calibration standard. For the samples presented here the instrument blanks are compliant. 5.3 Surrogates Surrogate spikes are not a component of the LC/MS/MS analytical method. 5.4 M atrix Spikes / laboratory Control Samples Matrix spikes were not prepared for these samples; however, two blank filter papers were spiked at 2 levels and analyzed for PFOA. Acceptable recoveries were set at 70-130%. Sample recoveries were within the acceptable range. Matrix spike recoveries are given in Attachment B. 5.5 Duplicates Sample duplicates were not performed for this study. PAGE3 OF5 C0 0 5 7 9 5.6 Sample Related Comments Two analytical runs were performed to complete the sample analysis. The following is a brief quality control narrative for each run. A nalytical-------Samples Analyzed------------------------ - Comments Run Number 040304 A WWK-A-E1-S1-1, WWK-A-E1-S1-2, WWK-A-E1-S1-3, WWK-A-E1-S1-4, WWK-A-E1-S1-5, WWK-A-E1 -S1-6A, WWK-A-E1 -S1-6B, WWK-A-FBLK1, WWK-A-E1-S2-1, WWK-A-E1-S2-2, WWK-E1-S2-3, WWK-A-E1-S2-4, WWK-A-E1-S2-5, WWK-A-E1-S2-6A, WWK-A-E1-S2-6B, WWK-A-E1-S3-1, WWK-A-E1-S3-2, WWK-A-E1-S3-3, WWK-A-E1-S3-4, WWK-A-E1-S3-5, WWK-A-E1-S3-6A, WWK-A-E1-S36B, WWK-A-E1-S5-1, WWK-A-E1S5-2, WWK-A-E1-S5-3, WWK-A-E1S5-4, WWK-A-E1-S5-5, WWK-A-E1 S5-6A, WWK-A-E1-S5-6B All samples except WWK-A-FBLK-1 require additional dilution. All other data is useable. r 040304 AR WWK-A-E1-S1-1, WWK-A-E1-S1-2, All data is useable. WWK-A-E1-S1-3, WWK-A-E1-S1-4, WWK-A-E1 -S1-5, WWK-A-E1 -S1-6A, WWK-A-E1 -S1-6B, WWK-A-E1-S2-1, WWK-A-E1-S2-2, WWK-E1-S2-3, WWK-A-E1-S2-4, WWK-A-E1-S2-5, WWK-A-E1-S2-6A, WWK-A-E1-S2- 6B, WWK-A-E1-S3-1, WWK-A-E1- S3-2, WWK-A-E1-S3-3, WWK-A-E1- S3-4, WWK-A-E1-S3-5, WWK-A-E1 - S3-6A, WWK-A-E1-S3-6B, WWK-A- E1-S5-1, WWK-A-E1-S5-2, WWK-A- E1-S5-3, WWK-A-E1-S5-4, WWK-A- E1-S5-5, WWK-A-E1-S5-6A, WWK- A-E1-S5-6B 6 Data Summary Please see Attachment A for a detailed listing of the analytical results. All results are reported as ug / filter as PFOA. PAGE4 OF5 cn o n so 7 Data/Sample Retention Samples are disposed of one month after the report is issued unless otherwise specified. All -- electronic data is archived on retrievable media- and hard copy reports-are- stored in data folders maintained by Exygen. 8 Attachments 8.1 Attachment A: Results 8.2 Attachment B: Matrix Spike Recoveries 8.3 Attachment C: Chain of Custody 8.4 Attachment D: LC/MS/MS Raw Analytical Data 8.5 Attachment E: Standards Data 9 Signatures Kevin J Lloyd, Vice President Other Lab Members Contributing to Data Karen Smith Date Date PAGE50F5 CROSSI Particle Size Distribution Study 3/04 DuPont Sample Identification PFOA (ug/ filter) WWK-A-E1-S1-1 WWK-A-E1-S1-2 W W K-A-E1-S 1-3 W W K-A-E1-S 1-4 WWK-A-E1-S1-5 WWK-A-E1-S1-6A W W K-A-E1-S 1-6B WWK-A-FBLK1 WWK-A-E1-S2-1 W W K-A-E1-S 2-2 WWK-A-E1-S2-3 W W K-A-E1-S 2-4 W W K-A-E1-S 2-5 W W K-A- E1-S2-6A W WK-A-E1-S2-6B WWK-A-E1-S3-1 WWK-A-E1-S3-2 W W K-A-E1-S 3-3 WWK-A-E1-S3-4 WWK-A-E1-S3-5 WWK-A-E1-S3-6A WWK-A-E1-S3-6B WWK-A-E1-S5-1 WWK-A-E1-S5-2 WWK-A-E1-S5-3 WWK-A-E1-S5-4 WWK-A-E1-S5-5 WWK-A-E1-S5-6A WWK-A-E1-S5-6B 4.28 9.64 5.44 5.12 3.76 14.6 11.1 NQ 23.1 76.0 48.8 30.3 3.40 239 145 18.8 64.8 58.8 36.2 35.2 240 106 1.26 1.65 1.41 1.37 1.37 6.60 4.88 Limit of Detection (LOD) for the procedure is appoximately 0.0004 ug/filter Limit of Quantitation (LOQ) for the procedure is 0.002 ug/filter i ND - Compound not detected NQ - Compound detected at a level between the LOD and LOQ. Result is not quantifiable. ND < LOD < NQ < LOQ J liu O fro 1 J ^ 3 03055i8 Research Drive # m s taSt1ate College, PA 16801, USA VT: 814.272.1039 F: 814.231.1580 exygen.com Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: Spiked Amount (ng/L): Slotted Paper Spike A 50 Ipfa Sample Concentration (ng/L) 0 Matrix Spike Result (ng/L) 44.5 Matrix Spike Result earn 89.0 Criteria (Pass / Fail) PASS Lower Recovery Limit: 70 Upper Recovery Limit: 130 Concentrations represent amount present in the sample extract 7 0 0 0 5 8 3 Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: Spiked Amount (ng/L): | W hatman 41 Spike B 50 [PFO Sample Concentration (ng/L) 0 Matrix Spike Result (ng/L) 52.7 Matrix Spike Result earn 105.4 Criteria (Pass / Fail) PASS Lower Recovery Limit: 70 Upper Recovery Limit: 130 Concentrations represent amount present in the sample extract oUU CO0 5 8 4 Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: Spiked Amount (ng/L): Slotted Paper Spike C 500 IPFOA Sample Concentration (ng/L) 0 Matrix Spike Result (ng/L) 437 Matrix Spike Result earn 87.4 Criteria (Pass / Fail) PASS Lower Recovery Limit: 70 Upper Recovery Limit: 130 Concentrations represent amount present in the sample extract 9 C095S5 Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: Spiked Amount (ng/L): | W hatman 41 Spike D 500 IPFOA Sample Concentration (ng/L) 0 Matrix Spike Result (ng/L) 399 Matrix Spike Result earn 79.8 Criteria (Pass / Fail) PASS Lower Recovery Limit: 70 Upper Recovery Limit: 130 Concentrations represent amount present in the sample extract a O O c c o rs G 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax:814-231-1580 .ogin -ogin onrorm ample: Project: P0000729 Conform COC: Conform Sample Company Name: DuPont de Nemours & Co, Inc. Conform Request: Submitted By: Michael D. Aucoin Login Type: Immediate Receipt of Samples Started: T Date Start: 03/29/2004 Due Date: 04/12/2004 Received Date: 03/27/2004 Received By: AMMERMAN, MARK Spread Sample: Label: Project Title/Type: Analysis of PFOA in Filter Paper (Particle Size Distribution Study) / ROUTINE Exygen SD/PI: RISHA, KAREN Login Notes: Conform Notes: l rue True TrueTrue Package PK0002812 Carton Packages / Containers Mail Date / Condition S hipper/ ID 3/29/2004 12:53:46PM Package & Contents Uncompromised FEDEX 8443482884530200 Temp. Control/Temp. None 23.3 Direction / Handled By RECEIVED AMMERMAN, MARK Container # C0030028 C0030029 C0030030 C0030031 C0030032 C0030033 C0030034 C0030035 C0030036 C0030037 C0030038 C0030039 C0030040 C0030041 C0030042 C0030043 C0030044 C0030045 C0030046 C0030047 C0030048 C0030049 C0030050 C0030051 C0030052 C0030053 C0030054 C0030055 C0030056 3/29/2004 Login.rpt Gross W eight 16.3 g 16.3 g 16.3 g 16.3 g 15.9 g 19.1 g 18.9 g 15.9 g 16.2 g 16.3 g 16.3 g 15.9 g 15.9 g 19.1 g 18.8 g 16.2 g 15.9 g 15.9 g 16.2 g 16.3 g 18.8 g 18.7 g 15.9 g 16.2 g 16.3 g 15.9 g 16.3 g 19.1 g 18.9 g pH Container Type 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic 50 ml clear plastic Preservative NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE Mfg. Lot j 01 1 R eport V ersion: Mar 11 2004 4:16PM Page 1 of 3 Instance: C-005S7 Mfg. ID R0093077 R0093077 Login Sample ID L0002178-0001 Container C0030028 L0002178-0002 C0030029 L0002178-0003 C0030030 j* L0002178-0004 C0030031 L0002178-0005 C0030032 L0002178-0006 C0030033 L0002178-0007 C0030034 L0002178-0008 C0030035 *" L0002178-0009 C0030036 L0002178-0010 C0030037 L0002178-0011 r C0030038 ' L0002178-0012 C0030039 L0002178-0013 C0030040 L0002178-0014 C0030041 ... L0002178-0015 C0030042 L0002178-0016 .... L L0002178-0017 C0030043 C0030044 L0002178-0018 C0030045 L0002178-0019 C0030046 .. L0002178-0020 C0030047 3/29/2004 Login.rpt Matrix SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID Fraction Filter Paper Samples Sample WWK-A-E1-S1-1 Date Sampled Pate Received 03/26/2004 03/27/2004 Date Due 04/12/2004 Filter Paper WWK-A-E1-S1-2 03/26/2004 03/27/2004 04/12/2004 Filter Paper WWK-A-E 1-S1-3 03/26/2004 TJ3727/2004 04/T2/2004 Filter Paper WWK-A-E 1-S1-4 03/26/2004 03/27/2004 04/12/2004 Filter Paper WWK-A-E1-S1-5 03/26/2004 03/27/2004 04/12/2004 Filter Paper WWK-A-E1 -S1-6A 03/25/2004 03/27/2004 04/12/2004 Filter Paper WWK-A-E 1-S1-6B 03/26/2004 03/27/2004 04/12/2004 Filter Paper WWK-A-FBLK1 03/26/2004 03/27/2004 04/12/2004 Filter Paper WWK-A-E1-S2-1 03/26/2004 03/27/2004 04/12/2004 Filter Paper WWK-A-E1-S2-2 03/26/2004 03/27/2004 04/12/2004 Filter Paper WWK-A-E1-S2-3 03/26/2004 03/27/2004 04/12/2004 Filter Paper WWK-A-E 1-S2-4 03/26/2004 03/27/2004 04/12/2004 Filter Paper WWK-A-E 1-S2-5 03/26/2004 03/27/2004 04/12/2004 Filter Paper WWK-A-E 1-S2-6A 03/25/2004 03/27/2004 04/12/2004 Filter Paper WWK-A-E 1-S2-6B 03/26/2004 03/27/2004 04/12/2004 Filter Paper WWK-A-E1-S3-1 03/26/2004 03/27/2004 04/12/2004 Filter Paper WWK-A-E 1-S3-2 03/26/2004 03/27/2004 04/12/2004 Filter Paper WWK-A-E 1-S3-3 03/26/2004 03/27/2004 04/12/2004 Filter Paper WWK-A-E 1-S3-4 03/26/2004 03/27/2004 04/12/2004 Filter Paper WWK-A-E1-S3-5 03/26/2004 03/27/2004 04/12/2004 J 0 1 2 Report Version: Mar 11 2004 4:16PM Instance: Page 2 of 3 CC05S8 R0093077 *^s ogin L0002178-0021 L0002178-0022 L0002178-0023 C0030048 C0030049 C0030050 SOLID SOLID SOLID Filter Paper WWK-A-E1-S3-6A Filter Paper WWK-A-E1-S3-6B Filter Paper WWK-A-E 1-S5-1 L0002178-0025 L0002178-0026 L0002178-0027 L0002178-0028 L0002178-0029 C0030051 C0030052 C0030053 C0030054 C0030055 C0030056 SOLID SOLID SOLID SOLID SOLID Filter Paper WWK-A-E 1-S5-3 Filter Paper WWK-A-E 1-S5-4 Filter Paper WWK-A-E1-S5-5 Filter Paper WWK-A-E 1-S5-6A Filter Paper WWK-A-E 1-S5-6B 03/25/2004 03/27/2004 04/12/2004 03/26/2004 03/27/2004 04/12/2004 03/26/2004 03/27/2004 04/12/2004 wU/i.V/1i.UU'1 03/26/2004 03/27/2004 04/12/2004 03/26/2004 03/27/2004 04/12/2004 03/26/2004 03/27/2004 04/12/2004 03/25/2004 03/27/2004 04/12/2004 03/26/2004 03/27/2004 04/12/2004 _ 3/29/2004 Login.rpt 001 3 Report Version: Mar 11 2004 4:16PM Instance: Page 3 of 3 C0 0 5 8 9 R0093077 R0093077 P LU CHAIN OF CUSTODY/ANALYSIS REQUEST FORM RESEARCH Exygen Research Sample Receiving *3117 Research Drive State College, PA 16801, USA T: 814.231.8032 F: 814.231.1580 exygenresearch.com Page -J -S PROJECT INFO RM ATION C lient (nam e & adc ress): Project M anager (Name & E-mail Address): P l'icss - A*/ \ f `T3k , A s \ fL k <k9A S ,, A J U f * J _____ -L/i ' GI %< Phone: ( j o h ) <n6>3 ~ L-N7G Fax: S a m p le r: S &JP/P--7,----A---- -P--i-e-r-r-e-_--_--_--_--_--_--_-- Ari ( 3 3) t o l l e n Project Nam e/ . . ' ic i s S>72e t s f r ' o tA i^ P.O. #: Q uotati on #: * Piease fill out this form completely to ensure correct analysis and proper handling of your samples. ANALYSES REQUESTED t*. ; I ( l) 3" Composite Number of Containers SAMPLE ANALYSIS ExyLIMS# Client Sam ale Identification Collection Collection P i Time -o(kQd_ vvk-A-E 1-S4-I wwk-A-1 A-<,1-3. / ijo4 Io04 X innS X ww k- 1r i-s i - 3 (066 X Ei-51 IdoT X V v lf- -E l- S i - S i 1o1> X v w k - A - E l-SI- fcA p r 6 1 fiS X Vvwk-yA - Z i - x - U 3bi lO0<l X - F ^ L K l 3 3$>4 Iona X Specify Matrix Comments PHvr /W 1 1 1 1 1 1 r___ A____ LL_ fv lf*r $*!kr 1 -L K X X X X X X X. CHAIN OF CUSTODY Relinquished by Date Time I1 O jif 3b6W 1i 1300 OTHER INFORMATION Cooler ID # Received by LAB USE ONLY Cooler Temp. (C) A Time w Wop PROJECT REQUIREMENTS Results Deadline: d S b rtiltrJ Laboratory Report Options: I | Sample results only Add case narrative EH Add quality control summary Add calibration summary I I Add raw data Other REV. 3-02 Em :e n R[ SEARCH PROJECT IN FO R M ATIO N CHAIN OF CUSTODY/ANALYSIS REQUEST FORM Exygen Research Sample Receiving *3117 Research Drive State College, PA 16801, USA T: 814.231.8032 * F: 814.231.1580 exygenresearch.com Page ^ Of ^f_ ANALYSES REQUESTED ri C lient (nam e & adc ress): . A M M - AP 5<rA /('ci 5 " UnfM W<s>30'A.fr\ \forkt RJt m Ph& X $ee;d /vV 6// Phone: ftpW ") Fax: Sam pler: $. Of)/? >. PttrCf Project M anager (Nam e & E-mail Address): A\ /juC/Vv i 302\ rfd' O f# Project Name: . Forilek RO. # : xir<'k ,H ^ Q uotation # : Please fill out this form completely to ensure correct analysis and proper handling of your samples. O c u IS sr-- o o SAMPLE A NALYSISExyLIMS# Client Sample Identification Collection Collection .oct Date Time O oo. -O.En) uEo ZE=UtO Specify Matrix W wk*1A* 1 v w W k -4 -i;i~ i3 ~ 2. m Io fo X \0i3 K -r I- /r lo i1? )D|5 w w K - ^ - E l- s a - A - 5 3 - ((do h ML. X iloS ]2 L li? 17 >1 <sf7^ Comments LAB USE ONLY CHAIN OF CUSTODY Relinquished by 3 * OpP v Date j1 31p d fo H Time \2 Cooler ID # Received by / Cooler Temp. (C) / J / j Time \4O 0 p ? jL 7 h J & L OTHER INFORMATI ON LAB USE ONLY f r pr? r *-" ! H" 7 r * * " i 4 >: X * X X. PROJECT REQUIREMENTS Results Deadline: M e j~L*J S 'h tr d f'd Laboratory Report Options: Q Sample results only [U Add case narrative 0 Add quality control summary 1 I Add calibration summary Add raw data IZ] Other REV. 3-02 ^riM IIN V^r L U ^ I K J U T/M NM LT i l i K tL JU tb I hUKAA RESEARCH Exygen Research Sample Receiving 3117 Research Drive State College, PA 16801, USA T: 814.231.8032 F: 814.231.1580 exygenresearch.com 3Page of N PROJECT INFORM ATION C lient (nam e & adc ress): Project M anager (Nam e & E-mail Address): AD A AP - U*rod W mJ&a M tkt, /J u Crtirs irti A Pule*} ( 3 o a ) y' - I(e9% Phone: *pA W v 1 G /tfl / 3 oh) `563- WV76 P rojectN am e: Al t / P o iX tc k 1/ ze i'sf/Y btfiio/s Cl 1 Fax: L' RO. # : S a m p le r: 5. i li.11 ----- A . / hvcV -------- -------------------- Q uotation # : Please fill out this form completely to ensure correct analysis and proper handling o f your samples. ANALYSES REQUESTED ILC O C 2 vO o n SAMPLE ANALYSIS ExyLIMS# Client Sam }le Identification Collection Collection -nQ) Date Time \a/W K ~A -1-53- I W w K -A gl-S S -a xia a l X Iq33 X w w K -A -& l~ S 3 -H wwlC- A P 1 -5 3 -S - i~l-i>3 -6/1 \odH 3 L lodS X W k ~ A - E4~53" 6 ^ lo 3 6 OO. 4J.E .q Ia uEo Ec = ZU Specify Matrix cr a Comments LAB USE ONLY CHAIN OF CUSTODY Relinquished by S O 1f 1t Date // JIX lcH 1l Time laoo OTHER INFORMATI ON Cooler ID # C P o v o b i] Cooler Temp. (C) Received by Date. Time T1la n1U l<\00 J S y ---.-.-.-.-.-.-.--.-.-.-.-.-.---------------.--- ------y-- t-- / ieo ft J LAB USE ONLY 2rt)' k. 21 X 2L X 21 PROJECT REQUIREMENTS Results Deadline: Laboratory Report Options: HU Sample results only CH Add case narrative CH Add quality control summary CD Add calibration summary I I Add raw data Other aatw pTf--a n i p yn t u . . 14 ^ prT-'"" T p--~ ----| p-------- REV. 3-02 a r - n ;-- i *-- I r r t yoe n V_|-|MIIN U l- t_Ub IUUY/AIMALYblb K tU U tb T FORM \ \ # ^ ^ rT s e a r c h Exygen Research Sample Receiving *3117 Research Drive State College, PA 16801, USA T: 814.231.8032 F: 814.231.1580 exygenresearch.com Page *j of co PROJECT INFORM ATION c\ ANALYSES REQUESTED L'- C lie n t (nam e & adc ress): is h , . , M Q / v\ AP A fr M\U\ ~ DuT-nf VrjlvVvA/, Wjfi/f Project M anager (Name & E-mail Address): M i K< A C c w ^ D Jm W V/C,2 k?*.A*ri ^ \ / Phone: ) % o a -liH l/ 0 ( W ) WSl' I M Project Name: , P /tr-ic U ,, a I I1 m rU uU -11 jU / iS Fax: S a m p le r: i>. 0 orf1. . P'^rce. RO. # : Q uotation # : CD D Please fill out this form completely to ensure correct analysis and proper handling o f your samples. H SAMPLE A NALYSISExyLIMS# Client Sam Dle Identification Collection Collection Time -Qid a OQIA . EO U \a>w K ~ A - ywk- A^v/k- A- O K O X. m o \ X. w ^U - E l-S ^ <?oi X k - A CA-5S--S X W V /k- w VVrk** A -- Str-^4 xo M M oS Specify Matrix Comments <y LAB USE ONLY CHAIN OF CUSTODY Relinquished by Date Time J . DFtip 3hdcM \d&> OTHER INFORMATI DN Cooler ID # CftooQfloJI Received b LAB USE ONLY Cooler Temp. (C) Date Time im . 2* //IV.. e rr c r a a a trr v -) t- Xx X X Z X PROJECT REQUIREMENTS Results Deadline: M iiU j Laboratory Report Options: CD Sample results only CD Add case narrative Add quality control summary Add calibration summary CD Add raw data CD Other REV. 3-02 3058 Research Drive Phone: 814-272-1039 State College, PA 16801 Fax: 814-231-1580 SAMPLE CONDITION UPON RECEIPT FORM Protocol # A >A Exvaen Studv # Date & Time Received U /A - Condition o f Samples ** 4^- f Temporary Storaqe Location UC2/LJ Initials & Date Waybill # 4 W ] Ht 2 4 H ^ /7 / { j'j y / i LIBRARY ID: V0001402-2 LABORATORY FORM 0018 S e n d e r's Name *Am ' O dd Company J U1. * c iU uktA ddre"ss *. IN ------------v - -- "'*k*p** . Citv ' wth,/'-pA Y o u r In te rn a l B Ilin g R e ftie n c e , ) m .m ta - w x / _________________________________________________ J. M a ri W V' 'State ZIP Mj Dept/Roor/Suita/Room 1* To ' , wrr**4Recipient's^ S Name 'A f it -- pr ty jPhone 3 3 1 - k )^ P Company A dd re ss ill7 To'HOLD' etFedExlocate n,print FedExaddress. Disc s ' - ' ' We cannotdelwarto P.Q. boxesor P.Q.ZIPcodes. Address City w S A CiiaY Ms ta te 443 43A fl453 Dept/Fkrar/Suite/Roorn zk 16901 Recipient's Copy 4a Express Package Service FedEx P riority Overnight Nextbusiness morning I Packagesupto ISOIks. Delivery commitmentmay be tetar te some areas. I FedEx Standard Overnight Nextbusiness afternoon I I FedEx First O vernight -- Earliestneia buanessniomkig detverytn selectlocations . I I FedEx 2Day FedEx E g re s s Saver Second business day ifp Third business I---------- FedEx Envelope rata notavailabia.Miramum c h a t ; Qne-pound rate -- *1------ 4b Express Freight Service * Packages over 150fbs. Delivery commitmentmay be later in some areas. . I l FedEx 1D ay Freight* I-- I N od business day C a l fo r Confirmation: - I I FedEx 2Day Freight '-- ' Second business day I I FedEx 3D ay Freight *-- I third.businessaay 5 Packaging Declared value britSQ O I I FedEx Envelope* FedExPak* Includes FedExSm alPak, FedEx Large Pak,and FedExSturdy Pak [jj^ O th e r 6 Special Handling In clud e FedEx addres in S ection 3. SATURDAYDelivery I j f ifeaiabte tally forFedExPriority CNemghtand FedEx2Day to selectZIP codes j-- i HOLDWeekday I__ I a t FedEx Location Notavalable fur FedExFirst Overnight D o this shipmentcontain dangerous poods? ,-- HOLDSaturday __ I a t FedEx Location Available onlyfo r FedEx Priorty Overnight and FedEx2Deyto1 selectlocations y One box m e t be checked. I If: C. Iff C C C Os O 3 Sign to authorize delivery w ithoutobtaining signature. By signing you authorize us to d e liv e rth is shipm entw ith ou t obtaining a signature and agree to indem nify and hold us harm less from any resulting claim s. Questions? Visit our Web site at fsd0x.com o r c a ll 1.8Q0.Go.FedEx* 800.463.3339. .. Rev.D3tBlO/01Part#1576121994-2QDlFedEx*PRINTEDiNU.SA WCSL03 ^ ' _____ - RAW DATA REPORT Sponsor Study No: NA Limit of Quantitation: 50 ng/L (2 ng/filter paper) Exygen Study No: L2178 Injection Volume: 15 pL Analyte: PFOA Matrix: Water Ions Monitored' 413->369 Sample Volume; 40.0 mL 1 Site: Washington Works Final Volume: 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 040304A Karen Risha LC/MS/MS Unit # 7 04/03/04 04/04/04 Amount S ii PFOA PFOA PFOA PFOA Exygen Sponsor Sample Run Cone. Dilution Peak Found FoUDd Found Added Recovery ID ID Code No. (ng/L) Factor Area (ng/L) (ng/filter paner) iufl/filter paper) (ng/L) (%) l XC032304-0 - C 040304A-1001 0 - 549 - -- XC032304-1 - CS 040304A-1002 25 3856 -- XC032304-2 - CS 040304A-1003 50 7233 - - XC032304-4 XC032304-5 ' CS 040304A-1005 250 CS 040304A-1006 500 . - 36094 73515 . - - XC032304-6 XC032304-7 Methanol Wash CS 040304A-1007 1000 CK 040304A-1008 250 C 040304A-1Q09 - 140882 34299 0 --- -- Slotted Filter Paper Control NA C 040304A-1010 1 855 ND ND ND Whatman 41 Filter PaperContrc NA C 040304A -lO il - 1 1114 ND ND ND - 1 Slotted Filter Paper Spk A NA LCS 040304A-1012 . 1 7740 44.5 1.78 0.00178 50 89 Whatman 41 Filter Paper Spk fi\ NA LCS 040304A-1013 1 8968 52.7 2.11 0.00211 50 105 Slotted Filter Paper Spk C NA LCS 040304A-1014 - 1 67056 437 17.5 0.0175 500 87 Whatman 41 Filter Paper Spk ^ NA LCS 040304A-1015 - 1 61288 399 16.0 0.0160 500 80 XC032304-1 - CS 040304A-1016 25 3960 -- L2178-1 WWK-A-E1-S1-1 S 040304A-1017 1 10649115 ** -- L2178-2 WWK-A-E1-S1-2 S 040304A-1018 - I 17237276 ** -- L2178-3 WWK-A-E1-S1-3 S 040304A-1019 - 1 12483933 * -- L2178-4 L2178-5 L2178-6 L2178-7 WWK-A-E1-S1-4 WWK-A-E1-S1-5 WWK-A-E 1-S1-6A WWK-A-E 1-S1-6B S 040304A-1020 - S 040304A-1021 - s 040304A-1022 - s 040304A-1023 - 1 11522153 1 6602706 1 15663896 1 14134673 ** ** ** * -- -- XC032304-2 CS 040304A-1024 50 14481 - -- L2178-8 L2178-9 L2178-10 L2178-11 WWK-A-FBLK1 WWK-A-E1-S2-1 WWK-A-E1-S2-2 WWK-A-E 1-S2-3 s 040304A-1025 - s 040304A-1026 - S 040304A-1027 - s 040304A-1028 - 1 8241 1 23033354 1 26154408 1 24987002 NQ * ** NQ NQ - --- -- t L2178-12 WWK-A-E 1-S2-4 s 040304A-1029 - 1 22539600 - -- L2178-13 WWK-A-E1-S2-5 s 040304A-1030 1 22819730 ** - -- L2178-14 WWK-A-E1-S2-6A s 040304A-1031 - l 28910008 ** - - XC032304-3* - CS 040304A-1032 100 - 182149 - - L2178-15 WWK-A-E 1-S2-6B s 040304A-1033 - 1 26480088 ** - L2178-16 WWK-A-EI-S3-1 s 040304A-1034 - 1 20976000 ** - * L2178-17 WWK-A-E 1-S3-2 s 040304A-1035 - 1 26969268 ** - L2178-18 WWK-A-E 1-S3-3 s 040304A-1036 - 1 24311208 ** - L2178-19 WWK-A-E1-S3-4 s 040304A-1037 - 1 23954196 * - L2178-20 WWK-A-E1-S3-5 s 040304A-1038 - 1 22281124 ** - L2178-21 WWK-A-E 1-S3-6A s 040304A-1039 - 1 29571072 ** - XC032304-4* L2178-22 WWK-A-E1-S3-6B CS 040304A-1040 250 s 040304A-1041 - 211881 1 26266948 * - L2178-23 WWK-A-E1-S5-1 s 040304A-1042 - 1 4267036 ** - L2178-24 WWK-A-E1-S5-2 s 040304A-1043 - 1 5411635 ** - L2178-25 WWK-A-E1-S5-3 s 040304A -1044 - 1 4727270 *+ - L2178-26 WWK-A-E1-S5-4 s 040304A-1045 1 4582807 ** - l. L2178-27 WWK-A-E 1-S5-5 s 040304A-1046 1 4082124 ** - L2178-28 WWK-A-E1-S5-6 A s 040304A-1047 1 10309808 ** - L2178-29 WWK-A-E1-S5-6B s 040304A-1048 I 8861053 * - XC032304-5 - CS 040304A-1049 500 - 84251 - - - - - XC032304-6 - CS 040304A-1050 1000 - 160139 * ' l PFOA Found (ng/L) = (peak area intercept) / slope x DF Recovery (%) = [PFOA found (ng/L)-PFOA found in control (ng/L)] x 100 amount PFOA added (ng/L) Standard Curve: Linear (1/x weighted) Intercept = 1012.08 Slope = 151.071 Coef. O f D et = 0.990013 PFOA Found (ng/filter paper) PFOA found (ng/L) x volume extracted (0.04L) PFOA Found (pg/filter paper) = PFOA found (ng/filter paper) / 1000 ng/pg CS - Calibration standard C Control sample S = Sample LF = Lab fortified sample FF = Field fortified sample LCS * Laboratory Control Spike Avg Resp. o f the 250 ppt Standards (area):A Response o f the Check Standard (area): Percent Difference (%): % difference acceptable if within 36094 34299 5 15% CK =Check Standard ND = Not detected = Response between 0 and LOD NQ = Not quantifiable = Response between LOD and LOQ Spreadsheet prepared by:_ Standard was excluded from the calculation o f the calibration curve. The standard is considered a statistical o u tlie by the Huge Error Test for outliers. ACalculation performed using only the first 250 ppt standard. 'Sample requires dilution. See data set 040304AR. 0020 000596 Exygen 3058 Research Drive m / ^ J RESE A RC H State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number: L2178 Matrix: Filter Paper Sponsor Study/Protocol No: NA . The samples listed below were removed from room temperature storage cabinet__ [ Time i3l> Date Initials CEE CLIENT SAMPLE ID EXYGEN ID NUMBER VOLUME (mL) FORTIFICATION (ng) na Slotted Filter Paper Control 40.0 - na Whatman 41 Filter Paper Control 40.0 - na Slotted Filter Paper SpkA 40.0 2.0 na Whatman 41 Filter Paper Spk B 40.0 2.0 na Slotted Filter Paper SpkC 40.0 20.0 na Whatman 41 Filter Paper Spk D 40.0 20.0 WWK-A-E1-S1-1 L2178-1 40.0 - WWK-A-E1-S1-2 L2178-2 40.0 - WWK-A-E1-S1-3 L2178-3 40.0 - WWK-A-E1- S 1-4 L2178-4 40.0 - WWK-A-E1- S 1-5 L2178-5 40.0 - WWK-A-E 1-S1-6A L2178-6 40.0 - WWK-A-E 1-S1-6B L2178-7 40.0 - WWK-A-FBLK1 L2178-8 40.0 - WWK-A-E 1-S2-1 L2178-9 40.0 - WWK-A-E1-S2-2 L2178-10 40.0 - WWK-A-E 1-S2-3 L2178-11 40.0 - WWK-A-E 1-S2-4 L2178-12 40.0 - WWK-A-E1-S2-5 L2178-13 40.0 - WWK-A-E 1-S2-6A L2178-14 40.0 - WWK-A-E 1-S2-6B L2178-15 40.0 - WWK-A-E1-S3-1 L2178-16 40.0 - WWK-A-E 1-S3-2 L2178-17 40.0 - WWK-A-E1-S3-3 L2178-18 40.0 - Slotted Filter Paper SpkA Whatman 41 Filter Paper Spk B Slotted Filter Paper Spk C Whatman 41 Filter Paper Spk D - . Spiking Solution Used F030804-5 (10 ng/mL) F030804-5 (10 ng/mL) F030804-4 (100 ng/mL) F030804-4 (100 ng/mL) - -. -- 40 mL of water was added to all samples: Time I$30 Date Volume Used for Spiking 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) - - Ipitial/Date f C " / 4 02-1 6CC- / 4 47 ( T T /M t>7{( 42-li 1/ - - - Initials Comments: Entire sample was used for extraction Analysis Summary: Data Set: Data Set: Data Set: Set extraction/analysis data verified by: T L Initials/Date: Initials/Date: Initials/Date: Date: D021 April 2, 2004/0 C00597 i i ,J i 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L2178 MATRIX: Filter Paper METHOD: 01M-008-046i$ ANALYTES: PFOA PROTOCOL NUMBER: NA 1% Client ID na na na na na Exygen ID Slotted Filter Paper Control Whatman 41 Filter Paper Control Slotted Filter Paper SpkA Whatman 41 Filter Paper Spk B Slotted Filter Paper SpkC STEP 1 i STEP 2 __ STEP 3 Dilutions (mL/mL) - - STEP 4 Dilutions (mL/mL) -- -- -- -- STEP 5 -- - Reage Mate: Meth nol C18. PE TypeI Vater . . Lot# W 0 2 5 3 H t> NA - na WWK-A-E1-S1-1 WWK-A-E1 -S1-2 WWK-A-E1-S1-3 Whatman 41 Filter Paper Spk D L2178-1 L2178-2 L2178-3 1 -- Aa-V>b.'A.o Q / t o "-V,,D r -'A o .^ L o .- _- -- WWK-A-E1-S1-4 WWK-A-E1-S1-5 WWK-A-E1 -S1-6A WWK-A-E1 -S1-6B WWK-A-FBLK1 WWK-A-E1-S2-1 WWK-A-E1-S2-2 WWK-A-E1-S2-3 WWK-A-E1-S2-4 WWK-A-E1-S2-5 L2178-4 L2178-5 L2178-6 L2178-7 L2178-8 L2178-9 1.2178-10 L2178-11 L2178-12 L2178-13 mn 11 -- l^ y V iO Initials 'Date CEE t x j e s ai _. -sA o -- - &>'/* 'A .o 1____ - - -- & -'A > .OAA .o ' y - - -- -- - -- ^V ^A o -- -- s 7 i o 0-'/\o HPLC 1 -- (z 0 Y,o.-'AO Methanol - s o-y.D .o,V io AmmoniujaAcetate V % I 5 ^ -- Typel water NA WWK-A-E1-S2-6A L2178-14 - WWK-A-E1-S2-6B L2178-15 -- S)0 -Mo.-Vto - C WWK-A-E1-S3-1 L2178-16 -- W B m m Sm E m SM - WWK-A-E1-S3-2 WWK-A-E1-S3-3 L2178-17 L2178-18 \V Nt 1V - ^ o i/to o -'/i - - li d m m O V iD t - Al *Initials/Date - atta\o* m 0 Initial. /Date STEP 1: Shake overnight on a wrist-action shaker STEP 2: Squeeze water from filter and water through SPE column clean-up STEP 3: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP 4: LC/MS/MS analysis STEP 5: LC/MS/MS reanalysis. hF*io ,o*4 Initials and date under each step indicates the personnel that performed this step. $$ MODIFIED "Method of Analysis for the Determination of Ammonium Perfluorooctanoate (APFO) in Water" COMMENTS: 32-Final extracts stored in refrigerator Initials: Date; July 19,2001/4 22 t r 598 Exygen % / ^_r esea rc h 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number: L2178 Matrix: Filter Paper Sponsor Study/Protocol No: NA The samples listed below were removed from room temperature storage cabinet___j Time I3 i6 Date Initials_ CLIENT SAMPLE ID WWK-A-E1-S3-4 WWK-A-E1-S3-5 WWK-A-E1-S3-6A WWK-A-E1-S3-6B WWK-A-E1-S5-1 WWK-A-E1-S5-2 WWK-A-E1-S5-3 WWK-A-E1-S5-4 WWK-A-E 1-S5-5 WWK-A-E 1-S5-6A WWK-A-E1-S5-6B - EXYGEN ED NUMBER L2178-19 L2178-20 L2178-21 L2178-22 L2178-23 L2178-24 L2178-25 L2178-26 L2178-27 L2178-28 L2178-29 _ 1 VOLUME (mL) | FORTIFICATION (ng) 40.0 _ 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 - -- - - -- - - -- - - -_ - - -- - - -- - - -- - - -- - - -- - - -- - - -- - - -- - - -- Spiking Solution Used -- -- -- -- -- -- -- -- 40 mL of water was added to all samples: Time <350______ Date Volume Used for Spiking - Initial/Date - Initials Comments: Entire sample was used for extraction Analysis Summary: Data Set: Data Set: Data Set:_____^ _____ Set extraction/analysis data verified by: _C U f _______ Initials/Date: Initials/Date: Initials/Date: . dM,)o4 | Date: April 2, 2004/0 02 3 c o K> 4^ O o oo Phone: 814-272-1039 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L2178 MATRIX: Filter Paper METHOD: 01M-008-046" ANALYTES: PFOA PROTOCOL NUMBER: NA Client ID WWK-A-E1-S3-4 WWK-A-E1-S3-5 WWK-A-E1-S3-6A WWK-A-E1-S3-6B WWK-A-E1-S5-1 WWK-A-E1-S5-2 WWK-A-E1-S5-3 WWK-A-E1-S5-4 WWK-A-E1-S5-5 WWK-A-E1-S5-6A WWK-A-E1-S5-6B - *Initials/Date Exygen ID L2178-19 12178-20 L2178-21 L2178-22 L2178-23 L2178-24 L2178-25 L2178-26 L2178-27 L2178-28 L2178-29 - - - - - - - STEP 1 STEP 2 1 STEP 3 \ Y / V - -- -- -_ - -- --- _ - -. - -- -- ---- -- -- (J S H d fS * t Dilutions (mL/mL) - -- -- - __ - - - - - - - - -- STEP 4 / \/ _ _ - Dilutions (mL/mL) ( V - V '/iO (T)0-'/w 0>Vvo n S V io .0 ;'/iu 0 o' ,/ o Jo'V\D 0-Vio y io V iO o .y io STEP 5 yD )/ ) D-'/i0-Xi. 3 V 1 . -- __ _- _- _- _- .- _- _- _- .- 12 tA M o ^lo tN 2 1 "S Z Reaj ents/ Mat<rials Met ianol C18 SPE Type! Water Lot# NA . _ _ Initial, 1/Date . _ - CEE o i h i ] l1 _ . HPLC Met ianol Ammonii tnAcetate Type water - NA . . . . i/Dale Jf STEP 2: Squeeze water from filter and water through SPE column clean-up STEP 3: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP 4: LC/MS/MS analysis STEP 5: LC/MS/MS reanalysis. Initials and date under each step indicates the personnel that performed this step. $$ MODIFIED "Method of Analysis for the Determination of Ammonium Perfluorooctanoate (APFO) in Water" COMMENTS: CELFinal extracts stored in refrigeratorZ k - Initials: Date: o H o sjo 1/ July 19, 2001/4 r Exygen % / ^ J r e s e a rR C H 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 PREPARATION OF EXTRACTED CALIBRATION STANDARDS Exygen study NO. LiX l b Protocol No.: None . Method No.: 01M-008-046* Exygen Study No. : NA Analytes: PFOA Matrix: Type I Water* Sample Vol: 40 mL Sponsor Sample ID NA Exygen Sample ID 0106020 Sample Description Type I Water* Fort. Solution ID - Fort. Soin. Cone. fng/mLj - Fort. Volume fuLl - Micropipet used (UL) Fort. Level (ppt) Final Solution ID # ** 4 XC032304-0 Reagents/ Materials Methanol Lot# NA 0106020 Type I Water* F030804-5 10 100 200 25 XC032304-1 C l8 SPE S5TBI NA 0106020 Type I Water* F030804-5 10 200 200 50 XC032304-2 Type I Water NA NA 0106020 Type I Water* F030804-5 10 400 200 100 XC032304-3 - - NA 0106020 Type I Water* F030804-4 100 100 200 250 XC032304-4 - - NA 0106020 Type I Water* F030804-4 100 200 200 500 XC032304-5 NA 0106020 Type I Water* F030804-4 100 400 200 1000 XC032304-6 - - - NA 0106020 Type I Water* F012804-2 100 100 200 250 XC032304-7 &Z - - - - - - - - - Initials/Date: C;/23|o4 Vertical arrows in a column indicate identical values. **This must be a unique number. Use this system: Extracted Calibration Soln ID #: XCMMDDYY-0,1,2,3. etc. Samples removed fromffelrigerahy / freezer # ^32- Time: c 40 mL of each sample measured using a SO mL graduated cylinder. o After measuring, samples returned to<tefrigeraTty / freezer # ,^ 2 . Time: ZD IV' CJl Samples fortified: Initials/Date: / &5A3 0^ SPE clean-up: Initials/Date: ('EE / 03j a flf/ Initials/Date Initials/Date Initials/Date CSE Jq3 [z IH - -THIS IS AN E KACT C O PY O F ; THE ORIGINAIJLDOCUMENT* BY. D A T E J i M rJ Final volume adjusted to 5 mL: Extracts placed in refrigerator # 3 1 - Initials/Date: CPU /fla|j3 Initials/Date: CpS /o^jzsjb^ STANDARD EXPIRATION DATE: 4/6/04 Comments: T h is type I water has been filtered through a hypercarb filter * Method of Analysis for the Determination of Ammonium Perfluorooctanoate (APFO) in Water. r> :y o m o h* July 10, 2001/0 Masslynx - Sample List Sample List: C:\MASSLYNX\008 APFO 'RO\SampieDB\040304A Filter paper.spl Printed: Sun Apr 04 07:18:13 2004 _______________________ Vial File Name MS ID Client ID Sample Description 1 1 040304A-1001 _ 2 2 040304A-1002 3 3 040304A-1003 -- 4 4 040304A-1004 -- 5 5 040304A-1005 -- 6 6 040304A-1006 ---7 7 040304A-1007 -- 8 8 040304A-1008 -- 9 92 040304A-1009 -- 10 11 040304A-1010 -- 11 12 040304A-1011 -- 12 13 040304A-1012 -- 13 14 040304A-1013 -- 14 15 040304A-1014 -- 15 16 040304A-1015 -- 16 2 040304A-1016 -- 17 17 040304A-1017 -- 18 18 040304A-1018 -- 19 19 040304A-1019 -- 20 20 040304A-1020 -- 21 21 040304A-1021 -- 22 22 040304A-1022 23 23 040304A-1023 -- 24 3 040304A-1024 -- 25 24 040304A-1025 -- 26 25 040304A-1026 -- 27 26 040304A-1027 -- 28 27 040304A-1028 -- 29 28 040304A-1029 -- 30 29 040304A-1030 -- 31 30 040304A-1031 -- 32 4 040304A-1032 -- 33 81 040304A-1033 -- 34 82 040304A-1034 -- 35 83 040304A-1035 -- 36 84 040304A-1036 -- 37 85 040304A-1037 -- 38 86 040304A-1038 -- 39 87 040304A-1039 -- 40 5 040304A-1040 -- 41 88 040304A-1041 -- 42 89 040304A-1042 -- 43 90 040304A-1043 -- 44 93 040304A-1044 -- ___ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- XC032304-0, 0 ng/L standard XC032304-1,25 ng/L standard XC032304-2, 50 ng/L standard XC032304-3,100 ng/L standard XC032304-4, 250 ng/L standard XC032304-5, 500 ng/L standard XC032304-6,1000 ng/L standard XC032304-7, 250 ng/L check standard Methanol Wash Slotted Filter Paper Control Whatman 41 Filter Paper Control Slotted Filter Paper Spk A, 50 ng/L Whatman 41 Filter Paper Spk B, 50 ng/L Slotted Filter Paper Spk C, 500 ng/L Whatman 41 Filter Paper Spk D, 500 ng/L XC032304-1,25 ng/L standard L2178-1 L2178-2 L2178-3 L2178-4 L2178-5 L2178-6 L2178-7 XC032304-2, 50 ng/L standard L2178-8 L2178-9 L2178-10 L2178-11 L2178-12 L2178-13 L2178-14 XC032304-3,100 ng/L standard L2178-15 L2178-16 L2178-17 L2178-18 L2178-19 L2178-20 L2178-21 XC032304-4, 250 ng/L standard L2178-22 L2178-23 L2178-24 L2178-25 26 Exygen studyNO. L 2 Lifo Page 1 Page Position: (1 ,1 ) Matrix Sample Type Cone (ng/L) Cone B Cone C Test ID DF MS Method ___ Blank 0 -- Standard 25 -- Standard 50 -- Standard 100 -- Standard 250 -- Standard 500 -- Standard 1000 -- QC 250 -- Blank -- -- Blank -- -- Blank -- -- QC 50 -- QC 50 -- QC 500 -- QC 500 -- Standard 25 -- Analyte -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- Analyte -- -- Standard 50 -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Standard 100 -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Standard 250 -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- ___ ___ 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA ------ -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA __ -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- . . . 0 1 008 PFOA Masslynx - Sample List Sample List: C:\MASSLYNX\008 APFO.f ?0\SampleDB\040304A Filter paper.spi Printed: Sun Apr 04 07:18:13 2004 HPLC Method MS Tune File Inj Volume (pL) 1 water PFOA Tune 15 2 water PFOA Tune 15 3 water PFOA Tune 15 4 water PFOA Tune 15 5 water PFOA Tune 15 6 water PFOA Tune 15 7 water PFOA Tune 15 8 water PFOA Tune 15 9 water PFOA Tune 15 10 water PFOA Tune 15 11 water PFOA Tune 15 12 water PFOA Tune 15 13 water PFOA Tune 15 14 water PFOA Tune 15 15 water PFOA Tune 15 16 water PFOA Tune 15 17 water PFOA Tune 15 18 water PFOA Tune 15 19 water PFOA Tune 15 20 water PFOA Tune 15 21 water PFOA Tune 15 22 water PFOA Tune 15 23 water PFOA Tune 15 24 water PFOA Tune 15 25 water PFOA Tune 15 26 water PFOA Tune 15 27 water PFOA Tune 15 28 water PFOA Tune 15 29 water PFOA Tune 15 30 water PFOA Tune 15 31 water PFOA Tune 15 32 water PFOA Tune 15 33 water PFOA Tune 15 34 water PFOA Tune 15 35 water PFOA Tune 15 36 water PFOA Tune 15 37 water PFOA Tune 15 38 water PFOA Tune 15 39 water PFOA Tune 15 40 water PFOA Tune 15 41 water PFOA Tune 15 42 water PFOA Tune 15 43 water PFOA Tune 15 44 water PFOA Tune 15 u o 2 7 C-0 0 S 03 Exygen STUDY NO. 11X1 b Page 2 Page Position: (2 ,1 ) Masslynx - Sample List Sample List: C:\MASSLYNX\008 APFO. Rp\SampleDB\040304A Filter paper.spl Printed: Sun Apr 04 07:18:13 2004 Dh Vial File Name LIMS ID Client ID Sample Description 45 94 040304A-1045 ___ 46 95 040304A-1046 -- 47 96 040304A-1047 -- 48 97 040304A-1048 -- 49 6 040304A-1049 -- 50 7 040304A-1050 -- L2178-26 L2178-27 L2178-28 L2178-29 XC032304-5, 500 ng/L standard XC032304-6,1000 ng/L standard c o !V CC o o o 'f i o Exygen study NO . Page 3 Page Position: (1, 2) Matrix Sample Type Conc(ng/L) ConcB Conci! Test ID DF MS Method -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- _ _ Standard 500 -- Standard 1000 -- -- 0 1 008 PFOA ---- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA Masslynx - Sample List Sample List: C:\MASSLYNX\008 APFO.PRO\SampleDB\040304A Filter paper.spl Printed: Sun Apr 04 07:18:13 2004 ^ ___________________ HPLC Method MS Tune File Inj Volume (pL) 45 water PFOA Tune 15 46 water PFOA Tune 15 47 water PFOA Tune 15 48 water PFOA Tune 15 49 water PFOA Tune 15 50 water PFOA Tune 15 C. O ro XL O O & o Cl Exygen STUDY N O . I M I ? ) Page 4 Page Position: (2, 2) LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: L2178 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #7) Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381 : Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Bin Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Genesis C-8, 5 cm x 2.1 mm i.d. x 4 p (Exygen ID: M AI3296) (JONESCHROMATOGRAPHY: Part No. FK5962EJ) Mobile Phase (A) Mobile Phase (B) 2 mM Ammonium Acetate in Type I Water Methanol Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. All Handwritten Peak HD's by: 030 C-00 5 0 6 Scanning Method Report Method: C:\MASSLYNX\008 A PFO.PRO\ACQUDB\008 PFOA Last Modified: Wed Mar 20 16:07:50 2002 Printed: Sun Apr 04 07:18:19 2004 Solvent Delay ( mins ) 0.00 Function : 1 MRM of 1 Mass Pair ( ESP- ) In ter Channel Delay ( Secs ) : Span ( Daltons ) : S ta rt Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 8.00 1 Dwell (Secs) C o ll Energy (eV) 1 413.00 369.00 0.20 10 Cone ( V ) 10 Page 1 j 31 C O O fv O ? Method Report Method File: Last Modified P r in te d : c :\masslynx\008 apfo.pro\acqudb\water Sunday, April 04, 2004 07:05:34 Sunday, April 04, HP1100 LC Pump Initial Conditions Solvents ___ AS______ ____________________________ 60.0 B% 40.0 C% 0.0 D% 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 15.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 10 entries which are : Time 0.00 0.40 1.00 7.00 7.50 9.00 9.50 13.50 14.00 15.00 A% 60.0 60.0 10.0 10.0 0.0 0.0 60.0 60.0 60.0 60.0 B% 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 40.0 C% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 0.300 HP1100 LC Pump External Event Timetable The Timetable contains 4 entries which are : Time Initial 0.00 0.10 8.00 Column Switch Off Off Off Off Contactl Off On Off Off Contact2 Off Off On Off Contact3 Off Off Off Off Contact4 Off Off Off Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (/1/min) Draw Position (mm) Stop Time (mins) Injection Volume (fil) Vial Number 200.0 200 0.10 15.00 15.0 7 Page 1 Pressure 400 400 400 400 400 400 400 400 400 400 ^ U 52 C00S08 Tuning Method Report Method: C:\MASSLYNX\008 APFO.PRO\ACQUDB\PFOA TUNE Printed: Sun Apr 04 07:18:36 2004 Page 1 Dau 413.00 SOURCE ( ESP- ) C a p illa ry Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. D esolvation Temp. Set Rdbk 3.00 -2.93 10 -10 0.0 0.0 0.0 100 100 300 300 Pressures Analyser Vacuum Gas C e ll Rdbk OFF 3 .3e-3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance C o llis io n E x it LM Res 2 HM Res 2 IEnergy 2 M ultiplier Gas Flows Cone Gas Desolvation Set Rd] 14.0 14.0 1.0 -2 8 10 9 2 11 14.0 14.0 2.0 700 -6: Rdbk 88.2 697.1 u033 C " 0 '- .0 9 . Precise Research. Proven Results. In order to verify mass resolution, a calibration check is performed on the mass spectrometer using a Nal/Rb/Cs tuning solution. The tuning solution is infused onto the mass spec using an infusion pump set to a flow rate o f 10 pL/min. An MS scan from 80 to 1380 amu is performed on both MSI and MS2. The calibration is considered acceptable if the following 11 peaks are found within 0.2 amu o f their known masses on both MSI 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 o f the masses are outride 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 the following 2 pages. Calibration Check on MS2 using NaIRbCs Tuning Solution CALCHK032904-2 1 (0.087) Cn (Cen,2, 80.00, Ht); Sm (SG, 2x0.60); Sb (1,40.00 ); Cm (1:12) 100-| LC/Mci/MS #7 29 Mar-2004 09:45:05 MS2 ES+ 1,38e8 041 U % O o 04 On r> /> \0 M 0-1 100 Exygen STUDY N O . TH IS IS AN EXACT COPY OF THE ORIGINAL DOCUJMMEf NTi* BY M L . - DATEJt 292.9 382.9 472.7 322.8 622.6 532.8 406.8 772.5 442.9 556.7 922.4 706.6 1072.3 856.5 12;22.2 iniL | 882.4 'A 1006.6 1156.3 | ' T'V'p .'-I'-r 1V 'l1 i | i i MV i 1372.1 1306.2 jpoijL m/7 300 400 ' 5 0 0 600 700 800 900 1000 1100 12C0a, 1300 Initial Calibration Curve Exygen Study No.: Set No: Extraction Date: Analyzed on: L2178 040304A 04/03/04 04/04/04 The first curve of the data set is used to determine performance. A linear regression (with no weighting) is performed using the first six standards of the analytical run. The coefficient of determination (R Square) must be 0.985 or greater. If the set fails to meet this requirement, the run must be rejected and the samples reanalyzed. ExygenID XC032304-1 XC032304-2 XC032304-3 XC032304-4 XC032304-5 XC032304-6 Standard Concentration (ng/L) 25 50 100 250 500 1000 Peak Area 3856 7233 14458 36094 73515 140882 Coefficient of Determination: 0.999540151 SUMMARY OUTPUT Regression Statistics Multiple R 0.999770049 R Square 0.999540151 Adjusted R Square 0.999425189 Standard Error 1274.602534 Observations 6 ANOVA Regression Residual Total df 1 4 5 SS MS 14125194087 14125194087 6498446.483 1624611.621 14131692533 F Significance F 8694.50514 7.93101E-08 Intercept X Variable 1 Coefficients Standard Error tStat 690.1132853 712.0106292 0.969245763 141.2453612 1.514787662 93.24433034 P-value 0.387308369 7.93101E-08 Lower 95% -1286.749235 137.0396277 Upper 95% Lower 95.0% Upper 95.0% 2666.975806 -1286.749235 2666.975806 145.4510947 137.0396277 145.4510947 0037 C09G13 Quantify Calibration Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 1 Calibration: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\CurveDB\040304A Filter Paper . u038Exygen Research, 3058 Research Drive, State College, PA 16801 C00G 14 Huge Error Test for Outliers1 Protocol No.: NA Exygen study no.: L2178 Compound: PFOA-------- Extraction Date: 04/03/04 Analysis Date: 04/04/04 M atrix: W ater__________ Approach: Omitting the suspect point, the data are plotted and a "best fitting" line is determined (Masslynx was used to calculate a linear curve and equation for this data). The average residuals from the fitted line are calculated and compared with the residual for the suspect point according to the following equation: M = [suspect - average] / average If M >4.0, the point is considered an outlier and may be rejected. Notes: 1. Brackets indicate absolute value. 2. The suspect point is indicated below in bold font. residuals C * predictedx** X (x- predictedx) [residuals] 25 4788.855 3856 -932.855 932.855 50 8565.630 7233 -1332.630 1332.630 100 16119.180 14458 -1661.180 1661.180 250 38779.830 36094 -2685.830 2685.830 500 76547.580 73515 -3032.580 3032.580 1000 152083.080 140882 -11201.080 11201.080 25 4788.855 3960 -828.855 828.855 50 8565.630 14481 5915.370 5915.370 100 16119.180 182149 166029.820 166029.820 250 38779.830 211881 173101.170 173101.170 500 76547.580 84251 7703.420 7703.420 1000 152083.080 160139 8055.920 8055.920 average: 4334.972 M (100): M (250): 37.3 38.9 1 from Statistical Techniques for Data Analysis * c = concentration of standard (ng/L) ** calculated from the following equation: response = ( 151.071 x (c)* ) + 1012.08 U039 Quantify Sample Report Study N o .:L2178, Set No.;040304A, Ext.Date:04/03/04, AnalysttK.Risha Page 1 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFO^ Last modified: Tue Mar 23 10:54:32 2004 Job Cod e :----------- ----------------------------------- Initials. Printed: Mon Apr 05 07:35:10 2004 Run# J i -toso Name: 040304A-1001 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 0040 G O -O S IG Quantify Sample Report Study No.:L2178, Set N o .s040304A, Ext.Date:04/03/04, Analyst:K .Risha Page 2 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code :---------------------------- -- --------- -- ________________ _ ________ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1002 Text: 1 : PFOA Exygen Research 3058 Research Drive State College PA 16801 U041 6 *0 5 3 .7 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 3 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 -Job Code:---- ----------------- --------------- ------------.__________ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1003 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College PA 16801 Quantify Sample Report Study No.:L2178, Set N o .:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 4 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 -Job Code i------ -- ____________________________ ________ ____ _________________________ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1004 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 o4j C 0 0 0 .1 9 Quantify Sample Report Study No.:L2178, Set N o .:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 5 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code :----------------------- ------------------- ------------ ------------ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1005 Text: 1: PFOA XC032304-4, 250 ng/L standard 040304A-1005 Sm (Mn, 2x2) 100- %- 5.37 1360941 1 04-Apr-2004 09:26:25 LC/MS/MS #7 MRM of 1 Channel ES413 > 369 3.76e5 Area Qh' I ' m nj=,-v-t= f r r i T T ! Tim e'-H r r i 'T '~r i r I r r M i i " i i m r i i i I r i I T I I T I l ' T ' 1 ' - T l I 1I" 11 '1 |1 | 11 |1"1I '1...H 1 l|1~ '1~1' T ~^r-''1-, r - r 11 1T-i1 11 l i1 i1 M i ' , 1 1 1 1 1m 1 1, 1 p 1 1 1 1 i i1 ,1 1I 1, I 1I I 1 1I I 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive State College PA 16801 C u 0 44 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 6 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Coder:-- -- --------------------- -- ------------------------------ ------------------ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1006 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 45 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 7 Sample List: P:\Data\LCMSMS7\Masslynx\008 A PFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code :-- -- -------------------- _____________ __________ ________________ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1007 Text : 1 : PFOA XC032304-6,1000 ng/L standard 040304A-1007 Sm (Mn, 2x2) 100-, %- 5.37 140882 04-Apr-2004 09:59:46 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.51e6 Area 1.00 2.00 1I 11 11 I T 111T' T r 3.00 4.00 i 1111I 1'"[r1'-1' '|i~r' ~Ir *1' 5.00 6.00 7.00 T-n Time 8.00 Exygen Research 3058 Research Drive State College, PA 16801 uQ46 Quantify Sample Report Study N o .:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst-.K.Risha Page 8 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:-- --- -- -- -- -------------------- --- ------------------------- ------------ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1008 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 4 00' Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 9 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:_______________________ ____________________________ ________________ Printed: Mon Apr 05 07:35:10 2004 Marne: 040304A-1009 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 U48 Quantify Sample Report Study No. .-L2178, Set No. :040304A, Ext .Date :04/03/04, Analyst:K .Risha Page 10 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:---------------------------------- -- --------- -- ------------ -------------------- Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1010 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 C00G?5 U49 Quantify Sample Report Study N o .:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 11 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Hon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:------ -- ------------ -- ------------------------------- ---------------------- _ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1011 Text: 1: PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 C^O'3^6 050 Quantify Sample Report Study N o .:L2178, Set No.:040304A, Ext.Date;04/03/04, Analyst:K.Risha Page 12 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:----------------- -- -- --------- -------------------------- -------- ---------- Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1012 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 0051 Quantify Sample Report Study No.:L2178, Set N o .:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 13 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code: -- ----- -- .....................-- ____ ____________ ___________ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1013 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 C 00S & 8 Quantify Sample Report Study No.:L2178, Set No.s040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 14 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:..... .... ...........-- -- ......... ........................ .................. Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1014 Text: 1 : PFOA Slotted Filter Paper Spk C, 500 ng/L 040304A-1014 Sm (Mn, 2x2) hI n\Jn\J %- 5.36 670561 I J 04-Apr-2004 11:56:43 LC/MS/MS #7 MRM of 1 Channel ESCancelDx 6.94e5 Area 0- I I II '"I I I I I I I I I r I I I I T I I I r i I p m I I1 1 1 I I 1 I 11 `T M 11 1111 W ! ' 1 r t"t I I r n I r-r-r--I i i i i i i i i Tim e 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive State College , PA 16801 u 053 Quantify Sample Report Study N o .:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 15 Sample List; P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified; Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 "Job.Code-------------------------------- ----- --- -- ----- ---------------------------- Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1015 Text: 1 : PFOA Whatman 41 Filter Paper Spk D, 500 ng/L 040304A-1015 Sm (Mn, 2x2) 100-1 %- 5.35 61288 04-Apr-2004 12:13:27 LC/MS/MS #7 MRM of 1 Channel ES413 >369 5.94e5 Area 3.00 T 4.00 ' 1' 5.00 T-n Time Exygen Research, 3058 Research Drive, State College, PA 16801 U054 Cn0G30 Quantify Sample Report Study N o .:L217 8, Set No.:040304a . Ext.Date:04/03/04 , Analyst:K.Risha Page 16 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 7TQt> C o d e :-- -- --------------------- -- -------------- ---------------------------------- Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1016 Text: 1 : PFOA Exygen Research, 3058 Research Drive State College, PA 16801 U055 C00G31 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, AnalystrK.Risha Page 17 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 "Job Code: ------ -- --------------------------------------- Printed: Mon Apr 05 07:35:10 2004 Karne: 040304A-1017 Text: 1: PFOA L2178-1 040304A-1017 Sm (Mn, 2x2) 100n %- 5.34 10649115 04-Apr-2004 12:46:52 LC/MS/MS #7 MRM of 1 Channel ES413 >369 9.12e7 Area 1.00 2.00 3.00 4.00 5.00 ToO ........... I I ' 1 I Time 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 u 056 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 18 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:-------- -- ---------------------- .-- ___ ______________________________________ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1018 Text: 1 : PFOA L2178-2 040304A-1018 Sm (Mn, 2x2) 100- %: 5.35 172372761 1 1 04-Apr-2004 13:03:31 LC/MS/MS #7 MRM of 1 Channel ES413 > 369 1.32e8 Area 0J 11111 1111i 1111r 1" 1-7 111' 11111t-t-h - ' 11111 11' T_,_r< <1 1 1.00 2.00 3.00 4.00 5.00 1' 1 M 11 1 1 ......................... Time 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 u 057 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 19 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Uob Code:------------- -- ------------------- -------------------- ------------------- _ _ _ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1019 Text: 1 : PFOA L2178-3 040304A-1019 Sm (Mn, 2x2) 10Ch %: 5.35 12483933 04-Apr-2004 13:20:09 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1,09e8 Area 0 1<11I 11 11"I '"`TI I I ' ' 11I ' ' ' ' I 1.00 2.00 3.00 4.00 5.00 6.00 ' ' ' M ' 1I 111 I Time 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 u 058 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 20 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code :----------- ---------------- -- ---------------- ------------- ------------------- Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1020 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 059 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 21 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:---------------- -- ------------------------ -- --------------- ------------------- Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1021 Text : 1 : PFOA______________________ __ ________________________________________________________________ L2178-5 04-Apr-200413:53:49 LC/MS/MS #7 040304A-1021 Sm (Mn, 2x2) MRM of 1 Channel ES5.33 413 > 3 6 9 5.69e7 Area 1.00 2.00 3.00 4.00 T 1111I r 1 '"I .<" 1I 11 1' I 1111I Time 5.00_______ 6XX)_______ 7,00_______ 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 u060 C09S36 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 22 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 "Job Code:-- -------------------------- -------------------- -- -- . -__________________ _ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1022 Text: 1 : PFOA L2178-6 040304A-1022 Sm (Mn, 2x2) 100n %- 5.34 15663896 04-Apr-2004 14:10:30 LC/MS/MS #7 MRM of 1 Channel ES413 > 369 1.27e8 Area 0 1.00 2.00 6.00 ^ I--, '-- !.r-i-r-r r i | T i m e 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L2178, Set N o .:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 23 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:-------------------------- --------------- -- -- ___________________ __ ______ _ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1023 Text: 1 : PFOA L2178-7 040304A-1023 Sm (Mn, 2x2) 100- %: 114153 4673l [ 04-Apr-2004 14:27:19 LC/MS/MS #7 MRM of 1 Channel ES413 > 369 1.20e8 Area o: , , I I T',"rr TI i I1 II ', 1, 1, II ,I II-"1, II-'TT II nr_l I'"-"TH-1I~r I-I--TI11--II 1111 pI'' 11 1 I1TT'' 11....11 1i 11l'"r1i1111 1 1 I1'1-1r-11ir--yy11-i--'I iTt 1' 11...."r 11- 1 1 1 1 1I- 1 I 1 1 1I TI ime 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive State College, PA 16801 u 062 COOSJ8 Quantify Sample Report Study N o .:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 24 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:.... ... ............................ -- .................... .-- ------------- Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1024 Text: 1 : PFOA Exygen Research, 3058 Research Drive State College , PA 16801 COQaa U063 Quantify Sample Report Study No.:L2178, Set N o .:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 25 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:----------------------- ----- -- --- -- -------------------- -------------------- Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1025 Text: 1 : PFOA Exygen Research, 3058 Research Drive State College PA 16801 0064 CC0S40 Quantify Sample Report Study N o .:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 26 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:--------------------------------- -- ---------------------------------------- - Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1026 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 C O O G A ' i ^ ^ 6 ) Quantify Sample Report Study N o .:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K .Risha Page 27 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:---- ---------------------- -- -- ------------------ ----------------- ---------- Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1027 Text: 1: PFOA L2178-10 040304A-1027 Sm (Mn, 2x2) 100- %- 5.29 26154408 04-Apr-2004 15:34:10 LC/MS/MS #7 MRM of 1 Channel ES413 > 369 1.34e8 Area Time 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 ; 066 CC0^4 2 Quantify Sample Report Study No.:L2178, Set No.:040304a , Ext.Date:04/03/04, AnalystsK.Risha Page 28 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 "Job Code :-- -- --------------------------- -- ................... -- ____________________ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1028 Text: 1 : PFOA L2178-11 040304A-1028 Sm (Mn, 2x2) 100~i %- 5.30 249 04-Apr-2004 15:50:54 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.34e8 Area a 'I T~' 'I''11!1111I1111I1 1.00 2.00 3.00 4.00 6.00 7.00 Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 OU7 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 29 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 "Job Code:--- -- -------------------- -- --------------- -- -- -------------------- ------- Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1029 Text: 1 : PFOA L2178-12 040304A-1029 Sm (Mn, 2x2) 100- %: 5.32 22539600"! I 1 04-Apr-2004 16:07:44 LC/MS/MS #7 MRM of 1 Channel ES413> 369 1.34e8 Area (y 1111111111 I111!111 111I' 111111 r .I...1..1..1..'..I..1..1..1 -11I 1 1111'1"1I 1....'....r...i....1...<~Ir i1 '1~In1 11 1' 11I1.1...^....^...1........1...1....1...........................'...II ....................................'..1..'I I..'...I..'..I..ITIim e 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 u 068 C005-14 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K .Risha Page 30 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code :------- -- ------------------------ -------------------------------- ---------- Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1030 Text: 1 : PFOA L2178-13 040304A-1030 Sm (Mn, 2x2) 1 OOn %- 5.33 122819730'* J 04-Apr-2004 16:24:21 LC/MS/MS #7 MRM of 1 Channel ES413 > 369 1,34e8 Area o: "T -r I I I 1 1 I I II I1I1I1I1III1I1"M I1' '' .'"'P-1'1I''1'I''1'1''11I'''''I.... ......... .......1..1... ....`"T"1" 1 1 1 1 ' ' 1 1 1 1 ' 1 ' I 1 > 1 1 1 '' '" I ' ^ ^ 1 1 1 ` I 1 .......................... ..... 1 1.... * 11 1'111ITIim e 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive State College, PA 16801 U6 9 Quantify Sample Report Study No.:L2178, Set N o .:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 31 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job code: " --------------- -- ------------------------------------ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1031 Text: 1 : PFOA L2178-14 040304A-1031 Sm (Mn, 2x2) 10CH %: 5.27 28910008 I 04-Apr-2004 16:41:08 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.34e8 Area O ' ....................... I r , , H ' , T, H~ 1.00 2.00 3.00 4.00 5.00 6.00 i '' ' i t i i"T-i I "ri1"' I i ~i Tim e 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 0070 C00S46 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04 , Analyst:K.Risha Page 32 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 "Job Code: -- ---------------------------------------- Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1032 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 u07 i 17 Quantify Sample Report Study N o .:L2178, Set No.:040304A, Ext.Date:04/03/04, AnalystsK.Risha Page 33 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:-------- -- ---------------------------------------------- _ -- ______________ Printed: Mon Apr 05 07:35:10 2004*1 Name: 040304A-1033 Text : 1 : PFOA L2178-15 040304A-1033 Sm (Mn, 2x2) 100-1 %- 5.26 26480088 04-Apr-2004 17:14:35 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.34e8 Area a 1.00 ' 2.00 3.00 4.00 5.00 6.00 1 I jjm e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study N o .:L2178, Set N o .:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 34 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:------- ---------------------------------------------------------------------- Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1034 Text: 1 : PFOA L2178-16 040304A-1034 Sm (Mn, 2x2) 100- %- 5.32 20976000"! 1 1 04-Apr-2004 17:31:14 LC/MS/MS #7 MRM of 1 Channel ES413 > 369 1.34e8 Area 0 - 1111r 111'1I11r1i' 1!! 111il__iI 111111 1I1I1I1I i1I1I1I1I1I1I1I1I1I1:' I1I1I1I' 1T1-.1.1.......11111' 1I 1' 11r1~r1~rI .'...'..............................................'I 1ITim e 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 u 073 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 35 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code :-- ____________________________ ____ ___________________________________________ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1035 Text : 1 : PFOA Exygen Research, 3058 Research, Drive, State College, PA 16801 . u074 Quantify Sample Report Study No.:L2178, Set N o .:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 36 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:------- -- ----------------------------- -- ---------------- _ ---------------- Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1036 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 - 75 cn e ssi Quantify Sample Report Study No .:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 37 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code :-------------------------------------__-------- ------------------------------ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1037 Text: 1 : PFOA L Exygen Research, 3058 Research Drive, State College, PA 16801 U076 Quantify Sample Report Study No.:L2178, Set N o .j040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 38 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 "Job Code:----------------------------------------------- ---- - ________________________ _ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1038 Text : 1 : PFOA L2178-20 040304A-1038 Sm (Mn, 2x2) 100-, % 5.32 22281124 04-Apr-2004 18:37:50 LC/MS/MS #7 MRM of 1 Channel ES413 > 369 1,34e8 Area 0 - h Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 39 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Cod e :......................... .... ............. ..-- ------------------------ ______ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1039 Text : 1 : PFOA L2178-21 040304A-1039 Sm (Mn, 2x2) 10CH % 5.24 29571072 04-Apr-2004 18:54:43 LC/MS/MS #7 MRM of 1 Channel ES413 > 369 1.34e8 Area a 1.00 4.00 5.00 I111ri1111I1 ' I 1111I Time 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 40 Sample List: P:\Data\LCMSMS7\Masslynx\008 APPO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 job Code: ------------------------------ ----------------------------------- -----------. Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1040 Text: 1 : PFOA I 1 Exygen Research, 3058 Research Drive, State College, PA 16801 u(j/9 /\* , * Quantify Sample Report Study No.:L2178, Set No .:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 41 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 -Job Code :--------------------------------------------------- ___________________ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1041 Text : 1 : PFOA L2178-22 040304A-1041 Sm (Mn, 2x2) 10CH %- 5.28 26266948 04-Apr-2004 19:28:16 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.34e8 Area 0 h ...........'I Time 1.00 2.00 3 . 0 0 .........4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 U O Quantify Sample Report Study N o .:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 42 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code :------------------ -- -- ------------------------------------------------- Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1042 Text: 1 : PFOA L2178-23 040304A-1042 Sm (Mn, 2x2) 100- %: 5.33 142670361 1 04-Apr-2004 19:44:59 LC/MS/MS #7 MRM of 1 Channel ES413 >369 3.80e7 Area 0: I 111M 1111I111111111I11111' 1111I11111rri 1I111rr ~-'"'"""T1 1I l1"r1 11<1 II 11 11 !1 11II 111111 11II 11-1' 1( 11II '. ' ' ' II ......>........................-................................................................................I II Time 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Q81 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K .Risha Page 43 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code :------------------------------ -- -- -- -- -- ---- -------------------------------------_ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1043 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, FA 16801 U082 O': 0 0 5 8 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 44 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job_Code:__________________________________________________________________________ _ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1044 Text: 1 : PFOA L2178-25 040304A-1044 Sm (Mn, 2x2) 10On %- 5.31 4727270 04-Apr-2004 20:18:28 LC/MS/MS #7 MRM of 1 Channel ES413 > 369 4.30e7 Area 1.00 2.00 3.00 4.00 5.00 6.00 ' I M 11I 11 1I Time 7.00 8.00 Exygen Research, 3058 Research Drive State College PA 16801 , u083 CCG59 Quantify Sample Report Study No.:L2178, Set No .:040304A, Ext.Date:04/03/04, Analyst:K .Risha Page 45 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 nlob Code:------------------- -- -- -- --------------------------------- . _____________ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1045 Text : 1 : PFOA L2178-26 040304A-1045 Sm (Mn, 2x2) 10CH %- 5.31 4582807 04-Apr-2004 20:35:10 LC/MS/MS #7 MRM of 1 Channel ES413 >369 3.85e7 Area 0 I1111I11 - h Time 1.00 2.00 3.00 4.00 " ' " 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 U084 C00560 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 46 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:______________________________ _________________________ ____________ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1046 Text : 1 : PFOA L2178-27 040304A -1046 Sm (Mn, 2x2) 100n %- 'S32 408212^ 04-Apr-2004 20:51:47 LC/MS/MS #7 MRM of 1 Channel ES413 > 369 3.62e7 Area 0- 1I 1 1I 1I 111I I Time 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 085 C00S61 Quantify Sample Report Study N o .:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 47 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code : _____________________________________ _________ _ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1047 Text: 1 : PFOA L2178-28 040304A-1047 Sm (Mn, 2x2) 10Ch %- 5.30 10309808 04-Apr-2004 21:08:25 LC/MS/MS #7 MRM of 1 Channel ES413 >369 9.47e7 Area 0 ..................- 1I Time 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 U086 Quantify Sample Report Study No.:L2178, Set No.:040304A, Ext.Date:04/03/04, Analyst:K.Risha Page 48 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:------------------------.. __________________ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1048 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 : uUb7 *a ... "^*7 Quantify Sample Report Study N o .:L2178, Set No.:040304A, Ext.Date;04/03/04, Analyst:K.Risha Page 49 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:----------- -- _________________________________ ___________ _______________ Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1049 Text: 1 : PFOA XC032304-5, 500 ng/L standard 040304A-1049 Sm (Mn, 2x2) 100- 5.32 842511 %: (T | 1 1 i i i rmir ' i 1" i i i" f i' i i I i i t t " i .. r i Iii ... v t t i i i 1.00 2.00 3.00 1 1 l " H " 1 1 1 I' 1 ' i i i I i 4.00 5.00 04-Apr-2004 21:41:49 LC/MS/MS #7 MRM of 1 Channel ES413 >369 8.40e5 Area 1 ' 1 1 Time1 1 1 1 1 1 1 1 1 1 1 r-r r-r i , i 6.00 7.00 8.00 Exygen Research, 3058 Research Drive State College PA 16801 088 C0Q664 Quantify Sample Report Study N o .:L2178, Set No.:040304A, Ext.Date:04/03/04 , Analyst:K.Risha Page 50 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper Last modified: Mon Apr 05 06:48:24 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:--------------------------- ---- ------------------------ -- ------------------ . Printed: Mon Apr 05 07:35:10 2004 Name: 040304A-1050 Text: 1 : PFOA Exygen Research 3058 Research Drive State College PA 16801 U089 C00G65 Sponsor Study No: Exygen Study No: Analyte: Ions M onitorei Site: NA L2178 PFOA 413->369 Washington Works RAW DATA REPORT Limit o f Quantitation: Injection Volume: Matrix: Sample Volume: Final Volume: 50 ng/L 15 pL Water 40.0 mL 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 040304AR Karen Risha LC/MS/MS Unit # 7 04/03/04 04/06-07/04 Exygen ID XC040504-0 XC040504-1 XC040504-2 ----------- XC0405Q4 3-----XC040504-4 XC040504-5 XC040504-6 XC040504-7 L2178-1 L2178-2 L2178-3 L2178-4 L2178-5 L2178-6 L2178-7 XC040504-1 L2178-9 L2178-10 L2178-11 L2178-12 L2I78-13 L2178-14 L2178-15 XC0454-2 XC040504-3 L2178-16 L2178-17 L2178-18 L2178-19 L2178-20 L2178-21 L2178-22 XC040504-4 L2178-23 L2178-24 L2178-25 L2178-26 L2178-27 L2178-28 L2178-29 XC040504-5 XC040504-6 Sponsor ID - - WWK-A-E1-S1-1 WWK-A-E1-S1-2 WWK-A-E1-S1-3 WWK-A-E1-S1-4 WWK-A-E 1-S1-5 WWK-A-E 1-S1-6A WWK-A-E1-SI-6B WWK-A-E1-S2-1 WWK-A-E 1-S2-2 WWK-A-E1-S2-3 WWK-A-E1-S2-4 WWK-A-E1-S2-5 WWK-A-E 1-S2-6A WWK-A-E 1-S2-6B WWK-A-E1-S3-1 WWK-A-E 1-S3-2 WWK-A-E 1-S3-3 WWK-A-E1-S3-4 WWK-A-E1-S3-5 WWK-A-E 1-S3-6A WWK-A-E1-S3-6B WWK-A-E1-S5-1 WWK-A-E I-S5-2 WWK-A-E1-S5-3 WWK-A-E1-S5-4 WWK-A-E1-S5-5 WWK-A-E1-S5-6A WWK-A-E1-S5-6B Sample Code C CS CS Run No. 040304AR-301 040304AR-302 040304AR-303 CS 040304AR-305 CS 040304AR-306 CS 040304AR-307 CK 040304AR-308 S 040304AR-309 s 040304AR-310 s 040304AR-311 S 040304AR-312 S 040304AR-313 s 040304AR-314 S 040304AR-315 CS 040304AR-316 S 040304AR-317 S 040304AR-318 S 040304AR-319 S 040304AR-320 s 040304AR-321 S 040304AR-322 s 040304AR-323 CS 040304AR-324 CS 040304AR-325 s 040304AR-326 s 040304AR-327 s 040304AR-328 s 040304AR-329 s 040304AR-330 S 040304AR-331 s 040304AR-332 CS 040304AR-333 s 040304AR-334 s 040304AR-335 s 040304AR-336 s 040304AR-337 s 040304AR-338 s 040304AR-339 s 040304AR-340 CS 040304AR-341 CS 040304AR-342 Std. Cone. w 0 25 50 250 500 1000 250 25 - 50 100 - 250 - 500 1000 PFOA Found (ng/L) = (peak area - intercept) / slope x DF Recovery (%) * fPFOA found (ng/L)-PFQA found in control (ng/L)] amount PFOA added (ng/L) x 100 Dilution Factor - 1000 1000 1000 1000 100 1000 1000 10000 10000 10000 10000 10000 10000 10000 1000 10000 10000 10000 10000 10000 10000 100 100 100 100 100 1000 1000 - Peak Area 988 4634 8064 34776 70740 141547 35140 15859 34356 19792 18768 131253 51427 39519 4545 9011 27288 17884 11493 12759 83768 51240 7864 14478 66267 23391 21372 13520 13195 84170 37680 34729 44851 58038 49852 48332 48414 23876 17865 69196 140345 PFOA Found (ng/filter paper) = PFOA found (ng/L) x volume extracted (0.04L) PFOA Found (pg/filter paper) = PFOA found (ng/filter paper) / 1000 ng/pg PFOA Found (ng/L) - 107000 241000 136000 128000 94000 364000 278000 578000 1900000 1220000 757000 849000 5970000 3630000 - 471000 1620000 1470000 904000 880000 6000000 2650000 31600 41200 35300 34200 34200 165000 122000 PFOA Found (ng/filter paper) PFOA Found (pg/fflter paper) Amount PFOA Added (ng/L) Recovery (%) . - 4280 9640 5440 5120 3760 14600 11100 23100 76000 48800 30300 3400 239000 145000 18800 64800 58800 36200 35200 240000 106000 1260 1650 1410 1370 1370 6600 4880 - 4.28 9.64 5.44 5.12 3.76 - 14.6 11.1 . . . . 23.1 76.0 48.8 30.3 3.40 239 145 - -- 18.8 . 64.8 58.8 36.2 35.2 240 106 - - 1.26 1.65 1.41 1.37 1.37 6.60 4.88 -- . . - - -- Standard C u rv e: Linear (1/x weighted) Intercept = 996.314 Slope = 138.596 Coef O f Det. = 0.999725 CS = Calibration standard C = Control sample S * Sample LF = Lab fortified sample FF - Field fortified sample LCS * Laboratory Control Spike CK = Check Standard ND = Not detected = Response between 0 and LOD NQ = Not quantifiable = Response between LOD and LOQ Avg Resp. o f die 250 ppt Standards (area): Response ofthe Check Standard (area): Percent Difference (%): % difference acceptable if within 34753 35140 -1 15% Spreadsheet prepared by:_; U090 C"OGGG e V en8 R E S E A R C H 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 PREPARATION OF EXTRACTED CALIBRATION STANDARDS Exygen STUDY N O . p - n Protocol No.: None Method No.: OlM-008-046* Exygen Study No.: NA Analytes: PFOA Matrix: Type I WaterA Sample Vol: 40 mL Sponsor Sample ID NA Exygen Sample ID 0106020 Sample Description Type I WatcrA Fort. Solution ID - Fort. Soin. Cone. (ng/mL) - Fort. Volume __(pL) Micropipet Fort. used Level (PL) ....(PPt) Final Solution ID # ** \ XC040504-0 Reagents/ Materials Methanol Lot # NA 0106020 Type I Water* F030804-5 10 100 200 25 XC040504-1 C l8 SPE v s &7i NA 0106020 Type I WaterA F030804-5 10 200 200 50 XC040504-2 Type I Water NA NA 0106020 Type I WaterA F030804-5 10 400 200 100 XC040504-3 - _ NA 0106020 Type I WaterA F030804-4 100 100 200 250 XC040504-4 - - NA 0106020 Type I Water* F030804-4 100 200 200 500 XC040504-5 _ - NA 0106020 Type I Water* F030804-4 100 400 200 1000 XC040504-6 - - NA 0106020 Type I Water* F012804-2 100 100 200 250 XC040504-7 a - - - - - - - - - Initials/Date: t//s/W Vertical arrows in a column indicate identical values. **This must be a unique number. Use this system: Extracted Calibration Soln ID #: XCMMDDYY-0,1,2,3. etc. Samples removed from tefrigeratoh / freezer # Time: IQQd Initials/Date: Q-\ / 40 mL of each sample measured using a mL graduated cylinder. Initials/Date: & / After measuring, samples returned to refrigeratory freezer # Time: lO-^fS Initials/Date: 4 /V / Samples fortified: Initials/Date: SPE clean-up: Initials/Date: E^ W / '/Us/fH TH IS IS AN EXACT COPY OF THE ORIGINAL DO JMENT.' B Y ------& L , dat it Final volume adjusted to 5 mL: Extracts placed in refrigerator # 3 3 - Initials/Date m / y y w Initials/Date 74- / STANDARD EXPIRATION DATE: 4/19/04 Comments: *This type I water has been filtered through a hypercarb filter * Method of Analysis for the Determination of Ammonium Perfluorooctanoate (APFO) in Water. u 09 M y 10, 2001/0 vl Masslynx - Sample List Sample List: C:\MASSLYNX\008 APF0..PRO\SampleDB\040304AR Filter paper.spl Printed: Tue Apr 06 15:30:43 2004 U L Exygen study n o . L 2 H & _ Page 1 'age Position: (1,1) 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 C 38 CD K n 4410 N J 42 Vial File Name LIMS ID Client ID Sample Description Matrix Sample Type Cone (ng/L) Cone B Cone C Test ID DF 1 040304AR-301 -- 2 040304AR-302 -- 3 040304AR-303 -- 4 040304AR-304 -- 5 040304AR-305 -- 6 040304AR-306 -- 7 040304AR-307 -- 8 040304AR-308 -- 11 040304AR-309 -- 12 040304AR-310 -- 13 040304AR-311 -- 14 040304AR-312 -- 15 040304AR-313 -- 16 040304AR-314 -- 17 040304AR-315 -- 2 040304AR-316 -- 18 040304AR-317 -- 19 040304AR-318 -- 20 040304AR-319 -- 21 040304AR-320 -- 22 040304AR-321 -- 23 040304AR-322 -- 24 040304AR-323 -- 3 040304AR-324 -- 4 040304AR-325 -- 25 040304AR-326 -- 26 040304AR-327 -- 27 040304AR-328 -- 28 040304AR-329 -- 29 040304AR-330 -- 30 040304AR-331 -- 81 040304AR-332 -- 5 040304AR-333 -- 82 040304AR-334 -- 83 040304AR-335 -- 84 040304AR-336 -- 85 040304AR-337 -- 86 040304AR-338 -- 87 040304AR-339 -- 88 040304AR-340 -- 6 040304AR-341 -- 7 040304AR-342 -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- XC040504-0, 0 ng/L standard XC040504-1, 25 ng/L standard XC040504-2, 50 ng/L standard XC040504-3, 100 ng/L standard XC040504-4, 250 ng/L standard XC040504-5, 500 ng/L standard XC040504-6,1000 ng/L standard XC040504-7, 250 ng/L check standard L2178-1, DF=1000 L2178-2, DF=1000 L2178-3, DF=1000 L2178-4, DF=1000 L2178-5, DF=100 L2178-6, DF=1000 L2178-7, DF=1000 XC040504-1, 25 ng/L standard L2178-9, DF=10000 L2178-10, DF=10000 L2178-11, DF=10000 L2178-12, DF=10000 L2178-13, DF=10000 L2178-14, DF=10000 L2178-15, DF=10000 XC040504-2, 50 ng/L standard XC040504-3, 100 ng/L standard L2178-16, DF=1000 L2178-17, DF=10000 L2178-18, DF=10000 L2178-19, DF=10000 L2178-20, DF=10000 L2178-21, DF=10000 L2178-22, DF=10000 XC040504-4, 250 ng/L standard L2178-23, DF=100 L2178-24, DF=100 L2178-25, DF=100 L2178-26, DF=100 L2178-27, DF=100 L2178-28, DF=1000 L2178-29, DF=1000 XC040504-5, 500 ng/L standard XC040504-6, 1000 ng/L standard ___ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- ... Blank Standard Standard Standard Standard Standard Standard QC Analyte Analyte Analyte Analyte Analyte Analyte Analyte Standard Analyte Analyte Analyte Analyte Analyte Analyte Analyte Standard Standard Analyte Analyte Analyte Analyte Analyte Analyte Analyte Standard Analyte Analyte Analyte Analyte Analyte Analyte Analyte Standard Standard 0 25 50 100 250 500 1000 250 -- -- -- -- -- -- -- 25 -- -- -- -- -- -- -- 50 100 -- -- -- -- -- -- 250 -- -- -- -- -- -- -- 500 1000 __0 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- ------ --- 0 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- . . . 0-- -- 0-- -- 0-- -- 0-- -- ___ -- 0 0-- . . . 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- --. . . 0 1 1 1 1 1 1 1 1 1000 1000 1000 1000 100 1000 1000 1 10000 10000 10000 10000 10000 10000 10000 1 1 1000 10000 10000 10000 10000 10000 10000 1 100 100 100 100 100 1000 1000 1 1 Masslynx - Sample List Sample List: C:\MASSLYNX\008 APFOO..PROCA\SSaammpplleDB'\040304AR Filter paper.spl Printed: Tue Apr 06 15:30:43 2004 MS Method HPLC Method MS Tune File Inj Volume (pL) 1 008 PFOA 2 008 PFOA 3 008 PFOA 4 008 PFOA 5 008 PFOA 6 008 PFOA 7 008 PFOA 8 008 PFOA 9 008 PFOA 10 008 PFOA 11 008 PFOA 12 008 PFOA 13 008 PFOA 14 008 PFOA 15 008 PFOA 16 008 PFOA 17 008 PFOA 18 008 PFOA 19 008 PFOA 20 008 PFOA 21 008 PFOA 22 008 PFOA 23 008 PFOA 24 008 PFOA 25 008 PFOA 26 008 PFOA 27 008 PFOA 28 008 PFOA 29 008 PFOA 30 008 PFOA 31 008 PFOA 32 008 PFOA 33 008 PFOA 34 008 PFOA 35 008 PFOA 36 008 PFOA 37 008 PFOA 38 008 PFOA 39 008 PFOA 40 008 PFOA 41 008 PFOA 42 008 PFOA water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 U093 Exygen STUDY NO. Page 2 3age Position: (2, 1) LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: L2178 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #7) Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381 : Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Bin Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Genesis C-8, 5 cm x 2.1 mm i.d. x 4 p (Exygen ID: MA13296) (JONESCHROMATOGRAPHY: Part No. FK5962EJ) Mobile Phase (A) : Mobile Phase (B) : Analyst: 2 mM Ammonium Acetate in Type I Water v\ Methanol W t A v 0' Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 VJ NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. All Handwritten Peak ID's by:_____ 094 Cv^u.70 Scanning Method Report Method: C:\MASSLYNX\008 A P F O .PRO\ACQUDB\008 PFOA Last Modified: Wed Mar 20 16:07:50 2002 Printed: Tue Apr 06 15:28:34 2004 Solvent Delay ( mins ) : 0.00 Function : 1 MRM of 1 Mass Pair ( ESP- ) In ter Channel Delay ( Secs ) : Span ( Daltons ) : S ta rt Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 8.00 1 Dwell (Secs) C o ll Energy (eV) 1 413.00 369.00 0.20 10 Cone ( V ) 10 Page 1 uOS5 C h a r 'd'* ' n- . r j L Method Report Method File: Last Modified: Printed: c :\masslynx\008 apfo.pro\acqudbYwater Tuesday, April 06, 2004 15:28:45 Tuesday, April 06, 2004 15:28:49 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 60.0 4U .0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 15.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 10 entries which are : Time 0.00 0.40 1.00 7.00 7.50 9.00 9.50 13.50 14.00 15.00 A% 60.0 60.0 10.0 10.0 0.0 0.0 60.0 60.0 60.0 60.0 B% 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 40.0 C% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 0.300 HP1100 LC Pump External Event Timetable The Timetable contains 4 entries which are : Time Initial 0.00 0.10 8.00 Column Switch Off Off Off Off Contactl Off On Off Off Contact2 Off Off On Off Contact3 Off Off Off Off Contact4 Off Off Off Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (/il/min) Draw Position (mm) Stop Time (mins) Injection Volume (ptl) Vial Number 200.0 200 0.10 15.00 15.0 7 Page 1 Pressure 400 400 400 400 400 400 400 400 400 400 u 096 Tuning Method Report Method: C:\MASSLYNX\008 APFO.PRO\ACQUDB\PFOA TUNE Printed: Tue Apr 06 15:29:11 2004 Page 1 SOURCE ( ESP- ) C a p illa ry Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 -2.94 10 -10 0.0 0.0 0.0 100 102 300 300 Pressures Analyser Vacuum Gas C e ll Rdbk OFF 2 .8e- 3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance C o llis io n E x it LM Res 2 HM Res 2 IEnergy 2 M ultiplier Gas Flows Cone Gas Desolvation Set Rdbk 14.0 14.0 1.0 -2 8 10 9 2 11 14.0 14.0 2.0 700 -695 Rdbk 88.2 692.7 l U 097 r r etC: Z f RESEARCH Precise Research. Proven Results. In order to verify mass resolution, a calibration check is performed on the mass spectrometer using a Nal/Rb/Cs tuning solution. The tuning solution is infused onto the mass spec using an infusion pump set to a flow rate o f 10 pL/min. An MS scan from 80 to 1380 amu is performed on both M SI and MS2. The calibration .is considered acceptable if the following 11 peaks are found within 0.2 amu o f their known masses on both M SI 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 o f 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 the following 2 pages. 1 I C alibration C heck on MS u sing NaIRbCs T u n in g S o lution CALCHK040504-1 1 (0.086) Cn (Cen,2, 80.00, Ht); Sm (SG, 2x0.60); Sb (1,40.00 ); Cm (1:31) ; 100-, 155-2 Q\\pS\o^ 4 LC/IVio/MS #7] 05 Apr-2004 07:55:59 Scan ES+ 1.38e8 $ Exygen STUDY NO. THIS IS AN EXACT COPY OF THE ORIGINAL DOCUMi BY--------- B L DATE % 99.1 o o vo \Q 233.0 293.1 382.9 n o a ci 11i 100 200 tfl* 300 472.7 532.8 622.5 406.8 556.7 682.6 (ik 400 Mil 500 600 700 772.4 922.3 856.4 800 882.3 lil.l-.-Liflli 900 1072.2 1006.3 982.3 ..I,..I. 1000 1156.1 1222- ''i `i"'11 1100 1200 1306.0 1371.9 , !1. rv-n-i-l-i m/z 1300 Cr a- ^ '-i 7 6 Initial Calibration Curve Exygen Study No.: Set No: Extraction Date: Analyzed on: L2178 040304AR 04/03/04 04/06-07/04 The first curve of the data set is used to determine performance. A linear regression (with no weighting) is performed using the first six standards of the analytical run. The coefficient of determination (R Square) must be 0.985 or greater. If the set fails to meet this requirement, the run must he rejected and the samples reanalyzed. Exygen ID XC040504-1 XC040504-2 XC040504-3 XC040504-4 XC040504-5 XC040504-6 Standard Concentration (ng/L) 25 50 100 250 500 1000 Peak Area 4634 8064 14633 34776 70740 141547 Coefficient of Determination: 0.999889312 SUMMARY OUTPUT Regression Statistics Multiple R 0.999944655 R Square 0.999889312 Adjusted R Square 0.99986164 Standard Error 622.4435051 Observations 6 ANOVA Regression Residual Total df 1 4 5 SS MS 13999470110 13999470110 1549743.668 387435.9171 14001019853 F Significance F 36133.64041 4.5946E-09 Intercept X Variable 1 Coefficients Standard Error tStat 618.2368692 347.7055629 1.778047104 140.6153656 0.739736284 190.0885068 P-value 0.150025364 4.5946E-09 Lower 95% -347.1505385 138.5615242 Upper 95% Lower 95.0% Upper 95.0% 1583.624277 -347.1505385 1583.624277 142.669207 138.5615242 142.669207 0 01 -<7 Quantify Calibration Report Study N o .:L2178, Set N o .:040304AR, Ext.Dates04/03/04, Analyst:K.Risha Page 1 Calibration: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\CurveDB\040304AR Filter Paper Exygen Research, 3058 Research Drive, State College, PA 16801 cnocvrs 0102 Quantify Sample Report Study No.:L2178, Set N o . :040304AR, Ext.Date:04/03/04, Analyst:K .Risha Page 1 Sample Lists Ps\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 FOA Last modified: Tue Mar 23 10:54:32 2004 Job Code : ____________________________ Initials Printed: Wed Apr 07 08:04:00 2004 Date__ Run# Ql 50\To Name: 040304AR-301 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 13 Quantify Sample Report Study No.:L2178, Set N o .:040304AR, Ext.Date:04/03/04, AnalystsK.Risha Page 2 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code :------ ------------------------------------------------------ ---------------------- Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-302 Text: 1 : PFOA L. I Exygen Research, 3058 Research Drive, State College, PA 16801 0 C 1'"0O4'"''.so Quantify Sample Report Study No.:L2178, Set No.:040304AR, Ext.Date:04/03/04, Analyst:K .Risha Page 3 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:-------------------------- . _____ ___________________________________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-303 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 0 * 6 5 -o g s i Quantify Sample Report Study N o .:L2178, Set No.:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 4 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code :_______________ ___________________ _____________________ _______________________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-304 Text: 1 : PFOA XC040504-3,100 ng/L standard 040304AR-304 Sm (Mn, 2x2) 10Ch %: 1C H ~ f = r r r I T T T T - p - i n " I . . . . . . . . . I 1.00 2.00 3.00 5.12 14633 T^f rT-r"' 1I 4.00 5.00 06-Apr-2004 20:43:20 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.33e5 Area ^'jTTTr^pfTTTy'i I I I' r I"I i ~ Time 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 1 06 -.82 Quantify Sample Report Study No.:L2178, Set N o .:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 5 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54.-32 2004 Job C o d a : _________________________________________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-305 Text: 1 : PFOA XC040504-4, 250 ng/L standard 040304AR-305 Sm (Mn, 2x2) 100n %- 5.14 34776 06-Apr-2004 21:00:02 LC/MS/MS #7 MRM of 1 Channel ES413 >369 3.08e5 Area 0 I-- I I I I I I " I T I I I ! 1.00 2.00 3.00 4.00 5.00 6/30 7.00 Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L2178, Set No.:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 6 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:------------------------- -------------- -------------------------------- Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-306 Text: 1 : PFOA XC040504-5, 500 ng/L standard 040304AR-306 Sm (Mn, 2x2) 100n %: 0 ' ' 1 T I T" T 1 I ; I I I I I I I r I I I I I I I , I , I I , 1.00 2.00 3.00 5.14 70740 TT 4.00 5.00 06-Apr-2004 21:16:49 LC/MS/MS #7 MRM of 1 Channel ES413 >369 6.36e5 Area 11I"' 6.00 I I i ' ' I r I I 1' 1 Time 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 u i Q8 Quantify Sample Report Study No.:L2178, Set No.:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 7 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code :----------------------- --------------- _ _ _ _ _ ---------------- Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-307 Text : 1 : PFOA XC040504-6,1000 ng/L standard 040304AR-307 Sm (Mn, 2x2) I VJU %: 5.14 11415471 06-Apr-2004 21:33:32 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.22e6 Area 0: 1 , 1 1 i 1' 1 ......... ' ' i i i i ' ' i ' ' Tim e1 1 ' ~ n 1, 1| H'|-- l-- r1 "1 1 1i I) 11 11 "1 i )] 11 "i 1 1i Ij 1i t * i 11 [1..... 11..1- 7 1 "iH' 1' 1' I' Ii 11 1 1 1 I 1 1 1 ' I 1 1 T"Hm ' 1 1 1i II 1 Ii 1i 'i Ii 1 1 1i 1 II 1 1i 1 1 II I 1.00 2.00 3.00 4.00 5.00 6.00 7.00_______ {TOO Exygen Research, 3058 Research Drive, State College, PA 16801 n 1na Quantify Sample Report Study No.:L2178, Set N o .:040304AR, Ext.Date:04/03/04, AnalystsK.Risha Page 8 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 T n h f ? o d e _____________ ___________________________________________________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-308 Text: 1 : PFOA XC040504-7, 250 ng/L check standard 040304AR-308 Sm (Mn, 2x2) 100- %- 0: 1.00_______ 2.00 3.00 5.13 351401 1 06-Apr-2004 21:50:18 LC/MS/MS #7 MRM of 1 Channel ES413 > 369 3.06e5 Area 1 { 111111111 11<1'- '"I ' '"'--I 4.00 5.00 6.00 I 1'n ' 1 1i'i ' I Time 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 01 IQ Quantify Sample Report Study N o .:L2178, Set N o .:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 9 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code: Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-309 Text: 1 : PFOA t Exygen Research, 3058 Research Drive, State College, PA 16801 [ UI i I *1I C''0^S7 Quantify Sample Report Study No.:L2178, Set N o .:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 10 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:-------------------------- --- -- ________________________ _____________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-310 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 U i 12 G 0S88 Quantify Sample Report Study No.:L2178, Set N o .:040304AR, Ext.Dates 04/03/04, AnalystsK.Risha Page 11 Sample List; P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:_________________ _______________________________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-311 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 Olii C00G89 I Quantify Sample Report Study N o .:L2178, Set No.s040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 12 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 -Job Code:------------ --- ----------------- -- -- ------------- Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-312 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 G 0 9 G 9 0 U * 14 Quantify Sample Report Study N o .:L2178, Set N o .:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 13 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code :_________ ________________ __________________________________________________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-313 Text: 1 : PFOA L2178-5, DF=100 040304AR-313 Sm (Mn, 2x2) a %: 5.13 11312531 1 06-Apr-2004 23:13:47 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.14e6 Area (y ' I 111111Hn 111111'MI 111` '' 'M! 1111111MI 11'111'1""TT 11r11r -rT]I Il-TI TI II ;I I...I..I..I..I..T"!. . 1 t > 1 .1..1..!..1..1 n1 1 iIl ....n......1....r.r. -IT, 1, ,I II I...1....,...,...I....,...,...,...,I IITim e 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 0115 C "0 0 !> i Quantify Sample Report Study No.:L2178, Set N o .:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 14 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:______ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-314 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 U1 ' J Quantify Sample Report Study No.:L2178, Set No.:040304AR, Ext.Date:04/03/04, AnalystsK.Risha Page 15 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Joh_C o d e ______________ __________________________________________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-315 Text : 1 : PFOA L2178-7, DF=1000 040304AR-315 Sm (Mn, 2x2) 100~I %- 5.13 3951S 06-Apr-2004 23:47:00 LC/MS/MS #7 MRM of 1 Channel ES413 >369 3.48e5 Area 0 "yi-T I I I I I'I r i Time 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 0117 0 10S93 Quantify Sample Report study N o .:L2178, Set No.:040304AR Ext.Date:04/03/04, Analyst :K .Risha Page 16 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 tjob-- Cod e :----------- -------------------------- ----------- -- -- _________________ _ _ ___ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-316 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 U1 ] 8 r 'N a/0 i > A Quantify Sample Report Study No.:L2178, Set No.:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 17 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:_____________ __ _________________________ _______________________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-317 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 . 0119 Quantify Sample Report Study No.:L2178, Set No.:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 18 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 do b Code:-- -- --------------------------------- -------------------- _ _ _ ----------- -------- Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-318 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 0 120 Quantify Sample Report Study N o .:L2178, Set N o .:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 19 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Cod e :-------------------------------------------------------------- ._____________________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-319 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 121 Quantify Sample Report Study No. .-L2178, Set No.:040304AR, Ext.Date: 04/03/04, Analyst :K.Risha Page 20 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:------------------------ ---------------------------------------- Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-320 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 1 O Quantify Sample Report Study No.:L2178, Set No.:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 21 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:----------- ---- -- ________________________________ ________________________ ________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-321 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 u 123 009^99 Quantify Sample Report Study No.:L2178, Set No.:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 22 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:------- ---------------------------------------- ------------- Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-322 Text: 1: PFOA L2178-14, DF=10000 040304AR-322 Sm (Mn, 2x2) 10CH % :_ 07-Apr-2004 01:43:53 LC/MS/MS #7 MRM of 1 Channel ES413 >369 7.57e5 Area 0 111I111H I"1" I1 1 I111~'~l1111I1 1.00 2.00 3.00 T I'In~rr]--I-iriy iiii|iiii|Time 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 0124 C "0700 Quantify Sample Report Study No.:L2178, Set N o .:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 23 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Cod e :--------------------- ------------------------ --- ----- ---------------------- Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-323 Text : 1: PFOA L2178-15, DF=10000 040304AR-323 Sm (Mn, 2x2) 100~| 5.13 51240 07-Apr-2004 02:00:38 LC/MS/MS #7 MRM of 1 Channel ES413 >369 4.47e5 Area 1I1111I11ri I 3.00 4.00 5.00 1'.rI'~1i1T1"i1TIT1I1I1'1II!|111''.rrT^~T '1 r1"iITime 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L2178, Set N o .:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 24 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:-------------------------------------------- ---------------------------- ----------- Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-324 Text: 1: PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 C " 0 `0 2 u i 26 Quantify Sample Report Study No.:L2178, Set No.:040304AR Ext.Date:04/03/04, Analyst:K.Risha Page 25 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Cede:------------------- --------------- ------------------ -------- Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-325 Text: 1: PFOA XC040504-3,100 ng/L standard 040304AR-325 Sm (Mn, 2x2) 10CH %: 07-Apr-2004 02:34:03 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.37e5 Area 0~ r T ~ r r I T-I T-TT-T-- .-T-- Ir-1 r T T ~ r r r - T - . . . . '................... 1.00 2.00 3.00 ~TT r ~r r n~n ~ ^ 6.00 7.00 Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 C Quantify Sample Report Study No.:L2178, Set N o .:040304AR, Ext.Date:04/03/04, AnalystsK.Risha Page 26 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Cod e :------- ------------------------- -- --------- ------ _ _ ---------------- Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-326 Text : 1 : PFOA L2178-16, DF=1000 040304AR-326 Sm (Mn, 2x2) 10Ch %- 5.14 66267 07-Apr-2004 02:50:41 LC/MS/MS #7 MRM of 1 Channel ES413 >369 6.00e5 Area 0- 1 1 1n "r I" r T 1 I T 1 T 'I-- I' T M M ' I 1.00 2.00 3.00 5.00 !jIr n""T ''J['li'ItII rr II''"IIt"r I-- I1"J.!" 6.00 7.00 1 I ' I ' I Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L2178, Set N o .:040304AR, Ext.Date:04/03/04, AnalystsK.Risha Page 27 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code :............................. .... ................................ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-327 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 U1 2 9 Quantify Sample Report Study N o .:L2178, Set N o .:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 28 Sample Lists P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 'Job--Code-:----------------------------- _____________________ ______________ ___________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-328 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 U i G0 0 7 0 6 Quantify Sample Report Study No.:L2178, Set No.:040304AR, Ext.Date:04/03/04, AnalystsK.Risha Page 29 Sample Lists P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 tTo b C o d er: ------------------------ ---- -- ____________________________________________ ______________ ________________________________________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-329 Text: 1 : PFOA________ __________________________________________________________________________________________________ L2178-19, DF=10000 07-Apr-2004 03:41:03 LC/MS/MS #7 040304AR-329 Sm (Mn, 2x2) MRM of 1 Channel ES413 >369 1.26e5 Area 1.00 2.00 3.00 4.00 5.00 TTTTTTTry^rr-r-pi -, Time 6.00 7.00_______ 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 1 31 : 0 >?07 Quantify Sample Report Study N o .:L2178, Set No.:040304AR, Ext.Date:04/03/04, AnalystiK.Risha Page 30 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Cod e :-------- ............................. .... ............... .................... Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-330 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 Q1 32 C0 0 ^ 0 8 Quantify Sample Report Study No.:L2178, Set No.:040304AR, Ext.Date:04/03/04, AnalystjK .Risha Page 31 Sample Lists P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job-- Code:------------------------- ------------------- ----------------- -------------- - Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-331 Text: 1 : PFOA L2178-21, DF=10000 040304AR-331 Sm (Mn, 2x2) 10Ch %: 0 J ., , , .,T ITTT-f I 'I I I' I r-T I . | I I I I | 1.00 2.00 3.00 07-Apr-2004 04:14:30 LC/MS/MS #7 MRM of 1 Channel ES5.14 413 > 3 6 9 7.58e5 Area 4.00 5.00 1" I I ! i ! ! | 11! i | ! I I r I t i I I I Time 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 u i 33 cno>09 Quantify Sample Report Study No.:L2178, Set No.:040304AR, Ext-Date:04/03/04, Analyst:K.Risha Page 32 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:------------ ----------------------------- ------------ __--------------- Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-332 Text: 1 : PFOA L2178-22, DF=10000 040304AR-332 Sm (Mn, 2x2) 100n %: 07-Apr-2004 04:31:15 LC/MS/MS #7 MRM of 1 Channel ES413 >369 3.50e5 Area 0~ I I 1 I I I I -T "I--f 1 I ' ' I H 1.00 I T~| l- T -l 1 -J - n 2.00 ' I IV 3.00 --- r r-i", h 1 I I ' I 6.00 7.00 I -n-| Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 o I S4 Quantify Sampld Report Study No.:L2178, Set N o .;040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 33 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code: -- ---- __________________________________________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-333 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 1 35 Quantify Sample Report Study No.:L2178, Set N o .:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 34 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 -Job Code :---------------------------- ---- -- _____________________ _________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-334 Text: PFOA L2178-23, DF=100 040304AR-334 Sm (Mn, 2x2) 100- %: 5.16 1448511 I 07-Apr-2004 05:04:36 LC/MS/MS #7 MRM of 1 Channel ES413 > 369 4.21e5 Area 0: 111I I I I 1r n I I I I ) >"T1-1 11r 1' r-7 i r i i i i i ' U ' 1|,'"TM I 1111.........TM .......... ' I ........... 11 1 1 I 1I ' I n ! ! 1 Time 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 l [ [ I Exygen Research, 3058 Research Drive, State College, PA 16801 0136 Quantify Sample Report Study No.:L2178, Set No.:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 35 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:-------------- ---------------- ______------------------ .____________________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-335 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 01 37 C 'J ? .1.3 Quantify Sample Report Study No.:L2178, Set N o . :040304AR, Ext-Date:04/03/04, Analyst:K.Risha Page 36 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 -Job Code:-- ------------------------ -------- -- -- _______________________________________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-336 Text: 1 : PFOA L2178-25, DF=100 040304AR-336 Sm (Mn, 2x2) 10CH %- 5.13 498E 07-Apr-2004 05:37:51 LC/MS/MS #7 MRM of 1 Channel ES413 > 369 4.54e5 Area 0 iM 1fi1rr t -i Time 4.00 5.00 6.00 Exygen Research, 3058 Research Drive, State College, PA 16801 I 'm -, Quantify Sample Report Study No.:L2178, Set N o .:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 37 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:..................... .... ....................... .............................. Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-337 Text: 1 : PFOA L2178-26, DF=100 040304AR-337 Sm (Mn, 2x2) 100- %: 5,14 483321 I I 07-Apr-2004 05:54:26 LC/MS/MS #7 MRM of 1 Channel ES413 >369 4.44e5 Area 0: H' ' 1 '' 1 1 1 1 H 11111'11""1I 1111''''...HH I1 I1 I1 I1 II 11 11 11 'I1 II 11 11 11''1 T 11 11 'I''1T1'1 1 11 Tr I111 1 'T* .I .... .1..1 .|--.r ;.r ,1 ,1'I.II" rII1I1 I1 .1.r .i .r.i -.p.- .i .i.i -|ITim e 1.00 2.00 3.00 4.00 5.00 6.00 7.00_______ 8/X) Exygen Research, 3058 Research Drive, State College, PA 16801 0139 0 ^0 7 1 5 Quantify Sample Report Study No.:L2178, Set No.:040304AR, Ext.Date:04/03/04 , Analyst:K.Risha Page 38 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:------------------------------------- -- -- -- -- ______________ __________________ Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-338 Text: 1 : PFOA L2178-27, DF=100 040304AR-338 Sm (Mn, 2x2) 100- %" 5.14 I484141 07-Apr-2004 06:11:04 LC/MS/MS #7 MRM of 1 Channel ES413 > 369 4.34e5 Area o: 1' r 11 11r H ' 11 l' r ` 11 it 11111111' 11! j"T M l - p l-l-T-pT' . |W 1' ' r"r i r 1"T I 11r 11 r 1"i"11 1,rT 11 Time 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 1 6 8 0 1 U1 40 cny^.e Quantify Sample Report Study No.:L2178, Set N o .:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 39 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:----------- -- ------------------------ --------------- ____------------- ----------- Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-339 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 U1 41 Quantify Sample Report Study No.:L2178 , Set N o .:040304AR, Ext.Date:04/03/04, AnalystrK.Risha Page 40 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code : -- ------------- -- --------------------- --........ ................... Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-340 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 U1 42 g Quantify Sample Report Study No.:L2178, Set N o .:040304AR, Ext.Date:04/03/04, Analyst:K.Risha Page 41 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code:------- -- --------------------- -- --------------------- -- --------------------- Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-341 Text : 1 : PFOA XC040504-5, 500 ng/L standard 040304AR-341 Sm (Mn, 2x2) 10CH % 5.11 69196 07-Apr-2004 07:01:09 LC/MS/MS #7 MRM of 1 Channel ES413 >369 6.56e5 Area 1.00 7.00 t- h Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 r ^ 7 i9 Quantify Sample Report Study No.:L2178, Set N o .:040304AR, Ext.Dates04/03/04, Analyst:K.Risha Page 42 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\040304AR Filter paper Last modified: Wed Apr 07 08:02:10 2004 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\031704 PFOA Last modified: Tue Mar 23 10:54:32 2004 Job Code: Printed: Wed Apr 07 08:04:00 2004 Name: 040304AR-342 Text: 1 : PFOA XC040504-6, 1000 ng/L standard 040304AR-342 Sm (Mn, 2x2) 100- %- 5.12 I1403451 1 07-Apr-2004 07:17:53 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.22e6 Area O 1111 111 11T '" ' ' M' 11I 11....... '-'-I ......... . ' 'i i i ' 1 1 1 " 1 1I 1I 'I 1I 1I 1I 1I 1I 1I 1I 1I 1! I1 I1 I1 I1 I1 ! I I I '1I'"r 1-1 1 1I I I r ~] I" I1I' I I 1 1 1 1 ................................................I I I i ! 'I I I I I I I I T M I' |1 TI ime 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 U 44 en RESEARCH Precise Research. Proven Results. The following pages are exact copies o f information for the standards used in this study. Pentadecafluorooctanoic acid (Inventory #: SP3800), obtained from Aldrich (lot # 23116HB) was Used to make a stock solution (ID # S030204-1) which in turn, was used to make intermediate solutions (ID#'s F030804-1, F030804-2, F030804-3, F030804-4 and F030804-5). These intermediate solutions are used to prepare extracted calibration standards, laboratory control samples, and matrix spike samples. Pentadecafluorooctanoic acid (Inventory#: SP2651), obtained from Oakwood Products Inc., Fluorochem USA (lot # 210002) was used to make a stock solution (ID # S 1027031) which in turn, was used to make intermediate solutions (ID#'s F012804-1 and F012804-2). These intermediate solutions are used to prepare the check standard, which is designed as an independent source verification o f the calibration standards. The information on the following pages provides the exact sources, lot numbers, shipping information, expiration dates and storage conditions of the neat standards. Also included are the preparation o f stock standard and fortification solution forms. These pages show the exact details o f the preparation of each o f the stock and fortification solutions, as well as their expiration dates and storage conditions. RESEARCH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 P rim a ry Description: Pentadecafluorooctanoic acid Type: Routine Sponsor Contact: Matrix: Solids (Gravimetric) Catalog #: 171468 Lot#: 23116HB CAS #: 335-67-1 Solvent: NONE Removed: False Condition Reev'd: Room Temperature Condition Stored: Room Temperature Current Location: B1-105 Vendor: SIGMA-ALDRICH, INC. Company Name: Contact: Phone #: Notes: Purity is 97.64% (GC purity of 97.7% minus Karl Fischer purity 0.06%) See phone log for explanation of expiration date. Addition 5.00000 c* >t vO g Component 3 _3j a3 ^ a> Withdrawal 0.10242 0.10242 Units 9 Notes: g Notes: g Notes: Component Balance 14 Balance 14 Date Received: Expires: Special: Flammable: Health: Reactive: Gross: Gross Units: Net Balance: Net Units: 12/08/2003 12/8/05 12:00:00AM None None Slightly hazardous None 43.82511 \ g 4.79516 g iq u o t n x i m m m Purpose INITIAL ANALYSIS ANALYSIS Computer BALANCE5 BALANCES Created On 12/8/03 12:56:03PM 12/8/03 1:53:57PM 3/2/04 11:45:51AM G -ft* C\ Created By RISHA, KAREN RISHA, KAREN SHEEHAN. AMY 3/2/04 Report Version: Feb 12 2004 11:30AM onn 1 nf 1 Instance: R0088843 W : ; SIGMA-ALDRICH ,, .; l lentow distribution Center ; Aldrich Cheleal CoMpany, Inc. 950 AMBASSADOR DRIVE Allentown PA iSIO v;'^ ; SHIP TO: j EXYGEW RESEARCH KAREN 34S RESEARCH DR i STATE COLLEGE PA lSOi vi Vi i WCustomer Semce8Q-325-30t0^http//v " , i t . - --*-m fs IlS r.S iiiig i Gr'=t'c_ .1 qf X- OUVEE fe ^PURCHASi 12/05/2003 Us WlpliS^pHT; ^0t3.iKRi IBOISEI " B ^ a j ^ l l I :MgPf^^BP.ERSONJrO CONTACT^ AIRBORNE GROUND FCA SHIPPING POTN KIN DOOLITTLE The SIGM A-ALDRICH Family <&S I G M A Biochemicals and Reagents for Life Science Research JFiuka Specialty Chemicals and Analytical Reagents for Research Q A L D R IC H * Organics and Inorganics for Chemical Synthesis Laboratory Chemicals and Reagents for Research and Analysis SU PELCO Chromatography Products for Analysis and Purification ALL SALES ARE EXPRESSLY LIMITED TO AND CONDITIONED UPON THE TERMS AND CONDITIONS APPEARING ON THE FRONT AND BACK OF THIS FORM. SIGMA-ALDRICH BRAND PRODUCTS ARE SOLD THROUGH SIGMA-ALDRICH, INC. V.v '.'o-v>vt7 'VV-V"''rv`V\ V' ^^svj. , * -V ,i,*->i- t h i s is a n e x a c t c o p y o f . THE ORIGINAL DOCUMENT.* Mp y - -DATE CM47 007 73 ___ Customer Service 800-325-3010 -- siGMA-ALDRiCH T e c h n i c a l Service - EXYGEN RESEARCH KAREN 3043 RESEARCH DR - STATE COLLEGE PA laOl S P 'S ftO O __ AXRBORWE-GflMD--- ,_______---------- "OUR DELIVERY NUMBER 814930362 THIS PACKAGE CONFORTO TO 49 CFR 1 7 3 .4 from: ALDRICH CHEMICAL CO 6950 AMBASSADOR DR ALLENTOWN, PA 18106 610-3S1-S107 T H IS IS AN EXACT COPY OF ------- THFQPipiMAI n o n IMFNT* . B Y ..... O L HATP W 7 W WEIGHT(LBS) 003 1PIECES EXYGEN RESEARCH KAREN 3848 RESEARCH DR STATE COLLEGE PA REF# 814S30862 ZIPCQDE 16801 SHIPMENT NO. ABE 46275417462 ADDITIONAL INFORMATION 46275417462 81493086 4931KR10 Tre ck #: 46275417462 Document 814938882 PHONE: 314-771-5765 4031KR10 SHIP DATE 12/05/2603 GGGGGGGGGGGGGGGGGGG EDS HON WCEA 3Q SPECIAL HANDLING SERVICES Q46275417462 AIRBORNE EXPRESS 2.50 LBS C ~ 0 ' -et1, g 46275417462 U1 48 1 OF 1 IR 3.5.00 CL433 04/02 SP3fifo Product Name Product Number CAS Number Molecular Formula Molecular Weight TEST APPEARANCE INFRARED SPECTRUM TITRATION GAS LIQUID CHROMATOGRAPHY TITRATION QUALITY CONTROL ACCEPTANCE DATE Pentadecafluorooctanolc add 17,146-8 335-67-1 c8h f 15o 2 414.1 SPECIFICATION WHITE TO OFF-WHITE POWDER CONFORMS TO STRUCTURE AND STANDARD AS ILLUSTRATED ON PAGE 507B OF EDITION I, VOLUME 1 OF 'THE ALDRICH LIBRARY OF FT-IR SPECTRA'. 95 .5 % - 104.5% (WITH NAOH) 95.5% (MINIMUM) 2% H20 (MAXIMUM) LOT 23116HB RESULTS WHITE CRYSTALLINE POWDER CONFORMS TO STRUCTURE AND STANDARD 101.1% (W ITH NAOH) 97.7% 0.0 6 % H 2 0 (WITH 'KARL FISCHER' REAGENT) JUNE, 2003 Ronnie J Martin, Supervisor Quality Control THIS IS AN EXACT COPY OF THE ORIGINAL DOCUMENT' BY HATH /\4ln7M 0149 r Exyeen m / (^RESEARCH 3058 Research Drive State College, PA 16801 SP 3oo Phone: 814-272-1039 Fax: 814-231-1580 Protocol No.: Exygen Study No: STUDY TELEPHONE/C03V1MUNICATIONS LOG Page I of I Person: Ken Company: Aldrich __ _ Originator: Date: Time: Exygen Sponsor 12/08/03 1022 X Notes: I called Aldrich tech service at 1-800-231-8327 to ask the shelf life of the PFOA standard 1 received today. Ken, an Aldrich rep in technical service, told me that the shelf life is 2 years from the date of receipt stored at room temperature.___________________________ THIS IS AN EXACT COPY OF 0 -0 7 ^ 6 01 50 August 7, 2001/1 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 PREPARATION OF STOCK STANDARD SOLUTION ......... ..'T i l l Exygen Study / Project Number: Customer Project Number: MA IIHprimarv StDnls&Wsi Compound Name: W oA Purity: 97, t,V Exygen ID: S'?0 0 0 3 8 0 0 Primary Standard Expiration Date: * l2toloS istock Soiutic I Net Wt. of Compound: I O ./0 2V 2 fl I Final Volume: lC?n mL Solvent Exygen Inventory ID: 1ZEoooqm L Stock Solution ID: ( S M M D D Y Y -1,2,3, etc.) S030Z0H - I [Storage Cone111ion and Location ' Net Wt. Adjusted for Purity: o .loooo Stock Solution Concentration: IO D O Solvent Name: methanol Stock Solution Expiration Date: 0 5 [ 02-| P5~ fl pg/mL Freezer ID: ~ II Walkin Freezer ID: Remarks. Refrigerator ID: 3 3 - Walkin Cooler ID: - Room Temperature: Storace Cabinet: - (Enter the Instrument or R o o m ID under the appropriate condition) - ' ` .' `JR f ' SS* '-1****. <1 tit* -/y* II || - .11 > i l Signature: LIBRARY ID: V0000986-4 `THIS IS AN EXACT COPY OF THE ORIGINAL DOCUMENT." RY B i DATE M b l l o M _ : (T 9 Date: - o s Jq z Jq Q LABORATORY FORM I fi 3058 Research Drive - State College, PA 16801 'R E S E A R C H Phone: 814-272-1039 Fax: 814-231-1580 PREPARATION' OF FORTIFICATION STANDARD SOLUTIONS Project t? Exygen Study / Project Number: ' - 31 y ^ Customer Project Number: v ", ~ P4V& 4 /\ fo rtifica tio n Solution Preparation > I'"-? 4 flf2 vernare tmtiasaiuttonsvare,cofnmd?indicate the com>medsolutions wittf bracket)'1 1 ` / Date Prepared: Fortification Solutions Expiration Date: 0 3 |o@ |0 4 i b b \c \o t\ Solvent Exygen Inventory ID: Solvent Name: M e iHAsHOL Initial Soin. ID Compound Description Initial Soin. Cone. (pg/mL) Initial Soin. Aliquoted Volume (mL) Final Soin. Volume (mL) Final Soin. Cone. (Pg/mL) Final Soin. ID (FMMDDYY-1,2,3, etc.) $036204- 1 PR A loco 10 IDO IDD F 0 3 6 0 0 4 -1 &d3o4~l Pr A to o 10 \o o lo F0 3 0 8 0 4 - Z F 58 4 - z \~ 3 8 4 ~ $ f D 3D B -1- ^ ?&>k ffb k PFcA 10 10 VO 10 o .l 10 (OO loo \oO 1.0 0-1 .OI F0 3 0 3 0 4 -3 f 6 3 0 8 0 4 '4 F0 3 0 6 0 4 -5 -- r~ --- - F- - - -- ~ -F - - --- - F_ -- - - - F-- - " --- -- -F Storage Condition and Location ^ ; \ Freezer ID: Walkin Freezer ID: Refrigerator 1C): 3 3 Room Tempe ature: Walkin Cooler ID: - SI orage Cabir et: (Enter the Instrument or Roorr ID under the appropriate condition) Remarks!W * * ; * t v *? , `v ' ^ 'iK \ * ' ' " ' W ' -- ~ 4 "THIS IS AM EXACT COPY OF THE ORIGINAL DOCUMENT." : R Y p i t ... D A T E - i m O T H - Signature: Date: 0152 5 NOVEMBER 2003/4 RESEARCH 3058 Research Drive State College, PA 16801 Standards - Primary Phone: 814-272-1039 Fax: 814-231-1580 Description: Type: Pentadecafluorooctanoic acid Routine Sponsor Contact: Vlatrix: SOLID Datalog #: 001319 _ot #: 210002 DAS #: 335-67-1 Solvent: NONE Density: Density Units: g/cm3 Current Location: B1-105 Vendor: OAKWOOD PRODUCTS, INC. Company Name: Contact: Phone #: Notes: Addition 100.0000 n c: .D q CTJ US <> Component Withdrawal 03 -< HH XX - * 2> D ?* m Sq ^go (?. m 5 z: < vHO A "n 0.0103 Units Component g Notes: g Balance 14 Notes: 008-APFO Date Received: Expires: Condition Reev'd: Condition Stored: Removed: Special: Flammable: Health: Reactive: 04/09/2003 4/9/04 12:00:00AM Room Temperature Refrigerated False Unknown Unknown Unknown Unknown Aliauot - SP0002651 Balance 99.9897 Purpose INITIAL ANALYSIS Computer BALANCE5 Created On 4/9/03 11:58:38AM 10/27/03 8:48:34AM Created Bv DECKER, EMILY RISHA, KAREN 10/27/03 Report Version: Oct 23 2003 9:58AM Instance: R0070515 min ui u m u m m u m u m u mil im mi O A iC W O G D P R O D U C T ^ IN C , Fl UOHOCHEM USA 1M l OtP DUNBAR ROAD W EST C Q U J M & A , SC 7BUA Phom<" z n Ai9 B H u O f-AV 803 730 bvSI 11 TO; ra;::a S, : i i ;> It,0 3:lOX: ; AcoOuffl* Payable D&pi > Bs. t , E,f- l;;*'1- |li#|EAf7':M O O O 3MJD aRP EE SHIP E%y<x&n Mm&x<sh L&h TO? A t t k i % .m .4m xz 3AS$ t>wIve St&te Colls-i^E PA l8;5i K e f EO A O iv li)il3 a ' 9<-ar-, ;m > ?; :? C f: e 7 a o ^ 5 4 TO : ExypmiResearefo La te Ortes \sm^Omm m i i Rerpo hmmtm 00#* &rnmm T Lo/# m tt eesp^idd*i iIhMvwz tjh^igs IS AN EXACT COPY OF $t*<* dte*<:<PA P X r '! O( RIGINAL D O C U M ^ N T ^ SteTte STATTE' THt< . ___ DATE -6U afV'^ PO >Y TX m ltete-? S TU I HAZ K > i* WCEA 3Q ABH /HRBORNE E X P R E S S ^/Wui >Z) ^ vcsr cuoaasK 'X ^ 8*ii* niiK Mi f>*i>' -i0.> J ....................... ..... ' | M M M i .... *>s <. SXk X t.10 *>' S ''V > H .'/ Jij'i'tf' '} P s*>ia-'-. K >*' O J. i Cl 0731. ^ U155 31VC3 A9 vN 3 w n o o a iV N io ia o 3 H i 3 0 AdOO 1 0 V X 3 NV SI S!H < \ ><1UM K '.! b ' ? ? * n * i 3 0 < ' \ r i >tn.tt > cO fN H i. " ,}v i * ` t s i t ' ' > j i m -.? ii i i t r . i 'iiH-Kmn p ??$?s .% $ .......... 11V 3E >nij? m m - m (mi m m s*a -mm.:! ?>:*>ihi g&y ^ e . i|# 0 3058 Research Drive Phone: 814^272-1039 State College, PA 16801 Fax: 814-231-1580 Page ------------ !------------------------------ '_____________ PREPARATION OF STOCK STANDARD SOLUTION ^Protocol Number: VI ^ ______________ (p p a V Compound: lENTAtecAF-t IJURncctAoniC A a K Exygen Study Number: D08~APFO .. Lot Number: 2-10 0 Q 2-__________ Source: Purity: 9T!________% Date Last Characterized: C5~|\\cr[o2. Date Standard Received: ______ Storage Location: COOLER^ Compound Expiration Date: o 4 \o ct |o vf Exygen Inventory #: S P 2 k S 1 _______ A calibration check must have been conducted with the balance on the day ofsample weighing. Balance Calibration Stock Solution Balance Number: Logbook page for calibration data: ______ UMS Net Wt. o f Material: 0 i 6 \ D 8 > \ g Wt. Adjusted for Purity: D, Ql OO g Solvent: NVETMAsM -- Manufacturer: M K> Lot Number: Stock Solution Expiration Date* : Final Volume:______ \ b O ________ mL Concentration:______ _____________pg/mL *TH!S IS AN EXACT COPY OF THE ORIGINAL DOCUMENT" / DATE. oflbl 04 Stock Solution ID: S \Q X lO ^ ~ 1 Stock Soin ID #: SMMDDYY-l,2,3,etc. * Assign a one year expiration date for all stock solutions unless otherwise indicated bv sponsor. Storage Conditions for Solution: Freezer Number: --- Refrigerator Number: Room Temperature: Indicate which of the above is applicable, and location. REMARKS: 3058 Research Drive :e n State College, PA 16801 3 3j R E S E A R C H Phone: 814-272-1039 Fax: 814-231-1580 PREPARATION1OF FORTIFICATION STANDARD SOLUTIONS Project Exygen Study / Project Number: Customer Project Number: Fortification Solution Preparation , A VV ' 'A ' * Z(If2 or m o r e initialsolutions'are c o m b i n e d indicate the c o m b i n e d solutions with a bracket) < Date Prepared: . . . Fortification Solutions Expiration Date: Solvent Exygen Inventory ID: P E to iim b Initial Soin. ID Compound Description Initial Soin. Cone. (pg/mL) c H lo ilo ^ Solvent Name: H etfkuol Initial Soin. Al quoted Volume (mL) Final Soin. Volume (mL) Final Soin. Cone. (pg/mL) Final Soin. ID (FMMDDYY-1,2,3, etc.) S \b Z ]o 5-1 FFOAr 1o o 1 .0 lo o 1 .0 F 0 \2 O 4 -| F 012- O -M -- Tp?oA _ 1.0 10 1DO 0.1 f 0 \2 _ ^ 0 4 -2 . -~ -F - -- - - F- - - - - - F_ - V. -- - -F - ' - - - -F - - -- - - F~ - - -F - - -- F- Storage Condition and Location;, * * <\ ^ w Freezer ID: -- Walkin Freezer ID: Refrigerator IE): 2>?> R Dorn Tempeiature: - Walkin Cooler ID: - Storage Cabir et: ~ (Enter the Instrument or R o o m ID u n d e r the appropriate condition) Remarks " , -W * " *< < ' `THIS IS AN EXACT COPY OF THE ORIGINAL DOCUMENT." RY DATF (W < Signature: ____________________ D ate: Qil,2g)|o^_______ I , u i b 8. 0(ab) r J ^^ ^ ~ ^ ,, , C i 0 ? -, 4 f | 5 NOVEMBER 2003/4
Contact UsLoginSign Up
CUNY - The Graduate CenterColumbia University Mailman School of Public Health - Sociomedical Sciences