Document K6d4q62XBoXmvQ4qLzG9rVb2w

Northwest Bioanalytical A H & 8 l6 - >A I J L Study No. NWBSOO-128 Report No. NWB RO1-066 Quantitative Determination of PFOS and Related Compounds in Human Serum by LC/MS/MS Sample Analysis Report for Protocol EPI-0013 Northwest Bioanalytical (NWB) A Division of NWT Inc. 1121 East 3900 South Salt Lake City, UT 84124 PREPARED FOR: 3M Company Coiporate Occupational Medicine, Medical Department 220-3W-05 St. Paul, MN 55144 ro-o "'T) mex ~x? rn C~.J ko ~"![ j <">n Z Z o !- J CD AUTHOR: , yi /c-u Connie O. Sakashita, B.S., NWB Project Manager _____ DATE: / - 9-Q2- Rodger L. Foltz, Ph.D., N W `Technical Director DATE: / - ? - 1 2L CONTAIN HO OBI Page 1 GC0463 Northwest Bioanalytical .Study No. NWBSOO-128 Report No. NWBRO1-066 QUALITY ASSURANCE STATEMENT LABORATORY: Northwest Bioanalytical (NWB) A Division of NWT, [nc. 1121 East 3900 South Salt Lake City, UT 84124 SPONSOR: 3M Company Corporate Occupational Medicine, Medical Department 220-3W-05 St. Paul, MN 55144 COMPOUND(S): PFOS, PFOA (POAA), PFHS, PFOSA, PFOSAA, M556, M570 NWB STUDY NUMBER: NWBSOO-128 SPONSOR STUDY NUMBER: EPI-0013 NWB STUDY TITLE: Quantitative Determination of PFOS and Related Compounds in Human Serum by LC/MS/MS The clinical study described in this report is not included within the definition of a GLP regulated nonclinical study. However, Northwest Bioanalytical conducts all projects in accordance with the guidelines of the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58), the OECD Principles of Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety of Drugs (Ordinance No. 21, PAB Notification No. 424.) The following inspections were performed by the NWB QAU per SOP. Inspection and Reporting Statement. Inspection Date 28 Nov 2000 20-23 Mar 2001 05-06 Apr 2001 02-04 May 2001 31 Dec 2001 - 0 7 Jan 2002 09 Jan 2002 Phase of Study Analytical Plan Sample Analysis Sample Receipt QC Preparation Report Draft/ Raw Data Final Report Date Inspection Report Issued To NWB Project Manager 'NWB Management 28 Nov 2000 30 Nov 2000 23 Mar 2001 31 Mar 2001 06 Apr 2001 30 Apr 2001 04 May 2001 31 May 2001 07 Jan 2002 31 Jan 2002 09 Jan 2002 31 Jan 2002 'Reports to NWB Management are issued monthly. As can reasonably be established, the methods and procedures described and the results incorporated into this final report accurately reflect the raw data. Sheryl A. Mathews, A.K.S. NWB QAU Compliance Auditor 69 J tlj!.._2003-- Date Page 2 00044 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 COMPLIANCE STATEM ENT The clinical study described in this report is not included within the definition o f a GLP regulated nonclinical study. However, to the best o f our knowledge, this project was conducted in accordance with the guidelines o f the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58) and according to the methods and procedures described within this report. In addition, the study followed the guidelines o f the OECD Principles of Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety o f Drugs (Ordinance No. 21, PAB Notification No. 424.) Any known incidents that may have affected the quality or integrity o f the project or reported data is included in this report. This report represents an accurate record o f the raw data. (J.-C7UCL.C Connie O. Sakashita, B.S. NWB Project Manager R o d le t L. Foltz, Ph.D NWB Technical Director / - */- $ 2 -- Date ____ 1, Date Page 3 0 0 0 4 .6 5 Northwest Bioanalytical TABLE OF CONTENTS Study No. NWBSOO-128 Report No. NWBRO1-066 SIGNATURE PAGE....................................................................................................................................1 QUALITY ASSURANCE STATEM ENT..............................................................................................2 COMPLIANCE STATEM ENT.................................................................................................................3 TABLE OF CONTENTS........................................................................................................................... 4 LIST OF TA B LES...................................................................................................................................... 4 LIST OF FIGURES..................................................................................................................................... 5 1. INTRODUCTION............................................................................................................................... 8 2. METHODOLOGY..............................................................................................................................9 3. SAMPLE A N A LY SIS..................................................................................................................... 11 4. RESULTS AND D ISCUSSION.....................................................................................................13 5. REFER EN C ES................................................................................................................................. 19 6. DATA R ETEN TIO N ....................................................................................................................... 20 LIST OF TABLES Table 1. Calibration Curve Summary for PFO S................................................................................. 21 Table 2. Calibration Curve Summary for PFH S............................................ :................................... 22 Table 3. Calibration Curve Summary for P F O A .................................................................................23 Table 4. Calibration Curve Summary for PFO SA A ........................................................................... 24 Table 5. Calibration Curve Summary for PFO SA .............................................................................. 25 Table 6. Calibration Curve Summary for M 556..................................................................................26 Table 7. Calibration Curve Summary for M 570..................................................................................27 Table 8. Back-Calculated Concentrations o f Calibration Standards for P F O S ..............................28 Page 4 0G04o Northwest Bioanalytical Study No. NWBSOO-128 Report No. N\VBR01-066 Table 9. Back-Calculated Concentrations o f Calibration Standards for P F H S ..............................30 Table 10. Back-Calculated Concentrations o f Calibration Standards for PFOA............................32 Table 11. Back-Calculated Concentrations o f Calibration Standards for PFOSAA...................... 36 Table 12. Back-Calculated Concentrations o f Calibration Standards for PFOSA......................... 39 Table 13. Back-Calculated Concentrations o f Calibration Standards for M 5 5 6 ........................... 41 Table 14. Back-Calculated Concentrations o f Calibration Standards for M 5 7 0 ........................... 43 Table 15. Analytical QC Summary for PFO S...................................................................................... 45 Table 16. Analytical QC Summary for PFHS...................................................................................... 48 Table 17. Analytical QC Summary for P F O A ..................................................................................... 51 Table 18. Analytical QC Summary for PFO SA A ................................................................................54 Table 19. Analytical QC Summary for PFO SA ................................................................................... 57 Table 20. Analytical QC Summary forM 556............. ........................................................................60 Table 21. Analytical QC Summary for M 570..................................................................................... 62 Table 22. Study Sample Concentrations................................................................................................65 Table 23. Repeat Analysis Table for P F O S .......................................................................................104 LIST OF FIGURES Figure 1. Representative Calibration Curve for P F O S ..................................................................... 105 Figure 2. Representative Calibration Curve for P F H S ..................................................................... 105 Figure 3. Representative Calibration Curve for PFO A ..................................................................... 106 Figure 4. Representative Calibration Curve for PFOSAA............................................................... 106 Figure 5. Representative Calibration Curve for PFOSA.,.................................................................107 Figure 6. Representative Calibration Curve for M556 ..................................................................... 107 Figure 7. Representative Calibration Curve for M 5 7 0 ..................................................................... 108 Page 5 0G047 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Figure 8. Human Plasma Blank for PFO S......................................................................................... 109 Figure 9. Human Plasma Blank for PFH S......................................................................................... 110 Figure 10. Human Plasma Blank for P F O A ......................................................................................111 Figure 11. Human Plasma Blank for PFO SA A ................................................................................ 112 Figure 12. Human Plasma Blank for PFOSA ................................................................................... 113 Figure 13. Human Plasm a Blank for M 556.......................................................................................114 Figure 14. Human Plasm a Blank for M 570...................................................................................... 115 Figure 15. Human Plasm a Blank with Internal Standard (QCO) for P F O S ................................... 116 Figure 16. Human Plasm a Blank with Internal Standard (QCO) for P F H S ................................... 117 Figure 17. Human Plasma Blank with Internal Standard (QCO) for PFOA................................... 118 Figure 18. Human Plasm a Blank with Internal Standard (QCO) for PFOSAA..............................119 Figure 19. Human Plasm a Blank with Internal Standard (QCO) for PF O SA ................................120 Figure 20. Human Plasm a Blank with Internal Standard (QCO) for M 5 5 6 ...................................121 Figure 21. Human Plasm a Blank with Internal Standard (QCO) for M 5 7 0...................................122 Figure 22. Low Standard for PFOS...................................................................................................... 123 Figure 23. Low Standard for PFHS...................................................................................................... 124 Figure 24. Low Standard for PFOA.....................................................................................................125 Figure 25. Low Standard for PFOSAA............................................................................................... 126 Figure 26. Low Standard for PFOSA...................................................................................................127 Figure 27. Low Standard for M556...................................................................................................... 128 Figure 28. Low Standard for M570...................................................................................................... 129 Figure 29. High Standard for PFOS..................................................................................................... 130 Figure 30. High Standard for PFHS..................................................................................................... 131 Figure 31. High Standard for PFO A .................................................................................................... 132 Page 6 0G04fc8 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Figure 32. High Standard forPFO SA A .............................................................................................133 Figure 33. High Standard for P F O S A ...................................................................................... 134 Figure 34. High Standard for M 556.........................................................................................135 Figure 35. High Standard for M 570.........................................................................................136 Page 7 '04 6 3 Northwest ioanalytical Study No. NWBSOO-I28 Report No. NWBRO1-066 Quantitative Determination ofPFOS and Related Compounds in Human Serum by LC/MS/MS Sample Analysis for Protocol EPI-0013 1. INTRODUCTION This report summarizes the analytical results from the quantitation ofPFO S, PFHS, PFOA, PFOSAA, PFOSA, M556, and M570 in human serum samples for 3M Company in support o f Protocol EPI-0013 [5.1]. The LC/MS/MS method for the analytes exhibited a quadratic response and had target LLOQ and ULOQ values o f 1.00 ppb (2.50 ppb for M556) and 500 ppb for the analytes. The testing facility was 3M Company (Corporate Occupational Medicine, Medical Department, 220-3W -05, St. Paul, MN 55144), and the Study Director was Jeffrey H. Mandel, M.D. The Study Contacts at 3M Company were Jean Burris, M.P.H, R.N., and James Lundberg, Ph.D. The following is a list o f NWB supervisory personnel involved in the completion o f this work: Connie O. Sakashita, B.S. (NWB Project Manager); Tonya Felix, M.A. (NWB Acting Project Manager); Patrick Bennett, M.S., M.B.A. (NWB Laboratory Director); Rodger L. Foltz, Ph.D. (NWB Technical Director). Laboratory personnel involved in the completion o f this study included Suzanne Newman, B.S. (NWB Research Scientist), Toni Peacock, B.S. (NWB Assistant Scientist) and Emily Yardimci, B.S. (NWB Associate Research Scientist). NWB SOPs and guidelines were used in the conduct o f this study and were available to study personnel in electronic and hard copy formats. Date Study Initiated: 15-Nov-2000 Date Analyses Completed: 11-May-2001 The clinical study described in this report is not included within the definition o f a GLP regulated nonclinical study. However, Northwest Bioanalytical conducts all studies within the guidelines o f the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58), the OECD Principles o f Good Page 8 CG0470 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety o f Drugs (Ordinance No. 21, PAB Notification No. 424). Any changes to or deviations from the original protocol (Analytical Plan) were documented through approved protocol amendments or deviation memos and are retained within the raw data. 2. M ETH O D O LO G Y The assay used for this study is reported in Northwest Bioanalytical reports NWBR00108 [5.2] and NWBR00-122 [5.3]. Chinese human plasma was used for the calibration curves and quality control samples. Serum sample results obtained using plasma curves are discussed in N W BR00-122. Samples for this study were received at NWB on the following dates: Receipt Date 22-NOV-2000 21-Feb-2001 06-Mar-2001 15-Mar-2001 05-A p r-2 001 Number o f Samples Received 100 108 330 16 125 Storage Condition (except during analysis) -20 C -20 C -20 C -20 C -20 C Reference Material Analyte Lot Number Purity PFOS (FC-95) 193 100% PFHS SE-036 100% PFOA (FC-143) 245 100% PFOSAA (FC-129) 617 53.8% PFOSA 214 100% M556 NB113047-8D 99.89% M570 118506-26 99.75% THPFOS 59909 90.0% Expiration Date 31-D e c - 2 0 10 0 1 - J a n - 2 0 10 3 1 -D e c - 2 0 10 31-D e c -2 0 10 31-D e c -2 0 10 31-D e c - 2 0 10 31-D e c -2 0 10 31-D e c -2 0 10 Source Storage Conditions 3M Room temperature* 3M -20 C 3M Room temperature* 3M Room temperature 3M Room temperature 3M Room temperature 3M Room temperature 3M Room temperature ^Stored dry Page 9 000471 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Eight or more calibration standards were prepared on the day o f each run by adding 100 pL o f blank human plasma and 400 pL o f 50 mM ammonium acetate in water (unadjusted pH ~6.9) to 13 x 100 mm polypropylene tubes. After a brief vortex mixing, 10.0 pL o f the appropriate spiking solution was added. The absolute purity of PFOS, PFOSA, PFOA, and PFHS reference material was not available prior to the conduct o f this study. Therefore, the reference material purity was assumed to be 100%. 3M contracted with Centre Analytical Laboratories, Inc., in State College, Pennsylvania to determine the absolute concentration o f PFOS, PFHS, and PFOA in NW B stock solutions used to prepare the analytical standards and controls used for this studies. All arrangements for purity determinations and the transfer o f NWB solutions to Centre Analytical Laboratories, Inc., were performed by 3M. Based on Centre Analytical Laboratories' results, the concentrations o f plasma calibrator and quality control samples were corrected using the following factors: Analyte PFOS PFHS PFOA Correction Factor 0.836 0.909 0.855 The final calibration standard concentrations in human plasma for each analyte can be found in Tables 8 - 1 4 . NOTE: Due to the use o f different matrix pools with different persistent levels, there are several standard concentrations in these tables. However, only eight (for M556) or nine (all other analytes) standards are used for a single curve. The target calibration curve range is 1.00 ppb (2.50 ppb M556) to 500 ppb prior to correction for purity. In addition, blank plasma samples, both with and without internal standard (designated as QCOs and Blanks, respectively), were assayed in each analytical run. Analytical QCs were prepared in human plasma on October 27,2000, March 8,2001, April 5,2001 and May 2, 2001 and frozen in a -20 C freezer. For each run, analytical QC levels were assayed in duplicate. In addition, for each dilution level, dilution QCs Page 10 000472 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 were run in triplicate in any analytical run that contained diluted subject samples. The QC concentrations are shown below: Analyte PFOS PFHS PFOA PFOSAA PFOSA M556 M570 Low QC Concentrations* All concentrations are expressed as ppb. M edium High 5.75, 6.40 4.48 4.32, 4.81 4.30, 4.60 4.00 4.00 4.00 126 156,157 145 150, 151 150 150 150 331,332 417,418 385 400,401 400 400 400 Dilution DF=5 348 * The target QC concentrations are 4.00 ppb, 150 ppb and 400 ppb prior to correction for purity. Each analyte has different QC concentrations based upon the persistent levels of the analyte in the human plasma used. The internal standard (THPFOS) was added to all plasma and serum samples (except Blanks) for a final concentration o f approximately 200 ppb. The analytical method consisted o f a liquiddiquid extraction procedure followed by evaporation and reconstitution of the extract residue with 20 mM ammonium acetate in water: 20 mM ammonium acetate in methanol (30:70, v/v). The samples were analyzed by liquid chromatography/tandem mass spectrometry using an API 3000. The instrument was operated in the multiple reaction monitoring (MRM) mode under optimized conditions for PFOS, PFHS, PFOA, PFOSAA, PFOSA, M556 and M570 detection o f the negative ions formed by TurboIonSprayTM ionization. 3. SAM PLE ANALYSIS PFOS, PFHS, PFOA, PFOSAA, PFOSA, M556, M570, and THPFOS chromatographic peaks were integrated using the MacQuan software (version 1.6) with a smooth factor o f one. Quantitation was based upon quadratic regression analysis o f weighted (1/x2) calibration curves using area ratio vs. concentration utilizing Watson DMLIMS software (version 6.1.1.04). The samples were injected in a systematic order. Page 11 050473 Northwest Bioanalytcal Study No. NWBSOQ-128 Report No. NWBR01-066 For sample 11689, the measured concentration o f PFOS was corrected for the persistent level o f analyte present in the dilution matrix. The concentration is reported as a whole number and has not been rounded to 3 significant figures. 3.1. Acceptance Criteria For an analytical run to be accepted, it must have m et the acceptance criteria listed below which are consistent with regulatory and industry recommendations. Calibration Curve Each run will include calibration standards in duplicate at six or more concentrations covering the lower to upper limit o f quantitation. For all analytes except PFOSA and PFOSAA, at least three-fourths o f the calibration standard's back-calculated concentrations must be within 15% ( 20% for LLOQ) o f their individual target concentrations. For PFOSA and PFOSAA, at least three-fourths o f the calibration standard's back-calculated concentrations must be within 20% ( 25% for LLOQ) o f their individual target concentrations. A calibration standard will be considered an outlier if it is greater than two times the acceptance criteria for that standard. Lower Limit o f Quantitation The back-calculated concentrations o f at least one o f the duplicate lowest points in the calibration curve must be within 25% of the target concentration for PFOSA and PFOSAA to qualify as the LLOQ and within 20% o f the target concentration to qualify as the LLOQ for all other analytes. If this criterion is not met, the next level is subjected to the same test and the LLOQ raised accordingly. Quality Control Samples Each analytical run will include low, medium and high QC samples in duplicate. The measured concentrations of at least two-thirds o f all analytical QCs must be within 20% o f their target concentrations ( 25% for PFOSA and PFOSAA), and no two QCs at the same concentration can be outside the limit. If study samples require Page 12 00474 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 dilution, a dilution QC will be analyzed in triplicate for each dilution level (except for PFOSA and PFOSAA which should not be diluted with control matrix). At least two dilution QCs at each level must be within 20% o f its target concentrations in order to accept diluted study samples at that level. The dilution QC acceptance is independent o f the undiluted analytical QC acceptance. 4. RESULTS AND DISCUSSION Serum sample results obtained using plasma curves for PFHS, PFOA, PFOSAA, PFOSA, M556, and M570 did not meet NWB SOP requirements for validation. Results may vary on average up to 26% from results obtained using human serum calibration curves at some concentration levels for PFHS, PFOA, PFOSAA, M556, and M570. For PFOSA, results may vary on average up to 43% from results obtained using human serum calibration curves. These data are reported in Assay Revalidation Addendum Report NWBROO-122 [5.3]. However, in order to obtain the lower limit o f quantitation o f less than 5 ppb required by the sponsor, it was necessary to use plasma calibration curves. Each accepted run met the acceptance criteria set for the calibration curve points, for the lower limit o f quantitation (LLOQ) and for the analytical quality control (QC) samples. Run Analyte Regression Extraction No. Status Date 1 PFOS Accepted 2 7 -N o v -2 0 0 0 1 PFOSA Accepted 27-NO V-2000 1 PFOSAA Accepted 27-NO V-2000 1 PFOA Accepted 27-NO V-2000 I PFHS Accepted 27-NO V-2000 1 M 556 Accepted 27-NO V-2000 1 M 570 Accepted 27-NO V-2000 2 PFOS Accepted 27-NO V-2000 2 PFOSA Accepted 27-NO V-2000 2 PFOSAA Accepted 2 7 -N o v -2 0 0 0 2 PFOA Accepted 27-NO V-2000 2 PFHS Accepted 27-NO V-2000 Assay Date 27-NOV-2000 27-N O V -2000 27-NOV-2000 27-N O V -2000 27-NOV-2000 27-N o v-2 000 27-NOV-2000 28-NOV-2000 28-N O V -2000 2 8-N ov-2000 28-N O V -2000 28-NOV-2000 LLOQ ULOQ 3.94 1.00 1.60 1.92 1.36 2.50 1.00 3.94 1.00 1.60 1.92 1.36 414 500 501 481 523 500 500 414 500 501 481 523 Comment Page 13 000475 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Run Analyte Regression Extraction No. Status Date Assay Date LLOQ ULOQ Comment 2 M356 Accepted 27-NOV-2000 28-NOV-2000 2.50 500 2 M570 Accepted 27-NOV-2000 28-NOV-2000 1.00 3 PFOS - - - 3 PFOSA - - - 3 PFOSAA - - - 3 PFOA - - - 500 Run aborted due to power outage (repeated in run 6) Run aborted due to power outage (repeated in run 6) Run aborted due to power outage (repeated in run 6) Run aborted due to power outage (repeated in run 6) 3 PFHS - - - Run aborted due to power outage (repeated in run 6) 3 M556 - - - Run aborted due to power outage (repeated in run 6) 3 M570 - - - Run aborted due to power outage (repeated in run 6) 4 PFOS Accepted 21-Mar-2001 23-Mar-2001 3.94 414 4 PFOSA Accepted 21-Mar-2001 23-Mar-2001 1.00 500 4 PFOSAA Accepted 21-Mar-2001 23-Mar-2001 1.60 501 4 PFOA Accepted 21-Mar-2001 23-Mar-2001 1.92 481 4 PFHS Accepted 21-Mar-2001 23-Mar-200l 1.36 523 4 M556 Rejected 21-Mar-2001 23-Mar-200l 2.50 500 QCs failed 4 M570 Rejected 21-Mar-2001 23-Mar-2001 1.00 500 QCs failed 5 PFOS Accepted 22-Mar-2001 24-Mar-2001 3.94 414 5 PFOSA Accepted 22-Mar-200l 24-Mar-2001 1.00 500 5 PFOSAA Accepted 22-Mar-2001 24-Mar-2001 1.60 501 5 PFOA Accepted 22-Mar-2001 24-Mar-2001 1.92 481 5 PFHS Accepted 22-Mar-2001 24-Mar-2001 1.36 523 5 M556 Accepted 22-Mar-2001 24-Mar-2001 2.50 500 5 M570 Accepted 22-Mar-2001 24-Mar-2001 1.00 500 6 PFOS Accepted 26-Mar-2001 26-Mar-2001 4.27 414 6 PFOSA Accepted 26-Mar-2001 26-Mar-2001 1.40 500 6 PFOSAA Accepted 26-Mar-2001 26-Mar-2001 2.80 502 6 PFOA Accepted 26-Mar-200l 26-Mar-2001 2.11 482 6 PFHS Accepted 26-Mar-2001 26-Mar-2001 2.09 523 Page 14 GS470 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBROl-066 Run Analyte Regression Extraction No. Status Date Assay Date LLOQ ULOQ Comment 6 M556 Accepted 26-Mar-2001 26-Mar-200l 3.20 501 6 M570 Accepted 26-Mar-2001 26-Mar-2001 1.80 501 7 PFOS Accepted 26-Mar-2001 26-Mar-2001 4.27 414 7 PFOSA Accepted 26-Mar-2001 26-Mar-2001 1.40 500 7 PFOSAA Accepted 26-Mar-2001 26-Mar-2001 2.80 502 7 PFOA Accepted 26-Mar-2001 26-Mar-2001 2.11 482 7 PFHS Accepted 26-Mar-2001 26-Mar-2001 2.09 523 7 M556 Accepted 26-Mar-2001 26-Mar-2001 3.20 501 7 M570 Accepted 26-Mar-2001 26-Mar-2001 1.80 501 8 PFOS Accepted 28-Mar-200l 28-Mar-2001 4.27 414 8 PFOSA Accepted 28-Mar-2001 28-Mar-2001 1.40 500 8 PFOSAA Accepted 28-Mar-2Q01 28-Mar-2001 2.80 502 8 PFOA Accepted 28-Mar-2001 28-Mar-2001 2.11 482 8 PFHS Accepted 28-Mar-2001 28-Mar-2001 2.09 523 8 M556 Accepted 28-Mar-2001 28-Mar-2001 3.20 501 8 M570 Accepted 28-Mar-2001 28-Mar-2001 1.80 501 9 PFOS Accepted 28-Mar-2001 28-Mar-2001 4.27 414 9 PFOSA Accepted 28-Mar-2001 28-Mar-2001 1.40 500 9 PFOSAA Accepted 28-Mar-2001 28-Mar-2001 2.80 502 9 PFOA Accepted 28-Mar-2001 28-Mar-200i 2.11 482 9 PFHS Accepted 28-Mar-2001 28-Mar-2001 2.09 523 9 M556 Rejected 28-Mar-2001 28-Mar-2001 3.20 501 Low QCs failed 9 M570 Rejected 28-Mar-2001 28-Mar-2001 1.80 501 Curve and QC fail 10 PFOS. Accepted 30-Mar-2001 30-Mar-2001 4.27 414 10 PFOSA Accepted 30-Mar-2001 30-Mar-2001 1.40 500 10 PFOSAA Accepted 30-Mar-2001 30-Mar-2001 2.80 502 10 PFOA Accepted 30-Mar-2001 30-Mar-2001 2.11 482 10 PFHS Accepted 30-Mar-2001 30-Mar-2001 2.09 523 10 M556 Accepted 30-Mar-2001 30-Mar-2001 3.20 501 10 M570 Accepted 30-Mar-2001 30-Mar-2001 1.80 501 11 PFOS Accepted 30-Mar-2001 30-Mar-2001 4.27 414 11 PFOSA Accepted 30-Mar-2001 30-Mar-2001 1.40 500 11 PFOSAA Rejected 30-Mar-2001 30-Mar-2001 2.80 502 Curve fails Page 15 0G0477 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Run Analyte Regression Extraction No. Status Date Assay Date LLOQ ULOQ Comment 11 PFOA Rejected 30-Mar-200l 30-Mar-2001 2.11 482 Curve fails 11 PFHS Accepted 30-Mar-2001 30-Mar-2001 2.09 523 11 M556 Accepted 30-Mar-200l 30-Mar-2001 3.20 501 11 M570 Rejected 30-Mar-2001 30-Mar-2001 1.80 501 Curve fails 12 M556 Accepted 28-Mar-2001 01-Apr-2001 3.20 501 Run 12 was a reinjection o f run 9 for M556 and M570 only 12 M570 Accepted 28-Mar-2001 01-Apr-2001 1.80 501 Run 12 was a reinjection o f run 9 for M556 and M570 only 13 PFOS Accepted 02-Apr-2001 02-Apr-2001 4.27 414 13 PFOSA Accepted 02-Apr-2001 02-Apr-2001 1.40 500 13 PFOSAA Accepted 02-Apr-200I 02-Apr-2001 2.80 502 13 PFOA Accepted 02-Apr-2001 02-Apr-2001 2.11 482 13 PFHS Accepted 02-Apr-2001 02-Apr-2001 2.09 523 13 M556 Rejected 02-Apr-2001 02-Apr-2001 3.20 501 Low QCs failed 13 M570 Accepted 02-Apr-2001 02-Apr-2001 1.80 501 14 PFOS Accepted 04-Apr-2001 07-Apr-2001 4.27 414 14 PFOSA Accepted 04-Apr-2001 07-Apr-2001 1.40 500 14 PFOSAA Accepted 04-Apr-2001 07-Apr-2001 2.80 502 14 PFOA Accepted 04-Apr-2001 07-Apr-2001 2.11 482 14 PFHS Accepted 04-Apr-2001 07-Apr-2001 2.09 523 14 M556 Accepted 04-Apr-2001 07-Apr-2001 3.20 501 14 M570 Accepted 04-Apr-2001 07-Apr-2001 1.80 501 15 PFOS Accepted 06-Apr-2001 09-Apr-2001 4.27 414 15 PFOSA Accepted 06-Apr-2001 09-Apr-2001 1.40 500 15 PFOSAA Accepted 06-Apr-2001 09-Apr-2001 2.80 502 15 PFOA Accepted 06-Apr-2001 09-Apr-2001 2.11 482 15 PFHS Accepted 06-Apr-2001 09-Apr-2001 2.09 523 15 M556 Accepted 06-Apr-2001 09-Apr-2001 3.20 501 15 M570 Accepted 06-Apr-2001 09-Apr-2001 1.80 501 16 PFOS Accepted 09-Apr-2001 11-Apr-2001 4.27 414 16 PFOSA Accepted 09-Apr-2001 11-Apr-2001 1.40 500 16 PFOSAA Rejected 09-Apr-2001 11-Apr-2001 2.80 502 Curve fails Page 16 000478 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Run Analyte Regression Extraction No. Status Date Assay Date LLOQ ULOQ Comment 16 PFOA Rejected 09-Apr-2001 ll-Apr-2001 2.11 482 Curve fails 16 PFHS Accepted 09-Apr-2001 11-Apr-2001 2.09 523 16 M556 Rejected 09-Apr-2001 11-Apr-2001 3.20 501 Curve fails 16 M570 Rejected 09-Apr-2001 11-Apr-2001 1.80 501 Curve fails 17 PFOS Accepted 10-Apr-2001 12-Apr-2001 4.27 414 17 PFOSA Accepted 10-Apr-2001 12-Apr-2001 1.40 500 17 PFOSAA Accepted 10-Apr-2001 12-Apr-2001 2.80 502 17 PFOA Accepted 10-Apr-2001 12-Apr-2001 2.11 482 17 PFHS Accepted 10-Apr-2001 12-Apr-2001 2.09 523 17 M556 Accepted 10-Apr-2001 12-Apr-2001 3.20 501 17 M570 Accepted 10-Apr-2001 12-Apr-2001 1.80 501 18 PFOS Accepted 19-Apr-2001 23-Apr-2001 4.27 414 18 PFOSA Accepted 19-Apr-2001 23-Apr-2001 1.40 500 18 PFOSAA Accepted 19-Apr-2001 23-Apr-200I 2.80 502 18 PFOA Accepted 19-Apr-2001 23-Apr-2001 2.11 482 18 PFHS Accepted 19-Apr-2001 23-Apr-2001 2.09 523 18 M556 Accepted 19-Apr-2001 23-Apr-2001 3.20 501 18 M570 Rejected 19-Apr-2001 23-Apr-2001 1.80 501 Curve and Low QC failed 19 PFOS Rejected 09-Apr-2001 14-Apr-2001 4.02 414 Reinjection of run 16: Analyte results not needed 19 PFOSA Rejected 09-Apr-2001 14-Apr-2001 1.30 500 Reinjection of run 16: Analyte results not needed 19 PFOSAA Accepted 09-Apr-2001 14-Apr-2001 2.80 502 Reinjection of run 16 19 PFOA Accepted 09-Apr-2001 14-Apr-2001 2.11 482 Reinjection of run 16 19 PFHS Rejected 09-Apr-2001 14-Apr-2001 2.09 523 Reinjection of run 16: Analyte results not needed 19 M556 Accepted 09-Apr-2001 14-Apr-2001 3.20 501 Reinjection of run 16 19 M570 Accepted 09-Apr-2001 14-Apr-2001 1.80 501 Reinjection of run 16 20 PFOS Accepted 06-Apr-2001 13-Apr-2001 4.27 414 Pre-study assay evaluation (new Chinese plasma pool and QCs) 20 PFOSA Accepted 06-Apr-2001 13-Apr-2001 1.40 500 Pre-study assay evaluation (new Chinese plasma pool and QCs) Page 17 0S04V9 Northwest Bioanalytieal Study No. NWBSOO-128 Report No. NWBRO1-066 Run Analyte Regression Extraction No. Status Date Assay Date LLOQ ULOQ Comment 20 PFOSAA Accepted 06-Apr-2001 13-Apr-2001 2.80 502 Pre-study assay evaluation (new Chinese plasma pool and QCs) 20 PFOA Accepted 06-Apr-2001 13-Apr-200l 2.10 482 Pre-study assay evaluation (new Chinese plasma pool and QCs) 20 PFHS Accepted 06-Apr-2001 13-Apr-2001 2.09 523 Pre-study assay evaluation (new Chinese plasma pool and QCs) 20 M556 Rejected 06-Apr-2001 13-Apr-2001 1.60 501 Pre-study assay evaluation (new Chinese plasma pool and QCs); Low QC fail. 20 M570 Accepted 06-Apr-2001 13-Apr-2001 1.90 501 Pre-study assay evaluation (new Chinese plasma pool and QCs) 21 PFOSAA Accepted 17-Apr-2001 22-Apr-2001 2.80 502 Run was analyzed for PFOSAA, PFOA and M570 only 21 PFOA Accepted 17-Apr-2001 22-Apr-2001 2.11 482 Run was analyzed for PFOSAA, PFOA and M570 only 21 M570 Accepted 17-Apr-2001 22-Apr-2001 1.80 501 Run was analyzed for PFOSAA, PFOA and M570 only 22 M570 Accepted 19-Apr-2001 24-Apr-2001 1.80 501 Reinjection o f run 18 for M570 only 23 PFOS Accepted 02-May-2001 05-May-2001 3.86 414 Pre-study assay evaluation o f new low QC 23 PFOSA Accepted 02-May-2001 05-May-2001 1.50 501 Pre-study assay evaluation of new low QC 23 PFOSAA Accepted 02-May-2001 05-May-2001 2.40 501 Pre-study assay evaluation o f new low QC 23 PFOA Accepted 02-May-2001 05-May-2001 2.31 482 Pre-study assay evaluation o f new low QC 23 PFHS Accepted 02-May-2001 05-May-2001 2.50 523 Pre-study assay evaluation o f new low QC 23 M556 Accepted 02-May-2001 05-May-2001 3.80 501 Pre-study assay evaluation o f new low QC 23 M570 Accepted 02-May-2001 05-May-200l 2.30 501 Pre-study assay evaluation o f new low QC 24 PFOSAA Rejected 10-May-2001 10-May-2001 1.50 501 Sample preparation error 24 PFOA Rejected 10-May-2001 10-May-2001 25.4 482 Sample preparation error Page 18 030480 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBR01-066 Run Analyte Regression Extraction No. Status Date 24 PFHS Rejected 10-May-2001 24 M570 Rejected 1Q-May-20Q1 25 PFOSAA Accepted 11-May-2001 25 PFOA Accepted 11-May-2001 25 PFHS Rejected 11-May-2001 25 M570 Accepted 11-May-2001 Assay Date LLOQ ULOQ Comment 10-May-2001 10-May-2001 11-May-2001 11-May-2001 11-May-2001 11-May-2001 2.50 2.30 1.30 1.44 1.36 1.00 523 Sample preparation error 501 Sample preparation error 500 481 522 Analyte results not needed 500 In run 4 for PFOSA and PFOSAA, one of the medium QC samples gave extremely high results. These results appear to skew the overall statistics for these analytes. Without this "outlier", the overall %CV was 9.2% for PFOSA and 12.3% for PFOSAA. The overall %Bias was 2.0% for PFOSA and 5.3% for PFOSAA. In run 8 for PFOA, one o f the low QC samples gave an extremely low result o f 0.161 ppb. This result appears to skew the overall statistics for the analyte. Without this "outlier", the overall %CV was 14.1% and the %Bias was -10.0% / Any known circumstances that may have affected the quality or integrity o f the data are included in this report. 5. REFERENCES 5.1. 3M Company Protocol EPI-0013. "Identification ofFluorochemicals in Sera of American Red Cross Blood Donors in the United States." September 29, 2000. 5.2. C. Sakashita. "Quantitative Determination o f PFOS, PFOSA, PFOSAA, POAA, PFHS, M556 and M570 in Human Serum by LC/MS/MS." Assay Revalidation Report. NWB Study NWBS00-040. NWB Report NW BR00-108. January 24, 2001. 5.3. C. Sakashita. "Quantitative Determination o f PFOS, PFOSA, PFOSAA, POAA, PFHS, M556 and M570 in Human Serum by LC/MS/MS." Assay Revalidation Addendum Report. NWB Study NWBS00-040. NWB Report NW BR00-122. November 20, 2001. Page 19 0S0481 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NW BR0I-066 6. DATA R ET EN TIO N The raw data and final report for this study will be stored in the NWB Archives, 1121 East 3900 South, Salt Lake City, UT 84124 per regulations and contract agreement. After submission o f the final report to the Sponsor, remaining study samples will be stored under required conditions until confirmation o f Sample Disposition/Retum Authorization is received from the Sponsor. 3M Company will be notified concerning final disposition o f records at completion o f contract obligations. Page 20 0S0482 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 1. Calibration Curve Summary for PFOS Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 28-NOV-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2Q01 28-Mar-2001 28-Mar-2001 30-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 11-Apr-2001 12-Apr-2001 23-Apr-2001 Run Number 1 2 4 5 6 7 8 9 10 11 13 14 15 16 17 18 ABC -0.000031 -0.000027 0.000002 -0.000002 -0.000001 0.000003 0.000000 0.000000 0.000000 0.000001 -0.000003 -0.000010 0.000004 -0.000006 -0.000009 -0.000002 0.052622 0.049661 0.039134 0.009354 0.010776 0.035721 0.037629 0.010093 0.011733 0.047343 0.045861 0.039827 0.045781 0.058787 0.055527 0.017703 0.012630 0.017690 0.020796 0.001128 -0.003903 0.024340 0.025011 0.007090 0.002809 0.024473 0.035036 0.014677 0.046887 -0.001384 0.020155 0.000222 R-Squared LLOQ ULOQ 0.9958 0.9926 0.9869 0.9985 0.9867 0.9943 0.9931 0.9895 0.9947 0.9733 0.9973 0.9925 0.9919 0.9942 0.9976 0.9935 3.94 414 3.94 414 3.94 414 3.94 414 4.27 414 4.27 414 4.27 414 4.27 414 4.27 414 4.27 414 4.27 414 4.27 414 4.27 414 4.27 414 4.27 414 4.27 414 Mean S.D. %CV n -0.000005 0.000010 -200.0 16 0.035472 0.017605 49.6 16 0.015479 0.014172 91.6 16 0.9920 0.0060 0.6 16 A, B, and C are coefficients used to define the calibration curve. Page 21 000483 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 2. Calibration Curve Summary for PFHS Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 28-NOV-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 30-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 11-Apr-2001 12-Apr-2001 23-Apr-2001 Run Number 1 2 4 5 6 7 8 9 10 11 13 14 15 16 17 18 A B C R-Squared LLOQ ULOQ -0.000013 -0.000013 -0.000002 -0.000002 -0.000002 -0.000004 -0.000003 -0.000002 -0.000001 0.000000 -0.000004 -0.000006 -0.000002 -0.000007 -0.000007 -0.000004 0.030678 0.031308 0.021861 0.007620 0.008120 0.023053 0.025470 0.008701 0.008569 0.028707 0.021870 0.021837 0.022158 0.029426 0.026000 0.011306 0.025452 0.026252 0.020425 0.006999 -0.002637 0.006759 0.002418 0.002381 0.003686 0.027904 0.016367 0.012060 0.030931 0.013375 0.009029 0.008022 0.9949 0.9950 0.9959 0.9966 0.9953 0.9902 0.9892 0.9972 0.9836 0.9813 0.9858 0.9915 0.9901 0.9881 0.9970 0.9875 1.36 523 1.36 523 1.36 523 1.36 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 Mean S.D. % cv n -0.000004 0.000004 -100.0 16 0.020418 0.008650 42.4 16 0.013089 0.010370 79.2 16 0.9912 0.0050 0.5 16 A, B, and C are coefficients used to define the calibration curve. Page 22 000484 Northwest Bioanaytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 3. Calibration Curve Summary for PFOA Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 28-Nov-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 12-Apr-2001 14-Apr-2001 22-Apr-2001 23-Apr-2001 11-May-2001 Run Number 1 2 4 5 6 7 8 9 10 13 14 15 17 19 21 18 25 A B C R-Squared LLOQ ULOQ -0.000001 -0.000002 0.000001 -0.000001 0.000000 0.000003 0.000002 0.000000 0.000000 -0.000001 -0.000003 0.000002 0.000000 -0.000001 0.000000 -0.000002 -0.000001 0.015479 0.016334 0.008393 0.007290 0.007392 0.008327 0.008675 0.007316 0.007744 0.008171 0.009779 0.007753 0.007833 0.007768 0.015981 0.016857 0.012990 0.005741 0.015052 0.007706 0.002187 -0.000487 0.004956 0.015973 0.005861 0.003135 0.003088 0.000405 0.019137 0.004324 0.001433 -0.001298 0.000933 -0.002765 0.9933 0.9877 0.9842 0.9979 0.9898 0.9865 0.9825 0.9940 0.9964 0.9901 0.9926 0.9872 0.9945 0.9954 0.9878 0.9905 0.9962 1.92 481 1.92 481 1.92 481 1.92 481 2.11 482 2.11 482 2.11 482 2.11 482 2.11 482 2.11 482 2.11 482 2.11 482 2.11 482 2.11 482 2.11 482 2.11 482 1.44 481 Mean S.D. %CV n 0.000000 0.000002 NCL 17 0.010240 0.003645 35.6 17 0.005022 0.006254 124.5 17 0.9910 0.0045 0.5 17 A, B, and C are coefficients used to defme the calibration curve. NCL = not calculable Page 23 C004&a Northwest Bioanalyticai Study No. NWBSOO-128 Report No. NWBRO1-066 Table 4. Calibration Curve Summary for PFOSAA Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 28-NOV-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 12-Apr-2001 14-Apr-2001 22-Apr-2001 23-Apr-2001 11-May-2001 Run Number 1 2 4 5 6 7 8 9 10 13 14 15 17 19 21 18 25 AB C R-Squared LLOQ ULOQ 0.000000 0.013246 0.000005 0.012198 0.000001 0.007894 0.000001 0.006730 0.000002 0.008322 0.000001 0.007111 0.000001 0.005138 0.000002 0.006742 0.000003 0.007717 0.000008 0.024032 0.000001 0.033688 0.000014 0.029651 0.000006 0.025674 0.000012 0.026710 0.000004 0.007075 0.000004 0.007908 0.000002 0.012005 0.007247 0.010441 0.004964 0.010546 -0.001161 -0.001354 -0.004421 0.011207 0.008093 0.015403 0.011384 0.017800 0.007502 -0.009422 -0.004642 0.000878 0.000362 0.9804 0.9797 0.9685 0.9935 0.9836 0.9760 0.9798 0.9666 0.9848 0.9884 0.9867 0.9846 0.9944 0.9813 0.9735 0.9744 0.9937 1.60 501 1.60 501 1.60 501 1.60 501 2.80 502 2.80 502 2.80 502 2.80 502 2.80 502 2.80 502 2.80 502 2.80 502 2.80 502 2.80 502 2.80 502 2.80 502 1.30 500 Mean S.D. %CV n 0.000004 0.000004 100.0 17 0.014226 0.009564 67.2 17 0.004990 0.007661 153.5 17 0.9818 0.0083 0.8 17 A, B, and C are coefficients used to define the calibration curve. Page 24 000486 Northwest Bioanalyticai Study No. NWBS00-128 Report No. NWBRO1-066 Table 5. Calibration Curve Summary for PFOSA Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 28-NOV-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 30-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 11-Apr-2001 12-Apr-2001 23-Apr-2001 Run Number 1 2 4 5 6 7 8 9 10 11 13 14 15 16 17 18 A B C R-Squared LLOQ ULOQ -0.000041 -0.000025 0.000002 -0.000002 -0.000001 -0.000002 0.000001 0.000000 -0.000003 0.000018 -0.000008 -0.000011 -0.000006 0.000034 -0.000010 0.000007 0.096146 0.087183 0.034802 0.018868 0.023192 0.034174 0.032420 0.022395 0.023907 0.108434 0.108295 0.097511 0.119455 0.124021 0.129002 0.040292 0.018081 0.015131 0.013699 0.003711 -0.012070 0.000108 0.015115 0.000709 0.000482 0.040511 0.054874 0.020730 0.031195 -0.030446 0.003170 0.010493 0.9920 0.9931 0.9847 0.9985 0.9931 0.9956 0.9965 0.9848 0.9934 0.9882 0.9885 0.9819 0.9923 0.9870 0.9944 0.9936 1.00 500 1.00 500 1.00 500 1.00 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 Mean S.D. %CV n -0.000003 0.000016 -533.3 16 0.068756 0.042828 62.3 16 0.011593 0.020139 173.7 16 0.9911 0.0047 0.5 16 A, B, and C are coefficients used to define the calibration curve. Page 25 000487 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 6. Calibration Curve Summary for IVI556 Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date 27-Nov-2000 28-NOV-2000 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 30-Mar-2001 30-Mar-2001 01-Apr-2001 07-Apr-2001 09-Apr-2001 12-Apr-2001 14-Apr-2001 23-Apr-2001 Run Number 1 2 5 6 7 8 10 11 12 14 15 17 19 18 AB C R-Squared LLOQ ULOQ 0.000001 0.000003 0.000001 0.000001 0.000001 0.000001 0.000001 0.000003 0.000001 0.000001 0.000003 0.000002 0.000003 0.000002 0.008245 0.007109 0.002937 0.003973 0.006232 0.004865 0.002628 0.004105 0.002392 0.007457 0.006599 0.006819 0.006308 0.003128 0.002637 0.006480 0.003249 -0.002024 -0.005748 -0.004285 0.000476 0.002505 0.001473 0.002028 0.008776 -0.003271 -0.001438 0.001358 0.9851 0.9931 0.9943 0.9809 0.9928 0.9923 0.9939 0.9789 0.9825 0.9924 0.9891 0.9913 0.9886 0.9870 2.50 500 2.50 500 2.50 500 3.20 501 3.20 501 3.20 501 3.20 501 3.20 501 3.20 501 3.20 501 3.20 501 3.20 501 3.20 501 3.20 501 Mean S.D. %CV n 0.000002 0.000001 50.0 14 0.005200 0.001993 38.3 14 0.000873 0.004007 459.0 14 0.9887 0.0051 0.5 14 A, B, and C are coefficients used to define the calibration curve. Page 26 0S488 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 7. Calibration Curve Summary for M570 Quadratic weighted I/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 28-Nov-2000 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 30-Mar-2001 01-Apr-2001 02-Apr-2001 07-Apr-200l 09-Apr-2001 12-Apr-2001 14-Apr-2001 22-Apr-2001 24-Apr-2001 11-May-2001 Run Number 1 2 5 6 7 8 10 12 13 14 15 17 19 21 22 25 A B C R-Squared LLOQ ULOQ -0.000003 0.000002 0.000000 0.000002 0.000001 0.000002 0.000001 0.000001 0.000007 -0.000001 0.000011 0.000004 0.000009 0.000001 0.000018 0.000000 0.022236 0.021764 0.003326 0.003649 0.017625 0.013605 0.003548 0.003371 0.027857 0.034478 0.032868 0.030324 0.030213 0.003114 0.038537 0.004063 0.026662 0.021002 0.003631 -0.000239 0.009909 0.006783 0.001744 0.002595 0.035353 0.018645 0.046246 0.016921 0.008691 -0.002037 0.040536 -0.001174 0.9910 0.9902 0.9937 0.9851 0.9880 0.9911 0.9859 0.9779 0.9890 0.9854 0.9863 0.9936 0.9817 0.9880 0.9873 0.9955 1.00 500 1.00 500 1.00 500 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.00 500 Mean S.D. %CV n 0.000003 0.000005 166.7 16 0.018161 0.013225 72.8 16 0.014704 0.015506 105.5 16 0.9881 0.0045 0.5 16 A, B, and C are coefficients used to define the calibration curve. Page 27 0S0489 Northwest Bioanalytical Study No. N W BS00-128 Report No. NWBRO1-066 Table 8. Back-Calculated Concentrations of Calibration Standards for PFOS Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 Run Number 1 28-NOV-2000 2 23-Mar-2001 4 24-Mar-2001 5 26-Mar-2001 6 26-Mar-2001 7 28-Mar-2001 8 28-Mar-2001 9 30-Mar-2001 10 3.94 4.27 5.17 5.50 11.3 11.7 23.6 24.0 44.2 44.5 85.4 85.5 209 332 414 4.04 5.05 11.1 24.1 48.3 80.9 234 307 432 3.98 5.02 11.4 *44.7 **18.9 77.2 209 321 417 4.05 4.91 10.9 25.4 49.5 84.5 234 299 450 4.00 5.24 10.6 *42.1 **18.1 74.2 204 319 416 4.01 5.70 10.6 26.0 41.2 81.4 232 293 419 3.42 5.60 11.3 20.3 48.5 89.2 186 380 399 3.99 5.05 11.6 23.2 46.8 82.0 209 351 421 3.94 5.07 11.6 24.2 44.0 81.3 205 314 415 4.13 4.95 11.4 22.1 42.0 73.8 191 319 419 4.46 5.64 13.7 23.7 53.9 81.8 223 368 399 4.75 5.64 11.4 25.7 46.6 80.7 214 365 392 3.85 5.34 11.4 23.8 41.9 86.0 218 304 422 4.25 5.23 12.4 24.8 52.8 86.1 203 332 437 4.54 5.26 11.0 24.3 40.5 80.3 190 340 406 5.01 5.55 11.3 26.7 49.0 89.0 207 335 415 4.07 4.86 10.0 23.0 46.2 76.3 224 314 415 4.55 4.89 13.0 24.7 45.4 81.5 199 345 391 4.54 5.10 10.8 23.8 44.1 86.6 221 342 413 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to preparation error Page 28 000430 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 8. Back-Calculated Concentrations of Calibration Standards for PFOS (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date Run Number \ 30-Mar-2001 11 02-Apr-2001 13 07-Apr-2001 09-Apr-2001 14 15 11-Apr-2001 16 12-Apr-2001 17 23-Apr-2001 18 3.94 4.27 5.17 5.50 11.3 11.7 23.6 24.0 44.2 44.5 85.4 85.5 209 332 414 5.45 4.97 10.6 20.5 44.9 81.5 204 311 397 3.63 5.49 11.1 24.2 52.8 106 169 381 428 4.16 5.28 11.1 24.8 44.9 85.4 213 351 426 4.59 5.54 11.5 22.9 46.0 86.2 208 337 374 4.24 5.75 12.2 26.9 46.3 88.3 225 373 409 4.47 4.96 11.2 21.3 42.0 81.9 195 329 380 5.00 5.11 10.5 25.9 47.1 90.8 223 359 407 4.03 5.46 10.5 23.5 45.0 80.4 206 320 394 4.66 5.37 11.1 22.8 47.4 72.9 224 328 395 3.92 5.69 11.6 24.5 47.7 87.9 209 342 417 4.45 5.20 11.3 25.4 44.2 86.4 196 328 435 ***2.26 5.38 12.5 23.3 45.9 82.6 207 341 405 4.61 5.25 11.2 25.3 44.9 76.0 201 314 377 4.33 5.25 11.3 22.9 48.1 90.0 230 364 426 Mean S.D. %CV %Bias n 3.93 0.208 5.3 -0.3 8 4.42 0.411 9.3 3,5 23 5.21 5.30 11.1 11.4 23.9 24.0 46.4 46.2 81.3 84.1 210 335 411 0.290 0.263 0.407 0.830 2.01 1.57 3.18 3.39 4.48 6.80 15.1 23.8 17.8 5.6 5.0 3.7 7.3 8.4 6.5 6.9 7.3 5.5 8.1 7.2 7.1 4.3 0.8 -3.6 -1.8 -2.6 1.3 0.0 5.0 3.8 -4.8 -1.6 0.5 0.9 -0.7 8 24 8 24 6 24 6 24 8 24 32 32 32 *** Sample deactivated due to unacceptable internal standard response Page 29 G0481 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 9. Back-Calculated Concentrations of Calibration Standards for PFHS Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 Run Number 1 28-NOV-2000 2 23-Mar-2001 4 24-Mar-2001 5 26-Mar-2001 6 1.36 1.39 1.46 1.42 1.42 1.41 1.31 1.33 1.48 26-Mar-2001 7 28-Mar-2001 8 28-Mar-2001 9 30-Mar-2001 10 2.09 2.92 3.65 10.7 11.5 26.5 27.1 52.6 53.2 104 105 262 418 523 2.66 10.8 27.4 54.5 2.54 11.4 *54.5 **26.8 2.78 10.7 28.0 57.6 2.46 10.9 *50.7 **25.0 3.13 10.6 28.1 52.5 2.71 10.8 28.5 48.1 2.76 11.1 26.5 55.2 2.58 11.3 27.3 53.8 2.08 3.70 11.0 26.9 50.8 2.12 3.64 10.7 28.7 62.9 2.42 3.23 11.6 27.3 52.6 1.94 3.39 12.4 29.4 54.0 2.20 2.96 12.3 30.9 60.1 2.30 3.21 11.3 27.6 52.9 2.22 3.66 11.6 26.4 52.3 1.99 3.49 12.0 28.8 55.5 2.11 2.83 13.2 31.4 51.1 2.27 3.71 10.3 28.8 58.8 * Sample deactivated as an outlier (not included in summary statistics) * * Sample deactivated due to preparation error 98.9 278 373 508 106 271 415 564 101 274 386 536 102 257 421 534 98.5 283 405 527 104 237 449 512 99.5 261 432 528 101 255 389 545 98.2 247 409 525 102 271 441 516 90.7 242 398 472 108 294 418 594 94.6 236 437 533 104 243 415 545 105 255 455 496 96.2 254 412 544 107 223 465 550 91.3 239 374 565 Page 30 G004S2 Northwest Bioanalytical Study No. N W BS00-128 Report No. NWBR01 -066 Table 9. Back-Calculated Concentrations of Calibration Standards for PFHS (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date Run 1.36 Number 2.09 2.92 3.65 10.7 11.5 26.5 27.1 52.6 30-Mar-2001 11 2.62 2.90 12.0 24.6 1.89 3.36 11.1 28.0 02-Apr-2001 13 1.77 2.88 10.9 27.4 2.68 3.61 11.7 27.2 07-Apr-2001 14 1.97 2.94 11.4 26.7 2.43 3.59 11.9 30.9 09-Apr-2001 15 2.60 3.30 11.0 28.0 1.75 3.56 10.7 27.2 11-Apr-2001 16 2.28 2.97 11.3 26.6 2.23 3.20 12.7 29.3 12-Apr-2001 17 2.12 3.87 10.9 28.5 ***1.93 3.29 12.0 28.3 23-Apr-2001 18 2.54 3.15 10.7 27.1 1.94 3.33 11.0 26.4 53.2 104 105 262 418 523 53.2 99.0 249 406 502 66.3 114 230 468 537 52.9 107 255 439 506 57.4 108 266 445 485 51.5 98.0 270 431 497 54.6 103 268 422 523 56.4 110 264 449 514 55.9 99.4 263 411 498 53.8 85.9 251 433 482 58.5 106 288 445 514 53.0 103 248 419 552 55.8 98.0 253 425 519 50.2 114 251 427 502 63.9 107 282 398 522 Mean S.D. %CV %Bias n 1.40 0.0585 4.2 2.9 8 2.19 2.70 3.32 11.0 11.5 27.6 28.0 53.6 55.6 0.266 0.205 0.305 0.288 0.717 0.715 1.60 3.19 4.29 12.1 7.6 9.2 2.6 6.2 2.6 5.7 6.0 7.7 4.8 -7.5 -9.0 2.8 0.0 4.2 3.3 1.9 4.5 23 8 24 8 24 6 24 6 24 *** Sample deactivated due to unacceptable internal standard response 101 102 258 422 523 2.59 7.17 17.1 24.2 26.4 2.6 7.0 6.6 5.7 5.0 -2.9 -2.9 -1.5 1.0 0.0 8 24 32 32 32 Page 31 OS04 S3 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 10. Back-Calculated Concentrations of Calibration Standards for PFOA Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date Run 1.92 3.36 10.6 25.0 49.0 97.1 241 385 481 Number 27-NOV-2000 l 1.88 3.04 9.65 25.3 51.6 87.9 252 356 457 2.13 3.14 11.5 *53.4 **22.5 103 261 387 503 28-NOV-2000 2 1.77 2.97 10.2 28.0 52.8 93.6 244 390 478 2.37 2.78 10.9 *46.6 **19 9 94.2 247 372 483 23-Mar-2001 4 1.54 2.87 12.5 27.4 50.2 90.7 256 383 492 2.40 3.40 10.7 20.7 48.5 99.6 222 400 465 24-Mar-2001 5 1.89 3.05 10.4 24.4 51.5 92.7 243 399 477 2.05 3.38 10.6 26.2 51.4 94.9 236 380 480 Mean S.D. %CV %Bias n 2.00 3.08 10.8 25.3 51.0 94.6 245 384 480 0.295 0.222 0.869 2.63 1.48 4.79 14.1 14.4 12.9 14.8 7.2 8.0 10.4 2.9 5.1 5.8 3.8 2.7 4.2 -8.3 1.9 1.2 4.1 -2.6 1.7 -0.3 -0.2 8 8 8 6 6 8 34 10 10 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to sample preparation error Page 32 G004B4 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 10. Back-Calculated Concentrations of Calibration Standards for PFOA (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 12-Apr-2001 Run Number 6 7 8 9 10 13 14 15 17 2.11 3.56 10.8 25.2 49.2 97.3 241 386 482 2.49 1.87 *4.06 2.45 2.06 2.44 2.40 2.09 2.03 2.30 1.83 *3.48 2.06 *4.56 1.84 2.30 2.13 ***M3 3.57 9.76 24.0 49.0 92.5 244 355 501 3.25 10.3 26.8 59.1 93.8 255 396 466 3.37 11.5 23.1 46.7 87.7 234 387 440 2.72 10.2 29.1 52.2 103 275 385 501 *1.68 7.94 27.8 55.8 90.6 249 372 477 2.73 13.2 26.0 46.7 93.2 245 400 480 3.26 11.4 25.5 48.8 99.5 242 392 465 3.07 10.0 23.9 55.2 96.2 251 392 470 3.10 11.4 25.7 52.4 95.3 236 389 474 3.69 10.1 24.8 49.1 94.9 256 386 479 3.48 10.2 25.1 49.5 95.0 250 419 489 4.55 10.5 23.8 50.1 94.9 238 390 437 3.54 10.4 25.1 45.5 85.6 240 390 459 *5.97 13.2 23.9 52.7 95.5 238 408 498 *0.842 7.81 25.3 45.7 98.2 228 389 431 4.05 10.9 27.1 53.9 101 261 407 498 2.95 11.0 26.1 47.2 102 225 380 489 4.03 11.3 24.6 49.9 91.7 246 408 472 * Sample deactivated as an outlier (not included in summary statistics) *** Sample deactivated due to unacceptable internal standard response Page 33 0G04S5 Northwest Bioanalytical Study No. N W B S00-128 Report No. NWBRO1-066 Table 10. Back-Calculated Concentrations of Calibration Standards for PFOA (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 14-Apr-2001 22-Apr-2001 23-Apr-2001 Run Number 19 21 18 2.11 2.13 *6.30 1.71 2.62 2.40 1.85 3.56 10.8 25.2 49.2 97.3 241 386 482 3.41 *6.57 3.35 3.45 3.82 3.21 10.4 26.2 47.9 94.7 225 382 506 12.2 23.8 49.9 93.1 275 364 474 10.4 24.8 51.8 95.2 226 384 466 10.7 28.4 48.9 99.2 213 435 489 10.7 27.5 49.8 80.4 262 388 483 10.9 23.4 54.2 92.6 255 381 465 Mean S.D. %CV %Bias n 2.16 0.266 12.3 2.4 19 3.43 0.449 13.1 -3.7 20 10.7 25.5 50.5 94.4 245 1.24 1.64 3.42 5.09 14.1 11.6 6.4 6.8 5.4 5.8 -0.9 1.2 2.6 -3.0 1.7 24 24 24 24 34 * Sample deactivated as an outlier (not included in summary statistics) 391 475 16.8 20.1 4.3 4.2 1.3 -1.5 24 24 Page 34 CG04, Northwest Bioanalytical Study No. NWBS00-128 Repon No. NWBRO1-066 Table 10. Back-Calculated Concentrations of Calibration Standards for PFOA (Continued) Quadratic weighted l / x \ All concentrations are expressed as ppb. Run Date 11-May-2001 Run Number 25 1.44 2.88 10.1 24.5 48.5 96.6 241 385 481 1.46 2.95 9.39 25.2 45.5 90.0 245 399 482 1.33 3.14 11.0 26.3 45.6 94.6 242 371 487 Mean S.D. %CV %Bias n 1.40 3.05 10.2 25.8 45.6 92.3 245 384 480 ISD ISD ISD ISD ISD ISD 14.1 14.4 12.9 ISD ISD ISD ISD ISD ISD 5.8 3.8 2.7 -2.8 5.9 1.0 5.3 -6.0 -4.5 1.7 -0.3 -0.2 2 2 2 2 2 2 34 10 10 ISD = insufficient data points for statistical calculations Page 35 OO4S7 Northwest Bioanalytical Study No. NWBS0-128 Report No. NWBRO1-066 Table 11. Back-Calculated Concentrations of Calibration Standards for PFOSAA Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date Run 1.60 3.10 10.6 25.6 50.6 101 251 401 501 Number 27-NOV-2000 1 1.81 3.48 10.3 26.6 61.0 97.6 303 395 538 1.39 2.80 9.64 *50.8 **17.1 77.2 252 369 467 28-NOV-2000 2 1.45 2.36 8.59 24.5 51.0 92.0 282 364 491 1.77 3.84 12.0 *58.2 **22.6 101 293 399 491 23-Mar-2Q01 4 *7.76 4.18 10.6 24.9 46.5 94.5 301 321 525 1.32 3.23 10.3 17.3 59.0 108 243 459 460 24-Mar-2001 5 1.62 2.75 11.0 25.6 55.3 103 272 413 511 1.80 2.59 10.3 26.8 49.2 97.0 255 369 484 Mean S.D. %CV %Bias n 1.59 3.15 10.3 24.3 53.7 96.3 275 386 496 0.207 0.641 0.987 3.54 5.72 9.20 23.3 40.7 27.2 13.0 20.3 9.6 14.6 10.7 9.6 8.5 10.5 5.5 -0.6 1.6 -2.8 -5.1 6.1 -4.7 9.6 -3.7 - 1.0 7886 6 8 8 8 8 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to sample preparation error Page 36 GG04S8 Northwest Bioanalytical Study No. N W B S00-128 Report No. NW BR0I-066 Table 11. Back-Calculated Concentrations of Calibration Standards for PFOSAA (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date Run 1.30 Number 2.80 4.30 10.3 11.8 25.3 26.8 50.3 51.8 100 102 250 252 400 402 500 502 26-Mar-2001 6 2.68 3.87 12.0 23.8 48.1 86.7 250 358 505 2.99 4.57 *19.7 26.7 65.1 99.3 287 461 463 26-Mar-2001 7 3.63 4.22 11.3 28.1 59.3 90.3 292 463 446 2.44 3.48 10.4 26.7 45.8 108 282 380 459 28-Mar-2001 8 3.28 2.92 10.6 24.9 58.9 97.5 242 378 503 3.05 3.75 14.6 27.2 51.7 101 269 439 481 28-Mar-2001 9 3.68 4.64 11.8 33.2 59.2 110 257 380 516 2.43 3.02 9.06 21.9 52.8 88.1 302 386 473 30-Mar-2001 10 2.98 3.21 14.6 28.0 48.4 103 253 417 459 3.21 3.82 10.6 25.9 47.1 111 271 419 495 02-Apr-2001 13 2.32 5.07 11.0 27.2 54.9 101 280 433 513 3.13 4.16 10.7 24.3 54.1 97.1 262 388 443 07-Apr-2001 14 2.68 3.97 12.1 29.8 49.7 107 266 422 454 3.29 3.72 12.1 20.8 54.2 107 244 451 468 09-Apr-2001 15 2.87 3.34 9.14 26.5 49.8 107 268 410 435 12-Apr-2001 17 3.18 4.62 3.20 3.67 10.8 26.9 56.0 .111 286 421 490 11.9 29.5 50.8 102 240 381 503 ***0.932 3.88 12.0 26.8 51.6 ' 105 254 420 510 * Sample deactivated as an outlier (not included in summary statistics) *** Sample deactivated due to unacceptable internal standard response Page 37 0-0409 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 11. Back-Calculated Concentrations of Calibration Standards for PFOSAA (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 14-Apr-2001 Run Number 19 1.30 22-Apr-2001 21 23-Apr-2001 18 11-May-2001 25 1.45 1.24 2.80 2.32 3.30 2.32 3.73 3.26 3.18 2.84 2.33 4.30 10.3 11.8 25.3 26.8 50.3 51.8 100 102 250 252 400 402 500 502 4.35 10.7 25.5 54.0 113 254 425 510 4.45 11.3 23.9 57.1 87.2 310 340 478 2.75 10.1 26.7 55.7 103 217 393 492 4.79 13.0 26.5 54.8 112 238 453 500 3.04 12.7 31.8 53.2 99.2 289 413 467 3.81 8.77 22.2 51.4 110 290 403 459 10.6 28.3 52.3 102 266 428 495 10.3 23.2 48.1 94.5 257 386 472 Mean S.D. %CV %Bias n 1.35 2.97 3.88 10.5 11.4 25.8 26.5 50.2 53.5 98.3 102 262 267 407 410 484 480 ISD 0.437 0.634 ISD 1.50 ISD 2.90 ISD 4.48 ISD 8.01 ISD 22.9 ISD 32.1 ISD 24.6 ISD 14.7 16.3 ISD 13.2 ISD 10.9 ISD 8.4 ISD 7.9 ISD 8.6 ISD 7.8 ISD 5.1 3.8 6.1 -9.8 1.9 -3.4 2.0 -1.1 -0.2 3.3 -1.7 0.0 4.8 6.0 1.8 2.0 -3.2 -4.4 2 25 24 2 23 2 24 2 24 2 24 2 24 2 24 2 24 ISD = insufficient data points for statistical calculations Page 38 GGLOd Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 12. Back-Calculated Concentrations of Calibration Standards for PFOSA Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 Run Number 1 28-NOV-2000 2 23-Mar-20Q l 4 24-Mar-2001 5 26-Mar-2001 6 26-Mar-2001 7 28-Mar-2001 8 28-Mar-2001 9 30-Mar-2001 10 30-Mar-2001 11 1.00 1.40 2.50 2.90 10.0 10.4 25.0 25.4 50.0 50.4 100 250 400 500 1.10 0.893 1.08 0.906 0.984 0.906 0.935 1.08 1.38 1.38 *2.12 1.41 *0.353 1.36 1.53 1.25 1.39 1.51 *2.96 1.39 2.57 9.38 27.4 52.7 97.7 287 378 569 2.46 10.0 *46.1 **18.1 87.8 242 349 497 2.40 9.06 26.8 50.2 97.9 283 354 560 2.70 10.2 *48.6 **19.1 93.3 256 377 480 2.94 9.66 26.3 50.7 93.2 285 370 522 2.80 10.6 17.0 49.6 106 240 431 458 2.47 10.1 24.6 51.2 98.1 255 406 517 2.40 10.1 26.3 49.2 98.4 247 382 497 2.93 9.65 24.1 43.9 94.7 245 382 491 3.10 *16.2 26.6 58.7 101 260 453 471 3.01 10.3 26.6 50.7 88.9 251 423 461 2.79 10.0 26.1 46.4 110 273 377 518 3.21 11.1 25.2 54.8 99.8 240 409 527 2.74 10.1 25.5 45.6 96.8 247 401 479 3.37 10.2 30.2 51.2 106 254 388 500 2.65 8.72 21.7 49.8 89.4 304 387 471 2.47 12.1 27.1 48.9 92.0 238 409 488 2.83 9.54 26.4 48.9 104 261 416 492 2.91 11.1 23.8 50.3 99.9 259 383 448 2.95 9.56 24.4 58.4 *154 203 476 524 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to sample preparation error Page 39 000501 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 12. Back-Calculated Concentrations of Calibration Standards for PFOSA (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 02-Apr-2001 Run Number 13 1.00 07-Apr-2001 14 09-Apr-2001 15 11-Apr-2001 16 12-Apr-2001 17 23-Apr-2001 18 1.40 2.50 2.90 10.0 10.4 25.0 25.4 50.0 50.4 100 250 400 500 1.06 1.66 1.14 1.66 *2.32 1.40 1.59 1.23 1.47 ***0.557 1.44 1.33 2.93 10.2 26.1 52.2 99.3 262 429 517 3.32 9.31 24.0 51.2 97.3 249 393 452 3.23 10.9 29.4 52.0 109 285 426 502 2.58 10.1 18.9 48.0 97.7 227 399 457 2.77 9.77 28.9 51.8 112 281 429 518 3.11 9.74 23.9 46.7 92.5 232 364 472 2.67 9.79 22.9 55.6 88.9 285 346 473 3.16 9.03 26.6 54.6 111 241 416 533 2.55 10.5 29.5 47.5 103 223 386 536 2.86 11.0 25.2 47.4 102 247 403 501 3.00 9.87 28.1 49.5 83.9 256 405 481 3.01 9.81 23.4 50.8 115 269 389 503 Mean S.D. %CV "/Bias n 0.986 0.0884 9.0 -1.4 8 1.40 0.158 11.3 0.0 19 2.59 2.92 9.89 10.1 24.7 25.6 0.201 0.244 0.493 0.758 3.90 2.63 7.8 8.4 5.0 7.5 15.8 10.3 3.6 0.7 -1.1 -2.9 -1.2 0.8 8 24 8 23 6 24 50.6 1.26 2.5 1.2 6 * Sample deactivated as an outlier (not included in summary statistics) *** Sample deactivated due to unacceptable internal standard response 50.6 98.9 256 398 497 3.78 7.71 21.8 29.0 30.3 7.5 7.8 8.5 7.3 6.1 0.4 -1.1 2.4 -0.5 -0.6 24 31 32 32 32 Page 40 Northwest Bioanalytical Study No. NWBS0-128 Report No. NWBRO1-066 Table 13. Back-Calculated Concentrations of Calibration Standards for M556 Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 Run Number 1 28-NOV-2000 2 24-Mar-2001 5 26-Mar-2001 6 2.50 2.81 2.23 2.20 2.83 2.05 2.98 26-Mar-2001 7 28-Mar-2001 8 30-Mar-200l 10 30-Mar-2001 11 01-Apr-2001 12 3.20 10.0 10.7 25.0 25.7 50.0 50.7 100 101 250 251 400 401 500 501 3.16 3.08 3.15 3.15 3.13 *4.76 2.75 3.55 3.36 3.00 3.90 2.63 10.2 27.5 8.65 *45.7 9.06 24.5 10.7 *53.6 9.42 24.5 10.0 24.7 9.86 13.9 10.5 12.1 9.57 12.2 12.4 10.4 12.2 10.2 10.7 8.84 56.0 **17.3 48.3 **21.2 52.5 49.8 23.1 25.7 25.7 26.0 29.3 25.6 27.1 24.0 23.8 23.2 29.4 23.4 98.1 84.1 91.1 106 104 99.5 43.9 60.8 55.1 45.1 53.8 47.5 49.3 47.4 52.0 58.2 56.4 52.9 287 235 269 274 256 248 86.7 97.4 85.8 101 91.5 96.3 96.9 101 102 *145 102 80.0 421 360 378 404 407 384 234 271 258 263 234 255 245 265 247 209 263 289 555 451 499 486 504 499 361 460 445 381 373 440 407 416 364 487 398 383 497 496 468 506 508 504 485 496 445 538 498 490 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to sample preparation error Page 41 GG0503 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBR01 -066 Table 13. Back-Calculated Concentrations of Calibration Standards for M556 (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date Run 2.50 3.20 10.0 10.7 25.0 25.7 50.0 50.7 100 101 250 251 400 401 500 501 Number 07-Apr-2001 14 3.47 9.97 28.4 49.5 99.9 258 425 478 2.95 11.4 20.9 54.3 104 239 427 477 09-Apr-2001 15 2.68 8.84 27.5 49.7 108 254 421 459 3.93 9.80 24.8 52.2 103 266 416 489 12-Apr-2001 17 2.67 10.5 25.8 46.2 97.3 226 368 490 3.68 11.4 26.2 54.6 105 255 441 523 14-Apr-2001 19 3.21 9.15 25.9 51.3 106 225 408 530 3.30 11.0 23.8 55.8 96.2 303 348 488 23-Apr-2001 18 2.89 10.2 25.8 51.1 81.9 253 402 461 3.65 9.66 23.7 53.8 115 295 419 488 Mean S.D. %CV %Bias n 2.52 3.20 9.67 10.7 25.3 25.4 51.7 51.9 97.1 97.9 262 255 392 409 499 492 0.400 0.387 0.765 1.29 1.47 2.12 3.38 4.29 8.23 8.74 18.9 22.7 22.3 34.9 33.6 22.4 15.9 12.1 7.9 12.1 5.8 8.3 6.5 8.3 8.5 8.9 7.2 8.9 5.7 8.5 6.7 4.6 0.8 0.0 -3.3 0.0 1.2 -1.2 3.4 2.4 -2.9 -3.1 4.8 1.6 -2.0 2.0 -0.2 -1.8 6 21 6 22 4 22 4 22 6 21 6 22 6 22 6 22 Page 42 000504 Northwest Bioanalytical Study No. NWBS00-128 Report No. NVVBRO1-066 Table 14. Back-Calculated Concentrations of Calibration Standards for M570 Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 Run Number 1 28-Nov-2000 2 24-Mar-2001 5 26-Mar-2001 6 26-Mar-2001 7 28-Mar-2001 8 30-Mar-2001 10 01-Apr-2001 12 02-Apr-2001 13 1.00 1.05 1.01 0.991 *1.56 0.927 1.15 1.80 2.50 3.30 10.0 10.8 25.0 25.8 50.0 50.8 100 101 250 251 400 401 500 501 2.47 9.76 26.4 58.7 94.4 275 390 530 2.09 10.1 *50.6 **18.6 87.5 266 374 472 2.16 8.82 23.2 52.0 88.8 269 374 480 2.90 11.4 *58.7 **21.2 101 274 407 507 2.07 10.3 26.0 55.4 96.9 263 414 507 2.40 9.59 26.1 50.6 97.2 241 382 492 1.60 2.96 10.5 24.6 48.6 90.0 238 354 489 2.08 3.37 *18.0 28.3 *69.4 108 296 461 474 2.04 3.40 9.97 25.7 56.3 89.3 274 462 464 1.49 3.55 10.2 27.4 44.2 105 262 385 469 1.89 3.04 9.96 25.8 60.0 101 228 405 503 1.90 2.84 12.3 25.4 48.3 94.2 262 435 473 1.87 2.55 12.8 28.6 48.7 98.3 234 413 468 2.08 2.73 9.87 26.2 47.6 109 279 410 500 2.15 3.70 10.3 32.2 56.2 103 254 387 508 1.60 2.53 8.98 22.4 53.2 86.3 297 370 496 1.53 2.87 10.3 27.1 54.5 98.1 258 426 522 2.25 3.19 10.3 24.4 54.2 101 266 382 450 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to sample preparation error Page 43 Northwest Bioanalytical Study No. N W B S00-128 Report No. NWBRO1-066 Table 14. Back-Calculated Concentrations of Calibration Standards for M570 (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 07-Apr-2001 Run Number 14 09-Apr-2001 15 12-Apr-2001 17 14-Apr-2001 19 22-Apr-2001 21 24-Apr-2001 22 11-May-2001 25 1.00 1.80 2.50 3.30 10.0 10.8 25.0 25.8 50.0 50.8 100 101 250 251 400 401 500 501 1.65 3.24 10.9 30.4 52.3 109 263 436 475 2.11 2.80 10.8 19.4 52.0 102 231 426 466 1.98 2.39 8.68 26.3 48.4 107 255 403 448 1.86 3.60 10.1 27.6 54.8 107 279 424 491 2.03 2.78 11.5 28.1 50.5 103 229 387 517 ***0.564 2.92 11.3 24.7 51.2 104 248 416 501 1.46 3.44 9.54 25.8 52.4 112 240 418 521 2.18 3.19 10.2 24.0 56.6 88.5 310 340 477 1.94 2.56 10.9 25.2 54.0 106 214 395 502 *3.02 3.40 12.4 27.2 48.9 101 214 448 518 1.68 3.12 10.1 22.5 53.7 119 268 390 508 2.15 2.76 10.4 29.0 52.8 86.3 263 406 470 1.03 2.64 10.3 26.8 50.8 99.5 257 435 466 1.01 2.12 9.85 24.6 46.9 98.6 267 370 508 Mean S.D. %CV %Bias n 1.02 0.0677 6.6 2.0 7 1.89 0.246 13.0 5.0 22 2.36 3.04 10.0 10.5 25.5 26.2 52.4 0.302 0.371 0.736 1.01 1.36 2.72 4.12 12.8 12.2 7.4 9.6 5.3 10.4 7.9 -5.6 -7.9 0.0 -2.8 2.0 1.6 4.8 8 24 8 23 6 24 6 52.1 95.5 101 264 257 393 407 495 488 3.64 4.94 8.50 10.9 25.4 23.2 30.6 21.7 22.4 7.0 5.2 8.4 4.1 9.9 5.9 7.5 4.4 4.6 2.6 -4.5 0.0 5.6 2.4 -1.8 1.5 -1.0 -2.6 23 8 24 8 24 8 24 8 24 * Sample deactivated as an outlier (not included in summary statistics) *** Sample deactivated due unacceptable internal standard response Page 44 0 G0 0 6 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table IS. Analytical QC Summary for PFOS All concentrations are expressed as ppb. Run Date Run Number Low QC 6.40 ppb Low QC 5.75 ppb Medium QC 126 ppb Preparation 27-Oct-2000 05-Apr-2001 27-Oct-20Q0 Date 27-NOV-2000 1 5.91 121 6.13 127 28-NOV-2000 2 6.49 121 5.82 125 23-Mar-2001 4 *4.60 135 6.50 *192 24-Mar-2001 5 6.36 134 6.49 131 26-Mar-2001 6 5.88 **74.2 6.49 119 26-Mar-2001 7 6.70 139 5.88 123 28-Mar-2001 8 5.58 117 6.29 133 28-Mar-2001 9 5.65 141 5.14 140 Medium QC 126 ppb 05-Apr-2001 High QC 332 ppb 27-Oct-2000 High QC 332 ppb 08-Mar-2001 High QC 331 ppb 05-Apr-2001 High QC 348 ppb DF=5 08-Mar-2001 320 372 347 351 354 333 343 362 304 344 326 323 348 323 357 344 * >20% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response Page 45 000507 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 15. Analytical QC Summary for PFOS (Continued) All concentrations are expressed as ppb. Run Date Run Number Low QC 6.40 ppb Low QC 5.75 ppb Medium QC 126 ppb Preparation 27-Oct-2000 05-Apr-2001 Date 30-Mar-2001 10 6.08 5.74 30-Mar-2001 11 6.60 5.82 02-Apr-2001 13 6.47 6.65 07-Apr-2001 14 6.21 6.22 09-Apr-2001 15 5.78 5.84 11-Apr-2001 16 6.99 6.51 12-Apr-2001 17 6.25 6.20 27-Oct-2000 127 138 126 118 130 137 123 125 132 135 130 122 137 141 Medium QC 126 ppb 05-Apr-2001 High QC 332 ppb 27-Oct-2000 High QC 332 ppb 08-Mar-2001 High QC 331 ppb 05-Apr-2001 High QC 348 ppb DF=5 08-Mar-2001 324 332 328 **149 346 330 373 330 332 357 339 345 357 352 353 357 365 ** Sample deactivated due to unacceptable internal standard response Page 46 C$0508 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 15. Analytical QC Summary for PFOS (Continued) All concentrations are expressed as ppb. Run Date Run Number Low QC 6.40 ppb Low QC 5.75 ppb Preparation 27-Oct-2000 05-Apr-2001 Date 23-Apr-2001 18 6.57 6.84 Medium QC 126 ppb 27-Oct-2000 Medium QC 126 ppb 05-Apr-2001 138 130 High QC 332 ppb High QC 332 ppb High QC 331 ppb 27-Oct-2000 08-Mar-2001 05-Apr-2001 296 330 High QC 348 ppb DF=5 08-Mar-2001 Mean S.D. %CV %Theoretical %Bias n 6.11 6.71 132 134 348 339 313 358 0.492 ISD 13.7 ISD 16.3 15.8 ISD 6.11 8.1 ISD 10.4 ISD 4.7 4.7 ISD 1.7 95.5 116.7 104.8 106.3 104.8 102.1 94.6 102.9 -4.5 16.7 4.8 6.3 4.8 2.1 -5.4 2.9 30 2 29 2 8 21 2 3 ISD = insufficient data points for statistical calculation Page 47 000503 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 16. Analytical QC Summary for PFHS All concentrations are expressed as ppb. Run Date 27-NOV-2000 28-NOV-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 Run Number Preparation Date 1 2 4 5 6 7 8 9 Low QC 4.48 ppb 27-Oct-2000 Low QC 4.48 ppb 05-Apr-2001 Medium QC 156 ppb 27-Oct-2000 Medium QC 157 ppb 05-Apr-2001 High QC 417 ppb 27-Oct-2000 3.61 4.28 3.70 3.86 4.29 4.06 3.96 4.02 4.85 5.07 4.71 4.95 5.31 4.35 4.32 3.92 161 148 157 153 155 171 164 161 **128 157 157 135 158 158 158 158 382 443 411 445 428 406 414 460 ** Sample deactivated due to unacceptable internal standard response High QC 417 ppb 08-Mar-2001 373 396 411 407 420 383 392 415 High QC 418 ppb 05-Apr-2001 Page 48 0 0 o 1 0 Northwest Bioanalytical Study No. N W BS00-128 Report No. NWBRO1-066 Table 16. Analytical QC Summary for PFHS (Continued) All concentrations are expressed as ppb. Run Date 30-Mar-2001 Run Number Preparation Date 10 30-Mar-2001 11 02-Apr-2001 13 07-Apr-2001 14 09-Apr-2001 15 11-Apr-2001 16 12-Apr-2001 17 Low QC 4.48 ppb 27-Oct-2000 Low QC 4.48 ppb 05-Apr-2001 Medium QC 156 ppb 27-Oct-2000 Medium QC 157 ppb 05-Apr-2001 High QC 417 ppb 27-Oct-2000 *3.48 4.29 4.08 4.06 4.20 4.38 4.87 4.25 3.92 3.68 4.85 3.62 4.14 4.43 136 146 151 154 158 158 153 149 156 152 155 155 157 153 * >20% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response High QC 417 ppb 08-Mar-2001 413 345 391 **200 428 436 408 378 444 401 387 383 397 404 High QC 418 ppb 05-Apr-2001 Page 49 G00 i1 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 16. Analytical QC Summary for PFHS (Continued) All concentrations are expressed as ppb. Run Date 23-Apr-2001 Run Number Preparation Date 18 Low QC 4.48 ppb 27-Oct-2000 Low QC 4.48 ppb 05-Apr-2001 3.87 4.05 Medium QC 156 ppb 27-Oct-2000 Medium QC 157 ppb 05-Apr-2001 166 145 High QC 417 ppb 27-Oct-2000 High QC 417 ppb 08-Mar-2001 High QC 418 ppb 05-Apr-2001 397 389 Mean S.D. %ev %Theoretical %Bias n 4.25 0.467 11.0 94.9 -5.1 30 3.96 ISD ISD 88.4 -11.6 2 155 7.17 4.6 99.4 -0.6 29 156 ISD ISD 99.4 -0.6 2 ISD = insufficient data points for statistical calculation 424 25.3 6.0 101.7 1.7 8 401 22.6 5.6 96.2 -3.8 21 393 ISD ISD 94.0 -6.0 2 Page 50 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 17. Analytical QC Summary for PFOA All concentrations are expressed as ppb. Run Date Run Number Low QC 4.81 ppb Low QC 4.32 ppb Low QC Medium QC Medium QC High QC 4.32 ppb 145 ppb 145 ppb 385 ppb High QC 385 ppb High QC 385 ppb Preparation 27-Oct-2000 05-Apr-2001 02-May-2001 27-Oct-2000 05-Apr-2001 27-Oct-2000 08-Mar-2001 05-Apr-2001 Date 27-NOV-2000 1 4.55 154 403 4.30 160 429 28-Nov-2000 2 4.35 151 416 3.92 162 439 23-Mar-2001 4 *2.72 159 412 4.85 152 381 24-Mar-2001 5 4.09 143 390 *3.69 151 377 26-Mar-2001 6 4.12 **124 393 4.81 152 395 26-Mar-200l 7 5.47 146 348 4.93 140 384 28-Mar-2001 8 4.63 151 404 *0.161 156 375 28-Mar-2001 9 4.33 158 404 3.89 157 433 * >20% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response Page 51 Northwest Bioanalytieal Study No. NWBS00-128 Report No. NWBRO1-066 Table 17. Analytical QC Summary for PFOA (Continued) All concentrations are expressed as ppb. Run Date Run Number Low QC 4.81 ppb Low QC 4.32 ppb Low QC Medium QC Medium QC High QC 4.32 ppb 145 ppb 145 ppb 385 ppb High QC 385 ppb High QC 385 ppb Preparation 27-ct-2000 05-Apr-2001 02-May-2001 27-Oct-2000 05-Apr-2001 27-Oct-2000 08-Mar-2001 05-Apr-2001 Date 30-Mar-2001 10 4.29 151 393 4.14 155 382 02-Apr-2001 13 4.56 145 381 4.15 139 336 07-Apr-2001 14 *5.97 145 381 4.77 136 361 09-Apr-2001 15 4.45 159 406 *3.61 147 351 12-Apr-2001 17 4.17 151 372 4.07 158 375 14-Apr-2001 19 *3.79 131 377 5.04 *109 401 22-Apr-2001 21 4.03 143 401 3.90 170 361 23-Apr-2001 18 3.82 141 370 4.67 151 414 * >20% deviation from theoretical Page 52 OO514  Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 17. Analytical QC Summary for PFOA (Continued) All concentrations are expressed as ppb. Run Date Run Number Low QC 4.81 ppb Low QC 4.32 ppb Low QC Medium QC Medium QC High QC 4.32 ppb 145 ppb 145 ppb 385 ppb High QC 385 ppb High QC 385 ppb Preparation 27-Oct-2000 05-Apr-2001 02-May-2001 27-Oct-2000 05-Apr-2001 27-Oct-2000 08-Mar-2001 05-Apr-2001 Date 11-May-2001 25 4.16 150 386 4.65 148 398 Mean S.D. %CV %Theoretical %Bias n 4.19 0.970 23.2 87.1 -12.9 30 4.25 ISD ISD 98.4 -1.6 2 4.41 ISD ISD 102.1 2.1 2 149 11.5 7.7 102.8 2.8 29 148 4.51 3.0 102.1 2.1 4 ' 406 22.3 5.5 105.5 5.5 8 382 22.5 5.9 99.2 -0.8 22 392 18.6 4.7 101.8 1.8 4 ISD = insufficient data points for statistical calculation Page 53 GGlo Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 18. Analytical QC Summary for PFOSAA All concentrations are expressed as ppb. Run Date Run Number Low QC 4.60 ppb Low QC 4.30 ppb Low QC 4.30 ppb Medium QC Medium QC High QC 151 ppb 150 ppb 401 ppb High QC 401 ppb High QC 400 ppb Preparation 27-Oct-2000 05-Apr-2001 02-May-2001 27-Oct-2000 05-Apr-2001 27-Oct-2000 08-Mar-2001 05-Apr-2001 Date 27-NOV-2000 1 4.22 141 398 *3.38 167 425 28-NOV-2000 2 4.50 150 378 3.66 165 368 23-Mar-2001 4 *2.38 4.11 172 463 *374 456 t 24-Mar-2001 5 4.22 157 422 4.11 157 389 26-Mar-2001 6 4.55 **71.5 348 4.98 130 445 26-Mar-2001 7 4.85 146 365 4.26 135 384 28-Mar-2001 8 *6.56 145 415 4.31 142 . 383 28-Mar-2001 9 4.16 183 440 - 4.41 175 415 * >25% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response Page 54 CG0S16 Northwest Bioanalytica Study No. NWBSOO-128 Report No. NWBRO1-066 Table 18. Analytical QC Summary for PFOSAA (Continued) All concentrations are expressed as ppb. Run Date Run Number Low QC 4.60 ppb Low QC 4.30 ppb Low QC 4.30 ppb Medium QC Medium QC 151 ppb 150 ppb High QC 401 ppb High QC 401 ppb High QC 400 ppb Preparation 27-Oct-2000 05-Apr-2001 02-May-2001 27-Oct-2000 05-Apr-2001 27-Oct-2000 08-Mar-2001 05-Apr-2001 Date 30-Mar-2001 10 5.47 149 380 4.96 170 376 02-Apr-2001 13 *6.00 154 412 5.38 153 360 07-Apr-2001 14 5.41 166 452 4.70 154 439 09-Apr-2001 15 4.61 170 426 3.71 165 380 12-Apr-2001 17 5.23 178 465 5.04 *189 448 14-Apr-2001 19 4.60 160 420 5.43 123 429 22-Apr-2001 21 *6.60 149 432 4.64 *218 413 23-Apr-2001 18 4.41 167 398 5.33 169 427 * >25% deviation from theoretical Page 55 0G057 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 18. Analytical QC Summary for PFOSAA (Continued) All concentrations are expressed as ppb. Run Date Run Number Preparation Date Low QC 4.60 ppb 27-Oct-2000 Low QC 4.30 ppb 05-Apr-2001 Low QC 4.30 ppb 02-May-2001 Medium QC 151 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 High QC 401 ppb 27-Oct-2000 High QC 401 ppb 08-Mar-2001 High QC 400 ppb 05-Apr-2001 11-May-2001 25 4.34 143 424 3.95 145 407 Mean S.D. %CV "/oTheoretical %Bias n 4.68 0.882 18.8 101.7 1.7 30 4.87 ISD ISD 113.3 13.3 2 4.15 ISD ISD 96.5 -3.5 2 167 44.2 26.5 110.6 10.6 29 156 13.9 8.9 104.0 4.0 4 ISD = insufficient data points for statistical calculations 412 35.1 8.5 102.7 2.7 8 410 33.2 8.1 102.2 2.2 22 414 13.8 3.3 103.5 3.5 4 Page 56 000518 Northwest Bioanalytical Table 19. Analytical QC Summary for PFOSA All concentrations are expressed as ppb. Run Date 27-NOV-2000 28-NOV-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 Run Number Preparation Date 1 2 4 5 6 7 8 9 Low QC 4.00 ppb 27-Oct-2000 4.39 4.12 4.86 3.97 2.33 4.47 3.94 4.21 3.85 3.85 4.80 3.98 4.16 3.58 3.84 3.82 Low QC 4.00 ppb 05-Apr-2001 Medium QC 150 ppb 27-Oct-2000 147 162 146 158 180 328 156 158 **72.6 133 141 133 146 155 173 157 Medium QC 150 ppb 05-Apr-2001 High QC 400 ppb 27-Oct-2000 399 466 416 386 434 417 423 399 * >25% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response Study No. NW BS00-128 Report No. NWBRO1-066 High QC 400 ppb 08-Mar-2001 High QC 400 ppb 05-Apr-2001 311 457 369 396 431 406 447 408 Page 57 G0513 Northwest Bioanalytical Table 19. Analytical QC Summary for PFOSA (Continued) All concentrations are expressed as ppb. Run Date 30-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 11-Apr-2001 12-Apr-2001 Run Number Preparation Date 10 11 13 14 15 16 17 Low QC 4.00 ppb 27-Oct-2000 4.16 3.96 *5.14 4.08 4.21 4.39 4.79 4.46 4.19 3.92 *5.84 4.95 4.53 4.38 Low QC 4.00 ppb 05-Apr-2001 Medium QC 150 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 144 161 138 124 148 159 150 147 157 157 165 127 155 170 High QC 400 ppb 27-Oct-2000 * >25% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response Study No. NWBS00-128 Report No. NWBRO1-066 High QC 400 ppb 08-Mar-2001 High QC 400 ppb 05-Apr-2001 400 368 392 **170 431 361 456 424 423 422 404 425 437 403 Page 58 0SG520 Northwest Bioanalytical Table 19. Analytical QC Summary for PFOSA (Continued) All concentrations are expressed as ppb. Run Date 23-Apr-2001 Run Number Preparation Date 18 Low QC 4.00 ppb 27-Oct-2000 Low QC 4.00 ppb 05-Apr-2001 4.95 4.73 Medium QC 150 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 178 170 High QC 400 ppb 27-Oct-2000 Study No. NW BS00-128 Report No. NWBRO1-066 High QC 400 ppb 08-Mar-2001 High QC 400 ppb 05-Apr-2001 392 436 Mean S.D. %CV %Theoretical %Bias n 4.24 0.596 14.1 106.0 6.0 30 4.84 ISD ISD 121.0 21.0 2 158 35.3 22.3 105.3 5.3 29 174 ISD ISD 116.0 16.0 2 418 24.9 6.0 104.5 4.5 8 ISD = insufficient data points for statistical calculations 408 34.9 8.6 102.0 2.0 21 414 ISD ISD 103.5 3.5 2 Page 59 CGG521 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 20. Analytical QC Summary for M556 All concentrations are expressed as ppb. Run Date Run Number Preparation Date 27-NOV-2000 1 28-NOV-2000 2 24-Mar-2001 5 26-Mar-2001 6 26-Mar-2001 7 28-Mar-2001 8 30-Mar-2001 10 30-Mar-2001 01-Apr-2001 11 12 Low QC 4.00 ppb 27-Oct-2000 4.09 3.23 4.52 3.60 4.77 3.60 3.52 4.07 4.45 *2.73 *6.68 4.15 *4.85 4.06 ***7.47 4.28 *5.69 4.35 Low QC 4.00 ppb 05-Apr-2001 Medium QC 150 ppb 27-Oct-2000 133 161 144 166 160 156 **79.4 137 137 124 164 166 149 171 146 126 162 158 Medium QC 150 ppb 05-Apr-2001 High QC 400 ppb 27-Oct-2000 423 439 393 389 High QC 400 ppb 08-Mar-2001 402 401 367 428 354 404 426 388 382 385 369 **173 396 388 High QC 400 ppb 05-Apr-2001 * >20% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response *** Sample deactivated due to carryover 000522 Page 60 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 20. Analytical QC Summary for M556 (Continued) All concentrations are expressed as ppb. Run Date Run Number Preparation Date Low QC 4.00 ppb 27-Oct-2000 Low QC 4.00 ppb 05-Apr-2001 Medium QC 150 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 High QC 400 ppb 27-Oct-2000 High QC 400 ppb 08-Mar-2001 High QC 400 ppb 05-Apr-2001 07-Apr-2001 14 4.73 152 407 3.51 145 387 09-Apr-2001 15 4.02 171 434 12-Apr-2001 17 *3.14 4.40 164 164 395 395 14-Apr-2001 19 4.29 3.75 162 155 387 396 4.71 *115 406 23-Apr-2001 18 4.51 180 381 4.11 160 395 Mean S.D. %CV %Theoretical %Bias n 4.21 0.818 19.4 105.3 5.3 25 4.31 ISD ISD 107.8 7.8 2 152 15.5 10.2 101.3 1.3 25 170 ISD ISD 113.3 13.3 2 406 21.0 5.2 101.5 1.5 6 * >20% deviation from theoretical ISD = insufficient data points for statistical calculations 395 20.3 5.1 98.8 -1.3 19 388 ISD ISD 97.0 -3.0 2 Page 61 000523 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 21. Analytical QC Summary for M570 All concentrations are expressed as ppb. Run Date Run Number Low QC 4.00 ppb Preparation 27-Oct-2000 Date Low QC 4.00 ppb 05-Apr-2001 Low QC 4.00 ppb 02-May-2001 Medium QC 150 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 High QC 400 ppb 27-Oct-2000 High QC 400 ppb 08-Mar-2001 High QC 400 ppb 05-Apr-2001 27-NOV-2000 1 3.61 149 388 *3.07 163 451 28-NOV-2000 2 4.10 151 383 3.59 169 394 24-Mar-2001 5 3.81 168 415 3.89 165 412 26-Mar-2001 6 3.63 **74.2 338 4.00 140 447 26-Mar-2001 7 4.75 150 344 3.26 133 403 28-Mar-2001 8 *5.01 156 433 3.25 161 396 30-Mar-2001 10 4.64 150 359 3.54 180 379 01-Apr-2001 12 3.78 166 411 3.60 169 364 * >20% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response Page 62 G00524 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 21. Analytical QC Summary for M570 (Continued) All concentrations are expressed as ppb. Run Date Run Number Low QC 4.00 ppb Low QC 4.00 ppb Low QC 4.00 ppb Medium QC Medium QC 150 ppb 150 ppb High QC 400 ppb High QC 400 ppb High QC 400 ppb Preparation 27-Oct-2000 05-Apr-2001 02-May-2001 27-Oct-2000 05-Apr-2001 27-Oct-2000 08-Mar-2001 05-Apr-2Q01 Date 02-Apr-2001 13 4.55 156 405 3.99 162 362 07-Apr-2001 14 4.80 159 446 4.37 156 423 09-Apr-2001 15 3.91 168 380 *2.69 163 375 12-Apr-2001 17 4.38 172 447 4.28 *185 446 14-Apr-2001 19 4.17 158 413 4.26 120 423 22-Apr-2001 21 *5.54 146 447 3.89 *207 413 24-Apr-2001 22 *3.11 178 373 4.18 168 393 * >20% deviation from theoretical Page 63 000525 Northwest Bioanalytical Study No. NWBS0-128 Report No. NWBRO1-066 Table 21. Analytical QC Summary for M570 (Continued) AH concentrations are expressed as ppb. Run Date Run Number Preparation Date Low QC 4.00 ppb 27-Oct-2000 Low QC 4.00 ppb 05-Apr-2001 Low QC 4.00 ppb 02-May-2001 Medium QC 150 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 High QC 400 ppb 27-Oct-2000 High QC 400 ppb 08-Mar-2001 High QC 400 ppb 05-Apr-2001 11-May-2001 25 4.51 143 417 *2.83 149 408 Mean S.D. %CV %Theoretical %Bias n 4.01 0.621 15.5 100.3 0.3 28 3.65 3.67 160 160 ISD ISD 16.6 16.3 ISD ISD 10.4 10.2 91.3 91.8 106.7 106.7 -8.8 -8.3 6.7 6.7 2 2 27 4 * >20% deviation from theoretical ISD = insufficient data points for statistical calculations 407 25.0 6.1 101.8 1.8 6 402 35.4 8.8 100.5 0.5 22 398 19.2 4.8 99.5 -0.5 4 Page 64 06052C Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations All concentrations are expressed as ppb. Sample PFOS ID Concentration (PPb) 10956 54.1 10957 51.3 10958 80.5 10959 69.3 10960 37.3 10961 48.4 10962 55.7 10963 42.0 10964 114 10965 45.0 10966 29.2 10967 31.7 10968 42.8 10969 37.9 10970 46.7 10971 13.4 10972 24.0 10973 34.1 PFHS* Concentration (PPb) 3.10 5.45 12.4 3.01 2.95 2.79 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 8.00 <LLOQ(2.09) <LLOQ(2.09) 9.26 2.96 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 3.68 PFOA* Concentration (ppb) 3.95 6.64 22.2 13.9 5.13 2.77 4.44 6.58 7.07 3.90 <LLOQ(2.11) <LLOQ(2.11) 5.17 <LLOQ(2.11) 3.35 <LLOQ(2.11) <LLOQ(2.11) 5.11 PFOSAA* Concentration (ppb) 3.68 <LLOQ(2.80) 7.59 4.13 <LLOQ(2.80) <LLOQ(2.80) 4.21 3.55 9.05 <LLOQ(2.80) 2.81 4.58 <LLOQ(2.80) 4.23 3.08 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) 3.10 <LLOQ(1.80) 2.26 <LLOQ(1.80) 6.18 <LLOQ(1.80) <LLOQ(1.80) 4.97 2.55 <LLOQ(1.80) <LLOQ(1.80) 4.72 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f die target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). A Page 65 *0**7 Northwest Bioanalytical Study No. N W BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample PFOS ID Concentration (PPb) 10974 51.8 10975 35.8 10976 44.0 10977 99.7 10978 48.7 10979 44.2 10980 57.7 10981 25.8 10982 46.4 10983 38.6 10984 75.1 10985 41.9 10986 57.7 10987 14.0 10988 39.2 10989 68.9 10990 38.6 10991 36.6 PFHS* Concentration (PPb) <LLOQ(2.09) 5.73 2.62 5.98 <LLOQ(2.09) <LLOQ(2.09) 3.66 4.98 7.28 <LLOQ(2.09) <LLOQ(2.09) 6.97 3.26 <LLOQ(2.09) 2.17 2.53 <LLOQ(2.09) 2.11 PFOA* Concentration (ppb) 3.37 3.04 7.32 6.94 3.23 3.16 4.86 2.59 2.20 <LLOQ(2.11) 17.4 2.22 5.04 <LLOQ(2.11) <LLOQ(2.11) 5.28 4.42 <LLOQ(2.11) PFOSAA* Concentration (PPb) 3.46 3.43 3.43 8.67 4.47 <LLOQ(2.80) 4.33 <LLOQ(2.80) <LLOQ(2.80) 3.90 3.44 <LLOQ(2.80) 5.09 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.45 PFOSA* Concentration (Ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) 2.03 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 5.13 <LLOQ(1.80) <LLOQ(1.80) 2.86 <LLOQ(1.80) 3.31 <LLOQ(1.80) 3.16 <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 66 000528 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 10992 PFOS Concentration (ppb) 19.4 10993 18.9 10994 44.6 10995 61.6 10996 39.2 10997 25.6 10998 70.6 10999 101 11000 42.3 11001 16.3 11002 127 11003 65.2 11004 40.1 11005 25.8 11006 39.1 11007 36.8 11008 26.2 11009 19.5 PFHS* Concentration (ppb) <LLOQ(2.09) <LLOQ(2.09) 2.18 2.26 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 8.84 <LLOQ(2.09) <LLOQ(2.09) 3.45 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.17 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (Ppb) <LLOQ(2.11) 2.29 2.51 4.38 3.69 <LLOQ(2.11) 6.92 8.54 <LLOQ(2.11) <LLOQ(2.11) 9.90 2.84 3.43 <LLOQ(2.11) <LLOQ(2.11) 9.12 4.76 <LLOQ(2.11) PFOSAA* Concentration (PPb) <LLOQ(2.80) 3.62 <LLOQ(2.80) 4.11 5.76 <LLOQ(2.8Q) 5.16 4.69 <LLOQ(2.80) <LLOQ(2.80) 6.22 3.69 3.63 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.01 PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 5.11 <LLOQ(1.80) 2.99 16.4 <LLOQ(1.80) <LLOQ(1.80) 3.99 <LLOQ(1.80) <LLOQ(1.80) 2.17 2.58 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). O AO & 94 Page 67 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 11010 PFOS Concentration (Ppb) 40.9 11011 33.6 11012 23.0 11013 47.8 11014 38.7 11015 105 11016 42.2 11017 27.7 11018 19.0 11019 84.9 11020 33.3 11021 19.4 11022 15.1 11023 50.3 11024 57.5 11025 57.5 11026 48.8 11027 48.7 PFHS* Concentration (PPb) 2.18 <LLOQ(2.09) 2.26 7.39 <LLOQ(2.09) 2.29 8.70 <LLOQ(2.09) 2.20 2.67 2.59 <LLOQ(2.09) 3.58 3.59 <LLOQ(2.09) <LLOQ(2.09) 2.74 5.70 PFOA* Concentration (ppb) 2.78 5.50 3.73 8.05 4.25 10.2 7.65 3.55 3.75 17.0 3.80 2.47 <LLOQ(2.11) 3.83 5.91 7.68 3.97 6.74 PFOSAA* Concentration (PPb) 3.95 6.00 <LLOQ(2.80) 4.93 6.10 6.49 4.12 3.34 <LLOQ(2.80) 3.96 4.63 <LLOQ(2.80) <LLOQ(2.8Q) <LLOQ(2.80) 7.77 7.48 3.49 4.95 PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (Ppb) <LLOQ(3.20) 12.7 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) 5.18 5.33 1.88 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.00 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.53 2.45 <LLOQ(1.80) 2.20 2.26 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 68 000530 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 11028 PFOS Concentration (ppb) 45.2 11029 21.9 11030 36.7 11031 54.5 11032 39.8 11033 63.2 11034 26.4 11035 38.6 11036 26.4 11037 17.3 11038 41.1 11039 60.7 11040 44.7 11041 42.8 11042 55.7 11043 27.1 11044 34.2 11045 49.0 PFHS* Concentration (ppb) 2.13 <LLOQ(2.09) <LLOQ(2.09) 8.04 <LLOQ(2.09) 4.36 9.84 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.23 2.85 <LLOQ(2.09) 3.07 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.16 PFOA* Concentration (PPb) 6.43 3.61 6.17 4.69 3.95 6.34 4.68 9.98 2.95 <LLOQ(2.11) 3.17 7.45 4.35 10.1 3.84 2.39 5.38 6.15 PFOSAA* Concentration (PPb) <LLOQ(2.80) <LLOQ(2.80) 3.00 <LLOQ(2.80) 3.25 3.25 4.83 <LLOQ(2.80) <LLOQ(2.80) 4.44 7.37 <LLOQ(2.80) <LLOQ(2.80) 3.19 3.85 <LLOQ(2.80) 2.84 <LLOQ(2.80) PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (Ppb) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 5.51 <LLOQ(1.80) <LLOQ(1.80) 1.84 2.57 <LLOQ(1.80) 5.93 <LLOQ(1.80) <LLOQ(1.80) 2.04 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 69 000541 Northwest Bioanalytical Study No. N W BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 11046 PFOS Concentration (ppb) 56.9 11047 73.8 11048 70.8 11049 33.5 11050 40.4 11051 26.7 11052 44.3 11053 44.8 11054 49.6 11055 27.5 11056 27.0 11057 51.9 11058 53.2 11059 48.7 11060 36.4 11061 18.3 11062 58.1 11063 25.8 PFHS* Concentration (PPb) 2.11 3.75 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.Q9) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 3.03 2.39 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (ppb) 5.98 7.45 8.77 4.71 4.11 <LLOQ(2.11) 3.41 8.70 5.27 3.32 6.01 7.40 5.78 6.82 4.67 2.34 20.2 5.08 PFOSAA* Concentration (PPb) 4.34 3.84 27.6 <LLOQ(2.80) 6.39 3.11 8.78 <LLOQ(2.80) 2.99 3.13 <LLOQ(2.80) <LLOQ(2.80) 6.47 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) 5.88 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.2Q) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.80) <LLOQ(1.80) 7.82 <LLOQ(1.80) <LLOQ(1.80) 2.51 <LLOQ(1.80) 2.96 2.02 <LLOQ( 1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 5.38 4.14 <LLOQ(1.80) 1.93 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 70 000532 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID PFOS Concentration (Ppb) 11064 56.0 11065 56.5 11066 30.1 11067 31.5 11068 6.63 11069 27.6 11070 205 11071 27.6 11072 49.4 11073 47.6 11074 29.7 11075 69.7 11076 27.4 11077 42.6 11078 46.9 L1079 32.3 11080 43.4 10556 14.1 PFHS* Concentration (ppb) 2.96 2.91 2.27 8.26 <LLOQ(2.09) <LLOQ(2.09) 2.63 2.73 3.74 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.42 <LLOQ(2.09) 5.27 <LLOQ(2.09) 3.88 PFOA* Concentration (PPb) 9.41 3.86 3.69 8.37 <LLOQ(2.11) 5.53 34.1 4.60 14.1 4.78 3.59 6.18 4.63 6.26 6.02 5.79 8.73 4.18 PFOSAA* Concentration (PPb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.23 <LLOQ(2.80) 5.28 <LLOQ(2.80) <LLOQ(2.80) 3.35 3.67 5.54 <LLOQ(2.80) 4.38 3.88 3.44 <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(l .40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.4Q) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3 20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.2Q) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) 5.29 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.89 <LLOQ(1.80) 2.13 3.35 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.89 <LLOQ(1.80) 3.46 2.01 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 71 000533 Northwest Bioanalytical Study No. NWBS00-128 Report No. NVVBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample PFOS ED Concentration (PPb) 10557 22.5 10558 33.1 10559 35.4 10560 16.9 10561 40.0 10562 25.3 10563 56.0 10564 18.1 10565 47.2 10566 29.5 10567 23.3 10568 13.6 10569 18.5 10570 19.9 10571 20.7 10572 26.0 10573 30.6 10574 21.1 PFHS* Concentration (ppb) 2.42 10.4 12.6 <LLOQ(2.09) 2.38 2.09 3.49 <LLOQ(2.09) 6.23 3.55 2.37 <LLOQ(2.09) 2.41 <LLOQ(2.09) 2.81 5.16 2.10 <LLOQ(2.09) PFOA* Concentration (PPb) 5.84 8.55 3.55 3.37 10.5 4.54 7.83 5.37 8.44 10.0 6.88 2.21 3.43 3.53 3.77 4.30 6.29 3.19 PFOSAA* Concentration (PPb) 2.81 3.51 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.8Q) 3.48 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 4.07 <LLOQ(2.80) PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.80) 4.26 <LLOQ(1.80) 2.47 2.40 2.60 <LLOQ(1.80) <LLOQ(1.80) 2.57 2.64 5.88 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.31 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 72 000534 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 10575 PFOS Concentration (ppb) <LLOQ(4.27) 10576 20.3 10577 23.6 10578 63.7 10579 37.4 10580 44.1 10581 9.83 10582 25.7 10583 39.2 10584 13.5 10585 37.6 10586 32.1 10587 11.0 10588 18.1 10589 37.2 10590 52.6 10591 38.2 10592 51.7 PFHS* Concentration (PPb) <LLOQ(2.09) 3.13 2.54 5.97 2.28 <LLOQ(2.09) <LLOQ(2.09) 2.10 2.56 <LLOQ(2.09) 3.67 2.71 8.05 <LLOQ(2.09) 4.96 8.80 4.18 11.2 PFOA* Concentration (ppb) <LLOQ(2.11) 4.17 4.60 9.31 7.36 6.25 5.84 4.11 9.18 4.81 7.23 3.87 3.50 6.97 6.73 11.8 6.75 13.6 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) 2.92 5.14 <LLOQ(2.80) 3.24 2.92 <LLOQ(2.80) 3.26 <LLOQ(2.80) 4.84 <LLOQ(2.80) <LLOQ(2.80) 3.10 4.40 <LLOQ(2.80) 3.29 2.98 PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.37 3.16 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 3.19 <LLOQ(1.80) 1.89 <LLOQ(1.80) 3.41 <LLOQ(1.80) 5.84 4.29 19.0 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 73 000535 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 10593 PROS Concentration (Ppb) 30.9 10594 74.2 10595 37.1 10596 21.8 10597 14.3 10598 29.9 10599 18.0 10600 47.7 10601 43.5 10602 20.8 10603 23.5 10604 10.2 10605 25.2 10606 27.6 10607 36.7 10608 30.8 10609 29.7 10610 65.8 PFHS* Concentration (PPb) 6.75 10.2 2.56 2.39 <LLOQ(2.09) 2.89 2.51 3.16 <LLOQ(2.09) 3.20 <LLOQ(2.Q9) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(1.36) 3.62 1.72 2.76 1.87 PFOA* Concentration (ppb) 6.20 13.9 4.59 3.91 3.36 9.69 4.10 7.19 3.04 5.09 5.23 2.67 3.49 7.16 7.89 8.13 6.53 13.7 PFOSAA* Concentration (ppb) <LLOQ(2.80) 6.71 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.58 3.13 <LLOQ(2.80) 3.35 3.24 3.01 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) MS56* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.80) 2.11 <LLOQ(1.80) . 2.40 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 3.78 2.05 1.93 <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 74 000536 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 10611 PFOS Concentration (Ppb) 22.2 10612 32.0 10613 67.6 10614 57.6 10615 36.0 10616 27.7 10617 25.8 10619 22.7 10620 54.3 10621 14.0 10622 35.5 10623 11.7 10624 25.3 10625 35.2 10626 41.7 10627 31.8 10628 25.4 10629 36.3 PFHS* Concentration (ppb) <LLOQ(1.36) 11.4 1.49 5.36 <LLOQ(l .36) <LLOQ(1.36) 3.31 2.16 6.80 <LLOQ( 1.36) <LLOQ(1.36) <LLOQ(1.36) 3.70 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) 2.84 <LLOQ(1.36) PFOA* Concentration (PPb) 5.82 7.23 10.7 10.1 4.01 5.76 5.24 4.40 9.52 2.47 6.63 4.13 5.89 4.17 7.28 6.28 6.87 4.55 PFOSAA* Concentration (PPb) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 2.42 <LLOQ(1.60) 2.59 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) PFOSA* Concentration (ppb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556* Concentration (PPb) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) 3.92 <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) 13.0 <LLOQ(3.20) . <LLOQ(1.80) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) 2.39 <LLOQ(3.20) 3.36 <LLOQ(3.20) 1.88 <LLOQ(3.20) 4.42 <LLOQ(3.20) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 75 n h A tlii IM IW dar Northwest Bioanalytical Study No. N W BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) AH concentrations are expressed as ppb. Sample ID PFOS Concentration (PPb) 10630 30.3 10631 54.1 10632 41.4 10633 87.2 10634 30.6 10635 36.8 10636 26.3 10637 12.7 10638 45.2 10639 44.7 10640 19.3 10641 19.8 10642 80.9 10643 40.5 10644 23.9 10645 26.5 10646 48.7 10647 26.7 PFHS* Concentration (ppb) 1.99 1.51 1.47 <LLOQ(1.36) <LLOQ(1.36) 1.79 1.84 <LLOQ(1.36) 2.80 <LLOQ(1.36) 2.36 <LLOQ(1.36) 2.08 2.29 3.45 <LLOQ(1.36) 1.60 1.40 PFOA* Concentration (ppb) 4.65 8.91 5.23 5.48 7.36 5.27 3.48 3.52 8.02 9.13 4.73 3.07 5.93 7.21 7.29 5.04 10.5 7.51 PFOSAA* Concentration (PPb) <LLOQ(1.60) 2.28 <LLOQ(1.60) 2.35 <LLOQ(1.60) <LLOQ(1.60) 3.32 1.61 1.62 4.68 <LLOQ(2.80) 1.78 2.99 2.45 <LLOQ(1.60) <LLOQ(1.60) 3.00 3.34 PFOSA* Concentration (PPb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) cLLOQ(l.OO) <LLOQ(1.40) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) MS70* Concentration (ppb) <LLOQ(1.80) <LLOQ(1.80) 3.03 2.65 <LLOQ(1.80) <LLOQ(1.80) 2.67 <LLOQ(1.80) <LLOQ(1.80) 2.12 <LLOQ(1.80) 1.83 3.65 <LLOQ(1.80) 2.41 <LLOQ(1.80) 3.48 6.35 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 76 000538 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) AH concentrations are expressed as ppb. Sample ID PFOS Concentration (ppb) 10648 16.7 10649 39.0 10650 14.3 10651 28.6 10652 32.7 10653 11.7 10654 28.5 10655 15.9 10656 33.9 10657 48.1 10658 45.7 10659 18.7 10660 26.1 10661 28.6 10662 44.5 10663 26.9 10664 31.4 10665 44.9 PFHS* Concentration (PPb) <LLOQ(1.36) 1.58 <LLOQ(1.36) 1.36 2.12 <LLOQ(1.36) 2.19 2.64 2.23 3.02 3.79 2.94 6.70 2.68 <LLOQ(2.09) 2.85 <LLOQ(2,09) 2.57 PFOA* Concentration (ppb) 3.49 10.1 2.86 5.69 11.4 2.13 11.4 4.26 2.14 3.46 5.80 4.57 4.58 5.56 6.28 2.80 3.28 5.48 PFOSAA* Concentration (PPb) 4.28 4.64 <LLOQ(1.60) <LLOQ(1.60) 2.81 <LLOQ(1.60) 2.43 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.8Q) <LLOQ(2.80) 5.09 <LLOQ(2.80) 4.40 PFOSA* Concentration (ppb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) 2.95 <LLOQ(1.80) 1.84 <LLOQ(1.80) 2.51 9.66 2.83 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 4.30 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f die target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 77 000539 Northwest Bioanalytical Study No. N W B S00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 10666 PFOS Concentration (ppb) 29.9 10667 40.8 10668 19.8 10328 24.3 10329 50.6 10330 47.7 10331 31.7 10332 30.8 10333 31.9 10334 24.6 10335 19.3 10336 42.5 10337 32.1 10338 19.3 10339 28.4 10340 39.2 10341 14.8 10342 23.1 PFHS* Concentration (PPb) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(1.36) 3.86 3.50 8.44 5.15 1.65 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(l,36) 1.52 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) 4.89 PFOA* Concentration (Ppb) 4.65 4.41 4.30 4.90 7.92 18.7 5.39 4.08 4.05 3.23 3.20 3.62 5.76 2.46 4.59 5.02 3.84 8.59 PFOSAA* Concentration (ppb) 4.52 <LLOQ(2.80) <LLOQ(2.80) 2.59 4.83 5.56 <LLOQ(1.60) 1.87 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 2.22 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 4.66 <LLOQ(1.60) 2.17 PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M5S6* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570* Concentration (ppb) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.00) 1.95 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 1.76 <LLOQ(1.00) <LLOQ(1.00) 1.21 6.28 3.92 <LLOQ(1.00) 1.35 <LLOQ(1.00) <LLOQ(1.00) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 78 000540 Northwest Bioanalytical Study No. N W BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) AH concentrations are expressed as ppb. Sample PFOS ID Concentration (ppb) 10343 29.6 10344 44.9 10345 45.6 10346 39.8 10347 14.7 10348 17.7 10349 33.0 10350 30.5 10351 34.8 10352 18.0 10353 23.8 10354 31.6 10355 95.7 10356 26.5 10357 22.0 10358 43.5 10359 71.0 10360 17.0 PFHS* Concentration (ppb) <LLOQ(1.36) <LLOQ(1.36) 2.07 2.44 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) 2.58 6.40 <LLOQ(2.09) 2.02 3.17 1.43 <LLOQ(1.36) <LLOQ(1.36) 4.08 1.37 <LLOQ(1.36) PFOA* Concentration (ppb) 6.45 3.03 5.74 4.38 2.28 3.58 4.94 2.35 3.95 <LLOQ(2.11) 6.55 4.74 10.7 3.80 4.05 4.92 5.30 4.90 PFOSAA* Concentration (PPb) 3.42 4.92 <LLOQ(1.60) 1.83 <LLOQ(1.60) <LLOQ(1.60) 2.05 4.32 <LLOQ(1.60) <LLOQ(2.80) <LLOQ(1.60) <LLOQ(1.6Q) 2.38 <LLOQ(1.60) 1.84 3.40 1.96 1.79 PFOSA* Concentration (PPb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.40) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556* Concentration (ppb) <LLOQ(2.S0) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(3.20) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570* Concentration (PPb) 1.50 2.51 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 2.83 1.39 5.37 3.17 <LLOQ(1.80) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 1.51 1.03 1.28 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 79 000541 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 10361 PFOS Concentration (ppb) 7.70 10362 41.7 10363 34.7 10364 22.8 10365 22.6 10366 21.9 10367 17.7 10368 74.3 10369 18.1 10370 24.7 10371 71.8 10372 59.5 10373 52.8 10374 ' 29.7 10375 49.2 10376 21.1 10377 88.4 10378 100 PFHS* Concentration (ppb) <LLOQ(1.36) 3.02 1.41 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) <LLOQ(2.09) <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) 7.12 12.0 3.87 <LLOQ(1.36) 10.8 <LLOQ(1.36) 6.67 1.37 PFOA* Concentration (ppb) 2.53 5.90 4.93 3.92 3.07 4.96 <LLOQ(2.11) 9.98 3.53 3.98 7.18 5.03 20.0 4.85 4.40 3.54 15.8 5.57 PFOSAA* Concentration (ppb) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 1.83 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(2.80) 10.3 <LLOQ(1.60) 2.75 5.41 <LLOQ(1.60) 1.79 1.94 <LLOQ(1.60) <LLOQ(1.60) 7.53 4.93 PFOSA* Concentration (ppb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.40) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.-00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) M556* Concentration (ppb) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(3.20) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570* Concentration (ppb) <LLOQ(1.00) 3.01 1.59 <LLOQ(1.00) 1.85 <LLOQ(l .00) <LLOQ(1.80) <LLOQ(1.00) 3.02 <LLOQ(1.00) 3.89 2.62 10.6 <LLOQ(1.00) 2.20 1.62 2.31 1.52 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 80 000542 Northwest Bioanalytical Study No. N W B S00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID PFOS Concentration (PPb) 10379 54.6 10380 31.3 10381 34.8 10382 35.8 10383 15.6 10384 24.7 10385 28.3 10386 10387 41.4 11.7 10388 79.1 10389 28.4 10390 15.8 10391 48.4 10392 55.5 10393 20.9 10394 21.7 10395 40.0 10396 36.3 PFHS* Concentration (ppb) <LLOQ(1.36) 1.49 <LLOQ(1.36) 1.72 <LLOQ(1.36) <LLOQ(1.36) 2.03 5.75 <LLOQ(1.36) <LLOQ(2.09) 1.60 <LLOQ(1.36) 2.45 1.61 1.41 1.65 4.73 1.81 PFOA* Concentration (PPb) 3.88 4.22 3.92 2.81 2.80 2.56 4.89 3.30 2.43 5.93 4.29 3.09 7.41 5.34 2.91 2.18 4.92 5.66 PFOSAA* Concentration (PPb) 3.27 <LLOQ(1.60) 2.56 <LLOQ(1.60) <LLOQ(1.60) 2.34 <LLOQ(1.60) 8.31 <LLOQ(1.60) 4.38 <LLOQ(1.60) <LLOQ(1.60) 3.27 2.54 1.98 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) PFOSA* Concentration (PPb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.40) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556* Concentration (ppb) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(3.20) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570* Concentration (ppb) <LLOQ(1.00) 1.72 1.69 1.70 2.84 <LLOQ( 1.00) 1.40 1.33 <LLOQ(1.00) <LLOQ(1.80) 1.29 2.42 3.07 4.03 3.12 <LLOQ(1.00) 1.41 2.32 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 81 000543 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 10397 PFOS Concentration (Ppb) 28.2 10398 36.9 10399 38.9 10400 27.5 10401 32.0 10402 25.2 10403 34.3 1044 30.6 10405 36.5 10406 24.1 10407 27.0 10408 80.4 10409 28.8 10410 88.8 10411 32.3 10412 53.5 10413 16.8 10414 27.0 PFHS* Concentration (PPb) 6.51 5.10 5.63 <LLOQ(1.36) 2.79 <LLOQ(1.36) 3.92 3.56 1.69 6.87 <LLOQ(1.36) 1.90 1.61 15.2 <LLOQ(1.36) 1.87 <LLOQ(1.36) <LLOQ(1.36) PFOA* Concentration (ppb) 4.57 5.59 3.38 4.57 5.63 <LLOQ(1.92) 2.97 2.78 7.05 6.27 4.62 10.6 3.49 13.8 3.26 8.98 2.53 3.17 PFOSAA* Concentration (PPb) <LLOQ(1.60) <LLOQ(1.60) 2.00 1.72 <LLOQ(2.80) 2.12 <LLOQ(1.60) 4.71 <LLOQ(1.60) 1.78 2.44 2.83 1.75 3.43 1.68 7.34 <LLOQ(1.60) 2.57 PFOSA* Concentration (PPb) <LLOQ(1.00) <LLOQ(1.00) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.40) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556* Concentration (PPb) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(3.20) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2 50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570* Concentration (Ppb) 1.62 4.39 <LLOQ(1.00) 1.34 <LLOQ(1.80) 4.05 <LLOQ(1.00) 1.34 <LLOQ( 1.00) 2.03 6.76 1.81 <LLOQ(1.00) 4.60 <LLOQ(1.00) 3.45 <LLOQ(1.00) 1.42 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 82 000544 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample PFOS ID Concentration (ppb) 10415 207 10416 17.2 10417 37.7 10418 29.1 10419 30.6 10420 56.6 10421 33.6 10422 14.4 10423 36.7 10424 38.8 10425 30.8 10426 115 10427 57.7 11883 17.8 11884 26.1 11885 26.5 11886 26.6 11887 60.1 PFHS* Concentration (ppb) 2.09 <LLOQ(1.36) 4.54 <LLOQ(1.36) <LLOQ(1.36) 2.70 1.83 <LLOQ(1.36) <LLOQ(1.36) 1.39 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (ppb) 14.9 <LLOQ(1.92) 4.28 4.43 2.82 11.5 4.61 2.40 5.76 3.38 3.59 10.3 5.95 2.40 <LLOQ(2.11) 6.13 4.07 26.7 PFOSAA* Concentration (Ppb) 7.76 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 2.58 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 12.9 1.91 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (PPb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (Ppb) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (Ppb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.0Q) 5.07 1.63 1.78 <LLOQ(1.00) 3.20 7.63 <LLOQ(1.00) 2.21 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.93 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f die target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 83 000545 Northwest Bioanalytical Study No. N W BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 11888 PFOS Concentration (ppb) 91.8 11889 33.8 11890 23.2 11891 71.3 11892 30.2 11893 35.0 11894 22.0 11895 12.5 11896 34.2 10756 166 10757 77.9 10758 133 10759 160 10760 38.1 10761 90.5 10762 41.7 10763 36.4 10764 30.3 PFHS* Concentration (ppb) 7.34 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 3.60 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 4.51 4.27 11.6 2.78 1.71 1.50 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) PFOA* Concentration (PPb) 10.1 5.85 3.64 6.40 7.40 4.90 4.55 4.48 4.71 29.0 11.7 6.25 15.3 5.39 8.54 6.09 6.25 3.29 PFOSAA* Concentration (PPb) 3.64 3.43 <LLOQ(2.80) 4.04 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 60.1 52.9 7.18 8.11 <LLOQ(1.60) 12.2 1.80 <LLOQ(1.60) <LLOQ(1.60) PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) cLLOQ(l.OO) <LLOQ(1.00) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 12.9 9.21 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570* Concentration (ppb) 13.3 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.90 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 3.75 <LLOQ(1.00) 5.21 1.28 1.55 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 84 O0O54C Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample PFOS ID Concentration (PPb) 10765 96.1 10766 40.7 10767 34.1 10768 28.1 10769 54.7 10770 42.7 10771 26.8 10772 36.1 10773 66.6 10774 77.2 10775 46.8 10776 159 10777 49.1 10778 31.0 10779 22.7 10780 57.3 10781 43.9 10782 79.0 PFHS* Concentration (PPb) 3.73 7.70 <LLOQ(1.36) 4.56 4.64 <LLOQ(1.36) 1.57 2.00 15.6 2.25 <LLOQ(1.36) 4.24 2.76 <LLOQ(1.36) <LLOQ(1.36) 3.76 2.78 4.71 PFOA* Concentration (ppb) 11.7 6.54 6.81 5.96 6.69 4.14 4.70 4.34 5.78 8.75 9.30 29.8 6.08 2.21 5.12 7.72 6.04 9.85 PFOSAA* Concentration (PPb) 1.75 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 2.19 <LLOQ(1.60) <LLOQ(1.60) 3.44 2.89 8.08 8.98 56.6 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 3.56 1.68 3.38 PFOSA* Concentration (PPb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556* Concentration (PPb) <LLOQ(2.5Q) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 12.2 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M57* Concentration (PPb) 2.82 <LLOQ(1.00) 1.65 <LLOQ(1.00) 1.18 1.59 4.22 <LLOQ(1.00) 2.77 1.86 <LLOQ(1.00) 2.45 <LLOQ(1.00) 2.07 <LLOQ(1.00) 1.73 <LLOQ(1.00) <LLOQ(1.00) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 85 000547 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID PFOS Concentration (ppb) 10783 54.2 10784 37.3 10785 31.6 10786 38.9 10787 73.0 10788 33.8 10789 49.3 10790 55.2 10791 69.8 10792 22.0 10793 31.1 10794 74.2 10795 105 10796 40.2 10797 52.5 10798 58.2 10799 117 10800 75.1 PFHS* Concentration (ppb) 1.78 2.12 1.91 5.22 6.27 2.19 2.00 <LLOQ(1.36) 2.67 1.38 1.64 3.86 2.09 19.8 4.12 4.96 1.70 3.15 PFOA* Concentration (PPb) 7.46 5.89 4.88 4.79 18.2 5.34 7.30 6.45 7.16 4.02 5.08 10.6 5.51 8.76 4.32 7.87 13.1 8.95 PFOSAA* Concentration (ppb) 4.60 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 2.28 <LLOQ(1.60) 1.95 4.51 2.36 <LLOQ(1.60) 2.31 13.7 1.96 2.09 1.76 1.81 5.44 8.62 PFOSA* Concentration (ppb) <LLOQ(1.00) <LLOQ(l.Q0) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.0Q) <LLOQ(1.0Q) M556* Concentration (PPb) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570* Concentration (ppb) 2.05 <LLOQ(1.00) <LLOQ(1.00) 1.98 2.16 <LLOQ( 1.00) 1.61 cLLOQ(l.OO) 1.57 1.21 <LLOQ(1.00) <LLOQ( 1.00) 2.67 <LLOQ(1.00) 4.69 1.97 1.27 2.97 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 86 00054 Northwest Bioanalytical Study No. NWBS0-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID PFOS Concentration (ppb) 10801 48.7 10802 33.3 10803 32.6 10804 68.5 10805 45.5 10806 110 10807 33.9 10808 40.3 10809 29.8 10810 42.9 10811 32.6 10812 69.9 10813 27.4 10814 38.4 10815 55.1 10816 50.1 10817 106 10818 67.6 PFHS* Concentration (ppb) 2.48 <LLOQ(1.36) 8.59 <LLOQ(1.36) 4.35 11.5 3.52 1.86 1.79 <LLOQ(2.09) <LLOQ(2.09) 3.77 <LLOQ(2.09) 2.82 <LLOQ(2.09) 4.39 4.58 9.17 PFOA* Concentration (ppb) 6.21 4.47 4.31 17.8 6.93 21.8 7.08 2.70 4.72 3.54 4.45 7.50 2.85 6.57 8.35 2.60 7.17 11.4 PFOSAA* Concentration (PPb) <LLOQ(1.60) 6.91 <LLOQ(1.60) 3.71 <LLOQ(1.60) 3.35 <LLOQ(1.60) <LLOQ(1.60) 3.58 3.58 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 6.45 4.05 3.04 3.25 <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1,OQ) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) 1.22 2.16 <LLOQ(1.00) 3.03 <LLOQ(1.00) 5.59 1.68 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.80) 2.99 2.46 1.95 3.66 <LLOQ(1.80) 5.68 <LLOQ(1.80) 5.34 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 87 000549 Northwest Bioanalytical Study No. N W BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) AH concentrations are expressed as ppb. Sample ID 10819 PFOS Concentration (PPb) 37.1 10820 71.0 10821 45.3 10822 54.4 10823 35.9 10824 109 10825 72.7 10826 30.6 10827 59.4 10828 143 10829 Not Received 10830 34.3 10831 75.8 10832 44.5 10833 68.9 10834 49.8 10835 71.3 10836 35.5 PFHS* Concentration (PPb) <LLOQ(2.09) 2.96 <LLOQ(2.09) 10.7 <LLOQ(2.09) <LLOQ(2.09) 14.1 2.47 5.37 3.33 Not Received 4.97 9.32 4.10 3.29 5.53 4.02 3.82 PFOA* Concentration (ppb) 4.65 3.88 4.17 7.46 7.14 6.50 6.90 3.42 8.35 13.4 Not Received 5.75 13.5 4.87 10.7 3.62 10.7 4.66 PFOSAA* Concentration (PPb) 3.21 4.70 <LLOQ(2.80) 15.1 <LLOQ(2.80) 9.12 <LLOQ(2.80) 3.76 6.62 8.59 Not Received <LLOQ(2.80) 4.28 <LLOQ(2.80) 3.51 5.10 <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) Not Received <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 3.91 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) Not Received <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) ' <LLOQ(1.80) 2.09 <LLOQ(1.80) 4.37 5.51 4.18 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 4.03 Not Received 8.31 5.26 <LLOQ(1.80) 10.8 <LLOQ(1.80) 4.47 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 88 * 000550 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) AH concentrations are expressed as ppb. Sample PFOS ID Concentration (ppb) 10837 Not Received 10838 36.5 10839 Not Received 10840 34.1 10841 68.2 10842 154 10843 41.8 10844 70.7 10845 Not Received 10846 65.8 10847 92.4 10848 44.2 10849 51.5 10850 40.7 10851 70.5 10852 19.3 10853 31.7 10854 50.5 PFHS* Concentration (ppb) Not Received 7.12 Not Received 2.50 22.4 12.1 2.34 9.59 Not Received 18.7 12.9 <LLOQ(2.09) 2.98 <LLOQ(2.09) 4.00 <LLOQ(2.09) <LLOQ(2.09) 2.46 PFOA* Concentration (ppb) Not Received 8.60 Not Received 6.97 5.68 18.2 4.37 14.9 Not Received 13.3 9.46 3.27 7.02 <LLOQ(2.11) 6.49 2.95 4.70 3.97 PFOSAA* Concentration (PPb) Not Received <LLOQ(2.80) Not Received <LLOQ(2.80) 4.33 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) Not Received 2.85 4.10 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.65 PFOSA* Concentration (PPb) Not Received <LLOQ(1.40) Not Received <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) Not Received <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) Not Received <LLOQ(3.20) Not Received <LLOQ(3.2Q) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) Not Received <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) Not Received 5.75 Not Received 2.83 <LLOQ(1.80) <LLOQ(1.80) 8.20 6.61 Not Received 2.83 3.57 <LLOQ(1.80) 1.99 <LLOQ(1.80) 2.11 <LLOQ(1.80) 3.44 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 89 , * __M 000551 Northwest Bioanalytical Study No. N W BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample PFOS ID Concentration (ppb) 10855 18.5 10856 36.3 10857 81.9 10858 54.7 10859 19.5 10860 Not Received 10861 39.9 10862 37.8 10863 70.6 10864 58.3 10865 56.8 10866 24.0 10867 57.4 10868 22.9 11649 17.6 11650 28.3 11651 48.8 11652 23.5 PFHS* Concentration (PPb) <LLOQ(2.09) 7.00 2.48 <LLOQ(2.09) <LLOQ(2.09) Not Received 2.57 4.03 <LLOQ(2.Q9) 2.34 6.25 <LLOQ(2.09) 2.28 4.80 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (PPb) 2.16 4.66 12.0 4.82 <LLOQ(2.ll) Not Received 3.35 4.23 4.20 3.80 3.85 3.03 5.32 3.46 3.96 3.49 4.07 2.71 PFOSAA* Concentration (ppb) <LLOQ(2.8Q) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.8Q) Not Received 5.15 <LLOQ(2.80) 3.11 <LLOQ(2.80) 24.7 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.20 3.24 25.1 <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) Not Received <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M5S6* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) Not Received <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 3.88 <LLOQ(3.20) 5.12 <LLOQ(3.20) M570* Concentration (ppb) 2.53 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) Not Received 3.21 2.23 3.10 <LLOQ(1.80) <LLOQ(1.80) 2.35 3.95 2.79 <LLOQ(1.80) 2.06 <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 90 000552 Northwest Bioanalytical Study No. N W B S00-128 Report No, NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID PFOS Concentration (PPb) 11653 25.2 11654 329 11655 31.2 11656 31.5 11657 70.3 11658 27.4 11659 43.9 11660 17.7 11661 46.4 11662 44.6 11663 14.0 11664 64.1 11665 45.0 11666 37.7 11667 9.45 11668 29.9 11669 31.9 11670 28.3 PFHS* Concentration (PPb) <LLOQ(2.09) 6.91 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.54 11.8 <LLOQ(2.09) <LLOQ(2.09) 10.9 <LLOQ(2.09) 2.48 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (Ppb) 4.76 16.7 3.77 3.13 6.63 2.94 3.61 3.13 3.91 4.92 3.77 6.96 4.49 5.07 <LLOQ(2.11) 3.81 6.28 4.08 PFOSAA* Concentration (PPb) 3.89 36.9 <LLOQ(2.80) <LLOQ(2.8Q) 13.3 <LLOQ(2.80) <LLOQ(2.80) 3.42 4.90 2.82 4.98 9.91 5.04 2.83 <LLOQ(2.80) 5.86 3.77 2.92 PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) MS56* Concentration (PPb) <LLOQ(3.20) 12.2 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 4.21 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.96 <LLOQ(1.80) <LLOQ(1.80) 2.43 <LLOQ(1.80) 2.63 2.06 <LLOQ(1.80) 2.03 <LLOQ(1.80) 2.86 <LLOQ(1.80) 1.82 <LLOQ(1.80) 3.64 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 91 0005S3 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID PFOS Concentration (PPb) 11671 37.7 11672 30.7 11673 36.2 11674 37.5 11675 14.2 11676 12.0 11677 43.4 11678 32.2 11679 17.0 11680 44.5 11681 15.8 11682 9.20 11683 40.3 11684 42.3 11685 24.4 11686 14.6 11687 36.1 11688 17.2 PFHS* Concentration (ppb) 2.16 <LLOQ(2.09) <LLOQ(2.09) 3.91 3.99 <LLOQ(2.09) 3.22 3.83 <LLOQ(2.09) 7.24 <LLOQ(2.09) <LLOQ(2.09) 8.61 <LLOQ(2.09) <LLOQ(2.09) 4.12 2.11 <LLOQ(2.09) PFOA* Concentration (ppb) 4.44 5.43 2.68 4.44 3.22 2.33 3.60 3.57 2.56 6.79 5.41 <LLOQ(2.11) 6.21 4.48 2.34 5.38 4.10 <LLOQ(2.11) PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.39 2.96 <LLOQ(2.80) 5.66 <LLOQ(2.80) <LLOQ(2.80) 4.72 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 4.43 PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.4Q) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) <LLOQ(1.80) 2.37 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.65 <LLOQ(1.80) 2.62 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 92 000SS4 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 11689 PFOS Concentration (ppb) 1656** 11690 25.6 11691 24.4 11692 14.2 11693 11694 27.1 33.4 11695 20.8 11696 14.5 11697 108 11698 124 11699 22.9 11700 25.5 11701 14.1 11702 39.0 11703 12.0 11704 78.7 11705 12.0 PFHS* Concentration (ppb) 9.87 <LLOQ(2.09) 2.59 <LLOQ(2.09) 2.58 <LLOQ(2.09) <LLOQ(2,09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.28 <LLOQ(2.09) <LLOQ(2.09) 3.27 <LLOQ(2.09) 6.54 <LLOQ(2.09) PFOA* Concentration (PPb) 4.32 2.92 3.13 2.71 3.91 <LLOQ(2.11) 3.04 <LLOQ(2.11) 12.2 12.0 4.24 3.48 3.11 5.61 <LLOQ(2.11) 12.9 3.09 PFOSAA* Concentration (Ppb) <LLOQ(2.80) <LLOQ(2.80) 3.88 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.03 13.0 9.58 <LLOQ(2.80) 5.45 <LLOQ(2.80) 6.74 2.97 15.6 <LLOQ(2.80) PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 3.58 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) ** Concentration corrected for amount o f persistent PFOS in dilution matrix. M570* Concentration (Ppb) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.14 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.07 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 3.70 <LLOQ(1.80) 3.68 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 93 000555 Northwest Bioanalytical Study No. NWBS0-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample PFOS ID Concentration (ppb) 11706 22.3 11707 17.5 11708 14.5 11709 43.5 11710 35.9 11711 30.3 11712 11.1 11713 50.8 11714 18.4 11715 36.8 11716 12.6 11717 13.2 11718 17.6 11719 16.1 11720 25.2 11721 37.4 11722 8.26 11723 30.2 PFHS* Concentration (ppb) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 3.37 <LLOQ(2.09) <LLOQ(2.09) 3.76 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.25 <LLOQ(2.09) <LLOQ(2.09) 2.26 <LLOQ(2.09) 5.64 PFOA* Concentration (ppb) 3.35 3.87 2.43 5.13 2.90 3.45 3.39 11.2 3.80 4.04 <LLOQ(2.11) <LLOQ(2.11) 5.15 3.22 2.11 4.13 2.53 4.19 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.48 <LLOQ(2.80) 20.6 6.13 <LLOQ(2.80) <LLOQ(2.80) <LL0Q(2.80) 2.63 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.21 PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ'(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) 1.96 <LLOQ(1.80) 4.82 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 5.27 <LLOQ(1.80) <LLQQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.55 5.50 <LLOQ(1.80) <LLOQ(1.80) 1.95 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 94 000556 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBR1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample PFOS ID Concentration (ppb) 11725 16.6 PFHS* Concentration (ppb) <LLOQ(2.09) PFOA* Concentration (ppb) <LLOQ(2.11) PFOSAA* Concentration (ppb) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.80) 11726 20.2 <LLOQ(2.09) 2.78 <LLOQ(2.80) <LLOQ(1.40) <LLOQ(3.20) <LLOQ( 1.80) 11727 25.7 <LLOQ(2.09) 8.48 2.90 <LLOQ(1.40) <LLOQ(3.20) 2.68 11729 21.6 <LLOQ(2.09) 4.08 7.58 <LLOQ(1.40) <LLOQ(3.20) <LLOQ(1.80) 11731 63.4 4.77 10.2 <LLOQ(2.80) <LLOQ(1.40) <LLOQ(3.20) 3.10 11732 30.3 <LLOQ(2.09) 4.07 <LLOQ(2.80) <LLOQ(1.40) <LLOQ(3.20) 2.85 11735 20.5 <LLOQ(2.09) 3.05 <LLOQ(2.80) <LLOQ(1.40) <LLOQ(3.20) <LLOQ(1.80) 11739 54.6 9.42 5.41 5.86 <LLOQ(1.40) <LLOQ(3.20) <LLOQ(1.80) 11745 26.9 <LLOQ(2.09) 4.97 4.48 <LLOQ(1.40) <LLOQ(3.20) 2.06 11746 24.6 <LLOQ(2.09) 3.76 <LLOQ(2.80) <LLOQ(1.40) <LLOQ(3.20) <LLOQ(1.80) 11748 31.1 <LLOQ(2.09) 3.31 <LLOQ(2.80) <LLOQ(1.40) <LLOQ(3.20) <LLOQ(1.80) 11749 17.6 <LLOQ(2.09) 4.36 <LLOQ(2.80) <LLOQ(1.40) <LLOQ(3.20) 1.94 11750 11751 20.8 6.60 5.48 <LLOQ(2.09) 4.37 <LLOQ(2.11) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(1.8Q) 1.85 11752 45.3 <LLOQ(2.09) 4.09 <LLOQ(2.80) <LLOQ(1.40) <LLOQ(3.20) 2.05 11753 29.2 3.61 2.28 2.95 <LLOQ(1.40) <LLOQ(3.20) <LLOQ(1.80) 11754 37.8 <LLOQ(2.09) 3.66 7.38 <LLOQ(1.40) <LLOQ(3.20) <LLOQ(1.80) 11756 36.4 4.53 8.37 3.59 <LLOQ(1.40) <LLOQ(3.20) 6.89 y NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 95 000557 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) A11 concentrations are expressed as ppb. Sample ID 11757 PFOS Concentration (ppb) 34.1 11758 24.8 11759 17.9 11761 17.2 11762 20.0 11763 28.3 11765 22.3 11766 49.1 11767 16.6 11768 14.8 11769 26.0 11771 6.03 11772 40.4 11773 9.26 11156 44.3 11157 28.0 11158 21.5 11159 40.0 PFHS* Concentration (ppb) 6.63 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2,09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 4.13 <LLOQ(2.09) <LLOQ(2.09) 2.16 4.10 3.04 PFOA* Concentration (PPb) 3.58 4.65 4.20 <LLOQ(2.11) 2.82 6.68 2.62 4.74 2.97 2.52 4.17 2.76 7.03 <LLOQ(2.11) 6.33 3.28 4.16 4.72 PFOSAA* Concentration (PPb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.20 3.55 4.33 <LLOQ(2.80) 7.58 <LLOQ(2.80) 3.18 3.25 2.81 <LLOQ(2.80) 2.87 3.11 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 6.60 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) 2.02 2.22 <LLOQ(1.80) 2.59 2.85 2.94 4.62 2.93 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.93 <LLOQ(1.80) 3.84 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 96 000558 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 11160 PFOS Concentration (PPb) 31.5 11161 20.7 11162 30.9 11163 56.8 11164 76.4 11165 93.3 11166 17.7 11167 11.1 11168 48.1 1.1169 36.6 11170 41.4 11171 48.1 11172 50.3 11173 42.7 11174 65.4 11175 52.6 11176 24.3 11177 30.8 PFHS* Concentration (PPb) <LLOQ(2.09) <LLOQ(2.09) 3.08 2.40 4.42 13.7 3.64 <LLOQ(2.09) 3.33 3.51 <LLOQ(2.09) 5.19 15.3 <LLOQ(2.09) 3.24 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (ppb) 2.74 3.03 6.16 4.63 9.41 5.53 <LLOQ(2.11) <LLOQ(2.11) 4.69 5.19 8.30 4.74 5.31 4.77 6.58 5.50 <LLOQ(2.11) 3.33 PFOSAA* Concentration (PPb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.8Q) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.14 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.2Q) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.80) <LLOQ(1.80) 2.04 <LLOQ(1.8Q) 4.60 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.97 1.96 <LLOQ( 1.80) 3.96 3.37 <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 97 000559 Northwest Bioanalytical Study No. NWBS00-128 Repon No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample PFOS ID Concentration (PPb) 11178 41.0 11179 35.2 11180 28.3 11181 92.8 11182 50.0 11183 37.4 11184 48.8 11185 71.6 11186 21.7 11187 15.1 11188 23.2 11189 52.6 11190 81.9 11191 24.3 11192 27.1 11193 34.3 11194 17.1 11195 45.6 PFHS* Concentration (ppb) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 12.4 25.7 5.94 9.40 4.31 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (PPb) 9.73 3.68 3.44 4.16 14.2 <LLOQ(2.11) 5.68 9.01 4.50 <LLOQ(2.11) <LLOQ(2.11) 13.2 6.91 - 3.26 5.59 7.09 <LLOQ(2.11) 7.49 PFOSAA* Concentration (PPb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 9.91 <LLOQ(2.80) <LLOQ(2.80) 2.92 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) 3.84 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) 2.88 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.97 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 7.86 3.99 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 98 000560 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample PFOS ED Concentration (PPb) 11196 18.2 11197 21.4 11198 38.2 11199 28.8 11200 26.2 11201 24.1 11202 42.1 11203 25.2 11204 31.1 11205 12.8 11206 24.3 11207 44.2 11208 15.9 11209 25.7 11210 29.3 11211 47.5 11212 69.6 11213 51.9 PFHS* Concentration (ppb) <LLOQ(2.09) <LLOQ(2.09) 11.1 <LLOQ(2.09) <LLOQ(2.09) 4.20 10.7 2.79 3.27 2.26 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 4.41 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (Ppb) 4.69 3.76 3.02 <LLOQ(2.11) 2.87 3.00 6.93 3.45 5.55 2.47 6.67 5.25 3.61 4.69 4.32 2.81 7.25 5.10 PFOSAA* Concentration (PPb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 4.64 <LLOQ(2.80) 3.34 3.98 PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) 2.09 <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) 2.07 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.96 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 3.30 2.10 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 99 . 000561 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample PFOS ID Concentration (ppb) 11214 36.4 11215 122 11216 42.5 11217 41.4 11218 57.9 11219 19.4 11220 29.8 11221 46.0 11222 26.5 11223 41.5 11224 64.9 11225 29.9 11226 18.7 11227 23.1 11228 41.4 11229 45.9 11230 85.2 11231 62.9 PFHS* Concentration (PPb) 6.25 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.91 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.Q9) 19.2 5.21 66.3 <LLOQ(2.09) <LLOQ(2.09) 2.33 <LLOQ(2.09) 3.22 2.45 2.51 PFOA* Concentration (ppb) 3.57 5.93 5.22 6.32 6.89 <LLOQ(2.11) 2.94 6.44 2.73 5.80 4.30 4.50 5.01 4.61 6.50 5.43 7.01 3.53 PFOSAA* Concentration (ppb) 4.34 3.21 2.98 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2,80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 4.60 6.36 PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.2Q) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 3.01 <LLOQ(1.80) 3.12 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 4.02 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.07 2.57 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 100 0O05S2 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample PFOS ID Concentration (ppb) 11232 21.6 11233 30.0 11234 39.0 11235 22.0 11236 26.7 11237 80.0 11238 37.8 11239 24.7 11240 37.2 11241 139 11242 65.9 11243 27.0 11244 64.9 11245 29.7 11246 28.2 11247 19.0 11248 36.2 11249 36.3 PFHS* Concentration (ppb) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.23 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.64 <LLOQ(2.09) 5.3 9.47 <LLOQ(2.09) 3.73 2.22 <LLOQ(2.09) <LLOQ(2.09) 5.00 <LLOQ(2.09) PFOA* Concentration (ppb) 4.87 3.10 4.81 3.39 4.13 9.10 4.97 4.41 3.29 20.6 6.87 3.01 8.74 5.21 2.44 3.14 5.70 5.58 PFOSAA* Concentration (PPb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.18 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.83 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.26 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) 4.44 2.15 2.58 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 6.15 2.56 1.88 <LLOQ(1.80) <LLOQ(1.80) 2.49 <LLOQ(1.80) <LLOQ(1.80) 2.17 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 101 000563 Northwest Bioanalytical Study No. N W BS00-128 Report No. NWBR01-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 11250 PFOS Concentration (ppb) 26.1 11251 34.6 11252 13.1 11253 56.8 11254 50.8 11256 47.8 11257 33.8 11258 23.1 11259 7.63 11260 34.7 11261 12.6 11262 17.7 11263 226 11264 42.2 11265 24.7 11266 27.2 11267 36.8 11268 39.7 PFHS* Concentration (PPb) 4.07 2.19 <LLOQ(2.09) 4.36 <LLOQ(2.09) 7.07 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 4.14 3.80 <LLOQ(2.09) <LLOQ(2.09) 5.11 2.45 <LLOQ(2.09) 11.3 <LLOQ(2.09) PFOA* Concentration (PPb) 2.32 5.07 <LLOQ(2.11) 7.39 4.81 2.64 5.55 4.33 <LLOQ(2.11) 5.12 2.53 4.07 52.3 3.54 5.69 3.47 2.84 2.47 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 21.2 3.65 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 7.22 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.87 <LLOQ(1.80) <LLOQ( 1.80) <LLOQ(1.80) <LLOQ(1.80) 1.86 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 102 000564 Northwest Bioanalytical Study No. N W B S00-128 Repon No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 11269 PFOS Concentration (ppb) 25.2 PFHS* Concentration (PPb) 3.67 PFOA* Concentration (PPb) 2.54 PFOSAA* Concentration (PPb) <LLOQ(2.80) PFOSA* Concentration (PPb) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 103 000565 Northwest Bioanalytical Table 23. Repeat Analysis Table for PFOS Study No. NWBS00-128 Report No. NWBRO1-066 Sample ID 11689 Original Cone, ppb >ULOQ(414) Original Run Number 10 Reason for Reassay 1 Reassay Cone, ppb 1670 Reassay Run Number 17 Reported Cone, ppb 1656* * Concentration corrected for amount o f persistent PFOS in dilution matrix. Reason for Reported Cone. 1 REASONS FOR REASSAY: 1). Greater than the ULOQ. REASONS FOR REPORTED CONC: 1). Original result outside o f quantitation range. Reassay results reported. Page 104 00056 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Figure 1. Representative Calibration Curve for PFOS Analytical Run I analyzed on 27-Nov-2000 Calibration Standards for PFOS (ppb) Regression Method - QUADRATIC - Weighting Factor - l/X**2 Quadratic Limit - 349 Insttumenl Response Figure 2. Representative Calibration Curve for PFHS Analytical Run l analyzed on 27-Nov-2000 Calibration Standards for PFHS (ppb) Regression Method - QUADRATIC - Weighting Factor * l/X**2 Quadratic Limit "1 1 9 0 lustrumoil Response Page 105 000567 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Figure 3. Representative Calibration Curve for PFOA Analytical Run I analyzed on 27-Nov-2000 Calibration Standards for PFOA (ppb) Regression Method - QUADRATIC Weighting Factor l/X**2 Quadratic Limit 10400 Instrument Response Figure 4. Representative Calibration Curve for PFOSAA Analytical Run I analyzed on 27-Nov>2000 Calibration Standards for PFOSAA (ppb) Regression Method " QUADRATIC * Weighting Factor I/X**2 Quadratic Limit -1 11000 Insmimou Response Page 106 0005C * Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Figure 5. Representative Calibration Curve for PFOSA Analytical Run I analyzed on 27-Nov-2000 Calibration Standards for PFOSA (ppb) Regression Method * QUADRATIC Weighting Factor - 1/X**2 Quadratic Limit - 1160 Instrument Response Figure 6. Representative Calibration Curve for M556 Analytical Run l analyzed on 27-Nov-2000 Calibration Standards for M556 (ppb) Regression Method - QUADRATIC *Weighting Factor - 1/X**2 Quadratic Limit *-5890 Instrument Response Page 107 000569 Northwest Bioanalytieal Study No. NWBS00-128 Report No. NWBRO1-066 Figure 7. Representative Calibration Curve for M570 Analytical Run I analyzed on 27-Nov-2000 Calibration Standards for M570 (ppb) Regression Method QUADRATIC * Weighting Factor t/X**2 Quadratic Limit - 3420 Page 108 000370 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Figure 8. Human Plasma Blank for PFOS (PFOS Internal Standard; fHPfOS Use Area Absolute Retention Time Expected RT 5.31 I Current Method Norse Hues. 5.0 5.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 12 12 Oase. Width 150 150 RT Win. (secs) 20 20 Smooth l 1 sOOl 2 0014M 1011 S00128 CONTROLJ3LANK I No Comment ITHPFOS use as Internal Standard Expccied RT 4.63 Current Method Noise Thres. TQ.O 10.0 Quant Thres. 0.2 0.2 M in. Width 33 Mult. Width 10 10 Base. Width ISO 150 TW In. (secs) 20 20 Smooth 11 SOOI2001411 1 011 SCOI 28 CONTROL.BLANK I No Comment Page 109 000571 Northwest Bioanalytical Study No.NWBSOO-128 Report No. NWBRO1-066 Figure 9. Human Plasma Blank for PFHS iP fH S Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 4.00 ~I Current Method Noise Threi. 3 0 3.0 Quant Thres. 0.5 0.5 Min. Width 44 Mult. Width 12 11 Base. Width 150 150 T Win. (secsl 20 20 Smooth 1 >0012801 -O il 1 011 500128 CO NTR Ol.BlANK ! No Comment [THPFOS use as Internal Standard Expected RT 4.63 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. width 33 Mult. Width 10 10 Base. Width 150 150 T W in. (secs) 20 20 Smooth 11 1 011 S00128 CONTROl.SLANtC 1 Mon, Nov 27. 2000 7:20 PM 9.96 in 1 period 38 lo a -, No Comment 285 intensity: 23 eps 1: 8.98 m RM. 571 scam ; 9 o - 427.0>407.0 80 ;:: Area 0 Heisht 0 Start Time End Time imeeration Width Retention Time Integration Tvoe 70- 0.00 0.00 0.00 0.00 IE@ S O -' 504030- ` 33S ? : --tjHrt z 120 210 260 422 304 20- 10- 101 - 201 301 401 3 0 1 1.59 5.1? 4.74; 6 .3 2 ". 7.90 l r , r Page 110 000572 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NW BR0I-066 Figure 10. Human Plasma Blank for PFOA IPOAA Internal Standard: THPfOS U$e Area Absolute Retention Time Expected RT 4.59 Current Method ] Noise fhres. 10 1.0 Quenl Thres. 0.9 0.9 Min. Width 3J Mult. Width 10 10 Base. Width 150 ISO RT Win. (tecs) 20 20 Smooth 1 1 ITHPFOS u m as Internal Standard Expected RT 4.63 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 ISO T W in. (secs) 20 20 Smooth 1 1 $0012801-011 1 011 s o o t28 CON TROt,,BLANK 1 Mon, Nov 27, 2000 7:20 PM 8.98 in 1 period 1: 8.9BMRM. 571 scans 4 2 7 .0 > 407.0 Area 0 Height 0 Start Time End Time frweeration Width Retention Time Integration Tvoe 0.00 0.00 0.00 0.00 |g]gx No Comment intensity : 23 op 000573 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Figure 11. Human Plasma Blank for PFOSAA IPFOSAA Interrul Standard: THPP05 Use Area Absolute Retention Time Expected RT S.93 | Current Method Noise Ihres. 4.0 4.0 Quant Hires. IS 1.5 Win. w id th 33 Mull. Width 13 13 Base. Width 150 150 IT W in. (secs! 20 20 Smooth 11 t 011 $00120 CONfRCX_8LANlC 1 Mon, NOW 27, 2000 7:20 PM 8.98 in 1 period 100 1: 8.98 MRM, 571 scans 90 S84.1->4I9.1 30 Area 2658 Heiehl 383 Start Time End Time Integration Width Retention Time Integration Tvoe iti4HM a S.78 6.19 0.41 6.04 A -B B 70' 60 30 40 30 20- ::ro o Intensity : 406 cps 383 3 0 t OCenr-p* 7*90 ITHPFOS use as Internal Standard ~I Expected RT 4.63 Current Method Noise Thres. 10.0 10.0 Q uint Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width ISO ISO T Win. (secs) 20 20 Smooth 11 $0012801-011 1 011 500128 CON TROL_BLANK 1 No Comment Page 112 000574 Northwest Bioanalytieal Study No. NWBS00-I28 Report No. NWBRO1-066 Figure 12. Human Plasma Blank for PFOSA jPFOSA ~ Internal Standard: IHPFOS Use .\<ea Absolute Retention firne Expected R f 5.70 I Current Method Noise Hues. JO J.O Quant Hues. t.O 1.0 Min. Width 5S Mull. Width 10 to Base. Width ISO ISO T Win. (secs) 20 20 Smooth 11 sQQI 2801 OU 1 011 SOOt 28 CONTROL BLANK 1 Mon, Nov 27. 2000 7:20 PM 8.99 in 1 period 1: 8.9B MAM, 571 scans 498.0- >78.0 Area 2097 Height 140 Stan Time End Tme tntetrarion Width Retention firne Inteeration Tvoe S.56 6.07 0.50 5.80 A B8 E ia No Comment intensity : 157 ops ' 368 .1 ITHPfOS use as Internal Standard Expected R f 4.63 I Current M ethod Noise Hires. 10.0 Quant Thres. 0.2 Min. Width 3 Mull. Width ___ 10 10 Base. Width 150 ISO RT Win. (secs) 20 20 Smooth 1 S0012801-011 1 O il $00128 C0NTRO1.8LANK 1 Mon, Nov 27, 2000 7:20 PM 8.96 in 1 period 1: 8.98 MAM. 571 scans 427.0-> 407.0 Area 0 Height 0 Start Time End Time Integration w idth Retention Time Integration Tvoe 0.00 0.00 0.00 0.00 IS IS No Comment Page 113 000575 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Figure 13. Human Plasma Blank for M556 IM55& Internai Standard: THPfOS Us Are Absolute Retention Time Expected RT 5.37 I Current Method Noise Hues. 0.4 0.4 Q u.tft fhres. 0.1 0.1 Min, Width 3 3 Mult. Width 11 U Base. Width 150 ISO T W in. (secs) 20 20 Smooth 1 1 sOOl2601-011 1 O il SOOl28CONTROL_BLANK 1 No Comment ITHPfOS use as Internal Standard Expected RT 4.63 I Current Method Noise Hires. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 IQ Base, Width 150 ISO RT W in. (secs) 20 20 Smooth 11 0012801-011 1 011 S00128 CONTROl_8LANK 1 No Comment 000576 Northwest Bioanalytieal Study No. NWBSOO-128 Report No. NWBRO1-066 Figure 14. Human Plasma Blank for IYI570 ITHWOS u w as Internal Standard Expected RT 4,63 Current Method NotieThres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 10 8ase. Width ISO 150 RT W in. (seal 20 20 Smooth 1 $0012801-011 1 011 S00128 COn TROL_8LANK 1 Mon, Nov 27. 2000 7 0 0 PM 0.98 in 1 period 3d TOO- No Comment 285 ; intensity : 23-ops 1: 8.98 M RM, 571 scans 90- 4 2 7 0 -> 407.0 Area 0 Heieht 0 Start Time End Time Infiltration W idth Retention Time (mentation Tvoe 19 0.00 0.0Q 0.00 0.00 EGI 80 * 'So-: so- : so40- 30- t2 0 210 260 336 422 "304 -20 101- 0 -- 101 201 . 301 401 30t 1.39 3.17 4.74 6 3 2 7.90 tSSBT Page 115 000577 Northwest Bioanalytieal Study No. N W BS00-128 Report No. NWBRO1-066 Figure 15. Human Plasma Blank with Internal Standard (QCO) for PFOS iPFb Internal Standard: THPfOS Use Area Absolute Retention Tima Expected RT SJ1 ] Current Method Noise Hues. 5.U 5.0 Quant Ihres. 0.2 0.2 Min. Width 33 M ull. Width 12 12 Base. Widlh ISO 150 RT Win. (secs) 20 20 Smooth 11 $0012001-012 1 012 SOO128QC0 1 No Commet ITHPfOS u w as Internal Standard Expected ST 4.63 | Current Method Noise Thfes. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Widlh 10 10 Base. Width 150 150 TW In. (secs) 20 20 Smooth 1 1 $0012601-012 I 012 S00128 QCO 1 Mon. Nov 27, 2000 7 J2 PM 8.98 in 1 period 1: 8.90 m Rm , 571 scans 427.0-> 407.0 Area 185736 HeiJtht 27311 Start Time End Time [mentation Width Retention Time Integration Tvoe miwHttl 4.30 4.04 0.54 4.51 A -B B IE No Comment Page 116 000578 Northwest Bioanalytieal Study No. NWBSOO-128 Report No. NWBRO1-066 Figure 16. Human Plasma Blank with Internal Standard (QCO) for PFHS [PFHS Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 4.00 1 Curie Method Noise rhres. 3 0 3.0 Quant Thres. a.s 0.5 Min. Width 4 4 M ull. Wldlh 12 12 Base. Width ISO 150 RT Win. (secs) 20 20 Smooth 11 sOQUBQt-OU 10USOQU8QCO1 No Comment ITHPFOS use as Internal Standard Expected RT 4.63 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 10 Base. Width 150 ISO RT W in. (secs) 20 20 Smooth 11 *0012801-012 1 012 500128QC0 1 No Comment Page 117 000579 Northwest Bioanalytical Study No. mVBSOO-128 Report No. NWBRO1-066 Figure 17. Human Plasma Blank with Internal Standard (QCO) for PFOA |P O A .\ Internai Standard: THPFOS Use Area Absolute Retention Time Expected RT 4.59 I Current Method Noise Thres. 1.0 1.0 Quant Hires. 0.9 0.9 Min. Width Mult. Width 33 to 10 Base. Width 150 150 RT Win. {secs) 20 20 Smooth 1I 10012801-012 1 012 S00128 QCO I NoConuncnl |TH WPS u m as Internal Standard Expected RT 4.63 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 10 Bas. Width 150 ISO T Win. (sea) 20 20 Smooth 1 1 $00128014312 1 012 SCOT28 QCO I No Comment Page 118 000580 Northwest Bioanalytieal Study No. NWBSOO-128 Report No. NW BRO1-066 Figure 18. Human Plasma Blank with Internal Standard (QCO) for PFOSAA IfPOSAA Internal Standard: THPFOS U w Area Absolute Retention Time Expected RT S.93 I Current Method Noise Thres. 4.0 4.0 Quant Thres. t.S 1.5 Min. Width 33 Mult. Width 13 13 Base. Width ISO ISO T w in , (seal 20 20 Smooth I 1 1 012 $00129 QCO 1 ITHPfOS use as Internal Standard Expected RT 4.63 I Current Method Noise Thres. !0.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 10 Base. Width ISO ISO TW In. (secs) 20 20 Smooth I 1 S00128Q1-Q12 1 012 S0Q128 QCQ 1 No Comment Page 119 000581 Northwest Bioanalytical Study No. NWBSQ-128 Report No. NWB RO1-066 Figure 19. Human Plasma Blank with Internal Standard (QCO) for PFOSA iPfQS Internal Siandard: THPPOS Use Area Absolute Retention Time Expected RT S.70 \ Current Method Nose Thes. 3.0 3.0 Quant Thres. 1.0 1.0 Mm. Width SS Mult. Width 10 10 Base. Width ISO 150 T W in. (secs) 20 20 Smooth 11 1 012 S00128 QCO I Mon. Nov 27. 2000 732 PM 8.98 in 1 period U 8.98 MUM, 571 scans 498.0->78.0 1 X * -* Area MSI Height 192 Starr Time End Time Integration Width Retention Time Integration Tvoe 5.61 6.10 0.49 s.aa A - 08 ES intensity: 208 ops 20 r 301 401 4.74 _0.32 ITHPfOS use as Internal Standard Expected RT 4.63 I Current Method Noise Thres. 10.0 1.0 Quant Thres. 0.2 0.2 Min. width 33 Mult. Width to 10 Base. Width ISO 150 T W in. (seat Smooth 20 20 11 10012801-012 I 012 SCOI 28 QCO 1 No Comment iScanrj-- Tvm fi Page 120 000582 Northwest Bioanalytical Study No. NWBS00-12S Report No. NWBRO1-066 Figure 20. Human Plasma Blank with Internal Standard (QCO) for M556 |MSSi internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5J7 I Current Method No*se Thtus. 0.4 0.4 Quant Three. 0.1 0.1 Min. Width 3 3 Mult. W idth 11 11 Base. W idth 150 150 RTWin. (secs) 20 20 Smooth 1 1 $0012801-012 I 012 S00128 QCO I No Comment 1THPFOS use as internal Standard Expected RT 4.63 I Current Method Noise Thres. 10.0 >0.0 Quant Thres. 0.2 0.2 Min. Width 3 3 M u lt Width 10 10 Base. Width 150 150 RT W in. (secs) 20 20 Smooth 1 1 0012801-012 1 012 500128 QCO I No Comment Page 121 000583 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Figure 21. Human Plasma Blank with Internal Standard (QCO) for M570 Internai Standard: THPFOS Use Area Absolute Rtention Tim Expeaed RT 5.63 Current Method Noise Thres. 3.0 3.0 Quant Thres. (3.5 0.5 Min. Width 55 Mult. W idth 15 15 Base. Width 150 ISO RT Win. (seal 2Q 20 Smooth 11 JQI28I-012 1 012 S0012B QCO 1 No Comment IHPFOS use as Internal Standard Expected RT 4.63 Current Method Noise Thres. 10.0 !0.0 Quant Thres. 0.2 0.2 Min. Width 33 Mull. Width 10 10 Base. W idth 150 150 RT Win. (sea) 20 20 Smooth 11 *0012801-012 1 012 50012 QCO I No Comment Page 122 000584 Northwest Bioanalytieal Figure 22. Low Standard for PFOS Study No. NWBSOO-128 Report No. NWBRO1-066 IPFOS Internal Standard: THPfOS Ute Area Absolute Retention Time Expected RT $.31 S.OI Current Method Noise Thres. Quant Thres. Min. Width Mult. Width 0.2 3 !2 Base. Width 150 RT Win. (secs) Smooth 20 1 S012801-002 1 002S00128 Sfdl 1 1 NoCommeni ITHPFOS use as Internal Standard Expected RT 4.63 1 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 10 Base. Width ISO 150 RT Win. {secsl 20 20 Smooth t sOOl 2801-002 1 002 S00128 Sidl 1 No Comment Page 123 005S5 Northwest Bioamlytical Figure 23. Low Standard for PFHS Study No. NWBSOO-128 Report No. NWBRO1-066 IPFHS Internal Standard: THPfOS U i .Area Absolute Retention Time Expected RT 4.00 1 Current Method Not* Thres. 3.0 3.0 Quant Thres. O.S 0.5 Min. Width 4 4 Mult. W idth 12 12 Base. Width 150 ISO RT W in. (sees) 20 20 Smooth 11 10012901002 t 0O2SOOt29Sld1 I 1 NoCommnl ITHPFOS use a s Internal Standard Expected RT 4.63 Current Method I Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width ISO ISO RT W in. (secs) 20 20 Smooth 1 1 S00F28O1-O02 1 002 S00129 SkM 1 1 NoCommenl Page 124 000586 Northwest Boanalytical Figure 24. Low Standard for PFOA Study No. NWBSOO-128 Report No. NW BRO1-066 Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 4.S9 Current Method Noise Hires. 1.0 1.0 Quant Hires. 0.9 0.9 Min. Width Mult. Width Base. Width 33 10 to ISO ISO RTWin. (seal 20 20 Smooth 1t I 002 500128 Stdl 1 1 Mon. Nov 27, 2000 S:J6 PM 8.98 in t period 1QCH 1: 8.98 MRM, S71 scans 90* 413.0-> 169.0 :'8 ; Area 6248 Hetehr 669 Start Time End Tim Integration W idth Retention Time Integration Tvoe 4.25 4.77 0.52 4.54 A 88 BQ -70- 60- 30- : 49-' j- 30- No Comment 288 ; intensity : 884 ops :; 421 rot 1.3 :230.i1:t' - 30t 4.74 :"48d.3r.2- St ; h-7:90t iI:STcW^pISr- ITHPfOS use as Internal Standard Expected RT 4.63 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width to 10 Base. Width ISO 150 IT W in. (secs) 20 20 Smooth 1 1 >0012801-002 t 002 S00128 Stdl t 1 Mon, Nov 17. 2000 5:36 PM 8.9S in 1 period 1: 8.98 MRM, 571 scans 427.0->407.0 Area 178943 Height 26839 Start Time End Time Integration Width Retention Time Integration Type 4.30 4.87 0.57 4.51 A -88 No Comment intensity : 26841; ops Page 125 000587 Northwest Bioanalytical Figure 25. Low Standard for PFOSAA Study No. NWBS00-128 Report No. NWBRO1-066 Use Atea Absolute Retention Time Expected RT 5.93 Current Method Noise Thres. 4.0 4.0 Quant Thres. Min. Width 1.5 1.5 33 M ull. Width T3 13 Base. Width 150 150 RT W in. (secs) 20 20 Smooth 11 sOOl 2801 >002 i 002 S0128 Sidl t I No Comment ITHPFOS us* as Internal Standard Expected RT 4.63 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 150 *T Win. (secs) 20 20 Smooth 11 $0012801-002 I 002 S00l28Std1 1 1 No Comment Page 126 000588 Northwest Bioanalytical Figure 26. Low Standard for PFOSA Study No. NWBS00-I28 Report No. NWBRO1-066 I P fOSA Internal Siandatd: THPfOS U s e Area Absolute Retention Time Expected RT S.70 I Current Method Noise ritrei. 3.0 3.0 Quant Thres. t o 1.0 Min. Width S5 Mull. Width 10 10 Base. Width ISO 150 T Win. (secs) 20 20 Smooth 1I 40012801-002 1 002 S00128 Steil 1 1 No Comment ITHPfOS use es Internal Standard Expected RT 4.63 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 10 Base. Width 50 150 *T W in. (sees! 20 20 Smooth 11 50012801 -002 1 002S0012BSld1 1 1 No Page 127 00058 Northwest Bioanalytical Figure 27. Low Standard for M556 Study No. NWBSOO-128 Report No. NWBRO1-066 iMSSi. Internai Standard: THPFOS Use Area Absolute Retention Time Expected RT 5J7 I Current Method Notte ihres. 0.4 0.4 Quant Thres, 0.1 0.1 Min. Width 3 3 M ull. Width 11 11 Base. Width ISO ISO T Win. (seal 20 20 Smooth 11 sOOl 2801 <003 1 003 S00128 Sid2 1 1 No Comment ITHPfOS use as internal Standard Expected RT 4.63 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mull. Width 10 10 Base. Width ISO ISO RT Win. (sea) 20 20 Smooth 11 sOOl 2801 <003 1 003 SOOl 28 Std2 1 t Mon. Nov 27, 2000 S:47 PM 8.98 in 1 period 1: 8.98 MRM, 571 scans 427.0- >407.0 Area 179259 Height 27253 Start Time End Time Integration Width Retention Time Integration Tvoe 4.30 4.84 0.54 4.51 A< 88 B9 No Comment Page 128 000590 Northwest Bioanalytical Figure 28. Low Standard for M570 Study No. NWBSOO-128 Report No. NWBRO1-066 IMS 70 Internai Standard: THPFOS Use Area Absolute Retention Time Expected RT S.63 ] Current Method Noise Hires. 3.0 3.0 Quant Thres. 0.5 0.5 Min. Width 5 5 Mult. Width Base. Width IS IS ISO ISO RTWin. (secs) 20 20 Smooth 1 1 I 002 SO128 Sedi ! I ITHP f OS us M Internal Standard Expected KT 4.63 > Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 J Mult. Width 10 10 Base. Width 150 150 IT Win. (sea) 20 20 Smooth 1 1 *0012801*002 1 002S00128 Stdl 1 1 No Comment Page 129 000591. Northwest Bioanalyttcal Figure 29. High Standard for PFOS Study No. NWBSOO-128 Report No. NWBR01-066 IPFOS ] Current Method Internai Standard: D-tPFOS Noise Thr. Quant fives. 5.0 5.0 0.2 0.2 U m Area Min. Width 3 3 Absolute Retention Time Mult. Width 12 12 Expected RT 5,31 Base. Width 150 150 TWin. (secs) 20 20 Smooth ' 1 S0!2fl01<oe0 1080S0012BStd9 2 1 No Comment ITHPfOS use as Internal Standard Expected RT 4.63 Current Method I Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Muit. Width 10 10 Bast. Width ISO 150 TWin. (sees} Smooth 20 20 11 Page 130 000592 Northwest B ioanalytical Figure 30. High Standard for PFHS Study No. NWBSOO-128 Report No. NWBR01-066 Internal Standard: THPfOS Use Area Absolute Retention Urne Expected RT 4.00 Current Method Noise Thres. JO 3.0 Quant Thres. 0.5 0.5 Min. Width 4 4 Mult. Width 12 12 Base. Width 150 150 RT Win. (sees! 20 20 Smooth 1 1 jOO2801-000 060 S0012B Std9 2 1 No Comment ITHPfOS us as Internal Standard Expected RT 4.63 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 MulU Width 10 10 Base. Width 150 150 TWIn. (secs) 20 20 Smooth 11 sOO 2801-060 1 080 $00128 Std9 2 t No Comment Page 131 000593 Northwest Bioanalytical Figure 31. High Standard for PFOA Study No. NW8S00-128 Report No. NWBRO1-066 IPOAA internai Standard: THPEOS Use Are Absolute Retention Time Expected RT 4.59 I Current Method Noise Hires. 1.0 Quant Thres. Min. Width 0.9 3 Mult. Width 10 Base. Width 150 RT Win. (seal Smooth 30 1 tOQ12601-060 1 080 SQQ126 Std9 2 1 No Comment ITHPfOS use as internal Standard Expected RT 4.63 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mull. Width to 10 Base. Width 150 ISO T Win. (sea) Smooth 20 20 11 *0012001-080 1 080S00128Std9 2 1 No Comment Page 132 000594 Northwest Bioanalytical Figure 32. High Standard for PFOSAA Study No. NWBSOO-128 Report No. NWBRO1-066 IPFOSAA Internai Standard: THPFOS Use Area Absolute Retention Time Expected RT S.93 I Current Method Noise Thres, 4.0 4.0 Quant Hires. 15 1.5 Min. Width ] 3 Mull. Widih 13 13 Base. Width 150 ISO TWin. (secs) 20 20 Smooth 11 *0012801-060 1 080S00128$id9 2 1 No Comment ITHPfOS use as Internal Standard Expected RT 4.63 I Current Method Noise Three. 10.0 10.0 Quant Hires. 0.2 0.2 Min. Width 33 Mult. Width 10 10 Base. Width ISO 150 ETWin. (sea) 20 20 Smooth 11 sOOl 2801-080 l 060 500128 Std9 2 1 No Comment Page 133 000595 Northwest Bioanaiytical Figure 33. High Standard for PFOSA Study No. NWBSOO-128 Report No. NWBRO1-066 Internal Standard: THPfOS Use Area Absolute Retention Time Expected RT S.70 Current Method Noise Thres. 3.0 3.0 Quant Thres. 1.0 1.0 Min. Width 5s Mult. Width 10 10 Base. Width ISO (SO RT Win. (secs) 20 20 Smooth ' 1 sOQl2B01-080 I OBOSOOt28Sid9 2 1 NoComment ITHPPOS use as Iruemal Standard Cxpected RT Current Method Noise Thres. 10.0 10.0 Quant Thres. 0-2 0.2 Min. Width 33 Mult. Width 10 10 Base. Width ISO 150 T w in, (secs) 20 20 Page 134 000596 Northwest Bioaiialytical Figure 34. High Standard for M556 Study No. NWBSOO-128 Report No. NWBRO1-066 Im 5S6 Internat Standard: THPFOS Use Area Absoiute Rtention Time Expected RT 5.J7 1 Cumm Method Noise Thres. a.* 0.4 Quant Thres. 0.1 0.1 Min. Width i 3 Mult. Width 11 M Base. Width ISO 150 RT Win. (secs) 20 20 Smooth ' 1 30012801-OSO 1 0OSO0128SKJ9 2 I No Comment ITHPfQS use as Internai Standard Expected XT 4.63 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Muit. Width 10 10 Base. Width ISO 150 TWin. (secs) 20 20 Smooth 11 30012801-000 1 oao S00128 Sid9 2 1 No Page 135 000597 Northwest Bioanalytical Figure 35. High Standard for M570 Study No. NWBS00-I28 Report No. NWBRO1-066 (M57 Internal Standard: THPFOS Ute Aree Absolute Retenuon firne Expected RT 163 I Current Method Norse Thres. 3.0 3.0 Quant Thres, 0.5 0.5 Min. Width S S Muir. Width 15 IS Base. Width ISO 150 RT Win. (sees) 20 20 Smooth 11 tOGt28Ql-Q8 t 080 S0QI28 Std9 2 \ No Comment ITHPfOS use as Internal Standard Expected RT 4.63 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 M ult Width 10 10 Base. Width 150 ISO RT Win. (secs) 20 20 Smooth 11 10012801-060 1 080S00l2BStd9 2 1 Tue. Nov 2B. 2000 5:39 AM 3.98 in 1 period 1: 8.98 MRM, 571 scans 427.0-> 407.0 Area 160597 Height 18653 Stan Time End Time Inteeration Width Retention Time Integration Type gL lkH ffl 4.27 4.73 0.46 4.51 A . 88 E IS No Comment Page 136 000599