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STUDY TITLE Extraction o f Potassium Perfluorooctanesulfonate from Quail Serum and Quail Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry DATA REQUIREM ENTS Analytical Method Requirements STUDY DIRECTO R Sean Gallagher STUDY COM PLETED ON September 06, 2001 PERFO RM ING LABO RATO RY / TESTIN G FA C ILITY Centre Analytical Laboratories, Inc. (Centre) 3048 Research Drive State College, PA 16801 Phone: 814-231-8032 STUDY SPONSOR 3M Environmental Technology and Safety Services Building 2-3E-09 PO Box 33331 St. Paul, MN 55133-3331 PR O JE C T Centre Protocol Number: 00P-023-041 Centre Study Number: 023-041 Total Pages: 102 C O O l '3 Centre Study No.: 023*041 GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT Centre Study Number 023-041, entitled "Extraction o f Potassium Perfluorooctanesulionate from Quail Serum and Quail Liver for A nalysis U sing HFLCEleetrospray/M ass Spectrometry," conducted for 3M Environmental T echnology and Safety Services, was petformed in compliance with U S EFA TSC A G ood Laboratory Practice Standards (40 CFR Part 792) by Centre Analytical Laboratories, Inc. fry-QlkdLe/._____ smily Ilj Decker Principal Investigator Centre Analytical Laboratories, Inc. ,3luUi Date Study Director W ildlife International, Ltd. Date Bfojyror Representative 3M Environmental Technology and Safety Services Centre Analytical Laboratories, Inc. Page 2 of 102 O O O l* Centre Study No.: 023-041 QUALITY ASSURANCE STATEMENT Centre Analytical Laboratories' Quality Assurance Unit reviewed Centre Study Number 023-041, entitled, "Extraction of Potassium Perfluorooctanesulfonate from Quail Serum and Quail Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry". All phases were reviewed for conduct according to Centre Analytical Laboratories' Standard Operating Procedures, the Study Protocol, and all applicable Good Laboratory Practice Standards. All findings were reported to the Study Director and to management. Phase 1. Protocol Review 2. Extraction 3. Raw Data & Summary Table Review 4. Raw Data and Draft Report Review 5. Final Report Review Date Inspected Date Reported to Date Reported to Centre Study Director and Management Sponsor Management 12/19/00 12/21/00 12/28/00 12/19/00 12/21/00 12/28/00 2/28,3/1/01 3/19/01 3/23/01 3/23-26/01 4/9/01 5/7/01 9/6/01 9/6/01 9/6/01 'U Naomi Lovallo Sr. Quality Assurance Auditor Date Centre Analytical Laboratories, Inc. Page 3 of 102 Cenere Study No.: UZ3-041 CERTIFICATION OF AUTHENTICITY This iep o it. for Centre Study Number 023-041, ia a true and com plete representation o f the raw data for the study. Submitted by: Centre Analytical Laboratories, Inc, 3048 Research Drive State College, PA 16801 (814)231-8032 Principal Investigator, Centre: Centre Analytical Laboratories, Inc Centre Analytical Laboratories. Inc. Facility Management: Centre Analytical Laboratories, Inc. Study Director, W ildlife International: jU w . ^ y Sean Gallagher W ildlife International, Ltd. Sponsor Representative, 3M: Date Centre Analytical Laboratories, Inc. Page 4 of 102 ft'Ol Centre Study No.: 023-041 STUDY IDENTIFICATION Extraction of Potassium Perfluorooctanesulfonate from Quail Serum and Quail Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry CENTRE PROTOCOL NUMBER: 00P-023-041 CENTRE STUDY NUMBER: 023-041 TYPE OF STUDY: Analytical SAMPLE MATRIX: Quail Serum and Quail Liver TEST SUBSTANCE: Perfluorooctanesulfonate (PFOS) SPONSOR: 3M Environmental Technology and Safety Services Building 2-3E-09 POBox 33331 St. Paul, MN 55133-3331 STUDY DIRECTOR: Sean Gallagher Wildlife International, Ltd. 8598 Commerce Drive Easton, MD 21601 SPONSOR REPRESENTATIVE: Rochelle Robideau 3M Environm ental Technology and Safety Services Building 2-3E-09 POBox 33331 St. Paul, MN 55133-3331 TESTING FACILITY: Centre Analytical Laboratories, Inc. 3048 Research Drive State College, PA 16801 ANALYTICAL PHASE TIMETABLE: Study Initiation Date: Experimental Start Date: Experimental Termination Date: Study Completion Date: 12/08/00 12/18/00 03/08/01 09/06/01 Centre Analytical Laboratories, Inc. Page 5 o f 102 Centre Study No.: 023-041 PROJECT PERSONNEL The Study Director for this project was Sean Gallagher at Wildlife International, Ltd. The following personnel from Centre Analytical Laboratories, Inc., were associated with various phases of the study: Name Emily Stauffer Dave Bell Melissa Kennedy Whitsel John Flaherty Tiffany Proctor Angela Morgan Michelle Atjmand Lawrence Ord Rickey Keller Shawn Robb Karen Risha Title Scientist Scientist Supervisor Operations Manager Technician Technician Technician Sample Custodian Sample Custodian Sam ple Custodian Scientist Centre Analytical Laboratories, Inc. Page 6 o f 102 C O O l'8 Centre Study No.: 023-041 TABLE OF CONTENTS Page TITLE PA G E............................................................................................................................. 1 GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT............................... 2 QUALITY ASSURANCE STATEMENT..............................................................................3 CERTIFICATION OF AUTHENTICITY...............................................................................4 STUDY IDENTIFICATION.....................................................................................................5 PROJECT PERSONNEL..........................................................................................................6 TABLE OF CONTENTS..........................................................................................................7 LIST OF TABLES.................................................................................................................... 8 LIST OF FIGURES..................................................................................................................10 LIST OF APPENDICES......................................................................................................... 11 1.0 SUMMARY......................................................................................................................12 2.0 OBJECTIVE.....................................................................................................................12 3.0 INTRODUCTION............................................................................................................ 12 4.0 TEST SYSTEM............................................................................................................... 13 5.0 REFERENCE MATERIAL.............................................................................................13 6.0 DESCRIPTION OF ANALYTICAL METHOD........................................................... 14 6.1 Extraction Procedure..................................................................................................... 14 6.2 Preparation of Standards and Fortification Solutions..................................................14 6.3 Chromatography............................................................................................................ 15 6.4 Instrument Sensitivity.................................................................................................... 15 6.5 Description o f Instrument and Operating Conditions................................................. 15 6.6Quantitation and Example Calculation.........................................................................16 7.0 EXPERIMENTAL DESIGN...........................................................................................18 8.0 RESULTS......................................................................................................................... 18 9.0 CONCLUSIONS........................................................................................................... 18 10.0 RETENTION OF DATA AND SAM PLES................................................................ 19 Centre Analytical Laboratories, Inc. Page 7 of 102 Centre Study No.: 023-041 LIST OF TABLES Page Table I. Summary o f PFOS in Reagent Blanks................................................................21 Table II. Summary o f PFOS in Quail Liver Blanks......................................................... 22 Table III. Summary of PFOS in Quail Serum B lanks....................................................... 22 Table IV. Summary of PFOS Recoveries in Quail Liver................................................... 23 Table V. Summary o f PFOS Recoveries in Quail Serum.................................................24 Table VI. Summary o f PFOS in Adult Liver Samples at 0 ppm a.i. (Test Termination 19 W eeks)......................................................................................25 Table VII. Summary o f PFOS in Adult Liver Samples at 1.8ppm a.i. (Test Termination 6W eeks)........................................................................................ 26 Table VIII. Summary o f PFOS in Adult Liver Samples at 6.2 ppm a.i. (Test Termination 6 W eeks)........................................................................................ 27 Table IX. Summary of PFOS in Adult Liver Samples at 17.6 ppm a.i. (Test Termination 19 W eeks)...................................................................................... 28 Table X. Summary o f PFOS in Juvenile Liver Samples at 0 ppm a.i. (Test Termination 12 W eeks)......................................................................................29 Table XI. Summary o f PFOS in Juvenile Liver Samples at 1.8ppm a.i. (Test Termination 12 W eeks)...................................................................................... 30 Table XII. Summary of PFOS in Juvenile Liver Samples at 6.2 ppm a.i. (Test Termination 12 W eeks)...................................................................................... 31 Table XIII. Summary of PFOS in Juvenile Liver Samples at 17.6 ppm a.i. (Test Termination 12 W eeks)...................................................................................... 32 Table XIV. Summary o f PFOS in Adult Serum Samples at 0 ppm a.i. (Test Termination 19 W eeks)...................................................................................... 33 Table XV. Summary of PFOS in Adult Serum Samples at 1.8 ppm a.i. (Test Termination 6W eeks)........................................................................................ 34 Table XVI. Summary o f PFOS in Adult Serum Samples at 6.2 ppm a.i. (Test Termination 6W eeks)........................................................................................ 35 Table XVII. Summary of PFOS in Adult Serum Samples at 17.6 ppm a.i. (Test Termination 19 W eeks)...................................................................................... 36 Table XVIII. Summary o f PFOS in Juvenile Serum Samples at 0 ppm a.i. (Test Termination 12 W eeks)...................................................................................... 37 Table XIX. Summary of PFOS in Juvenile Serum Samples at 1.8 ppm a.i. (Test Termination 12 W eeks)...................................................................................... 38 Table XX. Summaiy of PFOS in Juvenile Serum Samples at 6.2 ppm a.i. (Test Termination 12 W eeks)...................................................................................... 39 Centre Analytical Laboratories, Inc. Page 8 of 102 000150 Centre Study No.: 023-041 LIST OF TABLES (continued) Page Table XXI. Summary of PFOS in Juvenile Serum Samples at 17.6 ppm a.i. (Test Termination 12 W eeks).....................................................................................40 Table XXII. Summary o f Percent Moistures for Quail Liver Samples............................. 41 Centre Analytical Laboratories, Inc. Page 9 of 102 Centre Study No.: 023-041 Figure 1. LIST OF FIGURES Page Typical Calibration Curve for PFO S................................................................. 43 Figure 2. Chromatogram Representing a 0.1 ng/mL standard for PFOS........................ 44 Figure 3. Chromatogram Representing a 1.0 ng/mL standard for PFOS........................ 45 Figure 4. Chromatogram Representing a Reagent Blank for PFOS (Centre ID Reagent Blank A, Set: 122000A)..................................................................... 46 Figure 5. Chromatogram Representing Control Quail Serum for PFOS (Centre ID: 0011424 Blank A, Set: 122000A).................................................................... 47 Figure 6. Chromatogram Representing Control Quail Liver for PFOS, (Centre ID: 0007870 Blank A, Set: 121900A).................................................................... 48 Figure 7. Chromatogram Representing Control Quail Serum Fortified with 500 ng/mL of PFOS (Centre ID: 0011424 Spk A, Set: 122000A)........................ 49 Figure 8. Chromatogram Representing Control Quail Liver Fortified at 10 ppb with PFOS (Centre ID: 0011423 Spk A, Set: 121800A).................................50 Figure 9. Chromatogram Representing Juvenile Quail Serum Sample (Centre ID: 0007965, Sponsor ID: 9544, Set: 122000A).....................................................51 Figure 10. Chromatogram Representing Juvenile Quail Liver Sample (Centre ID: 0007926, Sponsor ID: 9544, Set: 121800B).....................................................52 Centre Analytical Laboratories, Inc. Page 10 of 102 L :~ 2 Centre Study No.: 023-041 LIST OF APPENDICES Page A p p en d ix A Study Protocol 00P-023-041 (Centre Study No. 023-041) and Amendments and Deviations.......................................................................53 Centre Analytical Laboratories, Inc. Page 11 of 102 0001 3 Centre Study No.: 023-041 1.0 SUMMARY Centre Analytical Laboratories, Inc. (Centre) extracted quail liver samples and quail serum samples for the determination o f perfluorooctanesulfonate (PFOS) according to protocol 00P-023-041 (Appendix A). The limit of quantation for quail liver was 10 ppb and for quail serum 10 ng/mL. These were determined in the method verification study (Centre study 023-054). PFOS in the quail liver samples ranged from non-quantifiable levels (a peak was detected at the corresponding analyte retention time but was less than the lowest concentration o f the calibration standards (0.0001 pg/mL)) to 8.37 pg/g. These results are reported on a wet weight basis. Residues o f PFOS in the quail serum samples ranged from 0.00212 pg/mL levels to 263 pg/mL. The average percent recovery standard deviation for PFOS in serum samples was 108% 10%. The average percent recovery standard deviation for PFOS in liver samples was 95% 11%. 2.0 OBJECTIVE The objective o f this study was to determine levels of perfluorooctanesulfonate (PFOS) in specimens of quail liver and quail serum using the analytical methods described in protocol 00P-023-041. 3.0 INTRODUCTION This report details the results of the analysis for the determination o f PFOS in quail serum and quail liver, using the analytical methods entitled, "Extraction o f Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds From Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry" and "Extraction o f Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds From Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry" with the modifications listed in Section 6. The study was initiated on December 8, 2000, when the study director signed Centre protocol number 00P-023-041. The experimental start date was December 18, 2000, and the experimental termination date was March 8, 2001. Centre Analytical Laboratories, Inc. Page 12 of 102 Centre Study No.: 023-041 4.0 TEST SYSTEM The control quail serum and liver used for the matrix blanks and matrix fortifications was received on November 28,2000 from Wildlife International Ltd., Easton, MD. The control quail liver was assigned the Centre ID o f 0011423 and the control quail serum was assigned the Centre ID o f 0011424. Fifty-six quail serum samples and sixty quail liver samples were received at Centre on August 10, 2000. The samples were stored frozen until they were logged in by Centre personnel on August 16, 2000 and stored frozen. An additional twenty quail serum samples and twenty quail liver samples were received on February 23, 2001 and stored frozen until they were logged in by Centre personnel on February 26,2001. Sample login and chain o f custody information can be found in the raw data package associated with this study. Storage records will be kept at Centre Analytical Laboratories, Inc. and a true copy o f the storage records can be found in the raw data package associated with this study. 5.0 REFERENCE MATERIAL The analytical standard PFOS was received at Centre on June 3, 2000 from 3M Environmental Technology and Services. The available information for the reference material is listed below. The reference material was stored frozen. Stability was not assessed in this study but the reference material was stored according to the certificate of analysis and was used prior to expiration. The solubility o f the reference material was not relevant to this study. Compound PFOS Centre Control No. TCR No. Purity (%) Expiration Date 00-023-042 TCR 00017-46 97.9 08/31/01 The molecular structure of PFOS is given below. PFOS Chemical Name Molecular weight O = = Perfluorooctanesuifonate 499 (C8F17SO3-) C8F17S -- O' o Note: 'Die neutral molecule and standard form from which PFOS (anion) is derived, is potassium perfluorooctanesuifonate [C8F17SO3K], molecular weight 538. Centre Analytical Laboratories, Inc. Page 13 of 102 C C -01 Centre Study No.: 023-041 6.0 DESCRIPTION OF ANALYTICAL METHOD Analytical methods entitled "Extraction of Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds From Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry" and "Extraction of Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds From Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry" with the modifications listed below were used for this study. 6.1 E xtraction P roced u re A 100 pL aliquot o f the serum and ~ 0.50 g sample o f liver was used for the extraction procedure. After fortification o f appropriate samples, the samples were vortexed for ~ 15 seconds. One mL o f 0.5 M TBA was added to the liver samples and 0.5 mL was added to the serum samples. Two mL of 0.25 M sodium carbonate/sodium bicarbonate was added to the liver samples and 1 mL was added to the serum samples. Five mL of MTBE was added to both the serum and liver samples. Each sample was placed on wrist-action shaker for ~ 20 min. and then centrifuged for ~ 15 min. Four mL o f the organic layer was taken and dried on an N-Evap and then reconstituted with 1 mL o f methanol. Each sample was analyzed by LC/MS/MS electrospray. 6.2 P reparation o f Standards and F ortification S olutions Standard solutions were prepared on September 18, 2000 as specified in Centre Analytical Laboratories' protocol 00P-023-041. An individual stock standard solution of PFOS was prepared at a concentration o f 100 pg/mL by dissolving 10 mg o f the standard (corrected for purity and salt content) in methanol. From this solution, a 1.0 pg/mL fortification standard solution was prepared by taking 1 mL o f the stock and bringing the volume up to 100 mL with methanol. T he 0.1 |ig/m L fortification standard w as prepared by taking 10 m L o f the 1.0 pg/m L fortification standard and bringing the volume up to 100 mL with methanol. A 0.01 pg/mL standard was prepared by taking 10 mL o f the 0.1 pg/mL standard and bringing to 100 mL with methanol. A set o f standards containing PFOS was prepared by dilution o f the 0.1 pg/mL and 0.01 pg/mL solutions in the following manner. Initial Cone. (pg/mL)1 Volume (mL) 0.1 5 0.1 2 0.1 1 0.01 5 0.01 2 0.01 1o f PFOS 1 Centre Analytical Laboratories, Inc. Diluted to (mL) 100 100 100 100 100 100 Final Cone. (pg/mL) 0.005 0.002 0.001 0.0005 0.0002 0.0001 Page 14 of 102 -0 0 1 .: Centre Study No.: 023-041 The stock standard solution and all fortification and calibration standard solutions were stored in a refrigerator (4 2C) when not in use. Documentation o f standard preparation can be found in the raw data associated with this report. 6.3 C hrom atograp h y Quantification of PFOS was accomplished by LC/MS/MS analysis using electrospray LC/MS/MS. The retention time o f PFOS was ~ 4.4 min. Peaks were detected in the control matrices corresponding to the analyte retention time and some o f the amounts detected were significant enough to alter the results reported in this study. 6.4 Instrum ent Sensitivity The smallest standard amount injected during the chromatographic run was equivalent to 0.0001 pg/mLofPFOS. 6.5 D escription o f Instrum ent and O perating C onditions Mass Spec: PE SCIEX API 3000 Biomolecular Mass Analyzer Interface: SCIEX Turboion Spray Liquid Introduction Interface Harvard infusion pump Computer: Dell UltraScan PI 110 Software: HPLC: PE SciexAnalyst 1.1 Windows NT Hew lett Packard (HP) Series 1100 HP Quat Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column:Genesis Cs (Jones Chromatography), 2.1 mm x 50 mm, 4p Column Temp.: 35 C Injection Vol.: 10 pL Mobile Phase (A): 2 mM Ammonium Acetate in ASTM type I water Mobile Phase (B): Methanol Flow Rate: 0.3 mL/min. Centre Analytical Laboratories, Inc. Page 15 of 102 CCOi Centre Study No.: 023-041 Time % A % B 0 60 40 1.0 0 100 7.0 0 100 7.5 60 40 11.0 60 40 Ions monitored: Analyte PFOS Mode Transition Monitored negative 499 -> 99 Approximate Retention Time (min') 4.40 T une File Param eters Controls IS-Iospray DP-Declustering Potential FP-Focusing Potential EP-Entrance Potential CE-Collision Energy CXP-Collision Cell Exit Potential DF-Deflector CEM-Channel Electron Multiplier Set -4200.0 -51.0 -230.0 10.0 -70 -5 300.0 2800.0 Gas Flows Nebulizer Gas Curtain Gas Collision Gas TIS Temperature Set 12 13 4 350C 6.6 Q uantitation and E xam ple C alculation Ten microliters o f sample or calibration standard was injected into the LC/MS/MS. The peak area was measured and the standard curve was generated (using 1/x fit weighted linear regression) by Analyst software using six concentrations of standards. The concentration for quail serum and quail liver was determined from the following equations: Use Equation 1 to calculate the amount of analyte found (in ng/mL, based on peak area) using the standard curve (linear regression parameters) generated by the Analyst software program. Then use Equation 2 to calculate the amount of analyte found in pg/g (pg/mL for serum samples). Centre Analytical Laboratories, Inc. Page 16 of 102 G G 0158 Centre Study No.: 023-041 Equation 1: Analyte found (ng/mL) = (Peak area - intercept! slope Equation 2: Analyte found (pg/g) = (anal, found (ng/mL1 x FV (mLl x DF x EV (mLY) x 1 ue (AV (mL) x sample wt. (g)) 1000 ng Where: FV = Final Volume DF = Dilution Factor EV = Extraction Volume AV = Aliquot Volume For samples fortified with known amounts o f PFOS prior to extraction, use Equation 3 to calculate the percent recovery. Equation 3: Recovery (%) = (anal, found fu e /e l - ave. analvte in Ctrl (ue/gY> x 1000 ng x 100% amount added (ng/g) x 1 pg An example of a calculation using an actual sample follows: Quail liver sample Centre ID 0007870 Spk A (Set: 121900A), fortified at 1000 ng/g with PFOS. Where: peak area = 11483 intercept = 463 slope = 2790 dilution factor = 100 ng/g added (fort level) = 1000ng/g avg. amt in controls = 0(Not quantifiable) final volume 1 mL extraction volume = 5 mL aliquot volume = 4 mL sample weight 0.5 g F rom eq u ation 1: Analyte found (ng/mL) = f11483- 4631 2790 From equation 2: Analyte found (pg/g) 3.9 ng/mL (3.9 ne/mL x 1 mL x 100 x 5 mLt x 1ue (4mLx0.5g) 1000 ng = 0.975 pg/mL Centre Analytical Laboratories, Inc. Page 17 of 102 Centre Study No.: 023-041 From equation 3: % Recovery = (0.975 ug/mL - 0 ug/mL'l x HOOP n g /lu el x 100% 1000ng/g = 98% 7.0 EXPERIMENTAL DESIGN Each set of samples (liver or serum) consisted of one reagent blank, one matrix blank, two matrix blanks fortified at known concentrations, and ~ 20 samples. Each sample was extracted using the appropriate method and then analyzed in duplicate. 8 0 RESULTS The PFOS found in the reagent blanks are listed in Table I. The PFOS in the quail liver blanks and quail serum blanks are given in Tables II & III. Individual recoveries for PFOS in the liver samples are detailed in Table IV. The average percent recovery standard deviation for PFOS in liver samples was 95% 11%. Individual recoveries for PFOS in the serum samples are detailed in Table V. The average percent recovery standard deviation for PFOS in serum samples was 108% 10% . PFOS in the quail liver samples ranged from non-quantifiable levels (a peak was detected at the corresponding analyte retention time but was less than the lowest concentration of the calibration standards (0.0001 pg/mL)) to 8.37 pg/g. Individual results are listed in Tables VI-XIII. The results are reported on a wet weight basis. PFOS in the quail serum samples ranged from 0.00212 pg/mL levels to 263 pg/mL. Individual results are listed in Tables XIV-XXI. The average percent moistures for the quail liver samples are given in Table XXII. 9.0 CONCLUSIONS The quail liver and serum samples were successfully extracted and analyzed according to protocol 00P-023-041. Centre Analytical Laboratories, Inc. Page 18 of 102 Centre Study No.: 023-041 10.0 RETENTION OF DATA AND SAMPLES When the final report is complete, all original paper data generated by Centre Analytical Laboratories, Inc. will be shipped to the sponsor. This does not include facility-specific raw data such as instrument logs, however exact copies o f temperature logs will be submitted. Exact copies o f all raw data, as well as a signed copy o f the final analytical report and all original facility-specific raw data, will be retained in the Centre Analytical Laboratories, Inc. archives for the period o f time specified in 40 CFR Part 792. Retained samples of reference substances are archived by the sponsor. Centre Analytical Laboratories, Inc. Page 19 of 102 C O O l .J5h. Centre Study No.: 023-041 TABLES Centre Analytical Laboratories, Inc. Page 20 of 102 0001^2 Centre Study No.: 023-041 Table I. Summary o f PFOS in Reagent Blanks Sponsor ID na na na na na na na na na na na na na na na na Centre ID Reagent Blank A Reagent Blank A* Reagent Blank A Reagent Blank A* Reagent Blank A Reagent Blank A* Reagent Blank A Reagent Blank A* Reagent Blank A Reagent Blank A* Reagent Blank A Reagent Blank A* Reagent Blank A Reagent Blank A* Reagent Blank A Reagent Blank A* * Duplicate injection Set Number 121800A 121800A 121800B 121800B 121900A 121900A 121900B 121900B 122000A 122000A 122000B 122000B 030501A 030501A 030601A 030601A Extraction Analysis Analyte Date Date Found (ng/mL) 12/18/00 12/18/00 12/18/00 12/18/00 12/19/00 12/19/00 12/19/00 12/20/00 12/20/00 12/21/00 NQ NQ NQ NQ NQ 12/19/00 12/21/00 NQ 12/19/00 12/19/00 12/20/00 12/20/00 12/20/00 12/20/00 3/5/01 3/5/01 3/6/01 12/21-22/00 12/21-22/00 12/22/00 12/22/00 12/22-23/00 12/22-23/00 3/6-7/01 3/6-7/01 3/7/01 NQ NQ 0.000200 0.000200 NQ NQ ND ND NQ 3/6/01 3/7/01 ____ m ____ AVERAGE: NQ STANDARD DEVIATION: NQ NQ = Not Quantifiable (A peak was detected at the corresponding analyte retention time but was less than the lowest concentration o f the calibration standards (0.0001 pg/mL)) ND = Not Detected For values recorded as ND.zero was used to calculate the average and standard deviation. For values recorded as NQ, 0.00005 pg/mL (half the value o f the lowest calibration standard, 0.0001 pg/mL) was used to calculate the average and standard deviation. LOQ = 0.01 pg/g for liver and 0.01 pg/mL for serum Centre Analytical Laboratories, Inc. Page 21 of 102 m o i* Centre Study No.: 023-041 Table II. Summary of PFOS in Quail Liver Blanks Sponsor ID na na na Na 454 454 456 456 Centre ID 0011423 Blank A 0011423 Blank A* 0011423 Blank A 0011423 Blank A* 0007870 Blank A 0007870 Blank A* 0007872 Blank A 0007872 Blank A* Set Number 121800A 121800A 121800B 121800B 121900A 121900A 030601A 030601A Extraction Analysis Date Date 12/18/00 12/19/00 12/18/00 12/19/00 12/18/00 12/20/00 12/18/00 12/20/00 12/19/00 12/21/00 12/19/00 12/21/00 3/6/01 3/7/01 3/6/01 3/7/01 AVERAGE: STANDARD DEVIATION: Analyte Found (m r /r ) NQ NQ 0.00113 0.00109 NQ NQ 0.00120 0.00110 0.000590 0.000578 Table III. Summary o f PFOS in Quail Serum Blanks Sponsor ID na na na na na na na na Centre ID 0011424 Blank A 0011424 Blank A* 0011424 Blank A 0011424 Blank A* 0011424 Blank A 0011424 Blank A* 0011424 Blank A 0011424 Blank A* Set Number 121900B 121900B 122000A 122000A 122000B 122000B 030501A 030501A Extraction Analysis Analyte Date Date Found (uR/mL) 12/19/00 12/21-22/00 0.0136 12/19/00 12/21-22/00 0.0144 12/20/00 12/20/00 12/22/00 12/22/00 0.0138 0.0151 12/20/00 12/22-23/00 0.0127 12/20/00 3/5/01 3/5/01 12/22-23/00 3/6-7/01 3/6-7/01 0.0109 0.00555 0.00559 AVERAGE: 0.0115 STANDARD DEVIATION: 0.00384 * Duplicate injection NQ = Not Quantifiable (A peak was detected at the corresponding analyte retention time but was less than the lowest concentration of the calibration standards (0.0001 pg/mL)) For values recorded as NQ, 0.00005 pg/g (half the value o f the lowest calibration standard, 0.0001 pg/mL) was used to calculate the average and standard deviation. LOQ = 0.01 pg/g for liver and 0.01 pg/mL for serum Centre Analytical Laboratories, Inc. Page 22 of 102 GOOlt' Centre Study No.: 023-041 Table IV. Summary of PFOS Recoveries in Quail Liver Sponsor ID na na na na na na na na 454 454 454 454 456 456 456 456 Centre ID 0011423 Spk A 0011423 Spk A* 0011423 Spk B 0011423 Spk B* 0011423 Spk A 0011423 Spk A* 0011423 Spk B 0011423 SpkB* 0007870 Spk A 0007870 Spk A* 0007870 Spk B 0007870 Spk B* 0007872 Spk A 0007872 Spk A* 0007872 Spk B 0007872 Spk B* Set Number 121800A 121800A 121800A 121800A 121800B 121800B 121900A 121900A 121900A 121900A 121900A 121900A 030601A 030601A 030601A 030601A Extraction Analysis Amt Date Date Added (ng/g) 12/18/00 12/19/00 10 12/18/00 12/19/00 10 12/18/00 12/19/00 2000 12/18/00 12/19/00 2000 12/18/00 12/18/00 12/20/00 12/20/00 1000 1000 12/18/00 12/20-21/00 20000 12/18/00 12/20-21/00 20000 12/19/00 12/21/00 1000 12/19/00 12/21/00 1000 12/19/00 12/21/00 20000 12/19/00 12/21/00 20000 3/6/01 3/7/01 20 3/6/01 3/7/01 20 3/6/01 3/7/01 200 3/6/01 3/7/01 200 AVERAGE: STANDARD DEVIATION: RELATIVE STANDARD DEVIATION: % Recovery 102 104 101 103 113 110 80 80 99 103 85 84 93 86 82 84 94 11 12 * Duplicate injection LOQ = 0.01 ng/g for liver and 0.01 ng/mL for serum Centre Analytical Laboratories, Inc. Page 23 of 102 Centre Study No.: 023-041 Table V. Summary of PFOS Recoveries in Quail Serum Sponsor ID na na na na na na na na na na na na na na na na Centre ID 0011424 Spk A 0011424 Spk A* 0011424 Spk B 0011424 Spk B* 0011424 Spk A 0011424 Spk A* 0011424 Spk B 0011424 Spk B* 0011424 Spk A 0011424 Spk A* 0011424 Spk B 0011424 Spk B* 0011424 Spk A 0011424 Spk A* 0011424 Spk B 0011424 Spk B* Set Number 121900BD 121900BD 121900BD 121900BD I22000A 122000A 122000A 122000A 122000B 122000B 122000B 122000B 030501A 030501A 030501A 030501A Extraction Analysis Amt Date Date Added (ng/mL) 12/19/00 12/19/00 12/19/00 12/19/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 3/5/01 3/5/01 3/5/01 3/5/01 12/23-24/00 12/23-24/00 12/23-24/00 12/23-24/00 12/22/00 12/22/00 12/22/00 12/22/00 12/22-23/00 12/22-23/00 12/22-23/00 12/22-23/00 3/6-7/01 3/6-7/01 3/6-7/01 3/6-7/01 500 500 100000 100000 500 500 100000 100000 500 500 100000 100000 100 100 1000 1000 AVERAGE: STANDARD DEVIATION: RELATIVE STANDARD DEVIATION: % Recovery 103 106 90 93 106 103 97 103 108 110 113 98 122 122 107 115 106 9 9 * Duplicate injection LOQ = 0.01 (ig/g for liver and 0.01 ng/mL for serum Centre Analytical Laboratories, Inc. Page 24 of 102 O -'iO iS Centre Study No.: 023-041 Table VI. Summary o f PFOS in Adult Liver Samples at 0 ppm a.i. (Test Termination 19 Weeks) Sponsor ID 451 451* 452 452* 453 453* 454 454* 455 455* 456 456* 457 457* 458 458* 459 459* 460 460* Centre ID 0007867 0007867 0007868 0007868 0007869 0007869 0007870 0007870 0007871 0007871 0007872 0007872 0007873 0007873 0007874 0007874 0007875 0007875 0007876 0007876 Set Number 121800AD 121800AD 121800A 121800A 121800AD 121800AD 121800A 121800A 121800AD 121800AD 121800A 121800A 121800AD 121800AD 121800A 121800A 121800AD 121800AD 121800A 121800A Extraction Date Analysis Date 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/19/00 12/18/00 12/19/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/19/00 12/18/00 12/19/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/19/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/19/00 12/18/00 12/19/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/19/00 12/18/00 12/19/00 AVERAGE: STANDARD DEVIATION: Analyte Found (pg/g) 0.215 0.215 NQ NQ 0.303 0.304 NQ NQ 0.114 0.111 NQ NQ 0.0762 0.0739 0.0103 0.0104 0.236 0.235 0.00117 0.00117 0.09S3 0.113 * Duplicate injection NQ = Not Quantifiable (A peak was detected at the corresponding analyte retention time but was less than the lowest concentration of the calibration standards (0.0001 pg/mL)) For values recorded as NQ, 0.00005 pg/g (half the value o f the lowest calibration standard, 0.0001 pg/mL) was used to calculate the average and standard deviation. LOQ = 0.01 pg/g for liver and 0.01 pg/mL for serum Centre Analytical Laboratories, Inc. Page 25 of 102 COOliSV Centre Study No.: 023-041 Table VII. Summary of PFOS in Adult Liver Samples at 1.8 ppm a.i. (Test Termination 6 Weeks) Sponsor ID EOI-0259-20780 E01-0259-20780* E01-0259-20781 EOI-0259-20781* EOI-0259-20782 EOI-0259-20782* EOI-0259-20783 EOI-0259-20783* E01-0259-20784 E01-0259-20784* EOI-0259-20790 EOI-0259-20790* EOI-0259-20791 EOI-0259-20791* EOI-0259-20792 E01-0259-20792* EOI-0259-20793 EOI-0259-20793* EOI-0259-20794 EOI-0259-20794* Centre ID 0102997 0102997 0102998 0102998 0102999 0102999 0103000 0103000 0103001 0103001 0103007 0103007 0103008 0103008 0103009 0103009 0103010 0103010 0103011 0103011 Set Number 030601 AD 030601 AD 030601AD 030601 AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601 AD 030601 AD 030601 AD 030601AD 030601 AD 030601A 030601A 030601 AD 030601AD 030601 AD 030601AD Extraction Date Analysis Date 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/7/01 3/6/01 3/7/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 AVERAGE: STANDARD DEVIATION: Analyte Found (ME/g) 0.800 0.722 0.149 0.134 0.341 0.311 0.455 0.422 0.0988 0.0843 0.210 0.210 0.177 0.191 0.0124 0.0121 0.0381 0.0394 0.0629 0.0720 0.227 0.224 * Duplicate injection LOQ = 0.01 ng/g for liver and 0.01 jag/mL for serum Centre Analytical Laboratories, Inc. Page 26 of 102 G0 0 1 ^ 8 Centre Study No.: 023-041 Table VIII. Summary of PFOS in Adult Liver Samples at 6.2 ppm a.i. (Test Termination 6 Weeks) Sponsor ID EOI-0259-20785 E01-0259-20785* E 0 1-0259-20786 EOI-0259-20786* E01-0259-20787 EOI-0259-20787* EOI-0259-20788 E01-0259-20788* E01-0259-20789 EOI-0259-20789* EOI-0259-20795 E01-0259-20795* EOI-0259-20796 E01-0259-20796* EOI-0259-20797 E01-0259-20797* EOI-0259-20798 EOI-0259-20798* EOI-0259-20799 EOI-0259-20799* Centre ID 0103002 0103002 0103003 0103003 0103004 0103004 0103005 0103005 0103006 0103006 0103012 0103012 0103013 0103013 0103014 0103014 0103015 0103015 0103016 0103016 * Duplicate injection Set Number 030601AD 030601AD 030601 AD 030601 AD 030601 AD 030601 AD 030601 AD 030601 AD 030601 AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601 AD 030601 AD 030601 AD 030601 AD 030601 AD 030601 AD Extraction Analysis Date Date 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/6/01 3/8/01 3/8/01 3/6/01 3/8/01 3/6/01 3/6/01 3/6/01 3/8/01 3/8/01 3/8/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 AVERAGE: STANDARD DEVIATION: Analyte Found 0ig/g) 1.15 1.20 1.18 1.19 1.43 1.42 1.60 1.51 1.06 1.17 0.216 0.208 0.115 0.0934 0.0801 0.0797 0.187 0.218 0.0901 0.0954 0.715 0.606 LOQ = 0.01 ng/g for liver and 0.01 pg/mL for serum Centre Analytical Laboratories, Inc. Page 27 of 102 0001^9 Centre Study No.: 023-041 Table IX. Summary of PFOS in Adult Liver Samples at 17.6 ppm a.i. (Test Termination 19 Weeks) Sponsor ID 481 481* 482 482* 483 483* 484 484* 485 485* 486 486* 487 487* 488 488* 489 489* 490 490* Centre ID 0007877 0007877 0007878 0007878 0007879 0007879 0007880 0007880 0007881 0007881 0007882 0007882 0007883 0007883 0007884 0007884 0007885 0007885 0007886 0007886 Set Number 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD Extraction Date Analysis Date 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 AVERAGE: STANDARD DEVIATION: Analyte Found (gg/g) 1.05 1.05 4.10 4.17 8.37 8.30 1.41 1.43 1.54 1.51 0.415 0.392 1.17 1.15 0.511 0.509 2.42 2.48 0.351 0.360 2.13 2.39 * Duplicate injection LOQ = 0.01 p.g/g for liver and 0.01 pg/mL for serum Centre Analytical Laboratories, Inc. Page 28 of 102 000170 Centre Study No.: 023-041 Table X. Summary of PFOS in Juvenile Liver Samples at 0 ppm a.i. (Test Termination 12 Weeks) Sponsor ID 9503 9503* 9506 9506* 9508 9508* 9512 9512* 9515 9515* 9518 9518* 9520 9520* 9522 9522* 9525 9525* 9526 9526* Centre ID 0007907 0007907 0007908 0007908 0007909 0007909 0007910 0007910 0007911 0007911 0007912 0007912 0007913 0007913 0007914 0007914 0007915 0007915 0007916 0007916 Set Number 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B Extraction Date Analysis Date 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 AVERAGE: STANDARD DEVIATION: Analyte Found (ufi/g) NQ NQ NQ NQ NQ NQ NQ NQ 0.000785 0.000755 NQ NQ 0.000734 0.000672 0.000718 0.000656 NQ NQ NQ NQ 0.000251 0.000316 * Duplicate injection NQ = Not Quantifiable (A peak was detected at the corresponding analyte retention time but was less than the lowest concentration o f the calibration standards (0.0001 pg/mL)) For values recorded as NQ, 0.00005 pg/g (half the value o f the lowest calibration standard, 0.0001 pg/mL) was used to calculate the average and standard deviation. LOQ = 0.01 pg/g for liver and 0.01 pg/mL for serum Centre Analytical Laboratories, Inc. Page 29 of 102 O ^ O i.7 * Centre Study No.: 023-041 Table XI. Summary of PFOS in Juvenile Liver Samples at 1.8 ppm a.i. (Test Termination 12 Weeks) Sponsor ID 9528 9528* 9529 9529* 9530 9530* 9531 9531* 9533 9533* 9535 9535* 9540 9540* 9541 9541* 9543 9543* 9544 9544* Centre ID 0007917 0007917 0007918 0007918 0007919 0007919 0007920 0007920 0007921 0007921 0007922 0007922 0007923 0007923 0007924 0007924 0007925 0007925 0007926 0007926 Set Number 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 12I800B 121800B 121800B 121800B 121800B 121800B 121800B Extraction Analysis Date Date 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 AVERAGE: STANDARD DEVIATION: Analyte Found Gig/g) 0.0130 0.0128 0.00295 0.00295 0.00904 0.00876 0.00417 0.00435 0.0119 0.0117 0.0113 0.0114 0.00635 0.00623 0.00305 0.00297 0.0126 0.0126 0.00514 0.00521 0.00792 0.00393 * Duplicate injection LOQ = 0.01 |Ag/g for liver and 0.01 (xg/mL for serum Centre Analytical Laboratories, Inc. Page 30 of 102 G O O l '^ Centre Study No,: 023-041 Table XII. Summary of PFOS in Juvenile Liver Samples at 6.2 ppm a.i. (Test Termination 12 Weeks) Sponsor ID 9548 9548* 9549 9549* 9551 9551* 9552 9552* 9555 9555* 9559 9559* 9561 9561* 9562 9562* 9563 9563* 9564 9564* Centre ID 0007927 0007927 0007928 0007928 0007929 0007929 0007930 0007930 0007931 0007931 0007932 0007932 0007933 0007933 0007934 0007934 0007935 0007935 0007936 0007936 Set Number 121900A 121900A 121900A 121900A 121900A 121900A 121900A 121900A 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900A 121900A 121900AD 121900AD 121900A 121900A Extraction Analysis Date Date 12/19/00 12/21/00 12/19/00 12/21/00 12/19/00 12/21/00 12/19/00 12/21/00 12/19/00 12/21/00 12/19/00 12/21/00 12/19/00 12/21/00 12/19/00 12/21/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/21/00 12/19/00 12/21/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/21/00 12/19/00 12/21/00 AVERAGE: STANDARD DEVIATION: Analyte 0.00303 0.00305 0.0100 0.0105 0.0123 0.0125 0.00316 0.00302 0.0410 0.0408 0.0340 0.0341 0.0446 0.0445 0.0116 0.0121 0.0193 0.0197 0.00184 0.00201 0.0182 0.0156 * Duplicate injection LOQ = 0.01 pg/g for liver and 0.01 pg/mL for serum Centre Analytical Laboratories, Inc. Page 31 of 102 0001"?3 Centre Study No.: 023-041 Table XIII. Summary of PFOS in Juvenile Liver Samples at 17.6 ppm a.i. (Test Termination 12 Weeks) Sponsor ID 9567 9567* 9570 9570* 9575 9575* 9579 9579* 9580 9580* 9581 9581* 9582 9582* 9583 9583* 9584 9584* 9588 9588* Centre ID 0007937 0007937 0007938 0007938 0007939 0007939 0007940 0007940 0007941 0007941 0007942 0007942 0007943 0007943 0007944 0007944 0007945 0007945 0007946 0007946 Set Number 121900A 121900A 121900AD 121900AD 121900A 121900A 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD Extraction Analysis Date Date 12/19/00 12/21/00 12/19/00 12/21/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/21/00 12/19/00 12/21/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 AVERAGE: STANDARD DEVIATION: Analyte Found (pg/g) 0.00904 0.00912 0.0424 0.0429 0.00629 0.00623 0.0880 0.0898 0.0461 0.0441 0.0492 0.0451 0.0747 0.0733 0.156 0.132 0.0983 0.101 0.0350 0.0370 0.0593 0.0417 * Duplicate injection LOQ = 0.01 gg/g for liver and 0.01 pg/mL for serum Centre Analytical Laboratories, Inc. Page 32 of 102 c - o o i ;1 Centre Study No.: 023-041 Table XIV. Summary o f PFOS in Adult Serum Samples at 0 ppm a.i. (Test Termination 19 Weeks) Sponsor ID 451 451* 452 452* 453 453* 454 454* 455 455* 456 456* 457 457* 458 458* 459 459* Centre ID 0007887 0007887 0007888 0007888 0007889 0007889 0007890 0007890 0007891 0007891 0007892 0007892 0007893 0007893 0007894 0007894 0007895 0007895 Set Number 121900BD 121900BD 121900B 121900B 121900BD 121900BD 121900B 121900B 121900B 121900B 121900BD 121900BD 121900BD 121900BD 121900BD 121900BD 121900BD 121900BD Extraction Analysis Date Date 12/19/00 12/23-24/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/23-24/00 12/2 1 -22/00 12/21-22/00 12/23-24/00 12/23-24/00 12/21-22/00 12/21-22/00 12/21-22/00 12/21-22/00 12/23-24/00 12/23-24/00 12/23-24/00 12/23-24/00 12/23-24/00 12/23-24/00 12/23-24/00 12/23-24/00 AVERAGE: STANDARD DEVIATION: Analyte Found (pg/mL) 11.6 11.8 0.0102 0.00909 9.04 10.4 0.00274 0.00212 0.0125 0.0123 6.32 6.46 6.58 6.35 0.105 0.102 8.75 8.50 4.78 4.64 * Duplicate injection LOQ = 0.01 ng/g for liver and 0.01 ng/mL for serum Centre Analytical Laboratories, Inc. Page 33 o f 102 Centre Study No.: 023-041 Table XV. Summary of PFOS in Adult Serum Samples at 1.8 ppm a.i. (Test Termination 6 Weeks) Sponsor ID EOI-0259-20752 EOI-0259-20752* EOI-0259-20753 EOI-0259-20753* EOI-0259-20754 EOI-0259-20754* EOI-0259-20755 EOI-0259-20755* EOI-0259-20756 E01-0259-20756* EOI-0259-20762 EOI-0259-20762* EOI-0259-20763 E01-0259-20763* E01-0259-20764 E01-0259-20764* EOI-0259-20765 EOI-0259-20765* E01-0259-20766 E01-0259-20766* Centre ID 0102969 0102969 0102970 0102970 0102971 0102971 0102972 0102972 0102973 0102973 0102979 0102979 0102980 0102980 0102981 0102981 0102982 0102982 0102983 0102983 Set Number 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD Extraction Date Analysis Date 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 AVERAGE: STANDARD DEVIATION: Analyte Found (uE/mL) 10.9 10.9 7.92 8.01 16.4 16.0 35.8 33.1 24.3 23.7 1.50 1.89 5.01 4.98 1.57 1.84 0.134 0.117 10.5 9.79 11.2 10.7 * Duplicate injection LOQ = 0.01 pg/g for liver and 0.01 (ag/mL for serum Centre Analytical Laboratories, Inc. Page 34 of 102 Centre Study No.: 023-041 Table XVI. Summary of PFOS in Adult Serum Samples at 6.2 ppm a.i. (Test Termination 6 Weeks) Sponsor ID EOI-0259-20757 EOI-0259-20757* E01-0259-20758 E01-0259-20758* EOI-0259-20759 EOI-0259-20759* EOI-0259-20760 EOI-0259-20760* EOI-0259-20761 EOI-0259-20761* EOI-0259-20767 EOI-0259-20767* EOI-0259-20768 E01-0259-20768* EOI-0259-20769 EOI-0259-20769* EOI-0259-20770 E01-0259-20770* EOI-0259-20771 EOI-0259-20771* Centre ID 0102974 0102974 0102975 0102975 0102976 0102976 0102977 0102977 0102978 0102978 0102984 0102984 0102985 0102985 0102986 0102986 0102987 0102987 0102988 0102988 Set Number 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD Extraction Date Analysis Date 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 AVERAGE: STANDARD DEVIATION: Analyte Found (tig/mL) 52.2 56.1 102 94.7 80.4 84.6 69.2 62.9 84.6 86.7 4.57 4.07 2.72 2.61 4.02 3.87 3.24 3.31 2.10 1.70 40.3 39.7 * Duplicate injection LOQ = 0.01 pg/g for liver and 0.01 pg/mL for serum Centre Analytical Laboratories, Inc. Page 35 of 102 e o o i i-- Centre Study No.: 023-041 Table XVII. Summary of PFOS in Adult Serum Samples at 17.6 ppm a.i. (Test Termination 19 Weeks) Sponsor ID 481 481* 482 482* 484 484* 485 485* 487 487* 488 488* 489 489* 490 490* Centre ID 0007896 0007896 0007897 0007897 0007898 0007898 0007899 0007899 0007900 0007900 0007901 0007901 0007902 0007902 0007903 0007903 Set Number 121900BD 121900BD 121900BD 121900BD 121900BD 121900BD 121900BD 121900BD 121900BD 121900BD 121900BD 121900BD 030501AD 030501AD 121900BD 121900BD Extraction Analysis Date Date 12/19/00 12/23-24/00 12/19/00 12/23-24/00 12/19/00 12/23-24/00 12/19/00 12/23-24/00 12/19/00 12/23-24/00 12/19/00 12/23-24/00 12/19/00 12/23-24/00 12/19/00 12/23-24/00 12/19/00 12/23-24/00 12/19/00 12/23-24/00 12/19/00 12/23-24/00 12/19/00 12/23-24/00 3/5/01 3/7-8/01 3/5/01 3/7-8/01 12/19/00 12/23-24/00 12/19/00 12/23-24/00 AVERAGE: STANDARD DEVIATION: Analyte iFound (ue/mL) 260 263 43.1 42.4 118 106 179 172 133 127 15.8 16.8 232 228 6.87 6.80 122 93.0 * Duplicate injection LOQ = 0.01 |ig/g for liver and 0.01 |ig/mL for serum Centre Analytical Laboratories, Inc. Page 36 of 102 000173 Centre Study No.: 023-041 Table XVIII. Summary of PFOS in Juvenile Serum Samples at 0 ppm a.i. (Test Termination 12 Weeks) Sponsor ID 9503 9503* 9506 9506* 9508 9508* 9512 9512* 9515 9515* 9518 9518* 9520 9520* 9525 9525* 9526 9526* Centre ID 0007947 0007947 0007948 0007948 0007949 0007949 0007950 0007950 0007951 0007951 0007952 0007952 0007953 0007953 0007954 0007954 0007955 0007955 Set Number 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A Extraction Analysis Date Date 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/20/00 12/22/00 12/22/00 12/20/00 12/20/00 12/22/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 AVERAGE: STANDARD DEVIATION: Analyte Found (ug/mL) 0.00486 0.00385 0.00718 0.00754 0.00365 0.00319 0.00431 0.00457 0.00789 0.00528 0.00378 0.00481 0.00367 0.00395 0.00552 0.00438 0.00354 0.00388 0.00477 0.00142 * Duplicate injection LOQ = 0.01 ng/g for liver and 0.01 fig/mL for serum Centre Analytical Laboratories, Inc. Page 37 of 102 Centre Study No.: 023-041 Table XIX. Summary of PFOS in Juvenile Serum Samples at 1.8 ppm a.i. (Test Termination 12 Weeks) Sponsor ID 9528 9528* 9529 9529* 9530 9530* 9531 9531* 9533 9533* 9535 9535* 9540 9540* 9541 9541* 9543 9543* 9544 9544* Centre ID 0007956 0007956 0007957 0007957 0007958 0007958 0007959 0007959 0007960 0007960 0007961 0007961 0007962 0007962 0007963 0007963 0007964 0007964 0007965 0007965 Set Number 122000D 122000D 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A Extraction Analysis Date Date 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/ 22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 AVERAGE: STANDARD DEVIATION: Analyte Found (ue/mL) 0.0762 0.0670 0.0273 0.0284 0.00785 0.00824 0.0480 0.0476 0.0488 0.0494 0.0416 0.0413 0.0192 0.0189 0.0321 0.0334 0.00969 0.00983 0.0158 0.0166 0.0324 0.0198 * Duplicate injection LOQ = 0.01 ng/g for liver and 0.01 ng/mL for serum Centre Analytical Laboratories, Inc. Page 38 of 102 000180 Centre Study No.: 023-041 Table XX. Summary of PFOS in Juvenile Serum Samples at 6.2 ppm a.i. (Test Termination 12 Weeks) Sponsor ID 9548 9548* 9549 9549* 9551 9551* 9552 9552* 9555 9555* 9559 9559* 9561 9561* 9562 9562* 9563 9563* 9564 9564* Centre ID 0007966 0007966 0007967 0007967 0007968 0007968 0007969 0007969 0007970 0007970 0007971 0007971 0007972 0007972 0007973 0007973 0007974 0007974 0007975 0007975 Set Number 122000D 122000D 122000D 122000D 122000D 122000D 122000B 122000B 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D Extraction Analysis Date Date 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/20/00 12/24/00 12/24/00 12/20/00 12/22-23/00 12/20/00 12/20/00 12/20/00 12/20/00 12/22-23/00 12/24/00 12/24/00 12/24/00 12/20/00 12/20/00 12/20/00 12/24/00 12/24/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/20/00 12/24/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 AVERAGE: STANDARD DEVIATION: Analyte Found (pg/mL) 0.137 0.160 0.382 0.390 0.222 0.208 0.0542 0.0535 0.243 0.218 0.161 0.168 0.185 0.171 0.231 0.229 0.259 0.254 0.171 0.173 0.203 0.0838 * Duplicate injection LOQ = 0.01 |ig/g for liver and 0.01 pg/mL for serum Centre Analytical Laboratories, Inc. Page 39 o f 102 C 0 1 . Q4 Centre Study No.: 023-041 Table XXI. Summary of PFOS in Juvenile Serum Samples at 17.6 ppm a.i. (Test Termination 12 Weeks) Sponsor ID 9567 9567* 9570 9570* 9575 9575* 9579 9579* 9580 9580* 9581 9581* 9582 9582* 9583 9583* 9584 9584* 9588 9588* Centre ID 0007976 0007976 0007977 0007977 0007978 0007978 0007979 0007979 0007980 0007980 0007981 0007981 0007982 0007982 0007983 0007983 0007984 0007984 0007985 0007985 Set Number 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D Extraction Analysis Date Date 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/20/00 12/24/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/20/00 12/24/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 AVERAGE: STANDARD DEVIATION: Analyte Found (ug/mL) 0.329 0.355 0.483 0.512 0.241 0.252 0.406 0.424 0.287 0.254 0.295 0.285 0.459 0.473 0.521 0.524 0.553 0.564 0.532 0.509 0.413 0.114 * Duplicate injection LOQ = 0.01 pg/g for liver and 0.01 pg/mL for serum Centre Analytical Laboratories, Inc. Page 40 o f 102 G0 0 1S Centre Study No.: 023-041 Table XXII. Summary of Percent Moistures for Quail Liver Samples Sponsor ID 451 452 453 454 455 456 457 458 460 482 484 486 488 490 9506 9508 9512 9518 9520 9522 9526 9530 9540 9543 9544 9548 9551 9552 9555 Centre ID 0007867 0007868 0007869 0007870 0007871 0007872 0007873 0007874 0007876 0007878 0007880 0007882 0007884 0007886 0007908 0007909 0007910 0007912 0007913 0007914 0007916 0007919 0007923 0007925 0007926 0007927 0007929 0007930 0007931 % Moisture Sponsor ID 66.7 9559 64.4 9561 68.4 9562 65.6 9563 64.1 9564 71.8 9570 59.5 9579 71.2 9584 69.0 9588 55.0 E01-0259-20780 60.6 E01-0259-20781 72.5 E01-0259-20782 61.5 E01-0259-20783 65.1 E01-0259-20784 70.7 E01-0259-20785 72.1 E01-0259-20786 67.4 E01-0259-20787 73.2 E01-0259-20788 73.5 EO1-0259-20789 68.3 EO1-0259-20790 67.9 EO1-0259-20791 70.0 EO1-0259-20792 66.7 EO1-0259-20793 57.1 E01-0259-20794 55.8 E01-0259-20795 59.4 EO1-0259-20796 81.3 EO1-0259-20797 53.5 E01-0259-20798 65.0 E01-0259-20799 Centre ID 0007932 0007933 0007934 0007935 0007936 0007938 0007940 0007945 0007946 0102997 0102998 0102999 0103000 0103001 0103002 0103003 0103004 0103005 0103006 0103007 0103008 0103009 0103010 0103011 0103012 0103013 0103014 0103015 0103016 % Moisture 78.3 80.6 57.8 63.4 34.6 85.2 88.7 59.6 65.2 70.3 57.8 70.6 67.0 67.7 64.5 72.3 67.6 68.0 68.0 69.3 70.9 67.0 65.3 74.5 65.7 71.7 72.8 71.3 72.1 Centre Analytical Laboratories, Inc. Page 41 of 102 0001 .S,,3 Centre Study No.: 023-041 FIGURES Centre Analytical Laboratories, Inc. Page 42 of 102 cool Centre Study N o.: 023-041 Figure 1. Typical Calibration Curve for PFOS 1 ! oo .<0 f<r Ih* L* Concentration, ng/mL ,<M ffoi iO iCN Mr O0 0 0 10 <o CM T" T" M* o o 0 O o oo o T" o o o o> 00 K o oo d dd o oo o oo CO 10 * S}UVK `B JV o o- o ddd o o o o- o CO CM I00 To <0 om; CM o Centre Analytical Laboratories, Inc. Page 43 o f 102 cool Centre Study No.: 023-041 Figure 2. Chromatogram Representing a 0.1 ng/mL standard for PFOS : M ap le Index: I M a p le Type : - C oncentration: Acq. Dete: : Acq. Tiae: QC 120/2.120/000 1 0 :2 7 :1 0 AH Modified: unehinq rietet: Nolee Thmkeld: Area fkieikeld: Mua. teeoehe: RT Window: expected RT: Sep. Width: Sep. Height: Cap. Seek Rede: Cap. Ad). Retie: tap. Vei. Ratio: One Relative RT: Tee 1 l.tl 9.55 1 30.0 4.SI 0.20 0.01 S.00 4.00 3.00 No eee ain l f 1 Int. Type: Retention Tie: Area: Height: Start Tlae: End Tine: Manuel 4.4 ala 1039.0 eounte 2.1fe*002 epe 4.40 aln 4.S9 Bln 200 ; i ISO i 1 100 i uo ; *j 920 i too' j to, 40 4 [z.*.. fry1V 0.9 - yVV^V.-W*. 1.0 1 Time, min Centre Analytical Laboratories, Inc, Page 44 of 102 0 0 0 1 Y2 Centre Study No.: 023-041 Figure 3. Chromatogram Representing a 1.0 ng/mL standard for PFOS ;AACSSaeeaomqqua..pcpallTaDeniataTeeIwnayi:dpcleeox:n:: S112t1a/1:n.214d205/a0:00r0d0AN mi 1100' '|1'1:'i!AEMNMSEEKStEoaTaxxxxuxoonapppppnpidaWe......eihcifAVHHSTSnltiaeTendahdaiaqddodahorljiwk.:.qeeoiaA*Fs:htfhAfah:Tatttha::oaac*:otlcctdoliiloode:xt:::i 3N002Y950t11......o...a00500295a011105000 aaaide ft 1 i 1000.1 000- 7000041: 500 iiAMEMsIenntaatdtaic.qnTe:hTcitnTi:yeapina:eo:T:im: 1M4,11a430n...0u54*.a0100l03acioUnunts 430000,1 210000;'I L 40 Tim*, n ta - Centre Analytical Laboratories, Inc. Page 45 o f 102 Centre Study No.: 023-041 Figure 4. Chromatogram Representing a Reagent Blank for PFOS (Centre ED Reagent Blank A, Set: 122000A) Sample Index; S n ^ U Typo: C o n c o n tta tio n : Acq. onto: Acq. Tima: 5 Rlank 0.000 12/22/00 12:05:41 PM M odifind: Tea unchlnq Factor: 1 Moiao Thzaabold: 1.91 A in Thzoahold: 5.55 Ham. Smootha; 1 RT Mindov: - 30.0 ane Sapeetod RT: 4.51 min Snp. Width: 0.20 Sap. Nalqht: 0.01 Cap. la ik Ratio: 5.00 Cap. M l. Ratio: exp. Vai. Ratio: Uaa RnXatiT RT: 4.00 3.00 Ko f f 1 Jne. Typn: R ntnntion Tiaw: Acna: Knight: S ta rt Tiaw: ' End Tiaw: Manual 4.50 in 2255.1 count! 4.<OQ0; epa 4.35 min 4 . 0 min | 450 J | au ! ! i 250*" 200 150 * loo : 50 0- ' J-M ! M . | 2 I . l u . 7.55 7.71 .*l 0 1.5 F * 1 * 0 * 5 4.0 0 5.5 5.0 5 5 T.O Tim, Min Centre Analytical Laboratories, Inc. Page 46 o f 102 Centre Study N o.: 023-041 Figure 5. Chromatogram Representing Control Quail Serum for PFOS (Centre ID: 0011424 Blank A, Set: 122000A) ' S ta p le loden: ' S ta p le Type: ! C o n cen tratio n : : A cq . Date: j Aeq. T ia e : 10 0l.0o0o0k 1122/:2221:/0000 fN ; Modlfladi ` Ranching Factor; | Molae Thiaahold: I Area Tbcaahold: > Mua. Saootha: . RT NiAdev: Expected RT: j Sap. width: Sep. Haight: Exp. Reek Ratio: Exp. Adj. Ratio: , exp. V e l . Katie: ! Uae Relative RT: ] In c . Typ.1 ! R e te n tio n T ia e : i Acaa: | H e igh t: 1 S ta r t T ia e : ; End T ia e : i Yea 1 l.tl .as i 30.0 4.Si 0.20 0.01 4.00 4.00 3.00 Ho aec auta . Maeeal 4 . SO ala m o . eoaata l.0 3 e * 0 3 epa 4 .3 4 ala 4 . 3 ala 1003 1000-I 00 4.41 Centre Analytical Laboratories, Inc. Page 47 o f 102 0001.39 Centre Study No.: 023-041 Figure 6. Chromatogram Representing Control Quail Liver for PFOS, (Centre ID: 0007870 Blank A, Set: 121900A) . S ta p le Index: | a ea p le Type: C on cen tration : | A cq. Date: Acq. T ie: 2 H ank 0 .0 0 0 12/ 21/00 1 1 : 2 9 :4 4 AN , M odified: Tas : O unching r a c t o t : l 1 N o lee T hreshold: 1 .9 1 } Area T hreshold: 9 .SS 1 Nun. Sm ooths: 1 ! r r window: 3 0 .0 sec ! e x p e c t e d AT: 4 . SI in ; S e p . M ldth: 0 .2 0 1 Sep. M igh t: ! Cxp. Seek A atle: 0 .0 1 .0 0 1 1 exp. A d]. R atio: 4 .0 0 4 ex p . V a l. R atio: 3 .0 0 ! U oe R e l a t i v e AT: No 1 ! Z nt. Type: f R e te n tio n Tiam: j Area: ! H eight: : S ta r t T ie: i End T in e : Manual 4.41 in 4 0 2 . c o ea te l.O le +002 cps 4.31 in 4.01 in i 10 j 100 i . ! 80 1 ! 70, j so ! 1 so ; i 40 ; I *1 20 i 10 ' 0- Time, min Centre Analytical Laboratories, Inc. Page 48 of 102 O W l^ O " Centre Study N o.: 023-041 Figure 7. Chromatogram Representing Control Quail Serum Fortified with 500 ng/mL o f PFOS (Centre ID: 0011424 Spk A, Set: 122000A) ; S aap la Zndx: iM U Typ: ? C oncantzatioa: | Acq. Oat; > Acq. T iaa: 12TM " gc 2.000 12/22/00 11:54:17 ; M odified; lunching ra c to t: Kola T h n s k e ld i Aza T hcaahold: Him . S a n o th a ; AT Window: E x p n e ta d KT: 9p. w idth: Sap. H aight: Exp. 1*<k R a tio : Exp, Adj. R atios tx p . v i. R atios Vaa 1 1.91 .95 l 3 0 .0 4.91 0 .2 0 0.01 5.00 4.00 3.00 HO I n t . Typi R * t n tto n Tims: A xes; H aight: S ta rt Tina: . End T iaa : Manual 4 .4 9 7570.1 counts 1.7H +003 cpa 4.40 oin 4.42 in 0.5 1.0 1.9 2.0 2.9 3.0 3.9 4.0 4.9 9.0 9. 4 0 __ '__________________________ Tim, min ___ Centre Analytical Laboratories, Inc. Page 49 o f 102 Centre Study No.: 023-041 Figure 8. Chromatogram Representing Control Quail Liver Fortified at 10 ppb with PFOS (Centre ID: 0011423 Spk A, Set: 121800A) e u/ti/oe1 (MimtntMi 4.W IliOtiM M j!IIAHMkmDMtM*WMfltTMlinhflc*ahhat*mMl4lAeii i Ah . smhUws : n WMwt , tIiy.HMMiSlTli i Ilf. lq . N it Ittiti 1| tl *ipf.. vM*lJ.. tIUlCl4k*Hl ; Vm M l i u v ST: 10.0 ill 0..0210 t.H (.N l.M ; In c. Tv*' ! N U IU H T im 1' tNiHu ifthii ! S i a n Tu m i ! CM fiM < im.SMu .'O* ej i 1 .0 i . . . 0 10 f l I I 1.1 II 4 4.9 i s 9.9 c.ft 74 70 Centre Analytical Laboratories, Inc. Page SO o f 102 000192 Centre Study No.: 023-041 Figure 9. Chromatogram Representing Juvenile Quail Serum Sample (Centre ID: 0007965, Sponsor ID: 9544, Set: 122000A) Sapl Index: I l u p i . Typ! 1 C oncantratiea: 1 Acq. Dat: j Ae. TU ni 57 Unknown a/a 12/22/00 1 0 :2 0 :1 0 RH i H edlfied: In \ Raschino ra c to r: 1 [ Kola Thraafeeld: 1.01 Ar< T h resh o ld : .55 ; Mi m . S a o o tb a : 1 - RT Hi d w : 30.0 MC 1 C * p ct d KT: 4.01 a ia Sep. N idth: 0.20 i t f . Naiofct: 0.01 1 Kap. N ak R atio: 5.00 ' Cap. A dj. R atio: 1 Kap. V al. R atio: 4.00 9.00 i 1 ! Os R e l a t i v * KT: No 1 - I n t. Typ: : R tnclon T im : A rasi H iqht: S ta tt Tm : Cnd T i*: Manual 4 .5 0 aUn 5149.2 1.1*009 epa 4.40 a ia 4.54 a lo ; 1200 t 1100 ! 1 1000 < MO ; 700 . j 00, 1 500- 400 j 300 200 - 100 ; fl ~ 4.0 Tun, m Centre Analytical Laboratories, Inc, Page SI o f 102 Centre Study No.: 023-041 Figure 10. Chromatogram Representing Juvenile Quail Liver Sample (Centre ID: 0007926, Sponsor ID: 9544, Set: 121800B) n "W r ; 1 l u * l * Index: ! Snapl a Type: C oncentration: | Acq. Oate: Acq. T lee: 59 (tailnoun l/A 13/20/00 -01:33:11 M 1101 1000, | M odified: Ye* lunchin fa c to r: * 1 e lse Threshold: 1.91 Area T hreshold: 9.95 I Him. Sam oths: 1 \ IT M ade*: 90.0 aec Expected IT: 4 .51 Ua ! Sap. W idth: | Sap. H aight: 0.20 0.01 * . Exp- faak K atlo: 1 Bap. Ad), la tlo : Bap. V al. R atio; 5.00 4.00 3.00 j; X 1 Use R e l a t i v e RT: He 1 I n t. Type: ! R etention T ine: j Area: H eight: . S ta rt Tie*: 1 Bud T in e: Manual 4.47 e le 7435. counts 2.0e003 cps 4.31 e in 4.3 ein <000 ! 1M 01 r 44001 ! tjo o .; 1000 100- 000- 4M 1 200- i 0-- 1.47 2.5 3.0 sT Tim*, ml* . 4 .S I 1.5 Centre Analytical Laboratories, Inc. Page 52 o f 102 000194 Centre Study No.: 023-041 APPENDIX A Study Protocol 00P-023-041 (Centre Study No. 023-041) and Amendments and Deviations Centre Analytical Laboratories, Inc. Page S3 o f 102 Centre Study No.: 023-041 r Centre Protocol No. OOP-023-041 STUDY PROTOCOL STUDY TITLE EXTRACTION OF POTASSIUM PERFLUOROOCTANESULFONATE FROM QUAIL SERUM AND QUAIL LIVER FOR ANALYSIS USING HPLC- ' ELECTROSPRAY/MASS SPECTROMETRY . SPONSOR 3M Environmental Technology and Safety Services Building 2-3E-09 PO Box 33331 St. Paul, MN 55133-3331 DATA REQUIREMENTS Analytical Method Requirements TESTING LABORATORY Centre Analytical Laboratories, Inc. (Centre) 3048 Research Drive State College, PA 16801 Phone 814-231-8032 PROTOCOL IDENTIFICATION NUMBER OOP-023-041 Centre Analytical Laboratories, Inc. Centre Analytical Laboratories, Inc. Page 1of 43 Page 54 o f 102 G 0 0 1 i> S Centre Study No.: 023-041 Centre Protocol No. OOP-023-041 Tide: EXTRACTION O F POTASSIUM PERFLUOROOCTANESULFONATE FROM QUAIL SERUM AND QUAIL LIV ER FOR ANALYSIS USING HPLC. . ELECTROSPRAY/MASS SPECTROMETRY ________ ;________ TABLE OF CONTENTS ______________________ _______________ Page TABLE OF CONTENTS...................... ..................................................... ................................ 2 1. PURPOSE i*.3 2. TEST M A TERIALS:..................................................................................................... 3 3. SPONSOR.............................i..........................................................................................4 4. T e s t in g f a c il it y a n d p e r f o r m in g l a b o r a t o r y ................... ;.........4 5. PROPOSED EXPERIMENTAL TIM E-FRAM E................. ................. .................... 4 6. JUSTIFICATION FOR THE SELECTION O F TH E TEST SYSTEM ...................4 7. . SAMPLE PROCESSING. STORAGE AND ID EN TIFICA TIO N ..................;........5 8. ANALYTICAL M ETHOD .. ................................................................................. 5 9. EXPERIMENTAL DESIGN..................... I........................:........ ............................... 10 10. PROTOCOL AMENDMENTS AND DEVIATIONS...................... .'..................... 10 11. RECO RD S................!......................................... ................................................... ......1 1 12. QUALITY ASSURANCE.........!............... .. ................... .......... .'............................ 12 13. DATA AND REPO RT.............. .....................-- ........................................................ 12 14. ARCHIVE STATEMENT.................................................................................... 13 15. REFERENCES____ ................................ ......1 3 16. PROTOCOL APPROVAL................................. .'......................... i............- ................14 APPENDIX: ANALYTICAL M ETHODS......................................... ....................................15 Centre Analytical Laboratories, Inc. Centre Analytical Laboratories, Inc. Page 2 of 43 Page 55 of 102 00019* Centre Study No.: 023-041 r Centn Protocol No. OOP-023-041 Study Title? J EXTRACTION O F POTASSIUM PERFLUOROOCTANESULFONATE FROM QUAIL SERUM AND QUAIL LIVER FOR ANALYSIS USING HPLCELECTROSPRAY/MSS SPECTROM ETRY 1. PURPOSE The purpose of this study is to analyze quail serum samples and quail liver sample! for residues of pofluorooctanesulfonate (PFOS) using methods entitled, "Extraction Of Potassium Perfluorooctanesulfonate Or Other Fluorochemical Compounds From Serum For Analysis Using HPLC-Electrospray/Mass Spectrometry" (3M method number ETS-8-4.1) and "Extraction Of Potassium Perfluorooctanesulfonate Or Other Fluorochemical Compounds From Liver For Analysis Using HPLC-Electrospray/Mass Spectrometry" (3M method number ETS-8-6.0) with the modifications listed in Section 8. The Quality Assurance Unit of Centre Analytical Laboratories, Inc., will audit the study for compliance with EPA TSCA Good Laboratory Practice standards 40 CFR Part 792(1). 2. T E ST M ATERIALS The following analytical standards will be used: Test Material PFOS TCR Number TCR00017-46 . Purity (%) 97.9 Expiration Date 08/31/01 Chemical name and structure of the compound is presented below. PFOS Chemical Name: IUPAC Name: CAS Number Molecular Weight: Perfluorooctanesulfonate 1-Octanesulfonic acid.1,1,2,2,3,3,4,4,5.5,6,6,7.7,8.8,8heptadecafluoro-, potassium salt 2795-39-3 499(CF,,SOT) O II C a F i7S -- O ' II O Note: The neutral molecule and standard form that PFOS (anion) is derived from is perfluorooctanesulfonate potassium salt [C1F17SO3K], molecular weight 538. Centre Analytical Laboratories, Inc. Page 3 of 43 Centre Analytical Laboratories, Inc. Page 56 of 102 000198 Centre Study No.: 023-041 Centre Protocol No. OOP-023-041 A record of test and reference substance receipt, storage conditions, and a record of use will be maintained at Centre Analytical Laboratories, Inc. Forms documenting chain-of-custody and shipping records for tracking of the test substances will be included as part of the raw data package. All standards/test substances and any prepared solutions must be identified with a unique label or number on the container or cross-referenced to the container. HAZARD INFORMATION A current MSDS for the chemical(s) used jn this study will be maintained at the testing facility. 3. SPONSOR 3M Environmental Technology and Safety Services Building 2-3E-09 PO Box 33331 ' SL Paul, MN 55133-3331 STUDY DIRECTOR: Rochelle Robideau TELEPHONE: 651-778-7065 FAX NUMBER: 651-778-6176 - 4. TESTING FACILITY AND PERFORMING LABORATORY Centre Analytical Laboratories, Inc. (Centre) 3048 Research Drive State College, PA 16801 PRINCIPAL INVESTIGATOR: Emily R. Stauffer, Centre TELEPHONE: 814-231-8032 FAX NUMBER: 814-231-1580 5. PROPOSED EXPERIMENTAL TIME-FRAME Experimental Start Date Experimental Termination Date Report Issued Dec. 11,2000 Dec. 15,2000 Dec. 30,2000 . 6. JUSTIFICATION FOR THE SELECTION OF THE TEST SYSTEM ' Quail serum samples arid liver samples collected by Wildlife International, Ltd. will be used as the test systems for this study. ' Quails .represent wild bird populations' and they are an EPA recommended species because they do well in a laboratory environment. Quail habitats include bushy pastures, grassy roadsides, Centre Analytical Laboratories, Inc. i Page 4 of 43 , L I Centre Analytical Laboratories, Inc. Page 57 of 102 G -0 0 19 S * Centre Study No.: 023-041 I Centre Protocol No. OOP-023-041 farmlands! and open woodlands, and they are considered land grazers. The use of these matrices for the study was to detennine if PFOS was deposited in the liver and serum of mating adults that were fed PFOS. A complete description of the test system along with all of the in-life parameters is documented in the sponsor's protocol no. 454/01060Q/QP/SUB454, Project No. 434-104 that is associated with this analytical protocol. 7. SAMPLE PROCESSING, STORAGE AND IDENTIFICATION No processing will be required for the serum samples. Due to the small amount of sample available, the liver samples will not be homogenized prior to extraction; however, they will be homogenized by laying the samples on a flat surface and . mashing them by hand as best as possible. Each sample will be assigned a unique sample identification number at Centre, which will be used for tracking and identification of the samples. The samples will be stored in a temperature-monitored freezer, maintained at < -10* C, except when removed for extraction and analysis as described in the method. The samples will be kept isolated from the test substancetiuring storage. Sample receipt and storage location and conditions during the jmidy will be documented.' All samples and any resulting sample extracts will be identified with a unique label or sample number. Such identification will be either on the container or cross-referenced to the container. 8. ANALYTICAL METHOD The serum samples will be analyzed according to the analytical method titled "Extraction Of Potassium Perfluorooctanesulfonate Or Other Buorochemical Compounds ` From Serum For Analysis Using HPLC-Electrospray/Mass Spectrometry" (3M method'number ETS-8-4.1) and the control liver samples will be analyzed according to the method titled "Extraction Of Potassium Perfluorooctanesulfonate Or. Other.Fluorochemical Compounds Bom Liver For Analysis Using HPLC-Electrospray/Mass Spectrometry" (3M method number ETS-8-6.0). The following modifications will be applied to each method: 1. There will be no surrogate standard used in the extraction procedure. The stock, fortification, and calibration standards will be prepared as follows: I Stock Solution Prepare a stock solution of PFOS at 100 pg/mL by weighing out 10.0 mg of analytical standard (corrected for percent salt and percent purity). Adjust final volume to 100 mL with methanol in a 100-mL volumetric flask. Store this stock solution (in 125-mL LDPE bottles) in a refrigerator at 2*C to 6*C for a maximum period of 6 months from the date of preparation. Centre Analytical Laboratories, Doc. Page 3 of 43 Centre Analytical Laboratories, Inc. Page 58 o f 102 Centre Study No.: 023-041 Cantre Protocol No. 00P-Q23-O41 Fortification Solutions a. 1.0 ue/mL Fortification Solution - Pipette 1.0 mL of the 100 [lf/mT tnrfr solution into a 100 mL volumetric flask. Bring up to volume with methanol. b. 0.1 ue/mL Fortification Solution - Pipette 10.0 mL of the 1.0 pg/ml fortification solution into a 100-mL volumetric flask and bring up to vertumrwtthTBaiufflorr --- c. 0.01 ue/mL Fortification Solution - Pipette 10.0 mL of the 0.1 pg/mL fortification solution into a 100-mL volumetric flask and bring up to volume with methanol Store all fortification standard solutions (in 125-mL LDPE bottles) in a refrigerator at 2C to 6C for a maximum period of 6 months from the date of preparation. Calibration Standards Prepare six LC/MS/MS calibration standards in methanol via dilution of the 0.1 pg/mL and the 0.01 pg/mL fortification solutions. This is a typical example; additional concentrations may be prepared as needed. Initial Cone. (ug/mL) 0.1 0.1 0.1 0.01 0.01 0.01 Volume (mL) 5 2 1 5 2 1 Diluted to (mL) 100 100 100 100 100 100 Final Cone. (ue/mL) 0.005 0.002 0.001 0.0005 0.0002 0.0001 Store all calibration standard solutions (in 125-mL LD PE bottles) in a refrigerator at 2C to 6C for a maximum period of 6 months from the date of preparation. 2. The liver samples will not be processed to make the homogenate described in the method Section 12.2 to 12.12. Due to limited sample available, samples will be mashed on a flat surface by hand prior to extraction. 3. The sample weight for'liver will be 0.50 g ( 0.05) and the sample volume for serum will be 100 pL. The amount of 0.5 M TBA added to the serum sample will be 0.5 mL and the amount of 0.25 M sodium carbonate/sodium bicarbonate buffer added will be 1.0 mL Samples will be placed on a wristaction shaker for - 20 min. at level 10 and then centrifuged for - 15 min @ ' -3000 ipm. The samples will only be filtered with 0.2 pm nylon mesh filter if Centre Analytical Laboratories, Inc. Page 6 of43 Centre Analytical Laboratories, Inc. Page 59 o f 102 0 0 0 2 0 .1 Centre Study No.: 023-041 i Centre Protocol No. OOP-023-041 necessaiy. Samples will be reconstituted in a final volume of 1 mL of methanol for both matrices. 4. The samples will be analyzed under the following conditions: LC/MS/MS System and Operating Conditions (Turbolonspray) Mass Spec: PE SCIEX API 3000 Biomolecular Mass Analyzer Interface: SCIEX Turbolon Spray Liquid Introduction Interface Harvard infusion pump Computer Power Macintosh G3 Software: PE SciexAnalyst 1.1 Windows NT HPLC: Hewlett Packard (HP) Series 1100 HPQuatPump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Columnenesis C (Jones Chromatography), 2.1 mm x 50 mm, 4p Column Temp.: 35 C Injection Vol.: 10 \iL Mobile Phase (A):'2 mM Ammonium Acetate in ASTM type I water Mobile Phase (B): Methanol Flow Rate: 0.3mLimin. T im e 0 1.0 7.0 7.5 11.0 S lA S l Bl 6 0 . .40 0 . 100 0 100 40. 60 40 . 60 It may be necessary to adjust the HPLC gradient in order to optimize instrument performance. Columns with different dimensions (e.g., 2.1 mm x 30 mm) and columns from different manufacturers (Keystone Betasil Cu etc.) can be used, provided equivalent chromatography is Obtained. Ions monitored: I Centre Analytical Laboratories, Inc. Centre Analytical Laboratories, Inc. Page 7 of 43 t I Page 60 o f 102 000202 Centre Study No.: 023-041 Centre Protocol No. OOP-023-041 AoabSfi PFOS i Approximate Mads TrsnaitianManitorwl Retention Time fmo negative 499-99 4.20 On a day-to-day basis, the retention times may vary slightly depending on the batch of mobile phase, etc. Example Tune File Parameters The following values are provided as an example. Actual values may vary from instrument to instrument Also, these values may be changed from time to time in order to optimize for greatest sensitivity. The mass spectrometer is tuned using a 0.5pg/mL PFOS solution, prepared via dilution of the stck solution in methanol. -The solution is infused (using a "T" connector) at 10 pL/min into a 0.2 mL/min stream of mobile phase consisting of 40% methanol and 60% 2 mM ammonium acetate. The analytes are initially tuned for the parent ion and then tuned for the product ion. Once the instrument is tuned, the optimized parameters are saved as a "tune file". This tune file is then used during routine analysis. The tuning procedure may be repeated as necessary to ensure optimal sensitivity. CmtreU IS-Iospray OR-Orifice RNG-Focus Ring QO-Quad 0 Rod Offset IQ1. Inter quad 1 lens ST-Stubbies ROl-Quadl Rod Offset IQ2-Inteiquad2 tens R02-Quad 2 rod offset SI3-Stubbies R03- Quad 3 rod offset DF-CEMDeflection Plate M-Channel Electron Multiplier ' 4000.0 -61.0 - -270.0 - 10.0 93 -15.0 . 9.3 20.0 84.0 100.0 86.0 300.0 2800.0 Oa?flaws ' Nebulizer Gas Curtain Gas Collision Gas' ' TIS Temperature Set 12 13 4 350C Calibration Procedures" a. Inject the same volume (between 10 to 20 pL) of each calibration standard (prepared in MeOH).into the LC/MS/MS. I Centre Analytical Laboratorio, Inc. Centre Analytical Laboratories, Inc. Page 8of 43 ! Page 61 of 102i j 000203 Centre Study No.: 023-041 Centre Protocol No. 00P-023-041 b. Use linear, 1/x weighted standard curves for quantification. TJny standard curves are generated for each set by linear regression using the appropriate software system. Any calibration standards falling outside 30%, based on its calculated concentration, must be excluded from the calibration curve. However, the total number of calibration standards that may be excluded must not exceed 30% of the total number of standards injected. c. The corielation coefficient (r) for calibration curves generated must be 0.9925 (r*0.985). If calibration results fall outside these limits, then appropriate steps should be taken to adjust instrument operation, and the relevant set of samples must be reanalyzed. Sample Analysis Inject the same volume used for the calibration standards (between 10 to 20 pL) of each sample, fortification, control, etc. into the LC/MS/MS. Each sample must be analyzed in duplicate. a. Standards corresponding to at least six concentrations must be included in an analytical set b. Inject an entire set of standards (six) at the beginning of the run and . inject standards interspersed about every 5-10 samples. All sample injections must be bracketed by standard injections. c. Each set of.samples analyzed (not to exceed 25) must include at least one reagent control (extraction solvents oiUy), at least one matrix control, and two matrix control samples fortified at known concentrations and carried through the procedure to verify recovery. d. The concentration of each sample, fortification, control, etc. is determined from' the standard curve based on the peak area of the analyte in all standards injected during a set. The standard responses must bracket responses of the residue found in the sample set -If necessary, dilute the samples and re-analyze to give a response within the standard curve range. e. Fortification recoveries within 80 to 120% are acceptable for fortifications at the LOQ level. Recoveries between 80 to 120% are acceptable for fortifications at levels greater than the LOQ, Failure to meet these criteria requires an investigation of cause and a full reanalysis of the affected samples. f. Samples in which no peaks are detected at the corresponding analyte retention times will be reported as ND (not detected). Samples in which peaks are detected at the corresponding analyte retention times Centre Analytical Laboratories, Inc. Page 9 of 43 Centre Analytical Laboratories, Inc. Page 62 o f 102 000204 Centre Study No.: 023-041 Centre Protocol No. OOP-023-041 i but are less than 3:1 signahnoise will be reported as NQ (not quantifiable). g. Background levels of analyte found in control/blank samples that correspond to values below the LOQ, but are still quantifiable, will be used to correct fortification recoveries. h. If samples are not loaded on the instrument to be analyzed the day they are extracted, samples must be stored refrigerated at approximately . 2C to 6C until analysis and analyzed preferably within a week. 9. EXPERIMENTAL DESIGN Samples obtained by Wildlife International Ltd. have been shipped to Centre Analytical Laboratories; Inc. for analysis. All samples will be analyzed according to methods, "Extraction of Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds From Serum for Analysis Using HPLC-Eiectrospray/Mass Spectrometry' and "Extraction of Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds From Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry" with-the modifications detailed in Section 8. Methods to control bias will include assay, of untreated control samples, fortification of untreated control samples to obtain recovery data, and replicate analysis of fortified samples to provide an indication of reproducibility. . The average recovery and relative standard deviation of the fortified samples will be calculated. Also, the average residue found and standard deviation for each matrix will be calculated. M oisture, determ ination w ill be perform ed On all liv er sam ples according to Centre SOP CAL-10B/11 with the following modifications: 1. The sample weight will be - 0.5 g. 2. The drying time will be -1 2 hours. 10. PROTOCOL AMENDMENTS AND DEVIATIONS Any deviations from the protocol or from the analytical method as provided will be documented and reported promptly to the Study Director. Planned changes to this protocol or to the analytical method will be made in writing as an amendment and approved by the Principal Investigator and the Study Director. Any amendments or deviations will be appended to this protocol and included in the final report 1 Centre Analytical Laboratories. Inc. Page 10 of 43 Centre Analytical Laboratories, Inc. Page 63 of 102 0^0205 Centre Study No.: 023-041 Centn Protocol N a OOP-023-041 Protocol amendments: Planned changes to the approved protocol shall be documented by amendments that clearly describe the change, justification for the change, and impact on the study. Amendments will be signed and by die.Principal Investigator and Study Director. Copies of amendments will be sent to the quality assurance unit. 2. Protocol deviations: Protocol deviations, which ate one time and unplanned deviations from the protocol, shall be documented in the study records, noting the nature of the deviation, potential effect or impact on the study, and collective action if required. Protocol deviations are signed and dated by the Principal Investigator and Study Director and reviewed by QU. 11. RECORDS Records to be maintained include,-but are not limited the following (as appropriate): 1. Sample tracking sheets) 2. Simple receipt records, storage history, and chains of custody 3. History and preparation of standards (stock, fortification, calibration) 4. Description of any modifications to the method 5. Instrument run sheets, bench-sheets or logs 6. Analytical data tables - 7. All chromatographic and instrumental conditions 8. Sample extraction and analysis dates 9. A complete listing of study personnel, signatures and initials 10. Chronological presentation of all study correspondence 11. Any other data necessary for the reconstruction of the study All chromatograms will contain the following: a. Sample identification, date, arrow or other indication of the area of interest, and injection number corresponding to the run. b. Additionally, fortifications will include the fortification level of the analyte. c. Analytical standard chromatograms will additionally: include the concentration (e.g., pg/ml, ngrinL, ppb, ppt, etc.). Each data set will contain infonnation on temperatures,, flow rates, column parameters, gases, instrument parameters, and instrument type, etc. The Centre study number will also be recorded on the first chromatogram of each daily analytical run. Centre Analytical Laboratories, Inc. Centre Analytical Laboratories, Inc. Page 11 of 43 Page 64 o f 102' 00020G entre Study N o.: 023-041 ~~ Cantre Protocol No. OOP-023-041. 12. QUALITY ASSURANCE Centre QA Unit will review the protocol, audit the study conduct and the study documentation (including raw data and final report) to ascertain that all QA/GLP procedures are adhered to. Centre QA Unit will inspect the study at intervals adequate to assure compliance to GLP's, and will report the findings of the audits to the.Principal Investigator, Centre Management, and die Study Director. 13. DATA AND REPORT 1. All raw data and the original sighed protocol-will be maintained in the study file. This data includes the protocol' amendments, protocol deviations, laboratory notebooks, analytical standard solution preparation, sample chain of custody sheets, sample work sheets, chromatograms, calibration curves, and any other appropriate data generated. Raw. data not used will be stored in th study file. The reason for exclusion will be documented. .2. A final report will be issued by Centre, approved and signed by the Study Director and sufficient for submission to EPA. The report contents should include, but not limited to: 1. Objectives and procedures stated in the protocol. 2. Analytical and statistical methods used 3. Test materials identified by name, lot, purity, and other characteristics 4. Name of testing facility and study initiation and completion dates 5. Statement prepared and s ig n e d by the qualify assurance unit 6. Tables containing all applicable data 7. All chromatographic and instrumental conditions S. A complete listing of Centre study personnel Centre will send a copy of the draft report to the Study Director, who will return the report with comments. Centre Analytical will make revisions and finalize the report with the approval of the Study Director. The Centre QA unit will conduct an audit of the final draft report and data files to assure accuracy and GLPcompliance. The final report must be approved by the Study Director prior to signature. A statement of QAU inspections and a statement of GLP compliance will be included in the final repot! Any corrections or additions to the final report diali be in the form of an amendment by the Principal Investigator. The amendment shall clearly identify the part of the .final report that is being corrected and the justification for correction. The amendment shall be signed and dated by the Principal Investigator and the Study Director. Centre Analytical Laboratories, Inc. C entre A nalytical Laboratories, Inc. 12 of 43 Page 65 o f 102 000?,07 Centre Study No.; 023-041 Centre Protocol No. 00P-023-041 REPORT DISTRIBUTION: Original: Study Director Copy: Centre Archives 14. ARCHIVE STATEMENT Study records to be maintained: Records to be maintained for the study include all raw data, observations recorded, during the conduct of the study, documentation, chromatograms, specimen tracking information, and study related correspondence. This includes a description of equipment used during the conduct of the study. All characterization data and any shipping records shall be retained. Document archives: Upon completion of the study, the study records, protocol and amendments, and the final report and amendments shall be retained in the 3M document archives. If it is necessary to substitute a copy for an original record, it will be certified as an exact copy. Centre will retain facility-related originals and a copy of the final report and raw data package. 15. REFERENCES 1 U.S. Environmental Protection Agency. Toxic Substances Control Act (TSCA). . Good Laboratory Practice-Standards. Final Rule, 40 CFR Part 792. Centre Analytical Laboratories, Inc. C entre A nalytical Laboratories, Inc. Page 13 of 43 Page 66 o f 102 Centre Study N o.: 023-041 Centre Protocol N a OOP-023-041 16. PROTOCOL APPROVAL This protocol was audited by the Quality Assurance Unit of Centre Analytical Laboratories, Inc. Quality Assurance Reviewer, Centre Naomi L o d ilo ,h Jb Quality Assurance Auditor Principal Investigator, Centre /.Itile* Date trulyg u tte r Scientis Facility Management, Centre Study Director, 3M ' a A t A * .. Date------------- -- / -A Z - . Date " Centre Analytical Laboratories, Inc. C entre A nalytical L aboratories, Inc. Page 14 of 43 Page 67 o f 102 C entre Study N o.: 023-041 Centre Protocol No. OOP-023-041 . APPENDIX: ANALYTICAL METHODS A. "Extraction of Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds From Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry" B. "Extraction of Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds From liv e r for Analysis Using HPLC-Electrospray/Mass Spectrometry" i Centre Analytical Laboratories, Inc. C entre A nalytical Laboratories, Inc. Page 15 o f 43 I Page 68 o f 102 best copy a v a i i a b l e / ' \ Centre Study N o.: 023-041 " Centre ProtocDtN<r00P-Q23-04t.... ........... { LP t o v n w n fTf.taTlUff U * other fluoroehem icalcompounds from senna. A p p lica b le cum poum U: Fluorochem ical jurfactw ts nr other fluorwatod M r a p o o n d i' ' lU bbit, rat, bovine, m onfay, end human actum dr other fla id i m >V-tj n irrf^ ' O: ' , ..Wni(V9j ' ` M x - i . siit-u ' h p 1r f 14 ' Centre Analytical Laboratories, {pc. . C entre A nalytical L aboratories, Inc. Page 16 o*43 Page 69 o f 102 O .'J A JP ,,4,- .. ..'M BEST COPY AVAILABLE Centre Study No.: 023-041 Centre Protocol 3.D ~^V- /.-. : ' ' 3.1 PFOS:poflMREtiDesu^StE^ffiioaofpotaninanit) C^FSO]* '* '/ " . " V. . 3 3 P F O S A ; p e rf la o r o o c te n e n i l f c n m n n i d e c j F 1TS O jN H , * s - 3j '. ' . , - '' -'- iL-.'ch -V ?;:a ' 0 3 .7 Surrogate a f a * 1H- 1H- 2H- 2Hperifact o t t t t ne a d f t n b t d - , \ * 3 * . / ' j .#* y ; # ' '** *^ * : - ifl Wakmm AMicumow ,;;- Health andjairtr wriagi : i - ' .. V . . .V 4.1.1 Vortex m ixer, V W R , Vortex Genie 2 t l J C e n tria te , M istral 1000 or IE C * .1 J Shaker, Ebabach o r V W R . - Centre Analytical Laboratories, Inc. C entre A nalytical L aboratories, Inc. Page 17 of 43 Page 70 o f 102 b e s t c o p y available Centre Study N o.: 023-041 Ccntrc-PTWacol-Nor-OOP-023-041- ; 3 2 * ' -i ` .7.4 ` .Centnfii|c ' 7.7 i \ ; 7J ' Oxftnd t.10,0mL 7*9 Syiinja,cqiit>le< asairarniiJ |tL to 50 jiL'^v :.>' .7.10 . G ra d ia iM ^ p e tia ^ ^ ^ i'ift v.vV 7.U Sygny fflte^`ayio^O.2 iunj25 .- t.13 W . f 7.14 Crimp cap sutoviab tad dps rt .z . . . A . . . j s i ( / . 4 . i l , _ . . . . >. : : v. iV^iK ' V. '*.. -.4'-^ ' !^ N f * : . . *. v j * I ^ y v y s x .; .,; .'\C1 ;' <s ; ' N o te: P rio r la w ing glsow arenod bottles, rinse 3 tim ^ jK n s in ^ D o ltn d 3 ta n a w ith O ; ; 1 M illL Q TM wster.' Rm syringes* m inim um o M tim a ^ ttm c tlu n o L 3 rinses fiom 3 . .' " g an te : * ' ' :' M Sodium carinoate^Na^COj; J.T .B a ite r w equrvaleot ' : *-6 M etb yW -B uw i E t t a ; O n a is o h ; g std lttiU e d oc H P L C grade . * . . /.i :; . . i : . h , `y .;.' . ^ ! j;>T 8.7 M ethanol, Om tiohr, |iu> disdlled or H P L C grade 8.8 Scramorblood,to m Ownsupplier ' M Flaorocfcemlcalstandards o W .1 P FO S (3M Specialty Chem ical D iv isio n ), m olecular weight -5 3 * * 2 P F Q S P M Specialty Chem iad D iv isio o L m oteculsr w eijh t - 499 .^ 8IS+4.1 tm cttaccrrrroossttaaiisrai .'.r. V. . PaploTM ^^S S F Centra Analytical Laboretones, Inc. Page 18 o f 43 C entre A nalytical L aboratories, Inc. Page 71 o f 102 0 0 0 2 .'..3 BEST COPY AVAILABLE ,Cntre Study No.: 023-041 CeWPrexCol Na-OQMWHi- - '41^*1*' ^1000 Sol#heSXeC^nMMnii^^^^p ^ mqmrnm -^r^ ~ |OTMMWIHIUI 4 > 1 1 K aigcbc b ottle.-;y -,> - \ . y : t tv^ !^ O B )^ i lONNtH'lia;ibas 10 n o ' r^ A N N t O H i lS i^ S t o * 100 m Lvot netc flask and dOnte to vohnne n . - to .3 03 m A : V * . . -"i o fT B A in to ; 1 L yo Im m S c con 'n g 300 m L M fflM ffim tto r.A d ju stte dH I ' ` vltOJ wr r inj jj ^ir o.i^, ti^* \^ to4mW ^k(M10NNtCW(WMe_TdTd8in* i*t*h**eWUjtPirLJOoff -.: .N tO H , add slo w ly because tlft rig c h jn p abrepfly). .D B tte tp vohnne w ith r v ... .*: . . v V ' . l f l l l i ^ 9 ' ' S k i * f a ^ S W v M . .^ v - v . . V ';? .I 0 J J T E X equirei ic h ^ ^ o r t ^ ff i& lo 'a o iu t e 'jiH - f o A d h u t W " \ :.,f..y .n e e d e d u i^ 8.1 (L4 f l^ t Vroitimw triwu te/mdmiH lwuran n ite ti ffifM fVt t `.` .' O. .;.whw w w w u n o w w w w * u tuumihw * '-.Q " .water. Store a 1 LNUgenbQte. :v..' v r^ : .; 1*tl Standards prtprtIoi.<';: " O:;... '. ;.v^..'ri ' ,* .1 U ' Prpm PFOS ststadiodsfcr tha standardcutW "j? r . * J 1 J P re p a ra other Oucuwdeiical stecdardt,as >ppnipriaM..,, 'fluorechcoical standards no aceptable (forexample;one O Sf. 'olution'conuining 1.00 ppm P F O S . 1.02 ppm P F O S A . ppm P#q s a C ^ : . I .I O ^ M S E - O H .) . . . a LS - llJ - W e ig h approxim ately 100 m g o f P FO S into 100 r h m e tiic fltn i n d ttB d ^- \ . *"' \ i , . V a 8.11^ B ring to vohim e w ith n ih in o !fb r i <tockstifldrd o f ^ ipreodnudy 1000 : 6*g/mL). ; ' " J - J ' ' .:.:','V:: <114 D ilute Ihe stock sohitioa w ith mcthxaol fo r iw o fi n g tix iiia rd 1 ohition o f " ^ p to x iffiite ly S O p p o . 1.*.. ''. *-11-6 D ihite w orking standard 1 w ith methanol fc r a w orking itvidard 2 solution o f / approx. 5.0 ppm . ; . m ii i - ' iV*. . .s * . . 1-. f .T y .- .o . . Centre Analytical Laboratories, Inc. Centre Analytical Laboratories, Inc. Page 19 of 43 Page 72 of 102 0 0 0 2 3 .4 BEST COPY AVAILABLE Centre Study No.: 023-041 - Centre Protoeel-NorOGP-023-041--------- :rn . I0.2J P re p m 'M in k l^ m ilr pike aad a d m is''.,. ,A lltel todiff^f tte conteol:.... cu rv e .' * ' Centre Analyticallaboratories, Inc. Centre Analytical Laboratories, Inc. Page 20 of 43 Page 73 o f 102 BEST COPY AVAILABLE Centre.StudyNo.: 023-041 'CentreProtocol No. 00P-O23-G444--- ( ww a ire w r me cmw a mo u w w w .% ' . . t lJ Extract ik e d n u tr ii tenitorii M o w in g 1 2 .6 -lX 16`bth 5 method. U se then- to n e h m itili i m do t^em a qpeetromete. ^ ^ Centn Analytical.Laboratories, Inc. Centre Analytical Laboratories, Inc. .:. ' ! *** m .-. '. . Page 21 of 43 Page 74 of 102 000216 eJim rn BEST COPY AVAILABLE- Centre Study No.: 023-041 'CentreProtocol No-fl0P-23041-r- C; V. 4*. ;*.**. TJV > A p prorim ata'ap O d ag'am aaott fo r a ta o d ard aaad ap lke i .i, H ity? ? ' y i l U rfi r i'B L 'f i it ' -W oddng stio d a n i .f,; w' ^ ro ro x . co n cV ' ^ *> : l -,'-isi/w , < m 'A H * ^ ,fin * l a c .o f analyte ht m abixY- ":*'? B la n k -t7 -, *?4V-i k i i ' 0 JO 0 ppm l.tv. *' .- /lO K V * r - . 0.005 ppm -`t : fflA O d iO O p p m ? -^ .v.20-:&\ - r 0.010 ppm i.- *`' ' ' S lt / 5 3 .0 0 ppm ` C - -i: l ' -i 3 V : . 0 0 25 p p m .; v *>^s.C3D ppm *sr\ 10 .W; : >:0 0 3 0 ppm :i ; - : J" >4-^jS009BPa r v ;^ 1..: .;20'> 3.i` -* -' .0.100 ppm i r *.:><f>'50.0ppnu.v'>- .- *. 3 0X50 ppm - ' 30.0 w in A . * 10 i . .- ` OJOOppm JO .O p p m * ' -. . 3 0 .0 m JSt*~ V ; IS ' 20- ,*. 0.750 ppm " - 1.00 ppm . 12.0 PRQr^.f||- Jet's: "/.vC-iVi;' 12.1 ' SB * j " * : ', v - . .* "3 thiw r* ---5---1-ta--a--p--m-- p--an-o-r--m--- lukewarm \\~ il . ' w atobatb.' o s p d V1 2 J V o tta m__ix.6. r. _I 5__ja_c_o_nd_a_,th.in-Ji^wJ T O mL'<B4. ip o th e r appropnaic volum e to i' l j m L :' Y ' * 1X3 p_ol^ypropylen*eSc.e.;aitr.i*fa,getnbcL - P ura tunned la m p l to ft e e a lter o c t r t c ^ j m ^ . n t I-'-' Y re m o v e d :W T :;" . ; v a r i th e in itiiil vohaaiw t the 12 ^ . L a b e lihe'tibe w ith rtS^ ic5janI^ /2^ ltD.` * ^ ^ j in it li. f i e i i j ' ' 8-'?.'.'? " . . w o d a h e d fb r d o a ioe n tm itlie r e a M ia in ja i^ -^ '^ ^ .- ^ '' ^ -^ 1Z.6 Spike a ll aam plci. in clud ing blankaandatandanla.ready fo r xw cS N rith wmap j , "''- '' _ wxVtr; .'A** ".'- /T .- -----.-7 >Sjp>fwlceweacyh ml uaituriux wwmithh^tuhibe aa|p^MpruoypirMiaWte amuoMuinwtwo tf iithaaudmarudaa* wde*a*gg*nWbcPd4jnH^,Anlvj LfOo cf T laf llCiV' "'. M 11 inn tHhatMt I Tctliomdt . f<rjyf HthwM'eilliiKbwiVrilnWH ' cBnMrW MmimInmJA -^'i' AAIml HpmnplirmW Mmh my i t^iai^j ^j j^l ^J j ^' ^ -t'".' ' -- -, . .wwtinuilrigwiuii V- ' Vortex m ix the standard curve am ple*, m atrix spike samplea, and c o n tm u m T ^ n A W i ' -!: 2 fci.w 1X 10 T o a c h a m p le, add 1 m L O S M 1 B A 2 4 2 m L o f 0 2 S M sodium tarbonate/aodhim ' bicarbonate buffer. .' -, 'V i* ..- '::,* '' Nt '<:& r!? rb !'*7 ^ 1X11 U a b j m O xford Dispenser, add 1 m L m tyW art-biyl e te r. **"' 1X 12 Cap each a m p le and put on the abater at a aettm t o f 300 rpm , b r 20 m m utea.''/ . o 1X13 Cemrift|efi)(20to23mmiitaataaettiiof33Q0ipm,, orimlillayenaRwdl *eP*nteL. -` :. ; *'-' '/V ; B T t A J I f t / " : - 1! * 4.L* ^ '. > ' -- - C e n tre A n a ly t ic a l L a b o ra to ric a , Joe. Page 22 o f 43 Centre Analytical Laboratories, Inc. Page 75 of 102 G 0 0 A 7 BEST CO PY AVAILABLE Centre Study No.: 023-041 CentreProtocol Nor00P-Q23-041- V.:V. r^adW M lA P'Z unn^oo meahfilterto 3.ceivraie andtnctfcx tbssu sle ta thi. - ^cboB ditejand lyd(s) perfarmliiji theed racd o iX ^: i^-zi -.Ctpsaa stefactncti st roomTmpaato.orti proxmai^y 4*CuntilicalvBe > l 13.0 DATAAf,A1;VsA?ni( _____ . J3-1 : :'.% # . . .....:. v. - ' ,134JC ^aiIite<^'concoB TO 0M '(rfPFO S,<rotbcr^B c^D urD chem icaLrn '*'. ;^C^lfc^bjiiT&iodfifc'?tfBraS1hIl^a^liaoE A-* **. -' ibL o f flmdsn! e r n b i t m ^ f f c tn d i n l (ufm l *" *_i I I4.1-1 R 2 .1 *j***ttj *?, " y ,y l? T S " t ; R e fe to D L report "Tjugenti B and C y*i*hwoftmtBiypmlBtiop ,, 14JJ MatrixntDceandmamaspikedopbcatesampiatodctemincaixur^i(jv :' . :. . .V^'predsmiofUssOEirnrtinu^i^^' V-;.;- : --` *** A "' ' -:-K; % & ` M- M3 Refg to cctiocU ofETS^-5.1 formethod pcrfbniuncecritai. ' .-". l . ~ - ' : RS'- \ ' "*r * *'"*: "*.:'*. ' .'*; v .i' Ilfl f OLLPnonRmvumowawpWasMMahaCIMEWT--- ' '' ' '' . D 12J hSijguhapBfeTwUacorbtadinbepa,oa&ndiunsebdiogllansisrpdicpoetateiawiKilt*rebfldaiisupiobsbalsionfborortkwenasgtleasbsconrotaaiendaiin ' . loeabi intbeJaboratory. Centre Analytical laboratories, Inc.. Centre Analytical Laboratories, Inc. Page 23 of 43 Page 76 o f 102 0 0 0 E .-..8 BEST COPY a v a i l a b l e ." Centre Study No.: 023-041 - T- : ------- ------- -- -------------------------------GeotrePrococol No.-fl0P-023-()44-- v ' vv y * A ttylTO ffT ifu C t u b n t m standard concentration w ocaneet ; . IW- or OtberFhdd Erlneti forFlumochemie*li vibe HPIX-EtectoipppAtoSirwM/!!,i - t >. . i . 12J AmcntD D ocPM Pfry-- '_ " --------- -------------L..: - ~ 7 R evirio n .m ba r Retiti ..; >: 1 la 8 a fstB e m # v ::; '>'/ w . ;.r -..- .4i--pDnii^e 1 . ." Sectiem 1241 d u n g e d to m elodeu m p k m a g e ttroom temperature. - 04/02/99 y i_ Section 1Z13 Added the shelter ip e e d T ^ r . X . . `-"'V ^ : Section 1247 F im i votan e is 1.0 m L ; not e d jio t jb rim tiriw h im e s 1 r 3 :: . sra+-u :' ' -' V'Kv 'hlftL,lt" .,|n? y y*?1? TV.'.\ l.. V: > %' C e n t A n a ly tic a l L a b o ra to rie s, In e. Centre Analytical Laboratories, Ine. r. H ftfftV i' . '' Page 24 o f 43 Page 77 of 102 BEST COPY AVAILABLE Centre Study No.: 023-041 -Centre ProtocoFNor0QIM?3-044-- '<*Mant -*<-s- -j; >&* *" --- v anilv h 'MM V.'i.'.:.' --1i-., * SiS!5h? f f tjy *& 'PtfcSfffladtAialyit ^ ' 1 W | i s S S T pjW f V' *% .y -' "tT" Centre Analytical Laboratories, Inc. Centre Analytical Laboratories, Inc. Page 25 of 43 Page 78 o f 102 .? v BEST COPY AVAILABLE C: Centre Study No.: 023-041 Centre Protocol No.O0P-O23-04- M D L ij LO .Q .- IJh a w C a U n ttte a J U a je ( L U D ... ;6 p b > | (PPb)' /*" <" ` r*Un" * * " *4 f o r p n p ir t B t t h a fS tU K la n i C abra on C a rr O j & S i > ,.? !& r g O S C iJ ir r i -i 1.74 v " I 3 ? 3 iig b X 1 0 0 0 p p b 'i!. ^ '- ....v - .^ ... . . , : F E Q S A X - b V 1-31*. 4.79 Jp p b -M O O O p p b -v " . . . . , " t P O S A A 3 - 3.46.V 2 0 J ? 5 m>b.-1000ppb ... .......... i . v lM i -403 P F O S E A '^ 'i v m * 3 6 J-. 19.2` >UL2;. J p p b r lO O O p p b 'i ! p p b -1 0 0 0 p p b xw 'i-. ; v .. i p p b - 1 0 0 0 p p b C! v . *.. 1 . . . . . : a-- .' 'y-, : J-: I _ fcfcnhf fafailMlM. c ;`V -"i V ?-" *\.\L . ;V :*- ' \ . * *'rf . O "v,<: V, i ' fJO d a ta tB:MDL/LOQSmmamj ' T O M .I ,| . H taiio fit " &t e A i r f i M ?*.: ; S7; '* f'* - \_. v..Af.r{a , v?<ySc/1->.'; -r-.." f : ? - ;aS s*3J:T :r Centre Analytical Laboratories. Inc. Page 26 of43 Centre Analytical Laboratories, Inc. Page 79 o f 102 BEST COPY AVAILABLE !' Centre Study No.: 023-041 r - v . Prepmdrm*- 7 LCRfttxa~ *% Roxivoy T p oe ^ r Rabbit Senin ^ of i d S .**c a r ;v Vi B n a o 'y ' V . * .'r* " (BlAnl.)' - .-..<'rovisiit.-ic4K-_Pfn;* -^yk. . :'t4j*.h! L~j^t -:K Y s i i-.'mr - *,. '>`05-106 *v:. :'i4J 4-0JD *> .k -] ; iT f c jli;.;- S.*M** - li1*i/t nr.v**V " -5`*"; . y *. > m . ' "JVuvJ.-V .* *' Prpertdtini' .LGRJfaoi^ KSUaney -.RSD;;,r RabbitSerum R*njc ; ' *r*' .<V :(ppb) ffaiy" . -V.' `. `.y Tr` * -v/.\ **,-*S; FuIlRanp.. / n-Vo; : 4'5..0.14VJ.-"*fc. ;4 *. \>.*'**a-;*?.;*..-- LowCurie ?W * * *4*5'"'v* ffilhcurw -- 4J-976 Xi MC . . .'V ' ; osM-r i * Jar -*****: ,.<*v. r' . v v ,a *.#. , Vri**.. *- j.t,fMi~2- rfc->v . .4;iWM4Jir |psPreptred naje LCR,from A% W a y rfkRSD Rabbit Soum .o fre a h rd i ' `/ ' f i ? ; " . ! CPI*) (|ftnL) .?:. (niteL) :;:r,,rv'^,n.>N FunSrege ' ! O lM I-m ; .***7*3 ?m ;? : ti - u i ;: 4.i i .j^ Low C a r V '^ r m k High OETC' r.w A jW 'v > $P *P . .* * MC . . . >ftS" 74 ; 4 .4 O . A m e ta m B: MDl/LOQ larD on y-k< `; "SX Centre Analytical Laboratories Inc. Centre Analytical Laboratories, Inc. >\v 'V'il. , P*IU iil4 Page 27 of 43 Page 80 of 102 BEST COPY AVAILABLE Centre Study No.: 023-041 f ty 3 S W W S jL C R & o m * X K ic o v a y U M jS m n ^ o fsta n M r S .' i W / ' ' t '. T i >.} r & L ' # p 9j V f W `X S sM S 1P P -F S -. '\ > i i v :; ! - *; ?. 77: 11 . ; 7; 1 L w S j .' .: *..`./[.y{*''*/t- . V 7; l 0 7 .:.- iu -iu ^ V .* V / } i i t ,.; $?*/ * :W J * 'iu -u ':.: - j . !; C o m o M A F Q S E " E 5l O v * ! errV S V -'^ .-*'/ V S * i ; 4 ; L C R f t U a' K K c c o t a y * ; . K i U n t S c r a n A * o T i i a S S f f ^ ' ^ ' c o r v B *7 .* / v * * i i ..; ' v I U m b j . * ' .*& * FuU R in g V ~ ;* ? N & : ' :^ i S '* 'i J -! . ` > 4 . 10* . ' J \ * . M u \ : # ' L ow C vr* g g t a ^ s . i ' f 'V :vr>Y* II ' - ,i. <i V 3: . 0 H igh c a r r e '-' m u ' : . - . M C .. 7 ^ O O T -n ^ i j w i .1 J ^ 8* .Frepnvdmf LCR4 ; .%Reey*ryv, w'-XJSD R*W>itSturo .VofrtiadardiTf R in g t' fa*) C*^),' . 4 fa * ):'$ -Jir ,k* % Hna/mL) ? FallHange , /aa*fw ;-. VggrUK . -. -**.-. . ; ' ' LowCurr';' y * h - r i '0 . -vioo-i m ;; Hi|)>cum'r:i ; v i '-ih !i, m - m ' ii-iti ; ' ."iwiT j x ": ^ ` j i n i i.- : 9 M - m ' :..7-U. '4.77-17 O Centre Analytical laboratories, Inc. Centre Analytical Laboratories, Inc, Page 28 of 43 Page 81 o f 102 Centre Study N o.: 023-041 -eo6e-Preoeol.No4X)Bd023d041___ F03 ,, Stdcooe }6*Tr. nrosiv. SidconelTSSId73 mosca ...MS. Sdcode ~' Mese' '.Uf.AI ,--. Al " .A art'J.ltaltil :0 OJSM 0.300: 100. 5X05X0; son . 30.01 . 30.0' 30j0 'v'"flftnL'i. (WL " j* L * mi, V. 0307 0332.9 *0301 ` 0321 0301 0.010 : ~ 1.01i 030? 03329 p3"3Ji\ .1.0321 k 0301 . . 5X7r*. 332 37 332 S3*. 332 30.1 .333. a rm .! rm s 'vww* TSEH "33 -J\531 ' 3*fai*. .- Sil . 331 . 161 :3o.i,. 0320 ~~1323 " .0303 , 1310 .0310 1315 : 6.66o - 7- 1.023.. 0.003.... 1310 30.1 . SW 30.1 333 . S33 - 333 sar*J .,311 y. 6.616 1313 . 3Ui4l lAjLi- 0315 i- .1320 V -30.1 i- i 0.020 . -1323 r i* ., , ;* t u . tu * -J*jfa^S2i^nUicw M * 4J3 ' 1X0t . 12*v* fe4J*V >- int --I2rU^ -- *J T 211 : ' 4*3 " 03 . 16 " 241 ..-*jui":. 493 7M .S444 'T' w .... ~ W ~ - I*t4 52.4 .. '104..' M3 - '.wm ion TSV .2 4 3 . rrw ..: T"OTv 'i.-iar: *.>494 , *.fW - ...**r-- r. S i"' v6j4 s 'Til . z-wrr ...232' . V.5W01 4v " MS'" iureri *100 ~ w 211 *I ! 3U ' j Fttalantf iri |.,mUs ra -- 3,2 1 ' g " 11 1 ?-V7` r x i *1 v* . * . :; *.. > # -*. A ~ '. Vv'.V'.. rX' 1 - 1 v. VtBdattdraa|4i-iwiM(orcrntriMoM'V^' T"'' "'V tv,;TV . t*^n.oasiu lonxoLix.ijfl. 1.- rfosAA ,'?r.irtraonsatouH..i 4prLest4*^'~-..i^Ts r5aryu.?jlgs, i s . .... Lf *>___---- -- r ---------------------- ttu. ' . i Centre Analytical Laboratories. Lie. C entre A nalytical L aboratories, Inc. Page 29 of 43 Page 82 o f 102 BEST COPY AVAILABLE Centre Study No.: 023-041 Centre Protocol-No. 0GP-O23-O44-- other flu o ro cb a n icil compoends irom 'Uver.'r Centr Analytical Laboratories. Inc. Centre Analytical Laboratories, Inc. Page 30 of 43 i Page 83 of 102! 1 )0 2 2 S BEST COPY AVAILABLE r Centre Study No.: 023-041 ~j-Protoeal-No.-0GP-Q23O4J- .3.1 PFO S-.pe 34 (anion o fp o U ^ th im n lQ C / n S O ] ' :A :\v w s -V ' , 3 ^ O S ^ p t r i l u o r o o c t i a e W ^ ^ ^ ^ (elfayi)ceMe ^ ,,S Q N ( C H H J C B ,C O , v il. 3.4 .E lF O S E -O H :2 (N ^ fty lp S ib n io ^ m ^ n lfo M im d o ) ^ ^ a lc o h o l*-' -' '' , '3 3 P F O S E A : perfluoroctae so i& n yl e tfiy ffi^ c n S O N fC B ^ C H J H , AP WW aAwk nm^ AwWPCb Aaimoww^p _-_"_' x__ 1 ;< 4 H ealth and Safety W arn in gs: ` ' '. w f. . L. 3 4 T h m We no iM erferencs known at this tim e. :- APlouwMPfT " ' A t The'fcDow ingequipm ent ij'u ie d w hile perfonning t o m th o i Equivalent t acceptable. ":'= " V '' 'T -* . . U l IH tra-T u ira T O G ritx ia for (rinding trveraam pks ' ; ..V 'J ' o 1 4 Vortex m ixer, V W R , Vortex Genie 2 . .'< 4 .3 Centri& ge, M istral 1000 o r DEC ' I .< 4.4 Shaker, Eberinch or V W R . r " i -V- .. ns i * Exaaedea ofPFOS fra m U w ;""* , Pate2<414 Centre Analytical Laboratories, Inc. Page 31 of 43 Centre Analytical Laboratories, Inc. Page 84 o f 102 BEST Centre Study Np.: 023-041 -Ctmrt Praterrol Nn flnpjm f!11 7.14 Syringe l tc n , aylon , Q j (im , ! 7.15 T i m e r ...i 7.16 C rim p cap autoviala nd c ip r ' 7.17 C rim p e n ' " - "y. / . O .. ^ N o te: P rio r to esiag glassware ad boules, r in 3 1 Sv.W *yriganaimPPi % \ UCBfMisT;>n>itM^ : in g h a M l n a 3 time* w ith m m -' 1 *" ',`3 im sesftom 3 separate ^ L -f* . o * 7 D ry ice from applier *10 F ln o ro th e m la l standards - v ,. ' *.10.1 P FO S (3M Specialty Chem ical D ivisio n ), m olocal*r weight - 53S Centre Analytical Laboratories, Inc. Centre Analytical Laboratories, Inc. Page 32 of 43 Page 85 o f 102 J f ' BEST COPY AVAILABLE ViV f K -X'rs, > -v. &; Centre Study No.: 023-041 Centre Protocol NorOOP-023-04-1 tn.30.5 Mteteto ay tS S M a mL? . ^ .if X B A into 1 L v d h ra d & c tm ^ iS ij_ J 0 0 water: A i^ u t to E 10 u jin| ' i p p r a d m i t d y m L o f ^ l O N N R fW n le 'a M n j tb e lts tm L o w w x re p a c uuwa iiuorocarauM M m iw uioti -- >yy*wpM8. m w uw KDoaeQT .** .. j : ^ ilno roehem ica!jtstoait!s a n acceptable (tor example, o o e m a t m f iS ^ r ^ V . '^ s o lu tio n conCuninj 1.00 ppm P F O S , 1.02 ppm P F O S A , 0 J8 7 ppm F F O s X a - i L i . .> '^ y T ' JLm*L I U W c i^ approximately i.O O n ig o fP F O S into a lO O m LypInaetxicflaalt and reco rd * i^ 'th e a jm ia la rd g h t.V :~ . ' v. U 2 A B ring to voloroew ithm etbsnpl t o r t stock it^ idard o f approximately 1000 p p s i . -1 2 5 D ilute the ito ck solution w ith m ethanol tor a w o ttin g Jtanrtnd 1 solm ion o f f.H approximately iO p p ra . . e- . .[ ; Paie 4 or 14 ytical Laboratories, Inc. Centre Analytical Laboratories, Inc. Page 33 of 43 Page 86 o f 102 BEST COPY AVAILABLE Centre Study No.: 023-041 Q m tre1,rotaarfN a-aO FM )23*04i-- O c Centre Analytical Laboratories, Inc. Centre Analytical Laboratories, Inc. Page 34 of 43' Page 87 of 102 000229 Centre Study No.: 023-041 -Gentle ProtocolNd-OOP-023-044------ * . . . i muaiKpuU) ut ^neinjLOUgU^ - -y . . I I J .7 ; T ypically m e t standard tnM BW c a im ^ t in g ainorata t e j a T r i ^ 'i :.- : t6e end o fttia taction,'to ^ 'm < l^ ^ g ^ iandrd e n rm ,'f ir 'total o f ' ,, eighteen aanpfea, two niai* b ia i^ 'V K p in e !l^ 7 -V '^ k ?." V.? , : C B 4 4 A Centre Analytical Laboratories. Inc. Centre Analytical Laboratories, Inc. '? , T f t o f u .. .. r.v *\ s :* Page 35 of 43 Page 88 o f 102 BEST COPY AVAILABLE Centre Study No.: 023-41 -- -------Centre-Protocol Na-O0P-O2J-O4-l- A pproxim ate S p fld n i m o n n ti fo r C a lib ra tio n S ta a d a ris * W rid n jS a n d u d , I - I iii c o ^ y a > : * f l s o ^ ;s ;V ' V u l *v:-;sy * V} l \ v S > ",V . A p p ra x .fim lc e n e .o f ;f r T P F S in 'W ' :> iT Blank `P i-?y..-*. v i v V v v v .'-j 0.005 p m ,-i v" ^ O J O b h Sv ^ : . 4 r? Y .'.V 0.010 ppm C . 10 ' 0.025 ppm . . - 2 0 . , . . .' 0.050 ppm " - o M t e r * *40 -i* 'y :**i 0.100 ppm ; ' 5.0 ppm ;I f;. A I 10 ? -#20 V 0.250 ppm ` . 0.560 ppm . !w 1 f : - 5.0 p p m '-` W - ^ 30 -<. 0.750 ppm - - -- r 7 : s k - " i'V" 1.00 ppm : J 1 2 .0 'P tto m iim ; X U Obtain ftw en liv e rtm fk L * V.t ^ - , V ` .tjv ,,^w v .;s *'poftinedcdddy,oot'aOowfegthsHvctadumC *' ' . *V> . -. f n*v**r ."e.vV. v*" ! i o f 0 procedure is b a t .'2 2 J W eigh the taum le directly into a tared p h itic m p u le 'v u lr^ . . 1 2 . 4 R e w r i the liv e r weight in the ilu d y notebook.- V* aY - r # . . ' ... R rtam unm edH vtrportion to f r e e z e r . . t . ' `VWJj Add 3 mLeo t v t t a tn trap alcv iiL ~ j ' -.'V ~ \ ; , 12.10 15Cap the in ^ e tad v o t e Ihr lecondL Label tlx aanqmlevial wiA the tody iinaiber, w eighs fiver ID , date and a ia ly ft initials.' .. O c -f. . v. t' Centre Analytical Laboratories, Inc. Page 36 of 43 Centre Analytical Laboratories, Inc, Page 89 o f 102 002 b e s t c o p y available Centre StjidyNo.: 023-041 ~Oenbe!Prctocol-ffor06P>d&-Q41--' C 443L M a t T a p ilc a i n i m k ix t p k a ^ U o t e a m p le & i fci C T 3 .7 r' ' M A S Cootmoing a ib n tio a y ^ c a tio a s a in p le s to dctenamw (be . '; o ffte in itia la E b n tio o q tn e .\^ J j v w ' & * $ * !: ? .jj = m t r m : .. -i '' ' '" ' 13.0 Poliutv^ ?g r ^ w w p W A ^M A W A t^pff l ' - -v " v 1* * 1 e ____ I ______ _ . . . j ___ _____ M _______ o Centre Analytical Laboratories, Inc. Page 37 of 43 Centre Analytical Laboratories, Inc. Page 90 o f lo i l i S T COPY AVAILABLE r Centre Study No.: 023-041 -Genut. Piutucul NorOBP-033 04j -------: V'::' -12is2*5:.V< rcobctbejS '* '? & & * * * * & $ : . 'V f ?"'' aUbndoD at p H 10. I fnot, *4iot ccontingly. : .'._ a n'.V?t! ~t ^ p oo O e d # e r tt a K tti-aVg-^o'`f*.r3j0'i.0' n s . fc r 20n in it."a!.;:j' 'W * '* ,,< . . ..l ^ a M n ftjtfo r2 0 to 2 5 m im it a y * e ttin g < jf3 0 Q .ip o i,o riin ia iw e n ire w e n ie D r ii!rf '& $ & ^ r v r s & & -; l U l . U b d i f i c a i 15 m LcentciA ge lube W itrth s same infi)rmxbcifl as in 13.10. ' . - 1123 P n t h sample on this ily t i o l nitrogen'e v jS iito r uatjdry,' ^ ipraxim itely i 2 boiBlif'v >. J ' :x? -' vTr - ` 1 0 'in L to ncfa w nttif o ie tu h e M in s t grad aitciigipetteffi .' .'. H l i V oitaTm ix fofO secoda^ ;;-^ "^ ^ " I V " '-. '-r' v 'iL s s s .' V - ; ? ' ' 1 I2d Atlvh Al mii mJm mmA fihaoM 1 iv>tvf{niMand trawfa rmowmII aa!.*___> i^27aLabd the antovial with the studynumber, animal number and fender, u .^matnx^fia&I aotvant extraction dke,and analyses) prferiiof tba'md v * /sf.v * v - * ^ ,* 7 .* ..* 'j *?' *- . - *y' '* a ; . \ _ - ^ r 1128.CVdstore e ^ rM kmom tempentnre or a! vpromatdy 4*C nntilS iS " *2 >, 'i v i V, ' ' - ' '' . . . 1229 Complete the n tnicticn W w, tacherf to thisrtncnmrni, aod tape ip stttdyj<UKWW. .. ;' orpeladeinstudybinder, inippibtrriite. " ?' ':;-\ " :' *'*. ' F T ' : .* : ;.. . ./..: : ? r' *' v r i l > ' ' * ? / * : * v ? ' ' : "* ; -;' 'r y 4 O Centre Analytical Laboratories, Inc. C entre A nalytical Laboratories, Inc. Page 38 of43 Page 91 o f 102 Centre Study No.: 023-041 <3nfiSTro(b66I No. OOP-023-041 m-+; 'jn. ***' "/ j'.'M. \ :. *v\i*'. I\* C "', * ' /. *' ': ' *i\ ;Q . ^ ------- : - -, .h|10AfU v;.\ s f u a t m t n m i m u m ^ nr . . .jV'.'* ' !`.'I--,.';vj{;-'^ Centre Analytical Laboratories, Inc. Page 39 of 43 Centre Analytical Laboratories, Inc. Page 92 o f 102 000 1/ *. best c o py available Centre Study No.;. 023-041 ---- CentrerProtocol No. OOP-023O'll- .7 -' /yV v% '.* '.v v o ^ i'- - - r S ^ - . - i ' / - ?T*;* .' * * 'U-\** >* S tu d y } v"..v S an o g H eS td ,^ t M ittix i'- v - -- '-- * f # V * A y/Yflyty 'prj^hiL v^> * a c i n i % p p ' t i a s i iF C M ix S M i .;F C i * S td : ' p p ra tJO p p m 'a e t n a l P p m - r t s a l '. - y p p m > '.' ' y * v V-, , s t1 ! , r D te S iJikS d/A ialva Vice Iff V . U S ... i ~.... , , . . . . -1.*. ' 1 * .. 'i u-J.V- .** 'r'M t- i f / tf* v V-* . -N . ...r'v * $ K ? . `* r ' - . t i ..-i-.V i 1- . .* V,. > *' r'V t , V < * :.:r: - * *. - . . a .VSt*v - V. '-'T ***" f> . ,f ' **' ;7.* . - r 1^'s ** "*'** * > a r W ' . - ' - r- " V' *M* y*1 ' "'-% . * A' *W1 ../ y y ' - ` r.:1^ . i` 'XBifV -V i't? *.'** A '*.' *-- aTT^S^T V > > A t f - 'X '* & fc w W > .V jR l^ aU * -*J*W *'* " * i > . ,:. < . > ; - ..^ w v *' * * ' ' L* . . . S l - i M ... `"7; .. V -W T W M - f . - * * . - 'fir #< ' . a \ < -g M 'jk >' i o f t ^ j a r i r / i> * V.f'-i'A .- .*" * ' ........ A w V ! ' c r W Ss.V^f^WH ' -" 'j- ' r : :- . ** :r - ............ 1 ' ' ' (3 ~------------- ------------------ ... .* . . v .. . ^ . *. V -'* u.-.v'*.* 1- y . A_ teX.IrTZ+f'J&l .. ,*. ii < . 7 fy**?-:S<r9':> . ^*k.-.>-` '* . ti.*' :* '*?.- s '. .. * \ ' .# rVw*;t r W l l > ,.w k M ! a r ^ j s q f . V/'V . ,. *r . * .**>'- .* -iiT n. ' ' i , -'*r -" <i4 *1? *W. W A* 1* * '* * V ' .y * '* - s. ' . -* ` p* * * . ; ' A*V'V* -;> . * * * / N J * '. .' * tr - ')*** s . V i ^ .' - Crane Analytical taboratqrie, Inc. Centre Analytical Laboratories, Inc. Page40of43 ' Page 93 of 102 BESTCO PY AVAILABLE Centre Study No.: 023-041 CentreProtocol No. 00P-023^4i- ' lFO SE-O H ooJy f or k D l" 1 ,fa w li* r ti* . j .- . v , ' f : ~ r .i. fctp tm d . ' - "- .'U m > n*oi. n a a n - and*Hb avenge A i (M O Jhbit < . 1 2 3 7 ^ * ,M0 - --' ' e Jo itsm V n w r a f l n iff*? fM J o Prepand: Unt : u afa aad u d i.' A M I m M .) JUbbii ; f u - i o r . <"*> j^ S S S fe (M ^totoU ^ 1 1 ;u -3 o o n an 't S f u b u S w & isP r V B .1 IT Lm r B asil XabM ^v-^VVs^ * n o u i y S & r -'if& f * rxptR d Range o f . ~ L O L ft a ^ ' JU apaof V L O L ta a ^ n attaT - tveage --'a.lv eO T ^ -' . daadaidr sr A M M A I w h m i W m o - to*) M M ) .-(M V m 3 (K -1232 u -1 2 0 0 . -re o .. i*vt<* ,o:v Hw -tr >r:-------- f; `f r i l l - A iactoM B: MDL/LOQVita ' r " ' *- : ET&&40 . B a te d flfOS Ana U rn "'v>* . ': ..htirfti '* *t*'"`V` 1%'. Centre Analytical Laboratories., Inc. Page 41 of43 Centre Analytical Laboratories,.Inc. Page 94 o f 102 ; BEST COPY AVAILABLE Centre Study No.,: 023-041 Centre ProtocolNa00P-0234Mr MISS W-- : *r. r . : . o AaxhmntCSaadaidCikihtioa ' ?: ETSMO . . .vl EmetiatorPFOSfroaUvir Centre Analytical Laboratories, Inc. Centre Analytical Laboratories, Inc. hptltfM Page 42 of 43 Page 95 of 102 0 0 0 2 :1 7 BEST COPY AVAILABLE Centre Study No'.: 023-041 Centre Protocol No. 00P-023-041 ' C tlcn lated eo a ctn trid o n j o f ita e iU n li la tie lam ple.m itrixV rV p ro s w a . rro sA x t i f o s i W O StA : F t a l '% cooe.*.,- 4 `t t t . V c o n V. failca c ' V j F U ``I / r i ! : * coao'V 1 COBS : V .to1" - J tS i 2 X : SM . 9 9 tft 5J9 . 1X0 T9S 1X0 m o . 29.9 29.9 1X0 a . 1X0 4*1 SSS 59.9 5 9 . 9 59.9 5 9 J 120 120 V 120 120 120 W9 299 T M .....4 * 4 ...! 4 4 T -n JV mi rt 5.99 1X0 29.9 59a 120 1** y S u n p u - A0 S ld u b e ; SU ccoe - n .. Aon ' '* u .a m aL H*y : 1 8 -- -- 0 0 4 -- tt 'v / K . 1 C " . r 5*9 " m. 599 9 599 . 599 599 191 - " 'i* 4 ...... 198 599 : m > N '?r\r& F u n . J1 1191 119* 1191 1191 ' Uvtr ---- f oe -- m a-- B W ---- i-MvJk 5-1000M b S r . " " EanM h . M aW< nine. n ssr 5 -io U n fa W M if MOOOn " M al - r n w c m 5-1000Mfc 4-ioqo ppb ka .... . fu t o n a li.in tfiW im lM L tmuuM--hr. n nWnnHi Amrlwnn c-siaArf ITS-M J Smodo* ofT0S fe n U nr Pop Mof14 Centre Analytical Laboratories, Inc. Centre Analytical Laboratories, Inc. Page 43 of43 Page 96 of 102 V% SEP. 6. 2001 11:39AM ENVIOHMENTAL LAB 2 3E 09 Centre Study N o.: 023-041 HO. 5647 P .2 3041 Kcmrcb Drlr,5UU CoUtf, PA 18M1. Rtoau (314)231-3032,Fiatasi (I14)23M253 PROTOCOL AMENDMENT Page l o f i Centre Study Number 023-041 Amendment Number 1 Effective Date: 12/18/00 Centre Protocol Number OQP-023-041 DfiSQUPTIQN .QFA 1. $ 9: Experiments! Design .SECTION AMENDEDIQ 1. Change the last paragraph to read as follows: Moisture detennination will be performed on all liver samples according to AOAC Officii! Method 9S0.46 Section B. (a), with the following modifications: 1. The sample weight will be - 0.5 g. 2. The drying time will be -12-14 hour. RATIONAL 1. At the request of the sponsor, moisture determinations will be done for every liver sample. Due to limited sample size, the sample weight used will be -0.5 g instead of -2 g. The drying dme required for such a small sample size does not have to be 16-18 houn, so the samples will be dried for -12-14 hours IMPACTQiifflE STUDY 1. No negative impact on the study. vestigator Signature Date ntativeTStudy Director) Signature 5^ Centre QAU Review A/4L n J x . f r * _______________ Pahroatv 12.19W1 RECEIVED T II C SEP. 6 . 1 :32PM C entre A nalytical L aboratories, Inc. Page 97 o f 102 SEP. 6.2001 11.39AU EKVIEOHKEHTAL LAB 2 3E 09 Centre Study N o.: 023-041 0.56*7 P. 5 Centre Analytical Laboratories, Inc. W l t o t t r c h P rit . S titt College. F A 1S01. iagai-W M . T**mam m<03i.|3O PROTOCOL AMENDMENT AmendmentNumber 2 Effective Date: Q3/2MH Page 1of 1 Centre StudyNumber 22HM1 Centre Protocol Number OOPJB^Atl D ESC R IPTIO N O P A M E N D E D SEC TIO N 1. | t ; Sanale Analysis (f) 2. 1 9: ExperimentalDesign 3. 8 S: LOMS/MS System end Operating Condition (Turbofansprsy) AMENDED TO 1. Change die left sentence to reed the following: Simple* in which peaks are detected at the corresponding analyte retention time*but are teat than the lowest concentration of the calibration standard! (0.0001 pg/mL) will be reported as NQ(not quantifiable). Z Add die following: The following equations will be need far quantitation af the simples: 1.AnalyteFound(ng/mL) - (peakarea - intercept) / slope 2- Analyte Found (pg/g) - faiuilvte found fnerinD x FVfraLlx DF x EV fm y B| ,,r AV (mL) x sample wt (g) x 1000ng WhereFV - final volume, DF dilution fsctor, EV extraction volume, AV . aliquot volume 3-Recoveiy (% ). final, found (u etm L ) - ave. analvte hi Ctrl fnrfmL x 1000 nr inn tmoont added (ng/mL) x 1pg 3.Change the computerlisted to DellUltnScin PI110 RATIONALE 1-3. Clarifybow the samplea re quantitated and repotted and dmbutrumenti used to acquire data. IMPACTONTHESTUDY 1-3. Nonegative impact on the study. 3 L D e j& Uny Sj^ithire | Signature Date Centre OAUReview Ih a k t RECEIVED TICE SEP. 6 . 1 :32PM C entre A nalytical L aboratories, Inc. Page 98 o f 102 O O O ^O Centre Study N o.: 023-041 Centre Analytical Laboratories, Inc. 364# Bonrtk Orto, Stata CoUtft, PA 16*01. Pbea (14)231-8032, FiaiuQe: (814)231-1253 Centre StudyNumber 023-041 PROTOCOL AMENDMENT AmendmentNumber 2 Date ofOccurrence: 08/24/01 Page 1of 1 Centre Protocol Number OQP-023-041 DESCRIPTION OF AMENDED SECTION 1. 3: SPONSOR AMENDED TO 1. Change the study director from Rochelle Robideau at 3M Environmental Technology and Safety Services to Sean Gallagher at Wildlife International, LTD, 8598 Commerce Drive, Easton, MD 21601, phone: 410-822-8600, fax: 410-822-0632. 2. Change Rochelle Robideau to the Sponsor Representative. RATIONALE 1-2. By request ofRochelle Robideau (fax dated 08/24/01 included in correspondence section of die taw data associated with this study) IMPACT ON THEJSTUDY 1-2. No negative impact on the study. l L . /y ? /U # z f Jemng Facility Management Signature i M l Date Incomtiinn g SCttuwdlyv nDiriwreActhovr SCiigmnMatuimre ' flpl) o\ Date Centre QAU Review fcfefc ^"130^0* February 12,1998/1 C entre A nalytical Laboratories, Inc. Page 99 o f 102 0002 SEP. 6.2001 11:40AM E P I0 M N T A L LAB 2 3E 09 Centre Study No.: 023-041 0.5647 P. 8 Centre Analytical Laboratories, Inc. 304*JUw*r*DrtTt,SUUO>*i,PA 11. Phooti (IM)I3I-WS3,Faotirile (*M)23M2J3 J PROTOCOL DEVIATIO N Deviation Number 1 Dite of Occurrence: (1) 12/21/00 Centn StudyNumber 023-041 CentreProtocol Number OOP-023-041 D ESCRIPTIO N O F D EV IA TIO N 1. j Amendment #1: Did notperformmoliture detennhutioo onthe followingample*became there wu no ampleavailable afterattraction: C lim i m Q fa a n p 0007*75 459 0007920 9531 0007*79 413 0007921 9533 ! 0007*11 4*5 0007922 9335 ! 0007*13 0007*15 417 4*9 0007924 000792* 9541 954 0007907 9503 0007937 957 0007911 9515 0007941 95*0 0007915 9525 0007942 ' 93*1 0007917 952* 0007943 95*2 000791* 9529 0007944 95*3 I ACTIONS TA K EN M u t tim ed SOP virino, te.. 1. Protocol deviadcnitcued.^. Record*! By/Date: l IM PACT O N T H E STU D Y iI 1. No remit for the mouture determination will bo available far the ample*. native Signature CALQAU Review. ,iu a c .. % in )t( Frtwny U.W9M RECEIVED T i l t SEP. 6 . 1 :32PM Centre Analytical Laboratories, Inc. Page 100 of 102 0 ()()? . *T* SEP. 6.2001 11:40AM ENVIRONMENTAL LAB 2 3E 09 Centre Study No.: 023-041 NO. 5647 P .7 3048RauarcliDrir,Sut* CoOeft,PA1*801. Phase; (814)331-8033,PacalmO*:(814)231-1253 PROTOCOL DEV IA TIO N DeviationNumber: 2 Dite ofOccurrence: (1) 12/21/00 Centre Study Number 023-041 Cent Protocol Number; OOP-023-041 D ESCRIPTIO N O F D EVIATIO N 1. i Amendment#1: Weighed lesitfca-0.5g for die moisture determination on the following umplei beceuM it wu all of the ampleevilltble after extraction; CflK W fowl III 0007913 0007*67 0007*80 0007927 0007936 0007931 P H e e tin 9320 4SI 484 9541 - 9564 9570 W e ia h tfa l 0.34 0.30 0.33 0.32 0 .2 6 on 1. Protocol deviation isn^d. ACTIONSTAKEN od.SOPTBritian. RecordedBy/Date: 3j isj] IMPACTONTHESTUDY 1. No negative impact became moUnira wu till calculated and the reaulta did not varyalgnlflcantly from the moiicurc lu for tamp! that weighed ~04g. RECEIVED TIIC SEP. 6. 1*3HPM Centre Analytical Laboratories, Inc. Febcmr 1Z 199V2 Page 101 o f 102 SEP. 6. 2001 11:40AM EHVIEONMEHTAL LAB 2 3E 09 Centre Study No.: 023-041 0. 5647 P. 6 3048 RwaarcfaDrirt, State Colkf*, PA 14*01- PImm 1*14)33140, Pecriml! (4)231-1383 PROTOCOL DEVIATIO N Deviation Number 3 Date of Occurrence: (1) 12/21/00, (2) 12/21/00 and 3/12/01 . Centre Study Number 023-041 Centre Protocol Number 0OP-O23-G41 DESCRIPTIONOP DEVIATION 1. {Amendment#!: Did n perfora moisture determination the following samples became there w u no (ample available after extraction: C om Saronic ID 0007877 0007939 0011423 ClientIB 4*1 9575 at 2. { Aroendrrent!: The oven temperature for the moiiture detenninationi waa 110*C ACTIONSTAKEN 1-X Protocol deviation iM tpdr~\ Recorded By/Date: A .3 jjl$ 0 ,------------ IMPACTONTHE STUDY 1. No n>lu for the znoUturc detenninatioo will be available for these aamplea. X No Deprive impact. pwayel l^eatigaiar Signature ............. Date S tM ta atet/S p o iu o r R ententativt Signature Date ' ' CAL QAU Review__________ ________________________ Primary iz, 1991/2 RECEIVED T i r e SEP. 6 . 32PM Centre Analytical Laboratories, Inc. Page 102 o f 102
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