Document OzZy6142RXEEkJJed8ke6LKjM

3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACLTRTNO-UX2-010013 Study Title 104-Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats Analytical Laboratory Report Title Determination of the Presence and Concentration of PFOS, PFOSA, PFOSAA, EtFOSE-OH, M556, and PFOSEA in Serum and Liver Samples of Crl:CD(SD) IGS BR Rats Exposed to N-Ethyl Perfluorooctanesulfonamido Ethanol Data Requirement Not Applicable Author 3M Environmental Laboratory Study Completion Date June 06, 2001 Performing Laboratories Liver and Serum Analyses 3M Environmental Laboratory Building 2-3E-09, 935 Bush Avenue St. Paul, MN 55106 Project Identification 3M Medical Department Study: T-6316.1 Covance In-Life Study: 6329-212 Analytical Report: FACT TOX-001 3M Laboratory Request No. U2103 Total Number of Pages 310 3M Environmental Laboratory 3MEnvironmental Laboratory Page 1 Page 1 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACLTRTNO-UX2-010013 This page has been reserved for specific country requirements. 3M Environmental Laboratory 3MEnvironmental Laboratory Page 2 Page 2 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 GLP Compliance Statement Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACT TOX-001 LRN-U2103 Analytical Laboratory Report Title: Determination of the Presence and Concentration of PFOS, PFOSA, PFOSAA, EtFOSE-OH, M556, and PFOSEA in Serum and Liver Samples of Crl:CD(SD) IGS BR Rats Exposed to N-Ethyl Perfluorooctanesulfonamido Ethanol Study Identification Numbers: T-6316.1, FACT TOX-001, LRN-U2103 This study was conducted in compliance with United States Food and Drug Administration (FDA) Good Laboratory Practice (GLP) Regulations 21 CFR Part 58, with the exceptions in the bulleted list below. Exceptions to GLP compliance: There were two study directors in this study. This study was designed as two separate studies. The in-life phase study was considered to end at the generation and shipment of specimens. The analytical study was considered to start at the receipt of these specimens for analysis. This resulted in having two separate study directors, one for each phase of the same study. However, since the technical performance of each phase was entirely separate, no effect is expected from this exception. Sample storage stability will not be determined. Characterization of the analytical standards is underway, but has not yet been completed (21 CFR 58.105 (a)). Lot No. 59905 of the surrogate, THPFOS, will not be characterized for purity since quantities of this standard are exhausted. The electronic data systems in use have not been validated and there is not an Aeluetchteronntiiccaateuddithatrradil coofpcieosrreocftciohnrsomcuartroegnrtalymasvaanildabaless(o2c1iaCteFdRd5o8c.u1m30en(ets)).will be considered as the original raw data. Some changes in the raw data entries were not all made in accordance with 21 CFR 58.130 (e). Some reagents and solutions did not have expiration dates on the labels, as required according to 21 CFR 58.83. (See next page for signatures) 3M Environmental Laboratory 3MEnvironmental Laboratory Page 3 Page 3 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 GLP Compliance Statement (continued) Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACLTRTNO-UX2-010013 ~2IA . . John L. Butenhoff, Ph.D., Director Date T(e.a_ Marvin T. Case, D.M.V., Ph.D., Sponsor Representative k %H> Date William K. Reagen, Ph.D., Laboratory Manager Date 3M Environmental Laboratory 3MEnvironmental Laboratory Page 4 Page 4 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACT TOX-001 LRN-U2103 GLP Study-- Quality Assurance Statement Analytical Laboratory Report Title: Determination of the Presence and Concentration of PFOS, PFOSA, PFOSAA, EtFOSE-OH, M556, and PFOSEA in Serum and Liver Samples of Crl:CD(SD) IGS BR Rats Exposed to N-Ethyl Perfluorooctanesulfonamido Ethanol Study Identification Numbers: T-6316.1, FACT TOX-001, LRN-U2103 This study has been inspected by the 3M Environmental Laboratory Quality Assurance Unit (QAU) as indicated in the following table. The findings were reported to the study director and laboratory management. Inspection Dates Phase Date Reported to Management Study Director 4/7/00-4/11/00 In-phase 5/8/00 5/8/00 1/15/01-2/4/01 Data 2/5/01 2/5/01 3/23/01,3/26/01-3/30/01 3/26/01-3/27/01,3/29/013/30/01,4/2/01-4/5/01 4/3/01 -4/6/01,4/12/01-4/13/01, 4/17/01 5/3/01,5/7/01-5/10/01, 5/15/01-5/16/01 Data Data Data Draft Report 3/30/01 4/6/01 4/18/01 5/16/01 3/30/01 4/6/01 4/18/01 5/16/01 QAU Representative 11 - o j Date 3M Environmental Laboratory 3MEnvironmental Laboratory Page 5 Page 5 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 Table of Contents Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACT TOX-001 LRN-U2103 GLP Compliance Statement............................................................................................... 3 GLP Study--Quality Assurance Statement........................................................................5 Study Personnel and Contributors......................................................................................8 Introduction and Purpose.................................................................................................... 9 Test System....................................................................................................................9 Specimen Collection and Analysis................................................................................. 10 Specimen Receipt and Maintenance.................................................................................. 10 Chemical Characterization of the Reference Materials.......................................................12 Dose Confirmation Analyses.......................................................................................... 12 Method Summaries..............................................................................................................13 3M Environmental Laboratory........................................................................................ 13 Preparatory Methods................................................................................................. 13 Analytical Methods.................................................................................................... 14 Analytical Equipment................................................................................................. 14 Data Quality Objectives and Data Integrity.........................................................................15 Data Summary, Analyses, and Results............................................................................... 15 Summary of Quality Control Analyses Results for PFOS, PFOSA, PFOSAA, M556, EtFOSE-OH and PFOSEA............................................................................................. 16 Statement of Data Quality.............................................................................................. 18 Summary of Sample Results......................................................................................... 19 Statistical Methods and Calculations.................................................................................. 19 Statement of Conclusion..................................................................................................... 19 References.......................................................................................................................... 19 Appendix A: Chemical Characterization and Control Matrices............................................... 20 Appendix B: Protocol, Amendments and Deviations......................................................... 21 Appendix C: Extraction and Analytical Methods............................................................. 105 Appendix D: Data Summary Tables................................................................................. 185 Appendix E: Data Spreadsheets....................................................................................... 198 Appendix F: Example Calculations................................................................................... 284 Appendix G: Interim Certificates of Analysis..................................................................... 285 Appendix H: Report Signature Page................................................................................. 3-1n 3M Environmental Laboratory 3MEnvironmental Laboratory Page 6 Page 6 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 List of Tables Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACT TOX-001 LRN-U2103 Table 1. Test System Population Demographics for Study 6329-212...............................9 Table 2. Specimen Collection for FACT TOX-001..............................................................10 Table 3. Characterization of the Analytical Reference Standards in Study FACT TOX-001.................................................................................................................12 Table 4. Target Ions Monitored in 3M Laboratory Analyses............................................... 15 Table 5. Matrix Spikes--Sera............................................................................................ 17 Table 6. Matrix Spikes--Liver............................................................................................. 18 Table 7. Characterization of the Control Matrices Used for Sera Analyses in Study FACT TOX-001...................................................................................................... 20 Table 8. Characterization of the Control Matrices Used for Liver Analyses in Study FACT TOX-001...................................................................................................... 20 Table 9. Characterization of Test Article in Study FACT TOX-001....................................20 Table 10. FACT TOX-001 Data Summary of PFOS Concentration--Serum (pg/mL)...... 186 Table 11. FACT TOX-001 Data Summary of PFOSA Concentration--Serum (pg/mL) 187 Table 12. FACT TOX-001 Data Summary of PFOSAA Concentration--Serum (pg/mL).. ^qq Table 13. FACT TOX-001 Data Summary of EtFOSE-OH Concentration--Serum (pg/mL)..................................................................................................................189 Table 14. FACT TOX-001 Data Summary of M556 Concentration--Serum (pg/mL)....... 190 Table 15. FACT TOX-001 Data Summary of PFOSEA Concentration--Serum (pg/mL) ..191 Table 16. FACT TOX-001 Data Summary of PFOS Concentration--Liver (pg/g)............. 192 Table 17. FACT TOX-001 Data Summary of PFOSA Concentration--Liver (pg/g)......... 193 Table 18. FACT TOX-001 Data Summary of PFOSAA Concentration-- Liver (pg/g)........ 1 9 4 Table 19. FACT TOX-001 Data Summary of EtFOSE-OH Concentration--Liver (pg/g)... 195 Table 20. FACT TOX-001 Data Summary of M556 Concentration--Liver (pg/g)..............196 Table 21. FACT TOX-001 Data Summary of PFOSEA Concentration--Liver (pg/g)....... 197 3M Environmental Laboratory 3MEnvironmental Laboratory Page 7 Page 7 3M M edical D epartm ent Study: T6316.1 3M Medical Department Study: T-6316.1 Study Personnel and Contributors Analytical Report: FACT-TOX-001 L R N -U 2103 Analytical Report: FACT TOX-001 LRN-U2103 Study Director John L. Butenhoff, Ph.D. 3M Corporate Toxicology - Medical Department 3M Center Building 220-2E-02 St. Paul, MN 55144-1000 651-733-1962 Sponsor Marvin T. Case, D.V.M., Ph.D. 3M Corporate Toxicology - Medical Department 3M Center Building 220-2E-02 St. Paul, MN 55144-1000 Analytical Chemistry Laboratories Liver and Serum Analyses 3M Environmental Laboratory Kristen J. Hansen, Ph.D., Principal Analytical Investigator 3M Lab Contributing Personnel David R. Barnidge, Ph.D.* Lisa A. Clemen Lisa A. Dick, Ph.D. Rhonda S. Dick* Kelly J. Dorweiler* Mark E. Ellefson Sara E. Estes* Tina M. Galloway Barb A. Gramenz* Sarah A. Heimdal* C a ri S . H e w itt* 'Contract lab professional service employees Marlene M. Heying* Joy D. Jenkins Harold O. Johnson Ognjenka Kruplijanin* Sally A. Linda* Ian A. Smith* Kathleen M. Stock* Kelly J. (Kuehlwein)*Swartout Anh-Dao Vo Bob W. Wynne* R ic h a rd D . Y o u n g b lo m * Location of Archives All original raw data, protocol, and analytical report have been archived at the 3M Environmental Laboratory. The test article and analytical reference standard reserve samples, as well as the specimens pertaining to the analytical phase of this study are archived at the 3M Environmental Laboratory. 3M Environmental Laboratory 3M E nvironm ental Laboratory Page 8 Page 8 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 Introduction and Purpose Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACT TOX-001 LRN-U2103 The purpose of the study is to determine the presence and concentration of PFOS, PFOSA, PFOSAA, EtFOSE-OH, M556, and PFOSEA in serum and liver specimens collected from Covance Study No.: 6329-212 titled: 104-Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats. The Covance in-life study was initiated on January 21,1998. The analytical phase of the study was initiated on April 9, 1998. Test System A total of 410 males and 410 female rats were used as the test system. Table 1 outlines the rat population demographics and dosage levels for study 6329-212. The test system species and strain selected was the Crl:CD(SD) IGS BR rat received from Charles River Laboratories, Inc., identified using an implanted microchip device. At the initiation of treatment the rats were approximately 45-51 days old and weighed between approximately 100-310 g. Table 1. Test System Population Demographics for Study 6329-212 Study Group Number of Animals Male Female Approximate Dietary Levels of EtFOSE-OH (ppm) Group 1 Control 70 70 Group 2 Low 60 60 Group 3 Mid 60 60 Group 4 Mid-High 70 70 Group 5 High3 Group 6 Mid-High Recovery13 70 40 70 40 Group 7 High Recovery3 40 40 a Groups 5 and 7 were terminated during week 8 of treatment due to toxicity. b Group 6 was placed on recovery after 52 weeks of treatment. 0 3 30 100 300 100 300 3M Environmental Laboratory 3MEnvironmental Laboratory Page 9 Page 9 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACT TOX-001 LRN-U2103 Specim en Collection and Analysis Specimens were collected by Covance (study 6329-212) and sent to the 3M Environmental Laboratory for analysis. Table 2 lists the sampling intervals and types of specimens that were collected for this study. Table 2. Specimen Collection for FACT TOX-001 Week # 4 8 14 27 53 105 Number and Type of Specimens 50 serum and liver specimens 40 serum and 20 liver specimens 120 serum and 40 liver specimens 80 serum specimens 100 serum and 20 liver specimens 156 serum and 157 liver specimens Group # and Sex of Animal Groups 1-5 males and females Groups 1 and 5 males and females Groups 1-4 males and females Groups 1-4 males and females Groups 1 and 4 males and females Groups 1-4 and Group 6 males and females The total number and type of specimens collected for analyses in the analytical phase of this study are presented below. Specimens Collected from Study Groups 1 through 5 (through 2/01/00): Serum Specimens--524 specimens (423 samples were analyzed.) Liver Specimens--265 specimens (All 265 samples analyzed.) Specimens Collected from Study Group 6 (Recovery) on 2/01/00: Serum Specimens--22 specimens (All 22 samples analyzed.) Liver Specimens--22 specimens (All 22 samples analyzed.) Liver and sera specimens were shipped to the 3M Environmental Laboratory frozen and on dry ice. Sera and liver samples were extracted beginning on April 23, 1998 using an ion pairing reagent and either ethyl acetate or methyl-fert-butyl ether (MtBE). Liver samples were homogenized prior to the extraction procedure. Sample extracts were analyzed using high-pressure liquid chromatography-electrospray/tandem mass spectrometry (HPLC-ESMSMS) in the multiple reaction monitoring mode. PFOS, PFOSA, PFOSAA, EtFOSE-OH, M556, and PFOSEA levels were evaluated by external calibration using extracted curves. Analytical details are included in this report. Specimen Receipt and Maintenance The 3M Environmental Laboratory received liver and serum specimens collected at predetermined time points during and at the end of the in-life phase of Covance Study 6329-212 from February 1998 through February 2000 from Covance. All specimens were received frozen on dry ice and were immediately transferred to storage at -20C 10C. 3M Environmental Laboratory 3MEnvironmental Laboratory Page 10 Page 10 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACLTRTNO-UX2-010013 Control matrices used in liver and sera analyses performed during TOX-001 were obtained from commercial sources and are presented in Appendix A (see Tables 7 and 8). Samples analyzed at the 3M Environmental Laboratory will be maintained for a period of 10 years and will be stored at the laboratory at -20C 10C to -80C 20C. 3M Environmental Laboratory 3MEnvironmental Laboratory Page 11 Page 11 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Analytical Report: FACT TOX-001 LRN-U2103 Chemical Characterization of the Reference Materials Chemical characterization information on the analytical reference materials used in this study is presented in tabular form below. Table 3. Characterization of the Analytical Reference Standards in Study FACT TOX-001 Reference Standard / Form ula Potassium Perfluorooctanesulfonate C8 F17S O 3-K+ N-Ethyl Perfluorooctanesulfonam ido ethyl alcohol CaFuSOzNit^HslCHzCHaOH Sodium P e rflu o ro oc tan es ulfon y la m ido (eth yl) acetate C 8 Fi7S02N (C H 2C H 3)C H 2C 0 0-N a P erflu o ro o c tan es u lfo n y la m id o (eth yl)ac id C 8 F i7 S 02 N(CH2CH3)CH2C 0 0 - h P erflu o ro o c tan es u lfo n y la m id e C8F17SO2NH2 P e rflu o ro o c tan es u lfo n y le th y la m id e C8F i7S 02NHCH2CH3 M 556 C8F, 7S 0 2N (H )CH2C 0 0 H 1H, 1H, 2H, 2HTetrahydroperfluorooctanesulfonic acid C 8H 4 F i 3 S 0 3H 'This lot is exhausted and cannot be characterized. NR-- Not recorded NA-- Not applicable TB D -- To be determined Acronym Source Expiration Date 3M 08/31/01 KPFOSa 3M 2010 3M 2010 EtFOSE-OH 3M 3M 2010 11/26/01 Storage C o n d itio n s Ambient temprature Ambient temprature Ambient temprature Ambient temprature Ambient temprature Chem ical Lot Number 171 193 215 936 Unknown (SD013) Physical D es crip tio n Ught colored powder W hite crystals W hite powder Amber waxy solid Amber waxy solid Purity 86.4% 88.0% TBDC NA* 88.9% 3M 01/01/2010 Ambient temprature 617 Yellow to amber liquid TBDC PFOSAAb PFOSA PFOSEA M556 THPFOS 3M 01/01/2010 Ambient NB 112999-99 Tan waxy solid TBDC temprature Ambient 3M 01/01/2010 temprature L2353 Amber to brown waxy solid TBDC 3M 2010 Ambient NR NR temprature (TN-A-1886) TBDC 3M 01/01/2010 Ambient temprature L15709 Ught yellow waxy solid TBD 3M 01/01/2010 Ambient 529 Amber waxy TBDC temprature solid Ambient 3M 01/01/2010 temprature NB113047-80 W hite powder TBD ICN 01/01/2010 Ambient temprature 59909 Brown powder NA* Ambient ICN 01/01/2010 temprature 53406 Brown W axy Solid TBDC "Target analyte is PFOS, C aF17S 0 3 "Target analyte is C8F,7S 02{(CH2C H 3)(C H 2C 0 0 ') } cUnless otherwise indicated, at the time of quantitation the purity for all analytes was assumed to be 100%. Dose Confirmation Analyses Dose preparation methods and analysis were performed by Covance, using a validated analytical method provided by the Sponsor (MP-M312-MA), and are reported separately (Reference Covance 6329-212). 3M Environmental Laboratory 3MEnvironmental Laboratory Page 12 Page 12 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 Method Summaries Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACT TOX-001 LRN-U2103 Following is a brief description of the methods used during this analytical study by the 3M Environmental Laboratory. Detailed descriptions of the methods used in this study are located in Appendix C. Data collected prior to November 1999 was reworked in 2000 to accommodate improvements in data reduction methods. Both the original and "reworked" data are archived; reworked data is presented in the final results. The improved methods are documented in the form of method modifications. As the present study progressed, more advanced methods evolved and these methods were used with deviations until amendments to the protocol were written. Protocol and method deviations are located in Appendix B of this report. 3M Environmental Laboratory Preparatorymethods FACT-M-1.0. "Extraction of Potassium Perfluorooctanesulfonate or Other Anionic Fluorochemical Surfactants from Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry." This method was used for week 4, week 8, and week 14 samples. FACT-M-3.0, "Extraction of Potassium Perfluorooctanesulfonate or Other Anionic Fluorochemical Surfactants from Serum for Analysis using HPLC-Electrospray/Mass Spectrometry." This method was used for week 4, week 8, and week 14 samples. ETS-8-4.1, "Extraction of Potassium Perfluorooctanesulfonate or other Fluorochemical Compounds from Serum for Analysis using HPLC-Electrospray/Mass Spectrometry." This method was used for week 27, week 53, and week 105 samples. ETS-8-6.0, "Extraction of Potassium Perfluorooctanesulfonate or other Fluorochemical Compounds from Liver for Analysis using HPLC-Electrospray/Mass Spectrometry." This method was used for week 53 and week 105 samples. An ion-pairing reagent was added to the sample and the analyte ion pair was partitioned into ethyl acetate (FACT-M-1.0 and FACT-M-3.0) or MtBE (ETS-8-4.1 and ETS-8-6.0). The extract was transferred to a centrifuge tube and put onto a nitrogen evaporator until dry. Each extract was reconstituted in 1.0 mL of methanol, and then filtered through a 3 cc plastic syringe attached to a 0.2 pm nylon filter into glass autovials. 3M Environmental Laboratory 3MEnvironmental Laboratory Page 13 Page 13 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACT TOX-001 LRN-U2103 Analytical Methods FACT-M-2.0, "Analysis of Liver Extracts for Fluorochemicals Using HPLC-Electrospray/Mass Spectrometry" . FACT-M-4.0, "Analysis of Fluorochemicals in Serum Extracts Using HPLC-Electrospray/Mass Spectrometry". ETS-8-5.1, "Analysis of Potassium Perfluorooctanesulfonate or other Fluorochemicals in Serum Extracts Using HPLC-Electrospray/Mass Spectrometry". ETS-8-7.0, "Analysis of Potassium Perfluorooctanesulfonate or other Fluorochemicals in Liver Extracts Using HPLC-Electrospray/Mass Spectrometry". The analyses were performed by monitoring one or more product ions selected from a single primary ion characteristic of a particular fluorochemical using HPLC-ES/MS/MS. For example, molecular ion 499, selected as the primary ion for PFOS (C8Fi7S 03-) analysis, was fragmented further to produce ion 99 (FS03-). The characteristic product ion 99 was monitored for quantitative analysis. Analytical Equipment The actual analytical equipment settings used in the present analytical phase of this study varied slightly during actual data collection. The following is representative of the settings used during the analytical phase of this study. Liquid Chromatograph: Hewlett-Packard Series 1100 Liquid Chromatograph system Analytical column: Keystone BetasilTM Ci82x50 mm (5 pm) Column temperature: Ambient Mobile phase components: Component A: 2mM ammonium acetate Component B: methanol FInlojewctiroantev: o3l0u0mep:L/1m0inpL Solvent Gradient: 13.5 minutes Time (m inutes) 0.0 8.5 11.0 12.0 13.5 %B 40% 90% 90% 40% 0% 3M Environmental Laboratory 3MEnvironmental Laboratory Page 14 Page 14 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACLTRTNO-UX2-010013 Mass Spectrometer: Micromass API/Mass Spectrometer Quattro IITMTriple Quadrupole system Software: Mass LynxTM 2.3, 3.1,3.2, 3.3, 3.4 Cone Voltage: 30-60 V Collision Gas Energy: 25-45 eV Mode: Electrospray Negative Source Block Temperature: 150C 10C Electrode: Z-spray Analysis Type: Multiple Reaction Monitoring (MRM) Table 4. Target Ions Monitored in 3M Laboratory Analyses Target Analyte Primary Ion ( a m u ) Product Ion (a m u ) PFOS 499 80, 99, 130 PFOSA 498 78 PFOSAA 584 83, 169 EtFOSE-OH 630 59 PFOSEA 526 65 M556 556 65, 78, 83, 169 THPFOS 427 80 Data Quality Objectives and Data Integrity The following data quality objectives were indicated in the method performance section of ETS8-5.1, Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Serum Extracts Using HPLC-Electrospray/Mass Spectrometry and ETS-8-7.0, Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Liver Extracts Using HPLC-Electrospray/Mass Spectrometry: Linearity: The coefficient of determination (r2) equal to or greater than 0.980. Limits of Quantitation (LOQ): The LOQ is equal to the lowest acceptable standard in the calibration curve. Acceptable Precision: Precision is better than 30% for the method. Acceptable Spike Recoveries: 70-130% Data Summary, Analyses, and Results Data quality objectives for the analytical phase of this study outlined in the 3M Environmental Laboratory protocol for FACT TOX-001 (see Appendix B) were met with the exceptions noted in this report. See Appendix B for deviations. 3M Environmental Laboratory 3MEnvironmental Laboratory Page 15 Page 15 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACT TOX-001 LRN-U2103 Summary o f Quality Control Analyses Results for PFOS, PFOSA, PFOSAA, M 556, EtFOSE-OH and PFOSEA Linearity: The coefficient of determination (r2) of the standard curve was >0.980. Calibration Standards: Quantitation of the target analytes was based on linear regression analysis weighted 1/x of a single, opening or two bracketing extracted matrix curves for each group of samples. Rat and rabbit sera were used for matrix curves for sera analyses, while rabbit liver was used for matrix curves for liver analyses. High or low points on the curve may have been deactivated to provide a better linear fit over the curve range most appropriate to the data. Low curve points with peak areas less than two times that of the extraction blanks were deactivated to disqualify a data range that may have been significantly affected by background levels of the analyte. Occasionally, a single mid-range curve point that was an obvious outlier may have been deactivated. Quantitation of each analyte was based on the response of one or more specific product ion(s) using the multiple reaction monitoring mode of the instrument (see Appendix C, Analytical Methods). Calibration standards were prepared to run, undiluted, approximately within the linear range of the instrument (approximately 5 1000 ng/g). Limits of Quantitation (LOQ): The LOQ is equal to the lowest acceptable standard in the calibration curve (defined as a standard within 30% of the theoretical value), and is at least two times the analyte peak area detected in the surrogate matrix blanks, (see Appendix D). Blanks: All blanks were below the limit of quantitation for the compounds of interest, except PFOSA Week 8 H20 + liver Blk-2 (0.0663 pg/g and 0.0414 pg/g) and PFOS Week 105 liverBlk-2 (0.0163). To simplify analyses that were complicated by endogenous levels of fluorochemicals in unexposed rat sera and liver, rabbit sera and liver were selected as suitable surrogate matrices. Precision, Instrumental: Instrumental precision was determined by replicate injections of a single serum extract. Instrumental precision was determined for PFOS, PFOSAA, and M556; variation was less than 7.0 % for all targeted analytes. eMaacthrixbaStcphikoesf :seSrearasa--mMpaletsri.xSsapmikeplesasmwpelreesswpeikreedpbreeptwareeednfraopmprocoxnimtraotlerlayt7s5e--ra25a0lonngg/mwLith, levels that approximate the levels detected in the Group 1--Group 5 samples, depending upon the analyte. All spikes were prepared to run, undiluted, within a ten-fold limit of the linear range of the calibration curve. For some analytes, samples for some high dose animals may be much higher than the range of these prepared spikes. Sera matrix spike recoveries are presented in tabular form in Table 5. 3M Environmental Laboratory 3MEnvironmental Laboratory Page 16 Page 16 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACT TOX-001 LRN-U2103 Table 5. Matrix Spikes--Sera # of Spikes RAevecoravgeerySpiSkDe Range # of Spikes Deviating # of Spikes > 30% and < 50% Deviating > 50% PFOS 28 95 25% 65-183% PFOSA 28 103 20% 72-143% PFOSAA 28 111 24% 57-186% EtFOSE-OH 22 39 29% 18-127% M556* 22 126 22% 86-153% PFOSEA 22 63 14% 37-87% 3 4 3 0 8 8 1 0 1 20 3 6 M 556 was identified as a metabolite of E tF O S E -O H after initiation of the analytical work. Standard materia) was unavailable and had to be synthesized. N o M 5 56 data is provided for the W e e k 4 through W e e k 14. N O T E : T h e matrix spikes for E tF O S E -O H and P F O S E A were inconsistent or were not conducted with all groups of samples and indicate that data presented for these two analytes should be considered qualitative only. Liver--Matrix spike samples were prepared from control rat liver along with each batch of liver samples. Samples were spiked between approximately 100-1000 ng/g, levels that approximate the levels detected in the Group 1--Group 5 samples, depending on the analyte. All spikes were prepared to run, undiluted, within a ten-fold limit of the linear range of the calibration curve. For some analytes, samples for some high dose animals may be much higher than the range of these prepared spikes. Liver matrix spike recoveries are presented in tabular form in Table 6. 3M Environmental Laboratory 3MEnvironmental Laboratory Page 17 Page 17 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACT TOX-001 LRN-U2103 Table 6. Matrix Spikes--Liver PFOS # of Spikes 24 Average Spike Recovery SD 90 61% Range 0-196% # of Spikes Deviating > 30% and < 50% 4 # of Spikes Deviating > 50% 9 PFOS, revised(1) PFOSA 18 119 38% 60-196% 18 94 27% 26-128% 4 0 3 2 PFOSA, revised(1) PFOSAA 16 102 17% 71-128% 20 86 44% 0-147% 0 1 0 4 PFOSAA, revised(1) 16 105 19% 74-147% EtFOSE-OH 16 133 166% 25-567% 1 1 0 8 EtFOSE, revised(1) M556* PFOSEA 14 148 173% 26-567% 12 102 15% 85-141% 10 97 12% 80-117% 1 1 0 6 0 0 M 5 56 was identified as a metabolite of E tF O S E -O H after initiation of the analytical work. Standard material was unavailable and had to be synthesized. No M 5 56 data or Q C is provided for the W e e k 4 through W e e k 14 samples. ' N O T E : After matrix spikes had been prepared, unexpectedly high levels of the analytes were identified in the control animals. Spikes were originally prepared at either approximately 100 ng/g or 2 5 0 ng/g. Both of these levels were unacceptably low as they were less than 3 0 % of the endogenous levels found in the control animals. Data from these M S /M S D s were not included in the revised data presented above. N O T E : T h e matrix spikes for E tF O S E -O H and P F O S E A were inconsistent or were not conducted with all groups of samples and indicate that data presented for these two analytes should be considered qualitative only. Surrogates: The surrogate (THPFOS) was added to all samples and standards. THPFOS was not used for quantitation, but was used to monitor for gross instrument failure. After 11/04/99, the surrogate response of each analytical run was verified to determine that it did not vary more than 50% from the mean within each analytical run. Deviations of greater than 50% are noted in the results table. Statem ent of Data Quality It is not possible to verify true recovery of endogenous analyte from tissues without radio-labeled reference material. The only measurement of accuracy available at this time, matrix spike studies, indicate that the sera and liver data can be considered accurate to within one standard deviation of the average fortified samples recovery. For example, in liver, PFOS data is accurate to 119 38%. Please see bolded values in Tables 4 and 5 for specific values relating to data quality. The results of quality control analyses (curve fit, CCVs, and MS/MSDs) for EtFOSE-OH and PFOSEA were inconsistent and indicate that data presented for these two analytes should be 3M Environmental Laboratory 3MEnvironmental Laboratory Page 18 Page 18 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACT TOX-001 LRN-U2103 considered to be qualitative only. Values for these two analytes are presented in data tables in the spirit of full disclosure, but should not be used in any quantitative assessment of the data. Summary of Sam ple Results Some PFOS results (those obtained using lot 171) have been corrected for purity of the analytical reference material. Uncorrected results are noted in the data tables. Samples from Control Animals: The target analytes were often detected in the sera and liver samples from the control animals. These levels were usually lower than those found in the low dose test animals. Samples from Dosed Animals: In general, levels of the target analytes present in the sera and liver samples from the test animals increased with dose group, with the exception of Group 6, which was taken off the compound after 53 weeks. Detailed sample data tables are presented in Appendices D and E. Statistical Methods and Calculations Statistical methods were limited to the calculation of means and standard deviations. See Appendix F for example calculations used to generate the liver and serum sample data in FACT TOX-001. Statement of Conclusion Under the conditions of the present study, PFOS, PFOSA, PFOSAA, EtFOSE-OH, M556, and PFOSEA were observed in the sera and liver of rats dosed with N-Ethyl Perfluoroctanesulfonamido Ethanol during the in-life phase of the study. References Covance Study No.: 6329-212,104-Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluoroctanesulfonamido Ethanol in Rats 3M Environmental Laboratory 3MEnvironmental Laboratory Page 19 Page 19 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACT TOX-001 LRN-U2103 Appendix A: Chemical Characterization and Control Matrices Table 7. Characterization of the Control Matrices Used for Sera Analyses in Study FACT TOX-001 Control Matrix Rat Serum Rat Serum Rabbit Serum Source Expiration Date Storage Conditions Chem ical Lot # Physical Description NR-- not recorded Sigm a 2010 -20C 10C 17H9306 Rat Serum Sigm a 2010 -20C 10C 19H89291 Rat Serum Sigm a 2010 -20C 10C 47H4641 Rabbit Serum Table 8. Characterization of the Control Matrices Used for Liver Analyses in Study FACT TOX-001 Control Matrix Rabbit Liver Rabbit Liver Rabbit Liver Rabbit Liver Rabbit Liver Source Covance Laboratories, Inc.* Covance Laboratories, Inc.* Covance Laboratories, Inc.* Covance Laboratories, Inc.* Unknown Expiration D ate 2010 2010 12/99 2010 12/01/99 Storage Conditions -20C 10C -20C 10C -20C 10C -20C 10C -20C 10C Chem ical Lot # F00014 F00008 F00007 F00016 NR (T C R -9 9 0 6 2 -2 2 ) Physical Description Rabbit Liver Rabbit Liver Rabbit Liver Rabbit Liver Rabbit Liver N R -- not recorded "The control source is listed as C H W (Coming Hazelton Wisconsin) in the raw data This is the former name of Covance Laboratories, Inc. Table 9. Characterization of Test Article in Study FACT TOX-001 Test Article Chemical Name Source E tF O S E -O H N-Ethyl Perfluorooctanesulfonamido ethanol 3M Expiration Date 11/26/01 Storage Conditions Ambient temperature Chemical Lot # 30035, 30037, 30039 Physical Description W a x y solid Purity 97.4% * *This purity value is from the interim COA. The in-life report lists the purity as 98.1%; however, the C O A is considered the more accurate purity. 3M Environmental Laboratory 3MEnvironmental Laboratory Page 20 Page 20 3M Medical Department Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACT TOX-001 LRN-U2103 Appendix B: Protocol, Amendments and Deviations 3M Environmental Laboratory 3MEnvironmental Laboratory Page 21 Page 21 3M Medical Department Study: T6316.1 t % C O V A H ^l> THE DEVELOPMENT SERVICES COMPANY Analytical Report: FACT-TOX-001 LRN-U2103 Sponsor: 3M St. Paul, Minnesota PROTOCOL Study Title: 104-W eek Dietary Carcinogenicity Study with Narrow Range (98.1 %) N-Ethyl Perfluorooctanesulfonanrido Ethanol in Rats D ate: January 21,1998 Performing Laboratory: Covance Laboratories Inc. 3301 Kinsman Boulevard Madison, Wisconsin 53704 Laboratory Study Identification: Proposal No. 6777 Covance 6329-212 3MEnvironmental Laboratory Page 22 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 _____________________________________ !_____________________ ___________________ Page 2 Study 104-W eek Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats Purpose To assess the carcinogenicity o f the test material when administered in the diet to rats for at least 104 weeks Sponsor 3M Toxicology Services Building 220-2E-02, 3M Center St. Paul, Minnesota 55144-1000 Study Monitor Andrew M. Seacat, PhD 3M Telephone No.: 612.575.3161 Facsimile No.: 612.733.1773 Study Location Covance Laboratories Inc. 3301 Kinsman Boulevard Madison, Wisconsin 53704 Mailing Address: PO Box 7545 Madison, Wisconsin 53707 Study Director Peter J. Thomford, PhD Covance Laboratories Inc. Telephone No.: 608.241.7207 Facsimile No.: 608.242.2736 3MEnvironmental Laboratory Page 23 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Toxicologist Thomas E. Ryan, BS Covance Laboratories Inc. Covance 6329-212 _____________ P a g e 3 Proposed Study Timetable In-Life Start Date: January 26, 1998 In-Life End Date: January 31, 2000 Regulatory Compliance This study w ill be conducted in compliance with the Food and Drug Administration Good Laboratory Practice Regulations as set forth in Title 21 of the US Code o f Federal Regulations, Part 58, issued December 22, 1978 (effective June 20, 1979), and with any applicable amendments. Animal Care and Use Statement All procedures in this protocol are in compliance with the Animal Welfare Act Regulations, 9 CFR 1-4. In the opinion o f the Sponsor and study director, the study does not unnecessarily duplicate any previous work. Quality Assurance The protocol, study conduct, and final report will be audited by the Covance Quality Assurance Unit (QAU). The proliferation cell nuclear antigen evaluation, data, and report will be audited by the QAU o f Pathology Associates International. Test Material Identification T-6316 (Narrow Range N-Ethyl Perfluorooctanesulfonamido Ethanol, NEtFOSE) Lot Numbers The lot numbers will be maintained in the raw data. Purity 98.1% NEtFOSE (w/w) 3MEnvironmental Laboratory Page 24 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Stability Responsibility o f the Sponsor Covance 6329-212 _____________ P ag e 4 Storage Conditions At room temperature Characteristics Information on synthesis methods, composition, or other characteristics that define the test material is on file with the Sponsor. Reserve (Archive) Samples A reserve sample (approximately 5 g) will be taken and stored at room temperature. This sample will be transferred to the Sponsor after completion o f the in-life phase to be retained in accordance with 21 CFR 58.195. Disposition of Test Material After authorization from the Sponsor, any remaining test material will be returned to: Andrew M. Seacat, PhD 3M Toxicology Services Building 220-2E -02, 3M Center St. Paul, Minnesota 55144-1000 Telephone N o.: 612.575.3161 Facsimile N o.: 612.733.1733 Animals Species Rat Strain Crl:CD(SD)BR 3MEnvironmental Laboratory Page 25 - 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Source Charles River Laboratories, Inc., Raleigh, North Carolina Covance 6329 -212 _____________ P a g e 5 Age at Initiation of Treatment Preferably 6 weeks o f age, but not more than 8 weeks o f age Weight at Initiation of Treatment 100 to 300 g Number and Sex 410 males and 410 females Identification Implantable microchip identification device Husbandry Housing Individual (may be group-housed during acclimation) Diet Certified Rodent Diet #5002 (PMI Feeds, Inc.) a d libitum, unless otherwise specified. The diet is routinely analyzed by the manufacturer for nutritional components and environmental contaminants. Specified nutrient and contaminant analyses are on file at Covance-Madison. Water A d libitum . Samples of the water are routinely analyzed for specified microorganisms and environmental contaminants. The results are on file at Covance-Madison. Contaminants There are no known contaminants in the diet or water at levels that might interfere with this study. 3MEnvironmental Laboratory Page 26 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 _______________________________________ _________________________Page 6 Environment Environmental controls for the animal room will be set to maintain 18 to 2 6 C, a relative humidity o f 30 to 70%, a 12-hour light/12-hour dark cycle, and minimum o f 10 room air changes/hour. The light/dark cycle may be interrupted to accommodate study-related activities. Acclimation At least 1 week Randomization Selection o f animals for the study will be based on body weights, clinical observations, and other data as appropriate. Animals will be assigned to treatment groups using a computerized blocking procedure designed to achieve body weight balance with respect to treatment groups. At the time o f randomization, the weight variation o f the animals o f each sex used will not exceed 2 standard deviations o f the mean weight, and the mean body weight for each group o f each sex will not be statistically different at the 5.0% probability level. Justification Rats historically have been used in safety evaluation studies and are recommended by appropriate regulatory agencies. 3MEnvironmental Laboratory Page 27 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Group Designations and Dietary Levels Covance 6329-212 _________ Page 7 Group Number of Animals Male Female Dietary Levels (ppm NEtFOSE)6 1 (Control)bcd 2 (Low)c 3 (Mid)c 4 (Mid-High)c,d 5 (High)c,d 6 (Mid-High Recovery)6 7 (High Recovery)6 70 60 60 70 70 40 40 70 60 60 70 70 40 40 0 3 30 100 300 100 300 a T-6316 is 98.1% n-ethyl perfluorooctanesulfonamido ethanol (NEtFOSE); dose levels are expressed as ppm o f NEtFOSE. b The control animals will receive the basal diet only. c Five animals/sex in Groups 1 through 5 will be sacrificed during Weeks 3 and 14 for hepatocellular proliferation rate measurements and biochemical analyses (palmitoyl-CoA oxidation). d Ten animals/sex in Groups 1, 4, and 5 will be designated as interim sacrifice animals and will be sacrificed after at least 78 weeks o f treatment, e Animals in Groups 6 and 7 will be treated for at least 78 weeks, then treatment will be discontinued, and the animals will be observed for reversibility, persistence, or delayed occurrence o f toxic effects for at least 26 weeks posttreatment. During recovery, the animals w ill receive basal diet only. Dosing Procedures Method of Administration Dietary. Animals in Groups 1 through 5 will receive test diet for at least 104 weeks. Animals in Groups 6 and 7 will receive test diet for 78 weeks only. Reason for Dosing Route The potential human exposure is by the oral route. Dose Preparation Before initiation o f treatment, all dose preparations will be mixed once, and low- and high-dose preparations will be mixed four times for determination o f homogeneity and stability. 3MEnvironmental Laboratory Page 28 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 _____________________________________________________________________________ ______________________ P ag e 8 During treatment, all dose preparations will be mixed at least once every 4 weeks according to the study-specific mixing procedure developed by Covance. Dose concentrations will be based on the NEtFOSE content as supplied; the Sponsor has stated the T-6316 is 98.1% NEtFOSE (w/w) as supplied. All dose preparations will be stored at room temperature. Retention Samples Samples (approximately 100 g) will be taken from each dose preparation during the in-life phase and stored at room temperature. Unless used for analyses, these samples will be discarded at least 1 month after completion of the in-life phase. Dose Analyses By Covance using a method supplied by the Sponsor and validated by Covance Homogeneity Homogeneity will be determined for all dose level preparations once pretest and for the preparations for Weeks 1 through 3; for two additional pretest high-dose level preparations; and for four additional pretest low-dose level preparations. One sample (approximately 100 g) each from the top, middle, and bottom o f the dose preparations mixed for homogeneity analyses will be collected, divided into three subsamples for extraction and analysis, and analyzed for test material content. A ll samples will be stored at room temperature until analyzed within 7 days o f mixing. Homogeneity analysis will be repeated if batch size changes by more than 30%. Stability Four sets o f samples (approximately 100 g each) will be taken from the low - and high-dose level concentrations o f diet preparations mixed pretest to establish stability. One set will be analyzed on the day o f mixing. One set will be stored at room temperature for at least 19 days, then analyzed. The third set w ill be stored at room temperature after at least 32 days, then analyzed. The remaining set will be stored in a freezer set to maintain -10 to -30C for 8 weeks, then analyzed. 3MEnvironmental Laboratory Page 29 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 _________ Page 9 In addition, samples (approximately 100 g each) will be taken from the low - and high-dose level concentrations o f diet preparations mixed pretest. The samples will be stored at room temperature for 5 days, then for 7 days under animal room conditions (room temperature in a feeding container), then analyzed. Dose C onfirm ation Samples (approximately 100 g each) will be collected from all dose preparations and analyzed in duplicate. Homogeneity samples collected from the middle o f the dose preparations for W eeks 1 through 3 will be used for dose confirmation results. All samples will be stored at room temperature until analyzed. Observation of Animals Clinical Observations Each animal w ill be observed twice daily (a.m. and p.m.) for mortality and moribundity, recording findings as they are observed. Once prior to treatment and weekly thereafter, each animal will be removed from its cage and examined; abnormal findings or an indication of normal will be recorded. The following information on each grossly visible or palpable mass will be recorded. time o f onset location size (small or large) appearance progression Body Weights Prior to treatment (at randomization), weekly for Weeks 1 through 17, once every 4 weeks thereafter, and at Week 105 3MEnvironmental Laboratory Page 30 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 ________ Page 10 Food Consumption Weekly for Weeks 1 through 16 and once every 4 weeks thereafter Clinical Pathology Frequency and Number of Animals Unscheduled Collection When possible, a blood film will be made and held for possible future examination from animals sacrificed at unscheduled intervals. Scheduled Collections Hematology, clinical chemistry, urinalysis, urine chemistry, and serum sampling will be done on 10 animals/sex/group in Groups 1 through 5 during Weeks 14, 27, and 53. A blood film will be made and held for possible future examination for animals at scheduled sacrifices after at least 78 and 104 weeks o f treatment. Method of Collection Hematology, Clinical Chemistry, Urinalyses, Urine Chemistry, Serum Samples Animals will be fasted overnight; blood will be collected from a jugular vein. The anticoagulant will be potassium EDTA for hematology tests. Samples for clinical chemistry and serum samples will be collected without anticoagulant. Urine will be collected chilled overnight (approximately 16 hours). Blood Films Blood films will be taken as part o f the necropsy procedure. 3MEnvironmental Laboratory Page 31 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Covance 6329-212 Page 11 T ests H em atology red blood cell (erythrocyte) count hemoglobin hem atocrit m ean corpuscular volume m ean corpuscular hemoglobin m ean corpuscular hemoglobin concentration platelet count white blood cell (leukocyte) count differential blood cell count blood cell m orphology reticulocyte sm ear (made, but not exam ined) glucose urea nitrogen creatinine total protein album in globulin cholesterol to tal bilirubin C linical C hem istry alanine am inotransferase gamma glutamyltransferase aspartate am inotransferase calcium inorganic phosphorus sodium potassium chloride appearance volume specific gravity pH protein urobilinogen sodium potassium U rinalysis glucose ketones bilirubin blood microscopic exam ination o f sedim ent -- U rine C hem istry 16 hour excretion of: sodium potassium 3M E nvironm ental Laboratory Page 32 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 ________ Page 12 Serum Samples Serum not used for clinical chemistry will be stored in a freezer set to maintain -60 to -80C . Samples will be packed on dry ice and shipped to: Kris J. Hansen, PhD 3M Environmental Technology and Safety Services 935 Bush Avenue Building 2-3E-09 St. Paul, M innesota 55133-3331 Telephone No.: 612.778.6018 Facsimile No.: 612.778.6176 Samples will be retained by the Sponsor for possible future analysis. Hepatocellular Proliferation and Biochemical Analyses Frequency and Number of Animals Five animals/sex in Groups 1 through 5 during Weeks 3 and 14 Cell Proliferation Tissue Collection and Immunohistochemical Evaluation At each interval, animals will be fasted overnight, anesthetized with sodium pentobarbital weighed, and exsanguinated. The abdominal cavity o f each animal will be opened, and the liver will be removed, weighed, and representative samples o f left lateral, right median, and right lateral lobes o f the liver and any macroscopic lesions o f the liver will be collected and preserved in zinc formalin. After fixation, each sample o f liver will be embedded in paraffin, and the paraffin blocks will be shipped to: Sandra R. Eldridge, PhD Pathology Associates International 15 Worman's Mill Court, Suite I Frederick, Maryland 21701 Telephone No.: 301.663.1644, ext. 2201 Facsimile No: 301.663.8994 Proliferation cell nuclear antigen (PCNA) evaluation will be done on the samples. Results will be provided for inclusion in the final report. 3MEnvironmental Laboratory Page 33 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 ________________________________________________________________________________ _________________ Page 13 Palmitoyl-CoA Oxidase Tissue Collection and Analyses A sample (approximately 500 mg) o f the right lateral lobe o f the liver will also be collected from each animal and flash-frozen in liquid nitrogen. The liver tissue will be stored in a freezer set to maintain -60 to -80C until analyzed by Covance for palmitoyl-CoA oxidase activity. Animal Disposition Animals will be discarded after liver collection. Termination Unscheduled Sacrifices and Deaths Necropsies will be done. Animals to be sacrificed will be anesthetized with sodium pentobarbital, weighed, and exsanguinated. A blood film will be taken as part o f the necropsy procedure for sacrificed animals. Scheduled Sacrifices Interim Sacrifice After at least 78 weeks o f treatment, 10 animals/sex from Groups 1,4, and 5 will be fasted overnight, anesthetized with sodium pentobarbital, weighed, exsanguinated, and necropsied. A blood film will be taken as part o f the necropsy procedure. Terminal Sacrifice After at least 104 weeks o f treatment, the remaining animals in Groups 1 through 5 will be fasted overnight, then anesthetized with sodium pentobarbital, weighed, exsanguinated, and necropsied. A blood film will be taken as part o f the necropsy procedure. Recovery Sacrifice After at least 78 weeks o f treatment and 26 weeks without treatment, the remaining animals in Groups 6 and 7 will be fasted overnight, then anesthetized with sodium pentobarbital, weighed, exsanguinated, and necropsied. A blood film w ill be taken as part o f the necropsy procedure. 3MEnvironmental Laboratory Page 34 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Postmortem Procedures Covance 6329-212 ________ Page 14 Necropsy The necropsy will include an examination o f the external features o f the carcass; all external body orifices; the abdominal, thoracic, and cranial cavities; organs; and tissues. Organ Weights At the scheduled sacrifices, the following organs (when present) will be weighed; paired organs will be weighed separately: adrenal (2) brain kidney (2) liver lung ovary (2) spleen testes thyroid (2) with parathyroid uterus with cervix Organ-to-body weight percentages and organ-to-brain weight ratios will be calculated. Bone Marrow Smear From the femur o f each animal at scheduled sacrifices only; made but not examined Tissue Preservation The following tissues (when present) from each animal will be preserved in 10% neutral-buffered formalin: 3MEnvironmental Laboratory Page 35 . 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Covance 6329-212 Page 15 adrenal (2) pancreas brain pituitary cecum prostate cervix rectum colon salivary gland [m andibular (2)] duodenum sciatic nerve epididymis (2) seminal vesicle (2) esophagus skeletal muscle (thigh) eye (2) skin fem ur with bone m arrow (articular surface spinal cord (cervical, thoracic, and o f the distal end) lumbar) H arderian gland spleen heart sternum with bone m arrow ileum sto m ach jejunum testis (2) kidney (2) thymus lesions thyroid (2) with parathyroid liver trachea lung w ith mainstem bronchi urinary bladder .. lym ph n o d e (m esenteric) uterus m am m ary gland (females only) vagina ovary (2) Histopathology Tissues (as appropriate) from each animal in Groups 1 ,5 , and 7 and from each animal that dies o r is sacrificed at an unscheduled interval will be em bedded in paraffin, sectioned, stained w ith hem atoxylin and eosin, and examined microscopically. M acroscopic lesions will also be examined microscopically from each anim al in G roups 2 ,3 ,4 , and 6. Reports O ne copy o f each draft report w ill be sent to the Sponsor. The report will include the following information: 3M E nvironm ental Laboratory Page 36 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Experimental Design and Methods Covance 6329-212 ________ Page 16 Results dose analyses mortality clinical observations body weights body weight changes food consumption test material consumption clinical pathology results palmitoyl CoA oxidase activities macroscopic observations microscopic observations cell proliferation assessments (provided by the Sponsor's designee) Statistical Evaluation body weights body weight changes food consumption survival rates clinical pathology values palmitoyl CoA oxidase activities neoplastic and nonneoplastic lesions Statistical methods will be those presented in Attachments N os. 1 and 2. For each sex, Groups 2 through 7 will be compared to Group 1 (Control). At the end o f 1 year after issuance o f the audited draft report, if no requested revisions or instructions to finalize have been communicated by the Sponsor, then the audited draft report will be considered 'final' and issued as the final report, signed by the study director, and submitted to the Sponsor. Any modifications or changes to the audited draft report requested 1 year after issuance will be performed at additional cost to the Sponsor. . Two copies o f the signed final report (one unbound and one bound) will be sent to the Sponsor. 3MEnvironmental Laboratory Page 37 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 ________ Page 17 Record Retention All raw data, documentation, records, protocol, specimens, and final report generated as a result o f this study, including those items listed below, will be archived in the storage facilities o f Covance-Madison for a period o f 1 year following submission o f the final report to the Sponsor. A ll raw data stored on magnetic media, the protocol and protocol amendments, study correspondence, and the original report will be retained by Covance. One year after submission o f the final report, all of the aforementioned materials will be sent to the Sponsor, and a return fee will be charged. The Sponsor may elect to have the materials retained in the Covance archives for an additional period o f time, and Covance will charge a storage fee. If the Sponsor chooses to have Covance dispose o f the materials, a disposal fee will be charged. protocol and protocol amendments dose preparation records in-life records animal receipt acclimation animal room maintenance randomizations dose administration clinical observations body weights food consumption sample collection clinical pathology records anatomical pathology records statistical analyses study correspondence tissue specimens (wet and in paraffin) blood, bone marrow, and tissue slides final report (original signed copy) 3MEnvironmental Laboratory Page 38 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 ________________________________________________ .______________________ Page 18 The following supporting records will be retained at Covance-Madison but will not be archived with the study data. feed analysis records water analysis records animal room environment records refrigerator and freezer temperature records room temperature records for test material storage instrument calibration and maintenance records PCNA evaluation data and paraffin blocks and tissue slides for PCNA will be retained by Pathology Associates International. Serum samples sent to the Sponsor will be retained by the Sponsor 3MEnvironmental Laboratory Page 39 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 PROTOCOL APPROVAL Covance 6329-212 ________ Page 19 Andrew M. Seacat, PhD Study Monitor 3M Covance Laboratories Inc. 3MEnvironmental Laboratory Page 40 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Attachment No. 1 Covance 6 3 2 9 -2 1 2 ___________ P a g e 2 0 Statistical Analyses The statistical methods that will be used are described below. Only data collected on or after the first day o f treatment will be analyzed statistically. One-way analysis o f variance [ANOVA (Winer, 1971)] will be used (if applicable) to analyze body weights; body weight changes; food consumption; clinical chemistry and hematology values (except blood cell morphology); urine specific gravity, pH, and volume; urine chemistry values; palmitoyl CoA oxidase activities; organ weights; organ-to-body weight percentages; and organ-to-brain weight ratios. Levene's test (Levene, 1960) will be done to test for variance homogeneity. In the case o f heterogeneity of variance at p < 0.05, transformations will be used to stabilize the variance. ANOVA will be done on the homogeneous or transformed data. If the ANOVA is significant, Dunnett's t-test (Dunnett, 1964) will be used for pairwise comparisons between treated and control groups. If the ANOVA shows significance for body weights at Week 1, one-way analysis o f covariance [ANCOVA (Winer, 1971)] will be used to analyze body weights, with initial body weights as the covariate, using untransformed data. If the ANCOVA is significant, least squares means t-test (Winer, 1971) will be used for pairwise comparisons between treated and control groups. Group comparisons will be evaluated at the 5.0%, two-tailed probability leveL References Dunnett, C. W,, "New Tables for Multiple Comparisons with a Control," Biometrics. 2(1:482-491 (1964). Levene, H., "Robust Tests for Equality of Variances," Contributions to Probability and Statistics, (eds.) I. Olkin et a l, Ch. 25, pp. 278-292, Stanford University Press: Stanford, California (1960). Winer, B. J,, Statistical Principles in Experimental Design. Second Ed., McGraw-Hill: New York, New York (1971b). 3MEnvironmental Laboratory Page 41 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Attachment No. 2 Covance 6329-212 _________ Page 21 Adjusted survival data are analyzed by the National Cancer Institute (NCI) lifetable package (Thomas, 1977). The tests include: Graphical (Kaplan-Meier product-limit estimation curves), Cox-Tarone binary regression methods for trend and heterogeneity, and Gehan-Breslow nonparametric methods for trend and heterogeneity. Non-neoplastic lesions. Non-neoplastic lesions are analyzed by the Cochran-Armitage test for trend and the Fisher-Irwin exact test for heterogeneity (Thakur, 1985). Neoplastic lesions. Incidental tumors are analyzed by Dinse-Lagakos logistic prevalence methods (Dinse, 1983) for trend and heterogeneity. Rapidly lethal and palpable tumors are analyzed in the same manner as survival In the cases where the study pathologist can assign particular occult neoplastic lesions as the cause o f death in the animals, such information will be taken into appropriate analysis as in the IARC document (Peto et al, 1980). References Thomas, D. G., Breslow, N., and Gart, J. J., "Trend and Homogeneity Analyses of Proportions and Life Table Data," Comput. Biomed. Res.. 10:373-381 (1977). Thakur, A . K ., Berry, K. J., and Mielke, Jr., P. W ., "A FO R TRA N Program fo r Testing T rend and H om ogeneity in Proportions," C om put. P ro er. B iom ed.. 12:229-233 (1985). Dinse, G. E., and Lagakos, S. W., "Regression Analysis o f Tumor Prevalence Data," J. Roy. Stat. Soc. Series C (AppL S tall. 32:236-248 (1983). Peto, R., Pike, M. C., Day, N. E., Gray, R. G., Lee, P. N., Parish, S., Peto, J., Richards, S., and Wahrendorf, J., "Guidelines for Simple Sensitive Significance Tests for Carcinogenic Effects in Long-term Animal Experiments, in Long-term and Short-term Screening Assays for Carcinogens: A Critical Appraisal," Lvon: International Agency for Cancer Research, pp. 3 11-426 (1980). 3MEnvironmental Laboratory Page 42 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 C O V /W iC E> THE DEVELOPMENT SERVICES COMPANY PROTOCOL AMENDMENT NO. 1 Covance 6329-212 104-Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats Sponsor: Study Monitor: Testing Facility: Study Director: 3M, St. Paul, Minnesota Andrew M. Seacat, PhD Covance Laboratories Inc., Madison, Wisconsin Peter J. Thomford, PhD This amendment modifies the following portions of the protocol: Effective January 21,1998 1. Page 4, Animals, Strain. To correct the strain of the animals used in this study, delete the text in this section and replace with the following: Crl:CD(SD)IGS BR Effective February 6,1998 2. Page 7, Group Designations and Dietary Levels, Footnote C. To reflect the decision to delay the Week 3 collection, delete the text in this section and replace with the following: c Five animals/sex/group in Groups 1 through 5 will be sacrificed during Weeks 4 and 14 for hepatocellular proliferation rate measurements and biochemical analyses (palmitoyl-CoA oxidation). 3MEnvironmental Laboratory Page 43 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 Protocol Amendment No. 1 _____________ Page 2 3. Page 12, Hepatocellular Proliferation and Biochemical Analyses, Frequency and Number of Animals. To reflect the decision to delay the Week 3 collection, delete the text in this section and replace with the following: Five animals/sex/group in Groups 1 through 5 during Weeks 4 and 14 4. Page 13-, Hepatocellular Proliferation and BiochemicaLAnalysesT^To reflect the decision to performjmlochondrial^Sy^Sr^dtrtfie following sectknTafier "Palmitoyl-CoA Oxidase Tissue CpfleCfion and AnalysesJI^"^ Mitochondrial Analyses At the WekAcollection, a sam ple^pproxim atelvj^g) from the remaining portiptfof the liyefw ill bepollected from sekotd animals. Samples will be placed wet ice ana transferred to the Sponscjr'for mitochondrial analysis. Results will be rerouted separately by the Sponsc Effective February 17,1998 5. Page 12. To reflect the decision to collect serum samples for possible future analysis, add the following section after "Clinical Pathology". Serum Analyses Frequency and Number of Animals Five animals/sex/group in Groups 1 through 5 during Weeks 4 and 14 (animals selected for hepatocellular proliferation and biochemical analyses); five animals/sex/group from Groups 1,4, and 5 (from animals selected for interim sacrifice) after at least 78 weeks of treatment; and five animals/sex/group from Groups 1 through 5 at the terminal sacrifice Method of Collection Animals will be fasted overnight; blood (approximately 2 mL) will be collected from a jugular vein. Samples will be collected without anticoagulant. 3MEnvironmental Laboratory Page 44 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 Protocol Amendment No. 1 ________________ Page 3 Sample Handling Blood samples will be allowed to clot at room temperature and centrifuged. Serum samples will be harvested and stored in a freezer set to maintain -60 to -80C. Samples will be packed on dry ice and shipped to Kris J. Hansen, PhD, 3M Environmental Technology and Safety Services. Samples will be retained by the Sponsor for possible future analysis. 6. Page 13, Hepatocellular Proliferation and Biochemical Analyses. To reflect the decision to collect liver samples for possible future analyses, add the following section after "Palmitoyl-CoA Oxidase Tissue Collection and Analyses": Additional Liver Sample Collection At the collections during Weeks 4 and 14, the remaining liver will be stored in a freezer set to maintain -60 to -80C. Samples will be packed on dry ice and shipped to Kris J. Hansen, PhD, 3M Environmental Technology and Safety Services. Samples will be retained by the Sponsor for possible future analysis. 7. Page 14, Postmortem Procedures. To reflect the decision to collect liver samples for possible future analyses, add the following section after "Bone Marrow Smear": Additional Liver Sample Collection A portion of the liver will be collected from five animals/sex/group from Groups 1, 4, and 5 at the interim sacrifice and from five animals/sex/group from Groups 1 through 5 at the terminal sacrifice and stored in a freezer set to maintain -60 to -80C. Samples will be packed on dry ice and shipped to Kris J. Hansen, PhD, 3M Environmental Technology and Safety Services. Samples will be retained by the Sponsor for possible future analysis. 8. Page 17, Record Retention, Paragraph 4. To indicate that frozen liver samples sent to the Sponsor will be retained by the Sponsor, delete this paragraph and replace with the following: 3MEnvironmental Laboratory Page 45 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 Protocol Amendment No. 1 __________________________________________________________________________________________________P ag e 4 Frozen liver samples and serum samples sent to the Sponsor will be retained by the Sponsor. Effective March 13,1998 9. Page 7, Group Designations and Dietary Levels. To reflect the decision to sacrifice five animals/sex/group from Groups 1 and 5 and to terminate the remaining animals in Group 5 and 7 during Week 8, delete the text in this section and replace with the following: Group Number of Animals Male Female Dietary Levels (ppm NEtFOSE)8 1 (Control)"'0'"'6 2 (Low)0 3 (Mid)c 4 (Mid-High)c'e 5 (High)0-" 6 (Mid-High R ecovery/ 7 (High Recovery)" 70 60 60 70 70 40 40 70 60 60 70 70 40 40 0 3 30 100 300 100 300 a T-6316 is 98.1% n-ethyl perfluorooctanesulfonamido ethanol (NEtFOSE); dose levels are expressed as ppm of NEtFOSE. b The control animals will receive the basal diet only. c Five animals/sex/group in Groups 1 through 5 will be sacrificed during Week 4 and five anim als/sex/group in G roups 1 through 4 w ill be sacrificed during Week 14 for hepatocellular proliferation rate measurements and biochemical analyses (palmitoyl-CoA oxidation). d Five animals/sex/group in Groups 1 and 5 will be sacrificed during Week 8; the remaining animals in Groups 5 and 7 will be sacrificed and discarded during Week 8. e Ten animals/sex/group in Groups 1 and 4 will be designated as interim sacrifice animals and will be sacrificed after at least 78 weeks o f treatment, f Animals in Group 6 will be treated for at least 78 weeks, then treatment will be discontinued, and the animals will be observed for reversibility, persistence, or delayed occurrence of toxic effects for at least 26 weeks posttreatment. During recovery, the animals will receive basal diet only. 3MEnvironmental Laboratory Page 46 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 Protocol Amendment No. 1 ___________________________________________________________ _______________ Page 5 10. Page 7, Dosing Procedures, Method of Administration. To reflect the decision to terminate Groups 5 and 7 during Week 8, delete the text in this section and replace with the following: Dietary. Animals in Groups 1 through 4 will receive test diet for at least 104 weeks. Animals in Group 6 will receive test diet for 78 weeks only. Animals in Groups 5 and 7 will receive test diet for at least 7 weeks. 11. Page 9, Observation of Animals, Body Weights. To reflect the decision to record body weights before sacrifice during Week 8, add the following to this section: Body weights will also be recorded for all animals in Groups 5 and 7 before sacrifice during Week 8. 12. Page 10, Clinical Pathology, Frequency and Number of Animals, Scheduled Collections. To reflect the decision to collect clinical pathology samples from animals in Groups 1 and 5 during Week 8 and to terminate Groups 5 and 7 during Week 8, delete the text in this section and replace with the following: Hematology, clinical chemistry, urinalysis, and urine chemistry will be done on five animals/sex/group from Groups 1 and 5 during Week 8. Hematology, clinical chemistry, urinalysis, urine chemistry, and serum sampling will be done on 10 animals/sex/group in Groups 1 through 4 during Weeks 14, 27, and 53. A blood film will be made and held for possible future examination for animals at scheduled sacrifices after at least 78 and 104 weeks of treatment. 13. Page 12, Serum Analyses, Frequency and Number of Animals. To reflect the decision to collect serum samples from animals in Groups 1 and 5 during Week 8 and to terminate Groups 5 and 7 during Week 8, delete the text in this section and replace with the following: 3MEnvironmental Laboratory Page 47 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 ' LRN-U2103 Covance 6329-212 Protocol Amendment No. 1 ____________________________________________________________________ _____________Page 6 Five animals/sex/group in Groups 1 through 5 during Week 4 (animals selected for hepatocellular proliferation and biochemical analyses); five animals/sex/group in Groups 1 and 5 during Week 8; five animals/sex/group in Groups 1 through 4 during Week 14 (animals selected for hepatocellular proliferation and biochemical analyses); five animals/sex/group from Groups 1 and 4 (from animals selected for interim sacrifice) after at least 78 weeks of treatment; and five animals/sex/group from Groups 1 through 4 at the terminal sacrifice 14. Page 12, Hepatocellular Proliferation and Biochemical Analyses, Frequency and Number of Animals. To reflect the decision to perform analyses on livers from animals in Groups 1 and 5 during Week 8 and to terminate Groups 5 and 7 during Week 8, delete the text in this section and replace with the following: Five animals/sex/group in Groups 1 through 5 during Week 4; five animals/sex/group in Groups 1 and 5 during Week 8; and five animals/sex/group in Groups 1 through 4 during Week 14 15. Page 13, Hepatocellular Proliferation and Biochemical Analyses, Additional Liver Sample Collection. To reflect the decision to collect livers from animals in Groups 1 and 5 during Week 8, delete the text in this section and replace with the following: At the collections during Weeks 4, 8, and 14, a portion of the remaining liver will be stored in a freezer set to maintain -60 to -80C. Samples will be packed on dry ice and shipped to Kris J. Hansen, PhD, 3M Environmental Technology and Safety Services. Samples will be retained by the Sponsor for possible future analysis. 16. Page 12, Hepatocellular Proliferation and Biochemical Analyses, Cell Proliferation Tissue Collection and Immunohistochemical Evaluation, Paragraph 1. To reflect the decision to collect only the left lateral lobe of the liver at the Week 8 and 14 collections, delete the text in this paragraph and replace with the following: 3MEnvironmental Laboratory Page 48 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 Protocol Amendment No. 1 _________________________________________ ,_____ ________________________ __________ Page 7 At each interval, animals will be fasted overnight, anesthetized with sodium pentobarbital, weighed, and exsanguinated. The abdominal cavity o f each animal will be opened, and the liver will be removed and weighed. At the W eek 4 collection, representative samples o f left lateral, right median, and right lateral lobes of the liver and any macroscopic lesions o f the liver will be collected and preserved in zinc formalin. At the Week 8 and 14 collections, representative samples of the left lateral lobe o f the liver and any macroscopic lesions o f the liver will be collected and preserved in zinc formalin. 17. Page 13, Termination, Scheduled Sacrifices. To reflect the decision to sacrifice five animals/sex/group from Groups 1 and 5, to terminate the remaining animals in Groups 5 and 7 during Week 8, and to sacrifice five animals/sex/group from Groups 1 through 4, delete the text in this section and replace with the following: Interim Sacrifices During Week 8, five animals/sex/group from Groups 1 and 5 will be fasted overnight, bled for clinical pathology and serum analyses, anesthetized with sodium pentobarbital, weighed, exsanguinated, and necropsied. Liver samples will be collected for palimitoyl CoA, PCNA, and frozen samples for possible analysis. The remaining animals in Groups 5 and 7 will be euthanatized with carbon dioxide and discarded without necropsy. During Week 14, five animals/sex/group from Groups 1 through 4 will be fasted overnight, bled for clinical pathology and serum analyses, anesthetized with carbon dioxide, weighed, exsanguinated, and necropsied. Liver samples will be collected for palimitoyl CoA, PCNA, and frozen samples for possible analysis. After at least 78 weeks of treatment, five animals/sex/group from Group 1 and 10 animals/sex from Group 4 will be fasted overnight, anesthetized with carbon dioxide, weighed, exsanguinated, and necropsied. A blood film will be taken as part of the necropsy procedure. 3MEnvironmental Laboratory Page 49 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 _________________________________ Covance 6329-212 Protocol Amendment No. 1 .. _________________ ______________ Page 8 Terminal Sacrifice After at least 104 weeks o f treatment, the remaining animals in Groups 1 through 4 will be fasted overnight, then anesthetized with carbon dioxide, weighed, exsanguinated, and necropsied. A blood film will be taken as part o f the necropsy procedure. Recovery Sacrifice After at least 78 weeks o f treatment and 26 weeks without treatment, the remaining animals in Group 6 will be fasted overnight, then anesthetized with carbon dioxide, weighed, exsanguinated, and necropsied. A blood film will be taken as part o f the necropsy procedure. 18. Page 14, Postm ortem Procedures, A dditional Liver Sam ple C ollection. To reflect the decision to sacrifice five animals/sex/group from Groups 1 and 5 and to terminate the remaining animals in Group 5 and 7 during W eek 8, delete the text in this section and replace with the following: A portion of the liver will be collected from five animals/sex/group from Groups 1 and 4 at the Week 79 sacrifice and from five animals/sex/group from Groups 1 through 4 at the terminal sacrifice and stored in a freezer set to maintain -60 to -80C . Samples will be packed on dry ice and shipped to Kris J. Hansen, PhD, 3M Environmental Technology and Safety Services. Samples will be retained by the Sponsor for possible future analysis. . 19. Page 15, Postm ortem Procedures, H istopathology. To reflect the decision to terminate Groups 5 and 7 early, to examine tissues from animals sacrificed during Weeks 8 and 14, and to examine tissues from Groups 4 and 6, delete the text in this section and replace with the following: Tissues (as appropriate) from each animal in Groups 1, 4, and 6 sacrificed at the Week 79 interim sacrifice and terminal sacrifice and from each animal that dies or is sacrificed at an unscheduled interval will be embedded in paraffin, sectioned, stained with hematoxylin and eosin, and examined microscopically. Adrenals, brain, eyes, kidneys, liver, mesenteric lymph node, pancreas, spleen, testes, and 3MEnvironmental Laboratory Page 50 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 Protocol Amendment No. 1 _______________________________________________________ ________________ Page 9 ovaries from the animals necropsied at Weeks 8 and 14 interim sacrifice will also be embedded in paraffin, sectioned, stained with hematoxylin and eosin, and examined microscopically. Macroscopic lesions will also be examined microscopically from each animal in Groups 2 and 3 sacrificed at terminal necropsy. 20. Page 16, R eports, R esults. To reflect the decision to include results from Covance 6329-228 as an appendix to this report, add the following: The study report for Covance 6329-228 will be included as an appendix to this report. E ffective M arch 30,1998 21. Page 12, H epatocellular Proliferation and Biochem ical Analyses, Cell Proliferation Tissue C ollection and Inununohistochem ical E valuation, Paragraph 3. To include the microscopic examinations o f liver sections stained with hematoxylin and eosin and to indicate that evaluations will be done on the left lateral lobe o f the liver only, delete the text in this section and replace with the following: Proliferation cell nuclear antigen (PCNA) evaluation will be done on the samples (left lateral lobe only). In addition, sections o f the left lateral lobe o f the liver will be stained with hematoxylin and eosin and examined microscopically. Results will be provided for inclusion in the final report. 3MEnvironmental Laboratory Page 51 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 AMENDMENT APPROVAL Covance 6329-212 Protocol Amendment No. 1 _______________ Page 10 (kJkbj % Amndrreew M. Seacat, PhD Study Monitor 3M %uh Date 3MEnvironmental Laboratory Page 52 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 CO V/H i^ir^ THE DEVELOPMENT SERVICES COMPANY PROTOCOL AMENDMENT NO. 2 Covance 6329-212 104-Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats Sponsor: Study Monitor: Testing Facility: Study Director: 3M, St. Paul, Minnesota Andrew M. Seacat, PhD Covance Laboratories Inc., Madison, Wisconsin Peter J. Thomford, PhD This amendment modifies the following portions o f the protocol: Effective April 23,1998 1. Page 13, Term ination, Unscheduled Sacrifices and Deaths. To reflect the decision to anesthetize animals with carbon dioxide for unscheduled sacrifices, delete the text in this section and replace with the following: Necropsies w ill be done. Animals to be sacrificed will be anesthetized, weighed, and exsanguinated. Animals sacrificed before Week 13 will be anesthetized with sodium pentobarbital, animals sacrificed during or after Week 13 will be anesthetized with carbon dioxide. A blood film will be taken as part o f the necropsy procedure for sacrificed animals. Effective April 28,1998 2. Page 2, Alternate Study M onitor. To include alternate study monitor in the protocol, add the following after "Study Monitor:" 3MEnvironmental Laboratory Page 53 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Alternate Study Monitor Marvin T. Case, DVM, PhD 3M Toxicology Services Telephone No.: 612.733.5180 Facsimile No.: 612.733.1773 Covance 6329-212 Protocol Amendment No. 2 ________________ Page 2 3. Page 7, Group Designations and Dietary Levels. To reflect the decision to begin recovery after 52 weeks o f treatment and to change the Week 79 interim sacrifice to Week 53, delete the text in this section and replace with the following: Group Number o f Animals Male Female Dietary Levels (ppm NEtFOSE)* 1 (Control)"0"'6 2 (Low)c 3 (M id)c 4 (M id-High)0'6 5 (High)c d 6 (M id-High Recovery)* 7 (High Recovery)" 70 60 60 70 70 40 40 70 0 60 3 60 30 70 100 70 '300" 40 100 40 ... 300 a T -6316 is 98.1% n-ethyl perfluorooctanesulfonamido ethanol (NEtFOSE); dose levels are expressed as ppm o f NEtFOSE. b The control animals will receive the basal diet only. c Five animals/sex/group in Groups 1 through 5 will be sacrificed during Week 4, and five animals/sex/group in Groups 1 through 4 will be sacrificed during W eek 14 for hepatocellular proliferation rate measurements and biochemical analyses (palmitoyl-CoA oxidation). d Five animals/sex/group in Groups 1 and 5 will be sacrificed during Week 8; the remaining animals in Groups 5 and 7 will be sacrificed and discarded during W eek 8. e Ten animals/sex/group in Groups 1 and 4 will be designated as interim sacrifice animals and will be sacrificed after at least 52 weeks o f treatment, f Animals in Group 6 will be treated for at least 52 weeks, then treatment will be discontinued, and the animals will be observed for reversibility, persistence, or delayed occurrence of toxic effects for at least 52 weeks posttreatment. During recovery, the animals will receive basal diet only. 3MEnvironmental Laboratory Page 54 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 Protocol Amendment No. 2 ______________________________________________________________________ Page 3 4. Page 7, Dosing Procedures, Method of Administration. To reflect the decision to begin recovery after 52 weeks o f treatment, delete the text in this section and replace with the following: Dietary. Animals in Groups 1 through 4 will receive test diet for at least 104 weeks. Animals in Group 6 will receive test diet for 52 weeks only. Animals in Groups 5 and 7 will receive test diet for at least 7 weeks. 5. Page 10, Clinical Pathology, Frequency and Number of Animals, Scheduled Collections, Paragraph 2. The Week 79 interim sacrifice will be moved to W eek 53, therefore blood films will be prepared from animals sacrificed after 52 weeks o f treatment. To reflect this decision, delete the text in this paragraph and replace with the following: A blood film will be made and held for possible future examination for animals at scheduled sacrifices after at least 52 and 104 weeks o f treatment. 6. Page 12, Serum Analyses, Frequency and Number of Animals. The Week 79 interim sacrifice will be moved to Week 53, therefore serum samples will be collected from animals sacrificed after 52 weeks o f treatment. To reflect this decision, delete the text in this section and replace with the following: Five animals/sex/group in Groups 1 through 5 during Week 4 (animals selected for hepatocellular proliferation and biochemical analyses); five animals/sex/group in Groups 1 and 5 during Week 8; five animals/sex/group in Groups 1 through 4 during Week 14 (animals selected for hepatocellular proliferation and biochemical analyses); five animals/sex/group from Groups 1 and 4 (from animals selected for interim sacrifice) after at least 52 weeks o f treatment; and five animals/sex/group from Groups 1 through 4 at the terminal sacrifice. 7. Page 13, Termination, Scheduled Sacrifices. To reflect the decision to move the Week 79 interim sacrifice to Week 53 and to begin recovery after 52 weeks of treatment, delete the text in this section and replace with the following: 3MEnvironmental Laboratory Page 55 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 Protocol Amendment No. 2 ________________ Page 4 Interim Sacrifices During Week 8, five animals/sex/group from Groups 1 and 5 will be fasted overnight, bled for clinical pathology and serum analyses, anesthetized with sodium pentobarbital, weighed, exsanguinated, and necropsied. Liver samples will be collected for palimitoyl CoA analysis and PCNA evaluation; additional liver samples will be frozen for possible analysis. The remaining animals in Groups 5 and 7 will be euthanatized with carbon dioxide and discarded without necropsy. During Week 14, five animals/sex/group from Groups 1 through 4 w ill be fasted overnight, bled for clinical pathology and serum analyses, anesthetized with carbon dioxide, weighed, exsanguinated, and necropsied. Liver samples w ill be collected for palimitoyl CoA analysis and PCNA evaluation; additional liver samples will be frozen for possible analysis for possible analysis. After at least 52 weeks o f treatment, five animals/sex/group from Group 1 and 10 animals/sex from Group 4 will be fasted overnight, anesthetized with carbon dioxide, weighed, exsanguinated, and necropsied. Term inal Sacrifice After at least 104 weeks o f treatment, the remaining animals in Groups 1 through 4 will be fasted overnight, then anesthetized with carbon dioxide, weighed, exsanguinated, and necropsied. A blood film will be taken as part o f the necropsy procedure. Recovery Sacrifice After at least 52 weeks o f treatment and 52 weeks without treatment, the remaining animals in Group 6 will be fasted overnight, then anesthetized with carbon dioxide, weighed, exsanguinated, and necropsied. A blood film will be taken as part of the necropsy procedure. 8. Page 14, Postmortem Procedures, Organ W eights. To reflect the decision to record organ weights at the Week 8, 14, and 53 interim sacrifices only, delete the text in this section and replace with the following: 3MEnvironmental Laboratory Page 56 3M,Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 Protocol Amendment No. 2 ________________________________________________________________________________________________ P ag e 5 At the Week 8, 14, and 53 interim sacrifices, the following organs (when present) will be weighed; paired organs will be weighed separately: adrenal (2) brain kidney (2) liver lung ovary (2) spleen testis (2) thyroid (2) with parathyroid uterus with cervix Organ-to-body weight percentages and organ-to-brain weight ratios will be calculated. 9. Page 14, Postmortem Procedures, Additional Liver Sample Collection. The Week 79 interim sacrifice will be moved to Week 53, therefore liver samples will be collected from animals sacrificed after 52 weeks oftreatment. To reflect this decision, delete the text in this section and replace with the following: A portion of the liver will be collected from five animals/sex/group from Groups 1 and 4 at the Week 53 sacrifice and from five animals/sex/group from Groups 1 through 4 at the terminal sacrifice and stored in a freezer set to maintain -60 to -80C. Samples will bepacked on dry ice and shipped to Kris J. Hansen, PhD, 3M Environmental Technology and Safety Services. Samples will be retained by the Sponsor for possible future analysis. 10. Page 15, Postmortem Procedures, Histopathology, Paragraph 1. The Week 79 interim sacrifice will be moved to Week 53, therefore histopathology will be done for animals sacrificed after 52 weeks of treatment. To reflect this decision, delete the text in this section and replace with the following: 3MEnvironmental Laboratory Page 57 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 Protocol Amendment No. 2 _________________________________________________________________________________ Page 6 Tissues (as appropriate) from each animal in Groups 1,4, and 6 sacrificed at the Week 53 interim sacrifice and terminal sacrifice and from each animal that dies or is sacrificed at an unscheduled interval will be embedded in paraffin, sectioned, stained with hematoxylin and eosin, and examined microscopically. Adrenals, brain, eyes, kidneys, liver, mesenteric lymph node, pancreas, spleen, testes, and ovaries from the animals necropsied at the Week 8 and 14 interim sacrifices will also be embedded in paraffin, sectioned, stained with hematoxylin and eosin, and examined microscopically. 11. Page 15, Reports, Paragraph 1. To reflect the decision to provide unaudited summary reports after the Week 14 and 53 interim sacrifices, delete the text in this paragraph and replace with the following: After the Week 14 and 53 interim sacrifices, unaudited summary reports will be sent to the Sponsor. The summary reports will include a briefdescription of methods and results and summarytables of in-life data, clinical pathology data, and anatomical pathology data. After completion of the study, one copy of the draft report will be sent to the Sponsor. The draft report will include the following information: Effective May 15,1998 12. Page 12, Seram Analyses, Method of Collection. To reflect the decision to increase the volume collected for serum analyses at the Week 53 and 105 sacrifices, delete the text in this section and replace with following: Animals will be fasted overnight; blood (approximately 2 mL at the Week 4, 8 and 14 sacrifices, approximately 3 mL at the Week 53 and 105 sacrifices) will be collected from ajugular vein. Samples will be collected without anticoagulant. 3MEnvironmental Laboratory Page 58 3MJMedical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 AMENDMENT APPROVAL Covance 6329-212 Protocol Amendment No. 2 ________________ Page 7 /J 'a aA sJ Andrew M. Seacat, PhD Study Monitor 3M A/rVv~ 3MEnvironmental Laboratory Page 59 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 COVMT' THE DEVELOPMENT SERVICES COMPANY PROTOCOL AMENDMENT NO. 3 Covance 6329-212 104-Week Dietary Carcinogenicity Study with Narrow Range (98.1 %) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats Sponsor: Study Monitor: Testing Facility: Study Director: 3M, St. Paul, Minnesota Andrew M. Seacat, PhD Covance Laboratories Inc., Madison, Wisconsin Peter J. Thomford, PhD This amendment modifies the following portions ofthe protocol: Effective January 21,1998 1. Page 4. To include the vehicle used to dissolve the test material before mixing with the diet, add the following section. Vehicle Identification Acetone Lot Numbers The lot numbers will be maintained in the raw data Purity On file with the manufacturer Stability On file with the manufacturer Storage Conditions At room temperature 3MEnvironmental Laboratory Page 60 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 _P_r_o_t_oc_o_l_A_m__e_n_d_m_e_n_tPNaog.e32 Characteristics Information on synthesis methods, composition, or other characteristics that define the vehicle is on file with the manufacturer. 2. Page 16, Reports, Results. To include organ weights as a result to be reported, add "organ weights" to this section. 3. Page 16, Reports, Statistical Evaluation. To include statistical evaluation of organs weights, add "organ weights (Weeks 8, 14, and 53 interim sacrifices only)" Effective April 28,1998 4. Page 7, Group Designations and Dietary Levels, Footnote e. To correct the number of Group 1 animals to be sacrificed at the Week 53 interim sacrifice, delete this sentence and replace with the following: e Five animals/sex in Group 1 and 10 animals/sex in Group 4 will be designated as interim sacrifice animal.; and will be sacrificed after at least 52 weeks of treatment. Effective June 30,1998 5. Page 8, Dosing Procedure, Retention Samples. To reflect the decision to send retention samples ofcontrol diet to the Sponsor, delete the text in this section and replace with the following: Samples (approximately 100 g) will be taken from each dose preparation during the in-life phase and stored at room temperature. Unless used for analyses, retention samples from the treated groups will be discarded at least 1 month after completion of the in-Hfe phase. Samples from control diets prepared for Weeks 24 and before will be shipped to: 3MEnvironmental Laboratory Page 61 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Kris J. Hansen, PhD 3M Environmental Technology and Safety Services 935 BushAvenue Building 2-3E-09 St. Paul, Minnesota 55133-3331 Telephone No.: 651.778.6018 Facsimile No.: 651.778.6176 Covance 6329-212 Protocol Amendment No. 3 ________________ Page 3 Effective July 20,1998 6. Page 2, Study M onitor and Alternate Study Monitor. To indicate the change in the area code, delete the text in these sections and replace with the following: Study Monitor Andrew M. Seacat, PhD 3M Telephone No.: 651.575.3161 Facsimile No.: 651.733.1773 v '' Alternate Study Monitor Marvin T. Case, DVM , PhD 3M Toxicology Services Telephone No.: 651.733.5180 Facsimile No.: 651.733.1773 7. Page 4, Disposition of Test Material. To indicate the change in the area code, delete the text in these section and replace with the following: After authorization from the Sponsor, anyremaining test material will be returned to: Andrew M. Seacat, PhD 3M Toxicology Services Building 220-2E-02,3M Center St. Paul, Minnesota 55144-1000 Telephone No.: 651.575.3161 Facsimile No.: 651.733.1733 3MEnvironmental Laboratory Page 62 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 Protocol Amendment No. 3 __________________________________________________________________________ Page 4 8. Page 12, Clinical Pathology, Serum Samples. To indicate the change in the area code, delete the text in these section and replace with the following: Serum not used for clinical chemistry will be stored in a freezer set to maintain -60 to -80 C. Samples will be packed on dry ice and shipped to: Kris J. Hansen, PhD 3M Environmental Technology and Safety Services 935 Bush Avenue Building 2-3E-09 St Paul, Minnesota 55133-3331 Telephone No.: 651.778.6018 Facsimile No.: 651.778.6176 Samples will be retained by the Sponsor for possible future analysis. 3MEnvironmental Laboratory Page 63 . 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 AMENDMENT APPROVAL Covance 6329-212 Protocol Amendment No. 3 _______________ PageS Andrew M. Seacat, PhD Study Monitor 3M 6> /tV /ff Date 3ateX / 3MEnvironmental Laboratory Page 64 3M Medical Department Study: T6316.1 THE DEVELOPMENT SERVICES COMPANY Analytical Report: FACT-TOX-001 LRN-U2103 PROTOCOL AMENDMENT NO. 4 Covance 6329-212 104-W eek Dietary Carcinogenicity Study with Narrow Range (98.1% ) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats Sponsor: Study Monitor: Testing Facility: Study Director: 3M , S t Paul, Minnesota . Andrew M. Seacat, PhD Covance Laboratories Inc., Madison, Wisconsin Peter J. Thomford, PhD This amendment modifies the following portion o f the protocoL Effective January 13,2000 1. Page 14, Postm ortem Procedures, Tissue Preservation. The Sponsor has requested that a subset o f tissues be collected for possible electron microscopy. Therefore, add the following to this section At the terminal sacrifice, sections o f the heart and liver will be collected from 10 animals/sex/group in Groups 1 ,3 ,4 , and 6 and preserved in 2.0% paraformaldehyde/2.5% glutaraldehyde in 0.1 M phosphate buffer. These tissues w ill be processed and embedded in epoxy blocks for possible future examination by electron microscopy. 3MEnvironmental Laboratory Page 65 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 AMENDMENT APPROVAL Covance 6329-212 Protocol Amendment No. 4 __ _____________ Page 2 Andrew M. Seacat, PhD Study Monitor 3M / / t- I / ' l o o o Date 3MEnvironmental Laboratory Page 66 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 COV/UYCE^ THE DEVELOPMENT SERVICES COMPANY PROTOCOL AMENDMENT NO. 5 Covance 6329-212 104-Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats Sponsor; Study Monitor: Testing Facility: Study Director: 3M , St. Paul, Minnesota Andrew M. Seacat, PhD Covance Laboratories Inc., Madison, Wisconsin Peter J. Thomford, PhD This amendment modifies the following portion o f the protocol. Effective January 21,2000 1. Page 10, Clinical Pathology, Frequency and Number ofAnimals, Scheduled Collections. The Sponsor has requested that specific clinical chemistry parameters be determined for animals at terminal and recovery sacrifice. To reflect this decision, add the following to this section. In addition, samples for clinical chemistry parameters (cholesterol and triglycerides) will be collected from all remaining animats at terminal and recovery sacrifice. 2. Page 12, Serum Analyses, Frequency and Number of Animals. The Sponsor has requested that serum be collected from all animals at terminal and recovery sacrifice. To reflect this decision, delete the text in this section and replace with the following. Five animals/sex/group in Groups 1 through 5 during Week 4 (animals selected for hepatocellular proliferation and biochemical analyses); five animals/sex/group in Groups 1 and 5 during Week 8; five animals/sex/group in Groups 1 through 4 during Week 14 (animals selected for hepatocellular proliferation and biochemical analyses); five animals/sex/group from Groups 1 and 4 (from animals selected for interim sacrifice) after at least 52 weeks o f treatment; and all remaining animals at terminal and recovery sacrifice. 3MEnvironmental Laboratory Page 67 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Covance 6329-212 Protocol Amendment No. 5 _________________________________________________________________ ________________ Page 2 3. Page 14, Postm ortem Procedures, Additional L iver Sam ple C ollection. The Sponsor has requested that frozen liver samples be collected from all animals at terminal and recovery sacrifice. Therefore, delete the text in this section and replace with the following. A portion o f the liver will be collected from five animals/sex/group from Groups 1 and 4 at the Week 53 sacrifice and from all remaining animals at the terminal and recovery sacrifice and stored in a freezer set to maintain -60 to -80C. Samples will be packed on dry ice and shipped to Kris J. Hansen, PhD, 3M Environmental Technology and Safety Services. Samples will be retained by the Sponsor for possible future analysis. Effective January 26,2000 4 Page 15, Postm ortem Procedures, H istopathology. The Sponsor has requested that all tissues from animals in Groups 1 and 4 at terminal sacrifice and selected tissues from animals in Groups 2, 3, and 6 at the terminal and recovery sacrifice be examined microscopically. To reflect this decision, delete the text in this section and replace with the following. Tissues (as appropriate) from each animal in Groups 1 and 4 sacrificed at the terminal sacrifice and from each animal that dies or is sacrificed at an unscheduled interval will be embedded in paraffin, sectioned, stained with hematoxylin and eosin, and examined microscopically. Tissues (as appropriate) from each animal in Groups 1, 4, and 6 sacrificed at the W eek 53 interim sacrifice will be embedded in paraffin, sectioned, stained with hematoxylin and eosin, and examined microscopically. Lesions, liver, lungs, kidneys, pancreas, thyroid, testes, and mammary glands (females) from each animal in Groups 2, 3, and 6 sacrificed at the terminal and recovery sacrifice w ill be embedded in paraffin, sectioned, stained with hematoxylin and eosin, and examined microscopically. Parathyroids will be processed with the thyroids, but will not be examined. Adrenals, brain, eyes, kidneys, liver, mesenteric lymph node, pancreas, spleen, testes, and ovaries from the animals necropsied at the Week 8 and 14 interim sacrifices will also be embedded in paraffin, sectioned, stained with hematoxylin and eosin, and examined microscopically. 3MEnvironmental Laboratory Page 68 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 AMENDMENT APPROVAL Cvance 6329-212 Protocol Amendment No. 5 ________________ Page 3 Andrew M. Seacat, PhD Study Monitor 3M Peter. Study Director Covance Laboratories Ine. 3MEnvironmental Laboratory Page 69 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 3M Environmental Laboratory___________________ Protocol - Analytical Study Phase 104-Week Dietary Carcinogenicity Study with Narrow Range N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats In-Vivo Study Reference Number: Covance # 6329-212 Study Number: AMDT-092597.1 Test Material: T-6316 Name and Address of Sponsor: 3M Toxicology Services Building 220-2E-02,3M Center St. Paul, MN 55144-1000 Name and Address of Testing Facility: 3M Environmental Technology and Services 935 Bush Avenue St. Paul, MN 55106 Proposed Initiation Date: April 7,1998 Proposed Completion Date: October, 31,1998 Method Numbers and Revisions FACT-M-1.0, Extraction o f Perfluorooctanesulfonate from Liver for Analysis using HPLC-Electrospray/Mass Spectrometry FACT-M-2.0, Analysis o f Liver Extracts for Fluorochemicals using HPLC- Electrospray/Mass Spectrometry FACT-M -3.0, Extraction o f Perfluorooctanesulfonate from Sera for Analysis using HPLC-Electrospray/Mass Spectrometry FACT-M-4.0, Analysis o f Sera Extracts for Fluorochemicals using HPLC- Electrospray/Mass Spectrometry Author: Lisa Clemen Kris J. Hanpen, PhD Study Director Hiwi Date M&________ -- Dale Bacon Study Director Management (-1 h Date Andrew M. Seacat, PhD Sponsor Representative 3MEnvironmental Laboratory Date Page 1 of 5 Page 70 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 1.0 PURPOSE___________________________________________________ ._______ 1.1 According to this analytical protocol, the 3M Environmental Laboratory w ill analyze the tissue and fluid samples from the Covance study number 6329-212, "104-Week Dietary Carcinogenicity with Narrow Range N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats." The collected data w ill be given to the sponsor for their use in the assessment o f toxicological effects o f the test material when administered in the diets o f rats for at least 104 weeks. 1.2 Data collected in the Environmental Laboratory w ill be considered non-quantitative screening data until future studies have been conducted to determine absolute recoveries o f specific or general fluorochemical compounds. 2.0 REGULATORY COMPLIANCE_________________________________________ . 2.1 This analytical phase o f the study w ill be conducted in accordance with the FDA Good Laboratory Practices Regulations 21 CFR 58, with the following exceptions: 2.1.1 The analytical phase is being conducted as a separate study and therefore has a separate Study Director, protocol, and final report, from those listed in the Covance protocol 6329-212. 2.1.2 The characterization o f the reference material, including purity, identity, and stability, are the responsibility o f the sponsor. 2.1.3 Sample storage stability w ill not be determined. 3.0 TEST MATERIALS__________________________________________________ 3.1 Control, and reference Materials and Matrices 3.1.1 Analytical Reference Material: T-6316, from 3MICP/PCP Division 3.1.2 Analytical Reference Matrix: Rat liver, from Covance and rat serum, from Sigma Chemical Company. 3.1.3 Analytical Control Material: None. 3.1.4 A nalytical Control M atrix: Rat liver, from Covance and rat serum, from Sigma Chemical Company. 3.2 Number of Test and Control Samples: Liver and serum from 680 test animals and 140 control animals w ill be made available; samples w ill be analyzed as requested by the sponsor or the study director. Other biological tissues (kidney, bile, dermal application site, and cellular fraction) w ill be available for analysis if deemed appropriate. 3.3 Identification of Test and Control Samples: The samples w ill be identified using the Covance animal identification number which consists o f a letter and five digit number, plus the tissue identity and day identity (serum). 3.4 Purity and Identity ofReference Material: To be determined by Sponsor. 3.5 Stability of Reference Material: To be determined by Sponsor. 3.6 Storage Conditions for Reference Materials: Reference materials w ill be stored at room temperature (3.1.1), and samples w ill be stored at -20 10C (3.1.2, 3.1.4). Test and Control samples w ill be received according to AMDT-S-10-0. 3MEnvironmental Laboratory Page 2 of 5 Page 71 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 3.7 Disposition of Specimens: Biological tissues and fluids w ill be retained per GLP Regulation for the time period required for studies longer than 28 days. 3.8 Safety Precautions: Refer to appropriate MSDS. Wear appropriate laboratory attire. Use caution when handling knives for cutting tissue samples. 4.0 EXPERIMENTAL - Overview________________________________ :___________ 4.1 The tissues from animals dosed as described (Covance# 6329-212), w ill be available for analysis for fluorine-containing compounds. At the discretion o f the Study Director, a series o f analytical tests can be performed. All high dose and control sera and livers w ill be analyzed initially using HPLC-electrospray mass spectrometry to identify fluorine-containing compounds o f interest present in the sera and liver (if any). The screening for fluoride in liver via combustion may be performed to present definitive data for fluorine in the liver. Based on the findings from these analyses, additional samples, tissues, or fluids may be analyzed at the discretion o f the Study Director to determine the presence o f fluorochemicals in these matrices. 5.0 EXPERIMENTAL - Methods____________________________________________ 5.1 Methods (attached): 5.1.1 FACT-M-1.0, " Extraction o f Perfluorooctanesulfonate from Liver for Analysis using HPLC-Electrospray/Mass Spectrometry" 5.1.2 FACT-M-2.0, "Analysis o f Liver Extracts for Fluorochemicals using HPLCElectrospray/Mass Spectrometry" 5.1.3 FACT-M-3.0, " Extraction o f Perfluorooctanesulfonate from Serum for Analysis using HPLC-Electrospray/Mass Spectrometry" 5.1.4 FACT-M-4.0, "Analysis o f Serum Extracts for Fluorochemicals using HPLCElectrospray/Mass Spectrometry" 6.0 DATA ANALYSIS_____________________________________________________ 6.1 Quality Control: Matrix spikes w ill be extracted and analyzed to determine accuracy o f the method. A lso, continuing calibration checks w ill be analyzed to determine response bias. 6.2 Transform ations: Any transformations performed on data collected during the analytical phase o f the study w ill be documented in the final report. 6.3 Statistics: At the discretion o f the Study Director, statistics used may include regression analysis o f serum concentrations with time, averages, and standard deviations o f concentrations for the different dose groups. If necessary, simple tests such as the Student's t-test may be applied to determine statistical difference. Any statistical analysis performed w ill be documented in the final report. 6.4 Data Reporting: A final data package w ill be submitted to 3M Toxicology Services. The data package w ill include the following with additional data included as deemed appropriate. 6.4.1 A summary o f individual sample results, reported as a concentration (weight/weight, weight/volume) o f fluoride per tissue or fluid, or as the mass o f a specific fluorochemical (HPLC-electrospray mass spectrometry) per unit o f tissue or fluid. 6.4.2 A summary o f quality control results (continuing calibration checks, method blanks, instrument blanks, matrix spikes, and matrix spike duplicates). 3MEnvironmental Laboratory Page 3 of 5 Page 72 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 6.4.3 Certified copies or originals o f the written validated methods. 6.4.4 Certified copies or originals o f sample identification sheets sent from Covance. 6.4.5 Certified copies or originals o f study specific raw data. 6.4.6 A summary o f key personnel involved with the analytical phase o f the study. 6.4.7 A signed QAU statement listing the dates o f inspections and reports o f findings to management and Study Director. 7.0 MAINTENANCE OF RAW DATA AND RECORDS________________________________ 7.1 The following raw data and records (or certified copies thereof) will be maintained in the study folder in the archives according to appropriate SOPs. 7.1.1 7.1.2 7.1.3 7.1.4 7.1.5 7.1.6 7.1.7 Approved protocol Approved methods Data summaries Study correspondence Shipping records Raw data Electronic copies o f data 7.2 Supporting records to be retained separately from the study folder in the archives according to 3M ET & SS SOPs, will include, but not necessarily be limited to the following: 7.2.1 7.2.2 7.2.3 7.2.4 7.2.5 7.2.6 Approved validation reports Training records Calibration records Instrument maintenance logs Standard operating procedures, equipment procedures, and methods Appropriate specimens 8.0 REFERENCES _________________'______________________________;_________________ . 8.1 AMDT-S-1, "Chemical Tracking" 8.2 AMDT-S-2, "Solutions and Standards Making" 8.3 AMDT-S-3, "Training" 8.4 AMDT-S-4, "General Lab Documentation Systems" 8.5 AMDT-S-5, "GLP-related Documentation Systems" 8.6 AMDT-S-6, "General Lab Records" 8.7 AMDT-S-7, "GLP-Related Records" 8.8 AMDT-S-8, "Archives" 8.9 AMDT-S-9, "GLP Program and Responsibilities" 8.10 AMDT-S-10, "Sample Tracking System" 3MEnvironmental Laboratory Page 4 of 5 Page 73 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 8.11 AM DT-S-12, "Analytical Method Validation" 8.12 AMDT-S-13, "Equipment Installation" 8.13 AMDT-S-14, "Quality Assurance Unit" 8.14 AMDT-S-15, "Laboratory Practices and Data Management" 8.15 AMDT-S-17, "Analytical Equipment Systems Documentation" 8.16 AMDT-S-18, "Routine Calibration Checks o f Balances" 8.17 AM DT-S-20, "Daily Calibration Check o f Automatic Pipettors" 8.18 AM DT-S-21, "Annual Calibration Checks o f Automatic Pipettors" 8.19 AM DT-S-25, "Labeling, Storage, and Use o f Test, Control, and Reference Substances" 8.20 AM DT-S-30, "Project Control and Data Review in the AMDT" 9.0 ATTACHM ENTS_________________________________;_______________________________ 9.1 FACT-M -1.0, Extraction o f Perfluorooctanesulfonate from Liver for Analysis using HPLC- Electrospray/Mass Spectrometry 9.2 FACT-M -2.0, Analysis o f Liver Extracts for Fluorochemicals using HPLC- Electrospray/Mass Spectrometry 9.3 FACT-M -3.0, Extraction o f Perfluorooctanesulfonate from Serum for Analysis using HPLC- Electrospray/Mass Spectrometry 9.4 FACT-M -4.0, Analysis o f Serum Extracts for Fluorochemicals using HPLC- Electrospray/Mass Spectrometry 3MEnvironmental Laboratory Page 5 of 5 Page 74 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Study Title 104-Week Dietary Carcinogenicity Study with Narrow Range N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats . PROTOCOL AMENDMENT NO. 1 Amendment Date: 20 January 2000 Performing Laboratory 3M Environmental Technology & Safety Services 3M Environmental Laboratory 935 Bush Avenue St. Paul, MN 55106 Laboratory Project Identification ET&SS LRN-U2103 FACT TOX-001 Covance Study: 6329-212 3M Medical Department Study: T-6316.1 3M Environmental Laboratory 3MEnvironmental Laboratory Page 75 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Protocol LRN-U2103 Amendment Number 1 This amendment modifies the following portion(s) of the protocol: 1. Protocol Reads: The following methods will be used: FACT-M -1.0, Extraction of Perfluorooctanesulfonate from Liver for Analysis using HPLC-Electrospray/Mass Spectrometry FACT-M -2.0, Analysis of Liver Extracts for Fluorochemicals using HPLCElectrospray/Mass Spectrometry FA C T-M -3.0, Extraction of Perfluorooctanesulfonate from Sera for Analysis using HPLC-Electrospray/Mass Spectrometry FA C T-M -4.0, Analysis of Sera Extracts for Fluorochemicals using HPLCElectrospray/Mass Spectrometry Amend to Read: The following methods will be used: ETS-8-4.1, Extraction of Potassium Perfluorooctanesulfonate or Other Fluorochemical compounds from Serum for Analysis Using HPLCElectrospray/Mass Spectrometry ETS-8-5.1, Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Serum Extracts Using HPLC-Electrospray/Mass Spectrometry ETS-8-6.0, Extraction of Potassium Perfluorooctanesulfonate or other Fluorochemical Compounds from Liver for Analysis using HPLC-Electrospray/Mass Spectrometry ETS-8-7.0, Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Liver Extracts Using HPLC-Electrospray/Mass Spectrometry Reason: The methods originally listed were superseded during the course of the study. 2. Protocol Reads: There is no independent section of the protocol that addresses sample retention. Amend to Read: Specimens will be maintained in the 3M Environmental Laboratory specimen archives. Any specimens sent to sub-contract laboratories will be returned to the 3M Environmental Laboratory upon completion of analysis and submission of the sub contract laboratory(s) final report. Specimens analyzed at sub-contract laboratories will be returned with the following documentation: the signed original chain of custody and records of storage conditions while at the sub-contract facility. Reason: To define in detail the appropriate disposition of specimens analyzed at subcontract laboratories. 3M Environmental Laboratory 3MEnvironmental Laboratory Page 76 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Protocol LRN-U2103 Amendment Number 1 3. Protocol Reads: Section 7 states that the following raw data and records will be retained in the study folder in the archives according to AMDT-S-8: Approved protocol and amendments; approved methods; data summaries; study correspondence; shipping records; raw data; and electronic copies of data. Additionally, Section 7 states that supporting records to be retained separately from the study folder in the archives according to AM DT-S -8 will include at least the following: Approved validation reports; training records; calibration records; instrument maintenance logs; Standard Operating Procedures, Equipment Procedures, and Methods; and appropriate specimens. Amend to Read: Section 7 states: "The original data, or copies thereof, will be available at the 3M Environmental Laboratory to facilitate audits of the study during its progress and before acceptance of the final report. When the final report is completed, all original paper data, including: approved protocol and amendments, study correspondence, shipping records, raw data, approved final report, and electronic copies of data will be retained in the archives of the 3M Environmental Laboratory. All corresponding training records, calibration records, instrument maintenance logs, standard operating procedures, equipment procedures, and methods will be retained in the archives of the facility performing each analysis." Reason: To direct subcontract laboratories in the disposition of the items listed above. 4. Protocol reads: The study director for the present study was identified in the protocol as Kristen J. Hansen, Ph.D. Amend to read: The role of study director for the present study was reassigned to John L. Butenhoff, Ph.D., as of 20 January 2000. The previous study director, Kristen Hansen, has been reassigned to the role of Principle Analytical Investigator. Reason: The role of study director was reassigned in an effort to ensure compliance with Good Laboratory Practice Standards that outline study personnel requirements (refer to 21 CFR Part 58). 5. Protocol reads: The sponsor for the present study was identified as Andrew M. Seacat, Ph.D. Amend to read: The role of sponsor for the present study was reassigned to Marvin T. Case, D.V.M., Ph.D., as of 20 January 2000. Reason: The change was made at the request of the sponsor. 3M Environmental Laboratory 3MEnvironmental Laboratory Page 77 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Protocol LRN-U2103 Amendment Number 1 Amendment Approval A ndrew M. Seacat, Ph.D ., O utgoing Sponsor Representative K risten J. H ansen, P h D ., Outgoing Study Director 2 //0/ / l5ate t t ' p A b -7 0 0 0 D ate / n i f a j L u ^ -i - ~ M a rv in T. C ase, D .V .M ., P h D ., Incom ing Sponsor R epresentative ^ Date 2. Jo h n L. Butenhoff, P h D ., Incom ing Study Director t& j 2L^Z>&<2> D ate 3M Environmental Laboratory 3M E nvironm ental Laboratory Page 78 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Study Title 104-Week Dietary Carcinogenicity Study with Narrow Range N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats PROTOCOL AMENDMENT NO. 2 Amendment Date: January 8, 2001 Performing Laboratory 3M Environmental Technology & Safety Services 3M Environmental Laboratory 935 Bush Avenue St. Paul, MN 55106 Laboratory Project Identification ET&SS LRN-U2103 FACT TOX-OOl Covance 6329-212 3M Medical Department Study: T-6316.1 3M Environmental Laboratory 3MEnvironmental Laboratory Page 79 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Protocol FA C T TOX-001 Amendment No. 2 This amendment modifies the following portion(s) of the protocol: 1. Protocol reads: 1.2 Data collected in the Environmental Laboratory will be considered non-quantitative screening data until future studies have been conducted to determine absolute recoveries of specific or general fluorochemical compounds. Amend to read: 1.2 If matrix spike studies provide accurate representation of recovery of endogenous levels of PFOS, PFOSA, PFOSAA, PFOSEA, M556, and EtFOSE-OH, the 3M Environmental Laboratory will provide semi-quantitative data for sera and liver samples collected from test animals. Reason: Due to improved analytical methods, the decision was made to change the purpose of the study results from non-quantitative to semi-quantitative. 3M Environmental Laboratory 3MEnvironmental Laboratory Page 80 3M Medical Department Study: T6316.1 ' Amendment Approval Analytical Report: FACT-TOX-001 L R N -U 2103 Protocol FA C T TO X -001 Amendment No. 2 M arvin T. Case, D .V.M ., Ph.D., Sponsor Representative l <hn>/ Date 1_ John L. Butenhoff, Ph.D., Study Director Date 3M Environmental Laboratory 3MEnvironmental Laboratory Page 81 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Study Title 104-Week Dietary Carcinogenicity Study with Narrow Range N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats PROTOCOL AMENDMENT NO. 3 Amendment Date: February 15,2001 Performing Laboratory 3M Environmental Technology & Safety Services 3M Environmental Laboratory 935 Bush Avenue St. Paul, MN 55106 Laboratory Project Identification ET&SS LRN-U2103 FACT TOX-OOl Covance 6329-212 3M Medical Department Study: T-6316.1 3M Environmental Laboratory 3MEnvironmental Laboratory Page 82 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Protocol FA C T TOX-001 Amendment No. 3 This amendment modifies the following portion(s) of the protocol: 1. Protocol reads: Specimens will be maintained in the Environmental Laboratory specimen archives. Any specimen sent to sub-contract laboratories will be returned to the 3M Environmental Laboratory upon completion o f analysis and submission o f the sub-contracted laboratory(s) final report. Specimens analyzed at sub-contracted laboratories will be returned with the following documentation: the signed original chain o f custody and records o f storage conditions while at the sub-contracted facility. Amend to read: Specimens will be maintained in the Environmental Laboratory specimen archives. Specimens sent to sub-contract laboratories for analysis of PFOS will be returned to the 3M Environmental Laboratory upon completion o f analysis and submission of the sub-contracted laboratory(s) final report. Specimens sent to sub-contract laboratories for analysis of compounds other than PFOS will not be returned. Specimens returned by sub-contracted laboratories will be returned with the following documentation: the signed original chain o f custody and records o f storage conditions while at the sub-contracted facility. Reason: Some specimens sent to sub-contract laboratories will not be returned. Portions o f these specimens have been retained at the 3M Environmental Laboratory. 3M Environmental Laboratory 3MEnvironmental Laboratory Page 83 3M Medical Department Study: T6316.1 Amendment Approval Analytical Report: FACT-TOX-001 L R N -U 2103 Protocol FA C T T O X -001 Amendment No. 3 T&c. M arvin T. Case, D. V.M., Ph.D ., Sponsor Representative lFJr 9 m>( Date <?*-> ______________________ John L. Butenhoff, Ph.D ., Study Director X, Date 3M Environmental Laboratory 3MEnvironmental Laboratory Page 84 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Study Title 104-Week Dietary Carcinogenicity Study with Narrow Range N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats . PROTOCOL AMENDMENT NO. 4 Amendment Date: April 2, 2001 Performing Laboratory 3M Environmental Technology & Safety Services 3M Environmental Laboratory 935 Bush Avenue St. Paul, MN 55106 Laboratory Project Identification ET&SS FACT TOX-OOl 3M Laboratory Request No. U2103 3M Environmental Laboratory 3MEnvironmental Laboratory Page 85 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Protocol FA C T TOX-001 Amendment #4 This amendment modifies the following portion(s) of the protocol: 1. The amended protocol reads: (Amendment #1) The following methods will be used: ETS-8-4.1, "Extraction o f Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds from Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry" ETS-8-5.1, "Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Serum Extracts Using HPLC-Electrospray/Mass Spectrometry" ETS-8-6.0, "Extraction of Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds from Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry" ETS-8-7.0, "Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Liver Extracts Using HPLC-Electrospray/Mass Spectrometry" Amend to read: The following methods will be used: . ETS-8-4.1, "Extraction of Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds from Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry" ETS-8-5.1, "Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Serum Extracts Using HPLC-Electrospray/Mass Spectrometry" with the fo llo w in g exception: (Section 14.5.1) "Matrix spike recoveries must be within 30% of the spiked concentration for all analytes except M556, which must be within 50%. ETS-8-6.0, "Extraction of Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds from Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry" ETS-8-7.0, "Analysis o f Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Liver Extracts Using HPLC-Electrospray/Mass Spectrometry" with the follow in g exception: (Section 14.5.1) "Matrix spike recoveries must be within 30% o f the spiked concentration for all analytes except PFOS, which must be 50%. R E A S O N : The analytical method and resulting QC data support a 50%-150% acceptable range for spike recoveries for these analytes and matrices. 3M Environmental Laboratory 3MEnvironmental Laboratory Page 86 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Protocol FA C T TOX-001 Amendment #4 Amendment Approval John L. Butenhoff, Ph.D., Study Director f/-// S S / Date M arvin T. Case, D .V.M ., Ph.D., Sponsor Representative ! _______ Date 3M Environmental Laboratory 3MEnvironmental Laboratory Page 87 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Record of Deviation I. Identification Study / Project No. FACT-TOX-OOl Covanee 6329-212 Deviation Type (Check one) SOP X Method Equipment Procedure Protocol Q Other: Document Number(s): Date(s) o f occurrence: FACT-M-2.0, FACT-M-4.0, ETS-8-5.0, Entire Study ETS-8-7.0________________________________________________________________________ II. Description: Required Procedure/process: These methods state: Typically the analytical batch run sequence begins and ends with a set o f extracted matrix standards. Actual Procedure/process: ' In many analytical runs, only the initial extracts matrix curve was used to evaluate the extracts. Either the second curve was not injected or the bracketing curve was deactivated since this calibraton curve was divergent. III. Actions Taken: (such as amendment issued, SOP revision, etc.) This deviation was written and a few method modifications were also written stating that the second bracketing calibration curve may be deactivated if instrumental drift affects the data. The first curve and acceptable calibration checks shall then bracket usable data. Recorded By Date A Cxft*b~ oA /A o, IV. Impact on Study / Project No adverse impact on the outcome o f this study since data were sufficiently bracketed by calibration checks. ................ ~ .......... / n A'ridwS^Zj *f XTl /l Authorized B y (Study D irecto r / P ro je ct Lead) Date SD -John B(dwhoff sponsor >p: M a / v CalC 3! ihH> 3M Environmental Laboratory Form ETS-4-8.0 3MEnvironmental Laboratory Deviation No. _______ 1_____ (assigned by Study Director or Project Lead at the end o f study or project) Page 88 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Record of Deviation I. Identification S tu d y /P ro ject No. FACT-TOX-OOl Covance 6329-212 D eviation Type (Check one) SOP Protocol X M ethod Equipment Procedure Other: Docum ent Num ber(s): FACT-M -3.0 ........... ............... ........................................... . .............................................. 1Date(s) o f occurrence: ! 04/23/98, 04/28/98, 05/11/98 II. Description: Required Procedure/process: Section 11.1.2 states: If the majority o f the serum samples are less than 1.0 mL, extract the standards in the same volume as the samples. .............. ' ....................................... . .................... ' ..................... " " ........ ........ ........ ....................................~ ......... Actual Procedure/process: Initial sera volum es for weeks 4, 8, and 14 were below 1.0 mL (0.6 mL, 0.5 mL, & 0.5 mL respectively) The curves prepared for these samples were m ade using 1.0 mL o f serum. III. Actions Taken: (such as amendment issued, SOP revision, etc.) This deviation was written. Recorded By O ik * A C $ ly y ^ IV. Impact on Study / Project No adverse impact on the study. Authorized By (Study D irector / Project Lead) Date te -in k ... a u a w .. Spcvuor R^rtJetvtaliirC- MrvA ( W ^ DirecW. ToKa Bulen hoVP - K rJtiL d,*/ f *** ' 3M Environmental Laboratory Form ETS-4-8.0 3MEnvironmental Laboratory Deviation No. 1 (assigned by Study Director or Project Lead at the end of study or project) Page 89 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Record of Deviation I. Identification f Study / Project No. FACT-TOX-OO Covance 6329-212 D eviation Type (Check one) SOP X M ethod Equipment Procedure Protocol Other: D ocum ent Num ber(s): ETS-8-5.1 Date(s) o f occurrence: 05/05/98 II. Description: Required Procedure/process: Acceptable data must be bracketed by the curve and passing CCVs. Actual Procedure/process: The M atrix spike (MSP 4/28/98) analyzed on 05/05/98 was above the range of the calibration curve. III. Actions Taken: (such as amendment issued, SOP revision, etc.) This deviation was written. Recorded By A ($m h ^ IV. Impact on Study/ Project The sample result will be flagged in the data as an estimate. Authorized By (Study Director / Project Lead) Date 0 2 / 17/ Dl ! Date sponsor Moti/a Caie. OrtcW ToKr\ uWVw T t& v O l R *Jr Z-S0 ' 3M Environmental Laboratory Form ETS-4-8.0 3MEnvironmental Laboratory Deviation No. ~->_______ (assigned by Study Director or Project Lead at the end of study or project) Page 90 3M Medical Department Study: T6316.1 Record of Deviation Analytical Report: FACT-TOX-001 LRN-U2103 /. Identification I Study / Project N o. TOXOOl (LIM S #112103) D eviation type (Check one) SOP X M ethod Equipment Procedure Protocol Other: D ocum ent number FA CT-M -4.0 and ETS-8-5.1 Date(s) o f occurrence 05/05/98, 4/20/00, 4/21/00, 5/02/00, 5/24/00, 5/30/00, 8/23/00,02/28/00, 03/15/00, 02/27/00, 04/17/00, 04/18/00, 04/19/00, 05/31/00, 06/19/00, 06/20/00, 06/21/00, 08/02/00,04/06/00 II. Description Required procedure/process: Section 10.1.2: A nalyze a m ethod blank and a m atrix blank prior to each calibration curve. Actual procedure/process: On several occasions, the blanks w ere either a) analyzed after the calibration curves o r b) not analyzed at all for a particular M S run. / / / ' ; / III. Actions Taken (such as am endm ent issued, SOP revision, etc.) D eviation written. Recorded by IV. Impact on Study / Project (completed by Study Director or Project Lead) D ate k fE <>i ( t ! l A ll blanks w ere analyzed at least once during the course o f the study. W hen blanks w ere run after the calibration curve, all control-of-bias practices were followed. In the instances w here blanks w ere not run at all, the samples being analyzed were usually w ell above the typical run LOQ. In addition, the vast m ajority o f samples run w ithout blanks were high level dilutions. The function o f the blank is to determ ine if contam ination was introduced during extraction; any low -level contam ination w ould be inconsequential to extracts requiring dilution. This deviation has no adverse affect on the study data. . ........... .~.... ..~ ..~~... bjh.h/io/cT .~ A uthorized by fieprutidc.kvt/. Mo w \.Cg*C ^ OirtcW. TcU BUtnkPft^'^A'2. 3M Environmental Laboratory D ate QfVu{!h*>l Q Q yjgfQ f N o . 2* . Page 91 3M Medical Department Study: T6316.1 Record of Deviation Analytical Report: FACT-TOX-001 LRN-U2103 Study / Project No. I. Identification TOXOOl (LIMS #U 2103) Covance 6329-212 Deviation type O SOP X Method Equipment Procedure (Check one) \ Protocol Other: D ocu m ent number: ETS-8-5.1 (Modified method) 1D ate(s) o f occurrence: ETS-8-7.0 (Modified method) | 05/05/98 (ETS-8-5.1), 02/18/99, 12/06/00 i (ETS-8-7.0) II. Description Required procedure/process: Section 14.3.6: A valid calibration curve must contain at least 5 active points Actual procedure/process: A suitable calibration curve (i.e. with all points within 30% o f theoretical and with an rA2>0.980) could not be derived from 5 points; four points were used for the calibration curve for PFOS and PFOSAA (5/5/98), for Et-FOSE-OH (2/18/99), and for PFOSAA (12/06/00). III. Actions Taken (such as amendment issued, SOP revision, etc.) Deviation written. Data evaluated against 4 point curve is specifically marked in the table o f final results. Recorded by IV. Impact on Study / Project (completed by Study Director or Project Lead) D ate 0/n /o i The data quality o f samples evaluated against the four-point curve is adversely affected. I 1 Authorized by jfjk ^ / m o i Date iPcruor II Melvin___ ChrecW- Toha !5fab Deviation No. . (assigned by Study Director or Project Lead at the end o f study or project) ~ l~C ? 0 0 / 3MEnvironmental Laboratory Page 92 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Record of Deviation I. Identification Study/Project No. FACT-TOX-OOl Covance 6329-212 Deviation Type (Check one) SOP Q Method Equipment Procedure X Protocol Other: Document Number(s): FACT-TOX-OOl Date(s) o f occurrence: 05/06/98, 05/13/98, 05/14/98, 05/15/98,. 05/17/98, 06/03/98, 06/05/98, 06/12/98, 06/14/98,06/18/98,06/25/98, 06/26/98, 07/06/98, 07/09/98, 12/14/98, 12/29/98, 01/06/99,01/18/99, 02/16/99, 02/18/99 II. Description: Required Procedure/process: The protocol states: Methods FACT-M-2.0 and FACT-M-4.0 are to be used to analyze liver and sera extracts. Actual Procedure/process: Methods were not documented or the incorrect methods were listed for analyses o f these extracts. III. Actions Taken: (such as am endm ent issued, S O P revision, etc.) This deviation was written. Recorded By Date C fe* A . CAyvi^ 57/?/<m IV. Impact on Study / Project These analyses were reviewed and these data were analyzed according to methods as listed in the protocol. No adverse impact on the outcome o f this study. b j h . 5' p y u I Authorized B y (Study D irecto r / P ro je ct Lead) Date 5Z): J ohn B u -U h h e ff 3M Environmental Laboratory Form ETS-4-8.0 3MEnvironmental Laboratory S f^ scY V /fa , Deviation No. L' (assigned by Study Director or Project Lead at the end o f study or project) Page 93 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Record of Deviation 1. Identification Study/Project No. FACT-TOX-001 Covance 6329-212 1 Deviation Type (Check one) SOP X Method Equipment Procedure Protocol Other: Document Number(s): ETS-8-5.1 Date(s) o f occurrence: 05/14/98 II. Description: Required Procedure/process: The continuing calibration verification (CCV) must he within +/- 30% o f the theoretical concentration. Actual Procedure/process: The Week 8, Sera, PFOS and PFOSAA MS, MSD, H 20 Blank, and Sera Blank data were entered even though CCVs did not meet criteria. The CCV analyzed prior to the PFOS data was within criteria and the curve immediately following these data were within criteria. Three CCVs in a row, prior to the good CCV, failed the 30% criteria. Two CCVs analyzed prior to the PFOSAA data were within criteria and the curve immediately following these data were within criteria. Two CCVs prior to the good CCVs failed the 30% criteria. III. Actions Taken: (such as amendment issued, SOP revision, etc.) This deviation was written and data will be flagged as tentative in the raw data. Recorded By A C IetH u IV. Impact on Study / Project i/C&t, tsnJLt f t , & t - l/srjhj'r\ +/-2>o'/o "' Authorized B y (Study D ire c to r / P ro je ct Lead) T .(L . A k W Sponsor R.pre,K,rvbdivc. Cas, Slu^ Olracur. Date li>r/oL Oi/b tio t Q yfV * 3M Environmental Laboratory Form ETS-4-8.0 3MEnvironmental Laboratory Deviation No. ? _______ (assigned by Study Director or Project Lead at the end of study or project) Page 94 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Record of Deviation I. Identification Study / Project No. FACT-TOX-OOl Covanee 6329-212 Deviation Type (Check one) SOP X Method Equipment Procedure Protocol Other: Document Number(s): ETS-8-7.0 Date(s) of occurrence: 05/29/98,06/01/98 II. Description: Required Procedure/process: five point curve or better is used for plotting the calibration curve. Actual Procedure/process: ................. A four point curve was used for plottting the EtFOSE calibration curve for the Week 14, Liver curve, generated on 12/14/98. III. Actions Taken: (such as amendment issued, SOP revision, etc.) These data were flagged in the raw data and this deviation was written. Recorded By Date ____ A ClitwK 01 __ ____________ ___ ___ ___ ____ IV. Impact on Study / Project...... ....... ....... ........ ........ EtFOSE-OH data is flagged as qualitative, so this data will not be adversely affected. ..... ...................... ............. .............................................................. ................ i j h 02-11*1 o f Authorized By (Study D irecto r / P ro je ct L ead) Date Spenser Rtpresexilali^t/- Wwvin C&. Tghn 3M Environmental Laboratory Form ETS-4-8.0 rfyfadLiAA'Wv Qi F-lfr / 2- t Ie r Deviation No. A. (assigned by Study Director or Project Lead at the end of study or project) 3MEnvironmental Laboratory Page 95 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Record of Deviation I. Identification Study / Project No. FACT-TOX 001 Covance 6329-212 Deviation Type (Check one) SOP X Method Equipment Procedure Protocol Other: Document Number(s): ETS-8-7.0 Date(s) o f occurrence: __________________________________________ I 06/02/98,01/14/99,01/17/99 II. Description: Required Procedure/process: Section 14.4.1 states: matrix spike percent;recoveries m ust be within 30% o f the spiked concentration.......... .... ................................................... ................. .... ........ ....... Actual Procedure/process: The week 14, liver matrix spike and matrix spike duplicate samples prepared for PFOS and PFOSAA analysis (extracted 06/02/98) weren't within criteria. The non-compliance o f the PFOS and PFOSAA data on 06/02/98 can be attributed to inappropriate preparation: spikes were prepared at 100 ng/g, a ___ level not distinguishable from background levels of the analyte in the controls. Spikes were reprepped at a higher level (250 ng/g) on 01/14/99, but again, for PFOS analysis, the spike level was not............ distinguishable from background levels; PFOSAA. was inadvertently omitted from analysis...Spikes .... for the week 14 liver samples were prepared a third time on 01/17/99 at 750 ng/g. Results of the third analysis showed an average PFOS recovery o f 132%; one of the two matrix spikes was recovered..... outside the stated 130% criteria (138%). Results o f matrix spike recovery from PFOSAA at the 750 ng/g level were acceptable............................................................. ............... .................................. ......... III. Actions Taken: (such as amendment issued, SOP revision, etc.) This deviation was written. A note will be added to the week 14 live;r data stating that one PFOS MS was recovered at 132% and that week 14 PFOS analytical results mav be biased high. Recorded By ! Date IV. Impact on Study/ Project PFOS results for week 14 liver samples may be biased high. : o a/tfh .......... ... o z - M / t l ........ Authorized By (Study Director /P ro ject Lead) Date Sponsor RtprejmkW. Margin Cwe, T.W, U u ,U i 01 f u j2-r ' 3M Environmental Laboratory Form ETS-4-8.0 3MEnvironmental Laboratory Deviation No. ^ _______ (assigned by Study D irect car Project Lead at the end of study or project) Page 96 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Record of Deviation A Identification Study / Project No. FACT-TOX-OOl Covance 6329-212 Deviation Type (Check one) SOP X Method Equipment Procedure Protocol Other: Document Number(s): ETS-8-7.0 Date(s) of occurrence: I 06/03/98 II. Description: Required Procedure/process: .............. ................. ............... .............................. .... Section 14.4.1 states: matrix spike percent recoveries must be within 30% o f the concentration. Actual Procedure/process: ,, All week 4 liver MS recoveries are outside criteria, however, the matrix spike and sample data appeared to be mislabeled. _ _ ....................... When the MS and sample labels are corrected, all recoveries are within criteria with the: .... Exception of PFOS and EtFOSE. Average PFOS recoveries are 192% and average EtFOSE Recoveries are 133%. III. Actions Taken: (such as amendment issued, SOP revision, etc.) ...................... ...................... ......... ...... ........ ........... .................. The MS and sample data labels w ere corrected in the raw data, the PFOS data were flagged in the spreadsheet, sample results are noted to have a potential high bias, and this deviation ... was written. Recorded By j Date : D lh lloi IV. Impact on Study / Project.......................... ....... ...................................... PFOS data in week 4 liver samples is noted to be potentially biased high. EtFOSE-OH data.... designated as qualitative only and is not further affected by the deviant recoveries. ...... ................ ........................h)h o ^ f t V o ) ..... _.............. ........ Authorized By (Study D ire c to r / P ro je c t L ead) Date Sponsor Represented;^'. MarW/i Ccoe- Shdj Director: 3ohn BuUwiP 3M Environmental Laboratory Form ETS-4-8.0 3MEnvironmental Laboratory C / f U ~ O h >i *2. >0 f Deviation No. 10_______ (assigned by Study Director or Project Lead at the end of study or project) Page 97 3M Medical Department Study: T6316.1 Record of Deviation I. Identification Study / Project No. FACT-TOX-OOl Covance 6329-212 Analytical Report: FACT-TOX-001 LRN-U2103 Deviation Type (Check one) SOP X Method Equipment Procedure Protocol Other: Document Number(s): ETS-8-7.0 Date(s) o f occurrence: __________________________________________ ! 12/29/98____________________ II. Description: Required Procedure/process: Section 14.5.1 states: Continuing calibration verification percent recoveries must be ... within +/-30% o f the spiked concentration,....._ ..... ................. ....... ....... ...... .............. _. Actual Procedure/process: . The continuing calibration verification samples for PFOS. PFOSA, and PFOSAA analyzed on 12-29-98 had percent recoveries greater than 130% o f expected,........ .... ..... ........... ........ ..................... ........ III. A ctions Taken: (such as amendment issued, SOP revision, etc.) This deviation was written; affected data is noted in the data tables Recorded I <s. IV. Im p a c t on S tu d y / P r o je c t ............ ..................... Affected data may be biased high. ..... O Z ~ ( \ Z I 0 \ Authorized By (Study Director / Project Lead) i Date i o( Date 'Spenser S-fud^ Director'- 'Solm Duttn^o / f FA- 3M Environmental Laboratory Form ETS-4-8.0 3MEnvironmental Laboratory Deviation No. )l________ (assigned by Study Director or Project Lead at the end of study or project) Page 98 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Record of Deviation 1. Identification Study /Project No. FACT-TOX-OOl..... Covanee 6329-212 Deviation Type (Check one) SOP X Method Equipment Procedure Protocol Other: Document Number(s): ETS 8-7.0 Date(s) of occurrence: 01/18/99 II. Description: Required Procedure/process: Section 14.5.1 states: Continuing calibration verification percent recoveries must be within 30% of the spiked concentration. Actual Procedure/process: The Week 14, liver samples C91281F, C91288F, C91293F, C91299F, and C91304F were bracketed by a continuing calibratioii verification that did not meet the + / - 30% criteria. (-31%) ........................................ .... -.............. - ..................-........ -- ....... -...... - ......... - ..... - ............... .................- ........................- .................... - .......................... - ................. - ....... - - ................ - ........ - ..................................... - ..........- ..........- - - - .......... ~ - - ......... -.................- ...................-...........- .........-............ - -- .......... - - .......- ----- ----------------------------------- ----------------------------- - ............... III. Actions Taken: These data were flagged in the raw data as having a potential low bias and this deviation was written. ............. .... .................. - .......... .................. - ....... - .................... ......................................................... - .................... Recorded By Date /)- C l W c ................................... IV. Impaizt on Study / Project Results for these analyses may be biased low. : Jo Authorized By (Study D irecto r / P ro je ct L ead) Date Spenser Reprerenla^i^' Plervin s t u d ^ O rec-W : T o U uitnV io f 3M Environmental Laboratory Form ETS-4-8.0 3MEnvironmental Laboratory (fo-O / -2, 2- f F F & ' Deviation No. 1^-_______ (assigned by Study Director or Project Lead at the end of study or project) Page 99 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Record of Deviation 1. Identification Study /Project No. FACT-TOX-001 Covance 6329-212 Deviation Type (Check one) SOP Q Method Equipment Procedure X Protocol Other: Document Number(s): FACT-TOX-OOl Date(s) o f occurrence: 02/07/00, 02/08/00, 02/09/00 II. Description: Required Procedure/process: The protocol states: Method FACT-M-3.0 is to be used when extracting the serum samples. Actual Procedure/process: Method ETS-8-4.1 was used to extract these serum samples. III. Actions Taken: (such as amendment issued, SOP revision, etc.) This deviation was written. Recorded By KC Date os/)?lo, IV. Im pact on Study / Project No adverse impact on the outcome o f this study. Sera method ETS-8-4.1 is an improvement over sera method FACT-M-3.0. ......... Jfh t$/?z/oJ Authorized By (Study D irecto r / P ro je ct Lead) Date 3M Environmental Laboratory Form ETS-4-8.0 3MEnvironmental Laboratory Deviation No. XL (assigned by Study Director or Project Lead at (he end o f study or project) Page 100 3M Medical Department Study: T6316.1 Record of Deviation Analytical Report: FACT-TOX-001 LRN-U2103 1. Identification 1 Study/Project No. FACT-TOX-001 Covance 6329-212 LIMSU2103 Deviation Type (Check one) Q SOP X Method Equipment Procedure Protocol Q Other: Document Number(s): ETS-8-7.0 Date(s) o f occurrence: 02/22/00, 04/24/00, 04/26/00, 04/28/00, 05/24/00, 07/28/00, 08/01/00, 08/14/00, 08/15/00, 08/21/00, 08/23/00, 03/22/01 II. Description: Required Procedure/process: Section 10.1.2 states: Analyze a method blank and a matrix blank prior to each calibration curve. Actual Procedure/process: On several occasions, the blanks were either a) analyzed after the calibration curves or b) not analyzed At all for a particular MS analysis. III. Actions Taken: (such as amendment issued, SOP revision, etc.) This deviation was written. .. ......................... :.p Recorded By Date | IV. Impact on Study / Project All blanks were analyzed at least once during the course o f the study. When blanks were analyzed after the calibration curve, all control-of-bias practices were followed. In the instances where blanks were not analyzed at all, the samples being analyzed were usually well above the typical run LOQ. In addition, the vast majority1o f samples analyzed without blanks were high level dilutions. The function of the blank is to determine if contamination was introduced during extraction; any low-level contamination would be inconsequential to extracts requiring dilutions. This deviation has no adverse affect on these study data. h 'h 0 ^ / 1 9 0 1 ... Authorized By (Study D irector / Project Lead) Date Sporti HjirtienUW MarV'ft StucU OiretW. 3M Environmental Laboratory Form ETS-4-8.0 3MEnvironmental Laboratory T 6k/- %3> /h ^ j Deviation No. 14_______ (assigned by Study Director or Project Lead at the end of study or project) Page 101 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Record of Deviation I. Identification Study / Project No. Deviation Type PACT- Toy- o o i SOP (Check one) Protocol Coy&noL..jkJSQEHMethod Equipment Procedure Other: Document Number _______ T S- 8~5A Date(s) o f occurrence O l o / a i j p o___________ II. Description: Required Procedure/process: lie ^ k p A ___ ArvcA^u- ft______________ Ciikrai>!pn.. ilo m W c l__ o.?-kr...e v t/^ k n lK .tarait , ud k a_minimum nP oml_p i baldi c c l'b r a k n . v t r i d c f t W feren ti re-co/t.-iej....mud ...L l ~ 3p '/ oP I L . jpiktA _____ .....CfcACi/virQ-kpri..____________ ____ ________ ___ ________________ ___ __ _______ Actual Procedure/process: Dd&...kn...Fkt..QtaupJi..fc>lrac.lj Cuk lps) tufcrt...rtpwltd...lor...PFpsAa..Qnd_.fFoJ- oil_ e v e n .iheu-k .... 4v ccALukve-..... &oJouib__ ................................................tat/*__BJBjL.__ wl ..im k a c l..oF...IP..fQmpki..W cW ltA....i W t ... M &......II..iQmplu...W k t U ..W ..... Col.brajton ducJCr loifov -Hit. y t \ Crikno,________________________________________ III. Actions Taken: (such as am endm ent issued, SO P revision, etc.) Dfi-IA to 6 f t Fooi/ioLl_iV l L rC,u) delft__QAA cW ialjtin__( M _ j4 u 3 k (L ______ Recorded By (.t i a Cl AJ o ___ * ] f r IV. Im pact on Study / Project Date Q ( a j /00 Authorized By (Study D irector / P ro jectJ(ead) ! Date r iA r /* e " / kluXji OhcApt' ToW/ Gult/ihcfl 3MA Environmental Laboratory Form ETS-4-8.0 3MEnvironmental Laboratory Spijoir Lp Mt w CftU. iDeviation No. 4JL (assigned by Study Director or Project Lead at the end o f study or project) Page 102 3M Medical Department Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Record of Deviation I. Identification Study / Project No. FACT-TOX-OOl Covance 6329-212 Deviation Type (Check one) n SOP Method Q Equipment Procedure X Protocol D Other: Document Number(s): FACT-TOX-OOl Date(s) o f occurrence: 07/28/00, 08/01/00, 08/14/00, 08/15/00, 08/21/00, 08/23/00, 08/28/00, 08/29/00 II. Description: Required Procedure/process: The protocol states: Method ETS-8-7.0 is to be used to analyze liver extracts. Actual Procedure/process: Method ETS-8-6.0 was incorrectly listed as the method used to analyze these liver extracts. . III. Actions Taken: (such as amendment issued, SOP revision, etc.) This deviation was written. Recorded By IV. Im pact on Study / Project ETS-8-6.0 is the extraction method, ETS-8-7.0 is the analytical method. These analyses were reviewed and data were analyzed according to ETS-8-7.0. No adverse impact on the outcome. o f this study. Authorized B y (Study D irecto r / P ro ject Lead) Date <2^S j b - 'J ohr\ a rc h h o ff 3M Environmental Laboratory Form ETS-4-8.0 X -f/o f M a t* (fi** Jk. (assigned by Study Director or Project Lead at the end of study or project) 3MEnvironmental Laboratory Page 103 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Record of Deviation 1. Identification Study / Project No. Deviation Type (Check one) '/C y ^ / SOP Protocol j3TMethod Equipment Procedure Other: Document Number 3 E F -Z .o JDate(s) o f occurrence 1 II. D escription: Required Procedure/process: --.... -C C lJ s ............................................................ ~ Actual Procedure/process: ' r t f a L .....C & O M .... .4 C ziL M l ' L .. l O o ..j ^ ^ ^ .. ........................................^......*../.......v.L..-*...C....sQDs3S S&i/s. III. A ctions Taken: (such as amendment issued, SO P revision, etc.) --yzL..2/E 2S .....................................(2 .^ 1 / ^ h . ^ /cD F 3 lp Z ^ ... ^ /O ... Recorded By Date 'on S tud y / P roject <Jb- d & fa U>&4 1 r \ t........................ OC...uh TW krph../ht C^(hcitlMOfi-WiL,.. ..V^r__cC eJfa-.=___ - __M l g d -W O M.__ u ^ t ^ L z . Authorized By (Study D irecto r 7 P ro ject Lead) */& < ? ,.. t h 03/23 ! 0 T Date 3M Environmental Laboratory Form ETS-4-8.0 .T S W )i D i r e c W ; JoU Bukokoff 3MEnvironmental Laboratory Deviation No. _____^2;______ A c ~ \ } C. , Jassigneaby Study Director or Project Lead at the end of study or project) ' Page 104 3M M edical D epartm ent Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Analytical Report: FACT TOX-001 LRN-U2103 Appendix C: Extraction and Analytical Methods This appendix includes the following methods: Preparatory Methods FACT-M-1.0. Extraction of Potassium Perfluorooctanesulfonate or Other Anionic Fluorochemical Surfactants from Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry, (8 pages) FACT-M-3.0, Extraction of Potassium Perfluorooctanesulfonate or Other Anionic Fluorochemical Surfactants from Serum for Analysis using HPLC-Electrospray/Mass Spectrometry, (8 pages) ETS-8-4.1, Extraction of Potassium Perfluorooctanesulfonate or other Fluorochemical Compounds from Serum for Analysis using HPLC-Electrospray/Mass Spectrometry, (14 pages) ETS-8-6.0, Extraction of Potassium Perfluorooctanesulfonate or other Fluorochemical Compounds from Liver for Analysis using HPLC-Electrospray/Mass Spectrometry, (14 pages) Analytical Methods FACT-M-2.0, Analysis of Liver Extracts for Fluorochemicals Using HPLCElectrospray/Mass Spectrometry, (8 pages) FACT-M-4.0, Analysis of Fluorochemicals in Serum Extracts Using HPLCElectrospray/Mass Spectrometry, (8 pages) ETS-8-5.1, Analysis of Potassium Perfluorooctanesulfonate or other Fluorochemicals in Serum Extracts Using HPLC-Electrospray/Mass Spectrometry, (9 pages) ETS-8-7.0, Analysis of Potassium Perfluorooctanesulfonate or other Fluorochemicals in Liver Extracts Using HPLC-Electrospray/Mass Spectrometry, (10 pages) 3MEnvironmental Laboratory Page 105 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 3M Environmental Laboratory M ethod E x t r a c t io n o f Po ta s s iu m perfluo ro o ctanesulfo nate o r O t h e r A n io n ic F l u o r o c h e m ic a l Su rfactants f r o m L iv e r fo r An a l y s is U sin g H P L C -E lectro spray/M ass Sp e c t r o m e tr y Method Number: FA C T -M -1.0. Author: L isa Clem en A p p ro v ed By: Adoption Date: 5 ^ Revision Date: l d j / \ n L A t W _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ shtht Technical Review er D ate ^ Initial 1 .0 S c o p e a n d A p p l ic a t io n __________________________________ ___________ _____________________ 1.1 Scope: T h is m e th o d is fo r the extraction o f P otassium P erfluorooctanesulfonate (P F O S ) o r j other fluorochem ical surfactants from liver. 1.2 Applicable Compounds: Fluorochem ical surfactants or other fluorinated com pounds. blSfo, Date 1.3 Matrices: R ab b it, rat, bovine, and m onkey livers or o th er livers as desig n ated in the * validation report. ) .'.M icrosoft 7.0.1/95 jj 3M E nvironm ental Laboratory FACT-M -1.0 Extraction o f PFOS from Liver Page 1 of 8 Page 106 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 2.0 S u m m a r y o f M e t h o d _________________________________________________________ ____________ 2.1 This method describes how to extract potassium perfluorooctanesulfonate (PFOS) or other fluorochemical surfactants from liver using ion pairing reagent and 5.0 mLs o f ethyl acetate. An ion pairing reagent is added to each sample and partitioned into ethyl acetate. Four mLs o f extract is removed to a centrifuge tube and put onto a nitrogen evaporator until dry. Each extract is reconstituted in 1.0 mL methanol then filtered through a 3 cc plastic syringe attached to a 0.2 pm filter into glass autovials. 3.0 D e f in it io n s ________________________________________________________________________________ 3.1 None. 4.0 W a r n in g s a n d C a u t io n s _________________________________________________________________ 4.1 Health and Safety Warnings: 4.1.1 Use universal precautions when handling animal livers, they may contain pathogens. 5.0 I n t e r f e r e n c e s ____________________________________________________________________________ 5.1 There are no known interferences at this time. 6.0 E q u ip m e n t _________________________________________________________________________________ 6.1 The following equipment is used while carrying out this method. Equivalent equipment is acceptable. 6.1.1 6.1.2 6.1.3 6.1.4 6.1.5 6.1.6 Ultra-Turrax T25 Grinder for grinding liver samples Vortex mixer, VWR, Vortex Genie 2 Centrifuge, Mistral 1000 or IEC Shaker, Eberbach or VWR Nitrogen Evaporator, Organomation Balance 7.0 S u p p l ie s a n d M a t e r ia l s _________________________________________________________________ 7.1 Gloves 7.2 Dissecting scalpels 7.3 Eppendorf or disposable pipettes 7.4 Nalgene bottles, capable o f holding 250 mL and 1 L 7.5 Glass, type A, volumetric flasks 7.6 40 mL glass I-CHEM vials 7.7 Plastic sampule vials, Wheaton, 6 mL 7.8 Polypropylene centrifuge tubes, 15 mL 7.9 Labels 3MEnvironmental Laboratory FACT-M-1.0 Extraction of PFOS from Liver Page 2 of 8 Page 107 3M M edical D epartm ent Study: T6316.1 .* Analytical Report: FACT-TOX-001 L R N -U 2103 7.10 Syringes, capable o f measuring 10 pL to 50 pL 7.11 Glass, type A, volumetric pipettes 7.12 Graduated pipettes 7.13 Electronic pipettor, Eppendorf or equivalent 7.14 Timer 7.15 Disposable plastic 3 cc syringes 7.16 Filters, nylon syringe filters, 0.2 pm, 25 mm 7.17 Crimp cap autovials Note: Prior to using glassware and bottles, rinse 3 times with methanol and 3 times with MilliQTM water. Rinse syringes a minimum of 9 times with methanol, 3 rinses from 3 separate vials. 8.0 R e a g e n t s a n d S t a n d a r d s 8.1 Reagents 8.1.1 Sodium Hydroxide (J.T Baker or equivalent), (NaOH) 10N: weigh approximately ' 200 grams NaOH. Pour into a 1000 mL beaker containing 500 liters (L) Milli-QTM water, mix until all solids are dissolved. Store in a 1 L nalgene bottle. 8.1.2 Sodium Hydroxide (J.T Baker or equivalent), (NaOH) IN. Dilute 10N 1:10. Measure 10 mL o f the 10N NaOH solution into a 100 mL volumetric flask and dilute to volume using Milli-QTM water. Store in a 125 mL nalgene bottle. 8.1.3 Tetrabutylammonium hydrogen sulfate (Kodak or equivalent), (TBA) 0.5M: Weigh approximately 169 grams o f TBA into a 1 L volumetric containing 500 L Milli-QTM water. Adjust to pH 10 using approximately 64 mL 10N NaOH and dilute to volume with Milli-QTM water. Add NaOH slowly while adding the last 1 mL o f NaOH because the pH changes abruptly. Store in a 1 L nalgene bottle. . 8.1.3.1 TBA requires a check prior to each use to ensure pH = 10. Adjust as needed using IN NaOH solution. 8.1.4 Sodium carbonate/Sodium Bicarbonate Buffer (J.T. Baker or equivalent), (NajCOj/NaHCOj) 0.25M: Weigh approximately 26.5 g o f sodium carbonate (Na2C03) and 21.0 g of sodium bicarbonate (NaHC03) into a 1 L volumetric flask and dilute to volume with Milli-QTM water. Store in a 1 L nalgene bottle. 8.1.5 PFOS (3M Specialty Chemical Division), molecular weight = 538. 8.1.6 Ethyl Acetate, Omnisolv, glass distilled or HPLC grade. 8.1.7 Methanol, Omnisolv, glass distilled or HPLC grade. 8.1.8 Liver and control liver, received frozen from testing laboratory. - 8.1.9 Milli-QTM water, all water used in this method should be Milli-QTM water and may be provided by a Milli-Q TOC Plus system. 8.2 Standards 8.2.1 Prepare PFOS standards for the standard curve. 3MEnvironmental Laboratory FACT-M-1.0 Extraction of PFOS from Liver Page 3 of 8 Page 108 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 8.2.2 Weigh approximately 100 mg o f PFOS into a 100 mL volumetric flask and record the actual weight. 8.2.3 Bring to volume with methanol for a stock standard o f approximately 1000 ppm (pg/mL). 8.2.4 Dilute the stock solution with methanol for a working standard I solution o f approximately 50 ppm. 8.2.5 Dilute the stock solution with methanol for a working standard 2 solution o f approx. 5.0 ppm. 8.2.6 Dilute the stock solution with methanol for a working standard 3 solution o f approx. 0.50 ppm. 9.0 S a m p l e H a n d l in g ___________________________________________ ;_____________________ 9.1 All livers are received frozen and must be kept frozen until the extraction is performed. 1 0 .0 Q u a l it y C o n t r o l _________________________;______________________________________________ 10.1 Matrix Spikes 1 0 .1 .1 Prepare and analyze matrix spike and matrix spike duplicate samples to determine the accuracy o f the extraction. 10.1.2 Prepare each spike using liver chosen by the analyst, usually a control liver. 1 0 .1 .3 Expected concentrations will fall in the mid-range o f the initial calibration curve. 10.2 Continuing Calibration Checks 1 0 .2 .1 Prepare and analyze continuing calibration check samples to determine the continued linearity o f the initial calibration curve. 10.2.2 One check is prepared per group o f ten samples. For example, if a sample set = 34, four checks are prepared and extracted. 10.2.3 Prepare each continuing calibration check from the same liver homogenate used to prep the initial curve. 10.2.4 The expected concentration will fall within the mid-range o f the initial calibration curve. 1 1 .0 C a l i b r a t io n a n d S t a n d a r d iz a t io n ____________________________________________________ 11.1 Prepare Liver Homogenate to Use for Standards 11.1.1 Weigh approximately 40 g o f liver into a 250 mL Nalgene bottle containing 200 - mLs Milli-QTM water. Grind to a homogeneous solution. 11.1.2 If 40 g is not available, use appropriate amounts o f liver and water in keeping with a 1:5 ratio. 11.1.3 See section 13.0 to calculate the actual density o f liver. 3MEnvironmental Laboratory FACT-M-1.0 Extraction of PFOS from Liver Page 4 of 8 Page 109 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 11.1.4 Add 1 mL o f homogeneous solution to a 15 mL centrifuge tube. Re-suspend homogeneous solution by shaking between aliquots while preparing a total o f sixteen 1 mL aliquots o f homogeneous solution in 15 mL centrifuge tubes. 11.1.5 Two 1 mL aliquots serve as matrix blanks. Use the standard concentrations and spiking amounts listed in table 1 to spike, in duplicate, two standard curves for a total o f fourteen samples. ` Table 1 Approximate Spiking Amounts for Calibration Standards Working Standard (Approx. Cone.) 0.50 ppm 0.50 ppm 0.50 ppm 5.0 ppm 5.0 ppm 5.0 ppm 50 ppm pL 4 20 40 10 . 20 30 4 Approx, final cone, of PFOS in liver Blank 0.010 ppm 0.050 ppm 0.100 ppm 0.250 ppm 0.500 ppm 0.750 ppm 1.000 ppm 11.1.1 See section 13.0 to calculate actual concentrations o f PFOS in calibration standards. 11.2 Extract spiked liver homogenates following 12.14-12.24 o f this method. Use these standards to establish each initial curve on the mass spectrometer. 12.0 P r o c e d u r e s _____________________________________________________________ ' 12.1 Obtain frozen liver samples. In spent tissue, note that the liver has not been packaged with other tissues. 12.2 Cut approximately 1 g o f liver using a dissecting scalpel. 12.3 Weigh the sample directly into a tared plastic sampule vial. 12.4 Record the liver weight in the study notebook. 12.5 Label the sampule vial with the study number, weight, liver ID, date and analyst initials. 12.6 Add 2.5 mLs o f water to sampule vial. 12.7 Grind the sample. Put the grinder probe in the sample and grind for about 2 minutes, or until the sample is homogeneous. 12.8 Rinse the probe into the sample with 2.5 mLs water using a pipette. 12.9 Take the grinder apart and clean it with methanol after each sample. Follow AMDT-EP-22. 12.10 Cap the sample and vortex for 15 seconds. 3MEnvironmental Laboratory FACT-M-1.0 Extraction of PFOS from Liver Page 5 of 8 Page 110 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 12.11 Pipette 1 mL homogenate into a 15 mL polypropylene centrifuge tube. Label the centrifuge tube with the identical information as the sampule vial. (See Worksheet for documenting the remaining steps.) 12.12 Spike liver homogenates with the appropriate amount o f PFOS standard as described in section 11.1 or Table 1. 12.13 Pipette two 1 mL aliquots o f Milli-QTM water to centrifuge tubes. These will serve as instrument blanks. - 12.14 Add 1 mL 0.5 M TBA and 2 mL o f the 0.25 M sodium carbonate/sodium bicarbonate buffer. 12.15 Using a volumetric pipette, add 5 mLs ethyl acetate. 12.16 Cap each sample and put on the shaker for 20 minutes. 12.17 Centrifuge for 20 to 25 minutes, until layers are well separated. Set power on the centrifuge to approximately 3500 rpm. 12.18 Remove 4 mLs o f organic layer, using a 5 mL graduated glass pipette, to a clean 15 mL centrifuge tube. Label this fresh tube with th same information as in 12.5. 12.19 Put each sample on the analytical nitrogen evaporator until dry, approximately 2 to 3 hours. 12.20 Add 1.0 mL o f methanol to each centrifuge tube using a graduated pipette. 12.21 Vortex mix for 30 seconds. 12.22 Attach a 0.2 pm nylon mesh filter to a 3 cc syringe and transfer the sample to this syringe. Filter into a 1.5 mL glass autovial. 12.23 Label the autovial with the study number, animal number and gender, sample timepoint, matrix, final solvent, extraction date, and analyst(s) who performed the extraction. 12.24 Cap and hold for electrospray mass spectrometry analysis. 12.25 Complete the worksheet and tape to page o f study notebook. 13.0 D a t a A n a l y s i s a n d C a l c u l a t io n s ______________________________________________________ 13.1 Calculations: 13.1.1 Calculate the density o f liver (mg) in 1.0 mL homogenate using the following equation: g o f Liver x Average weight o f ten 1 mL aliquots (mg) (g o f Liver + g o f Water) 3MEnvironmental Laboratory FACT-M -1.0 Extraction o f PFOS from Liver Page 6 of 8 P age 111 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 13.1.2 Calculate actual concentrations o f PFOS in calibration standards using the following equation: uL o f Standard x Concentration pig /mL) = Final Concentration (pg/g or mg/kg) mg Liver /1 mL homogenate o f PFOS in Liver *Average weight o f liver in solution as determined in 13.1.1, by weighing ten 1 mL homogenates o f approximately 40 mg liver in 200 mL o f Milli-Q water. 1 4 .0 M e t h o d P e r f o r m a n c e _________________________________________________________________ 14.1 The method detection limit is equal to half the lowest standard in the calibration curve. 1 5 .0 P o l l u t i o n P r e v e n t i o n a n d W a s t e M a n a g e m e n t ____________________________________ 15.1 Sample waste is disposed in biohazard containers, flammable solvent waste is disposed in high BTU containers, and used glass pipette waste is disposed in broken glass containers located in the laboratory. ' 1 6 .0 R e c o r d s __________________________________________________________________________________ 16.1 Complete the extraction worksheet and tape into the study notebook. 1 7 .0 T a b l e s , D i a g r a m s , F l o w c h a r t s , a n d V a l id a t io n D a t a ____________________________ 17.1 The validation report associated with this method is FACT-M-1.0 & 2 .0 -V -l. 1 8.0 References___________________________________________________________________ 18.1 AMDT-EP-22, "Routine Maintenance o f Ultra-Turrax T-25" 1 9 .0 A f f e c t e d D o c u m e n t s _______________________________________________ ;___________________ 19.1 FACT-M-2, "Analysis o f Liver Extracts for Fluorochemicals using HPLC-Electrospray Mass Spectrometry" 20.0 R e v isio n s R ev isio n N um ber. Reason For Revision R ev isio n D ate 3MEnvironmental Laboratory FACT-M-1.0 Extraction of PFOS from Liver Page 7 of 8 Page 112 3M M edical D epartm ent Study: T6316.1 if Extraction Worksheet for FACT-M-1 Analytical Report: FACT-TOX-001 L R N -U 2103 Study # 1 Sam ple N um ber set # H20 Blank Liver Blank PFOS approx. 0.5 ppm actual ppm #W - PFOS approx. 5 ppm actual ppm #W - - * .- - -- -- -- -- ' -' - -- -- -- -- -- -- -- -- -- -- -- -- -- PFOS approx. 50 ppm actual #W ppm - - - - - - - - Date and Initials for Std. 1Study num b er w here the original worl csheet is located. B lank L iver H om ogenate: S td # L iver am ount = g L iver E xtraction M ethod : D ate & Initials V o rtex 15 sec. Pipette 1 m L o f L iver Solution P ip ette 1 m L o f f 0.5 M T B A , pH 10. Std. # P ipette 2 m L o f 0.25 N a 2 C O y 0 .2 5 M N aH C O ^ B uffer Std. # Pipette 5 m L o f E thyl A cetate TN -A - S hake 20 m in. C entrifuge 20-25 m in. C entrifuge Speed R em ove a 4 m L aliquot o f organic layer Put on N itrogen E vaporator to drvness E vaporator Tem perature A dd 1.0 m L o f M ethanol TN -A - V ortex 30 sec. F ilter u sin g a 3 cc B -D sy rin g e w ith a 0 .2 u m SR I filter into a 1.5 m L autosam ple vial MS/MSD/___Cont. Checks: Spiked_____ uL of a _____ ppm std (_____________ ) for a final concentration of ________ ppm. MS/MSD used sample______________ . Cont. Checks used same homogenate as for std curve. 3MEnvironmental Laboratory FACT-M-1.0 Extraction of PFOS from Liver Page 8 of 8 P age 113 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 3M Environmental Laboratory Method Extraction of Potassium perfluorooctanesulfonate or other Anionic Fluorochemical surfactants from Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry Method Number: FACT-M-3.0 Author: Lisa Clemen Adoption Date: ^ j <13 Revision Date: Group Leader 'Ol'W A jjtni.%. Technical Reviewer Date nluh 2 Date lA mX (7 fU o f 1 if ^ ) 1.0 Sc o pe a n d A pplicatio n . . 1.1 Scope: This method is for the extraction o f potassium perfluorooctanesulfonate (PFOS) or other fluorochemical surfactants from serum. 1.2 Applicable Compounds: Fluorochemical surfactants or other fluorinated compounds. (T -4, 1.3 Matrices: Rabbit, rat, and bovine serum or other sera as designated in the validation report. o CO o ' Microsoft 7.0.1/95 to FACT-M-3.0 Extraction of PFOS from Serum Page 1 o f 8 3MEnvironmental Laboratory Page 114 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 2.0 Summary of M ethod_______________________ _______ ;______________________ 2.1 This method describes how to extract potassium perfluorooctanesulfonate (PFOS) or other anionic fluorochemical surfactants from serum using an ion pairing reagent and 5.0 mL o f ethyl acetate. An ion pairing reagent is added to the sample and the analyte ion pair is partitioned into ethyl acetate. Four mL o f extract are removed and put onto a nitrogen evaporator until dry. Each extract is reconstituted in 1.0 mL o f methanol, then filtered through a 3 cc plastic syringe attached to a 0.2 pm nylon filter into glass autovials. 3.0 Definitions__________________________________ ______________ _________________ 3.1 None. 4.0 Warnings and Cautions 4.1 Health and Safety Warnings: _____________________________ ;______________ 4.1.1 Use universal precautions, especially laboratory coats, goggles, and gloves when handling animal serum, it may contain pathogens. 5.0 Interferences_____________ ;__________________ _________________________________ 5.1 There are no known interferences at this time. 6.0 Equipment_______________ ;______ _____________________________ ;__________ 6.1 The following equipment is used while carrying out this method. Equivalent equipment is acceptable. 6.1.1 6.1.2 6.1.3 6.1.4 6.1.5 Vortex mixer, VWR, Vortex Genie 2 Centrifuge, Mistral 1000 or IEC Shaker, Eberbach or VWR Nitrogen evaporator, Organomation Balance, (0.100 gm) . . 7.0 Supplies and M aterials _________________:____________________________ _ 7.1 Gloves 7.2 Eppendorf or disposable pipettes 7.3 Nalgene bottles, capable o f holding 250 mL and 1 L 7.4 Glass, type A, volumetric flasks 7.5 40 mL glass I-CHEM vials 7.6 Polypropylene centrifuge tubes, 15 mL 7.7 Labels 7.8 Syringes, capable o f measuring 10 pL to 50 pL 7.9 Glass, type A, volumetric pipettes 7.10 Graduated pipettes 3MEnvironmental Laboratory FACT-M-3.0 Extraction of PFOS from Serum Page 2 of 8 Page 115 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 7.11 Electronic pipettor, Eppendorf or equivalent 7.12 Timer 7.13 Disposable plastic 3 cc syringes 7.14 Filters, nylon syringe filters, 0.2 pm, 25 mm 7.15 Crimp cap autovials Note: Prior to using glassware and bottles, rinse 3 times with methanol and 3 times with M illi- QTMwater. Rinse syringes a minimum o f 9 times with methanol, 3 rinses from 3 separate vials. 8.0 Reagents and Standards 8.1 Reagents _______ ;______________________________________ 8.1.1 Sodium hydroxide (J.T Baker or equivalent), (NaOH) 1ON: weigh approximately 200 grams NaOH. Pour into a 1000 mL beaker containing 500 liters (L) Milli-QTM water, mix until all solids are dissolved. Store in a 1 L Nalgene bottle. 8.1.2 Sodium hydroxide (J.T Baker or equivalent), (NaOH) IN. Dilute 10N 1:10. Measure 10 mL o f 10N NaOH solution into a 100 mL volumetric flask and dilute to volume using Milli-QTM water. Store in a 125 mL Nalgene bottle. 8 .1 3 Tetrabutylammonium hydrogen sulfate (Kodak or equivalent), (TBA) 0.5M: Weigh approximately 169 grams o f TBA into a 1 L volumetric containing 500 L Milli-QTM water. Adjust to pH 10 using approximately 64 mL o f 10N NaOH and dilute to volume with Milli-QTM water. Add NaOH slowly while adding the last mL o f NaOH because the pH changes abruptly. Store in a 1 L Nalgene bottle. 8.1.3.1 TBA requires a check prior to each use to ensure pH = 10. Adjust as needed using IN NaOH solution. 8.1.4 Sodium carbonate/sodium bicarbonate buffer (J.T. Baker or equivalent), (Na2C03/NaHC03) 0.25M: Weigh approximately 26.5 g o f sodium carbonate (NajC03) and 21.0 g o f sodium bicarbonate (NaHC03) into a 1 L volumetric flask and bring to volume with Milli-QTM water. Store in a 1 L nalgene bottle. 8.1.5 PFOS (3M Specialty Chemical Division), molecular weight = 538. 8.1.6 Other fluorochemicals, as appropriate. 8.1.7 Ethyl Acetate, Omnisolv, glass distilled or HPLC grade. 8.1.8 Methanol, Omnisolv, glass distilled or HPLC grade. 8.1.9 Serum, frozen liquid from Sigma. 8.1.10 Control serum received with each sample set. 8.1.11 Milli-QTM water, all water used in this method should be Milli-QTM water and may be provided by a Milli-Q TOC Plus system. 3MEnvironmental Laboratory FACT-M-3.0 Extraction of PFOS from Serum Page 3 of 8 Page 116 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 . LRN-U2103 8.2 Standards 8.2.1 Prepare PFOS standards for the standard curve. 8.2.2 Prepare other fluorochemical standards, as appropriate. 8.2.3 Weigh approximately 100 mg o f PFOS into a 100 mL volumetric flask and record the actual weight. 8.2.4 Bring to volume with methanol for a stock standard o f approximately 1000 ppm (p-g/mL). 8.2.5 Dilute the stock solution with methanol for a working standard 1 solution o f approximately 50 ppm. 8.2.6 Dilute the stock solution with methanol for a working standard 2 solution o f approx. 5.0 ppm. 8.2.7 Dilute the stock solution with methanol for a working standard 3 solution o f approx. 0.50 ppm. 9.0 Sample Handling______ ,________________ ___________________________ ' 9.1 All sera are received frozen and must be kept frozen until the extraction is performed. 10.0 Quality Control __________;__________________________ ;___________________ 10.1 M atrix Blanks and Method Blanks 10.1.1 Two 1.0 mL aliquots o f the serum are extracted following this procedure and used as matrix blanks. See section 11.1.2. ' 10.1.2 Two 1.0 mL aliquots o f Milli-QTM water are extracted following this procedure and used as method blanks. 10.2 M atrix Spikes 10.2.1 Prepare and analyze matrix spike and matrix spike duplicate samples to determine the accuracy o f the extraction. 10.2.2 Prepare each spike using serum chosen by the analyst, usually control serum received with each sample set. . 10.2.3 Expected concentrations will fall in the mid-range o f the initial calibration curve. Additional spikes may be included and may fall in the low-range o f the initial calibration curve. 10 3 Continuing Calibration Checks 10.3.1 Prepare and analyze continuing calibration check samples to determine the continued linearity of the initial calibration curve. 10.3.2 One check is prepared per group o f ten samples. For example, if a sample set = 34, four checks are prepared and extracted. 3MEnvironmental Laboratory FACT-M-3.0 Extraction of PFOS from Serum Page 4 of 8 Page 117 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 10.3.3 Prepare each continuing calibration check from the same serum used to prep the initial curve. 10.3.4 The expected concentration will fall within the mid-range o f the initial calibration curve. 11.0 Calibration and Standardization_______ '_________________________ _________ _ 11.1 Prepare Serum Standards 11.1.1 Transfer 1 mL o f serum to a 15 mL centrifuge tube. 11.1.2 If the majority o f serum sample volumes are less than 1.0 mL, extract standards using serum volumes in the standards equal to the serum volumes in samples. Do not extract below 0.50 mL o f serum. Record the serum volume on the extraction sheet. 11.1.3 Mix or shake between aliquots while preparing a total o f sixteen aliquots o f serum in i 5 mL centrifuge tubes. 11.1.4 Two 1 mL or appropriate aliquots serve as matrix blanks. Typically use the standard concentrations and spiking amounts listed in table 1 to spike, in duplicate, two standard curves for a total o f fourteen samples. 11.1.5 Refer to the validation report FACT-M-3.0-V-1 and FACT-M-4.0-V-1 which lists the working ranges for calibration curves. Table 1 Approxim ate Spiking Amounts for Standards and Spikes - Using 1.0 mL of Serum Working Standard PL (Approx. Cone.) - .- 0.500 ppm 20 5.00 ppm 5 5.00 ppm 10 5.00 ppm 20 50.0 ppm 5 50.0 ppm 10 50.0 ppm 15 Approx, final cone, o f PFOS in serum Blank 0.010 ppm 0.025 ppm 0.050 ppm 0.100 ppm 0.250 ppm 0.500 ppm 0.750 ppm 11.1.4 See section 13.0 to calculate actual concentrations o f PFOS in calibration standards. 11.2 Extract spiked serum standards following 12.6-12.16 o f this method. Use these standards to establish each initial curve on the mass spectrometer. 3MEnvironmental Laboratory FACT-M-3.0 Extraction of PFOS from Serum Page 5 of 8 Page 118 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 12.0 Procedures______________________________ :___________________________________ 12.1 Obtain frozen serum samples and allow to thaw. 12.2 Vortex mix for 15 seconds then remove 1.0 mL or appropriate volume to a 15 mL polypropylene centrifuge tube. 123 Return serum samples to freezer after extraction amount has been removed. 12.4 Record the serum volume on the extraction worksheet. The final methanol volume w ill equal the initial serum volume. ' 12.5 Label the tube with the study number, serum ID, date and analyst initials. See attached worksheet for documenting the remaining steps. . 12.6 Spike serum with the appropriate amount o f PFOS standard as described in section 11.1 or Table I for the calibration curve standards. Also spike matrix spikes and continuing calibration standards. . 12.7 Vortex mix the standard curve samples, matrix spike samples, and continuing calibration samples for 15 seconds. 12.8 Add 1 mL 0.5 M TBA and 2 mL o f the 0.25 M sodium carbonate/sodium bicarbonate buffer. 12.9 Using a volumetric pipette, add 5 mL ethyl acetate. 12.10 Cap each sample and put on the shaker for 20 minutes. 12.11 Centrifuge for 20 to 25 minutes, until layers are well separated. Set power on the centrifuge to approximately 3500 rpm. 12.12 Transfer 4 mL o f organic layer, using a 5 mL graduated glass pipette, to a clean 15 mL centrifuge tube: Label this fresh tube with the same information as in 12.5. 12.13 Put each sample on the analytical nitrogen evaporator until dry, approximately 2 to 3 hours. 12.14 Add 1.0 mL or appropriate volume of methanol to each centrifuge tube using a graduated pipette. (This volume equals the initial volume o f serum used for the extraction.) 12.15 Vortex mix for 30 seconds. 12.16 Attach a 0.2 pm nylon mesh filter to a 3 cc syringe and transfer the sample to this syringe. Filter into a 1.5 mL glass autoviaL 12.17 Label the autovial with the study number, animal number and gender, sample timepoint, matrix, final solvent, extraction date, and analyst(s) who performed the extraction. 12.18 Cap and hold for HPLC-electrospray/mass spectrometry analysis. Extracts may be stored at 4 C until analysis. 12.19 Complete the extraction worksheet, attached to this document, and tape to page o f study notebook. 3MEnvironmental Laboratory FACT-M-3.0 Extraction of PFOS from Serum Page 6 of 8 Page 119 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 13.0 Data Analysis and Calculations ________________________ _______________ _ 13.1 Calculations: 13.1.1 Calculate actual concentrations o f PFOS, or other appropriate fluorochemical, in calibration standards using the following equation: mL o f Standard x Concentration (ug /m D = Final Concentration (pg/mL) mL o f Standard + Initial Serum Volume (mL) o f PFOS in Serum 14.0 Method Performance________________________;_____________________________ _ 14.1 The method detection limit is equal to half the lowest standard in the calibration curve. 15.0 Pollution Prevention and Waste Management___________________ ;__________ 15.1 Sample waste is disposed in biohazard containers, flammable solvent waste is disposed in high BTU containers, and used glass pipette waste is disposed in broken glass containers located in the laboratory. 16.0 Records ___________________ ;______ ,__________________________ _______ 16.1 Complete the extraction worksheet attached to this method, and tape into the study notebook. 17.0 T ables. Diagrams. Flowcharts, and Validation Data_______________________ 17.1 The validation report associated with this method is FACT-M-3.0 & 4.0-V -l. 18.0 R eferences________________________ ;_________ ;______ ;________________ ________ 18.1 None 19.0 Affected Documents______________ ______________ ;_____ ._______:_____ 19.1 FACT-M-4, "Analysis o f Serum Extracts for Fluorochemicals using HPLC-Electrospray Mass Spectrometry" 20.0 R ev isio n s Revision Number. Reason For Revision Revision Date 3MEnvironmental Laboratory FACT-M-3.0 Extraction of PFOS from Serum Page 7 of 8 Page 120 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Extraction Worksheet for FACT-M-3 Study # .i. Sample Number set # H ,0 B lank Serum B lank PFOS approx. 0.5 ppm actual #W ppm - - PFOS approx. 5 ppm actual ppm #W - - PFOS approx. 50 ppm actual ppm #W -` - Date and Initials for Std. or Comments - - -. -- - - .- - - -. -' - - - - - - -- - '-. - - - .-- - --- - -. - - - .- - .- - - - .- - - -. -- - 1S t u d v n u m t >er w h e r e t h e o r i g i n a l .w a r k s h e e t is l o c a te d . B lan k Serum Std # Serum am ount Serum E xtraction M ethod : _______ g-----------------------D ate & Initials V o rtex 15 sec. Pipette Serum P ip ette 1 m L o f 0.5 M T B A , pH 10. V olum e S td.# mL _ PiDette 2 m L o f 0.25 N a?C O V 0 .2 5 M N aH C O ^ buffer Std. # Pipette 5 m L o f ethyl acetate T N -A - Shake 20 m i n . ________________________ ;__________________________________________________ ______________________________ C en trifu se 20-25 m in. Centrifuge speed: R e m o v e a 4 m L a liq u o t o f o rg a n ic lay er____________________________ _____ ___ _______________________________________________ _-- ------- Put on N itrogen E vaporator to dryness Evaporator #: ' Tem perature: A dd m ethanol Volum e mL TN-A- V o rte x 3 0 s e c . _______________________________________________________________________ ___ ________________________ F ilter u sin s a 3 cc B -D syringe w ith a 0.2um SRI filter into a 1.5 m L autosam ple vial M S /M S D /___ Cont. Checks: Spiked ______ uL o f a ______ ppm std (________________ ) for a final concentration o f __________ppm . M S /M S D used sa m p le_________________ . Cont. C hecks used sam e serum as for std curve. FACT-M-3.0 Extraction of PFOS from Serum Page 8 of 8 3MEnvironmental Laboratory P age 121 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 3M Environmental Laboratory M ethod E x tr a c tio n o f P o tassium Perfluo ro o ctanesulfo nate o r O t h e r F l u o r o c h e m ic a l c o m p o u n d s f r o m Se r u m f o r A n a l y s is U s in g HPLC- E lectro spray/M a ss Spectro m etry M ethod Number: ETS-8-4.1 Adoption Date: 03/01/99 Author: Lisa Clemen, Glenn Langenburg Revision Date: Approved By: 0 / /S -- Laboratory Manager jjt-- ------ Group Leader - Technical Reviewer Date Date ov/at/w Date ,2 !? 1 .0 S c o p e a n d A p p l ic a t io n G)' 0) O 1.1 Scope: This method is for the extraction o f potassium perfluorooctanesulfonate (PFOS) O O a 1.2 or other fluorochemical compounds from serum. Applicable compounds: Fluorochemical surfactants or other fluorinated compounds. o 1.3 M atrices: Rabbit, rat, bovine, monkey, and human serum or other fluids as designated in the validation report. O, O Word 6/95 ETS-8-4.1 Extraction of PFOS from Serum Page 1 o f 14 3MEnvironmental Laboratory Page 122 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 2.0 S u m m a r y o f M e t h o d ______________;__________ ;_________________________ 2.1 This method describes the procedure for extracting potassium perfluorooctanesulfonate (PFOS) or other fluorochemical surfactants from serum, or other fluids, using an ion pairing reagent and methyl-tert-butyl ether (MtBE). In this method, seven fluorochemicals were extracted: PFOS, PFOSA, PFOSAA, EtFOSE-OH, PFOSEA, M556, and surrogate standard (see 3.0 Definitions). An ion pairing reagent is added to the sample and the analyte ion pair is partitioned into MtBE. The MtBE extract is removed and put onto a nitrogen evaporator until dry. Each extract is reconstituted in 1.0 mL o f methanol, then filtered through a 3 cc plastic syringe attached to a 0.2 pm nylon filter into glass autovials. 2.2 These sample extracts are analyzed following method ETS-8-5.1 or other appropriate methods. 3.0 D e f in it io n s _______ __ _________________________________________ .___________________ 3.1 PFOS: perfluorooctanesulfonate (anion o f potassium salt) C8FI7S 0 3' 3.2 PFOSA: perfluorooctane sulfonylamide C8F,7S 02NH2 3.3 PFOSAA: perfluorooctane sulfonylamido (ethyl)acetate C8F17S 0 2N(CH2CH3)CH2C 0 2' 3.4 EtFOSE-OH: 2(N-ethylperfluorooctane sulfonamido)-ethyl alcohol CgF17S 0 2N(CH2CH3)CH2CH20H 3.5 PFOSEA: perfluorooctane sulfonyl ethylamide C8F17S 0 2N(CH2CH3)H 3.6 M556: C8FI7S 0 2N(H)(CH2COOH) 3.7 Surrogate standard: 1H-1H-2H-2H perfluorooctane sulfonic acid 4.0 W a r n in g s a n d C a u t io n s __________________________________ ;_______________________ 4.1 Health and safety warnings 4.1.1 Use universal precautions, especially laboratory coats, goggles, and gloves when handling animal tissue, which may contain pathogens. 5.0 In t e r f e r e n c e s _______________________ __________________________________________ |_______ 5.1 There are no interferences known at this time. 6.0 E q u ip m e n t ______________________________________________________________________________ 6.1 The following equipment is used while performing this method. Equivalent equipment is acceptable. 6.1.1 Vortex mixer, VWR, Vortex Genie 2 6.1.2 Centrifuge, Mistral 1000 or IEC 6.1.3 Shaker, Eberbach or VWR 3MEnvironmental Laboratory ETS-8-4.1 Extraction of PFOS from Serum Page 2 of 14 P age 123 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 6.1.4 Nitrogen evaporator, Organomation 6.1.5 Balance ( 0.100 g) 7.0 S u p p l ie s a n d M a t e r ia l s ___________________ ;___________ ___________________ 7.1 Gloves 7.2 Eppendorfor disposable pipettes 7.3 Nalgene bottles, capable o f holding 250 mL and 1 L 7.4 Volumetric flasks, glass, type A 7.5 I-CHEM vials, glass, 40 mL glass 7.6 Centrifuge tubes, polypropylene, 15 mL 7.7 Labels 7.8 Oxford Dispenser - 3.0 to 10.0 mL 7.9 Syringes, capable o f measuring 5 pL to 50 pL 7.10 Graduated pipettes 7.11 Syringes, disposable plastic, 3 cc 7.12 Syringe filters, nylon, 0.2 pm, 25 mm 7.13 Timer 7.14 Crimp cap autovials and caps 7.15 Crimpers Note: Prior to using glassware and bottles, rinse 3 times with methanol and 3 times with Milli-QTM water. Rinse syringes a minimum o f 9 times with methanol, 3 rinses from 3 separate vials. 8.0 Reagents and Standards_________________________ ;____________________________ 8.1 Type I reagent grade water, Milli-QTM or equivalent; all water used in this method should be Milli-QTM water and may be provided by a Milli-Q TOC PlusTM system 8.2 Sodium hydroxide (NaOH), J.T Baker or equivalent 8.3 Tetrabutylammonium hydrogen sulfate(TBA), Kodak or equivalent 8.4 Sodium carbonate (Na^O j), J.T. Baker or equivalent 8.5 Sodium bicarbonate (NaHC03), J.T. Baker or equivalent 8.6 Methyl-T-Butyl Ether, Omnisolv, glass distilled or HPLC grade 8.7 Methanol, Omnisolv, glass distilled or HPLC grade 8.8 Serum or blood, frozen from supplier 8.9 Fluorochemical standards 8.9.1 PFOS (3M Specialty Chemical Division), molecular weight = 538 8.9.2 PFOSA (3M Specialty Chemical Division), molecular weight = 499 ETS-8-4.1 Extraction of PFOS from Serum Page 3 of 14 3MEnvironmental Laboratory Page 124 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 8.9.3 PFOSAA (3M Specialty Chemical Division), molecular weight = 585 8.9.4 EtFOSE-OH (3M Specialty Chemical Division), molecular weight = 570 8.9.5 PFOSEA (3M Specialty Chemical Division), molecular weight = 527 8.9.6 M556 (3M Specialty Chemical Division), molecular weight = 557 8.9.7 Surrogate standard: 4-H, perfluorooctane sulfonic acid (1-H,1-H, 2-H, 2-H C8Fl3S 0 3H) molecular weight = 428 8.9.8 Other fluorochemicals, as appropriate 8.10 Reagent preparation NOTE: When preparing larger volumes than listed in reagent, standard, or surrogate preparation, adjust accordingly. 8.10.1 10 N sodium hydroxide (NaOH): Weigh approximately 200 g NaOH. Pour into a 1000 mL beaker containing 500 mL Milli-QTM water, mix until all solids are dissolved. Store in a 1 L Nalgene bottle. 8.10.2 1 N sodium hydroxide (NaOH): Dilute 10N NaOH 1:10. Measure 10 mL o f 10 N NaOH solution into a 100 mL volumetric flask and dilute to volume using Milli-QTM water. Store in a 125 mL Nalgene bottle. 8.10.3 0.5 M tetrabutylammonium hydrogen sulfate (TBA): Weigh approximately 169 g o f TBA into a 1 L volumetric containing 500 mL Milli-QTM water. Adjust to pH 10 using approximately 44 to 54 mL o f 10 N NaOH (While adding the last mL o f ' NaOH, add slowly because the pH changes abruptly). Dilute to volume with Milli-QTM water. Store in a 1 L Nalgene bottle. 8.103.1 TBA requires a check prior to each use to ensure pH = 10. Adjust as needed using 1 N NaOH solution. 8.10.4 0.25 M sodium carbonate/sodium bicarbonate buffer (Na^CO/tSfaHCOj): Weigh approximately 26.5 g o f sodium carbonate (N a^O j) and 21.0 g o f sodium bicarbonate (NaHC03) into a 1 L volumetric flask and bring to volume with MilliQTM water. Store in a 1 L Nalgene bottle. 8.11 Standards preparation 8.11.1 Prepare PFOS standards for the standard curve. 8.11.2 Prepare other fluorochemical standards, as appropriate. Multicomponent fluorochemical standards are acceptable (for example, one working standard solution containing 1.00 ppm PFOS, 1.02 ppm PFOSA, 0.987 ppm PFOSAA, and 1.10 ppm EtFOSE-OH.) 8.11.3 Weigh approximately 100 mg o f PFOS into a 100 mL volumetric flask and record the actual weight. 8.11.4 Bring to volume with methanol for a stock standard o f approximately 1000 ppm (ug/mL). 8.11.5 Dilute the stock solution with methanol for a working standard 1 solution o f approximately 50 ppm. 8.11.6 Dilute working standard 1 with methanol for a working standard 2 solution o f approx. 5.0 ppm. ETS-8-4.1 Extraction of PFOS from Serum Page 4 of 14 3MEnvironmental Laboratory Page 125 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 8.11.7 Dilute working standard 1 with methanol for a working standard 3 solution o f approx. 0.50 ppm. 8.12 Surrogate stock standard preparation 8.12.1 Weigh approximately 50-60 mg o f surrogate standard 1-H,1-H, 2-H, 2-H, CgF13S 0 3H into a 50 mL volumetric flask and record the actual weight. 8.12.2 Bring to volume with methanol for a surrogate stock o f approximately 1000-1200 ppm. 8.12.3 Prepare a surrogate working standard. Transfer approximately 1 mL o f surrogate stock to a 10 mL volumetric flask and bring to volume with methanol for a working standard o f 100 ppm. Record the actual volume transferred. 9.0 S a m p l e H a n d l in g __________ ;__________________________________ '_______________________ 9.1 A ll samples are received frozen and must be kept frozen until the extraction is performed. 9.2 Allow samples to thaw to room temperature prior to extraction. 10.0 Q u a l it y C o n t r o l _________________________ ;____________ _____________________ 10.1 Solvent Blanks, Method blanks and matrix blanks 10.1.1 An aliquot o f 1.0 mL methanol is used as a solvent blank. 10.1.2 Extract two 1.0 mL aliquots o f Milli-QTM water following this procedure and use as method blanks. 10.1.3 Extract two 1.0 mL aliquots o f the serum following this procedure and use as matrix blanks. See 11.1.4. 10.2 Matrix spikes 10.2.1 Prepare and analyze matrix spike and matrix spike duplicate samples to determine the accuracy o f the extraction. 10.2.2 Prepare each spike using a sample chosen by the analyst, usually the control matrix received with each sample set. 10.2.3 Expected concentrations will fall in the mid-range o f the initial calibration curve. Additional spikes may be included and may fall in the low-range o f the initial calibration curve. 10.2.4 Prepare one matrix spike and matrix spike duplicate per 40 samples, with a minimum o f 2 matrix spikes per batch 10.3 Continuing calibration checks 10.3.1 Prepare continuing calibration check samples to ensure the accuracy o f the initial calibration curve. 10.3.2 Prepare, at a minimum, one continuing check per group o f 10 samples. For example, if a sample set = 34, four checks are prepared and extracted. 10.3.3 Prepare each continuing calibration check from the same matrix used to prepare the initial curve. 3MEnvironmental Laboratory ETS-8-4.1 Extraction of PFOS from Serum Page 5 of 14 Page 126 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 10.3.4 The expected concentrations will fall within the mid-range o f the initial calibration curve. Additional spikes may be included that fall in the low-range o f the initial calibration curve. This is necessary if the analyst must quantitate using only the low end o f the calibration curve (for example, 5 ppb - 100 ppb, rather than 5 p p b - 1000 ppb). 11.0 Calibration and Standardization__________________ ;_________ ;______ _________ 11.1 Prepare matrix calibration standards 11.1.1 Transfer 1 mL o f serum to a 15 mL centrifuge tube. 11.1.2 If most sample volumes are less than 1.0 mL, extract standards with matrix volumes equal to the sample volumes. Do not extract less than 0.50 mL o f . matrix. Record each sample volume on the extraction sheet. 11.1.3 While preparing a total o f twenty aliquots in 15 mL centrifuge tubes, mix or shake between aliquots. 11.1.4 Two 1 mL aliquots, or other appropriate volume, serve as matrix blanks. Typically use the standard concentrations and spiking amounts listed in Table 1, at the end o f this section, to spike, in duplicate, two standard curves, for a total o f eighteen standards, two matrix blanks, and two method blanks. 11.1.5 Refer to validation report ETS-8-4.0 & KTS-8-5.0-V-1, which lists the working ranges and the Linear Calibration Range (LCR) for calibration curves. 11.1.6 Use Attachment D as an aid in calculating the concentrations o f the working standards. See Section 13.0 to calculate actual concentrations o f PFOS in calibration standards. 11.2 To each standard, blank, or continuing check, add appropriate amount o f surrogate working standard for the concentration to fall within the calibration curve range 5 ppb 1000 ppb. 1 1 3 Extract spiked matrix standards following 12.6-12.16 o f this method. Use these standards to establish each initial curve on the mass spectrometer. 3MEnvironmental Laboratory ETS-8-4.1 Extraction of PFOS from Serum Page 6 of 14 Page 127 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Table 1 Approximate spiking amounts for standards and spikes Using 1.0 mL o f matrix Working standard pL Approx, final cone, o f (approx, cone.) analyte in matrix - - Blank 0.500 ppm 10 0.005 ppm 0.500 ppm 20 0.010 ppm 5.00 ppm 5 0.025 ppm 5.00 ppm 10 . 0.050 ppm 5.00 ppm . 20 0.100 ppm 50.0 ppm 5 0.250 ppm 50.0 ppm 10 0.500 ppm 50.0 ppm 15 0.750 ppm 50.0 ppm 20 1.00 ppm 12.0 Procedure_____________________________________________________ ______________ 12.1 Obtain frozen samples and allow to thaw at room temperature or in a lukewarm waterbath. 12.2 Vortex mix for 15 seconds, then transfer 1.0 ml- or other appropriate volume to a 15 mL polypropylene centrifuge tube. 12.3 Return unused samples to freezer after extraction,amounts have been removed. 12.4 Record the initial volume on the extraction worksheet. 12.5 Label the tube with the study number, sample ID, date and analyst initials. See attached worksheet for documenting the remaining steps. 12.6 . Spike all samples, including blanks and standards, ready for extraction with surrogate standard as described in 11.2. 12.7 Spike each matrix with the appropriate amount o f standard as described in 11.1, or Table 1 in that section, for the calibration curve standards. Also prepare matrix spikes and continuing calibration standards. 1 12.8 Vortex mix the standard curve samples, matrix spike samples, and continuing calibration samples for 15 seconds. 12.9 Check to ensure the 0.5 M TBA reagent is at pH 10. If not, adjust accordingly. 12.10 To each sample, add 1 mL 0.5 M TBA and 2 mL o f 0.25M sodium carbonate/sodium bicarbonate buffer. 12.11 Using an Oxford Dispenser, add 5 mL methyl-icri-butyl ether. 12.12 Cap each sample and put on the shaker at a setting o f 300 rpm, for 20 minutes. 12.13 Centrifuge for 20 to 25 minutes at a setting o f 3500 rpm, or until layers are well separated. ETS-8-4.1 Extraction of PFOS from Serum Page 7 of 14 3MEnvironmental Laboratory Page 128 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 12.14 Label a fresh 15 mL centrifuge tube with the same information as in 12.5. 12.15 Remove 4.0 mL o f the organic layer to this clean 15 mL centrifuge tube. 12.16 Put each sample on the analytical nitrogen evaporator until dry, approximately 1 to 2 hours. 12.17 Add 1.0 mL o f methanol to each centrifuge tube using a graduated pipette. 12.18 Vortex mix for 30 seconds. 12.19 Attach a 0.2 pm nylon mesh filter to a 3 cc syringe and transfer the sample to this . syringe. Filter into a 1.5 mL glass autovial or low-volume autovial when necessary. 12.20 Label the autovial with the study number, animal number and gender, sample timepoint, matrix, final solvent, extraction date, and analyst(s) performing the extraction. 12.21 Cap and store extracts at room temperature or at approximately 4 C until analysis. 12.22 Complete the extraction worksheet, attached to this document, and tape in the study notebook or include in study binder, as appropriate. 13.0 D a t a A n a l y s is a n d C a l c u l a t io n s ___________________________________ :______________ 13.1 Calculations 13.1.1 Calculate actual concentrations o f PFOS, or other applicable fluorochemical, in calibration standards using the following equation: mL o f standard x concentration o f standard fug /mL>___________ ;______ .= . mL o f standard + mL o f surrogate standard + initial matrix volume (mL) Final Concentration (pg/mL) o f PFOS in matrix 1 4 .0 M e t h o d P e r f o r m a n c e _______________________ ;________________________________________ 14.1 The method detection limit (MDL) is analyte and matrix specific. Refer to MDL report for specific MDL and limit o f quantitation (LOQ) values (see Attachments B and C). 14.2 The following quality control samples are extracted with each batch o f samples to evaluate the quality o f the extraction and analysis. 14.2.1 Method blanks and matrix blanks. . 14.2.2 Matrix spike and matrix spike duplicate samples to determine accuracy and precision o f the extraction. 14.2.3 Continuing calibration check samples to determine the continued accuracy o f the initial calibration curve. 14.3 Refer to section 14 o f ETS-8-5.1 for method performance criteria. 1 5 .0 P o l l u t io n P r e v e n t io n a n d W a s t e M a n a g e m e n t ____________________________ 15.1 Sample waste is disposed in biohazard containers, flammable solvent waste is disposed in high BTU containers, and used glass pipette waste is disposed in broken glass containers located in the laboratory. ETS-8-4.1 Extraction of PFOS from Semm Page 8 of 14 3MEnvironmental Laboratory Page 129 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 16.0 Records____________ ;____________ ;________________ ______________________ 16.1 Complete the extraction worksheet attached to this method, and tape in the study notebook or include in the 3-ring study binder, as appropriate. 17.0 Attachments____________________________________ __________.____________ 17.1 Attachment A, Extraction worksheet 17.2 Attachment B, MDL/LOQ values and summary 17.3 Attachment C, Calibration standard concentration worksheet 18.0 References______________________________ __________________________ __ 18.1 The validation report associated with this method is ETS-8-4.0 & 5.0-V -l. 18.2 FACT-M-3.1, "Analysis o f Serum or Other Fluid Extracts for Fluorochemicals using HPLC-Electrospray Mass Spectrometry" 19.0 Affected Documents____________________________________________________ 19.1 ETS-8-5.1, "Analysis o f Serum or Other Fluid Extracts for Fluorochemicals using HPLC-Electrospray Mass Spectrometry" 20.0 Revisions ______________;__________________ ;_________________________ Revision Number 1 Reason For Revision Section 12.21 Changed to include sample storage at room temperature. Section 12.13 Added the shaker speed. Section 12.17 Final volume is 1.0 mL; not adjusted for initial volumes less than 1.0 mL. Revision Date 04/02/99 3MEnvironmental Laboratory . ETS-8-4.1 Extraction of PFOS from Serum Page 9 o f 14 Page 130 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Extraction Worksheet ETS-8-4.1 Studv # Matrix Box# Wk/Dav DateSpiked/Analyst CCV MS MSD Surrogate Std approx, ppm actual ppm # FC -M ix approx. 0.5 pm actual ppm # FC-Mix approx. 5 ppm actual ppm # FC-Mix approx. 50 ppm actual ppm # Comments B la n k Serum Extraction M ethod Vortex 15 sec. Std# - - : - - - - - - '- am ount- Pipette M atrix Volum e mL Pipette 1 m L o f 0.5 M TBA , pH 10. pH = Std. # Pipette 2 m L o f 0.25 Na2CO.VO.25M N aH C O i buffer S td .# D ispense 5 m L o f m ethyl-t-butyl ether T N -A - Shake 20 min. Shaker speed: Centrifuge 20-25 m in. R em ove a 4 m L aliauot o f organic laver Centrifuge speed: Put on N itrogen Evaporator to drvness Temperature: Add methanol Volum e mL TN-A- Vortex 30 sec. Filter usin g a 3 c c B -D svringe with a 0.2 u m filter into a 1.5 mL autosam nle vial C ont. C al. V erificatio n s u sed sam e m atrix as for std curve. - - - - - - .- - - r - .- - - mL D ate & Initials A ttachm ent A 3MEnvironmental Laboratory ETS-8-4.1 Extraction of PFOS from Serum Page 10 of 14 P age 131 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 MDL/LOQ values for rabbit serum Compound MDL LOQ Linear Calibration Range (LCR) (PPb) (PPb) Approximate concentrations to be used for preparing the Standard Calibration Curve PFOS 1.74 5.55 5ppb- 1000ppb PFOSA 1.51 4.79 5ppb-1000ppb PFOSAA 3.46 20.5 5ppb- 1000 ppb EtFOSE-OH 11.4 36.2 5ppb - 1000 ppb M556 6.03 19.2 5 ppb -1000 ppb PFOSEA 5.71 18.2 5ppb-1000 ppb MDL/LOQ values in rat, bovine, monkey, and human serum, and monkey plasma were not statistically determined. Two curves in each of these matrices were extracted and analyzed with the rabbit serum curves to determine equivalence. Responses in the rat, bovine, monkey, and human were equivalent to the rabbit responses, therefore, their MDL and LOQ will be the same values as determined in rabbit serum. Please see LOQ Summary and MDL study in ETS-8-4.0 & 5.0-V-l for further information. Attachment B: MDL/LOQ Summary ETS-8-4.1 Extraction of PFOS from Serum 3MEnvironmental Laboratory Page 11 of 14 Page 132 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Compound: P FOS Prepared range Rabbit Serum of standards (ppb) (ng/mL) Full Range Low Curve High curve 1/X 0.995 - 978 4.94 - 248 97.8 - 978 0.995 - 978 LCR from curve (ppb) (ng/mL) 24.8 - 978 4.94 - 248 97.8-978 4.94 - 978 %Recovery Range 83-108 85-104 85-106 94-111 Compound: PFOSA Prepared range Rabbit Serum of standards (ppb) (ng/mL) Full Range Low Curve High curve 1/X . 0.993 - 976 4.93 - 97.6 24.8 - 976 0.993 - 976 LCR from curve (Ppb) (ng/mL) 4.93 - 976 %Recovery Range 88-103 4.93 - 97.6 . 87-105 24.8-978 93-102 4.93-976 94-103 Compound; PFOSAA Prepared range Rabbit Serum of standards (ppb) (ng/mL) Full Range Low Curve High curve !/X 0.991 - 974 4.92 - 247 49.2-974 0.991 - 974 LCR from curve (PPb) (ng/mL) 24.7 - 974 9.74 - 247 97.4 - 974 9.74-974 %Recovery Range 81-111 97-107 85-108 95-115 RSD Range 4.67-11.0 5.34-12.0 4.84-9.80 4.60-10.5 RSD Range 5.10-14.7 9.85-14.7 5.08-13.9 5.10-14.5 RSD Range 4.18-10.6 6.38-21.8 4.33-12.5 4.11-23.2 Attachment B: MDL/LOQ Summary 3MEnvironmental Laboratory ETS-8-4.1 Extraction of PFOS from Scrum Page 12 of 14 P age 133 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 0 1 I' Compound; EtFOSE-OH Prepared range Rabbit Serum of standards (ppb) (ng/mL) Full Range 0.993 - 976 LCR from curve (ppb) (ng/mL) . 49.3 -976 Low Curve 4.93-97.6 9.76-97.6 High curve 49.3 - 976 97.6 - 976 1/X 0.993 - 493 9.76 - 976 %Recovery Range 77-110 97-107 90-109 86-111 Compound: P Prepared range Rabbit Serum of standards (ppb) (ng/mL) Full Range Low Curve High curve 1/X 0.993-976 4.93 - 248 49.3 - 976 0.993 - 976 LCR from curve (Ppb) (ng/mL) 24,8 - 976 9.76 - 248 49.3 - 976 9.76 - 976 % Recovery Range 96-106 91-110 86-106 95-117 Compound: M556 Prepared range Rabbit Serum of standards (ppb) (ng/mL) Full Range Low Curve High curve 1/X 0.993 - 976 4.93 - 97.6 97.6-976 0.993 - 976 LCR from curve (ppb) (ng/mL) 24.8-976 9.76 - 97.6 97.6 - 976 9.76-976 %Recovery Range 88-106 100-105 81-111 97-110 RSD Range 11.2-25.5 14.1-21.3 11.5-19.6 11.1-21.2 RSD Range 10.1-16.2 11.8-19.5 10.2-18.2 10.1-19.1 RSD Range 4.82-17.9 5.95-18.2 5.11-9.74 4.77-19.5 Attachment B: MDL/LOQ Summary 3MEnvironmental Laboratory ETS-8-4.1 Extraction of PFOS from Serum Page 13 of 14 Page 134 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Ion Pair Standard Curves - Fluids Prep date(s): Standard number: Analyte(s): Equipment number: Sample matrix: Final solvent andTN: Blank fluid/identifier: Method/revision: Target analyte(s): FC mix std approx. O.SOOppm: FC mix std approx. 5.00ppm: . FC mix stdapprox. 50.0ppm: Surrogate std approx. 100ppm: Actual concentrations of standards in the FC mix PFOS PFOSA PFOSAA EtFOSE PFOSEA Std cone Std cone Stdcone Stdcone Stdcone ug/mL ug/mL ug/mL ug/mL ug/mL 0 .5 0 0 0 .5 0 7 0 .5 3 2 0 .5 0 1 0 .5 2 1 0 .5 0 0 0 .5 0 7 0 .5 3 2 0 .5 0 1 0 .5 2 1 5 .00 5 .0 7 5 .3 2 5 .0 1 5 .2 1 5 .00 5 .0 7 5 .3 2 5 .0 1 5 .2 1 5 .00 5 .0 7 5 .3 2 5 .0 1 5 .2 1 5 0.0 5 0 .1 5 3 .2 50.1 52.1 5 0 .0 5 0 .1 5 3 .2 50.1 5 2 .1 5 0 .0 5 0 .1 5 3 .2 50.1 5 2 .1 5 0 .0 5 0 .1 5 3 .2 50.1 5 2 .1 M556 Std cone ug/mL 0 .5 0 1 0 .5 0 1 5 .0 1 5.01 5 .0 1 5 0 .1 5 0 .1 5 0 .1 5 0 .1 AU Am't spikedmL 0 .0 1 0 0 .0 2 0 0 .0 0 5 0 .0 1 0 0 .0 2 0 0 .0 0 5 0 .0 1 0 0 .0 1 5 0 .0 2 0 All Final voi mL 1 .0 1 5 1 .0 2 5 1 .0 1 0 1 .0 1 5 1 .0 2 5 1 .0 1 0 1 .0 1 5 1 .0 2 0 1 .0 2 5 Calculated concentrations of standards in the sample matrix PFOS Final cone ng/m L 4.93 9.76 24.8 49.3 97.6 248 493 735 976 PFOSA Final cone ng/m L 5.00 9.89 25.1 5 0 .0 98.9 251 500 746 989 PFOSAA Final cone ng/m L 5.24 10.4 26.3 52.4 . 104 263 524 782 1038 EtFO SE Final cone ng/m L 4.94 9.78 24.8 49.4 97.8 248 494 737 978 PFOSEA Final cone ng/m L 5.01 9.93 25.2 50.1 99.3 252 501 749 993 M 556 Final cone ng/m L 5.13 10.2 25.8 51.3 102 258 513 766 1017 Surrogate Std cone ng/m L 100 Surrogate Final cone ng/m L 500 U A m t spiked mL 0.005 Validated ranges- approximate concentrations Serum Rabbit . B o v in e Rat M onkey & Plasm a PFOS PFOSA PFOSAA 5.00-1000 | 5.00-1000 1 5.00-1000 Estimates only. U se values for rabbit Estim ates only. U se values for rabbit. Estim ates only. U se values for rabbit. Human Estim ates on ly. U se values for rabbit. E tF O S E -O H 1 5.00-1000 | . PFOSEA 5 .0 0 -1 0 0 0 M 556 1 5.00-1000 Attachment C: Ion Pair Standard Curves ETS-8-4.1 . Extraction of PFOS from Serum 3MEnvironmental Laboratory Page 14 of 14 Page 135 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 3M Environmental Laboratory M ethod E x t r a c t io n o f P o ta ssiu m P er flu o r o o c ta n esu lfo n a te o r o th er F l u o r o c h e m ic a l C o m po u n d s fr o m L iv e r fo r A n a l y sis u sin g H P L C - E l e c t r o spr a y /M a ss Spe c t r o m e t r y M ethod Num ber: ETS-8-6.0 Author: Lisa Clemen, Robert Wynne Approved By: Adoption Date: Revision Date: Group Leader Date (d * A CtuYtJLU. Technical Reviewer ________ oi/wh'i Date 5 1$ m X D3 S - 1.0 S c o p e a n d A p pl ic a t io n 1.1 Scope: This method is for the extraction o f potassium perfluorooctanesulfonate (PFOS) or TJ other fluorochemical compounds from liver. D 1 1.2 A pplicable Com pounds: Fluorochemical surfactants or other fluorinated compounds. . q 1.3 M atrices: Rabbit, rat, bovine, and monkey livers or other tissues as designated in the 0 is. validation report. <o u' 9 ! Word 6.0/95 ETS-8-6.0 Page 1 of 14 3MEnvironmental Laboratory Page 136 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 2.0 Summary of Method_______________________________ _______________ _________ 2.1 This method describes the procedure for extracting potassium perfluorooctanesulfonate (PFOS) or other fluorochemical surfactants from liver, or other tissues, using an ion pairing reagent and methyl-teri-butyl ether (MtBE). In this method, seven fluorochemicals can be extracted: PFOS, PFOSA, PFOSAA, EtFOSE-OH,.PFOSEA, M556, and surrogate standard. An ion pairing reagent is added to the sample and the analyte ion pair is partitioned into MtBE. The MtBE extract is transferred to a centrifuge tube and put onto a nitrogen evaporator until dry. Each extract is reconstituted in 1.0 mL methanol then filtered through a 3 cc plastic syringe attached to a 0.2 pm nylon filter into glass autovials. 2.2 These sample extracts are analyzed following method ETS-8-7.0 or other appropriate methods. 3.0 Definitions_______________ :____________________________ _____________________ 3.1 PFOS: perfluorooctanesulfonate (anion o f potassium salt) C8FI7S 0 3 3.2 PFOSA: perfluorooctane sulfonylamide C8F17S 0 2NH2 3.3 PFOSAA: perfluorooctane sulfonylamido (ethyl)acetate C8F17S 0 2N(CH2CH3)CH2C 0 2 3.4 EtFOSE-OH: 2(N-ethylperfluorooctane sulfonamido)-ethyl alcohol C8F 17S 0 2N(CH2CH3)CH2CH20 H 3.5 PFOSEA: perfluorooctane sulfonyl ethylamide C8F17S 0 2N(CH2CH3)H 3.6 M556: C8F 17S 0 2N(H)(CH2C 00 H ) 3.7 Surrogate standard: 1H-1H-2H-2H perfluorooctane sulfonic acid 4.0 Warnings and Cautions________________________________ :___________________ 4.1 Health and Safety Warnings: 4.1.1 U se universal precautions, especially laboratory coats, goggles, and gloves when handling animal tissue, which may contain pathogens. 5.0 Interferences_____________________________________________________________ 5.1 There are no interferences known at this time. 6.0 Equipment________________________________________________________________ 6.1 The following equipment is used while performing this method. Equivalent equipment is acceptable. 6.1.1 6.1.2 6.1.3 6.1.4 Ultra-Turrax T25 Grinder for grinding liver samples Vortex mixer, VWR, Vortex Genie 2 Centrifuge, Mistral 1000 or IEC Shaker, Eberbach or VWR 3MEnvironmental Laboratory ETS-8-6.0 Page 2 of 14 Page 137 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 6.1.5 Nitrogen Evaporator, Organomation 6.1.6 Balance (sensitivity to 0.100 g) 7 .0 S u p p l ie s a n d M a t e r ia l s _____________________________________________ _____________________ 7.1 Gloves 7.2 Dissecting scalpels 7.3 Eppendorf or disposable pipettes 7.4 Nalgene bottles, capable o f holding 250 mL and 1 L 7.5 Volumetric flasks, glass, type A 7.6 I-CHEM vials, 40 mL glass 7.7 Plastic sampule vials, Wheaton, 6 mL (or appropriate size) 7.8 Centrifuge tubes, polypropylene, 15 mL 7.9 Labels 7.10 Oxford Dispensor - 3.0 to 10.0 ml 7.11 Syringes, capable o f measuring 5 pL to 50 pL 7.12 Graduated pipettes 7.13 Syringes, disposable plastic, 3 cc 7.14 Syringe filters, nylon, 0.2 pm, 25 mm 7.15 Timer 7.16 Crimp cap autovials and caps 7.17 Crimpers Note: Prior to using glassware and bottles, rinse 3 times with methanol and 3 times with Milli- QTM water. Rinse syringes a minimum o f 9 times with methanol, 3 rinses from 3 separate vials. 8 .0 R e a g e n t s a n d S t a n d a r d s ________________________________________________________________ 8.1 Type I reagent grade water, Milli-QTM or equivalent; all water used in this method should be Milli-QTM water and be provided by a Milli-Q TOC PlusTM system 8.2 Sodium hydroxide (NaOH), J.T Baker or equivalent 8.3 Tetrabutylammonium hydrogen sulfate(TBA), Kodak or equivalent 8.4 Sodium carbonate (N a^O j), J.T. Baker or equivalent 8.5 Sodium bicarbonate (NaHC03), J.T. Baker or equivalent 8.6 Methyl-teri-butyl ether, Omnisolv, glass distilled or HPLC grade 8.7 Methanol, Omnisolv, glass distilled or HPLC grade 8.8 Liver, frozen from supplier 8.9 Dry ice from supplier 8.10 Fluorochemical standards 8.10.1 PFOS (3M Specialty Chemical Division), molecular weight = 538 3MEnvironmental Laboratory ETS-8-6.0 Page 3 of 14 Page 138 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 8.10.2 PFOSA (3M Specialty Chemical Division), molecular weight = 499 8.10.3 PFOSAA (3M Specialty Chemical Division), molecular weight = 585 8.10.4 EtFOSE-OH (3M Specialty Chemical Division), molecular weight = 570 8.10.5 PFOSEA (3M Specialty Chemical Division), molecular weight = 527 8.10.6 M556 (3M Specialty Chemical Division), molecular weight = 557 8.10.7 Surrogate standard: 4-H, perfluorooctane sulfonic acid (1-H,1-H, 2-H, 2-H C8FI3S 0 3H) molecular weight = 428 8.10.8 Other fluorochemicals, as appropriate 8.11 Reagent preparation NOTE: When preparing larger volumes than listed in reagent, standard, or surrogate preparation, adjust accordingly. 8.11.1 10 N sodium hydroxide (NaOH): Weigh approximately 200 g NaOH. Pour into a 1000 mL beaker containing 500 mL Milli-QTM water, mix until all solids are . dissolved. Store in a 1 L Nalgene bottle. 8.11.2 1 N sodium hydroxide (NaOH): Dilute 1 0 N NaOH 1:10. Measure 10 mL o f 1 0 N NaOH solution into a 100 mL volumetric flask and dilute to volume using Milli-QTM water. Store in a 125 mL Nalgene bottle. 8.11.3 0.5 M tetrabutylammonium hydrogen sulfate (TBA): Weigh approximately 169 g o f TBA into a 1 L volumetric containing 500 mL Milli-QTM water. Adjust to pH 10 using approximately 44 to 54 mL o f 10 N NaOH (While adding the last mL o f NaOH, add slowly because the pH changes abruptly). Dilute to volume with Milli-QTM water. Store in a 1 L Nalgene bottle. 8.11.3.1 TBA requires a check prior to each use to ensure pH = 10. Adjust as needed using 1 N NaOH solution. 8.11.4 0.25 M sodium carbonate/sodium bicarbonate buffer (Na^Oj/NaHCO^: Weigh approximately 26.5 g o f sodium carbonate (N a^O j) and 21.0 g o f sodium bicarbonate (NaHC03) into a 1 L volumetric flask and bring to volume with MilliQTM water. Store in a 1 L Nalgene bottle. 8.12 Standards preparation 8.12.1 Prepare PFOS standards for the standard curve. 8.12.2 Prepare other fluorochemical standards, as appropriate. Multicomponent fluorochemical standards are acceptable (for example, one working standard solution containing 1.00 ppm PFOS, 1.02 ppm PFOSA, 0.987 ppm PFOSAA, and 1.10 ppm EtFOSE-OH.) . 8.12.3 Weigh approximately 100 mg o f PFOS into a 100 mL volumetric flask and record the actual weight. 8.12.4 Bring to volume with methanol for a stock standard o f approximately 1000 ppm (pg/mL). 8.12.5 Dilute the stock solution with methanol for a working standard 1 solution o f approximately 50 ppm. 3MEnvironmental Laboratory ETS-8-6.0 Page 4 o f 14 Page 139 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 8.12.6 Dilute the stock solution with methanol for a working standard 2 solution o f approx. 5.0 ppm. 8.12.7 Dilute the stock solution with methanol for a working standard 3 solution o f approx. 0.50 ppm. 8.13 Surrogate stock standard preparation 8.13.1 Weigh approximately 50-60 mg o f surrogate standard 1-H,1-H, 2-H, 2-H, C8FI3S 0 3H into a 50 ml volumetric flask and record the actual weight. 8.13.2 Bring to volume with methanol for a surrogate stock o f approximately 1000-1200 ppm. 8.13.3 Prepare a surrogate working standard. Transfer approximately 1.0 ml o f surrogate stock to a 10 ml volumetric flask and bring to volume with methanol for a working standard o f 10-20 ppm. Record the actual volume transferred. 9.0 Sample Handling_____________________________________ ____________________ 9.1 All samples are received frozen and must be kept frozen until the extraction is performed. 10.0 Quality Control_____________________________________ __________________ 10.1 Matrix blanks and method blanks . 10.1.1 An aliquot o f 1.0 mL methanol is used as a solvent blank. 10.1.2 Extract two 1.0 mL aliquots o f Milli-QTM water following this procedure and use as method blanks. 10.1.3 Extract two 1.0 mL aliquots o f liver homogenate following this procedure and use as matrix blanks. Refer to 11.1.6. 10.2 Matrix spikes 10.2.1 Prepare and analyze matrix spike and matrix spike duplicate samples to determine the accuracy o f the extraction. 10.2.2 Prepare each spike using a sample chosen by the analyst, usually a control liver received with each sample set. 10.2.3 Expected concentrations will fall in the mid-range o f the initial calibration curve. Additional spikes may be included and may fall in the low-range o f the initial calibration curve. 10.2.4 Prepare one matrix spike and matrix spike duplicate per 40 samples, with a minimum o f 2 matrix spikes per batch. 10.3 Continuing calibration verifications 10.3.1 Prepare continuing calibration verification samples to ensure the accuracy o f the initial calibration curve. 10.3.2 Prepare, at a minimum, one continuing calibration verification sample per group o f 10 samples. For example, if a sample set =. 34, four verifications are prepared and extracted. 3MEnvironmental Laboratory ETS-8-6.0 Page 5 o f 14 Page 140 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 10.3.3 Prepare each continuing calibration verification from the same matrix used to prepare the initial curve. 10.3.4 The expected concentrations w ill fall within the mid-range o f the initial calibration curve. Additional spikes may be included that fall in the low-range o f the initial calibration curve. This is necessary if the analyst must quantitate using only the low end o f the calibration curve (for example, 5 ppb - 100 ppb, rather than 5 ppb - 1000 ppb). 11.0 Calibration and Standardization___________________ ______________________ 11.1 Prepare matrix calibration standards ' 11.1.1 Weigh approximately 40 g o f liver into a 250 mL Nalgene bottle containing 200 mLs Milli-QTM water. Grind to a homogeneous solution. 11.1.2 If 40 g is not available, use appropriate amounts o f liver and water to ensure a 1:5 ratio. 11.1.3 Refer to 13.0 to calculate the actual density o f liver homogenate and the concentration o f solid liver tissue dispersed in 1.0 mL o f homogenate solution. 11.1.5 Add 1 mL o f homogenate to a 15 mL centrifuge tube. Re-suspend solution by shaking between aliquots while preparing a total o f eighteen 1 mL aliquots o f homogeneous solution in 15 mL centrifuge tubes. 11.1.6 Two 1 mL aliquots, or other appropriate volume, serve as matrix blanks. 11.1.7 Typically use the standard concentrations and spiking amounts listed in Table 1, at the end o f this section, to spike, in duplicate, two standard curves, for a total o f eighteen samples, two matrix blanks, and two method blanks. 11.1.8 Refer to validation reports ETS-8-6.0 and ETS-8-7.0-V-1 or Attachment B, which lists the working ranges and the Linear Calibration Range (LCR) for calibration curves. 11.1.9 U se Attachment C as an aid in calculating the concentrations o f the working standards. Refer to 13.0 to calculate actual concentrations o f PFOS in calibration standards. 11.2 To each working standard, blank, or continuing verification, add appropriate amount o f surrogate working standard for the concentration to fall within the calibration curve range 5 ppb-lOOOppb. 3MEnvironmental Laboratory ETS-8-6.0 Page 6 of 14 P age 141 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 11.3 Extract spiked liver homogenates following 12.14-12.25 o f this method. Use these standards to establish each initial curve on the mass spectrometer. Table 1 Approximate Spiking Amounts for Calibration Standards Working Standard (Approx. Cone.) 0.50 ppm 0.50 ppm 0.50 ppm 0.50 ppm 0.50 ppm 5.0 ppm 5.0 ppm 5.0 ppm 50 ppm l '2 4 10 20 40 10 20 30 4 Approx, final cone, o f PFOS in liver Blank 0.005 ppm 0.010 ppm 0.025 ppm 0.050 ppm 0.100 ppm 0.250 ppm 0.500 ppm 0.750 ppm 1.00 ppm 12.0 Procedure____________________________________________________ __________ 12.1 Obtain frozen liver samples. 12.2 Cut approximately 1 g o f liver using a dissecting scalpel. This part o f the procedure is best performed quickly, not allowing the liver to thaw. 12.3 Weigh the sample directly into a tared plastic sampule vial. 12.4 Record the liver weight in'the study notebook. 12.5 Return unused liver portions to freezer. 12.6 Add 2.5 mLs o f water to sampule vial. 12.7 Grind the sample. Put the grinder probe in the sample and grind for about 2 minutes, or until the sample is homogeneous. 12.8 Rinse the probe into the sample with 2.5 mLs water using a pipette. 12.9 Take the grinder apart and clean it with methanol after each sample. Refer to AMDT-EP- 22. 12.10 Cap the sample and vortex for 15 seconds. Label the sampule vial with the study number, weight, liver ID, date and analyst initials. 3MEnvironmental Laboratory ETS-8-6.0 Page 7 o f 14 Page 142 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 12.11 Pipette 1.0 mL, or other appropriate volume, o f homogenate into a 15 mL polypropylene centrifuge tube. Label the centrifuge tube with the identical information as the sampule vial. Refer to attached worksheet for documenting the remaining steps. 12.12 Pipette two 1 mL aliquots o f Milli-QTM water to centrifuge tubes. These will serve as method blanks. 12.13 Spike all samples, including blanks and standards ready for extraction with surrogate standard as described in section 11.2. 12.14 Spike each matirx with the appropriate amount o f standard as described in 11.1, or Table 1 o f that section, for the calibration curve standards. Also prepare matrix spikes and continuing calibration standards. . 12.15 Vortex mix the standard curve samples, matrix spike samples, and continuing calibration samples for 15 seconds. 12.16 Check to ensure 0.5 M TBA reagent is at pH 10. If not, adjust accordingly. 12.17 To each sample, add 1 mL 0.5 M TBA and 2 mL o f the 0.25 M sodium carbonate/sodium bicarbonate buffer. 12.18 Using an Oxford Dispenser, add 5 mL methyl-ter/-butyl ether. 12.19 Cap each sample and put on the shaker at a setting o f 300 rpm, for 20 minutes. 12.20 Centrifuge for 20 to 25 minutes at a setting o f 3500 rpm, or until layers are well separated. 12.21 Label a fresh 15 mL centrifuge tube with the same information as in 12.10. 12.22 Remove 4.0 mL o f the organic layer to the fresh 15 mL centrifuge tube. 12.23 Put each sample on the analytical nitrogen evaporator until dry, approximately 1 to 2 hours. 12.24 Add 1.0 mL to each centrifuge tube using a graduated pipette. 12.25 Vortex mix for 30 seconds. 12.26 Attach a 0.2 pm nylon mesh filter to a 3 cc syringe and transfer the sample to this syringe. Filter into a 1.5 mL glass autovial or low-volume autovial when necessary. 12.27 Label the autovial with the study number, animal number and gender, sample timepoint, matrix, final solvent, extraction date, and analyst(s) performing the extraction. 12.28 Cap and store extracts at room temperature or at approximately 4 C until analysis. 12.29 Complete the extraction worksheet, attached to this document, and tape in study notebook or include in study binder, as appropriate. 3MEnvironmental Laboratory ETS-8-6.0 Page 8 o f 14 P age 143 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 13.0 Data Analysis and Calculations____________________ _________________ _ 13.1 Calculations: 13.1.1 Calculate the average density o f the liver homogenate by recording each mass o f ten separate 1.0 mL aliquots o f homogenate. Average density (mg/mL) = Average mass fmel o f the aliquots 1.0 mL aliquot 13.1.2 Calculate the amount o f liver (mg) per 1.0 mL homogenate (or concentration o f dispersed solid tissue per mL o f homogenate suspension) using the following equation: g o f Liver x Average density* o f homogenate (mg/mLl (g o f Liver + g o f Water) * refer to 13.1.1 for details. 13.1.3 Calculate actual concentrations o f PFOS and other fluorochemicals in calibration standards using the following equation: uL o f Standard x Concentration fug /mL) = Final Concentration (pg/g or mg/kg) mg L iv e r /1 mL homogenate* o f PFOS in Liver *refer to 13.1.2 for details. 14 .0 M e t h o d P e r f o r m a n c e ___________________________________________________________________ 14.1 The method detection limit (MDL) is analyte and matrix specific. Refer to MDL report for specific MDL and limit o f quantitation (LOQ) values (refer to Attachments B and C). 14.2 The following quality control samples are extracted with each batch o f samples to evaluate the quality o f the extraction and analysis. 14.2.1 Method blanks and matrix blanks. 14.2.2 Matrix spike and matrix spike duplicate samples to determine accuracy and . precision o f the extraction. 14.2.3 Continuing calibration verification samples to determine the continued accuracy o f the initial calibration curve. 14.3 Refer to section 14 o f ETS-8-7.0 for method performance criteria. 1 5 .0 P o l l u t i o n P r e v e n t i o n a n d W a s t e M a n a g e m e n t _____________________________________ 15.1 Sample waste is disposed in biohazard containers, flammable solvent waste is disposed in high BTU containers, and used glass pipette waste is disposed in broken glass containers located in the laboratory. 3MEnvironmental Laboratory ETS-8-6.0 Page 9 of 14 Page 144 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 16.0 R ecords_______________________________________________________ _______________ 16.1 Complete the extraction worksheet attached to this method, and tape in the study notebook or include in the 3-ring study binder, as appropriate. 17.0 T ables. D iagrams. Flowcharts, and Validation Data 17.1 Attachment A, Extraction worksheet ______________________ 17.2 Attachment B, MDL/LOQ values and summary 17.3 Attachment C, Calibration standard calculation and concentration worksheet 18.0 R eferences_________________________________________________ __________________ 18.1 The validation report associated with this method is ETS-8-6.0 & 7.0-V-l. 18.2 AMDT-EP-22, "Routine Maintenance o f Ultra-Turrax T-25" 18.3 FACT-M-1.1, "Extraction o f PFOS or Other Anionic Fluorochemical Surfactants from Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry" 19.0 A ffected Documents__________________________________________________ ________ 19.1 ETS-8-7.0, "Analysis o f Liver Extracts for Fluorochemicals using HPLC-Electrospray Mass Spectrometry" 20.0 Revisions Revision Number. Reason For Revision Revision Date 3MEnvironmental Laboratory ETS-8-6.0 Page 10 of 14 Page 145 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Study # Matrix Box # Wk/Day Date Spiked/Analyst ccv MS MSD Surrogate Std approx, ppm actual ppm # FC Mix Std approx. 0.5 ppm actual ppm # FC Mix Std approx. 5 ppm actual ppm # FC Mix Std approx. 50 ppm actual ppm # Comments -- -- -- -- -- -- - - - - -- -- - - -- .- - -- -- B lan k L iver H om ogenate: L iver E x tractio n M eth od Std # : L iver am ount = Soike surrogate and S tan d ard m ix. V o rtex 15 sec. Pioette 1 m L o f L iver S olution Pipette 1 m L o f |0 .5 M T B A , pH 10. oH = S td.# Pipette 2 m L o f 0.25 N a2CC>3/0.25M N aH C O ^ B uffer S td.# D ispense 5m l o f M ethyl-t-B utyl E ther TN -A - Shake 20 m in. C entrifuge 20-25 m in. Rem ove a 4 m L aliquot o f organic laver Put on N itrogen EvaD orator to dryness A dd 1.0 m L o f M eth an o l Shaker Speed C entrifuge Speed Evanorator T em perature T N -A - V ortex 30 sec. Filter using a 3cc B -D sv rin g e w ith a 0 .2 u m SRI filter into autosam ple vial Cont. Cal. V erifications used the sam e m atrix as for the standard curve. Attachment B: MDL/LOQ Values 3MEnvironmental Laboratory ETS-8-6.0 . R - - D ate & Initials Page 11 of 16 Page 146 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 MDL/LOQ values for rabbit liver Compound MDL LOQ Linear Calibration Range (LCR) (PPb) (PPb) Approximate concentrations to be used for preparing the Standard Calibration Curve PFOS 8.45 26.9 3 0 p p b - 1200 ppb PFOSA 3.50 11.1 1 2 p p b - 1200 ppb PFOSAA 24.6 78.3 30 ppb - 1200 ppb EtFOSE-OH 108 345 60 ppb - 900 ppb* M556 82.3 262 60 ppb - 1200 ppb PFOSEA 33.9 108 30 p p b -1200 ppb MDL/LOQ values in rat, bovine, and monkey liver were not statistically determined. Two curves in each o f these matrices were extracted and analyzed with the rabbit liver curves to determine equivalence. Responses in the rat, bovine, and monkey liver curves were equivalent to the rabbit responses, therefore, their MDL and LOQ will be assumed to be equivalent to those values as determined for the rabbit liver. Refer to LOQ Summary and MDL study in ETS-8-6.0 & 7.0-V-l for further information * EtFOSE-OH estimates only for MDL and LOQ. Did not meet criteria for validation. Compound: PFOS_____________________________________ _________________ Prepared Range o f LCR from Range o f LCR from Range o f Liver range o f average ave curve low std low std high std m atrix standards curve : curve ' curve curve (ppb) (ng/mL) (ppb) (ng/mL) : (ppb) (ng/mL) (ppb) (ng/mL) (ppb) (ng/mL) (ppb) (ng/mL) LCR from h igh std -cu rv e (ppb) (ng/mL) R ab b it 6.19-123 7 12 - 1200 12 - 1200 6 -3 0 0 : 12-300 6 0 - 1200 : 60 - 1200 ! Compound: PFOSA Prepared Liver m atrix range o f s ta n d a rd s (ppb) (ng/mL) Range o f average curve (ppb) (ng/mL) LC R from ave curve . (ppb) (ng/mL) : Range o f low std curve (ppb) (ng/mL) LCR from . low std curve ` (ppb) (ng/mL) Range o f high std curve (ppb) (ng/mL) LCR from high std 1 curve (ppb) (ng/mL) Rabbit 6 .1 9 -1 2 3 7 12 - 1200 12- 1200 . 1 2 -3 0 0 1 2 -3 0 0 6 0 - 1200 60 - 1200 Compound: PFOSAA Liver m atrix Prepared range o f standards (ppb) (ng/mL) Range of average curve (ppb) (ng/mL) R a b b it 6 .1 6 -1 2 3 2 1 2 -1 2 0 0 LCR from ave curve (ppb) (ng/mL) 30 - 1200 Range o f low std curve (ppb) (ng/mL) 30 - 900 LCR from low std curve (ppb) (ng/mL) 6 0 -9 0 0 Range of high std curve (ppb) (ng/mL) N /A LCR from high std curve (ppb) (ng/mL) N /A Attachment B: MDL/LOQ Values 3MEnvironmental Laboratory ETS-8-6.0 Page 12 of 16 Page 147 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Compound: EtFOSE-OH Liver m atrix Prepared range o f standards (ppb) (ng/mL) Range o f average curve (ppb) (ng/mL) Rabbit 6 .1 7 -1 2 3 5 31 -9 0 0 LCR from ave curve (ppb) (ng/mL) 31 -9 0 0 Range of low std curve (ppb) (ng/mL) N /A LCR from low std curve (ppb) (ng/mL) N /A Range o f high std curve (ppb) (ng/mL) N /A LCR from high std curve (ppb) (ng/mL) N /A Compound: PFOSEA Prepared Range o f Liver m atrix range o f standards (ppb) (ng/mL) average curve (ppb) (ng/mL) R ab b it 6 .1 7 -1 2 3 5 3 1 -1 2 0 0 LCR from ave curve (ppb) :(ng/mL) 3 1 -1 2 0 0 Range of low std curve (ppb) (ng/mL) N /A LCR from low std curve. (ppb) (ng/mL) Range of high std curve (ppb) (ng/mL) N /A ' N /A LCR from high std curve. ' (ppb) (ng/mL) N /A . ' Compound: M556 Prepared Liver range o f m atrix standards (ppb) (ng/mL) Rabbit 6 .1 7 -1 2 3 5 Range o f average curve (ppb) (ng/mL) 31 - 1200 LCR from ave curve : (ppb) (ng/mL) Range o f lo w std curve (ppb) (ng/mL) 60 - 1200 N /A LCR from low std : 7 curve' (ppb) (ng/mL) Range o f high std curve (ppb) (ng/mL) LCR from h ig h std. - curve (ppb) (ng/mL) N /A N /A . N /A " ' A ttachm ent C: Standard Calculations 3MEnvironmental Laboratory E T S -8 -6 .0 Page 13 o f 14 Page 148 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Ion Pair Standard Curves - Tissue Prep date(s): Analyte(s): Sample matrix: Method/revision: Target analyte(s): FC mix std approx. 0.500 ppm: FC mix std approx. 5.00 ppm: FC mix std approx. 50.0 ppm: Surrogate std approx. 100 ppm: Standard number: Equipment number: Final solvent and TN: Blank liver/identifier: Actual concentrations of standards in the FC mix PFOS PFO SA PFO SA A EtFOSE PFO SEA Std cone Std cone Std cone Std cone Std cone ug/m L ug/m L ug/m L u g/m L ug/m L 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 50.0 50.0 50.0 50.0 50.0 M 556 Std cone ug/m L 0.500 0.500 0.500 0.500 0.500 5.00 5.00 5.00 50.0 Std cone u g/m L A ll Ain't spiked mL 0.002 0.004 0.010 0.020 0.040 0.010 0.020 0.030 0.004 A ll D ensity g 0.167 0.167 0.167 0.167 0.167 0.167 0.167 0.167 0.167 Calculated concentrations of standards in the sample matrix PFOS Final cone ng/g 5.99 PFOSA F in a l cone ng/g 5.99 PFOSAA Final cone n g /g 5.99 E tF O SE Final cone ng/g 5.99 PFOSEA Final cone ng/g 5.99 M 556 Final cone n g /g 5.99 Std cone n g /g 12.0 12.0 12.0 12.0 12.0 1.2.0 29.9 59.9 29.9 59.9 29.9 59.9 29.9 59.9 29.9 59.9 29.9 59.9 120 299 599 898 1198 120 299 599 898 1198 120 299 599 898 1198 120 299 599 898 1198 120 299 599 898 1198 oVCoOO 120 299 599 1198 Surrogate Std cone ng/m L 100 Surrogate Final cone ng/mL 0.500 A ll A m 't spiked mL 0.005 Validated ranges - approximate concentrations L iver R abbit PFO S 5-1000 ppb PFOSA 5-1000 ppb PFOSAA 5-1000 ppb B ovine E stim ates only, use rabbit values. R at E stim ates only, use rabbit values. M onkey E stim ates only, use rabbit values. E tF O S E -O H 5-1000 ppb POAA 5-1000 ppb PFOSEA 5-1000 ppb A ttachm ent C: Standard C alculations 3MEnvironmental Laboratory E T S -8 -6 .0 Page 14 o f 14 Page 149 3M M edical D epartm ent Study: T6316.1 3M Environmental Laboratory Analytical Report: FACT-TOX-001 L R N -U 2103 M ethod A n a l y s is o f F l u o r o c h e m ic a l s in L iv e r E x tr a c ts U sin g H P L C -E lectro spray/M ass Sp e c tr o m e tr y Method Number: FACT-M-2.0 Author: Lisa Clemen Approved By: At Laboratory Manager ---------------1-------- .. .. - ---------------------------Group Leader iA Technical Reviewer Adoption Date: Revision Date: Ac r A Date Date shihn Date Initial 11IP Scope and Application 7^ 1^j Scope: This method is for the analysis o f extracts o f liver or other tissues for fluorochemical '""surfactants using HPLC-electrospray/mass spectrometry. O i_ . IQ Applicable Compounds: Potassium perfluorooctanesulfonate, anionic fluorochemical surfactants, or other ionizable compounds. Date a Matrices: Rabbit, rat, bovine, and monkey livers or other livers as designated in the C~ validation report. c^n C-Q g'ord 7.0.1/95 FACT-M-2.0 Analysis of Liver Extract Using ES/MS Page 1 o f 8 3MEnvironmental Laboratory Page 150 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 2.0 Summary of Method_______________________________________________________ 2.1 This method describes the analysis o f fluorochemical surfactants extracted from liver using HPLC-electrospray/mass spectrometry. The analysis is performed by monitoring a single ion characteristic o f a particular fluorochemical, such as the potassium perfluorooctanesulfonate (PFOS) anion, M/Z= 499. Samples may also be screened to verify compound identification. 3.0 Definitions________________________________________________________________ 3.1 None. 4.0 Warnings and Cautions____________________________________________________ 4.1 Health and Safety Warnings: 4.1.1 Use caution with the voltage cable for the probe. When the voltage cable is plugged into the probe DO NOT TOUCH THE PROBE, there is risk o f electrical shock. 4.2 Cautions: 4.2.1 Do not run solvent pumps above capacity o f 400 bar (5800 psi). If pressure goes over 400 bar, the HP 1100 will initiate automatic shutdown. 4.2.2 Do not run solvent pumps to dryness. 5.0 Interferences__________________________________________________________________ 5.1 Teflon should not be used for sample storage or any part o f instrumentation that comes in contact with the sample or extract. 6.0 Equipment________________________________________________________________ 6.1 E quipm ent listed below m ay be changed in order to optim ize the system. 6.1.1 Micromass Electrospray Mass Spectrometer 6.1.2 HP 1100 low pulse solvent pumping system sind autosampler. 7.0 Supplies and Materials____________________________________________________ 7.1 Supplies 7.1.1 Nitrogen gas, refrigerated liquid, regulated to approximately 100 psi. 7.1.2 HPLC column, specifics to be determined by the analyst. 7.1.3 Capped autovials or capped 15 mL centrifuge tubes. 8.0 Reagents and Standards______________________________________________ _ 8.1 Reagents 8.1.1 Methanol, HPLC grade or equivalent. W ord 7.0.1/95 3M E nvironm ental Laboratory FACT-M -2.0 Analysis o f Liver Extract U sing ES/M S Page 2 of 8 P age 151 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 8.1.2 Milli-Q water, all water used in this method should be Milli-QTM water and may be provided by a Milli-Q TOC Plus system. 8.1.3 Ammonium acetate, HPLC grade or equivalent. 8.2 Standards 8.2.1 Typically one H20 blank, one liver blank, and seven liver standards are prepared during the extraction procedure. SeeFACT-M-1. . 9 .0 S a m p l e H a n d l in g __________________________________________________________________________ 9.1 Fresh liver standards are prepared with each analysis. Extracted standards and samples are stored in capped autovials or capped 15 mL centrifuge tubes until analysis. 9.2 If analysis will be delayed, extracted standards and samples may be refrigerated until analysis can be performed. 10.0 Q u a l it y C o n t r o l ________________________________________________________________________ 10.1 Matrix Blanks and Method Blanks 10.1.1 Analyze a method blank and matrix blank prior to each calibration curve. 10.2 Matrix Spikes 10.2.1 Analyze a matrix spike and matrix spike duplicate with each analysis. 10.2.2 Expected concentrations will fall in the mid- range o f the initial calibration curve. Additional spike concentrations may fall in the low-range o f the initial calibration curve. 10.2.3 See section 13 to calculate percent recovery. 10.3 Continuing Calibration Checks 10.3.1 A nalyze a m id-range calibration standard after every tenth sam ple. If a significant change ( 30%) in peak area occurs, relative to the initial standard curve, stop the run. Only those samples analyzed before the last acceptable calibration standard will be used. The remaining samples must be reanalyzed. 10.3.2 See section 13 to calculate percent difference;. 10.4 System Suitability 10.4.1 System suitability (e.g. peak area, retention time and peak shape, etc.) will be assessed for each run. 1 1 .0 C a l i b r a t io n a n d S t a n d a r d iz a t io n _____________________________________________________ 11.1 Analyze the extracted liver standards prior to and following each set o f extracts. The mean o f two standard values, at each standard concentration, will be plotted by linear regression for the calibration curve using MassLynx or other suitable software. 3MEnvironmental Laboratory FACT-M-2.0 Analysis of Liver Extract Using ES/MS Page 3 of 8 Page 152 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 11.2 The r2 value for the data should be 0.98 or greater. Lower values may be acceptable at the discretion o f the analyst. 11.3 If the curve does not meet requirements, perform routine maintenance or reextract the standard curve (if necessary) and reanalyze. 12.0 Procedures____________________________________________________________________ 12.1 Acquisition Set up ' 12.1.1 Click on start button in the Acquisition Control Panel. Set up a sample list. Assign a filename using letter-MO-DAY-last digit o f year-sample number, assign a method (MS) for acquiring, and type in sample descriptions. 12.1.2 To create a method click on scan button in the Acquisition control panel and select SIR. Set,,Ionization. Mode as appropriate and mass to 499 or other appropriate masses. A scan is usually collected along with the SIRs. Save method. 12.1.3 Typically the sample list begins with the first set o f liver standards and ends with the second set o f standards. 12.1.4 Samples are analyzed with a continuing calibration check injected after every tenth sample. Solvent blanks should be analyzed periodically to monitor possible analyte carryover and are not considered samples but may be included as such. 12.2 Using the Autosampler 12.2.1 Set up sample tray according to the sample list prepared in section 12.1.1. 12.2.2 Set-up the HP1100/autosampler at the follov/ing conditions or at conditions the analyst considers appropriate for optimal response. Record actual conditions in the instrument logbook: 12.2.2.1 Sample size = 10 p.L injection with a sample wash 12.2.2.2 Inject/sample = 1 12.2.2.3 Cycle time = 15 minutes 12.2.2.4 Solvent ramp = T im e 0.00 min. 7.5 min. 11.0 min. 11.5 min. M eO H 45% 90% 90% 45% 2.0 m M Am m onium acetate 55% 10% 10% 55% Note: In this instrum ent configuration, the run m ust be set up on the electrospray softw are w ith a "W aiting for inlet start" m essage before the "Start" button is pressed on the HP W orkstation. 12.2.2.5 Press the "Start" button. 3MEnvironmental Laboratory FACT-M-2.0 Analysis of Liver Extract Using ES/MS Page 4 of 8 P age 153 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 12.3 Instrument Sep-up 12.3.1 Refer to AMDT-EP-31 for more details. 12.3.2 Check the solvent level in reservoirs and refill if necessary. 12.3.3 Check the stainless steel capillary at the end o f the probe. Use an eye piece to check the tip. The tip should be flat with no jagged edges. If the tip is found to be unsatisfactory, disassemble the probe and replace the stainless steel capillary. 12.3.4 Set HPLC pump to "On". Set the flow to 10 500 uL/min or as appropriate. Observe droplets coming out o f the tip o f the probe. Allow to equilibrate for approximately 10 minutes. 12.3.5 Turn on the nitrogen. A fine mist should be expelled with no nitrogen leaking around the tip o f the probe. 12.3.6 The instrument uses these parameters at the following settings. These settings may change in order to optimize the response: 12.3.6.1 Drying gas 250-400 liters/hour ' 12.3.6.2 ESI nebulizing gas 10-15 liters/hour 12.3.6.3 LC constant flow mode flow rate 10 - 500 uL/min 12.3.6.4 Pressure <400 bar (This parameter is not set, it is a guide to ensure the instrument is operating correctly.) 12.3.7 Carefully guide the probe into the opening. Insert probe until it will not go any further. Connect the voltage cables to the probe. 12.3.8 Record tune parameters in the instrument log;. 12.3.9 Using the cross-flow counter electrode in the ES/MS source is recommended for the analysis o f biological matrices. 12.3.10 Click on start button in the Acquisition Control Panel. Press the start button at top o f sample list. Ensure start and end sample number includes all samples to be analyzed. 13.0 D ata A nalysis and Calculations_______________________________________________ 13.1 Calculations: 13.1.1 Calculate matrix spike percent recoveries using the following equation: % Recovery = Observed Result - Background Result x 100 Expected Result 13.1.2 Calculate percent difference using the following equation: % Difference = Expected Cone. - Calculated Cone, x 100 Expected Cone. 3MEnvironmental Laboratory FACT-M -2.0 Analysis o f Liver Extract U sing ES/M S Page 5 o f 8 Page 154 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 13.1.3 C alculate actual concentration o f PFOS anion in total liver (mg): f ug PFOS anion calc, from std curve^ v g o f liver used for analysis ) , -------------------------------------------------- x Total mass o f liver (g) 1000 ug/1 mg 14 .0 M e t h o d P e r f o r m a n c e _________________________________;________________________________ 14.1 The method detection limit is equal to at least three times the baseline noise in the matrix blank. 14.2 The practical quantitation limit is equal to the lowest standard in the calibration curve. 1 5 .0 P o l l u t i o n P r e v e n t i o n a n d W a s t e M a n a g e m e n t ____________________________________ 15.1 Sample waste is disposed in biohazard containers, flammable solvent waste is disposed in high BTU containers, and glass pipette waste is disposed in broken glass containers. All containers are located in the laboratory. 1 6 .0 R e c o r d s __________________________________________________________________________________ 16.1 Store chromatograms in the study folder. Each chromatogram should have the following information included either in the header or hand written on the chromatogram: study number, sample name, extraction date, and dilution factor (if applicable). 16.2 Plot calibration curve by linear regression and store in the study folder. 16.3 Print sample list from MassLynx and tape into the instrument runlog. 16.4 Print data integration summary from MassLynx and tape into the instrument runlog. 16.5 Copy instrument runlog pages, including instrument parameters and sample results, and tape into appropriate study notebook. 16.6 Summarize data using suitable software and store in the study folder. 16.7 Back up electronic data to appropriate media. Record in study notebook the file name and location o f backup electronic data. 1 7 .0 T a b l e s , D i a g r a m s , F l o w c h a r t s , a n d V a l i d a t i o n D a t a _____________________________ 17.1 Attachment A: FACT-M-2 Data reporting spreadsheet 17.2 The validation report associated with this method is FACT-M-1.0 & 2 .0 -V -l. 18.0 References___________________________________________________________________ 18.1 AMDT-EP-31, "Operation o f VG Platform Electrospray Mass Spectrometer" 3MEnvironmental Laboratory FACT-M -2.0 Analysis o f Liver Extract Using ES/M S Page 6 o f 8 Page 155 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 19.0 A ffected Documents__________________________________________________ _______ 19.1 FACT-M-1.0, "Extraction o f Potassium Perfluorooctanesulfonate from Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry" 20.0 Revisions Revision Number. . Reason For Revision Revision Date 3M Environmental Laboratory FACT-M-2.0 Analysis of Liver Extract Using ES/MS Page 7 of 8 Page 156 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Laboratory Study # Study: Test Material: M atrix/Final Solvent: M ethod/Revision: . Analytical Equipm ent System Number: Instrument Software/Version: F ilenam e: R-Squared Value: Slope: Y Intercept: Date o f Extraction/Analyst; . Date o f Analysis/Analyst: G roup D ose Sam ple# \ C oncentration ug/m L Initial V ol. mL D ilution Factor Final C one. ug/m L Slope: Taken from linear regression equation. G roup /D ose: Taken from the study folder. S am ple#: Taken from the study folder. C o n cen tra tio n (u g/m L ): Taken from the M assLynx integration summary. Initial V o lu m e (m L ): Taken from the study folder. D ilution F actor: Taken from the study folder. Final C on e. (ug/m L ): Calculated by dividing the initial volum e from the concentration 3MEnvironmental Laboratory FACT-M-2.0 Analysis of Liver Extract Using ES/MS Page 8 of 8 Page 157 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 3M Environmental Laboratory x. ........... Method Analysis of Fluorochemicals in Serum Extracts Using HPLC-Electrospray/Mass Spectrometry Method Number: FACT-M-4.0 . '. Author: Lisa Clemen - Adoption Date: H / h I ^S Revision Date: fojfi Approved By: , ' /'o - - Laboratory Manager v /" /9 f Date -- .....Group Leader Date ( l i t _________________________ _ Technical Reviewer ____________________ h I h H s Date 1.0 Scope and Application__________________________________________ .____________ 1.1 Scope: This method is for the analysis o f extracts o f serum or tissue for fluorochemical Oo surfactants using HPLC-electrospray/mass spectrometry. ~a 1.2 Applicable Compounds: Potassium perfluorooctanesulfonate, anionic fluorochemical o surfactants, or other ionizable compounds. D a 1 " K 1 3 Matrices: Rabbit, rat, and bovine serum or other sera as designated in the validation report. o ui O O ~ g Word 7.0.1/95 FACT-M-4.0 Analysis of Serum Extract Using ES/MS Page 1 of 8 3MEnvironmental Laboratory Page 158 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 2 .0 S u m m a r y o f M e t h o d __________________________________________________________ ;________ 2.1 This method describes the analysis o f fluorochemical surfactants extracted from serum using HPLC-electrospray/mass spectrometry. The analysis is performed by monitoring a single ion characteristic of a particular fluorochemiical, such as the potassium perfluorooctanesuifonate (PFOS) anion, M/Z= 499. Samples may also be screened to verify compound identification. 3 .0 D e f in it io n s ____________________ ^_________________ ;_______________________________________ 3.1 None. 4 .0 W a r n in g s a n d C a u t io n s ________________________________________________________________ 4.1 Health and Safety Warnings: 4.1.1 Use caution with the voltage cable for the probe. When the voltage cable is plugged into the probe DO NOT TOUCH THE PROBE, there is risk o f electrical shock. 4.2 Cautions: 4.2.1 Do not run solvent pumps above capacity o f 400 bar (5800 psi). If pressure goes over 400 bar, the HP1100 will initiate automatic shutdown. 4.2.2 Do not run solvent pumps to dryness. 5 .0 In t e r f e r e n c e s __________________________________________________________________________ 5.1 Teflon should not be used for sample storage or any part o f instrumentation that comes in contact with the sample or extract 6 .0 Equipment______________'_______ :_____________________________________________________ 6.1 Equipment listed below may be changed in order to optimize the system. 6.1.1 Micromass Electrospray Mass Spectrometer 6.1.2 HP1100 low pulse solvent pumping system and autosampler. 7 .0 S u p p l ie s a n d M a t e r ia l s _______________________________________________________________ 7.1 Supplies 7.1.1 Nitrogen gas, refrigerated liquid, regulated to approximately 100 psi. 7.1.2 HPLC column, specifics to be determined by the analyst. 7.1.3 Capped autovials or capped 15 mL centrifuge tubes. 8.0 R e a g e n t s a n d S t a n d a r d s ______________________________________________________________ 8.1 Reagents 8.1.1 Methanol, HPLC grade or equivalent. 3MEnvironmental Laboratory FACT-M-4.0 Analysis of Serum Extract Using ES/MS Page 2 of 8 Page 159 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 . LRN-U2103 8.1.2 Milli-QTM water, all water used in this method should be Milli-QTM water and may be provided by a Milli-Q TOC Plus system. 8.1.3 Ammonium acetate, HPLC grade or equivalent. 8.2 Standards 8.2.1 Typically one H20 blank, one serum blank, and seven serum standards are prepared during the extraction procedure. SeeFACT-M-3. 9.0 Sample Ha n d l i n g _____________________________ __________________________ 9.1 Fresh serum standards are prepared with each analysis. Extracted standards and samples are stored in capped autovials or capped 15 mL centrifuge tubes until analysis. 9.2 If analysis will be delayed, extracted standards and samples may be refrigerated at 4 C until analysis can be performed. 10.0 Quality Control________;__________________________ _________________________ 10.1 Matrix Blanks and Method Blanks 10.1.1 Analyze a method blank and a matrix blank prior to each calibration curve. 10.2 Matrix Spikes 10.2.1 Analyze a matrix spike and matrix spike duplicate with each analysis. . 10.2.2 Expected concentrations will fall in the mid-range o f the initial calibration curve. Additional spike concentrations may fall in the low-range of the initial calibration curve. 10.2.3 See section 13 to calculate percent recovery. 10.3 Continuing Calibration Checks 10.3.1 Analyze a mid-range calibration standard after every tenth sample. If a significant change ( 30%) in peak area occurs, relative to the initial standard curve, stop the run. Only those samples analyzed before the: last acceptable calibration standard will be used. The remaining samples must be reanalyzed. 10.3.2 See section 13 to calculate percent difference. 10.4 System Suitability 10.4.1 System suitability (e.g., peak area, retention time, peak shape, etc.) will be assessed for each run. 11.0 Calibration and Standardization___________________________________________ 11.1 Analyze the extracted serum standards prior to and following each set of extracts. The mean o f two standard values, at each standard concentration, will be plotted by linear regression for the calibration curve using MassLynx or other suitable software. 3MEnvironmental Laboratory FACT-M-4.0 Analysis of Serum Extract Using ES/MS Page 3 of 8 Page 160 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 11.2 The r2value for the data should be 0.98 or greater. Lower values may be acceptable at the discretion o f the analyst. 11.3 If the curve does not meet requirements, perform routine maintenance or reextract the standard curve (if necessary) and reanalyze. 12.0 Procedures___________ ;______________________________________________________ 12.1 Acquisition Set up 12.1.1 Click on start button in the Acquisition Control Panel. Set up a sample list. Assign a filename using letter-MO-DAY-last digit o f year-sample number, assign a method (MS) for acquiring, and type in sample descriptions. 12.1.2 To create a method click on scan button in the Acquisition control panel and select SIR (Single Ion Recording). Set Ionization Mode as appropriate and mass to 499 or other appropriate masses. A scan is usually collected along with the SIRs. Save method. 12.1.3 Typically the sample list begins with the first set o f serum standards and ends with the second set o f standards. 12.1.4 Samples are analyzed with a continuing calibration check injected after every tenth sample. Solvent blanks should be analyzed periodically to monitor possible analyte carryover and are not considered samples but may be included as such. 12.2 Using the Autosampler 12.2.1 Set up sample tray according to the sample list prepared in section 12.1.1. 12.2.2 Set-up the HP1100/autosampler at the following conditions or at conditions the analyst considers appropriate for optimal response. Record actual conditions in the instrument logbook: 12.2.2.1 Sample size = 10 pL injection with a sample wash 12.2.2.2 Inject/sample = 1 12.2.2.3 Cycle time = 15 minutes 12.2.2.4 Solvent ramp = Time 0.00 min. 7.5 min. 11.0 min. 11.5 min. MeOH 45% 90% 90% 45% 2.0 mM Ammonium acetate 55% 10% 10% 55% Note: In this instrument configuration, the nin must be set up on the electrospray software with a "Waiting for inlet start" message before the "Start" button is pressed on the HP Workstation. 12.2.2.5 Press the "Start" button. FACT-M-4.0 Analysis of Serum Extract Using ES/MS Page 4 of 8 3MEnvironmental Laboratory P age 161 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 12.3 Instrument Set-up 12.3.1 Refer to AMDT-EP-31 for more details. 12.3.2 Check the solvent level in reservoirs and refill if necessary. 12.3.3 Check the stainless steel capillary at the end o f the probe. Use an eye piece to check the tip. The tip should be flat with no jagged edges. If the tip is found to be unsatisfactory, disassemble the probe and replace the stainless steel capillary. 12.3.4 Set HPLC pump to "On". Set the flow to 10 - 500 uL/min or as appropriate. Observe droplets coming out o f the tip o f the probe. Allow to equilibrate for approximately 10 minutes. 12.3.5 Turn on the nitrogen. A fine mist should be expelled with no nitrogen leaking around the tip o f the probe. 12.3.6 The instrument uses these parameters at the following settings. These settings may change in order to optimize the response: 12.3.6.1 Drying gas 250-400 liters/hour 12.3.6.2 ESI nebulizing gas 10-15 liters/hour 12.3.63 HPLC constant flow mode flow rate 10 - 500 pL/min 12.3.6.4 Pressure <400 bar (This parameter is not set, it is a guide to ensure the HPLC is operating correctly.) 12.3.7 Carefully guide the probe into the opening. Insert probe until it w ill not go any further. Connect the voltage cables to the probe. 12.3.8 Record tune parameters in the instrument log. 12.3.9 Using the cross-flow counter electrode in the ES/MS source is recommended for the analysis o f biological matrices. 12.3.10Click on start button in the Acquisition Control Panel. Press the start button at top o f sample list. Ensure start and end sample number includes all samples to be analyzed. 13.0 Data Analysis and Calculations__________________________________ 13.1 Calculations: 13.1.4 Calculate matrix spike percent recoveries using the following equation: % Recovery = Observed Result - Background Result x 100 Expected Result 13.1.5 Calculate percent difference using the following equation: % Difference = Expected Cone. - Calculated Cone, x 100 Expected Cone. 3MEnvironmental Laboratory FACT-M-4.0 Analysis of Serum Extract Using ES/MS Page 5 of 8 Page 162 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 13.1.6 Calculate actual concentration o f PFOS, or other fluorochemical, anion in serum (pg/mL): |ug o f PFO calc, from std. Curve x Dilution Factor x Final Volume (m i.) Initial Volume o f serum (mL) 14.0 M e t h o d P e r f o r m a n c e ___________________________________________________________' 14.1 The method detection limit is equal to halfthe lowest standard in the calibration curve. 14.2 The practical quantitation limit is equal to the lowest standard in the calibration curve. 15.0 P o l l u t io n P r e v e n t io n a n d W a s t e M a n a g e m ent_______ :____________________________ 15.1 Sample extract waste and flammable solvent is disposed in high BTU containers, and glass pipette waste is disposed in broken glass containers located in the laboratory. 16 .0 R e c o r d s ______________^_________________________________________________________________ 16.1 Store chromatograms in the study folder. Each chromatogram must have the following information included either in the header or hand v/ritten on the chromatogram: study number, sample name, extraction date, and dilution factor (if applicable). 16.2 Plot calibration curve by linear regression and store; in the study folder. 16.3 Print sample list from MassLynx and tape into the instrument runlog. 16.4 Print data integration summary from MassLynx and tape into the instrument runlog. 16.5 Copy instrument runlog pages, including instrument parameters and sample results, and tape into appropriate study notebook. 16.6 Summarize data using suitable software and store in the study folder. 16.7 Back up electronic data to appropriate medium. Record in study notebook the file name and location o f backup electronic data. 1 7.0 T a b l e s . D ia g r a m s . F l o w c h a r t s , a n d V a l id a t io n D a t a ____________________________ 17.1 Attachment A: FACT-M-4 Data reporting spreadsheet 17.2 The validation report associated with this method is FACT-M-3.0 & 4.0-V -l. 18 .0 R e f e r e n c e s ____________________________________________________________________ ;_______ 18.1 AMDT-EP-31, "Operation o f VG Platform Electrospray Mass Spectrometer" 1 9 .0 A f f e c t e d D o c u m e n t s _______________________________________________ ,________________ 19.1 FACT-M-3.0, "Extraction o f Fluorochemical Anions from Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry" 3MEnvironmental Laboratory FACT-M-4.0 Analysis of Serum Extract Using ES/MS Page 6 of 8 P age 163 3M M edical D epartm ent Study: T6316.1 # Analytical Report: FACT-TOX-001 L R N -U 2103 20.0 Revisions Revision Number. Reason For Revision Revision rtntp 3M E nvironm ental Laboratory FA C T -M -4.0 Analysis o f Serum Extract Using ES/MS Page 7 of 8 Page 164 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 # Laboratory Study # Study: Test Material: Matrix/Final Solvent: M ethod/R evision: Analytical Equipment System Number: instrument Software/Version: F ilenam e: R-Squared Value: Slope: Y Intercept: Date o f Extraction/Analyst: Date o f Analysis/Analyst: Group D ose Sam ple# C o n cen tra tio n ug/m L Initial Vol. mL D ilu tion Factor Final Cone. ug/m L Slope: Taken from linear regression equation. G roup/D ose: Taken from the study folder. Sam ple#: Taken from the study folder. C oncen tration (ug/m L ): Taken from the M assLynx integration summary. Initial V olum e (m L ): Taken from the study folder. D ilution F actor: Taken from the study folder. Final C one. (ug/m L): Calculated by dividing the initial volum e from the concentration 3MEnvironmental Laboratory FACT-M-4.0 Analysis of Serum Extract Using ES/MS Page 8 of 8 Page 165 3M M edical D epartm ent Study: T6316.1 3M Environmental Laboratory Analytical Report: FACT-TOX-001 L R N -U 2103 M ethod A n a ly s is o f Po ta ssiu m Per flu o r o o c ta n esu lfo n a te o r O t h e r F l u o r o c h e m ic a l s in Se r u m E x tr a c ts U sin g H P L C -E lec tr o spr a y/M ass Sp e c tr o m e tr y M ethod Num ber: ETS-8-5.1 Author: Lisa Clemen, Robert Wynne Approved By: 'cH i i _ Laboratory Manager Adoption Date: 03/01/99 Revision Date: 1/ 2 Date Group Leader Technical Reviewer Date oh/ i-Im Date ExacTCpy of O riainai Initial ____ Is I a") Date .0 S c o p e a n d A p p l ic a t io n __________________________________________________________________ ,1 Scope: This method describes the analysis o f serum extracts for fluorochemical surfactants using HPLC-electrospray/mass spectrometry. .2 A pplicable Com pounds: Fluorochemical surfactants or other fluorinated compounds, or other ionizable compounds. ,3 M atrices: Rabbit, rat, bovine, monkey, and human serum, or other fluids as designated in the validation report. W ord 6/95 3MEnvironmental Laboratory E T S -8 -5 .1 A -n a lu c ie o f Q > n im P v t r a r t T T c in o "P/X/Q Page 1 of 9 Page 166 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 2.Q S u m m a r y o f M e t h o d _______________________________________ _____________________ __________ 2.1 This method describes the analysis o f fluorochemical surfactants extracted from serum or . other fluids, using HPLC-electrospray/mass spectrometry, or similar system as appropriate. The analysis is performed by monitoring a single ion characteristic o f a particular fluorochemical, such as the perfluorooctanesulfonate (PFOS) anion, m/z= 499. Additionally, samples may be analyzed using a tandem mass spectrometer to further verify the identity o f a compound by detecting daughter ions o f the parent ion. 3.0 Definitions__________________________:________________ ___________________________ 3.1 A tm ospheric Pressure Ionization (API): The Micromass Quattro II triple quadrupole systems allow for various methods o f ionization by utilizing various sources, probes, and interfaces. These include but are not limited to: Electrospray Ionization (ESI), Atmospheric Pressure chemical Ionization (APcI), Thermospray, etc. The ionization process in these techniques occurs at atmospheric pressure (i.e., not under a vacuum). 3.2 E lectrospray Ionization (ES, ESI): a method o f ionization performed at atmospheric pressure, whereby ions in solution are transferred to the gas phase via tiny charged droplets. These charged droplets are produced by the application o f a strong electrical field. 3.3 M ass Spectrom etry, M ass Spectrom eter (M S), Ta ndem M ass Spectrom eter (M S/M S): The API Quattro II triple quadrupole systems are equipped with quadrupole mass selective detectors. Ions are selectively discriminated by mass to charge ratio (m/z) and subsequently detected. A single MS may be employed for ion detection or a series (MS/MS) for more specific fragmentation information. 3.4 C onventional vs. Z-spray probe interface: The latest models o f Micromass Quattro II triple quadrupole systems (post 1998) utilize a "Z-spray" conformation. The spray emitted from a probe is orthogonal to the cone aperture. In the conventional conformation it is aimed directly at the cone aperture, after passing through a tortuous pathway in the counter electrode. Though the configuration is different, the methods o f operation, cleaning, and maintenance are the same. However, Z-spray components and conventional components are not compatible with one another, but only with similar systems (i.e., Z-spray components are compatible with some other Z-spray systems, etc.) 3.5 M ass L ynx Software: System software designed for the specifi c operation o f these Quattro II triple quadrupole systems. Currently MassLynx has Windows 95 and WindowsNT 4.0 versions. A ll versions are similar. For more details see the manual specific to the instrument (Micromass Quattro II triple quadrupole MassLynx or MassLynx NT User's Guide). 4.0 W a r n in g s a n d C a u tio n s 4.1 H ealth and Safety W arnings: 4.1.1 U se caution with the voltage cables for the probe. When engaged, the probe employs a voltage o f approximately 5000 Volts. 4.1.2 When handling samples or solvents wear appropriate protective gloves, eyewear, and clothing. 3MEnvironmental Laboratory A ___ 1. ___r ETS-8-5.1 T T . J -- ^ rc r \ Ko Page 2 o f 9 Page 167 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 4.2 Cautions: 4.2.1 D o not operate solvent pumps above capacity o f 400 bar (5800 psi) back pressure. If the back pressure exceeds 400 bar, the HP 1100 w ill initiate automatic shutdown. 4.2.2 Do not run solvent pumps to dryness. 5.0 Interferences__________________________________________________________ 5.1 To minimize interferences when analyzing samples, teflon should not be used for sample storage or any part o f instrumentation that comes in contact with the sample or extract. 6.0 Equipment____________________________________________ __________________________ 6.1 Equipment listed below may be modified in order to optimize the system. Document any m odifications in the raw data as method deviations. 6.1.1 6.1.2 Micromass Quattro II triple quadrupole M ass Spectrometer equipped with an electrospray ionization source HP 1100 low pulse solvent pumping system, solvent degasser, column compartment, and autosampler 7.0 Supplies and M aterials____________________ _____________________________________ 7.1 Supplies 7.1.1 H igh purity grade nitrogen gas regulated to approximately 100 psi (House air system ) 7.1.2 HPLC analytical column, specifics to be determined by the analyst and documented in the raw data. 7.1.3 Capped autovials or capped 15 mL centrifuge tubes 8.0 Reagents and Standards___________________________________ ;_____________________ 8.1 Reagents 8.1.1 M ethanol, HPLC grade or equivalent 8.1.2 M illi-QTM water, all water used in this method should be Milli-QTM water or equivalent, and may be provided by a M illi-Q TOC Plus system or other vendor 8.1.3 Ammonium acetate, reagent grade or equivalent 8.2 Standards 8.2.1 Typically two method blanks, two matrix blanks, and eighteen matrix standards are prepared during the extraction procedure. See ETS-8-4.1. 9.0 Sample H andling_______________________________________________________________ 9.1 Fresh matrix standards are prepared with each analysis. Extracted standards and samples are stored in capped autovials or capped 15 mL centrifuge tubes until analysis. 3MEnvironmental Laboratory ETS-8-5.1 Analysis of Serum Extract Using ES/MS Page 3 of 9 Page 168 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 9.2 If analysis will be delayed, extracted standards and samples can be refrigerated at approximately 4 C, or at room temperature, until analysis can be performed. 1Q.0 Quality Control____________________________________ __________________________ 10.1 Solvent Blanks, M ethod Blanks and M atrix Blanks 10.1.1 Solvent blanks, method blanks and matrix blanks are prepared and analyzed with each batch to determine contamination or carryover. 10.1.2 Analyze a method blank and a matrix blank prior to each calibration curve. 10.2 Matrix Spikes 10.2.1 Matrix spikes are prepared and analyzed to determine the matrix effect on the recovery efficiency. 10.2.2 Matrix spike duplicates are prepared and analyzed to measure the precision and the recovery for each analyte. 10.2.3 Analyze a matrix spike and matrix spike duplicate per forty samples, with a minimum o f 2 spikes per batch. 10.2.4 Matrix spike and matrix spike duplicate concentrations will fall in the mid-range o f the initial calibration curve. Additional spike concentrations may fall in the lowrange o f the initial calibration curve. 10.3 Continuing Calibration Verifications 10.3.1 Continuing calibration verifications are analyzed to verify the continued accuracy o f the calibration curve. 10.3.2 Analyze a mid-range calibration standard after eveiy tenth sample, with a minimum o f one per batch. 11.0 Calibration and Standardization_________________________________________ 11.1 Analyze the extracted matrix standards prior to and following each set o f extracts. The average o f two standard curves will be plotted by linear regression (y = my + b), weighted 1/x, not forced through zero, using MassLynx or other suitable software. 11.2 If the curve does not meet requirements, perform routine maintenance or reextract the standard curve (if necessary) and reanalyze. 11.3 For purposes o f accuracy when quantitating low Levels o f analyte, it may be necessary to use the low end o f the calibration curve rather than the full range o f the standard curve. Example: when attempting to quantitate approximately 10 ppb o f analyte, generate a calibration curve consisting o f the standards from 5 ppb to 100 ppb rather than the full range o f the curve (5 ppb to 1000 ppb). This will reduce inaccuracy attributed to linear regression weighting o f high concentration standards. 3MEnvironmental Laboratory 1A __ . E T S -8-5.1 7o _____ T ..J____ * t T-:___r ? o r\ .f c Page 4 of 9 Page 169 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 ' LRN-U2103 12.0 Procedures______________________________ __________________________;______ 12.1 Acquisition Set up 12.1.1 Click on start button in the Acquisition Control Panel. Set up a sample list. Assign a filename using MO-DAY-last digit o f year-sample number, assign a method (MS) for acquiring, and type in sample descriptions. 12.1.2 To create a method click on scan button in the Acquisition control panel and select SIR (Single Ion Recording) or MRM. Set Ionization Mode as appropriate and mass to 499 or other appropriate masses. A full scan is usually collected along with the SIRs. Save acquisition method. If MS/MS instruments are employed, additional product ion fragmentation information may be collected. See Micromass MassLynx GUIDE TO DATA ACQUISITION for additional information and MRM (Multiple Reaction Monitoring). 12.1.3 Typically the analytical batch run sequence begins with a set o f extracted matrix standards and ends with a set o f extracted matrix standards. 12.1.4 Samples are analyzed with a continuing calibration check injected after every tenth sample. Solvent blanks should be analyzed periodically to monitor possible analyte carryover and are not considered samples but may be included as such. 12.2 Using the Autosampler 12.2.1 Set up sample tray according to the sample list prepared in Section 12.1.1. 12.2.2 Set-up the HP1100/autosampler at the following conditions or at conditions the analyst considers appropriate for optimal response. Record actual conditions in the instrument logbook: 12.2.2.1 Sample size = 10 pL injection 12.2.2.2 Inject/sample = 1 12.2.2.3 Cycle time = 13.5 minutes 12.2.2.4 Solvent ram p = Time 0.00 min. 8.50 min. 11.0 min. 12.0 min. MeOH 40% 90% 90% 40% 2.0 mM Ammonium acetate 60% 10% 10% 60% 12.2.2.5 Press the "Start" button. 12.3 Instrument Set-up 12.3.1 Refer to ETS-9-24.0 for more details. 12.3.2 Check the solvent level in reservoirs and refill if necessary. 3MEnvironmental Laboratory ETS-8-5.1 Page 5 o f 9 Page 170 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 12.3.3 Check the stainless steel capillary at the end o f the probe. Use an eyepiece to check the tip. The tip should be flat with no.jagged edges. If the tip is found to be unsatisfactory, disassemble the probe and replace the stainless steel capillary. 12.3.4 Set HPLC pump to "On". Set the flow to 10 - 500 uL/min or as appropriate. Observe droplets coming out o f the tip o f the probe. Allow to equilibrate for approximately 10 minutes. 12.3.5 Turn on the nitrogen. A fine mist should be expelled with no nitrogen leaking around the tip o f the probe. Readjust the tip o f the probe if no mist is observed. 12.3.6 The instrument uses these parameters at the following settings. These settings may change in order to optimize the response: 12.3.6.1 Drying gas 250-400 liters/hour 12.3.6.2 ESI nebulizing gas 10-15 liters/hour 12.3.6.3 HPLC constant flow mode, flow rate 10 - 500 pL/min 12.3.6.4 Pressure <400 bar (This parameter is not set, it is a guide to ensure the HPLC is operating correctly.) 12.3.7 Carefully guide the probe into the opening. Insert probe until it will not go any further. Connect the voltage cables to the probe. 12.3.8 Print the tune page, with its parameters, and store it in the study binder with a copy taped into the instrument log. 12.3.9 Using the cross-flow counter electrode in file ES/MS source is recommended for the analysis o f biological matrices. 12.3.10Click on start button in the Acquisition Control Panel (this may vary among MassLynx versions, see appropriate MassLynx USER'S GUIDE). Press the start button. Ensure start and end sample number includes all samples to be analyzed. 13.0 Data Analysis and Calculations______________________________________________ 13.1 Calculations: 13.1.4 Calculate matrix spike percent recoveries using the following equation: % Recovery = Observed Result - Background Result x 100 Expected Result 13.1.5 Calculate percent difference using the following equation: % Difference = Expected Cone. - Calculated Clone, x 100 Expected Cone. 13.1.6 Calculate actual concentration o f PFOS, or other fluorochemical, in matrix (pg/mL): (rig o f PFOS calc, from std. Curve x Dilution Factor) x 1 pg /Initial Volume o f matrix CmU) + mL o f Surrogate Standard! 1000 ng Final Volume (ml,) 3MEnvironmental Laboratory E T S -8 -5 .1 .a _ _ 1 ___; n ___ __ * T 7:___-no r\ ttr> Page 6 of 9 P age 171 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 14.0 M ethod Performance__________________________________________________________ 14.1 Method Detection Limit (MDL) and Limit o f Quantitation (LOQ) are method, analyte, and matrix specific. Please see ETS-8-4.1, Attachment B, for a listing o f current validated MDL and LOQ values. 14.2 Solvent Blanks, Method Blanks, and Matrix Blanks 14.2.1 Solvent blanks, method blanks, and matrix blanks values are must be below the lowest standard in the calibration curve 14.3 Calibration Curves 14.3.1 The r2value for the calibration curve must be 0.980 or better. 14.4 Matrix Spikes 14.4.1 Matrix spike percent recoveries are must be within 30% o f the spiked concentration. 14.5 Continuing Calibration Verifications 14.5.1 Continuing calibration verification percent recoveries must be 30% o f the spiked concentration. 14.6 If criteria listed in this method performance section isn't met, maintenance may be performed on the system and samples reanalyzed or other actions as determined by the analyst. Document all actions in the appropriate logbook. 14.7 If data are to be reported when performance criteria have not been met, the data must be footnoted on tables and discussed in the text o f the report. 15.0 Pollution Prevention and W aste M anagement________________________________ 15.1 Sample extract waste and flammable solvent is disposed in high BTU containers, and glass pipette waste is disposed in broken glass containers located in the laboratory. 16.0 Records______________________;_________________________________________________ 16.1 Each page generated for a study must have the following information included either in the header or hand written on the page: study or project number, acquisition method, integration method, sample name, extraction date, dilution factor (if applicable), and analyst. 16.2 Print the tune page, sample list, and acquisition method from MassLynx to include in the appropriate study folder. Copy these pages and tape into the instrument runlog. 16.3 Plot the calibration curve by linear regression, weighted 1/x, then print these graphs and store in the study folder. 16.4 Print data integration summary, integration method, and chromatograms, from MassLynx, and store in the study folder. 3MEnvironmental Laboratory E T S -8-5.1 A nrsK /eie rv f Q ^ m m ^v+ r?n "* t T T c in o Page 7 of 9 Page 172 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 16.5 Summarize data using suitable software (Excel 5.0) and store in the study folder, see Attachment A for an example o f a summary spreadsheet. 16.6 Back up electronic data to appropriate medium. Record in study notebook the file name and location o f backup electronic data. 17.0 T ables. D iagrams. Flowcharts, and V alidation Data ______________________ 17.1 Attachment A: ETS-8-5.1 Data summary spreadsheet. 18.0 R eferences____________________________________________________________________ 18.1 FACT-M-4.1, "Extraction o f Potassium Perfluorooctanesulfonate or Other Fluorochemical compounds from Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry 18.2 ETS-9-24.0, "Operation and Maintenance o f the Micromass Atmospheric Pressure Ionization/Mass Spectrometer Quattro II triple quadrupole Systems" 18.3 The validation report associated with this method is ETS-8-4.0 & 5.0-V -l. 19.0 A ffected Documents______________________ ____________________________________ 19.1 ETS-8-4.1, "Extraction o f Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds from Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry" 20.0 Revisions_________________________________________________________________ Revision Number. 1 Reason For Revision Section 6.1.2 Clarification o f HP 1100 system components. Section 11.1 Average o f two curves, not standard values, are used for plotting linear regression and added the 1/x weighting o f the curve. Section 12.2.2.4 Clarification o f solvent ramp. Section 17.1 Changed from attachment B to A. Revision Date 04/02/99 3MEnvironmental Laboratory ETS-8-5.1 Analysis of Serum Extract Usina ES/MS Page 8 of 9 P age 173 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Laboratory Study # Study: T est Material: M atrix/Final Solvent: M ethod/Revision: A nalytical Equipm ent System Number: Instrument Software/Version: Filenam e: R-Squared Value: Slope: Y Intercept: D ate o f Extraction/Analyst: Date o f Analysis/Analyst: G roup D ose Sam ple# C oncentration ug/m L Initial V ol. mL D ilu tio n F a cto r Final C one. ug/m L Slope: Taken from linear regression equation. G rou p /D ose: Taken from the study folder. Sam ple#: Taken from the study folder. C o n cen tration (ug/m L ): Taken from the M assLynx integration summary. Initial V olu m e (m L ): Taken from the study folder. D ilu tion F actor: Taken from the study folder. F in al C on e. (u g/m L ): Calculated by dividing the initial volum e from the concentration Attachm ent A: Summary Spreadsheet E T S -8 -5 .1 3MEnvironmental Laboratory A t r s l t f c i c n f Q p n i m p Y t r a o t TTci-nCT P Q / \ / f C ! Page 9 of 9 Page 174 3M M edical D epartm ent Study: T6316.1 3M Environmental Laboratory Analytical Report: FACT-TOX-001 L R N -U 2103 M ethod A nalysis of P otassium Perfluorooctanesulfonate or Oth er F lu o r o c h em ic a ls in L iv er E xtracts U sing H PL C -E lectrospray/M ass Spectrom etry Method Number: ETS-8-7.0 Author: Lisa Clemen, Glenn Langenburg Approved By: iM /V -- Laboratory Manager Adoption Date: Revision Date: Date Group Leader Date Technical Reviewer Date 7^ 2r+. V0)' r7 m X O03 1.0 Scope and A pplication O O 1.1 Scope: This method is for the analysis o f liver extracts for fluorochemical surfactants using ^2 HPLC-electrospray/mass spectrometry. D ^ 9 ,1 .2 Applicable Compounds: Fluorochemical surfactants or other fluorinated compounds, or & jy 0 other ionizable compounds. ^ 1.3 Matrices: Rabbit, rat, bovine, monkey liver, or other tissues as designated in the validation report. 0 W ord 6/95 3MEnvironmental Laboratory ET S-8-7.0 A r a 1 x /c M r \ - f J it r o t - Th v t r < i ' F T T i m -m / y T 2 C / \ / f C Page 1 of 10 Page 175 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 2.0 Summary of M ethod_______________________________ ______________________ _ 2.1 This method describes the analysis o f fluorochemical surfactants extracted from liver using HPLC-electrospray/mass spectrometry, or similar system as appropriate. The analysis is performed by monitoring a single ion characteristic o f a particular fluorochemical, such as the perfluorooctanesulfonate (PFOS) anion, m/z ~ 499. Additionally, samples may be analyzed using a tandem mass spectrometer to further verify the identity o f a compound by detecting daughter ions o f the selected parent ion. 3.0 D efinitions_____________________________________________________________________ 3.1 Atmospheric Pressure Ionization (API): The Micromass Quattro II triple quadrupole systems allow for various methods o f ionization by utilizing various sources, probes, and interfaces. These include but are not limited to: Electrospray Ionization (ESI), Atmospheric Pressure chemical Ionization (APcI), Thermospray, etc. The ionization process in these techniques occurs at atmospheric pressure (i.e. not under a vacuum). 3.2 Electrospray Ionization (ES, ESI): a method o f ionization performed at atmospheric pressure, whereby ions in solution are transferred to the gas phase via tiny charged droplets. These charged droplets are produced by the application o f a strong electrical field. 3.3 Mass Spectrometry, Mass Spectrometer (MS), Tandem Mass Spectrometer (MS/MS): The API Quattro II triple quadrupole mass spectrometer is equipped with two quadrupole mass selective detectors and a collision cell. Ions are selectively discriminated by mass to charge ratio (m/z) and subsequently detected. A single MS may be employed for ion detection or an ion may be selected in the first quadrupole, fragmented in the collision cell, and these fragments may be analyzed in the second quadrupole. 3.4 Conventional vs. Z-spray probe interface: The latest models o f Micromass Quattro II triple quadrupole (post 1998) utilize a "Z-spray" conformation. The spray emitted from a probe is orthogonal to the cone aperture. In the conventional conformation it is aimed directly at the cone aperture, after passing through a tortuous pathway in the counter electrode. Though the configuration is different, the methods o f operation, cleaning, and maintenance are the same. However, Z-spray components and conventional components are not compatible with one another, but only with simil ar systems (i.e. Z-spray components are compatible with other Z-spray systems, etc.) 3.5 Mass Lynx Software: System software designed for the specific operation o f these Quattro II triple quadrupole systems. Currently MassLynx has Windows 95 and WindowsNT 4.0 versions. All versions are similar. For more details refer to the manual specific to the instrument (Micromass Quattro II triple quadrupole MassLynx or MassLynx NT User's Guide). 4.0 W arnings and Cautions__________________________________________________ 4.1 Health and Safety Warnings: 4.1.1 U se caution with the voltage cables for the probe. When engaged, the probe employs a voltage o f approximately 5000 Volts. 3MEnvironmental Laboratory ET S-8-7.0 .f* T tira r* "C v f r o T T c ir ir r In C / A / IO Page 2 o f 10 Page 176 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 4.1.2 When handling samples or solvents wear appropriate protective gloves, eyewear, and clothing. 4.2 Cautions: 4.2.1 Operate the solvent pumps below a back pressure o f 400 bar (5800 psi). If the back pressure exceeds 400 bar, the HP 1100 will initiate automatic shutdown. 4.2.2 Do not run solvent pumps to dryness. 5 .0 I n t e r f e r e n c e s _____________________________________________________________________________ 5.1 To minimize interferences when analyzing samples, Teflon shall not be used for sample storage or any part o f instrumentation that comes in contact with the sample or extract. 6 .0 E q u ip m e n t ______________________________________________ .___________________________________ 6.1 Equipment listed below may be modified in order to optimize the system. Document any modifications in the raw data as method deviations. 6.1.1 6.1.2 Micromass Quattro II triple quadrupole Mass Spectrometer equipped with an electrospray ionization source. HP 1100 low pulse solvent pumping system, solvent degasser, column compartment, and autosampler 7 .0 S u p p l ie s a n d M a t e r ia l s ____________________________ _____________________________________ 7.1 Supplies 7.1.1 High purity grade air regulated to approximately 100 psi (house air system) 7.1.2 HPLC analytical column, specifics to be determined by the analyst and documented in the raw data 7.1.3 Capped autovials or capped 15 ml centrifuge tubes 8 .0 R e a g e n t s a n d S t a n d a r d s ________________________________________________________________ . 8.1 Reagents 8.1.1 Methanol, HPLC grade or equivalent 8.1.2 Milli-QTM water (ASTM type I), all water used in this method should be ATSM type I, or equivalent, and be provided by a Milli-Q TOC Plus system or other vendor 8.1.3 Ammonium acetate, reagent grade or equivalent 8.1.3.1 When preparing different amounts than those listed, adjust accordingly. 8.1.3.2 2.0 mM ammonium acetate solution: Weigh approximately 0.300 g ammonium acetate. Pour into a 2000 mL volumetric container containing 2000 mL Milli-QTM water, mix until all solids are dissolved. Store at room temperature. 3MEnvironmental Laboratory E T S -8 -7 .0 _T ry r \ rt~\ Page 3 o f 10 Page 177 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 8.2 Standards 8.2.1 Typically two method blanks, two matrix blanks, and eighteen matrix standards are prepared during the extraction procedure. Refer to ETS-8-6.0. 9 .0 S a m p l e H a n d l in g ___________________________________________ ______________________________ 9.1 Fresh matrix standards are prepared with each analysis. Extracted standards and samples are stored in capped autovials or capped 15 ml centrifuge tubes until analysis. 9.2 If analysis will be delayed, extracted standards and samples may be stored at room temperature, or refrigerated at approximately 4 C, until analysis can be performed. 10.0 Q u a l it y C o n t r o l _________________________________________ _____________________________ 10.1 M ethod Blanks and Matrix Blanks 10.1.1 Solvent blanks, method blanks, and matrix blanks are prepared and analyzed with each batch to determine contamination or carryover. 10.1.2 Analyze a method blank and a matrix blank prior to each calibration curve. 10.2 M atrix Spikes 10.2.1 Matrix spikes are prepared and analyzed to determine the matrix effect on the recovery efficiency. 10.2.2 Matrix spike duplicates are prepared and analyzed to measure the precision and the recovery for each analyte. 10.2.3 Analyze a matrix spike and matrix spike duplicate per forty sample^. With a minimum o f 2 spikes per batch. 10.2.4 Matrix spike and matrix spike duplicate concentrations will fall in the mid-range o f the initial calibration curve. Additional spike concentrations may fall in the lowrange o f the initial calibration curve. 10.3 Continuing Calibration Checks 10.3.1 Continuing calibration verifications are analyzed to verify the continued accuracy o f the calibration curve. 10.3.2 Analyze a mid-range calibration standard every tenth sample, with a minimum o f one per batch. 1 1 .0 C a l i b r a t io n a n d S t a n d a r d iz a t io n ____________________________________________________ 11.1 Analyze the extracted matrix standards prior to and following each set o f sample extracts. The average o f two standard curves will be plotted by linear regression (y = mx + b), weighted 1/x, not forced through the origin, using MassLynx or other suitable software. 1 1.2 If the curve does not meet requirements perform routine maintenance or reextract the standard curve (if necessary) and reanalyze. 3MEnvironmental Laboratory ETS-8-7.0 Page 4 of 10 Page 178 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 11.3 For purposes o f accuracy when quantitating low levels o f analyte, it may be necessary to use the low end o f the calibration curve rather than the foil range of the standard curve. Example: when attempting to quantitate approximately 10 ppb o f analyte, generate a calibration curve consisting o f the standards from 5 ppb to 100 ppb rather than the full range o f the curve (5 ppb to 1000 ppb). This will reduce inaccuracy attributed to linear regression weighting o f high concentration standards. 12.0 Procedures____________________________________________________________________ 12.1 Acquisition Set up 12.1.1 Set up the sample list. 12.1.1.1 Assign a sample list filename using MO-DAY-last digit o f year-increasing letter o f the alphabet starting with a 12.1.1.2 Assign a method (MS file) for acquiring 12.1.1.3 Assign an HPLC program (Inlet file) 12.1.1.4 Type in sample descriptions and vial position numbers 12.1.2 To create a method click on method in the Acquisition control panel then mass spectrometer headings and select SIR (Single Ion Recording) or MRM (Multiple Reaction Monitoring). Set Ionization Mode as appropriate and mass to 499 or other appropriate masses. A full scan is usually collected along with the SIRs. Save acquisition method. If MS/MS instruments are employed, additional product ion fragmentation information may be collected. Refer to Micromass MassLynx GUIDE TO DATA ACQUISITION for additional information and MRM. 12.1.3 Typically the analytical batch run sequence begins and ends with a set o f extracted matrix standards. 12.1.4 Samples are analyzed with a continuing calibration verification injected standard after every tenth sample. Solvent blanks should be analyzed periodically to monitor possible analyte carryover and are not considered samples but may be included as such. 12.2 Using the Autosampler 12.2.1 Set up sample tray according to the sample; list prepared in Section 12.1.1. 12.2.2 Set-up the HP1100/autosampler at the following conditions or at conditions the analyst considers appropriate for optimal response. Record actual conditions in the instrument logbook: 12.2.2.1 Sample size = 10 pL injection 12.2.2.2 Inject/sample = 1 12.2.2.3 Cycle time = 9 minutes 3MEnvironmental Laboratory A ___1. ETS-8-7.0 __ * t ro/ikto Page 5 of 10 Page 179 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 12.2.2.4 Solvent ramp conditions Time MeOH 0.00 min. 1.0 min. 4.5 min. 6.5 min. 7.0 min. 9.0 mi. 40% 40% 95% 95% 40% 40% 2.0 mM Ammonium acetate 60% 60% 5% 5% 60% 60% 12.2.2.5 Press the "Start" button. 12.3 Instrument Set-up 12.3.1 Refer to ETS-9-24.0, "Operation and Maintenance o f the Micromass Quattro II Triple Quadrupole Mass Spectrometer Fitted with an Atmospheric Pressure Ionization Source," for more details. 12.3.2 Check the solvent level in reservoirs and refill if necessary. 12.3.3 Check the stainless steel capillary at the end o f the probe. Use an eyepiece to check the tip. The tip should be flat with no jagged edges. If the tip is found to be unsatisfactory, disassemble the probe and replace the stainless steel capillary. 12.3.4 Turn on the nitrogen. 12.3.5 Open the tune page. Clicks on operate to initiate source block and desolvation heaters. 12.3.6 Open the Inlet Editor. 12.3.6.1 Set HPLC pump to "On" 12.3.6.2 Set the flow to 10 - 500 uL/min or as appropriate 12.3.6.3 Observe droplets coming out o f the tip o f the probe. A fine mist should be expelled with no nitrogen leaking around the tip o f the probe. Readjust the tip o f the probe if no mist is o bserved 12.3.6.4 Allow to equilibrate for approximately 10 minutes. 12.3.7 The instrument uses these parameters at the following settings. These settings may change in order to optimize the response: 12.3.7.1 Drying gas 250-400 liters/hour 12.3.7.2 ESI nebulizing gas 10-15 liters/hour 12.3.7.3 HPLC constant flow mode flow rate 10 - 500 pL/min 12.3.7.4 Pressure <400 bar (This parameter is not set, it is a guide to ensure the HPLC is operating correctly.) 12.3.7.5 Source block temperature 150 12.3.7.6 Desolvation temperature 250 3MEnvironmental Laboratory ETS-8-7.0 Page 6 o f 10 Page 180 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 12.3.8 Print the tune page, with its parameters, and store it in the study binder with a copy taped into the instrument log. 12.3.9 Click on start button in the Acquisition Control Panel (this may vary among MassLynx versions, refer to appropriate MassLynx User's Guide). Ensure start and end sample number includes all samples to be analyzed. 1 3 .Q D a t a A n a l y s is a n d C a l c u l a t io n s _____________________ _________________________________ 13.1 Calculations: 13.1.4 Calculate matrix spike percent recoveries using the following equation: % Recovery = Observed Result - Background Result x 100 Expected Result ' 13.1.5 Calculate percent difference using the following equation: % Difference = Expected Cone. - Calculated Cone, x 100 Expected Cone. 13.1.6 Calculate actual concentrations in matrix (p.g/g): (ng o f PFOS calc, from std. Curve x Dilution Factor) (Initial Weight o f Liver (gl Final Volume (mL) x 1 fig 1000 ng 14.0 M e t h o d P e r f o r m a n c e __________________________________________________________ 14.1 Method Detection Limit (MDL) and Limit o f Quiintitation (LOQ) are method, analyte, and . matrix specific. Refer to ETS-8-6.0, Attachmen t B for a listing o f current validated MDL and LOQ values. 14.2 Solvent Blanks, Method Blanks and Matrix Blanks 14.2.1 S olvent blanks, m ethod blanks, and m atrix blanks m ust be below the low est standard in the calibration curve. . 14.3 Calibration Curves 14.3.1 The r2 value for the calibration must be 0.980 or better. 14.4 Matrix Spikes 14.4.1 Matrix spike percent recoveries must be within 30% o f the spiked concentration. 14.5 Continuing Calibration Verification 14.5.1 Continuing calibration verification percent recoveries must be within 30% o f the . spiked concentration. 14.6 If criteria listed in the method performance section are not met, maintenance may be performed on the system and samples reanalyzed or other actions as determined by the analyst. Document all actions in the appropriate logbook. 3MEnvironmental Laboratory ETS-8-7.0 Page 7 of 10 P age 181 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 14.7 If data are to be reported when performance criteria have not been met, the data must be footnoted on tables and discussed in the text o f the report. 1 5 .0 P o l l u t i o n P r e v e n t io n a n d W a s t e M a n a g e m e n t __________________________________ __ 15.1 Sample extract waste and flammable solvent is disposed in high BTU containers, and glass pipette waste is disposed in broken glass containers located in the laboratory. 1 6 .0 R e c o r d s _______________________________________________________________ ^___________________ 16.1 Each page generated for a study must have the fol lowing information included either in the header or hand written on the page: study or project number, acquisition method, integration method, sample name, extraction date, dilution factor (if applicable), and analyst. 16.2 Print the tune page, sample list, and acquisition method from MassLynx to include in the appropriate study folder. Copy these pages and tape into the instrument runlog. 16.3 Plot the calibration curve by linear regression, weighted 1/x, then print these graphs and store in the study folder. 16.4 Print data integration summary, integration method, and chromatograms from MassLynx and store in the study folder. 16.5 Summarize data using suitable software (Excel 5.0+) and store in the study folder, refer to Attachment A for an example o f a summary spreadsheet. 1 6.6 Back up electronic data to appropriate medium. Record in study notebook the file name and location o f backup electronic data. 1 7 .0 T a b l e s . D ia g r a m s . F l o w c h a r t s , a n d V a l i d a t i o n D a t a _____________________________ 17.1 Attachment A: ETS-8-7.0 Data summary spreadsheet 18.0 R eferences____________________________________________________________________ 18.1 FACT-M-2.1, "Extraction o f Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds from Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry" 1 8.2 ETS-9-24.0, "Operation and Maintenance o f the Micromass Atmospheric Pressure Ionization/Mass Spectrometer Quattro II triple quadrupole Systems" 18.3 The validation report associated with this method is ETS-8-6.0 & 7.0-V-l 19.0 A f f e c t e d D o c u m e n t s ___________________________________________________________________ 19.1 ETS-8-6.0, "Extraction o f Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds from Liver or Fluid for Analysis Using HPLC-Electrospray/Mass Spectrometry" 3MEnvironmental Laboratory ETS-8-7.0 -*r i Page 8 o f 10 Page 182 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 ' LRN-U2103 20.0 R e v isio n s Revision Number Reason For Revision Revision Date 3M E nvironm ental Laboratory E T S -8 -7 .0 Page 9 o f 10 P age 183 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Laboratory Study # Study: T est Material: M atrix/Final Solvent: M ethod/Revision: Analytical Equipment System Number: Instrument Software/Version: F ilenam e: R-Squared Value: Slope: Y Intercept: Date o f Extraction/Analyst: Date o f Analysis/Analyst: Group Sample# Concentration Dose ng/g initial Wt. g Dilution Factor Final Cone, g/g Slope: G roup/D ose: Taken from the study folder. Sam ple#: Taken from the study folder. C oncen tration (ng/g): Taken from the M assLynx integration summary. Initial W t. (g): Taken from the study folder. D ilution F actor: Taken from the study folder. F inal C one, (ug/g): Calculated by dividing the initial volum e from the concentration Attachment A: Summary Spreadsheet A ,, .1 3MEnvironmental Laboratory ET S-8-7.0 -r T : T T..: t ?p a # o Page 10 of 10 Page 184 3M M edical D epartm ent Study: T6316.1 3M Medical Department Study: T-6316.1 Appendix D: Data Summary Tables Analytical Report: FACT-TOX-001 LRN-U2103 Analytical Report: FACT TOX-001 LRN-U2103 3MEnvironmental Laboratory Page 185 3M M edical D epartm ent Study: T6316.1 3M E nvironm ental Laboratory 3M Medical Department Study: T-6316.1 Analytical Report: FACT TOX-001 LRN-U2103 Table 10. FACT TOX-001 Data Summary of PFOS Concentration--Serum (|jg/mL) Tim epoint Sex Group 1 Control Average SD Group 2 Low Average SD Group 3 M id Average SD Group 4 M id-High Average SD Group 5 High Average SD Group 6 M id-High Recovery Average SD W eek4a W rr+r q3 Male Female Male Female 0.0405 0.0215 (n = 5) 0.117 0.00828 (n = 5) 0.0518 0.0174 (n = 5) 0.181 0.0174 (n = 5) 1.86 0.252 (n = 5) 3.26 0.415 (n = 5) 21.6 1 .9 9 (n = 5) 29.9 3 .84 (n = 5) 60.4 8 .7 6 (n = 5) 70.7 1 6.8 (n = 5) 229 42.5 (n = 5) 357 65.2 (n = 5) 348 41.5 (n = 5) 576 40.1 (n = 5) W eek 14a Week 27 Week 53 W eek 105 Male Female Male Female Male Female Male Female 0.0779 0.00791 (n = 5) 0.196 0.0361 (n = 5 ) 0.0415 0.00951 (n = 10) 0.0793 + 0 0172 (n = 10) 0.0191 0.0134 (n = 15) 0.0755 0.0376 (n = 15) 0.00936 0.0123 (n = 14) 0.0271 0.0237 (n = 13) 6.14 0.688 (n = 5) 12.2 1 .83 (n = 5) 2.75 0.906 (n = 10) 4.85 0.954 (n = 10) 1.86 1.128 (n = 10) 4.67 1.63 (n = 10) 1.18 1.41 (n = 22) 3.75 2.65 (n = 11)* 59.1 1 1 .3 (n = 5) 104 25.4 (n = 5) 20.3 2 .85 (n = 10) on *7 i JL "17.oJnO (n = 10) 18.0 7.18 (n = 10) 3 3 .6 1 1 .4 (n = 10) 22.0 17.6 (n = 22) 55.2 27.4 (n = 15) 192 24.6 (n = 5) 268 34.0 (n = 5) 77.2 15.2 (n = 10) 170 38.3 (n = 10) 82.4 66.0 (n = 15) 163 87.2 (n = 15) 84.6 4 5.4 (n = 17) 122 70.5 (n = 19) 0.227 0.377 (n = 10) 2.41 2 .3 2 (n = 12) 'Animal C91216F sample lost during extraction. NOTE: Results are expressed as group/gender averages the standard deviation associated with that group/gender. NOTE: The only measurement of accuracy available at this time, matrix spike studies, indicate that the sera and liver data can be considered accurate to within one standard deviation of the average fortified samples recovery. The average fortified sample recoverywas 96% with a standard deviation of 25%. Analytical Report: FACT-TOX-OOl L R N -U 2103 Page 186 3M M edical D epartm ent Study: T6316.1 3M E nvironm ental Laboratory 3M Medical Department Study: T-6316.1 Analytical Report: FACT TOX-001 LRN-U2103 Table 11. FACT TOX-001 Data Summary of PFOSA Concentration--Serum (|jg/mL) Tim epoint Sex Group 1 Control Average SD Group 2 Low Average SD Group 3 M id Average SD Group 4 M id-High Average SD Group 5 High Average SD Group 6 M id-High Recovery Average SD W eek4a W eek8a Male Female Male Female <LOQb (n = 5) <LOQb (n = 5) <LOQ (n = 5) <LOQ (n = 5) 0.0310 0.00549 (n = 5) 0.0622 0.00874 (n = 5) 0.698 0.0818 (n = 5) 1.27 0.404 (n = 5) 1.81 0 .5 2 0 (n = 5) 2.48 0.344 (n = 5) 1.19 0.147 (n = 5) 3.04 2 .0 0 (n = 5) 1.10 0.288 (n = 5) 1.08 0.381 (n = 5) W eek 14a Male Female <LOQa (n = 5) <LOQe (n = 5) 0.0598 0.0110 (n = 5) 0.110 0.0280 (n = 5) 0.494 0.141 (n = 5) 0.769 0.141 (n = 5) 0.778 0.0605 (n = 5) 1.88 0 .5 0 3 (n = 5) 3 r -5 5 . Week 27a Male Female <LOQd (n = 10) 0.0177 0.0116 (n = 10) 0.0337 0.00608 (n = 10) 0.226 0.0368 (n = 10) 1 1A CAO j A 4r\4 V -W U _l_\J . \J (n = 10) 0.418 0.0903 (n = 10) 0.875 0.335 (n = 10) W eek 53a Male Female <LOQd (n = 15) <LOQd (n = i 5) <LOQd (n = 10) <LOQd (n = 10) 0.237 0.0751 (n = 10) 0.366 0.0824 (n = 10) 0.357 0.138 (n = 15) 1.10 0.536 (n = 15) W eek 105a Male <LOQd (n = U ) 0.0187 0.0119 (n = 22) 0.306 0.116 -(n = 22) 0.701 0.363 (n = 17) <LOQd (n = 10) Female <LOQd (n = 13) 0.0846 0.104 (n = 11)* 0.429 0.133 (n = 15) -------------------- T T T T --r 1.30 0.512 (n = 19) <LOQd (n = 12) ' LOO--Umit of Quantitation = 0.00249pgi'mL c. L,_OTOr--. U_mit of Quantitation = 0.0.0978pg/ml_ LOQ--Umit of Quantitation=0.0978 pg/mL 'Animal C91216F sample lost during extraction. N O TE: Results are expressed as group/gender averages the standard deviation associated with that group/gender. NOTE: J ^ o n ly m^surement of accuracy available atthis time, matrix spike studies, indicate that the sera and liver data can be considered accurate to within one standard deviation of the average fortified samples recovery. The average fortifiedsample recoverywas 100% with a standard deviation of 16%. Analytical Report: FACT-TOX-OOl L R N -U 2103 Page 187 3M M edical D epartm ent Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT TOX-001 LRN-U2103 Analytical Report: FACT-TOX-001 L R N -U 2103 Table 12. FACT TOX-001 Data Summary of PFOSAA Concentration--Serum (pg/mL) Tim epoint Sex Group 1 Control Average SD Group 2 Low Average SD Group 3 M id Average SD Group 4 M id -H ig h Average SD Group 5 High Average SD Group 6 M id-High Recovery Average SD W eek4a W eek8a Male Female Male Female 0.0511 0.0291 (n = 5) 0.0604 0.0152 (n = 5) 0.0169 0.00974 (n = 5) 0.0433 0.00973 (n = 5) 2.60 1 .6 3 (n = 5) 3.07 1 .45 (n = 5) 13.2 2 .3 0 (n = 5) 23.1 8 .9 5 (n = 5) 26.9 9.28 (n = 5) 33.8 13.6 (n = 5) 61.2 1 4 .2 (n = 5) 92.5 2 8.3 (n = 5) 67.0 1 2.0 (n = 5) 80.9 1 5.3 (n = 5) W eek 14a Male Female 0.0360 0.0145 (n = 5) 0.0363 0.00761 (n = 5) 1.23 0.506 (n = 5) 1.87 0.659 (n = 5) 13.8 6 .6 3 (n = 5) 16.4 8 .2 6 (n = 5) 20.8 4.38 (n = 5) 33.8 5.71 (n = 5) W eek 27s Male Female <LOQb (n = 10) <LOQb (n = 10) 0.577 0.455 (n = 10) 0.772 0.311 (n = 10) 2.27 0.848 (n = 10) 3.46 1 .03 (n = 10) 6.58 2.06 (n = 10) 8.04 2.13 (n = 10\ W eek53a Male Female <LOQd (n = 15) <LOQd (n = 15) 0.597 0.497 (n = 10) 0.556 0.199 (n = 10) 4.80 1.72 (n = 10) 4.22 1 .1 4 (n = 10) 9.0 6 .23 (n = 15) 12.8 6 .59 (n = 15) W eek 105a Male Female <LOQc (n = 14) <LOQc (n = 13) 0.553 0.345 (n = 22) 1.51 1 .4 2 (n = 11)' 4.14 1.92 (n = 22) 6 .1 4 2 .1 0 (n = 15) 10.7 7.93 (n = 17) 11.9 3.02 (n = 19) <LOQb (n = 10) <LOQb (n = 12) Not corrected for purity of the standard material. ''LOO--Umit of Quantitation = 0.0248 pg/mL cLOQ--Umit of Quantitation = 0.00493 pgfmL dLOQ--Umit of Quantitation = 0.0097 `Animal C91216F sample was lost during extraction. N O TE: Results are expressed as group/gender averages the standard deviation associated with that group/gender. N O TE: T h e only m easurem ent of accuracy available at this tim e, m atrix spike studies, indicate that the sera and liver data can be considered accurate to w ithin one standard deviation o f the average fortified sam ples recovery. The average fortified sample recovery was 109% w ith a standard deviation of 23%. 3MEnvironmental Laboratory Page 188 3M M edical D epartm ent Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT TOX-001 LRN-U2103 Analytical Report: FACT-TOX-001 L R N -U 2103 Table 13. FACT TOX-001 Data Summary of EtFOSE-OH Concentration--Serum (|jg/mL) Tim epoint Sex Group 1 Control Average SD Group 2 Low Average SD Group 3 M id Average SD Group 4 M id-High Average SD Group 5 High Average SD Group 6 M id-High Recovery Average SD W eek4a Male Female W eek8a Male Female W eek14a Male Female Week 27a Male Female <LOQb (n = 10) <LOQb (n = 10) <LOQc (n = 10) <LOQ (n = 10) <LOQ (n = 10) <LOQc (n = 10) <LOQc (n = 10) <LOQc (n = 10) W eek 53a Male Female <LOQb (n = 15) <LOQd (n = 15) <LOQd (n = 10) <LOQb (n = 10) <LOQb (n = 10) 0.0258 0.00252 (n = 10) 0.0215 0.00992 (n = 15) 0.0231 0.00963 (n = 15) W eek 105a Male Female <LOQb (n = 14) <LOQb (n = 13) <LOQb (n = 22) <LOQb (n = 11)* 0.00912 0.00430 (n = 22) rvt/.numi vou x. r\ \r\e.0 0 (n = 15) 0.0182 0.0170 (n = 17) 0.0354 0.0145 (n = 19) <LOQb (n = 10) <LOQ (n = 12) aNot corrected for purityot the standard material. bLOQ--Umit of Quantitation = 0.00977 pg/mL cLOQ--Limit of Quantitation = 0.0248 pg/mL dLOQ-- Umit of Quantitation = 0.00493 ug/mL 'Animal C91216F sample was lost during extraction. NOTE: Results are expressed as group/gender averages the standard deviation associated with that group/gender. N O TE: The results of qualitycontrol analyses (curve fit, CCVs, and MS/MSDs) for EtFOSE-OH were inconsistent and indicate that data presented should be considered to be qualitative only. Values are presented in this data table in the spirit of full disclosure, but should not be used in any quantitative assessment of the data. 3MEnvironmental Laboratory Page 189 3M M edical D epartm ent Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT TOX-001 LRN-U2103 Analytical Report: FACT-TOX-001 L R N -U 2103 Table 14. FACT TOX-001 Data Summary of M556 Concentration--Serum (pg/ml_) Tim epoint Sex Group 1 Control Average SD Group 2 Low Average SD Group 3 M id Average SD Group 4 M id-High Average SD Group 5 High Average SD Group 6 M id-High Recovery Average SD W eek4a Male Female * W eeks3 Male Female W eek143 Male Female Week 27a Male Female <LOQb (n = 10) <LOQb (n = 10) 0.267 0.0634 (n = 10) 0.303 0.0744 (n = 10) 2.03 0.449 (n = 10) 3.96 0.796 (n = 10) 6.61 1 .3 0 (n = 10) 6.36 2.11 (1 = 10) Week 53a Male Female <LOQc (n = 15) <LOQc (n = 15) 0.371 0 .1 1 0 (n = 10) 0.439 0.134 (n = 10) 4.00 0.970 (n = 10) 4.10 0.771 (n = 10) 10.4 5 .48 (n = 15) 12.6 6 .98 (n = 15) \*A/ vU Ti f\ H1A\JC\J Male Female <LOQ (n = 14) <LOQc (n = 13) 0.145 0.115 (n = 22) 0.680 0.667 (n = 11)* 2.86 1.191 (n = 22) 3.02 1 .08 (n = 15) 6.58 2.71 (n = 17) 5.06 1 .39 (n = 19) <LOQc (n = 10) <LOQc (n = 12) aNot corrected for purity of the standard material. bLOQ--Umit of Quantitation = 0.0248 pg/mL cLOQ--Umit of Quantitation = 0.00494 pgfmL 'Animal C91216F sample lost during extraction. N O TE: Results are expressed as group/gender averages th e standard deviation associated with that group/gender. N O T E : T h e only m e asu rem en t of accuracy available at this time, m atrix spike studies, indicate that the sera an d liver d ata can b e considered accurate to within o ne standard deviation of the average fortified sa m p le s recovery. T he average fortified sa m p le recovery w a s 1 2 3 % w ith a standard deviation of 2 0 % . 3MEnvironmental Laboratory Page 190 3M M edical D epartm ent Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT TOX-001 LRN-U2103 Analytical Report: FACT-TOX-001 L R N -U 2103 Table 15. FACT TOX-001 Data Summary of PFOSEA Concentration--Serum (pg/mL) Tim epoint Sex Group 1 Control Average SD Group 2 Low Average SD Group 3 M id Average SD Group 4 M id-High Average SD Group 5 High Average SD Group 6 M id-High Recovery Average SD W eek4a W eek 8a W eek 14a Week 27a Week 53a W eek 105a Male Female Male Female Male Female Male Female Male Female Male Female <LOQb (n * 10) <LOQb (n = 10) <LOQc (n = 15) <LOQc (n = 5) <LOQc (n = 14) <LOQc (n = 13) <LO Q bc (n = 10) <LOQc (n = 10) <LOQ (n = 10) <LOQa (n = 10) <LOQc (n=22) <LOQc (n = 11)' <LOQd (n = 10) <LOQd (n = 10) <LOQe (n = 10) <LOQb (n = 10) <LOQc (n = 22) <LOQc (n = 15) <LOQd (n = 10) <LOQd (n = 10) <LO Q b,c (n = 15) <LO Q bc (n = 15) <LOQc (n = 17) <LOQ (n = 19) <LOQc (n = 10) <LOQc (n = 12) bLOQ-- Umit of Quantitation = 0.0247 pg/mL cLOQ-- Umit of Quantitation = 0.00492 pg/mL dLOQ-- Umit of Quantitation = 0.00975 pg/mL eLOQ-- Umit of Quantitation = 0.0492 pg/mL 'Animal C91216F sample lost during extraction. NOTE: Results are expressed as group/gender averages the standard deviation associated with that group/gender. N O TE: The results of quality control analyses (curve fit, CCVs, and MS/MSDs) for PFOSEA were inconsistent and indicate that data presented for this analyte should be considered to be qualitative only. Values are presented here in the spirit of full disclosure, but should not be used in any quantitative assessment of the data. 3MEnvironmental Laboratory P age 191 3M M edical D epartm ent Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT TOX-001 LRN-U2103 Analytical Report: FACT-TOX-001 L R N -U 2103 Table 16. FACT TOX-001 Data Summary of PFOS Concentration--Liver (pg/g) Tim epoint Sex Group 1 Control Average *SD Group 2 Low Average SD Group 3 M id Average SD Group 4 M id-High Average SD W eek4a W eek8a W eek 14 Week 27 Week 53 Week 105 Male Female Male Female Male Female Male Female Male Female Mae Female 0.774 0.138 (n = 5) 0.368 0.144 (n = 5) 2.13 0.668 (n = 5) 0.549 0.328 (n = 5) 1.23 0.262 (n = 5) 0.402 0.129 (n = 5) 12.4 1 .6 7 (n = 5) 1 1 .3 1 .9 4 (n = 5) 23.4 2 .14 (n = 5) 23.6 3 .4 8 (n = 5) 0.571 0.175 (n = 5) 0.390 0.0993 (n = 5) 0.143 0.133 (n = 18) 0.178 0.111 (n = 14) 7.56 7 .1 0 (n = 22) 38.5 2 1 .9 (n = 13) 96.1 2 0 .4 (n = 5) 120 25.3 (n = 5) 80.8 5 0 .9 (n = 5) 141 5 6 .0 (n = 5) 90.1 7 0 .3 (n = 22) 127 68.5 (n = 15) 199 53.2 (n = 5) 229 121 (n = 5) 392 94.1 (n = 5) 335 178 (n = 5) 695 189 (n = 5) 694 123 (n = 5) 040 . non o i g x C -C X l (n = 17) 297 171 (n = 19) Group 5 High Average SD 499 208 (n = 5) 597 180 (n = 5) 1067 197 (n = 5) 1065 213 (n = 5) Group 6 M id-High Recovery Average SD 2.05 3 .36 (n = 10) 7.69 7.62 (n = 12) NOTE: Results are expressed as group/gender averages the standard deviation associated with that group/gender. NOTE: The only measurement of accuracy available at this time, matrixspike studies, indicate that the sera and liver data can be considered accurate to within one standard deviation of the average fortified samples recovery. The average fortified sample recoverywas 110% with a standard deviation of 29% (revised results). 3MEnvironmental Laboratory Page 192 3M M edical D epartm ent Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT TOX-001 LRN-U2103 Analytical Report: FACT-TOX-001 L R N -U 2103 Table 17. FACT TOX-001 Data Summary of PFOSA Concentration--Liver (pg/g) Tim epoint Sex Group 1 Control Average SD Group 2 Low Average SD Group 3 M id Average SD Group 4 M id-High Average SD Group 5 High Average SD Group 6 M id-H igh Recovery Average SD W eek4a Male Female 0.0150 0.00746 (n = 5) 0.0184 0.00804 (n = 5) 0.562 0.212 (n = 5 ) 0.681 0 .0 5 7 2 (n = 5) 6.82 1 .08 (n = 5) 6.14 1 .0 8 (n = 5) 9.57 2 .33 (n = 5) 8.25 2.19 (n = 5) 8.94 5 .05 (n = 5) 15.3 2.31 (n = 5) W eek8a Male Female 0.0313 0.00163 (n = 5) 0.0310 0.00189 (n = 5) 19.2 0.987* (n = 5) 15.5 1 .6 5 * (n = 5) W eek 14a Male Female 0.0284 0.0202 (n = 4)* 0.0156 0.00784 (n = 5) 1.11 0 .1 9 4 (n = 5) 1.80 0.0831 (n = 5) 8.25 2 .0 0 (n = 5) 7.98 1 .03 (n = 5) 16.5 1 .2 0 (n = 5) 14.6 1 .52 (n = 5) W eek 27a Male Female Week 53a Male Female 0.0182 0.0100 (n = 5) 0.0139 0.00677 (n = 5) 28.2 8 .44 (n = 5) 25.3 4.37 (n = 5) W eek 105a Male Female <LOQb (n = 18) <LOQb (n = 14) 0.744 0.294 " ( n = 21) 1.82 1 .7 2 (n = 13) ? A A 2.17 (n = 22) 6.77 1 .7 2 (n = 15) 13.5 4 .23 (n = 17) 15.6 3.61 (n = 19) <LOQc (n = 10) <LOQc (n = 12) a Not corrected for purity of the standard material. bLO Q -- Um it of Quantitation = 0.0123 pg/g cLO Q -- Limit of Quantitation = 0.00614 pg/g 'A nim al C 9 0 7 4 8 M sam ple lost during extraction. *C C V s failed, data entered as estimated. NOTE: Results are expressed as group/gender averages the standard deviation associated with that group/gender. NOTE: T he only m easurem ent of accuracy available atthis tim e, m atrix spike studies, indicate that the sera and liver data can be considered accurate to within one standard deviation of the average fortified sam ples recovery. The average fortified sample recovery was 102% w ith a standard deviation of 17% (revised results). 3MEnvironmental Laboratory P age 193 3M M edical D epartm ent Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT TOX-001 LRN-U2103 Analytical Report: FACT-TOX-001 L R N -U 2103 Table 18. FACT TOX-001 Data Summary of PFOSAA Concentration--Liver (|jg/g) Tim epoint Sex Group 1 Control Average SD Group 2 Low Average SD Group 3 Mid Average SD Group 4 M id-High Average SD Group 5 High Average SD Group 6 M id-High Recovery Average SD W eek4a Male Female 0.134 0.0617 (n = 5) 0.0995 0.0390 (n = 5) 3.63 3.42 (n = 5) 4.09 2.16 (n = 5) 59.6 22.6 (n = 5) 61.8 34.1 (n = 5) 53.1 2 1 .9 (n = 5) 52.5 1 4.9 (n = 5) 85.7 2 0 .4 (0 = 5) 80.1 5 0 .9 (0 = 5) Week 8a Male Female 0.0980 0.0351 (n = 5) 0.0920 0.0561 (n = 5) 483 72.7 (0 = 5) 330 67.2 (0 = 5) W eek 14a Male Female 0.145 0.0611 (n = 4)* 0.106 0.0699 (n = 5) 1.85 0.351 (n = 5) 2.66 0.462 (n = 5) 20.0 14.6 (n = 5) 14.9 8 .95 (n = 5) 81.1 2 4.1 (o = 5) 59.2 14.6 (n = 5) W eek 27a Male Female Week 53a Male Female <LOUt (n = 5) <LOQb (n = 5) 55.7 21.3 (n = 5) 47.6 5.67 (n = 5) W eek 105a Maie Female 0.0461 0.0174 (n = 18) 0.0354 0.0162 (n = 14) 1.86 2 .00 (n"= 2 1 ) 3.49 4 .47 (n = 13) 11.4 6 .95 (n = 22) 7.98 3 .48 (n = 15) 23.6 13.3 (0 = 17) 26.9 7 .0 8 (n = 19) 0.0522 0.0614 (n = 10) <LOQc (n = 12) a Not corrected for purity of the standard material. bLOQ-- Um it of Quantitation = 0.0307 pgfg cLO Q -- Um it of Quantitation = 0.0123 pgfg 'Anim al C 9 0748M lost during extraction. N O TE: Results are expressed as group/gender averages the standard deviation associated with that group/gender. N O T E : The o nly measurem ent of accuracy available a t this time, matrix spike studies, indicate that the sera and liver data can be considered accurate to within one standard deviation of the average fortified sam ples recovery. The average fortified sam ple recovery w a s 105% with a standard deviation of 19% (revised results). 3MEnvironmental Laboratory Page 194 3M M edical D epartm ent Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT TOX-001 LRN-U2103 Analytical Report: FACT-TOX-001 L R N -U 2103 Table 19. FACT TOX-001 Data Summary of EtFOSE-OH Concentration--Liver (pg/g) Tim epoint Sex Group 1 Control Average SD Group 2 Low Average SD Group 3 M id Average SD Group 4 M id -H ig h Average SD W eek4a W eek8a W eek14a Week 27a W eek 53a W eek 105a Male Female Male Female Male Female Male Female iviaie Female Male Female <LOQb (n = 5) <LOQb (n = 5) 0.0316 0.00402 (n = 5) <LOQd (n = 5) <LOQb (n = 5) <LOQb (n = 5) <LOQc (n = 5) <LOQ (n = 5) 0.0870 0.0351 (n = 5) 0.0442 0.00682 (n = 5) 0.464 0.154 (n = 5) 0.375 0.213 (n = 5) NA 0.206 0.0677 (n = 5) NA 0.148 0.0224 (n = 5) NA NA NR NR 0.0796 0.0287 (n = 18) 0.0906 0.0394 (n = 14) 0.0649 0.0130 (n = 22) 0.0766 0.0210 (n = 13) 0.0883 0.0415 (n = 22) 0.103 0.0276 (n = 15) NR NR 0.395 0.229 (n = 17) 0.994 1 .30 (n = 19) Group 5 High Average SD 0.704 0.335 (n = 5) 0.762 0.443 (n = 5) 0.338 0 .463 (n = 5) 0.352 0.359 (n = 5) Group 6 M id-High Recovery Average SD <LOQa (n = 10) <LOQa (n = 12) bLO Q -- Limit of Quantitation = 0.0596 pg/g cL O Q -- Limit of Quantitation = 0.119 pg/g dLO Q -- Limit of Quantitation = 0.0298 pg/g "LO O -- Limit of Quantitation = 0.0614 pg/g NA-- Not applicable NR-- Not reported Animal C 9 1 2 1 6 F sam ple lost during extraction. NOTE: Results are expressed as group/gender averages the standard deviation associated with that group/gender. N O TE : T h e results of quality control analyses (curve fit, CCVs, and M S/M SDs) for E tFO S E -O H w ere inconsistent and indicate that data presented for this analyte should be considered to be qualitative only. Values are presented here in the spirit of full disclosure, but should not be used in any quantitative assessm ent of the data. 3MEnvironmental Laboratory Page 195 3M M edical D epartm ent Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT TOX-001 LRN-U2103 Analytical Report: FACT-TOX-001 L R N -U 2103 Table 20. FACT TOX-001 Data Summary of M556 Concentration--Liver (|jg/g) Tim epoint Sex Group 1 Control Average SD Group 2 Low Average SD Group 3 M id Average SD Group 4 M id-High Average SD Group 5 High Average SD Group 6 M id-H igh Recovery Average SD W eek4 Male Female Week 8 Male Female W eek 14 Male Female Week 27 Male Female W eek53a W eek 105a Male Female Male Female <LOQb (n = 5 ) <LOQb (n = 5) - i r\/"\b.e (n = 18) < L O Q b,f (n = 14) 0.460 0.378 (n = 22) 2.03 2 .74 (n = 13) 9.5 i 3.29 (n = 22) 8.57 3.33 (n = 15) 58.9 1 7.0 (n = 5) 36.3 9.51 (n = 5) 27.1 9.41 (n = 17) 28.5 8 .86 (n = 19) <LO Q cd (n = 10) <LO Q od (n = 12) a Not corrected for purity of the standard material. bLO Q -- Limit of Quantitation = 0.0308 pgfg cL O Q -- Limit of Quantitation = 0.00615 pg/g dLO Q -- Um it of Quantitation = 0.123 pg/g *LO Q -- Limit of Quantitation = 0.0123 pg/g V O Q -- Limit of Quantitation = 0.0615 pg/g NOTE: Results are expressed as group/gender averages the standard deviation associated with that group/gender. N O T E : T he only m e a s u re m e n t of accuracy available a t this time, m atrix spike studies, indicate that th e sera an d liver d ata can b e considered accurate to within o n e standard deviation of the average fortified sam p les recovery. T he average fortified s a m p le recovery w a s 1 0 2 % with a standard deviation of 15% . 3MEnvironmental Laboratory Page 196 3M M edical D epartm ent Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT TOX-001 LRN-U2103 Analytical Report: FACT-TOX-001 L R N -U 2103 Table 21. FACT TOX-001 Data Summary of PFOSEA Concentration--Liver (pg/g) Tim epoint Sex Group 1 Control Average SD Group 2 Low Average SD Group 3 M id Average SD Group 4 M id-High Average SD Group 5 High Average SD Group 6 M id-H igh Recovery Average SD Male Female W eeks Male Female W eek 14 Male Female W eek 27 Male Female W eek 53 Male Female NR NR NR NR Male < L O Q bc (n = 18) < L O Q b,c (h = 22) <LOQb (n = 22) 0.0408 0.0566 (n = 17) <LOQb (n = 10) Female < L O Q bc (n = 14) I3I co <LOQb (n = 15) 0.0241 0.0139 (n = 19) <LOQb (n = 12) 8 Not corrected for purity of the standard material bLO Q -- Omit of Quantitation = 0 .0307 pgfg LO Q -- U m it of Quantitation = 0.0613 pg/g N O TE: Results are expressed as group/gender averages the standard deviation associated with that group/gender. N O TE : T h e results of quality control analyses (curve fit, CCVs, and M S/M S D s) for P F O S E A w ere inconsistent and indicate that data presented for this analyte should b e considered to be qualitative only. Values are presented here in the spirit of full disclosure, but should not be used in any quantitative assessm ent of the data. 3MEnvironmental Laboratory Page 197 3M M edical D epartm ent Study: T6316.1 3M Medical Department Study: T-6316.1 Appendix E: Data Spreadsheets Analytical Report: FACT-TOX-001 L R N -U 2103 Analytical Report: FACT TOX-001 LRN-U2103 3MEnvironmental Laboratory Page 198 3M M edical D epartm ent Study: T6316.1 Covance# 6329-212 PFOS PFOSA Study: Product Number(Test Substance): Matrix: 104 W eek Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol iin Rats T-6316 (ElFOSE-OH) Rat Serum 04/27/98 Lot 215 04/28/98 Lot 215 05/05/98 Lot 215 04/27/98 Lot L-2353 04/30/98 Lot L-2353 Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Intercept: Dates o f Extraction/Analyst: Dates o f Analysis/Analyst: Date o f Data Reduction/Analyst: Sample Data W EEK 4 RAT SERA REWORK FACT-M-3.0 & FACT-M-4.0 reworked using ETS-8-5.1 Chick 080697 and Madeline 041098 MassLynx 2.3 & 3.1 See listing to the right See Attachments See Attachments See Attachments 04/23/98,04/28/98 RWW 04/27/98, 04/28/98, 04/30/98,05/05/98 KJH/HOJ 09/01/00, 12/01/00, 12/04'00, 12/05/00 MMH/KJH Lot 215 Filenames Blks Grp 1 Grp 2 Grp 3 Grp 4 Grp 5 4/23/1998 MS, MSD 4/28/1998 MS, MSD PFOS R0427802-03 & 59-60 R0427813-24 R0505812-23 R0505826-37 R0505840-51 R0428813-24 R0427856-57 R0505852-53 PFOSA R0427802-03, R0430803-04 R0427813-24 R04308I4-25 R0430828-39 R0430842-53 R0427841-47, 52-53 R04278150-51 R0427856-57 R0430856-57 PFOSAA R0427802-03 & 59-60 R 0 4 2 7 8 13-24 R0505812-23 R0505826-37 R0505840-51 R0427827-38 R0427856-57 R0505852-53 ________________________________________________________________________________________________Lot L-23S3 Group Dose Sample 4 Extraction Voi. mL PFOS Std Correction Factor PFOS Purity Correction Factor PFOS Dilution Factor PFOS Cone. ng/mL Filename Concentration of PFOS ug/mL or % Ree Mean PFOS ug/mL RSD Std. Dev. MS/MSD RPD PFOSA Purity Correction Factor Method Blk Matrix Blk QC-250 ppb H 20 Blk-1 H 20 Blk-2 Rat Serum Blk-1 Rat Serum Blk-2 MS 4/23/98 MSD 4/23/98 MS 4/28/98 MSD 4/28/98 1 1 1 1 1 1 1 1 0.9275 0.9275 0.9275 0.9275 NA NA NA NA Unknown Unknown Unknown Unknown NA NA NA NA 1 0.00 RO427802 <LOQ (0.0231 ug/mL) 1 0.680 R0427859 <LOO (0.0231 ug/mL) 1 0.00 RO427803 <LOQ (0.0231 ug/mL) 1 2.48 R0427860 <LOQ (0.0231 ug/mL) 1 240 R0427856 96% 1 233 R0427857 93% 1 161 R0505852 65% 1 457 R0505853 183% * <LOQ <LOQ 95% 124% Unknown NA Unknown Unknown NA Unknown NA 3% NA NA 96% NA Group 1 Control 0.0 mg/kg Group 2 Low Dose 3.0 mg/kg C90719M C90732M C90725M C90753M C90775M C9I135F C91143F C91165F C91169F C9117IF C90789M C908I4M C90817M C90833M C90834M C91I98F C91205F C9I222F C9I230F C91237F 1 0.9275 Unknown 1 26.3 R0427813 1 0.9275 Unknown 1 32.5 R0427814 1 0.9275 Unknown 1 26.3 R0427815 1 0.9275 Unknown 1 80.1 R0427816 1 0.9275 Unknown 1 53.4 R0427817 1 0.9275 Unknown 1 120 R0427820 1 0.9275 Unknown 1 114 R0427821 1 0.9275 Unknown I 135 R0427822 1 0.9275 Unknown 1 133 R0427823 1 0.9275 Unknown 1 127 R0427824 1 0.9275 Unknown 50 32.5 R0505812 1 0.9275 Unknown 50 38.5 R0505813 1 0.9275 Unknown 50 41.3 R0505814 I 0.9275 Unknown 50 47.6 R0505815 1 0.9275 Unknown 50 40.2 R0505816 1 0.9275 Unknown 50 64.9 R0505819 1 0.9275 Unknown 50 78.2 R0505820 1 0.9275 Unknown 50 57.2 R0505821 1 0.9275 Unknown 50 74.7 R0505822 1 0.9275 Unknown 50 76.4 R0505823 0.0244 0.0302 0.0244 0.0743 0.0495 0.111 0.106 0.126 0.123 0.117 1.51 1.78 1.91 2.21 1.87 3.01 3.63 2.65 3.47 3.54 0.0405 0.117 1.86 3.26 53.0 0.0215 7.10 0.00828 13.6 0.252 12.7 0.415 Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown L'nknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Group 3 C90846M 1 0.9275 Unknown 250 84.0 R0505826 19.5 Unknown Mid Dose C90853M 1 0.9275 Unknown 250 102 R0505827 23.6 Unknown 30.0 mg/kg C90866M 1 0.9275 Unknown 250 99.5 R0505828 23.1 Unknown C90890M 1 0.9275 Unknown 250 84.2 R0505829 19.5 9.19 Unknown rorifto!" 0.9275 UrJmcv.r. 259 96.8 P.0595839 22.1 21.6 1.99 1'nknewr. C91251F 1 0.9275 Unknown 250 119 R0505833 27.6 Unknown C91272F 1 0.9275 Unknown 250 145 R0505834 33.7 Unknown C91285F 1 0.9275 Unknown 250 105 R0505835 24.3 Unknown C91287F 1 0.9275 Unknown 250 138 R0505836 31.9 12.8 Unknown C91291F 1 0.9275 L'nknown 250 138 R0505837 32.0 29.9 3.84 Unknown Group 4 C90935M 1 0.9275 Unknown 500 111 R0505840 51.5 L'nknown Mid-High Dose C90939M 1 0.9275 Unknown 500 141 R0505841 65.4 Unknown 100 mg/kg C90942M 1 0.9275 Unknown 500 116 R0505842 53.6 L'nknown C90961M 1 0.9275 Unknown 500 157 R0505843 72.8 14.5 Unknown C90966M 1 0.9275 Unknown 500 126 R0505844 58.4 60.4 8.76 Unknown C91316F 1 0.9275 Unknown 500 126 R0505847 58.6 Unknown C91317F 1 0.9275 Unknown 500 155 R0505848 71.9 Unknown C91333F 1 0.9275 Unknown 500 172 R0505849 79.7 Unknown ' C91345F 1 0.9275 l'n k n o w n 500 200 R0505850 92.8 23.7 Unknown C91350F 1 0.9275 Unknown 500 109 R0505851 50.5 70.7 16.8 Unknown Group 5 High Dose 300 mg^kg C90984M C91005M C91024M C91033M C91037M C91423F C91427F C91430F C91443F C91448F 1 0.9275 1 0.9275 1 0.9275 1 0.9275 1 0.9275 1 0.9275 1 0.9275 1 0.9275 1 0.9275 1 1 0.9275 Unknown Unknown Unknown Unknown L'nknown Unknown Unknown l'n k n o w n Unknown L'nknown 500 1000 1000 500 500 1000 1000 1000 1000 1000 404 R0427827 294 R0428814 293 R0428815 481 R0427830 406 R0427831 330 RO428820 291 R0428821 417 R0428822 451 R0428823 435 R0428824 188 273 272 223 188 306 270 387 419 403 Unknown Unknown Unknown 18.6 Unknown 229 42.5 Unknown Unknown Unknown L'nknown 18.3 Unknown 357 65.2 Unknown PFOS = Perfluorooctanesulfonate * Sample quantitated out o f linear range o f curve. PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonamidoacetate Date Entersd/By: 12/06/00 KJH Date Verified/By: 12/06/00 H O J /04/30/01 LAC Purity Entered/Verified: 12/27/00 LAC PFOSAA 04/27/98 Lot 617 05/05/98 Lot 617 Dilutions 1/1, 11, 1/1 1/1, 1/1,1/1 1/50, 1/10, 1/50 1/250, 1/50, 1/250 1/500, 1/100, 1/500 1/1000, 1/5, 1/500 1/500 1/1, 1/1, 1/1 1/1, 1/1, 1/1 PFOSA Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 l 10 10 10 10 10 10 10 10 10 10 50 50 50 50 59 50 50 50 50 50 100 100 100 100 100 100 100 100 100 100 5 5 5 5 5 5 500 500 5 5 Corrected PFOS LOQ (0.0249 ug/mL) to include std correction factors new LOQ is 0.02? 1 ug/mL. LAC 02/19/01 Analytical Report: FACT-TOX-001 L R N -U 2103 PFOSA Cone. ng/mL 0.00 0.00 0.00 0.00 243 228 295 283 0.00 0.06 0.00 0.59 0.31 0.35 0.83 0.64 0.37 0.21 2.55 2.68 2.97 3.89 3.39 5.39 6.56 7.32 5.26 6.57 14.0 13.4 12.2 13.6 16.6 25.9 34.4 12.3 27.0 27.8 19.2 12.6 12.9 24.2 21.7 23.4 30.0 26.6 22.3 21.8 208 266 208 267 239 476 6.96 12.6 382 233 Filename R0427802 R0430803 R0427803 R0430804 R0427856 R0427857 R0430856 R0430857 R 0 4 2 7 8 13 R0427814 R0427815 R04278I6 R0427817 R0427820 R0427821 R0427822 R0427823 R0427824 R0430814 R0430815 R0430816 R0430817 R0430818 R0430821 R0430822 R0430823 R0430824 R0430825 R0430828 R0430829 R0430830 R0430831 P.013083'' R0430835 R0430836 R0430837 R0430838 R0430839 R0430842 R0430843 R0430844 R0430845 R0430846 R0430849 R0430850 R0430851 R0430852 R0430853 R0427841 R0427842 R0427843 R0427844 R0427845 R0427849 R0427835 R0427836 R0427852 R0427853 Concentration o f PFOSA ug/mL or % Ree <LOQ (0.00249 ug/mL) <LOQ <LOQ (0.00249 ug/mL) <LOQ 97% 91% 118% 113% <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) 0.0255 0 0268 0.0297 0.0389 0.03390 0.0539 0.0656 0.0732 0.0526 0.0657 0.701 0.668 0.611 0.680 0.53'' 1.29 1.72 0.614 1.35 1.39 1.92 1.26 1.29 2.42 2.17 2.34 3.00 2.66 2.23 2.18 1.04 1.33 1.04 1 34 1.20 2.38 3.48 6.29 1.91 117 Mean PFOSA ug/mL <LOQ <LOQ 94% 116% <LOQ <LOQ 0.0310 0.0622 0.698 1.27 1.81 2.48 1.19 3.04 RSD Std. Dev. MS/MSD RPD NA NA 6% 4% NA NA NA NA 17.7 0.00549 14.1 0.00874 11.7 0.0818 31.7 0.404 28.7 0.520 13.8 0.344 12.3 0.147 65.6 2.00 3MEnvironmental Laboratory Page 199 3M M edical D epartm ent Study: T6316.1 Covance# 6329-212 Study: Product Number(Test Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Intercept: Dates o f Extraction/Analyst: Dates o f Analysis/Analyst: Date o f Data Reduction'Analyst: Sample Data WEEK 4 RAT SERA REWORK Group Dose Sample 9 Method Blk Matrix Blk QC-250 ppb Group 1 Control 0.0 mg/kg Group 2 Low Dose 3.0 mg/kg Group 3 Mid Dose 30.0 mg/kg Group 4 Mid-High Dose 100 mg/kg Group 5 High Dose 300 mg/kg H 20 Btk-1 H 20 Blk-2 Rat Serum Blk-1 Rat Serum Blk-2 MS 4/23/98 MSD 4/23/98 MS 4/28/98 MSD 4/28/98 C90719M C90732M C90725M C90753M C90775M C91135F C91143F C91165F C91169F C91171F C90789M C90814M C90817M C90833M C90834M C91198F C91205F C91222F C91230F C91237F C90846M C90853M C90866M C90890M r'o n jo iu C91251F C91272F C91285F C91287F C91291F C90935M C90939M C90942M C90961M C90966M C91316F C91317F C91333F C91345F C91350F C90984M C91005M C91024M C91033M C91037M C91423F C91427F C91430F C91443F C91448F 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N*Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum FACT-M-3.0 & FACT-M-4.0 reworked using ETS-8-5.1 Chick 080697 and Madeline 041098 MassLynx 2.3 & 3.1 See listing to the right See Attachments See Attachments - See Attachments 04/23/98,04/28/98 RWW 04/27/98, 04/28/98,04/30/98, 05/05/98 KJH/HOJ 09/01/00,12/01/00,12/04/00, 12'05/00 MMH/KJH Lot 617 PFOSAA Purity Correction Factor Unknown Unknown Unknown Unknown NA NA NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unkr.c.vn Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown LTnknown Unknown PFOSAA Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 50 50 50 50 50 50 50 50 50 50 250 250 250 250 250 250 250 250 250 250 500 500 500 500 500 500 500 50 500 500 500 500 500 500 500 500 500 500 500 500 PFOSAA Cone. ng/mL 0.00 0.00 0.00 0.00 271 252 143 466 13.7 43.2 37.7 82.4 78.7 44.9 85.7 54.4 57.2 59.7 31.1 42.7 32.1 109 45.0 112 49.3 54.2 37.9 53.9 56.4 45.8 45.3 49.5 67.2 73.9 139 54.4 74.3 121 44.6 44.8 39.0 85.3 55.5 47.5 60.4 64.0 115 51.5 123 137 151 126 75.8 175 168 196 271 115 Filename R0427802 R0427859 R0427803 R0427860 R0427856 R0427857 R0505852 R0505853 R0427813 R0427814 R0427815 R0427816 R0427817 R04279820 R04279821 R04279822 R04279823 R04279824 R0505812 R0505813 R0505814 R05058I5 R0505816 R0505819 R0505820 R0505821 R0505822 R0505823 R0505826 R0505827 R0505828 R0505829 R0505220 R0505833 R0505834 R0505835 R0505836 R0505837 R0505840 R0505841 R0505842 R0505843 R0505844 R0505847 R0505848 R0505849 R0505850 R0505851 R0427827 R0427828 R0427829 R0427830 R0427831 R0427834 R0427835 R0427836 R0427837 R0427838 Concentration of PFOSAA ug/mL or % Ree <LOQ (0.00256 ug/mL) <LOQ (0.00256 ug/mL) <LOQ (0.00256 ug/mL) <LOQ (0.00256 ug/mL) 108% 101% 57% 186% 0.0137 0.0432 0.0377 0.0824 0.0787 0.0449 0.0857 0.0544 0.0572 0.0597 1 55 2.13 1.60 5.46 2.25 5.61 2.47 2.71 1.90 2.70 14 1 11.4 11.3 12.4 15.2 18.5 349 13.6 18.6 30.2 22.3 22.4 19.5 42.6 27.8 23.8 30.2 32.0 57.3 25.8 61.3 68.4 75.6 63.1 37.9 87.5 83.9 97.8 136 57.6 * Mean PFOSAA ug/mL <LOQ <LOQ 104% 122% 0.0511 0.0604 2.60 3.07 12.2 23.1 26.9 33.8 61.2 92.5 RSD Std. Dev. MS/M SDRPD NA NA 7% 106% 56.8 0.0291 25.2 0.0152 62.7 1.63 47.3 1.45 17.4 2.20 38.7 8.95 34.5 9.28 40.1 13.6 23.2 14.2 30.6 28.3 * Sample quantitated out o f linear range of curve. Date Entered/By: Date Verified/By: Purity Entered/Verified: 12/06/00 KJH 12'06/00 HOJ/04/30/01 LAC 12/27/00 LAC Corrected PFOS LOQ (0.0249 ug/mL) to include std correction factors new LOQ is 0.0231 ug/mL. LAC 02/19/01 3MEnvironmental Laboratory Analytical Report: FACT-TOX-001 . LRN-U2103 Page 200 3M M edical D epartm ent Study: T6316.1 Covance# 6329-212 Analytical Report FACT-TOX-001 Study: Product Number(Test Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Intercept: Dates o f Extraction/Analyst: Dates o f Analysis/Analyst: Date o f Data Reduction/Analyst: Sample Data W EEK 4 RAT SERA REWORK 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum FACT-M-3.0 & FACT-M-4.0 reworked using ETS-8-5.1 Chick 080697 and Madeline 041098 MassLynx 2.3 & 3.1 See Attachments See Attachments See Attachments See Attachments 04/23/98, 04/28/98 RWW 04/27/98, 04/28/98, 04/30/98, 05/05/98 KJFLHOJ 09/01/00, 12/01/00,12/04/00, 12/05/00 MMH/KJH Group Dose Method Blk Matrix Blk QC-250 ppb Group 1 Control 0.0 mg/kg Group 2 Low Dose 3.0 mg/kg Group 3 Mid Dose 30.0 mg/kg Group 4 Mid-High Dose 100 mg/kg Group 5 High Dose 300 mg/kg Sample # H 20 Blk-1 H 20 Blk-2 Rat Serum Blk-l Rat Serum Blk-2 MS 4/23/98 MSD 4/23/98 MS 4/28/98 MSD 4/28/98 C90719M C90732M C90725M C90753M C90775M C91135F C91143F C91165F C91169F C91171F C90789M C90814M C90817M C90833M C90834M C91198F C91205F C91222F C9I230F C9I237F C90846M C90853M C90866M C90890M C99891M C91251F C91272F C91285F C91287F C91291F C90935M C90939M C90942M C90961M C90966M C91316F C91317F C91333F C91345F C91350F C90984M C91005M C91024M C91033M C91037M C91423F C91427F C91430F C91443F C91448F- Concentration o f PFOS ug/mL or % Ree <LOQ (0.0231 ug/mL) <LOQ (0.0231 ug/mL) <LOQ (0.0231 ug/mL) <LOQ (0.0231 ug/mL) 96% 93% 65% 183% 0.0244 0.0302 0.0244 0.0743 0.0495 0.111 0.106 0.126 0.123 0.117 1.51 1.78 1.91 2.21 1.87 3.01 3.63 2.65 3.47 3.54 19.5 23.6 23.1 19.5 22.-1 27.6 33.7 24.3 31.9 32.0 51.5 65.4 53.6 72.8 58.4 58.6 71.9 ' 79.7 92.8 50.5 183 273 272 223 188 306 270 387 419 403 * Mean PFOS ug/mL <LOQ <LOQ 95% 124% 0.0405 0.117 1.86 3.26 21.6 29.9 60.4 70.7 229 357 RSD Std. Dev. MS/MSD RPD NA NA 3% 96% 53.0 0.0215 7.10 0.0083 13.6 0.252 12.7 0.415 9 19 1.99 12.8 3.84 14.5 8.8 23.7 16.8 18.6 42.5 18.3 65.2 Concentration o f PFOSA ug/mL or % Ree <LOQ (0.00249 ug/mL) <LOQ <LOQ (0.00249 ug/mL) <LOQ 97% 91% 118% 113% <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) <LOQ (0.00249 ug/mL) 0.0255 0.0268 0.0297 0.0389 0.03390 0.0539 0.0656 0.0732 0.0526 0.0657 0.701 0.668 0.611 0.680 9.232 1.29 1.72 0.614 1.35 1.39 1.92 1.26 1.29 2.42 2.17 2.34 3.00 2.66 2.23 2.18 1.04 1.33 1.04 1.34 1.20 2.38 3.48 6.29 1.91 1.17 Mean PFOSA ug/mL <LOQ <LOQ 94% 116% <LOQ <LOQ 0.0310 0.0622 9.692 1.27 1.81 2.48 1.19 3.04 RSD Std. Dev. MS/MSD RPD NA NA 6% 4% NA NA NA NA 17.7 0.00549 14.1 0.00874 11.7 9.9212 31.7 0.404 28.7 0.520 13.8 0.344 12.3 0.147 65.6 2.00 Concentration o f PFOSAA ug/mL or / Ree <LOQ (0.00256 ug/mL) <LOQ (0.00256 ug/mL) <LOQ (0.00256 ug/mL) <LOQ (0.00256 ug/mL) 108% 101% 57% 186% 0.01372 0.0432 0.0377 0.0824 0.0787 0.0449 0.0857 0.0544 0.0572 0.0597 1.55 2.13 1.60 5.46 2.25 5.61 2.47 2.71 1.90 2.70 14.1 1)4 11.3 12.4 16.2 185 34.9 13.6 18.6 30.2 22.3 22.4 19.5 42.6 27.8 23.8 30.2 * 32.0 57.3 25.8 61.3 68.4 75.6 63.1 37.9 87.5 83.9 97.8 136 57.6 * Sample quantitated out o f linear range o f curve Date Entered/By: Date Verified/ By: Purity E nteredVerified: 12/06/00 KJH 12/06/00 H O J/ 04/30/01. LAC 12/27'00 LAC PFOS = Perfluorooctanesulfonate PFOSA = Perfluorooclanesulfonamide PFOSAA = Perfluorooctanesulfonamidoacetate Mean PFOSAA ug/mL <LOQ <LOQ 104% 122% 0.0511 0.0604 2.60 3.07 13.2 23.1 26.9 33.8 61.2 92.5 RSD Std. Dev. MS/MSD RPD NA NA 7% 106% 56.8 0.0291 25.2 0.0152 62.7 1 63 47.3 1.45 17.4 2.39 38.7 9.0 34.5 9.3 40.1 13.6 23.2 14,2 30.6 28.3 L R N -U 2103 Corrected PFOS LOQ (0.0249 ug/mL) to include std correction factors new LOQ is 0.0231 ug/mL. LAC 02'19 0 1 3MEnvironmental Laboratory Page 201 3M M edical D epartm ent Study: T6316.1 A J U I/llt U 7 J 7 /.l Covante# 6329-212 Study: Product N um ber(Test Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Filename: R -Squared Value: Slope: Y-Intercept: Date o f Extraction/Analyst: Date o f Analysis/Analyst: Date o f Data Reduction/Analyst: Sample Data W EEK 8 RAT SERA REWORK 104 W eek D ietary C arcinogenicity Study with N arrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum FACT-M-3.0 & FACT-M -4.0 reworked using ETS-8-5.1 Madeline 041098 M assLynx 2.3 & 3.1 See listing to the right See Attachments See Attachments See Attachments 05/11/98,05/14/98 RWW/OK 05/13/98, 05/14/98 HOJ/KJH/LAD/JJ 04/10/00,01/03/01 CSH/MMH Filenames Blks Grp 1 Grp 5 MS, MSD PFOS 05/14/98 Lot 215 PFOS R05149802-03 & 86-87 R05149812-23 R 0 5 149826-37 R 0 5 149883-84 Group Dose Method Blk Matrix Blk QC-75 ppb Group 1 Control 0.0 mg/kg Group 5 High Dose 300 mg/kg Sample # H 2 0 Blk-1 H 2 0 Blk-2 R at Serum Blk-1 R at Scrum Blk-2 MS 5/11/98 M SD 5/11/98 C90717M C90718M C90737M C90756M C90769M C91126F C91140F C91145F C91162F C91163F C90971M C90972M C90988M C90996M C91017M C91393F C91394F C91404F C91415F C91438F Extraction Voi. mL l 1 1 1 1 1 1 1 1 1 1 1 1 1 1 l 1 l l 1 1 l l l 1 1 PFOS Std Correction Factor 0.9275 0.9275 0.9275 0.9275 NA NA 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0.9275 0 .9 2 7 5 0.9275 0 .9 2 7 5 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 Date Entered/By: 05/24/00, 01/08/01 CSH/LAC D ate Verified/ By: 12/28/00 HOJ / 01/08/01 KJH / 04/30/01 LAC Purity Entered/Verified: 12/27/00 LAC PFOS Purity Correction Factor Unknown Unknown Unknown Unknown NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown PFOS Dilution Factor l I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 PFOS Coic. ng/mL 0.00 8.35 6.13 0.00 763 916 369 52.0 53.4 87.2 49.5 196 183 176 225 194 73.6 67.1 73.6 70.5 90.3 120 121 114 130 136 Filename R 05149802 R05149886 R 05149803 R 0 5 149887 R 05149883 R 0 5 149884 R05149812 R05149813 R05149814 R05149815 R05149816 R05149819 R05149820 R05149821 R05149822 R05149823 R 05149826 R05149827 R05149828 R05149829 R05149830 R05149833 R05149834 R05149835 R05149836 R05149837 C o n c e n tr a tio n of PFOS ug/mL or % Ree <LOQ (0.00905 ug/ml) <LOQ (0.00905 ug/ml) <LOQ (0.00905 ug/ml) <LOQ (0.00905 ug/ml) 104% 125% 0.0342 0 .0 4 8 2 0.0495 0 .0 8 0 9 0 .0 4 5 9 0.182 0.170 0.163 0.209 0.180 341 311 341 327 419 557 559 530 603 631 Mean RSD PFOSA Purity PFOS ng/mL ** <LOQ Std. Dev. MS/MSD RPD NA C orrection Factor Unknown Unknown Unknown * <LOQ * * 115% NA 18% Unknown NA NA Unknown Unknown 0.0518 33.5 0 .0 1 7 4 Unknown Unknown Unknown Unknown 0.181 9.60 0 .0 1 7 4 Unknown Unknown Unknown Unknown 11.9 348 41.5 Unknown Unknown Unknown Unknown Unknown Unknown 6.96 576 40.1 Unknown Unknown Unknown Unknown PFOS - Perfluorooctanesulfonate PFOSA = Perfluorooctanesulfonamide PFOSAA - Pcrfluorooctanesulfonamidoacetate PFOSA 05/14/98 Lot L-2353 PFOSA R05149802-03 & 86-87 R05149812-23 R05149854-65 R05149883-84 PFOSA Dilution Factor 1 1 l l l 1 1 1 1 1 1 1 1 1 1 1 15 15 15 15 15 15 15 15 15 15 Analytical Report: FACT-TOX-001 PFOSAA 05/14/98 U t 617 L R N -U 2103 PFOSAA R05149802-03 & 86-87 R05149812-23 R05149840-51 Dilutions l / l , 1/1, l / l 1/5000, 1/15, R 05149883-84 1/1. l / l , l / l PFOSA Cone. ng/m L 0.00 0.00 6.32 0.00 75.4 84.6 5.90 5.88 6.12 5.91 0.00 6.49 6.47 5.92 6.00 6.12 76.7 70.4 41.8 88.5 88.4 51.5 113 58.8 55.4 80.2 Filename R 0 5 149802 R05149886 R05149803 R08149887 R05149883 R05149884 R05149812 R05149813 R05149814 R05149815 R05149816 R05149819 R05149820 R 05149821 R05149822 R05149823 R05149854 R05149855 R05149856 R05149857 R05149858 R 05149861 R05149862 R 0 5 149863 R05149864 R05149865 Concentration of PFOSA ug/mL or % Ree <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) 103% 116% <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) 1.15 1.06 0.627 1.33 1.33 0.773 1.69 0.882 0.830 1.20 Mean PFOSA ug/mL <LOQ <LOO 110% <LOO <LOQ 1.10 1.08 C orrected PFOS LOQ (0.00976 ug/mL) to include std correction factors new LOQ is 0.00905 ug/mL. LAC 02/19/01 3MEnvironmental Laboratory Page 202 3M M edical D epartm ent Study: T6316.1 Study: Product Number(Test Substance): Matrix: M eth o d /R e v is io n : Analytical Equipment System Number: Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Intercept: Date o f Extraction/Analyst: Date o f Analysis/Analyst: Date o f Data Reduction/Analyst: S a m p le Data W EEK 8 RAT SERA REW ORK Covance# 6329-212 . 104 W eek Dietary Carcinogenicity Study w ith N arrow Range (98.1%) N -Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum FACT-M-3.0 & FACT-M-4.0 reworked using ETS-8-S. 1 Madeline 041098 MassLynx 2.3 & 3.1 See listing to the right See Attachments See Attachments See Attachments 05/11/98,05/14/98 RWW/OK 05/13/98, 05/14/98 HOJ/KJH/LAD/JJ 04/10/00,01/03/01 CSH/M MH Lot 617 RSD Std. Dev. MS/MSD RPD NA NA 12% NA NA NA NA G roup Dose Method Blk Matrix Blk QC-75 ppb Group 1 Control 0.0m g/kg Sample # H20 Blk-1 H20 Blk-2 R at Serum Blk-1 R at Serum Blk-2 MS 5/11/98 MSD 5/11/98 C907I7M C90718M C90737M C90756M C90769M C91126F C91140F C91145F C91162F C91163F PFOSAA Purity Correction F a c to r Unknown Unknown Unknown Unknown NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown PFOSAA Dilution Factor 1 1 1 1 1 1 1 1 1 l l l l 1 l l PFOSAA Cone ng/m L 0.00 0.00 0.00 0.00 76.9 78.3 18.6 24.3 17.9 30.4 24.2 30.2 55.2 38.1 43.4 49.5 Filenam e R05149802 R 05149886 R 05149803 R05149887 R 0 5 149883 R05149884 R05149812 R05149813 R05149814 R05149815 R05149816 R05149819 R 0 5 149820 R 05149821 R 05149822 R05149823 C o n c e n tra tio n of PFOSAA ug/mL or % Ree <LOQ (0.0100 ug/mL) < L O Q (0.0100 ug/mL) ** <LOQ (0.0100 ug/mL) <LOQ (0.0100 ug/mL) ** 103% ** 104% ** <LOQ (0.0100 ug/mL) 0.0243 <LOQ (0.0100 ug/mL) 0.0304 <LOQ (0.0100 ug/mL) 0.0302 0.0552 0.0381 0.0434 0.0495 Mean PFOSAA ug/m L <LOQ <LOQ 103% 0 .0 1 6 9 0.0433 26.2 0.288 35.4 0.381 Group 5 C90971M Unknown High Dose C90972M Unknown 300 rag/kg C90988M Unknown C90996M Unknown C91017M Unknown C91393F Unknown C91394F Unknown C91404F Unknown C91415F Unknown C91438F Unknown ** Tentative results, CCVs d id not meet criteria. LAC 01/08/01 Date Entered/By: 05/24/00,01/08/01 CSH/LAC Date Verified/ By: 12/28/00 HOJ / 01/08/01 K J H / 04/30/01 LAC Purity Entered/Verified: 12/27/00 LAC 500 500 500 500 500 500 500 500 500 500 151 R 05149840 165 R 05149841 103 R 05149842 126 R 05149843 125 R 05149844 212 R05149847 130 R05149848 157 R 0 5 149849 158 R05149850 152 R5149851 75.3 82.3 51.6 63.2 62.3 106 64.8 78.7 79.1 75.9 67.0 80.9 Corrected PFOS LOQ (0.00976 ug/mL) to include std correction factors new LOQ is 0.00905 ug/mL. LAC 02/19/01 Analytical Report: FACT-TOX-001 L R N -U 2103 RSD Std. Dev. MS/MSD RPD NA NA 2% 57.5 0.00974 22.5 0.00973 17.9 12.0 18.8 15.3 3MEnvironmental Laboratory Page 203 3M M edical D epartm ent Study: T6316.1 A JV iU 1 W U ! 5 y /.J Covance# 6329-212 Study: Product Number(Test Substance): Matrix: M cth o d /R e v is io n : 104 W eek Dietary Carcinogenicity Study with N arrow Range (98.1% ) N-Ethyl Pcrfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum FACT-M-3.0 & FACT'M -4.0 reworked using ETS-8-5.1 Analytical Equipment System Number: Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Intercept: Date o f Extraction/Analyst: Date o f Analysis/Analyst: Date o f Data Reduction/Analyst: Sample Data W EEK 8 RAT SERA REWORK Madeline 041098 MassLynx 2.3 & 3.1 See Attachments See Attachments See Attachments See Attachments 05/11/98,05/14/98 RWW/0K 05/13/98, 05/14/98 HOJ/KJH/LAD/JJ 04/10/00, 01/03/01 CSH/MMH Group Sample # Concentration Dose of PFOS ug/mL or % Ree Method Blk H 20 Blk-1 <LOQ (0.00905 ug/ml) H 2 0 Blk-2 <LOQ (0.00905 ug/m l) Matrix Blk Rat Serum Blk-1 <LOQ (0.00905 ug/ml) Rat Serum Blk-2 <LOQ (0.00905 ug/m l) QC-75 ppb MS 5/11/98 104% MSD 5/11/98 125% Group 1 C90717M 0.0342 C o n tr o l C90718M 0.0482 0.0 mg/kg C90737M 0.0495 C90756M 0.0809 C90769M 0.0459 C91126F 0.182 C91140F 0.170 C9U45F 0.163 C91162F 0209 C91163F 0.180 Group 5 C90971M 341 High Dose C90972M 311 300 mg/kg C90988M 341 C90996M 327 C91017M 419 C91393F 557 C91394F C91404F 559 530 C91415F 603 C91438F 631 Tentative results, CCVs did not m eet criteria. LAC 01/08/01 Date Entered/By: 05/24/00,01/08/01 CSH/LAC Date Verified/By: 12/28/00 HOJ / 01/08/01 KJH / 04/30/01 LAC Purity Entered/Verified: 12/27/00 LAC ** * ** * Mean PFOS u g/m L <LOQ <LOQ 115% 0.0518 0.181 348 576 RSD Std. Dev. MS/MSD RPD NA NA 18% 33.5 0.0174 9.60 0.0174 11.9 41.5 6.96 40.1 Concentration of PFOSA ug/mL or % Ree <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) 103% 116% <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) <LOQ (0.00978 ug/mL) 1.15 1.06 0.63 1.33 1.33 0.773 1.69 0.88 0.83 1.20 Mean PFOSA ug/mL <LOQ <LOQ 110% <LOQ <LOQ 1.10 1.08 RSD Concentration Std. Dev. of PFOSAA MS/MSD RPD ng/mL or % Ree <LOQ (0.0100 ug/mL) NA <LOQ (0.0100 ug/m L) ** <LOQ (0.0100 ug/mL) NA <LOQ (0.0100 ug/mL) * 103% * 12% 104% ** <LOQ (0.0100 ug/mL) 0.0243 <LOQ (0.0100 ug/mL) NA 0.0304 NA <LOQ (0.0100 ug/mL) 0 .0 3 0 2 0 .0 5 5 2 0.0381 NA 0.0434 NA 0.0495 75.3 82.3 51.6 26.2 63.2 0.288 62.3 106 64.8 78.7 35.4 79.1 0.381 75.9 PFOS = Perfluorooctanesulfonate PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonamidoacetate Corrected PFOS LOQ (0.00976 ug/m L) to include std correction factors new LOQ is 0.00905 ug/mL. LAC 02/19/01 Analytical Report: FACT-TOX-001 . LRN-U2103 Mean PFOSAA ug/m L <LOQ <LOQ 103% RSD Std. Dev. MS/MSD RPD NA NA 2% 0.0169 57.53 0.00974 0.0433 22.5 0.00973 17.9 67.0 12.0 18.8 80.9 15.3 3MEnvironmental Laboratory Page 204 3M M edical D epartm ent Study: T6316.1 AMD I ff U9Z597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product N um bettT est Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Intercept: Date o f Extraction/Analyst: Date o f Analysis/Anaiyst: Date o f Data Reduction/Analyst: Sample Data W E E K 14 R A T S E R A R E W O R K 104 W eek Dietary C arcinogenicity Study w ith N arrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats T -6316 (EtFOSE-OH) Rat Serum FACT-M-3.0 & FACT-M-4.0 reworked using ETS-8-5.1 Madeline 041098 M assLynx2.3, 3 .1 ,3 2. 3.3 See listing to the right See Attachments See Attachments See Attachments 05/11/98 RWW/OK 05/14/98, 05/15/98, 05/17/98, 6/05/98 HOJ/KJH 12/01/00, 12/29/00, 01/02/01 MMH/CSH Lot 215 G roup Dose Method Blk Sample # H 2 0 Blk-1 E x tractio n Voi. Ratio 1 PFO S Std C o rrection Factor 0.9275 PFOS Purity Correction Factor Unknown PFOS Dilution Factor 1 PFOS Cone. ng/m L 0.00 Filename 51598004 C o n cen tratio n of PFOS ug/mL o r % Ree <LOQ (0.0230 ug/mL) M ean PFOS ng/m L M atrix Blk QC-75 ppb H 2 0 Blk-2 Rat Serum Blk-1 Rat Serum Blk-2 M S 5/11/98 MSD 5/11/98 1 i ! 1 1 0.9275 0.9275 0.9275 NA NA Unknown Unknown Unknown NA NA l 0.00 51598123 <LOQ (0.0230 ug/m L) <LOQ 1 9.31 51598005 <LOQ (0.0230 ug/m L) l 6.03 51598124 <LOQ (0.0230 ug/m L) <LOQ 1 76.3 R05149883 104% * 1 91.6 R05149884 125% * 115% Group 1 Control O .O m g /k g C90731M C90746M C90748M C90768M C90780M C91129F C91155F C91160F C91174F C91181F 1 0.9275 Unknown 1 90.7 60598020 0.0842 1 0.9275 Unknown 1 952 60598021 0.0883 ! 0.9275 Unknown 1 81.2 60598022 0.0753 1 0.9275 Unknown 1 77.6 60598023 0.0720 1 0.9275 Unknown l 75.5 60598024 0.0700 1 0.9275 Unknown 1 159 60598027 0.148 l 0.9275 Unknown 1 246 60598028 0.228 1 0.9275 Unknown 1 232 60598029 0.215 l 0.9275 Unknown 1 240 60598030 0.223 l 0.9275 Unknown 1 181 60598031 0.168 0.0779 0.196 G roup 2 Low Dose 3.0 mg/kg C90797M C90807M C90818M C90831M C90836M C91192F C91223F C91233F C91241F C91248F 1 0.9275 Unknown 100 59.0 51598046 l 0.9275 Unknown 100 61.3 51598047 1 0.9275 Unknown 100 77.0 51598048 l 0.9275 Unknown 100 70.4 51598049 1 0.9275 Unknown 100 63.0 51598050 l 0.9275 Unknown 100 124 51598054 1 0.9275 Unknown 100 130 51598055 1 0.9275 Unknown 100 165 51598056 I 0.9275 Unknown 100 128 51598057 1 0.9275 Unknown 100 113 51598058 5.48 5.69 7.14 6.53 5.85 11.5 12.0 15.3 11.8 10.5 6.14 12.2 Group 3 Mid Dose 30.0 mg/kg C90843M C90852M C90863M C90877M C90880M C91281F 1 0.9275 Unknown 500 101 51598030 1 0.9275 Unknown 500 137 51598031 1 0.9275 Unknown 500 101 51598032 1 0.9275 Unknown 500 153 51598033 1 0.9275 Unknown 500 145 51598034 1 0.9275 Unknown 500 260 51598038 47.0 63.3 47.0 71.0 67.1 120 59.1 Group 4 Mid-High Dose 100 mg/kg C91288F C91293F C91299F C91304F C90905M C90907M C90917M C90921M C90960M C91329F C91337F C91355F C91370F C91379F 1 0.9275 Unknown 500 158 51598039 1 0.9275 Unknown 500 248 51598040 1 0.9275 Unknown 500 281 51598041 1 0.9275 Unknown 500 174 51598042 0.9275 Unknown 1000 237 51598014 1 0.9275 Unknown 1000 . 191 51598015 1 0.9275 Unknown 1000 233 51598016 1 0.9275 Unknown 1000 177 51598017 1 0.9275 Unknown 1000 197 51598018 1 0.9275 Unknown 1000 242 51598022 1 0.9275 Unknown 1000 304 51598023 1 0.9275 Unknown 1000 289 51598024 1 0.9275 Unknown 1000 339 51598025 1 0.9275 Unknown 1000 268 51598026 73.1 115 130 80.5 220 177 216 164 183 225 282 268 315 248 104 192 268 Extraction V olum e R atio = Initial volum e/final volume. For all samples and standards the initial volume is equal to the final volume for an extraction volum e ratio o f 1. Date Entered/By: 6/19/98 LAC, 12/06/00 KJH. 01/05/01 LAC PFOS = Perfluorooctanesulfonate Date Verified/By: 7/16/98 G M L / 12/07/00 HOJ / 01/08/01 K J H / 04/30/01 LAC PFOSA = Perfluorooctanesulfonamide Purity Entered/Verified: 12/27/00 LAC PFOSAA = Perfluorooctanesulfonamidoacetate Corrected PFOS LOQ (0.0248 ug/mL) to include std correction factors new LOQ is 0.0230 ug/mL. LAC 02/19/01 ** Tentative results, CCVs did n ot m eet criteria. LAC 01/08/01 Filenames Blks Grp 1 Grp 2 Grp 3 Grp 4 MS, MSD PFOS 05/14/98 Lot 215 05/15/98 Lot 215 06/05/98 Lot 215 PFOSA 05/14/98 LotL-2353 05/17/98 LotL-2353 06/05/98 Lot L-2353 PFOSAA 05/14/98 Lot 617 05/15/98 Lot 617 06/05/98 Lot 617 PFOS 51598004-5, 123-124 60598020-31 51598046-58 51598030-42 51598014-26 PFOSA 51798004-5, 97-98 60598020-31 51798016-38 51798043-64 51798069-90 R05149883-84 R05I49883-84 PFOSAA 51598004-5, 123-124 60598020-31 51598103-116 51598084-97 51598065-78 D ilutions 1/1, 1/1, 1/1 1/1, l / l , 1/1 1/100, 1/2, 1/25 1/500, 1/5, 1/100 1/1000, 1/5, 1/250 R05149883-84 l / l , 1/1, 1/1 RSD Std. Dev. MS/MSD RPD NA NA 18% 10.1 0.00791 18.4 0.0361 11.2 0.688 14.9 1.83 19.2 11.3 24 5 25.4 12.8 24.6 12.7 34.0 LotL-2353 PFOSA Purity Correction Factor Unknown Unknown Unknown Unknown NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown PFOSA Dilution F a c to r 1 1 1 1 1 1 1 l 1 l 1 1 l 1 1 1 2 2 2 2 2 2 2 2 2 2 5 5 5 5 5 5 5 5 4 5 5 5 5 5 5 5 5 5 5 5 . PFOSA Cone. n g/m L 6.62 6.71 6.59 6.83 75.4 84.6 7.65 0.00 0.00 ' 7.44 7.30 0.00 0.00 8.00 0.00 7.13 37.0 25.8 29.8 23.4 33.4 46.5 54.0 78.5 53.0 42.6 66.0 124 74.5 128 101 135 168 117 IRQ 160 142 151 162 173 151 274 408 397 285 518 F ilen am e 51798004 51798097 51798005 51798098 R05149883 R05149884 60598020 60598021 60598022 60598023 60598024 60598027 60598028 60598029 60598030 60598031 51798016 51798018 51798020 51798022 51798025 51798030 51798032 51798034 51798036 51798038 51798043 51798045 51798047 51798049 57198051 51798056 51798058 51798060 4170RnA'> 51798064 51798069 51798071 51798073 51798075 57198077 51798082 51798084 51798086 51798088 57198090 Concentration of PFOSA ug/m L o r % Ree <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) 103% 116% <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/m L) <LOQ(0.0978 ug/mL) 0.0740 0.0516 0.0597 0.0468 0.0667 0.0930 0.108 0.157 0.1059 0.0852 0.330 0.621 0.372 0.641 0.505 0.677 0.838 0.584 n oas 0.799 0.708 0.755 0.808 0.866 0.753 1.37 2.04 1.99 1.42 2.59 M ean PFOSA ug/m L <LOQ <LOQ 110% <LOQ <LOQ 0.0598 0.110 0.494 0.769 0.778 1.88 RSD Std. Dev. MS/MSD RPD NA NA 12% NA NA NA NA 18.4 0.0110 25.5 0.0280 28.5 0.141 i i 0.141 7.8 0.0605 26.7 0.503 3MEnvironmental Laboratory Page 205 3M M edical D epartm ent Study: T6316.1 A iV lli 1 ff U 9 3 y / .. Covance# 6329-212 Study: 104 Week Dietary C arcinogenicity Study w ith N arrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats Product Num bcr(Test Substance): T -6316 (EtFOSE-OH) Matrix: R at Serum Method/Revision: FACT-M-3.0 & FACT-M-4.0 reworked using ETS-8-5.1 Analytical Equipment System Number: Madeline 041098 Instrument Software/Version: MassLynx 2.3, 3.1, 3.2, 3.3 Filename: S ee listing to the right R-Squared Value: S ee Attachments Slope: S ee Attachments Y-Intercept: S ee Attachments Date o f Extraction/Analyst: 05/11/98 RW W /OK Date o f A nalysisAnalyst: Date o f Data Reduction/Analyst: Sample Data W E E K 14 R A T SERA REW O RK 05/14/98, 05/15/98, 05/17/98, 6/05/98 HOJ/KJH 12/01/00,12/29/00,01/02/01 MMH/CSH Lot 617 G roup Sample # PFOSAA Purity PFOSAA PFOSAA Filenam e C o n c e n tra tio n Dose Correction Factor Dilntion Factor Cone ng/m L of PFOSAA ug/m L or % Ree Method Blk H 20 Blk-1 H 2 0 Blk-2 Unknown Unknown l l 0.00 51598004 <LOQ (0.0255 ug/mL) 0.00 51598123 <LOQ (0.0255 ug/mL) Matrix Blk Rat Serum Blk-1 Unknown 1 0.00 51598005 <LOQ (0.0255 ug/mL) Rat Serum Blk-2 Unknown 1 0.00 51598124 <LOQ (0.0255 ug/mL) QC-75 ppb MS 5/11/98 MSD 5/11/98 NA NA 1 76.9 R05149883 103% "* 1 78.3 R05149884 104% ** Group 1 C90731M Unknown 1 53.9 60598020 0.0539 Control C90746M Unknown 1 49.6 60598021 0.0496 0.0 mg/kg C90748M Unknown 1 18.5 60598022 <LOQ (0.0255 ug/mL) C90768M Unknown 1 23.6 60598023 <LOQ (0.0255 ug/mL) C90780M Unknown 1 22.9 60598024 <LOQ (0.0255 ug/mL) C91129F Unknown 1 35.5 60598027 0.0355 C91155F Unknown 1 38.0 60598028 0.0380 C91160F Unknown 1 35.9 60598029 0.0359 C91174F Unknown 1 46.9 60598030 0.0469 C91181F Unknown 1 18.4 60598031 <LOQ (0.0255 ug/mL) Group 2 C90797M Unknown 25 65.4 51598103 1.63 Low Dose C90807M Unknown 25 28.5 51598104 0.711 3.0 mg/kg C90818M Unknown 25 69.5 51598105 1.74 C90831M Unknown 25 55.9 51598106 1.40 C90836M Unknown 25 27.1 51598107 0.68 C9II92F Unknown 25 56.6 51598112 1.41 C91223F Unknown 25 108 51598113 2.70 C91233F Unknown 25 99.0 51598114 2.47 C91241F Unknown 25 53.3 51598115 1.33 C91248F Unknown 25 57.6 51598116 1.44 G roup 3 Mid Dose C90843M C90852M Unknown Unknown 100 100 80.5 51598084 149 51598085 8.05 14.9 30.0 mg/kg C90863M Unknown 100 88.4 51598086 8.84 C90877M Unknown 100 246 51598087 24.6 C90880M Unknown 100 126 51598088 12.6 C91281F Unknown 100 106 51598093 10.6 C91288F Unknown 100 142 51598094 14.2 C91293F C91299F Unknown Unknown 100 100 141 51598095 309 51598096 14.1 309 C91304F Unknown 100 121 51598097 12.1 G roup 4 Mid-High Dose C90905M C90907M Unknown Unknown 250 57.7 5 i 598065 250 . 99.1 51598066 14.4 24.8 100 mg/kg C90917M Unknown 250 87.7 51598067 21.9 C90921M C90960M Unknown Unknown 250 250 97.8 51598068 73.5 51598069 24.4 18.4 C91329F Unknown 250 102 51598074 25.4 C91337F Unknown 250 153 51598075 38.1 C91355F C91370F C91379F Unknown Unknown Unknown 250 250 250 124 51598076 158 51598077 141 51598078 31.0 39.4 35.3 Extraction Volume R atio = Initial volume/fnal volume. For all sam ples and standards the initial volum e is equal to the final volum e for an extraction volume ratio o f 1. Date Entered/By: 6/19/98 LAC. 12/06/00 KJH, 01/05/01 LAC Date Verified/ By: 7/16/98 GML / 12/07/00 H0J / 01/08/01 K JH /04/30/01 LAC Purity Entcred/Verified: 12/27/00 LAC M ean PFOSAA ug/m L <LOQ <LOQ 103% 0.0360 0.0363 1.23 1.87 13.8 16.4 20.8 33.8 Corrected PFOS LOQ (0.0248 ug/mL) to include std correction factors new LOQ is 0.0230 ug/mL. LAC 02/19/01 Analytical Report: FACT-TOX-001 . LRN-U2103 RSD Std. Dev. MS/MSD RPD NA NA 2% 40.2 0.0145 20.9 0.00761 41.1 0.506 35.2 0.659 48.1 6.63 50 4 8.26 21.1 4.38 16.9 5.71 3MEnvironmental Laboratory Page 206 3M M edical D epartm ent Study: T6316.1 a m i # i . ix j y ^ y i Covanee# 6329-212 Study: Product N umber(Test Substance): Matrix: M eth o d /R e v is io n : Analytical Equipment System Number: Instrument Software/Version: F il e n a m e : R-Squared Value: Slope: Y-Intercept: Date o f Extraction/Analyst: D ate o f Analysis/Analyst: Date o f Data Reduction/Analyst: Sample Data W E E K 14 R A T S E R A R E W O R K 104 W eek D ietary C arcinogenicity Study w ith Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum FACT-M-3.0 & FACT-M-4.0 reworked using ETS-8-5.1 Madeline 041098 MassLynx 2.3, 3.1 ,3 .2 ,3 3 See Attachments See Attachments See Attachments See Attachments 05/11/98 RWW/OK 05/14/98, 05/15/98, 05/17/98, 6/05/98 HOJ/KJH 12/01/00, 12/29/00, 01/02/01 MMH/CSH Group Dose M ethod Blk M atrix Blk QC-75 ppb Sample # H 20 Blk-1 H 20 Blk-2 Rat Scrum Blk-1 Rat Serum Blk-2 MS 5/11/98 MSD 5/11/98 Concentration of PFOS ug/mL or % Ree <LOQ (0.0230 ug/mL) <LOQ (0.0230 ug/mL) <LOQ (0.0230 ug/mL) <LOQ (0.0230 ug/mL) 104% 125% * * Mean PFOS ug/mL <LOQ <LOQ 115% RSD Std. Dev. MS/M SD RPD NA NA 18% Concentration of PFOSA ug/mL or % Rec <LOQ(0 0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) 103% 116% Mean PFOSA ug/mL <LOQ <LOQ 110% RSD Std. Dev. MS/MSD RPD NA NA 12% Group 1 Control 0.0 mg/kg Group 2 Low Dose 3.0 mg/kg Group 3 Mid Dose 30.0 mg/kg C90731M C90746M C90748M C90768M C90780M C91129F C91155F C91160F C9U74F C91181F C90797M C90807M C90818M C90831M C90836M C91192F C91223F C91233F C9124IF C91248F C90843M C90852M C90863M C90877M C90880M C91281F C91288F C91293F C91299F C91304F 0.0842 0.0883 0.0753 0.0720 0.0700 0.148 0.228 0.215 0.223 0.168 5.48 5.69 7.14 6.53 5.85 11.5 12.0 15.3 11.8 10.5 47.0 63.3 47.0 71.0 67.1 120 73.1 115 130 80.5 0.0779 0.196 6. 14 12.24 59.1 104 10.1 0.00791 18.4 0.0361 11.2 0.688 14.9 1 83 19.2 11.3 2 4 .5 2 5 .4 <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) <LOQ(0.0978 ug/mL) 0 .0 7 4 0 0 .0 5 1 6 0 .0 5 9 7 0 .0 4 6 8 0 .0 6 6 7 0 .0 9 3 0 0.108 0.157 0 106 0 .0 8 5 2 0.330 0.621 0.372 0.641 0.505 0.677 0.838 0.584 0 945 0.799 <LOQ <LOQ 0.0598 0.110 0.494 0.769 NA NA NA NA 18.4 0.0110 2 5 .5 0.0280 28.5 0.141 18 3 0.141 Group 4 C90905M 220 0.708 M id-High Dose C90907M 177 0.755 100 mg/kg C90917M 216 0.808 C90921M 164 12.8 0.866 C90960M 183 192 ' 24.6 0.753 0.778 C91329F 225 1.37 C91337F 282 2.04 C91355F C91370F C91379F 268 315 248 1.99 12.7 1.42 268 34.0 2.59 1.88 E xtraction Volume Ratio = Initial volume/fmal volume. For all samples and standards the initial volume is equal to the final volum e for an extraction volum e ratio o f 1. Date Entered/By: 6/19/98 LAC, 12/06/00 KJH, 01/05/01 LAC PFOS = Perfluorooctanesulfonate Date Verified/By: 7/16/98 G M L / 12/07/00 H O J/ 01/08/01 K J H /04/30/01 LAC PFOSA = Perfluorooctanesulfonamidc Purity Entered/Verified: 12/27/00 LAC PFOSAA = Perfluorooctanesulfonamidoacetate 7.78 0.0605 2 6 .7 0.503 Concentration of PFOSAA ug/mL or % Rec <LOQ (0.0255 ug/mL) <LOQ (0.0255 ug/mL) <LOQ (0.0255 ug/mL) <LOQ (0.0255 ug/mL) 103% 104% 0.0539 0.0496 <LOQ (0.0255 ug/mL) <LOQ (0.0255 ug/mL) <LOQ (0.0255 ug/mL) 0.0355 0.0380 0.0359 0.0469 <LOQ (0.0255 ug/mL) 1.63 0.711 1.74 1.40 0.68 1.41 2.70 2.47 1 33 1.44 8.05 14.9 8.84 24.6 12.6 10.6 14.2 14.1 30 9 12.1 14.4 2 4 .8 2 1 .9 24.4 18.4 2 5 .4 38.1 31.0 39.4 35.3 ** ** C orrected PFOS LOQ (0.0248 ug/mL) to include std correction factors new LOQ is 0.0230 ug/mL. LAC 02/19/01 ** Tentative results. CCV s did not m eet criteria. LAC 01/08/01 Mean PFOSAA ug/mL <LOQ <LOQ 103% 0.0360 0 .0 3 6 3 1.23 1.87 13.8 16.4 20.8 33.8 Analytical Report: FACT-TOX-001 L R N -U 2103 RSD Std. Dev. MS/MSD RPD NA NA 2% 40.2 0.0145 20.9 0.00761 41.1 0.506 35.2 0.659 48.1 6 .63 so a 8.26 21.1 4 .38 16.9 5.71 3MEnvironmental Laboratory Page 207 3M M edical D epartm ent Study: T6316.1 Covance# 6329-212 Study: Product Number(Tesl Substance): Matrix: Method/Revision: 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (ElFOSE-OH) Rat Serum ETS-8-4.1 & ETS-8-5.1 Analytical Equipment System Numbe Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Intercepl: Dates of Extraction/Analyst: Davey 070799 & Ruby 100699 Masstynx 3.3 &3.4 See Below See Attachments See Attachments See Attachments 02/23/00,03(78/00 SAL Dates o f Analysis'Analyst: 03/07'00, 0327.00, 03/28/00.04 03 00,04/0$ 00,04/06 00, 5 17 00, 07/1900, 08/17/00 IAS/HOJ/MMH/CSH Date o f Data Reduction/Analyst: 03 `09'00,04 03 00, 04 04 00, 04'05'00,04/07'00,04/10'OO, 518 00, 07/25.00,08/18/00 1AS/HOJ/MMH Sample D ata Bex 00-021 WEEK 27 RAT SERA lot 171 _____ _______________________________________ Deac Sample # Extraction VoL Surrogate Verified PFOS Std Correction Fa c to r PFOS Purity Correction Fa c to r PFOS Dlhiban Fader PFOS Com. ng/mL Filename Concentration PFOS ng/mL or % Ree Method Blk Matrix Blk Matrix Blk QC-250 ng/mL RBS02230-H20 B!k-5 RBS02230-H2O Blk-6 RBS02230-Sera Blk-5 RBS02230-Sera Blk-6 RTS02230-Sera Blk-5 RTS02230-Sera Blk-6 RTS02230-MS-5-1 RTS02230-MS-5-1 RTS02230-MS-5-2 RTS02230-MS-5-2 1 t 1 1 1 1 1 1 1 1 NA 0.9275 0.8640 l 0.00 R032700006 <LOQ (0.00394 ug/mL) NA 0.9275 0.8640 l 0.00 D040300006 <LO0 (0.00781 ug/mL) NA 0.9275 0.8640 1 1.11 R032700007 <LOQ (0.00394 ug/mL) NA 0.9275 0.8640 t 0.00 D040300007 <LOQ (0.00781 ug/mL) NA 0.927 0.8640 1 1.28 R032700008 <LOQ (0.00394 ug/mL) NA 0.9275 0.8640 1 0.00 D040300008 <LOO (0.00781 ug/mL) NA NA NA 1 268 R032700020 109% NA NA NA NA NA NA NA NA NA NA 1 216 R032700021 88% NA NA NA NA NA NA NA RTS02230-MS-5-3 RTS02230-MS-5-3 1 NA NA 1 NA NA NA 1 166 R032700022 NA 1 154 R032800020 67% 62% RTS02230-MS-5-4 RTS02230-MS-5-4 1 NA NA 1 NA NA NA 1 184 R032700023 NA NA NA NA 74% NA Group 1 C90721M 1 NA 0.9275 0.8640 1 37.2 R032700027 0.0298 Control 0.0 mg/tg C90735M C90736M 1 NA 0.9275 0.8640 1 49.2 R032700028 0.0394 1 NA 0.9275 0.8640 1 44.6 R032700029 0.0357 C90738M C90739M C90747M C907S1M C90752M C90755M C90766M C9I127F C9I128F C9I133F C91137F C9I144F C9I13F C9I154F C9I158F C9I16IF C9I183F 1 NA 0.9275 0.8640 1 40.0 R032700030 0.0320 1 NA 0.9275 0.8640 1 68.5 R032700031 0.0549 1 NA 0.9275 0.8640 1 72.6 R032700035 0.0582 1 NA 0.9275 0.8640 1 55.9 R032700036 0.0448 1 NA 0.9275 0.8640 1 57.6 RH32700037 0.0462 1 NA 0.9275 0.8640 1 50.3 R032700038 0.0403 1 NA 0.9275 0.8640 1 42.2 R032700039 0.0338 1 NA 0.9275 0.8640 1 113 R032700043 0.0908 1 NA 0.9275 0.8640 1 142 R032700044 0.114 1 NA 0.9275 0.8640 1 120 R032700045 0.0966 1 NA 0.9275 0.8640 1 99.7 R032700046 0.0799 1 NA 0.9275 0.8640 1 79.4 R032700047 0.0636 1 NA 0.9275 0.8640 1 98.1 R032700051 0.0786 1 NA 0.9275 0.8640 1 88.1 R032700052 0.0706 1 NA 0.9275 0.8640 1 87.9 R032700053 0.0705 1 NA 0.9275 0.8640 1 68.3 R0327000S4 0.0547 1 NA 0.9275 0.8640 1 92.4 R032700055 0.0740 Group 2 Low Dose 3.0 mg/kg C90795M C90799M C90802M C9O803M C90805M C90806M C90824M C90825M C90839M C90840M C91196F C91207F C912I0F C912I1F C912I4F C91221F C91224F C91235F C91243F C91244F 1 NA 0.9275 0.8640 10 274 R032800052 1 NA 0.9275 0.8640 10 380 R032800053 1 NA 0.9275 0.8640 10 165 R032800054 1 NA 0.9275 0.8640 10 500 R032800055 1 NA 0.9275 0.8640 10 211 R032800056 1 NA 0.9275 0.8640 10 408 R032800059 1 NA 0.9275 0.8640 10 279 R032800060 l NA 0 9275 0 8640 to 366 R03280006! 1 NA 0.9275 0.8640 10 343 R032800062 1 NA 0.9275 0.8640 10 505 R032800063 1 NA 0.9275 0.8640 10 442 R032800066 1 NA 0.9275 0.8640 10 677 R032800067 1 NA 0.9275 0.3640 10 528 R032800068 1 NA 0.9275 0.8640 10 430 R032800069 1 NA 0.9275 0.8640 10 554 R032800070 1 NA 0.9275 0.8640 10 600 R032800073 1 NA 0.9275 0.8640 10 704 R032800074 1 NA 0.9275 0.8640 10 722 R032800075 1 NA 0.9275 0.8640 10 603 R032800076 1 NA 0.9275 0.8640 10 787 R032800077 2.19 3.05 1.32 4.01 1.69 3.27 2.23 2.93 2.75 4.05 3.54 5.42 4.23 3.44 4.44 4.81 5.64 5.78 4.83 6.31 PFOS = Periluorooctanesulfonate Corrected PFOS LOQs (0 00492 & 0.00974 ug/mL) to include sld correction factors PFOSA " Peefluorooctanesulfonamide new LOQs are 0 00394 A.0.00781 ug'mL LAC02/19'01 PFOSAA - Perfluorooctanesulfonamidoacetate EtFOSE - Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 - C8F17S02N((H)CH2C00) PFOSEA - Perfuorooclane sulfonyl elhylamide 2nd PFOS <LOQ <LOQ <LOQ 98% 68% 0.0415 0.0793 2.75 4.85 Dale Entered'By: Dale Verified/ By: Purity Entered/Verified: 04/11 00.04 12 00, 04/17'00, 5/4/00, 523 00,08/15 00,0901 00 CSHLAC 43/01 mmh 0222/01 KJH 04 30/01 LAC 02 1901 LAC RSD Std. Dev. M&/MSD RPD NA NA NA 21% 10% 22.9 0.00951 21.7 0.0172 33.0 0.906 19.7 0.954 Analytical Report: FACT-TOX-001 L R N -U 2103 lotL-15709 PFOSA Purity Correction F a c to r Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown I tnlrnown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown t InVnown Unknown I Tnlrnnwn t Tnknown TtnVrmwn Unknown tr-t. Unknown Unknown Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOSA Dilutlen Factor 1 1 1 1 1 1 1 NA 1 NA 1 NA 1 NA 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 ! 1 1 PFOSA Co m . 0.00 0.00 0.00 0.00 0.00 0.00 259 NA 242 NA 181 NA 202 NA 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 12.5 17.4 5.53 20.4 12.6 14.5 15.8 17.6 11.9 48.5 34.0 35.1 37.9 23.4 29.0 29.8 35.8 4 43.8 39 6 Filename R032700006 D040300006 R032700007 D040300007 R032700008 D040300008 R032700020 NA R032700021 NA R032700022 NA R032700023 NA R032700027 R032700028 R032700029 R032700030 R032700031 R032700035 R032700036 R032700037 R032700038 R032700039 R032700043 R032700044 R032700045 R032700046 R032700047 R032700051 R032700052 R032700053 R032700054 R032700055 RQ32700059 R032700060 R032700061 R032700062 R032700063 R032700067 R032700068 R032700069 R032700070 R032700071 R032700075 R032700076 R032700077 R032700078 R032700079 R032700083 R032700084 onv57rwiac R032700086 Rn327000R7 Concentration of PFOSA ug/mL or % Ree <LOQ (0.00493 ug/mL) "LOO (0.00493 ug'mL) <LOQ (0.00493 ug/mL) <LO0 (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOO (0.00493 ug/mL) 104% NA 98% NA 73% NA 81% NA <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ug/tnL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOO (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) 0.0125 0.0174 0.00553 0.0204 0.0126 0.0145 0.0158 0.0176 0.0119 0.0485 0.0340 0.0351 0.0379 0.0234 0.0290 0.0298 0.0358 nm sj 0.0438 0 0396 PFOSA ug/mL <LOO <LOQ <LOQ 101% 77% <LOO <LOQ 0.0177 n ort7 RSD Std. Dev. MS/MSD RPD NA NA NA 7% 11% NA NA NA NA 0.0116 0.00608 3MEnvironmental Laboratory Page 208 3M M edical D epartm ent Study: T6316.1 Covance# 6329-212 Study: Product NumbeifTest Substance): Matrix: Method/Revision: Analytical Equipment System Number Instrument Software-Version Filename: R-Squared Value: Slope: Y-Intereept Dates of Extraction/Analyst: Dates of Analysis'1Analyse Date o f Data Reduction/Analyst Sample Data WEEK 27 R A T SERA G re tt p Dote Sample # Method Blk Matrix Blk Matrix Blk QC-250 ng/mL Group 1 Control 0.0 mg/kg Group 2 Low Close 3.0 mg/kg RBS02230-H20 Blk-5 RBS02230-H20 Blk-6 RBS02230-Sera Blk-5 RBS02230-Scra Blk-6 RTS02230-Sere Blk-5 RTS02230-Sera Blk-6 RTS02230-MS-5-1 RTS02230-MS--1 RTS02230-MS-5-2 RTS02230-MS-5-2 RTS02230-MS-5-3 RTS02230-MS-5-3 RTS02230-MS-5-4 RTS02230-MS-5-4 C9072IM C90735M C90736M C90738M C90739M C90747M C9075IM C90752M C90755M C90766M C91127F C91128F C91133F C9I137F C91144F . C91153F C91154F C91158F C91161F C91183F C90795M C90799M C90802M C90803M C90805M C908U6M C90824M C90825M C90839M C90840M C91196F C9I207F C9I2I0F C9I211F C9I2I4F C9I221F C9I224F C91235F C91243F C9I244F 104 Week Dietary Carcinogenicity Study with Narrow Range (981%) N-Ethyl Perfluorooclanesulfonamido Ethanol in Rats T-6316 (EtfOSE-OH) Rat Serum ETS-8-4.1 &ETS-8-5.I Davey 070799 & Ruby 100699 Masslynx 3.3 & 3.4 See Below See Attachments See Attachments See Attachments 02-73'00,03,78/00 SAL 03/07/00, 0377 00, 0378/00,04/03/00, 04/05/00, 04/06/00, 5'17'00,07/19/00, 08/17/00 IASHOJ/MMH/CSH 0309'00, 04/03/00, 04/04 00, 04/05/00, 04/07 00, 04/10/00, 5/18/00,0775/00, 08/18/00 1ASHOJ/MMH Box 00-021 lotT-712l.l PFOSAA Purity Correction Factor Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOSAA Dilution F a c to r 1 1 1 1 1 1 NA 1 NA 1 NA 1 NA 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 10 1 1 1 1 10 1 1 1 PFOSAA Cone. ng/mL 0.00 0.00 0.00 0.00 0.00 0.00 321 NA 304 NA 241 NA 285 NA 0.00 0.00 0.50 0.28 0.00 2.10 4.49 0.00 3.04 0.47 0.00 8.07 0.00 0.05 0.00 0.00 0.00 0.00 0.00 0.00 270 455 237 713 356 369 410 646 512 180 578 641 663 699 165 684 685 655 702 766 Filennme R032700006 D040300006 R032700007 D040300007 R032700008 D040300008 R032700020 NA R032700021 NA R032700022 NA R032700023 NA R051700019 R051700020 R051700021 R051700022 R051700023 R05I700028 R051700029 R051700030 R051700031 R051700032 R051700037 R051700038 R051700039 R051700040 R051700041 R051700046 R051700047 R051700048 R051700049 R05170000 R032700059 R032700060 R032700061 R032700062 R032700063 R032700067 R032700068 R032700069 R032700070 R032800063 R032700075 R0327OOO76 R032700077 R032700078 R032800070 R032700083 D040600064 R032700085 R032700086 D040600067 C e uee nt ra ti on of PFOSAA ug/mL or % Ree <LOQ (0.0493 ug/mL) <LOO (0.0248 ug/mL) <LOQ (0.0493 ug/mL) <LOO (0.0248 ue/mLl <LOQ (0.0493 ug/mL) <LOO (0.0248 ug/mL) 129% NA 12254 NA 9754 NA 11554 NA <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) 0.270 0.455 0.237 0.713 0.356 0.369 0.410 0 646 0.512 1.80 0.578 0.641 0.663 0.699 1.65 0.684 0.685 0.655 0.702 0.766 PFOSAA ug/mL <LOQ <LOQ <LOO 12654 10654 <LOQ <LOQ 0.577 0.772 PFOSA = Perfluorooctancsulfonamide PFOSAA = Perfiuorooctanesulfonamidoacclatc EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2CCX)) PFOSEA - Perfuorooctane sulfonyl elhylanride w LOQs are 0.00394 & 0.00781 ug/mL LAC02/19/01 Date Enlered/By: Date Verified' By: Purity EnleredVerified: 04/11 00, 04/17'00, 04/17/00, 5/4/00, 5/23 00.08 15 00, 09 01 00 CSHLAC 4/3/01 mmh 02 22'01 K JH '0470/01 LAC 02/19/01 LAC RSD Std. Dev. MS/MSD RPD NA NA NA 654 1754 NA NA NA NA 78.9 0.455 40.3 0.311 lot Unknown/SDOI3 EtFOSE-OH Purity C e r re c tl n n F a c to r Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Analytical Report: FACT-TOX-001 L R N -U 2103 EtFOSE-OH Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 EtFOSE-OH Cone. 0.00 0.00 0.00 0.00 0.00 0.00 43.9 123 82.4 77.2 64.4 80.4 56.8 71.7 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 non 0.00 0.00 Filename R032700006 A081700017 R032700007 A0817000I8 R032700008 A081700019 R032700020 R032800018 R032700021 R032800019 R032700022 R032800020 R032700023 R03280002I R032700027 R032700028 R032700029 R032700030 R032700031 R032700035 R032700036 R032700037 R032700038 R032700039 R032700043 R032700044 R032700045 R032700046 R032700047 R032700051 R032700052 R032700053 R032700054 R032700055 D040600043 D040600042 D040600044 D040600045 D040600046 DO40600049 D040600050 1X140600051 D040600052 DO40600053 D040600056 D040600057 DO40600058 D040600059 D040600060 D040600063 D040600064 0040600064 D040600066 D040600067 Cencentratlen of EtFOSE-OH ug/mL or % Ree <LOQ (0.00977 ug/mL) ''LOO (0.00977 ue'mLi <LOQ (0.00977 ug/mL) <LOO (0.00977 ug/mLl <LOQ (0.00977 ug/mL) <LOO (0.00977 ug/mL) 1854 5054 3354 31% 2654 32% 2354 2954 <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOO (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOO 0.0248 ug/mL) 'L O Q (0.0248 ug'mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug'mL) <LOQ (0.0248 ugmL) <i r tn /n m is ,,,,-mi i <LOQ (0.0248 ug'mL) <LOQ (0 0248 ug/ml.) 2nd 2nd 2nd 2nd EtFOSE-OH 'LOO <LOQ <LOQ 25% 27% <LOQ <LOQ <LOQ <LOQ RSD Std. Dev. MS/MSD RPD NA NA NA 46% 11% NA NA NA NA NA NA NA 3MEnvironmental Laboratory Page 209 3M M edical D epartm ent Study: T6316.1 /VIVILI 1 f U V Z 3V /.1 Covance# 6329-212 Study: 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats Product NumbcrfTest Substance): T-6316 (EtFOSE*OH) Matrix: Rat Serum Mediod/Revision: ETS-8-4.1 & ETS-8-5.1 Analytical Equipment System Number Davey 070799 & Ruby 100699 Instrument Software/Version Masslynx 3.3 & 3.4 Filename: See Below R-Squared Value: See Attachments Slope: See Attachments Y-Intereepl: See Attachments Dates of Extraction/Analyst: Dates of Analysis'Analyst 02/23/00,03/28/00 SAL 03/07/00, 03/27/00.03'28 '00, 04 03'00, 04.05/00, 04/06/00, 5-17/00,07 19/00,08/17/00 lAS'HOJ/MMH/CSH Dale o f Data Reduction''Analyst: 03:09/00, 04.03/00,04 '04.00, 04/05 00, 04/07/00, 04 10 '00, S'18/00,07:25/00,08/18/00 IAS/HOJ/MMH Sample Data Box 00-021 W EEK 27 RAT SERA lolN BI 13047-80 G roup Dose Sample # M556 Purity Correction Verified M556 Dilution MS56 Cone. Filename Concentra tien of M556 Factor Factor ng/mL ug/oL or % Ree Method Btk RBSO2230-H2O Blk-5 Unknown NA 1 0.00 R032700006 <LOQ (0.00492 ug'mL) RBS02230-H20 Blk-6 Unknown NA 1 0.00 D040300006 <LOQ (0.0248 ua/mL) Matrix Blk RBS02230-Sere Blk-5 Unknown NA 1 0.00 R032700007 <LOQ (0.00492 ug/rnLl RBS02230-Sere Blk-6 Unknown NA 1 0.00 D040300007 <LOQ (0.0248 ua/mL) Matrix Blk RTS02230-Sere Blk-5 Unknown NA 1 0.00 R032700008 <LOQ (0.00492 ug/mLI RTS02230-Sere Blk-6 Unknown NA 1 0.00 D040300008 <LOQ (0.0248 ua/mL) QC-250 ng/mL RTS02230-MS-5-1 NA NA 1 375 R032700020 151% RTS02230-MS-5-I NA NA 1 272 R0328000I8 110% 2nd RTS02230-MS-5-2 NA NA 1 372 R032700021 150% RTS02230-MS-5-2 NA NA 1 262 R0328000I9 106% 2nd RTS02230-MS-5-3 NA NA 1 323 R032700022 130% RTS02230-MS-5-3 NA NA 1 222 R032800020 89% 2nd RTS02230-MS-5-4 NA NA 1 350 R032700023 141% RTS02230-MS-5-4 NA NA 1 243 R03280002I 98% 2nd Greap 1 Control 0.0 mg/kg C9072IM C90735M C90736M C90738M C90739M C90747M C9075IM C90752M C90755M C90766M C91127F C9I128F C9I133F C9I137F C9I144F C91153F C91154F C91158F C91I61F C91I83F Unknown NA 1 15.9 D071900018 <LOQ (0.0248 ug/mL) Unknown NA 1 0.00 D071900019 <LOQ (0.0248 ug/mL) Unknown NA 1 0.00 D07|900020 <LOQ (0.0248 ug/mL) Unknown NA 1 0.00 D071900024 <LOQ (0.0248 ug/mL) Unknown NA 1 0.00 R051700023 <LOQ (0.0248 ug/mL) Unknown NA 1 7.34 R051700028 <LOQ (0.0248 ug/mL) Unknown NA 1 0.330 R051700029 <LOQ (0.0248 ug/mL) Unknown NA 1 0.00 R051700030 <LOQ (0.0248 ug/mL) Unknown NA 1 0.00 R051700031 <LOQ (0.0248 ug/mL) Unknown NA 0.00 R0S1700032 <100(0.0248 oe/mLi Unknown NA 1 0.0900 R051700037 <LOQ (0.0248 ug/mL) Unknown NA 1 0.00 R051700038 <LOQ (0.0248 ug/mL) Unknown NA 1 0.00 R051700039 <LOQ (0.0248 ug/mL) Unknown NA I 0.00 R051700040 <LOQ (0.0248 ug/mL) Unknown NA 1 0.00 R051700041 <LOQ (0.0248 ug/mL) Unknown NA 1 2.95 R051700046 <LOQ (0.0248 ug/mL) Unknown NA 1 0.00 R051700047 <LOQ (0.0248 ug/mL) Unknown NA 1 0.00 R051700048 <LOQ (0.0248 ug/mL) Unknown NA 1 0.00 R051700049 <LOQ (0.0248 ug/mL) Unknown NA 1 o.oo ROSI700050 <LOQ (0.0248 ua/mL) Group 2 Low Dose 3 0 mg/kg C90795M C90799M C90802M C90803M C90805M C90806M C90824M C90825M C90839M C90840M C91I96F C91207F C91210F C91211F C91214F C91221F C91224F C91235F C91243F C91244F Unknown NA 1 218 D040500043 0.218 Unknown NA 1 229 D040500042 0.229 Unknown NA 1 202 D040500044 0.202 Unknown NA 1 273 D040500045 0.273 Unknown NA 1 214 D040500046 0.214 Unknown NA 1 213 D040500049 0.213 Unknown NA 1 315 D040500050 0.315 Unknown NA 1 299 D040500051 0299 Unknown NA 1 306 D040500052 0.306 Unknown NA 1 399 D040500053 0.399 Unknown NA 1 245 D040500056 0.245 Unknown NA 1 307 D040500057 0.307 Unknown NA 1 323 D040500058 0.323 Unknown NA 1 223 D040500059 0.223 Unknown NA 1 399 D040500060 0.399 Unknown NA 1 352 D040500063 0.352 Unknown NA 1 243 D040500064 0.243 Unknown NA 1 187 D040500065 0.187 Unknown NA 1 389 D040500066 0.389 Unknown NA 1 363 D040500067 0.363 PFOS - Periluorooctanesulfonati Corrected PFOS LOQs (0.00492 & 0.00974 ug/mL) to include std correction factors FFOSA = Periluorooctanesulfonamide PFQSAA " Periluorooctanesulfoaaxnidoacetate new LOQ .00394 & 0.00781 ug/mL. LACOl'19/01 EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcoli M556 = C8F17S02N((H)CH2C00) PFOSEA - Perfuorooctane sulfonyl ethylamide Dale Entered By: Dale Verified/ By: Purity Entered/Verified: 04,11 00.04 12/00,04 17 00, 5/4/00,5:23/01 0272/01 KJH / 04'30/0l LAC 0719/01 lAC 815 00,09 0100 CSH'LAC 43/01 mmh M556 <LOO <LOQ <LOQ 150% 136% <LOQ <LOQ 0.267 0.303 RSD Std. Dev. MS/MSD RPD NA NA NA 1% 8% NA NA NA NA 23.8 0.0634 246 0.0744 PFOSEA Purity Correction Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOSEA Dilution Factor 1 1 1 1 1 1 1 1 l t l 1 l 1 1 1 1 t 1 1 1 1 1 I I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 t Analytical Report: FACT-TOX-001 L R N -U 2103 PFOSEA Cone. ng/mL 0.00 0.00 0.00 0.00 0.00 0.00 164 265 124 204 91.0 143 116 141 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 000 Filename R032700006 D040300006 R032700007 D040300007 R032700008 D040300008 R032700020 R032800018 R032700021 R032800019 R032700022 R032800020 R032700023 R03280002I R032700027 R032700028 R032700029 R032700030 R032700031 R032700035 R032700036 R032700037 R032700038 R032700039 R032700043 R032700044 R032700045 R032700046 R032700047 R032700051 R032700052 R032700053 R032700054 R032700055 R032700059 R032700060 R032700061 R032700062 R0327OO063 D040600049 D040600050 DO40600051 D040600052 D040600053 D040600056 D040600057 D040600058 D040600059 D040600060 DO40600063 D040600064 rwijnsmu D040600066 D04060006t Concentration of PFOSEA ug/mL or % Ree <LOQ (0-0247 ug/mL) <LOO (0.0248 ug/mL) <LOQ (0.0247 ug/mL) <LOO (0.0248 ug/mL) <LOQ (0.0247 ug/mL) <LOO (0.0248 ue/mL) 67% 107% 50% 83% 37% 58% 47% 57% 2nd 2nd 2nd 2nd <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0 0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOO (0.024? ua/mLi <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug'mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0-0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.00492 ug/mL) <1.00(0 00497 iio/mn --LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOO (0.00492 ua/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) r wm.ll.cn > <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug'mL) PFOSEA <LOO <LOO <LOQ 58% 42% <LOO <LOQ <LOO <LOQ RSD Std. Dev. MS/MSD RPD NA NA NA 28% 24% NA NA NA NA NA NA NA NA 3MEnvironmental Laboratory Page 210 3M M edical D epartm ent Study: T6316.1 A1I1U1It U7AJ7/.1 Covanee# 6329-212 Study: Product Numbei(Test Substance): Matrix: Method Revision: Analytical Equipment System Number Instrument SoftwareVersion: Filename: R-Squared Value: Slope: Y-Intercept: Dates o f Extraction;Analyst: Dates o f Analysis/Analyst Date o f Data Reduction/Analyst: 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%)N-Elhyl Periluorooctaoesulfonamido Ethanol is Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 & ETS-8-5.1 Davey 070799 & Ruby 100699 M a ssly n x 3 .3 & 3 .4 See Attachments See Attachments See Attachments See Attachments 02/23/00,03/28/00 SAL ' 03/07 '00,03/27/00, 03'28 00 ,04 03/00,04/05 00,04/06/00, 5/17/00, 07.19/00,08/17/00 IAS/HOJ/MMH/CSH 03/09/00,04 03/00,04/04/00,04 05 '00,04'07'00,04/10/00, 5/18'0O, 0725/00,08'18/00 IASHOJ/MMH Sam ple D ata W EEK 27 RAT SERA Group Dose Method Blk Matrix Blk Matrix Blk QC-250 ng/mL Sample S RBS02230-H20 Blk-5 RBS02230-H20 Blk-6 RBS02230-Sera Blk-5 RBS02230-Sera Blk-6 RTS02230-Sern Blk-5 RTS02230-Sera Blk-6 RTS02230-MS-5-I RTS02230-MS-5-I RTS02230-MS-5-2 RTS0223O-MS-S-2 RTS0223O-MS-5-3 RTS02230-MS-5-3 RTS02230-MS-5-4 RTS02230-MS-5-4 Concentration Mean of PFOS PFOS ug/mL or % Ree <LOQ (0.00394 ug/mL) <LOO <0.00781 ua/mL) <LOO <LOQ (0.00394 ug/mL) <LOO (0.00781 ue/mL) <LQQ <LOQ (0.00394 ug/mL) -LOQ (0.00781 ugmL) <LOO 109% NA 88% NA 98% 67% 62% 2nd 74% NA 68% RSD Std. Dev. MS/MSD RPD NA NA NA 21% 10% Coocentratlen of PFOSA ug/mL o r % Ree <LOQ (0.00493 ug/mL) <LOQ (0.00493 ua/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ua/mU 104% NA 98% NA 73% NA 81% NA PFOSA <1.00 <LOQ <LOQ 101% 77% RSD Std. Dev. MS/MSD RPD NA NA NA 7% 11% Group 1 Control 0.0 mg/kg C9072IM C90735M C90736M C90738M C90739M C90747M C90751M C90752M C90755M C90766M C9I127F C91128F C91133F C91137F C91144F C91153F C91154F C91158F C91161F C91183F 0.0298 0.0394 0.0357 0.0320 0.0549 0.0582 0.0448 0.0462 0.0403 0.0338 0.0908 0.114 0.097 0.0799 0.0636 0.0786 0.0706 0.0705 0.0547 0.0740 0.0415 . 0.0793 22.9 0.00951 21.7 0.0172 <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) LOO (0.00493 ua/mL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ <L0Q NA NA NA NA Group 2 Low Dose 3.0 mg/kg C90795M C90799M C90802M C90803M C90805M C90806M C90824M C90825M C90839M C90840M C91196F C91207F C912I0F C91211F C912I4F C91221F C91224F C91235F C91243F C91244F 2.19 0.0125 3.05 0.0174 1.32 0.00553 4.01 0.0204 1.69 0.0126 3.27 0.0145 2.23 0.0158 2 93 0.0176 2.75 33.0 0.0119 65.4 4.05 2.75 0.906 0.0485 0.0177 0.0116 3.54 0.0340 5.42 0.0351 4.23 0.0379 3.44 0.0234 4.44 0.0290 4.81 0.0298 5.64 0.0358 5.78 0.0284 4.83 19.7 0.0438 18.0 6.31 4.85 0.954 0.0396 0.0337 0.00603 PFOS = Periluorooctanesulfonale Corrected PFOS LOQs (0 00492 A. 0.00974 ugmL) to include sld correction faclon PFOSA = Periluorooclanesulfonamide new LOQs are 0.00394 &0.00781 ug/mL LAC 02/19/01 PFOSAA - Periluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Periluorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2COO) PFOSEA - Perfuorooctane sulfonyl ethylamide Date EnleredBy: Dale Verified' By: Purity Entered/Verified: 04/11 00,04/12 00,04/17 00,5/4/00,523 00,08 15.00,09/01.00 CSII'LAC 43/01 mmh 02.22 01 KJH/ 0430/01 LAC 02 19 01 LAC Cenrentrattan of PFOSAA ug/mL or % Ree <LOQ (0.0493 ug/mL) <LOO (0.0248 ug'mL) <LOQ (0.0493 ug/mL) <LOQ (0.0248 ua/mL) <LOQ (0.0493 ug/mL) <LOQ (0.0248 ug/mL) 129% NA 122% NA 97% NA 115% NA <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <I.OQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug'mL) <LOQ (0.0248 ug/mL) <I.OQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) -LOQ (0.0248 ug/mL) 0.270 0.455 0.237 0.713 0.356 0.369 0.410 0 646 0.512 1.80 0.578 0.641 0.663 0.699 1.65 0.684 0.685 0.655 0.702 0.766 n # PFOSAA <LOQ <LOQ <LOO 126% 106% <LOQ <LOQ 0.577 0.772 RSD Std. Dev. MS/MSD RPD NA NA NA 6% 17% NA NA NA NA 78.9 0.455 40.3 0.311 Concentration of EtFOSE-OH ug/mL or % Ree <LOQ (0.00977 ug/mL) <LOQ (0.00977 ue/mL) <LOQ (0.00977 ug/mL) <LOO (0.00977 ug/mL) <LOQ (0.00977 ug'mL) <LOO (0.00977 ug'mL) 18% 50% 33% 31% 26% 32% 23% 29% <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug'mL) <LOQ (0.00977 ug'mL) <LOQ (0.00977 ug/mL) <LO0 (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug'mL) <LOQ (0.0248 ug/mL) -LOQ (0 0248 ug'mL) <LOQ (0.0248 ug/mL) <LO0 (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <1 Of) IO0243 up rril ) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) 2nd 2nd 2nd 2nd EtFOSE-OH < 100 <LOO <LOQ 25% 27% <LOO <LOQ <LO0 <I.OQ Analytical Report: FACT-TOX-001 . LRN-U2103 RSD Std. Dev. MS/MSD RPD NA NA NA 46% 11% NA NA NA NA NA NA NA NA Concentration of M556 ug/mL or % Ree <LOQ (0.00492 ug'mL) <LOQ (0.0248 ug'mL) <LOQ (0.00492 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.00492 ugmL) <LO0 (0.0248 ug/mL) 151% 110% 150% 106% 130% 89% 141% 98% <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ugmL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <L 00 (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ugmL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug'mL) 0.218 0.229 0.202 0.273 0.214 0.213 0.315 0.299 0.306 0.399 0.245 0.307 0.323 0.223 0.399 0.352 0.243 n 187 0.389 0 363 2nd 2nd 2nd 2nd MS56 <LOQ <LO0 <LOQ 150% 136% <LOQ <LOQ 0.267 0 303 RSD Std. Dev. MS/MSD RPD NA NA NA 1% 8% NA NA NA NA 23.8 0.0634 24.6 0 0744 Concentration ofPFOSEA PFOSEA ug/raL or % Ree ug/mL <LOQ (0.0247 ug/mL) <LOQ (0.0248 ug'mL) <LOO <LOQ (0.0247 ug/mL) <LOO (0.0248 ug/mL) <LO0 <LOQ (0.0247 ug/mL) <LOQ (0.0248 ug/mL) <LO0 67% 107% 2nd 83% 7nd 58% 2nd 57% <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) -LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) -LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug'mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.00492 ug/mL) <1.00 (0.00492 ue/ml .t '-LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LO0 (0.00492 ug/mLl <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug'mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <L0Q (0.00492 ugmL) ..,,,,,1<L0Q (0.00492 ugmL) WAT. IUUU1 \ <LOQ (0.00492 ugmL) -LOQ (0.00492 ug'mL) 2nd 42% <LOO <LOQ <LOQ -LOQ RSD Std. Dev. MS/MSD RPD NA NA NA 24% NA NA NA NA NA NA 3MEnvironmental Laboratory Page 211 3M M edical D epartm ent Study: T6316.1 m m / 1 ir U 7 J7 / . a Covance# 6329-212 Study: Product Number(Test Substance): M a tr ix : M ethod/R evision: Analytical Equipment System Number: Instrum ent Software/Version: F i le n a m e : R-Squared Value: Slope: Y-Intercept: 104 W eek D ietary C arcinogenicity Study w ith Narrow Range (98.1% ) N-Ethyl Periluorooctanesulfonam ido E thanol in Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 & ETS-8-5.1 Davey 070799 & Ruby 100699 M asslynx 3.3 & 3.4 See Below See Attachments See Attachments See Attachments Dates o f Extraction/Analyst: 02/23/00,03/28/00 SAL Dates o f Analysis/Analyst: 03/07/00, 03/27/00, 03/28/00, 04/03 /0 0 ,0 4 /0 5 /0 0 , 04/06/00, 05/19/00, 0626/00, 07/19/00,08/17/00 IAS/HOJ/M M H/CSH Date o f Data Reduction/Analyst: 03/09/00, 04/03/00, 04/04/00, 04/05 /0 0 ,0 4 /0 7 /0 0 , 04/10/00, 05/23/00, 0627/00, 07/25/00,08/18/00 IAS/HOJ/M M H Sample Data Box 00-021 W EEK 27 RAT SERA________ lot 171 Group Dose Sample # Extraction Voi. Surrogate Verified PFOS Std Correction Factor PFOS Purity Correction Factor PFOS Dilution Factor PFOS Cone. ng/mL Filename Concentration o f PFOS ug/mL or % Ree Group 3 C90847M 1 NA 0.9275 0.8640 100 183 R051900019 14.7 M id Dose 30.0 mg/fcg C90855M C90858M C90859M 1 NA 0.9275 0.8640 100 269 R051900020 21.6 1 NA 0.9275 0.8640 100 268 R051900021 2 1 .4 1 NA 0.9275 0.8640 100 305 R05I900022 24.4 C90864M 1 NA 0.9275 0.8640 100 268 R051900023 21.5 C90865M 1 NA 0.9275 0.8640 100 271 R051900028 21.7 C90871M 1 NA 0.9275 0.8640 100 281 R 051900029 22.5 C90872M 1 NA 0.9275 0.8640 100 235 R 051900030 18.9 C90882M 1 NA 0.9275 0.8640 100 243 R 051900031 19.5 C90886M 1 NA 0.9275 0.8640 100 213 R 051900032 17.0 C91252F 1 NA 0.9275 0.8640 100 629 R 051900037 50.4 C91254F 1 NA 0.9275 0.8640 100 536 R051900038 42.9 C91264F 1 NA 0.9275 0.8640 100 391 R 051900039 31.4 C91267F 1 NA 0.9275 0.8640 100 506 R051900040 40.5 C91283F 1 NA 0.9275 0.8640 100 419 R 051900041 33.5 C91286F 1 NA 0.9275 0.8640 100 587 R 051900046 47.0 C91292F 1 NA 0.9275 0.8640 100 481 R 051900047 38.5 C91295F 1 NA 0.9275 0.8640 100 552 R051900048 44.2 C91301F 1 NA 0.9275 0.8640 100 520 R 051900049 41.7 Group 4 Mid-High Dose C91303F C90916M C90931M 1 NA 0.9275 0.8640 100 329 R 051900050 26 .3 1 NA 0.9275 0.8640 2000 60.7 R 051900055 97.3 1 NA 0.9275 0.8640 2000 42.9 R 051900056 68.7 lO O m g /k g C90937M 1 NA 0.9275 0.8640 2000 50.9 R 051900057 81.6 C90940M C90944M 1 NA 0.9275 0 .8 6 4 0 100 836 R032800027 67.0 . 1 NA 0.9275 0.8640 2000 52.3 R 051900058 83.9 ' C90945M 1 NA 0.9275 0.8640 2000 50.9 R 0 5 1900059 81.5 C90954M 1 NA 0.9275 0 .8 6 4 0 100 874 R032800032 70.0 C90956M 1 NA 0.9275 0 .8 6 4 0 100 624 R032800033 50.0 C90957M 1 NA 0.9275 0 .8 6 4 0 2000 63.3 A 081700023 101 C90963M 1 NA 0.9275 0 .8 6 4 0 100 875 R032800035 70.1 C91312F 1 NA 0.9275 0 .8 6 4 0 2000 122 D 040300020 196 C91323F C91328F 1 NA 0.9275 0 .8 6 4 0 2000 145 D 04030002I 232 1 NA 0.9275 0 .8 6 4 0 2000 84.8 D040300022 136 C91339F 1 NA 0.9275 0 .8 6 4 0 2000 88.5 D 040300023 142 C91340F 1 NA 0.9275 0 .8 6 4 0 2000 73.6 D 040300024 118 C91351F 1 NA 0.9275 0 .8 6 4 0 M00 95.8 D 040300027 154 C91354F 1 NA 0.9275 0 .8 6 4 0 2000 138 D0403Q0028 221 C91357F 1 NA 0.9275 0 .8 6 4 0 2000 119 D040300029 190 C91369F C91371F 1 NA 0.9275 0 .8 6 4 0 2000 99.8 D 040300030 160 1 NA 0.9275 0 .8 6 4 0 2000 91.1 D040300031 146 PFOS = Perf! uorooctanesulfonate PFOSA - Perfluorooctanesulfonam ide Corrected PFOS LO Qs (0.00492 & 0.00974 ug/m L ) to include std correction factors new LOQs are 0.00394 & 0.00781 ug/mL. LAC02/19/01 PFOSAA = Perfluorooctanesulfonam idoacetate EtFOSE * Narrow Range N -Ethyl Perfluorooctanesulfonam ido ethyl alcohol PFOSEA = Perfuorooctane sulfonyl ethylam ide Date Entered/By: D ate V erified/ By: Purity Entered/Verified: 04/11/00, 04/12/00, 04/17/00, 0602/00, 06/07/00, 07/11/00, 08/15/00, 09/01/00 CSH/LAC 02/22/01 K J H / 04/30/01 LAC 02/19/01 LA C PFOS 2 0 .3 39.7 77.2 170 Analytical Report: FACT-TOX-001 L R N -U 2103 RSD Std. Dev. MS/MSD RPD 14.0 2 .85 18.6 7 .39 19.7 15.2 22 .6 38.3 lo tL -1 5 7 0 9 PFOSA Purity Correction Factor Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown 1tnknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOSA Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 ! 1 1 1 1 1 1 1 1 1 1 1 1 1 I 1 1 1 1 1 1 1 l t 1 10 PFOSA Cone. ng/mL 215 302 193 239 236 228 204 247 233 163 441 446 433 516 631 490 557 706 491 365 424 524 382 476 410 269 442 292 554 402 779 863 606 954 7 963 896 558 627 174 Filename A062600016 A062600017 A062600018 A062600019 A062600020 A062600024 A062600025 A062600026 A062600027 A062600028 A062600032 A062600033 A062600034 A062600035 A062600036 A062600040 A062600041 A062600042 A062600043 A062600044 A062600048 A062600049 A062600050 A062600051 A062600052 A062600056 A062600057 A062600058 A062600059 A062600060 A062600064 A062600065 A062600066 A062600067 A O ^A IW l** A062600072 A062600073 A062600074 A062600075 D071900017 Concentration of PFOSA ug/mL or % Ree 0 .2 1 5 0 .3 0 2 0 .1 9 3 0 .2 3 9 0 .2 3 6 0 .2 2 8 0 .2 0 4 0 .2 4 7 0 .2 3 3 0 .1 6 3 0.441 0 .4 4 6 0 .4 3 3 0 .5 1 6 0.631 0 .4 9 0 0 .5 5 7 0.706 0 .4 9 1 0 .3 6 5 0 .4 2 4 0 .5 2 4 0 .3 8 2 0.476 . 0.410 ' 0 .2 6 9 0 .4 4 2 0 .2 9 2 0 .5 5 4 0 .4 0 2 0 .7 7 9 0 .8 6 3 0 .6 0 6 0 .9 5 4 n 7X8 0 .9 6 3 0 .8 9 6 0 .5 5 8 0 .6 2 7 1.74 Mean PFOSA RSD Std. Dev. MS/MSD RPD 0.226 16.3 0.0368 0 .5 0 8 19.9 0.101 0 .4 1 8 2 1 .6 0.0903 0 .8 7 5 38.6 0 .3 3 8 3MEnvironmental Laboratory Page 212 3M M edical D epartm ent Study: T6316.1 A M U T # U9Z597.I Covanee# 6329-212 Study: Product Number(Test Substance): Matrix: M eth o d /R ev isio n : 104 W eek D ietary Carcinogenicity Study with Narrow Range (98.1% ) N-Ethyl Perfluorooctanesulfonam ido E thanol in Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 & ETS-8-5.1 Analytical Equipment System Number: Instrument Software/Version: Filename: Davey 070799 & Ruby 100699 M asslynx 3 3 & 3.4 See Below R-Squared Value: Slope: See Attachments See Attachments Y-Intercept: Dates o f Extraction/Analyst: See Attachments 02/23/00, 03/28/00 SAI. Dates o f Analysis/Analyst: 03/07/00, 03/27/00, 03/28 /0 0 ,0 4 /0 3 /0 0 , 04/0 5 /0 0 ,0 4 /0 6 /0 0,05/19/00, 06/26/00, 07/19/00, 08/17/00 IAS/HOJ/M M H/CSH Date o f Data Reduction/Analyst: 03/09/00, 04/03/00, 04/04/00, 04/05/00, 04/07/00, 0 4 /10/00,05/23/00, 06/27-00, 07/25/00, 08/18/00 IAS/HOJ/M M H Sample Data W EEK 27 RAT SERA Group Dom Sample tt PFOSAA Purity Correction Factor Surrogate Verified PFOSAA Dilution Factor PFOSAA Cone. ug/tnL Filename Concentration o PFOSAA ug/mL or % Ree Mean PFOSAA Group 3 C90847M Unknown N A 10 230 R032800080 2.30 M id Dose 30.0 mg/kg C9085SM C90858M Unknown Unknown N A 10 444 R032800081 4.44 NA 10 204 R032800082 2.04 C90859M Unknown NA 10 256 R032800083 2.56 C90864M Unknown N A 10 247 R032800084 2.47 C90865M Unknown NA 10 212 R032800087 2.12 C90871M Unknown NA 10 194 R032800088 1.94 C90872M Unknown NA 10 153 R032800089 1.53 C90882M Unknown NA 10 188 R032800090 1.88 C90886M Unknown NA 10 139 R032800091 1.39 2 .2 7 C91252F Unknown NA 10 378 R032800094 3.78 C91254F Unknown NA 10 305 R032800095 3.05 C91264F Unknown NA 10 284 R032800096 2.84 C91267F Unknown NA 10 326 R032800097 3.26 C91283F Unknown NA 10 278 R032800Q98 2.78 C91286F Unknown NA 10 606 R032800101 6.06 C91292F Unknown NA 10 293 R032800I02 2.93 C91295F Unknown NA 10 424 R032800I03 4.24 C91301F Unknown NA 10 280 R032800104 2.80 C91303F Unknown NA 10 286 R032800105 2.86 3.46 Group 4 C90916M Unknown NA 100 99.1 R032800024 9.91 M id-High Dose C90931M Unknown NA 100 70.5 R032800025 7.05 100 m g'kg C90937M Unknown NA 100 75.0 R032800026 7.50 C90940M Unknown NA 100 85.6 R032800027 8 56 C90944M Unknown NA 100 67.1 R032800028 6.71 C90945M C90954M Unknown Unknown NA 10 460 R032800045 4.60 NA 10 503 R032800046 5.03 C90956M Unknown N A 10 342 R032800047 3.42 C90957M Unknown N A 10 480 R032800048 4.80 C90963M Unknown NA 100 81.9 R032800035 8 .1 9 6 .5 8 C91312F Unknown N A 100 96.4 D040300034 9.64 C91323F Unknown NA 100 97.7 D040300035 9.77 C91328F C91339F C91340F C91351F Unknown Unknown Unknown Unknown NA 100 63.0 D040300036 6.30 NA 100 86.5 D040300037 8.65 NA 100 53.5 D040300038 5.35 NA 100 82.6 D040300041 8 .2 6 C91354F Unknown NA 100 113 D040300042 11.3 C91357F Unknown NA 100 55.5 D040300043 5.55 C91369F C91371F Unknown Unknown NA 100 5 8 0 D040300044 5.80 N A 100 98.0 D040300045 9.80 8 .0 4 e std correction factors PFOSA = Perfluorooctanesulfonamide w LO Q s are 0.00394 & 0.00781 ug/mL. LA C 02/19/01 PFOSAA = Perfluorooctanesulfonam idoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol PFOSEA = Perfuorooctane sulfonyl ethylam ide D ate Entered/By: D ate V erified/ By: Purity Entered/Verified: 04/11/00, 0 4 /12/00, 04/17/00, 06/02'00, 06/07/00, 07/11/00, 08/15/00, 09/01/00 CSH/LAC 02/22/01 K J H / 04/30/01 LAC 02/19/01 LAC RSD Std. Dev. MS/MSD RPD 37.4 0 .8 4 8 29.9 1.03 31.3 2.06 26.5 2.13 lot Unknown/SD013 EtFOSE-OH Purity Correction Factor Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA . NA EtFOSE-OH Dilution Factor 1 1 1 1 1 1 1 1 1 1 I 1 1 1 1 1 1 1 1 I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 Analytical Report: FACT-TOX-001 L R N -U 2103 EtFOSE-OH Cone. ng/mL 0.490 1 .0 0 0.00 0.00 0.00 0.490 0.400 1 .4 6 2.41 0.560 0.00 0.00 0.00 0.00 4.10 0.00 5.02 0.930 0.330 0.00 6.69 6.19 5.90 6.38 9.47 4.20 4.52 6.76 17.4 8.79 8.05 14.7 5.99 13.4 8 89 25.6 11.6 3.93 9.06 18.2 Filename A062600016 A062600017 A062600018 A062600019 A062600020 A062600024 A062600025 A062600026 A062600027 A062600028 A062600032 A062600033 A062600034 A062600035 A062600036 A062600040 A062600041 A062600042 A062600043 A062600044 A062600048 A062600049 A062600050 A062600051 A062600052 A062600056 A062600057 A062600058 A062600059 A062600060 A062600064 A062600065 A062600066 A062600067 A062600072 A062600073 A062600074 A062600075 A062600076 Concentration of EtFOSE-OH ug/mL or % Ree <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/tnL) <LO Q (0.0248 ug/mL) <LO Q (0.0248 ug/mL) <LO Q (0.0248 ug/mL) <LO Q (0.0248 ug/mL) <LO Q (0.0248 ug/mL) <LO Q (0.0248 ug/mL) <LO Q (0.0248 ug/mL) <LOQ (0.0248 ue/mL) <LOQ (0.0248 ug/mL) <LO Q (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LO Q (0.0248 ug/mL) <LO Q (0.0248 ug/mL) <LO Q (0.0248 ug/mL) <LO Q (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LO Q (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LO Q (0.0248 ug/tnL) <LOQ (0.0248 ug/mL) <LO Q (0.0248 ug/mL) <LO Q (0.0248 ug/mL) <LO O (0.0248 utt/mL) <LO Q (0.0248 ug/tnL) <LO Q (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) < in n m rms ..w t 0.0256 <LOQ (0.0248 ug/mL) <LO Q (0.0248 ug/mL) <LO Q (0.0248 ug/mL) <LOQ (0.0248 ug/mL) EtFOSE-OH <LOQ <LOQ <LOQ <LOQ RSD Std. Dev. MS/MSD RPD NA NA NA NA NA NA NA NA 3MEnvironmental Laboratory Page 213 3M M edical D epartm ent Study: T6316.1 A M I# U9Z597.1 Covance# 6329-212 Study: 104 W eek Dietary C arcinogenicity Study w ith Narrow Range (98.1% ) N -E thyl Perfluorooctanesulfonam ido E thanol in Rats Product Number(Test Substance): T-6316 (EtFOSE-OH) Matrix: Rat Serum M ethod/R evision: ETS-8-4.1 & ETS-8-5.1 Analytical Equipment System Number: Davey 070799 & Ruby 100699 Instrument Software/Version: Filename: M asslynx 3.3 & 3.4 See Below R-Squared Value: See Attachments Slope: See Attachments Y-Intercept: See Attachments Dates o f Extraction/Analyst: 02 /2 3 /0 0 ,0 3 /2 8 /0 0 SAL Dates o f Analysis/Analyst: 03/07/00, 03/27/00, 03/28/00, 04/03/00, 04/05/00, 04/06/00, 05/19/00,06/26/00,07/19/00, 08/17/00 IA S/H O J/M M H CSH Date o f Data Reduction/Analyst: 03/09/00, 04/03/00, 04/04/00, 04/05/00, 04/07/00, 04/10/00, 05/23/00,06/27/00,07/25/00, 08/18/00 IAS/HOJ/MMH Sample Data W EEK 27 RAT SERA lot N B 113047-80 Group Sample U M556 Purity Surrogate M556 M556 Filename Concentration Mean Dose Correction Factor Verified Dilution Cone. of MS56 ug/mL or % Ree M556 ug/mL Group 3 M id Dose C90847M C90855M Unknown Unknown NA NA 10 10 207 R051900083 205 R051900084 2.07 2.05 30.0 mg/kg C90858M Unknown NA 10 211 R051900085 2.11 C90859M Unknown NA 10 186 R 051900086 1.86 C90864M Unknown NA 10 182 R051900091 1.82 C90865M Unknown NA 10 251 A 081700024 2.51 C90871M C90872M C90882M C90886M C91252F C91254F Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA 10 10 10 10 10 10 167 R051900093 301 A081700025 149 R051900095 168 R051900100 385 A081700026 340 R051900102 1.67 3.01 1.49 1.68 3.85 3.40 2 .0 3 C91264F Unknown NA 10 331 R051900103 3.31 C91267F Unknown NA 10 480 R05I900104 4 .8 0 C91283F Unknown NA 10 398 R051900105 3 .9 8 C91286F Unknown NA 10 298 RO5I9OO1I0 2 .9 8 C91292F Unknown NA 10 550 R 051900 111 5.50 C91295F Unknown NA 10 432 R0519001I2 4 .3 2 C91301F Unknown NA 10 428 R0519001I3 4 .2 8 C91303F Unknown NA 10 314 R051900118 3.14 3.96 Group 4 C90916M Unknown NA 100 71.8 R051900065 7 .1 8 Mid-High Dose C90931M Unknown NA 100 84.7 R051900066 8 .4 7 100 mg/kg C90937M Unknown NA 100 81.7 R051900067 8 .1 7 C90940M Unknown NA 100 61.8 R051900068 6 .1 8 C90944M Unknown NA 100 69.8 R051900073 6 .9 8 C90945M Unknown NA 100 56.6 R051900074 5.66 C90954M Unknown NA 100 73.8 R051900075 7.38 C90956M Unknown NA 100 58.4 R051900076 5 .8 4 C90957M Unknown NA 100 61.4 R051900077 6 .1 4 C90963M Unknown NA 100 40.9 R051900082 4.09 6.61 C 9I3I2F Unknown NA 100 41.3 D040300034 4.13 C91323F Unknown NA 100 64.0 D040300035 6 .4 0 C91328F Unknown NA 100 44.1 D040300036 4.41 C91339F Unknown NA 100 88.4 DU403U0037 8 .8 4 C91340F Unknown NA 100 51.4 D040300038 5 .1 4 C9135IF Unknown NA 100 74.0 D040300041 7 .4 0 C91354F Unknown NA 100 77 2 D040300042 7.72 C91357F Unknown NA 100 43.6 D040300043 4.36 C91369F Unknown NA 100 49.6 D040300044 4.96 C91371F Unknown NA 100 102 D040300045 10.2 6.36 PFOS = Perfluorooctanesulfonate C orrected PFO S LO Qs (0.00492 & 0.00974 ug/m L) to include std correction factors PFOSA = Perfluorooctanesulfonam ide new LOQs are 0.00394 & 0.00781 ug/m L. L A C 02/19/01 PFOSAA = Perfluorooctanesulfonam idoacetate EtFO SE = Narrow Range N -E thyl Perfluorooctanesulfonam ido ethyl alcohol PFOSEA = Perfuorooctane sulfonyl ethylamide D ate Entered/By: Date Verified/ By: Purity Entered/Verified: 0 4 /11/00, 04/12/00, 04/17/00, 06/02-00, 06/07/00, 07/11/00, 08/15/00, 09/01/00 CSH /LAC 02/22/01 K JH / 04/30/01 LAC 02/19/01 LAC RSD Std. Dev. MS/MSDRPD 22.2 0.449 20.1 0.796 19.7 1.30 33.2 2.11 lot 529 PFOSEA Purity Correction Factor Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOSEA Dilution Factor 1 1 1 1 1 l 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 Analytical Report: FACT-TOX-001 . LRN-U2103 PFOSEA Cone. 0 .0 0 0 .1 5 0 0 .0 0 0 .1 4 0 0 .0 0 0 .0 0 0.00 0.00 0 .0 0 0 .0 0 0 .0 0 0 .0 0 0 .0 0 0 .0 0 0 .6 2 0 0 .0 0 0 .0 0 0 .0 0 0 .0 0 0 .0 0 0 .5 1 0 0 .0 0 0.00 0 .0 0 0 .1 7 0 0.00 0 .0 0 0.00 0 .0 0 0.00 0 .0 0 0 .3 5 0 0 .0 0 0 .4 9 0 n no 0 .0 0 1.65 0 .3 8 0 0.0100 0 .0 0 Filename A062600016 A062600017 A 0626000I8 A 0626000I9 A062600020 A062600024 A062600025 A062600026 A062600027 A062600028 A062600032 A062600033 A062600034 A062600035 A062600036 A062600040 A062600041 A062600042 A062600043 A062600044 A062600048 A062600049 A062600050 A062600051 A062600052 A062600056 A062600057 A062600058 A062600059 A062600060 A062600064 A062600065 A062600066 A062600067 Anfi^finooftS A062600072 A062600073 A062600074 A062600075 A062600076 Concentration or PFOSEA ug/mL or % Ree <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mLl <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 Ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <L O Q ( 0.00975 ug/mL) <t n n i n nnm *io/mi \ <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) PFOSEA ug/mL <LOO <LOQ <LOQ <LOQ RSD Std.Dev. MS/MSD RPD NA NA NA NA NA NA NA NA 3MEnvironmental Laboratory Page 214 3M M edical D epartm ent Study: T6316.1 AlYlUlff U W 3 ? / . I Covance# 6329-212 Study: Product N umber(Test Substance): 104 W eek Dietary C arcinogenicity Study w ith N arrow Range (98.1% ) N -E thyl Periluorooctanesulfonam ido E thanol in Rats T-6316 (EtFOSE-OH) Rat Serum Method/Revision: Analytical Equipment System N um ber ETS-8-4.1 &ETS-8-5.1 Davey 070799 & Ruby 100699 Instrument Software/Version: M asslynx 3.3 & 3.4 F i le n a m e : See Attachments R-Squared Value: See Attachments . Slope: See Attachments Y -I n te rc e p t : D ates o f Extraction/Analyst: See Attachments 02/23/00,03/28/00 SAL Dates o f Analysis/Analyst: 03/07/00, 03/27/00, 03/28/00, 04/03/00, 04/05/00, 04/06/00, 05/19/00, 06/26/00, 07/19/00, 08/17/00 IAS/HOJ/M M H/CSH Date o f Data Reduction/Analyst: 03/09/00, 04/03/00, 04/04/00, 04/05/00,04/07/00, 04/10/00,05/23/00, 06/27/00, 07/25/00, 08/18/00 IAS/H O J/M M H Sample Data WEEK 27 RAT SERA Group Dose Sample It C o D cen tratio n ofPFOS ug/mL nr % Ree PFOS RSD Std. Dev. MS/MSD RPD Concentration of PFOSA ug/mL or % Ree PFOSA RSD Std. Dev. MS/MSD RPD Group 3 M id Dose 30.0 mg/kg C90847M C90855M C90858M C90859M C90864M C90865M C90871M 14.7 21.6 21.4 24.4 21.5 21.7 22.5 0 .2 1 5 0.302 0 .1 9 3 0.239 0.236 0.228 0.204 C90872M C90882M C90886M C91252F 18.9 19.5 14.0 17.0 20.3 2.85 50.4 0.247 0.233 0.163 0.441 0.226 16.3 0.0368 C91254F C9I264F 42.9 31.4 0.446 0.433 C91267F C91283F 40.5 33.5 0.516 0.631 C91286F 47.0 0.490 C91292F 38.5 0.557 C91295F 44.2 0.706 Group 4 M id-H igh Dose C9I301F C91303F C90916M C90931M 41.7 18.6 26.3 39.7 7.39 97 68.7 0.491 0.365 0.424 0.524 0.508 19.9 0.101 100 mg/kg C90937M . C90940M C90944M 81.6 67.0 83.9 0.382 0.476 0.410 C90945M C90954M C90956M C90957M C90963M C913I2F C91323F 81.5 70.0 50.0 101 19.7 70.1 77.2 15.2 196 232 0.269 0.442 0.292 0.554 0.402 0.779 0 .8 6 3 0.418 21.6 0.0903 C91328F 136 0.606 C91339F C91340F 142 118 0.954 0 .7 5 8 C91351F C91354F C91357F 154 221 190 0.963 0.896 0.558 C91369F C91371F 160 22.6 0.627 . 38.6 146 170 38.3 1.74 0.875 0.338 PFOS = Periluorooctanesulfonate C orrected PFOS L O Q s (0.00492 & 0.00974 ug/m L) to include std correction factors PFOSA = Perfluorooctanesulfonamide new LO Q s are 0.00394 & 0.00781 ug/mL. LA C 02/19/01 PFOSAA = Perfluorooctanesulfonamidoacetate EtFOSE = Narrow Range N -Ethyl Perfluorooctanesulfonam ido e th y l alcohol PFOSEA = Perfuorooctane sulfonyl ethylamide Date E ntered/By: Date V erified/ By: Purity Entered/Verified: 04/11/00, 04/12/00, 04/17/00, 06/02/00,06/07/00, 07/11/00, 08/15/00, 09/01/00 CSH/LAC 02/22/01 K J H / 04/30/01 LA C 02/19/01 LAC Concentration of PFOSAA ug/mL or % Ree 2 .3 0 4.44 2 .0 4 2.56 2 .4 7 2.12 1.94 1.53 1.88 1 .3 9 3 .7 8 3 .0 5 2 .8 4 3.26 2 .7 8 6.06 2 .9 3 4.24 2 .8 0 2.86 9.91 7 .0 5 7.50 8.56 6.71 4.60 5 .0 3 3 .4 2 4.80 8.19 9 .6 4 9 .7 7 6.30 8 .6 5 5 35 8 .2 6 11.3 5 .5 5 5 .8 0 9.80 Analytical Report: FACT-TOX-001 L R N -U 2103 PFOSAA RSD Std. Dev. MS/MSD RPD 37.4 2.27 0.848 29.9 3.46 1.03 31.3 6.58 2.06 26.5 8.04 2.13 3MEnvironmental Laboratory Page 215 3M M edical D epartm ent Study: T6316.1 A in u i n /. i Covance# 6329-212 Study: 104 W eek Dietary C arcinogenicity Study w ith Narrow Range (98.1% ) N -Ethyl Periluorooctanesulfonam ido E thanol in Rats Product Number(Test Substance): T-6316 (EtFOSE-OH) Rat Serum Method/Revision: E T S - M .l & ETS-8-5.1 Analytical Equipment System Number: Davey 070799 & Ruby 100699 Instrument Software/Version: M asslynx 3.3 & 3.4 F i le n a m e : R-Squared Value: Slope: See Below S ee Attachments See Attachments Y-lntereept: See Attachments Dates o f Extraction/Analyst: 02/23/00, 03/38/00 SAL Dates o f Analysis/Analyst: 03/07/00, 03/27/00, 03/28/00, 04/03/00, 04/05/00, 04/06/00, 05/19/00, 06/26/00, 07/19/00, 08/17/00 IAS/H O J/M M H /CSH Date o f Data Reduction/Analyst: 03/09/00, 04/03/00, 04/04/00, 04/05/00, 04/07/00, 04/10/00, 05/23/00, 06/27/00, 07/25/00, 08/18/00 IAS/H O J/M M H Sample Data WEEK 27 RAT SERA Group Dose Sample M Concentration of EtFOSE-OH ug/mL or % Ree EtFOSE-OH ug/mL RSD Std. Dev. MS/MSD RPD Concentration of M556 ug/mL or % Ree M556 RSD Std. Dev. MS/MSD RPD Group 3 M id Dose 30.0 mg/kg C90847M C90855M C90858M <LOQ (0.0248 Ug/mL) <LOQ (0.0248 ug/m L) <LOQ (0.0248 ug/m L) 2 .0 7 2 .0 5 2.11 C90859M <LOQ (0.0248 ug/m L) 1.86 C90864M <LOQ (0.0248 ug/m L) 1.82 C90865M <LOQ (0.0248 ug/m L) 2.51 C90871M <LOQ (0.0248 ug/m L) 1.67 C90872M <LOQ (0.0248 ug/m L) 3.01 C90882M <LOQ (0.0248 ug/mL) N A 1.49 22.2 C90886M <LOQ (0.0248 ug/m L) <LOQ NA 1.68 2.03 0.449 C91252F <LOQ (0.0248 ug/mL) 3.85 C91254F <LOQ (0.0248 ug/m L) 3 .4 0 C91264F <LOQ (0.0248 ug/mL) 3.31 C91267F <LO Q (0.0248 ug/m L) 4.80 C91283F <LOQ (0.0248 ug/m L) 3 .9 8 C91286F <LOQ (0.0248 ug/m L) 2 .9 8 C91292F <LO Q (0.0248 ug/mL) 5 .5 0 C91295F <LO Q (0.0248 ug/mL) 4.32 C91301F <LO Q (0.0248 ug/m L) NA 4.28 20.1 C91303F <LO Q (0.0248 ug/m L) <LOQ NA 3.14 3.96 0.796 Group 4 C90916M <LOQ (0.0248 ug/m L) 7.18 Mid-High Dose C90931M <LOQ (0.0248 ug/mL) 8 .4 7 100 mg/kg C90937M C90940M <LOQ (0.0248 ug/m L) <LOQ (0.0248 ug/m L) 8 .1 7 6.18 C90944M <LOQ (0.0248 ug/m L) 6 .9 8 C90945M <LOQ (0.0248 ug/m L) 5 .6 6 C90954M <LOQ (0.0248 ug/mL) 7 .3 8 C90956M <LOQ (0.0248 ug/m L) 5 .8 4 C90957M <LOQ (0.0248 ug/m L) NA 6.14 19.7 C90963M <LOO (0.0248 ug/m L) <LOQ NA 4.09 6.61 1.30 C91312F C91323F <LOQ (0.0248 ug/m L) <LOQ (0.0248 ug/m L) 4 .1 3 6.40 C91328F <LOQ (0.0248 ug/m L) 4.41 C91339F <LOQ (0.0248 ug/m L) 8 .8 4 C91340F <LOO (0.0248 ug/m L t 5 .1 4 C91351F 0.0256 7 .4 0 C91354F <LOQ (0.0248 ug/m L) 7.72 C91357F <LOQ (0.0248 ug/m L) 4.36 C91369F C91371F <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/m L) <LOQ NA NA 4.96 10.2 33.2 6.36 2.11 PFOS = Perfluorooctanesulfonate C orrected PFO S LOQs (0.00492 & 0.00974 ug/m L) to include std correction factors PFOSA = Perfluorooctanesulfonamide new LO Qs are 0.00394 & 0.00781 ug/m L . LA C 02/19/01 PFOSAA = Perfluorooctanesulfonamidoacetate EtFOSE = N arrow Range N -Ethyl Perfluorooctanesulfonam ido e th y l alcohol PFOSEA = Perfuorooctane sulfonyl ethylamide Date Entered/By: Date V erified/ By: Purity Entered/Verified: 04/11/00, 04/12/00, 04/17. 00, 0 6 /02'00, 06/07/00, 07/11/00, 08/15/00, 09/01/00 CSH/LAC 0 2 /2 2 /0 l KJH / 04/30/01 LAC 02/19/01 LAC _ ' Concentration of PFOSEA ug/mL or % Ree <LOQ ( 0.00975 ug/mL) <LOQ ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <I.OQ {0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/m L) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/m L) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/m L) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/m L) <LO Q ( 0.00975 ug/m L) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO O ( 0.00975 ue/m L) <LO Q ( 0.00975 ug/m L) <LO Q ( 0.00975 ug'm L) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <1 O O t 0 00975 .io/m i t < L O Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) <LO Q ( 0.00975 ug/mL) PFOSEA ug/mL <LOQ <LOQ <LOQ <LOQ Analytical Report: FACT-TOX-001 . LRN-U2103 RSD Std. Dev. MS/MSD RPD NA NA NA NA NA NA NA NA 3MEnvironmental Laboratory Page 216 3M M edical D epartm ent Study: T6316.1 A M U I f f U ViSi<7.1 Covance# 6329-212 Study: Product NumberfTest Substance); Matrix: Method/R*vision: Analytical Equipment System Number. Instniment Soflware/Version: Filename: R-Squated Value: Slope: Y-Intarcept Dales ofExtrection'Analyst Dales of Analysis Analyst: Dale o f Data Reduction-Analyst: Sample Data W E E K 53 RAT SER A Group Dose Sample $ Method Blk Matrix Blk Matrix Blk QC-250 ng/mL Group 1 Control 0.0mg/kg RBS02250-H20 Blk-1-1 RBS02250-H2O Blk-1-2 RBS02250-H20 Blk-l-3 RBS02250-H20 Blk-1-4 RBS02250-Serm Blk- !-1 RBS02250-Sera Blit-1-2 RBSO2250-Scre Blk-l-3 RBS02250-Sera Blk-1-4 RTS02250-Sera Blk-1-1 RTS02250-Sere Blk-1-2 RTS02250-Sera Blk-l-3 RTS02250-Sera Blk-1-4 RTS02250-MS-1-1 RTS02250-MS-1-2 RTS02250-MS-1-3 RTS02250-MS-1-1 RTS02250-MS-1-2 RTS02250-MS-1-3 RTS02250-MSD-2-1 RTS02250-MSD-2-2 RTS02250-MSD-2-3 RTS02250-MSD-2-1 RTS02250-MSD-2-2 RTS02250-MSD-2-3 C90712M C907I4M C90723M C90727M C90730M C90751M C90752M C90754M C90755M C90758M C90759M C90764M C90766M C90767M C90774M C91I2IF C91I22F C91123F C91I25F C91131F C91132F C91133F C9I152F C9I153F C9I156F C9I158F C91178F C91180F 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctaoesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 & ETS-8-5.1 Amelia 062498, Soup 020199. Ruby 100699 Masslynx 3.3 & 3.4 See Below See Attachments See Attachments See Attachments 2'25'00 RWW 03'22'00,03'30'00,04'10/00,04/18.00, 04/20 00.04/21/00,05'0 l'OO,05/24/00, 08/18/00, 08/21'00, 08/23/00 CSH/MMH/1AS 04/12 '00, 04/13/00, 04/19/00, 04.20/00, 04/21'00,04/25/00,05.03 00,05,25/00, 0821-00, 0822/00, 0825/00 [AS/MMH/HOJ Eitractton VoL 1 1 1 1 1 1 1 1 1 1 1 I 1 1 t 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Confirmed High NA Confirmed High Confirmed High Confirmed High NA NA NA Confirmed High Confirmed High -- .......-- Confirmed High NA NA Confirmed High Confirmed High Confirmed High Confirmed High Confirmed High NA Confirmed High PFOS Std C o r r e c ti o n Fnctor 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 NA NA NA NA NA NA NA NA NA NA NA NA 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 -0.9275 0.9275 0.9275 0.9275 0,9275 0.9275 0.9275 0.9275 0.9275 0.9275 lot 171 PFOS Purity C o r r e c ti o n Fa c to r 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 NA NA NA NA NA NA NA NA NA NA NA NA 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 PFOS Dilution Fa c to r 1 1 1 1 1 1 l NA NA NA NA NA 1 1 1 1 1 1 1 1 1 1 1 1 0.8640 0.3640 0.8640 0.8640 0.3640 0.8640 0.3640 0.8640 0.3640 0.8640 1 1 1 1 1 1 1 1 PFOS Cone. 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 186 188 168 NA NA 194 240 269 278 NA NA NA 12.6 36.0 15.1 1.57 8.78 11.0 59.6 40.6 17.0 13.6 38.4 24.1 8.20 18.5 49.1 127 173 73.7 ..v 75.7 98.4 31.4 154 168 37.6 44.9 49.9 76.6 67.0 Filename D082100007 D042100018 D042100019 D042100020 D082100008 D042100021 D042100022 D042100026 D082100009 D042100027 D042100028 D042100029 R033000018 R033000019 R033000020 NA NA D050100035 D03300082 D03300083 D03300084 NA NA NA D050100042 R033000024 D050100044 D082100020 D08210002I D05010005 R033000031 R033000032 D050100053 D050100054 R033000037 D050100059 D082100022 D050100061 R033000041 R033000044 R033000045 R033000046 Concentro thin of PFOS ug/m Lor% Rec < LOQ (0.00394 ug/tnL) < LOQ (0.00394 ug/mL) < LOQ (0.00394 ug/mL) < LOO (0.00394 ug/mL) < LOQ (0.00394 ug/mL) < LOQ (0.00394 ug/tnL) < LOQ (0.00394 ug/tnL) < LOQ (0.00394 ug/mL) < LOQ (0.00394 ug/tnL) < LOQ (0.00394 ug/mL) < LOQ (0.00394 ug/mL) < LOQ (0.00394 ug/mL) 75% 76% 68% NA NA 78% 97% 109% 112% NA NA NA 0.0101 0.0288 0.0121 < LOQ (0,00394 ug/mL) 0.00704 0.0088 0.0477 0.0325 0.0136 0.0109 0.0307 0.0193 0.00657 0.0148 0.0393 0.101 0.138 0.0590 2nd PFOS <LOQ <LOQ <LOQ 73% 78% 106% NA 00191 K033000048 R033000051 R033000052 R033000053 R033000054 R033000055 R033000058 R033000059 R033000060 R033000061 0.0606 0.0788 0.0251 0.123 0.134 0.0301 0.0360 0.0400 0.0614 0.0537 Group 2 Low Dose 3.0 mg/kg C9078IM C90792M C90793M C90798M C90799M C90800M C90812M C90822M C90829M C90832M C91194F C91197F C91199F C91200F C91206F C91227F 1 1 1 1 1 1 1 1 1 1 1 1 1 C9123IF C91244F C9I250F PFOS = Periluorooctanesulfonate PFOSA Perfluorooctancsulfonamide PFOSAA = Perfluorooctanesulfonamidoacetate EtFOSE - Narrow Range N-Ethyl Periluorooctanesulfonamido ethyl alcohol M556 -C8F17S02N((H)CH2C00) PFOSEA - Periuorooctane sulfonyl elhylamide NA NA NA NA NA NA Confirmed High Confirmed High NA NA NA NA NA NA NA NA NA NA 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.8640 0.3640 0.8640 0.8640 0.8640 0.8640 0.3640 0.8640 . 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.3640 0.8640 0.8640 0.8640 0.8640 0.8640 10 10 1 10 10 10 1 1 10 10 10 10 10 10 10 10 10 10 10 10 Corrected PFOS LOQ (0.00492 ug'mL) to include std correction factors new LOQ is 0.00394 ug'mL LAC 02/19 01 206 377 459 153 278 363 841 705 304 440 350 620 615 459 292 729 831 370 849 713 R050200016 R05020001? R033000067 R050200019 R050200020 R050200025 A041800051 A04I800052 R050200027 R050200028 RQ50200029 R050200034 R050200035 R050200036 D041700086 R050200038 R050200043 R050200044 R050200045 R050200046 1.65 3.03 0.367 1.23 2.23 2.91 0.674 0.565 2.43 3.53 2.81 4.97 4.93 3.68 2.34 5.84 6.66 2.97 6.80 5.72 1.86 4.67 Dale Entered.'By: Dale Verified' By: Purity Enlered/Verified: 04 17 00, 04. 20/00, 04.24/0.0425 00,05 04'00, 05 05 00, 06-12 00,09-0! 00. 09 18 00. 11 06/00 CSH-MMH/LAC 02 23-01 KJH - 04,30/01 LAC 02 19 01 LAC RSD Std. Dev. MS/MSD RPD NA NA NA 6% 4% NA NA 7% 8% NA NA 70.3 00134 49.9 60.6 1.128 34.9 1.63 Analytical Report: FACT-TOX-001 L R N -U 2103 lotL-15709 PFOSA Purity Correction Fa c to r Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA NA 1Jnlrnnwn Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown VUMIUWU Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Confiimed High NA Confirmed High Confiimed High Confirmed High NA NA NA Confirmed High Confirmed High k.utiiiimcu rttgn Confirmed High NA NA Confirmed High Confiimed High Confirmed High Confirmed High Confirmed High NA Confirmed High PFOSA Dilution Fa c to r I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 NA NA NA 1 1 1 NA NA NA 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Confirmed High NA NA NA Confirmed High 2nd Analysis OK Confirmed High . Confirmed High Confirmed High Confirmed High Confirmed High Confirmed High Confirmed High Confirmed High Confirmed High Confirmed High Confirmed High NA NA NA 1 I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 PFOSA Cone. ng/mL 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 206 216 214 NA NA NA 232 253 275 NA NA NA 1.49 1.79 1.45 1.19 1.37 1.49 1.99 1.36 0.00 1.49 0.960 0.000 0.870 0.00 1.04 0.880 1.04 0.830 i.ii 1.010 0.950 0.970 1.10 1.18 0.900 1.18 0.00 0.00 1.04 Filename R033000004 D0501000I8 D0501000I9 D050100020 R033000005 D050100021 D050100022 D050100023 R033000006 D050100024 D050100025 D050I00026 R033000018 R033000019 R033000020 NA NA NA D03300082 D03300083 D033000S4 NA NA NA R033000023 R033000024 R033000025 R033000026 R033000027 R033000030 R033000031 R033000032 R033000033 R033000034 R041000040 R041000041 R041000042 R041000043 R041000044 R041000048 R041000049 R041000050 KueiuOwji R041000052 R041000056 R041000057 R041000058 R041000059 R041000060 R041000064 R041000065 R041000066 R041000067 C o n c en t rati o n of PFOSA ug/mL or % Ree <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ugmL) <LOO (0.00493 ug/mL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) <LOO (0.00493 ug/mL) 83% 87% 86% NA NA NA 94% 102% 111% NA NA NA <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.O493 ug'mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) ' L u y tu .w yj ugmLj <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) PFOSA <LOQ <LOQ <LOQ 85% NA 102% NA <LOQ 12.8 R041000072 <LOQ (0.00493 ug'mL) 16.1 R04000073 22.3 R04I000074 <LOQ (0.00493 ugmL) 12.8 R041000075 <LOQ (0.00493 ug/mL) 13.3 R041000076 <LOQ (0.00493 ug/mL) 15.2 R041000030 <LOQ (0.00493 ug/mL) 13.3 R04I000031 <LOQ (0.00493 ugmL) 11.8 R041000082 <LOQ (0.00493 ug'mL) 13.8 R041000083 <LOQ (0.00493 ug'mL) 23.6 R041000084 <LOQ (0.00493 ug/mL) 'LOQ 28.6 R04I000088 <LOQ (0.00493 ug/mL) 34.5 R041000089 <LOQ (0.00493 ug/mL) 32.4 R04I000090 <LOQ (0.00493 ug'mL) 19.2 R041000091 <LOQ (0.00493 ug'mL) 15.9 R041000092 <LOQ (0.00493 ug'mL) 27.4 R041000096 'L O Q (0.00493 ug'mL) 26.1 R041000097 <I.OQ (0.00493 ug'mL) 27.4 R041000098 <LOQ (0.00493 ug mL) 34.5 R041000099 <-LOQ (0.00493 ug'mL) 30.8 R041000100 <LOQ (0.00493 ug mL) <LOQ RSD Std. Dev. MS/MSD RPD NA NA NA 3% 2% NA 8% 9% NA NA NA NA NA NA NA NA 3MEnvironmental Laboratory Page 217 3M M edical D epartm ent Study: T6316.1 Covance# 6329-212 Study: Product Number(Test Substance): Matrix: Melhod/Revision: Analytical Equipment System Number Instrument Software,Version: Filename: R-Squared Value: Slope: Y-Intercpt: Dates of Extraelion'Analysl: Dales of Analysis/Analyst Dale of Data Reduction''Analyst Sample Data WEEK 53 RAT SERA G ro up Dose Sample # Method Blk Matrix Blk Matrix Blk QC-250ng'mL Group 1 Control 0.0 mg/kg RBS02250-H20 Blk-t-l RBS02250-H20 Blk-1-2 RBS02250-H2O Blk-l-3 RBS02250-H20 Blk-1-4 RBS02250-Sera Blk-1-1 RBS02250-Sera Blk-12 RBS02250-Sera Blk-l-3 RBS02250-Sen Blk-1-4 RTS02250-SeraBlk-i-l RTS02250-Sera Blk-1-2 RTS02250-Sera Btk-l-3 RTS02250-Seri Blk-1-4 RTS02250-MS-1-1 RTS02250-MS-1-2 RTS02250-MS-1-3 RTS02250-MS-1-1 RTS02250-MS-1-2 RTS02250-MS-1-3 RTS02250-MSD-2-1 RTS02250-MSD-2-2 RTS02250-MSD-2-3 RTS02250-MSD2-1 RTS02250-MSD-2-2 RTS02250-MSD-2-3 C90712M C90714M C90723M C90727M C90730M C90751M C90752M C90754M C90755M C90758M C90759M C90764M C90766M C90767M C90774M C9112IF C91I22F C91I23F 104 Week Dietary Carcinogenicity Study with Narrow Range (98 1%)N-Elhyl Perfluorooclancsulfonamido Ethanol in Rats T-6316 (ElFOSE-OH) Rat Serum ETS-8-4.1 &ETS-8-S.I Amelia 062498, Soup 020199, Ruby 100699 Masslynx 3.3 & 3.4 See Below See Attachments See Attachments See Attachments 2'25/00 RWW 03/22/00, 03/30/00,04/10/00.04/18 00, 0420'00, 0421/00,05/01 00,05/24/00,08/18/00,08/2100,08/23/00 CSH/MMH/IAS 04/12'00. 04/13 00,04/19/00, 04 20/00, 0 4 2 1/00,0425'00,05 03/00,0525/00, 0821/00,0822'00,08/25/00 IAS/MMH/HOJ lot T-7121.1 PFOSAA Purity Correctton Factor Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Confirmed High NA NA NA NA Confirmed High NA Confirmed High Confirmed High Confirmed High NA NA NA Confirmed High Confirmed High PFOSAA DUuttan Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 NA NA NA 1 1 1 NA NA NA 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 PFOSAA Com. its/m L 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 249 242 224 NA NA NA 268 278 291 NA NA NA 0.00 3.79 0.00 0.00 0.00 5.75 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 Filename D082100007 D050I00018 D050100019 D050I00020 D082100008 D050100021 D050100022 D050100023 D082100009 D050I00024 D050100025 D050I00026 R033000018 R033000019 R033000020 NA NA NA D042100034 D042100036 D042100041 NA NA NA R041700018 R041700019 R041700020 R041700021 R041700022 R041700026 R041700027 R041700028 R04I700029 R041700030 R041700034 R041700035 R041700036 R04I700037 R041700038 R041700042 R041700043 R041700044 CameDtratian a f PFOSAA ug/mL a r % Ree <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <-LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOO <0.0248 ug/mL) 100 98% 90% NA NA NA 108% 112% 117% NA NA NA <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.009? ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug'mL) <LOQ (0.0097 ug'mL) PFOSAA <LOQ <LOQ <LOQ 96% NA 113% NA <LOQ RSD Std. Dev. MS/MSD RPD NA NA NA 5% 5% NA NA 4% 5% NA NA NA NA Group 2 Low Dose 3.0 mg/kg C91I25F C91I31F C91I32F C91133F C91I2F C91I53F C91156F C91158F C91I78F C91180F C90781M C90792M C90793M C90798M C90799M C9O8O0M . C90812M C90822M C90829M C90832M C9U94F C91197F C91199F C91200F C91206F C91227F C9I229F C9I231F C9I244F C9I250F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Confirmed High NA NA Confirmed High Confirmed High Confirmed High Confirmed High Confirmed High NA Confirmed High Confirmed High NA NA NA Confirmed High 2nd Analysis OK NA Confirmed High Confirmed High NA 2nd Analysis OK 2nd Analysis OK 2nd Analysis OK 2nd Analysis OK 2nd Analysis OK Confirmed High 2nd Analysis OK NA NA NA 1 1 1 1 1 1 1 1 1 1 1 1 1 1 l 1 10 I l 10 1 1 1 1 l 1 1 1 1 1 0.00 0.00 0.00 0.00 13.64 0.00 0.00 0.00 0.00 0.00 342 504 366 378 289 123 462 333 177 809 870 680 322 365 629 582 341 590 375 R041700046 R041700050 R04170005I R041700052 R0417000S3 R04I700054 R041700058 R041700059 R041700060 R041700061 <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug'mL) 0.0136 <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ug/mL) R04I000072 R041000073 R041000074 R041000075 R041000076 R041000080 R052400022 R041000082 R041000083 R052400024 D042I00058 D042I00059 D041700084 D041700085 D041700086 D041700090 D041700091 D041700092 D041700093 D041700094 0.342 0.301 0.504 0.366 0.378 0.289 1.23 0.462 0.333 1.77 0.809 0.870 0.680 0.322 0.365 0.629 0 582 0.341 0.59 0.375 0.597 0.556 NA . 83.2 0.497 35.7 0.199 PFOSA = Periluorooctanesulfonanride PFOSAA Perfluorooclanesulfonamidoacetale EtFOSE = Narrow Range N-Ethyl Perfluorooetanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2COO) PFOSEA * Perfuorooctane sulfonyl ediylamide Corrected PFOS LOQ (0.00492 ug'mL) to include std correction factors new LOQ is 0.00394 ug'mL LAC 02/19/01 Date Entered'By: Date Verified/ By: Purity Entered'Verified: 04 17 00, 04 20 0 0 ,0 4 2 4 0 .0 4 2 5 00, 05 04,OO. 05 05 00.06 12/00,09 01 00,09 !8'00,11/06 00 CSHMMH/LAC 0 22301 K JH .0 4 3 0 0 1 LAC 02 1901 LAC lot Unknown/SDO13 EtFOSE-OH Purity Correctloii Factor Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Analytical Report: FACT-TOX-001 L R N -U 2103 Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Confirmed High NA Confirmed High Confirmed High Confirmed High NA NA NA 2nd Analysis OK 2nd Analysis OK 2nd Analysis OK NA NA Confirmed High 2nd Analysis OK Confirmed High 2nd Analysis OK Confirmed High NA 2nd Analysis OK 2nd Analysis OK NA NA NA Confirmed High 2nd Analysis OK Confirmed High Confirmed High Confirmed High Confirmed High NA NA NA NA NA NA NA NA NA NA EtFOSE-OH Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 l 1 1 1 1 I 1 I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 l 1 1 1 1 1 1 EtFOSE-OH Com. nc/mL 2.89 0.890 0.00 2.57 0.00 0.00 0.00 0.00 0.00 0.00 0.00 78.2 98.3 95.4 69.5 78.4 64.9 95.6 115 114 87.2 70.6 91.2 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.880 0.00 0.00 0.00 0.00 4.27 4.49 4.35 2.17 3.29 3.11 4.78 3.64 3.99 5.40 Filename A032200014 D050100018 D050100019 D050100020 A032200021 D050100021 D050100022 D050100023 A032200028 D050100024 D050100025 D050100026 R033000018 R033000019 R033000020 D050100030 D050100034 D050100035 D03300082 D03300083 D03300084 D050100036 D050100037 D050100038 R041000024 R041000025 R041000026 R041000027 R041000028 R041000032 R04I000033 R041000034 R041000035 R041000036 R041000040 R04100004I R041000042 R041000043 R041000044 A041800018 A041800019 A041800020 A04I800022 A041800026 A04I800027 A04I800028 A041800029 A041800030 A041800034 A041800035 A041800036 A041800037 CatMcntration of EtFOSE-OH ug/mL a r % Ree <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug'mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/tnL) 32% 40% 38% 28% 32% 26% 39% 46% 46% 35% 28% 37% <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) 'L O Q (0.00493 ug'mL) '-L uv iu.uu4yj ugml_) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) 2nd 2nd 2nd 2nd 2nd 2nd EtFOSE-OH <LOO <LOQ <LOQ 37% 29% 44% 33% <LOQ A041800042 A041300043 A041800044 A041800045 A041800046 A041800050 A041800051 A04I800052 A041800053 A041800054 R050200047 R050200052 R050200053 R050200054 R050200055 R050200056 R050200061 R050200062 R050200063 R050200064 <LOQ (0.00493 ug'mL) *-LOQ (0.00493 ugmL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mt) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ(0.00977 ug'mL) <LOQ(0.00977 ug'mL) <LOQ(0.00977 ug'mL) <LOQ(0.00977 ug/mL) <LOQ(0.00977 ug'mL) <LOQ(0.00977 ug'mL) <LOQ(0.00977 ug'mL) <LOQ(0.00977 ug'mL) <LOQ(0.00977 ug'mL) <LOQ(0.00977 ug'mL) <LOQ <LOQ RSD Std. Dev. MS/MSD RPD NA NA NA 12% 4% 10% 3% 10% 13% 4% NA NA NA NA NA NA NA 3MEnvironmental Laboratory Page 218 3M M edical D epartm ent Study: T6316.1 Covance# 6329-212 Study: Product Numbet(Test Substance): Matrix: Method/Revision Analytical Equipment System Number: Instrument Software/Vcision: Filename: R-Squaied Value: Slope: Y-Intercepl: ' Dates of Extrection/Analyst: Dates of Analysis/Analyst: Date of Data Reduction/Analyst: Sample Data 104 Week Dielaty Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluotooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Scrum ETS-8-4.1 & ETS-8-5 1 Amelia 062498, Soup 020199, Ruby 100699 Masslynx 3.3 & 3.4 See Below See Attachments See Attachments See Attachments 225/00 RWW ' 03 2 2'00,0320/00,04/10/00.04/18/00, 04/20 00,0421/00,05 01/00,0524/00, 08.18/00, 0821/00, 0823/00 CSH/MMH/'IAS 04.12 00,04 13.00,04/19/00,0420/00, 04/21/00,0425/00, 05.03/00,0525'00, 0821/00,0822/00, 0825/00 lAfvMMH/HOJ W E E K S3 R A T S E R A lotNB113047-80 Dose Method Blk Matrix Blk Matrix Blk QC-250 ng/mL Group 1 Control 0.0mg/kg s"'** RBS02250-H20 Blk-1-1 RBS02250-H2O Blk-12 RBS02250-H20 Blk-1-3 RBS02250-H20 Blk-1-4 RBS02250-Sera Blk- l-l RBS02250-Sera Btk-1-2 RBS02250-Sera Blk* 1-3 RBS02250-Sera Blk-1-4 RTSO22J0-Sent Blk-1-1 RTS02250-Sera Blk-12 RTSO2250-Sent Blk-1-3 RTS02250-Sera Blk-1-4 RTS02250-MS-1-I RTS02250-MS-1-2 RTS02250-MS-I-3 RTS02250-MS-1-I RTS02250-MS-12 RTS02250-MS-1-3 RTS02250-MSD-2-I RTS02250-MSD-2-2 RTS02250-MSD-2-3 RTS02250-MSD-2-I RTS02250-MSD-2-2 RTS02250-MSD-2-3 C907I2M C907I4M C90723M C90727M C90730M C9075IM C90752M C90754M C90755M C90758M C90759M C90764M C90766M C90767M C90774M C91121F C91122F C91123F M556 Purity C o r r e c tt e n Factor Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown C91125F C91131F C91132F C91133F C9112F C91153F C91I56F C91158F C91178F C91180F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Group 2 C90781M Unknown Low Dose C90792M Unknown 3.0mg/kg C90793M C90798M Unknown Unknown C90799M Unknown C90800M C908I2M Unknown Unknown C90822M Unknown C90829M Unknown C90832M Unknown C91194F Unknown C91197F Unknown C91199F Unknown C91200F Unknown C91206F C91227F Unknown l nknown C91229F l nknown C9123IF C91244F l nknown Unknown C91250F Unknown PFOS " Perfluorooctanesulfonate PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethy! Perfluorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2C00) PFOSEA = Perfuorooctane sulfonyl ethylamide Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Confirmed High NA Confirmed High Confirmed High Confirmed High NA NA NA Confirmed High Confirmed High M55 Dilution F a c to r 1 1 1 1 1 1 1 1 1 1 1 1 l 1 1 NA NA 1 1 1 1 NA NA 1 1 1 1 1 1 1 1 1 1 1 I l 1 1 1 1 1 1 Confirmed High NA NA Confirmed High Confirmed High Confirmed High Confirmed High Confirmed High NA Confirmed High 1 1 1 1 1 1 1 1 1 1 Confirmed High NA NA NA Confirmed High 2nd Analysis OK Confirmed High Confirmed High Confirmed High Confirmed Hieh Confirmed High Confirmed High Confirmed High Confirmed High Confirmed High Confirmed High Confirmed High NA 1 1 1 1 l 1 1 1 I 1 1 1 1 1 1 1 l l M556 Cone. rtf/mL 0.00 0.03 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 316 282 336 NA NA 305 307 308 329 NA NA 325 136 0.710 0.00 0.00 0.00 0.340 0.450 0.380 0.00 0.00 0.33 0.000 0.00 0.00 0.00 1.78 0.820 0.320 ..... 0.00 1.01 0.00 0.260 0.00 0.00 155 0.220 0.00 0.530 344 376 189 294 424 429 341 286 436 594 441 694 521 403 167 418 408 476 504 File ni me D042100004 D0501000I8 D050I00019 DO50100020 D042I00005 D05010002I D050100022 D050I00026 D042100006 D050I00027 D050100028 D050100029 R041000018 R041000019 R041000020 NA NA D042100037 D042100034 D042100036 D042100041 NA NA D050100038 D050100042 D050100043 D050100044 D050100045 D050100046 D050100050 D050100051 D050100052 D050100053 D050100054 D050100058 D050100059 D050100060 D050100061 D050100062 D050100066 D050100067 D050100068 " . '" "TM/ D050100070 D050100074 D050100075 D050100076 D050100077 D050100078 D050100082 D050100083 D050100084 D050100085 Cencentratlen of M556 ug/mL o r % Ree < LOQ (0.00494 ug/mL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOO (0.00494 ue/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOO (0.00494 ue/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOO (0.00494 ue/mL) 127% 114% 135% NA NA 123% 2nd 124% 124% 133% NA NA 131% 2nd < LOQ (0,00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 Ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ug/mL) R041000072 R041000073 R041000074 R041000075 R041000076 R041000080 R04100008I R04I000082 R041000083 R041000084 R041000088 R041000089 R041000090 R041000091 R041000092 R041000096 R04I000097 R04I000098 R041000099 R04I000100 0.344 0.376 0.189 0.294 0.424 0.429 . 0.341 0.286 . 0.436 0.594 0.441 0.694 0.521 0.403 0.167 0.418 0.408 0.476 0.504 0.356 M5S6 <LOO <LOQ <LOQ 125% 123% 127% 131% <LOQ <LUQ 0.371 0.439 Corrected PFOS LOQ (0.00492 ug'mL) to include std correction factors new LOQ is 0.00394 ug/mL LAC 02'19/01 Date Entered By: Dale Verified/ By: Purity EnteredVerified: 04.17 00,04 20 00. 04 24 0.04 25 00.05 04 00.05 05 00.06 12 00.09 01'00, 09 ISW). 11/06 00 CSH/MMH/LAC 0223 01 KJH ' 04.20/01 LAC 02 1901 LAC RSD Std. Dev. MS/MSD RPD NA NA NA 9% 11% NA NA 4% 5% NA NA NA NA NA 29.5 0.110 30.4 0.134 lot529 PFOSEA Purity Correction Fa c to r Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown X.'uaiiowu Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrognte Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Confirmed High NA Confirmed High Confirmed High Confirmed High NA NA NA 2nd Analysis OK 2nd Analysis OK mi rxmnysis v>r>. 2nd Analysis OK NA NA Confirmed High 2nd Analysis OK Confirmed High 2nd Analysis OK Confirmed High NA 2nd Analysis OK Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown 2nd Analysis OK NA NA NA Confirmed High 2nd Analysis OK Confirmed High Confirmed High Confirmed High Confirmed Hieh Confirmed High Confirmed High Confirmed High Confirmed High Confirmed High Confirmed High NA NA NA NA PFOSEA Dilution Fnctor 1 1 1 1 1 1 1 1 1 1 1 l 1 1 NA 1 1 1 1 1 1 NA NA 1 1 t 1 1 1 1 1 1 1 1 I I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 l l 1 1 l 1 1 l 1 1 1 1 1 1 1 1 1 1 1 3MEnvironmental Laboratory Analytical Report: FACT-TOX-001 L R N -U 2103 PFOSEA Cone. 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 174 159 114 NA 125 76.4 157 188 192 157 NA NA 0.00 0.00 0.00 o.oo 0.00 0.00 0.00 0.00 o.oo 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 Filename A032200014 D050100018 D050100019 D050100020 A032200021 D050100021 D050100022 D050100023 A032200028 D050100024 D050100025 D050100026 R033000018 R033000019 R033000020 NA R041000019 R041000020 D03300082 D03300083 D03300084 D050I00036 NA NA R041000024 R041000025 R041000026 D050100045 D050100046 R041000032 R041000033 R041000034 D050100053 R041000036 D050100058 D050100059 D050100060 D050100061 D050100062 A041800018 A 04I8 000I9 A041800020 Concentra ben o PFOSEA ug/mL or % Ree <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOO (0.00492 ue/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOO (0.00492 ue/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) 70% 64% 46% NA 51% 31% 63% 76% 78% 63% NA NA <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug'mL) <LOQ (0.00492 ug/mL) <LOO (0.00492 ue/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug'mL) <-LOQ (0.00492 ug/mL) NA 2nd 2nd 0.00 A041800022 <LOQ (0.00492 ugmL) 0.00 A041800026 <LOQ (0.00492 ug/mL) 0.00 A041800027 <LOQ (0.00492 ug'mL) 0.00 A041800028 <LOQ (0.00492 ugmL) 0.00 A041800029 <LOQ (0.00492 ugmL) 0.00 A04I800030 <LOQ (0.00492 ugmL) 0.00 A04IS00034 <LOQ (0.00492 ugmL) 0.00 A041800035 <LOQ (0.00492 ugmL) 0.00 A04I800036 <LOQ (0.00492 ugmL) 0.00 A04I800037 <LOQ (0.00492 ugmL) 0.00 A041S00042 <LOQ (0.00492 ugmL) 0.00 A041300043 0.00 A041800044 <LOQ (0.00492 ug/mL) 0.00 * A041800045 <LOQ (0.00492 ug/mL) 0.00 A041800046 <LOQ (0.00492 ug/mL) 0.00 A041800050 <LOQ (0.00492 ug/mL) 0.00 A041800051 <LOQ (0.00492 ugmL) 0.00 A041800052 <LOQ (0.00492 ug/mL) 0.00 A041800053. <LOQ (0.00492 ug/mL) 0.00 A041800054 <LOO (0.00492 ue/mL) 0.00 R041000088 <LOQ (0.0492 ugmL) 0.00 R041000089 <LOQ (0.0492 ugmL) 0.00 R041000090 <LOQ (0.0492 ugmL) 0.00 R04100009I <LOQ (0.0492 ugmL) 0.00 R041000092 <LOQ (0.0492 ug/mL) 0.00 R041000096 <LOQ (0.0492 ugmL) 0.00 R041000097 <LOQ (0.0492 ugmL) 0.00 R041000098 <LOQ (0.0492 ug/mL) 0.00 R041000099 <LOQ (0.0492 ugmL) 0.00 R041000100 <LOQ (0.0492 ug/mL) PFOSEA <LOO <LOO <LOQ 60% 41% 72% 63% <LOQ ,; <LOQ <LOQ RSD Std. Dev. MS/MSD RPD NA NA NA 21% 13% 14% 8% NA NA NA NA NA NA NA NA Page 219 3M M edical D epartm ent Study: T6316.1 C ovance# 6329-212 Study: Product Number(Test Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Veraon: R-Squaied Value: Slope: Y-Intercept: Dates of Extraction/Analyst Dates of AnalysigAnalyst; Date o f Data Redaction/Analyst: Sample Data WEEK 53 RAT SERA Greup Dase Sample # Method Blk Matrix Blk Matrix Blk QC-250 ng/mL Group 1 Control 0.0mg/kg RBS02250-H20 Blk-1-1 RBS02250-H20 Blk-1-2 RBS02250-H20 Blk-1-3 RBS02250-H20 Blk-1-4 RBS02250-Sera Blk-1-1 RBS02250-Sera Blk-1-2 RBS02250-Sera Blk-1-3 RBS02250-Sen> Blk-1-4 RTS02250-Sera Blk-1-2 RTS02250-Sera Blk-1-3 RTS02250-Sera Blk-1-4 RTS02250-MS-1-2 RTS02250-MS-1-3 RTS02250-MS-1-1 RTS02250-MS-1-2 RTS02250-MS-1-3 RTS02250-MSD-2-1 RTS02250-MSD-2-2 RTS02250-MSD-2-3 RTS02250-MSD-2-1 RTSO2250-MSD-2-2 RTS02250-MSD-2-3 C90714M C90723M C90727M C90730M C9075IM C90752M C90754M C907S5M C90758M C90759M C90764M C90766M C90767M C90774M C91121F C91122F C91I23F 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1V.) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 & ETS-8-5.1 Amelia 062498, Soup 020199, Ruby 100699 Masslynx 3.3 & 3.4 See Attachments See Attachments See Attachments See Attachments 2 25/00 RWW 03/22 00,03,30 00,04/10/00,04'18 '00,04/20'00, 04. 21/00, 05/01/00.0524.00,08.18/00,087E0O, 08/23 00 CSH/MMH/IAS 04.12/00,04/13 00,04/19 00.04 20/00, 04.21/00, 04.25'00, 05.03.00, 0525 '00,0821/00,0822 00, 0825/00 IAS/MMH/HOJ Concentration o f PFOS ugm L or % Ree < LOQ (0.00394 ug/mL) < LOQ (0.00394 ug/mL) LOQ (0.00394 ug/mL) < LOQ (0.00394 ugmL) < LOQ (0.00394 ug/mL) < LOQ (0.00394 ug/mL) < LOQ (0.00394 ug/mL) < LOQ (0.00394 ugmL) < LOQ (0.00394 ug/mL) < LOQ (0.00394 ug/mL) < LOQ (0.00394 ug'mL) < LOQ (0.00394 ug/mL) 75% 76% 6854 NA NA 78V. 97% 109% 112% NA NA NA 0.0101 0.0288 0.0121 < LOQ (0.00394 ug/mL) 0.0070 0.0088 0.0477 0.0325 0.0136 0.0109 0.0307 0.0193 0.0066 0.0148 0.0393 0.101 0.138 0.0590 2nd PFOS <LOQ <LOQ <LOQ 73% 78% 106% NA 0.0191 RSD Std. Dev. MS/MSD RPD NA NA NA 6% 4% NA NA 7% 8% NA NA 70.3 0.0134 Concentra tien af PFOSA ug/mL a r % Ree <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) <LOO (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ug/mL) LOO (0.00493 ug'mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ug/mL) LOQ (0.00493 ug'mL) 83% 87% 86% NA NA NA 94% 102% 111% NA NA NA <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ug'mL) <LOO (0.00493 ug/mL) PFOSA <LOQ <LOQ <LOQ 85% NA 102% NA <LOQ <IOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) RSD Std. Dev. MS/MSD RPD NA NA NA 3% 2% NA NA 8% 9% NA NA NA NA Concentra tian of PFOSAA ug/mL a r % Ree <LOQ (0.0248 ugmL) <LOQ (0.0248 ugmL) LOQ (0.0248 ugmL) <LOQ (0.0248 ugmL) <LOQ (0.0248 ugmL) <LOQ (0.0248 ugmL) <LOQ (0.0248 ugmL) <LOO (0.0248 ug'mL) <LOQ (0.0248 ugmL) <LOQ (0.0248 ugmL) <LOQ (0.0248 ugmL) <LOQ (0.0248 ugmL) 100% 98% 90% NA NA NA 108% 112% 117% NA NA NA <LOQ (0.0097 ugmL) <LOQ (0.0097 ug/mL) <LOQ (0.0097 ugmL) <LOQ (0.0097 ugmL) <LOQ (0.0097 ugmL) <LOQ (0.0097 ugmL) <LOQ (0.0097 ugmL) <LOQ (0.0097 ugmL) LOQ (0.0097 ugmL) <LOQ (0.0097 ugmL) <LOQ (0.0097 ugmL) <LOQ (0.0097 ugmL) <LOQ (0.0097 ugmL) <LOQ (0.0097 ug'mL) <LOO (0.0097 ugmL) <LOQ (0.0097 ugmL) LOQ (0.0097 ugmL) LOQ (0.0097 ugmL) PFOSAA <LOQ <LOQ <LOQ 96% NA 113% NA <LOQ Group 2 Low Dose 3.0 mg/kg C91I25F C91131F C91I32F C91133F C91I52F C91153F C91156F C91158F C91178F C91180F C90792M C90793M C90798M C90799M C90800M C90812M C90822M C90829M C90832M C9I194F C91197F C91199F C91200F C91206F C91227F C91229F C9123IF C91244F C91250F 0.0606 0.0788 0.0251 0.123 0.134 0.0301 0.0360 0.0400 0.0614 0.0537 0.367 1.23 223 2.91 0.674 0.565 2.43 3.53 2.81 4.97 493 3.68 2.34 5.84 6.66 2.97 6.80 5.72 <LOQ (0.00493 ugmL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) 49.9 LOQ (0.00493 ug'mL) <1rwv m n n io t ..n ani \ LOQ (0.00493 ug'mL) - LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ugmL) 60.6 <LOQ (0.00493 ug/mL) 1.86 1.128 <LOO (0.00493 ug/mL) <LOO <LOQ (0.00493 ug'mL) <LOQ (0.00493 ug'mL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) 34.9 <LOQ (0.00493 ugmL) 4.67 1.63 <LOO (0.00493 ug/mL) <LOQ <LOQ (0.0097 ugmL) <LOQ (0.0097 ugmL) <LOQ (0.0097 ugmL) <LOQ (0.0097 ugmL) 0.01 <LOQ (0.0097 ugmL) <LOQ (0.0097 ugmL) <LOQ (0.0097 ugmL) <LOQ (0.0097 ugmL) NA <LOQ (0.0097 ugmL) 0.342 0.301 0.504 0.366 0.378 0.289 . 1.230 0.462 NA 0.333 NA 1.770 0.809 0.870 0.680 0.322 0.365 0.629 0.582 0.341 NA 0.590 NA 0.375 0.597 0.556 PFOSA = Perfluorooclanesulfonamide PFOSAA - Perfluorooclanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl at M556 = C8F17S02N((H)CH2C00) PFOSEA = Perfuorooctane sulfonyl ethylamide Corrected PFOS LOQ (0.00492 ug'mL) to include std correction factors new LOQ is 0.00394 ug m L LAC 0219 01 Dale Entered/By: Dale Verified/ By: Purity EnteredVerified: 04.17/00, 0420'00, 0424/0, 0 4 2 5 00,05 04.00,05 05 00,06 12 00.09 01 00, 09 tB 00, 1l'06'00 CSH MMH1AC 0223/01 KJH/04.30/01 LAC 02 19.01 LAC RSD Std. Dev. MS/MSD RPD NA NA NA 5% 5% NA NA 4% 5% NA NA NA NA Cencentratien af EtFOSE-OH uf/mL or % Ree <LOQ (0.00977 ugmL) <LOQ (0.00977 ug'mL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) 32% 40% 38% 28% 32% 26% 39% 46% 46% 35% 28% 37% <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <I-OQ (0.00977 ugmL) LOQ (0.00977 ug'mL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00977 ugmL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ugmL) <I.OQ (0.00493 ugmL) 2nd 2nd 2nd 2nd 2nd 2nd EtFOSE-OH <LOQ <LOQ <LOQ 37% 29% 44% 33% <LOQ <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ug/mL) NA <LOQ (0.00493 ug/mL) 83.2 0.497 35.7 0.199 LOQ (0.00493 ug/mL) - LOQ (0.00493 ug/mL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ug/mL) LOQ (0.00493 ug/mL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) <LOQ (0.00493 ugmL) <LOQ(0.00977 ug/mL) <LOQ(0.00977 ugmL) LOQ(0.00977 ugmL) <LOQ(0.00977 ug/mL) <LOQ(0.00977 ugmL) <LOQ(0.00977 ugmL) LOQ(0.00977 ug/mL) <LOQ(0.00977 ugmL) <LOQ(0.00977 ug'mL) <LOQ(0.00977 ugmL) <LOQ <LOQ Analytical Report: FACT-TOX-001 L R N -U 2103 RSD Std. Dev. MS/MSD RPD NA NA NA 12% 4% 10% 3% 10% 4% 13% 4% NA NA NA NA NA NA NA Concentration af M556 ugm L ar % Ree < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ug'mL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOO (0.00494 ugmL) 127% -------------- 114% 135% NA NA 123% 2nd 124% 124% 133% NA NA 131% 2nd < LOQ (0.00494 ug'mL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ug'mL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) LOQ (0.00494 ugmL) L u v (U.W4<4 ugmL.) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ug/mL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ug'mL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) < LOQ (0.00494 ugmL) - LOQ (0.00494 ugmL) 0.344 0.376 0.189 0.294 0.424 0.429 0.341 0.286 0.436 . 0.594 0.441 0.694 0.521 0.403 0.167 0.418 0.408 0.476 ' 0.504 0.356 M556 <LOQ <LOQ <LOQ 125% 123% 127% 131% <LOQ 0.371 0.439 RSD Std. Dev. MS/MSD RPD NA NA NA 9% 11% NA NA 4% 5% NA NA NA NA NA 29.5 0.110 30.4 0.134 Cencentrition a f PFOSEA Uf/mL a r % Ree <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug'mL) LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) 70% 64% 46% NA 51% 31% 63% 76% 78% 63% NA NA <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ug'mL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) LOQ (0.00492 ugmL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ug/mL) LOQ (U.W494 ug'mL) <LOQ (0.00492 ugmL) LOQ (0.00492 ugmL) <LOQ (0.00492 ug'mL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ug'mL) <LOQ (0.00492 ug'mL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ug'mL) <LOQ (0.00492 ugmL) <LOQ (0.00492 ugmL) <LOQ (0.0492 ug/mL) <LOQ (0.0492 ugmL) <LOQ (0.0492 ugmL) <LOQ (0.0492 ugmL) <LOQ (0.0492 ug'mL) <LOQ (0.0492 ug/mL) <LOQ (0.0492 ug/mL) <LOQ (0.0492 ug/mL) <LOQ (0.0492 ug'mL) <LOQ (0.0492 ugmL) 2nd 2nd 2nd PFOSEA <LOQ <LOQ <LOO 63% <LOQ <LOO <LOQ RSD Std. Dev. MS/MSD RFD NA 21% 34% 11% NA NA NA NA NA NA NA NA 3MEnvironmental Laboratory Page 220 3M M edical D epartm ent Study: T6316.1 A jv u ii u y 3 y / .i Covance# 6329-212 Study: Product NumbeifTest Substance): Matrix: Method/Revision: Analytical Equipment System Number Instrument Software/Vereion: Filename: R-Squared Value: Slope: Y-Inlercept Dates of Extraction/Analyst Dates of Analysia'Analyst: Date o f Data Reduction'Analyst Sample Data WEEK 53 RAT SERA Dose Sample Group 3 Mid Dose 30.0 mg/kg Group 4 Mid-High Dose 100 mg/kg C90841M rooftxriM C90854M C90855M C90856M C90859M C90873M C90879M C90881M C90896M C91255F C91258F C9I264F C91269F C9I270F C91274F C91289F C9I294F C91297F C91305F C90902M C90908M C90914M C90918M C90923M C90926M C90927M C90934M C90936M C90944M C90946M C90950M C9095IM C90956M C90957M C91314F C91319F C91323F C91326F C91334F C91346F C91347F C91352F C91356F C91359F C91363F C91367F C91371F C91372F C91373F 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Elhyl Perfluorooclanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4 1& ETS-8-5.1 Amelia 062498, Soup 020199, Ruby 100699 Masslynx 3.3 & 3 4 See Below See Attachments See Attachments See Attachments 2 25/00 RWW 03/22 00,03'30 00, 04 10/00, 04/18,00,04/20/00, 0421/00, 05 0 00,05 30 00,08/18/00,08/21/00, 0823/00,02/27/01CSH/MMH/IAS 04 12/00,04.13/00, 04'19 00, 0420.'00,0 4 2 1'OO, 04 25/00, 05.03/00,05/31'00,0821/00,08 22'00, 0825/00,03/13/01 1AS/MMH/HOJ Extraetfoo VoL 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOS Std Correction Fa c to r 0.9275 0 9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.927 0.9275 PFOS Purity Correction Factor 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0 8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 PFOS Dilution Factor 100 too 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 IOOO IOOO 100 100 IOOO 100 IOOO IOOO 100 IU0O IOOO IOOO IOOO IOOO IOOO IOOO IOOO 100 100 PFOS Cene. ng/mL 208 256 330 179 222 306 341 45 151 214 701 342 368 491 142 442 475 363 480 392 880 697 680 837 777 613 751 464 640 761 750 330 274 614 911 218 917 274 184 824 167 395 395 164 174 154 354 228 698 951 Filena me D042100020 D042100021 D042100022 D042100023 D042100024 D042100028 D042100029 D042100030 D042100031 D042100032 D042100036 DO421O0O37 D042100038 D042100039 D042100040 D042100044 D042100045 D042100046 D042100047 D042100048 RD53000030 D042000015 D0420000I6 R053000033 D0420000I7 D042000018 D042000019 D042000023 D042000024 D042000025 D42000026 D081800023 D081800024 D042000027 R053000034 R053000023 D042100051 R053000016 R053000024 D042I00053 R0S3000025 R053000017 R053000018 R053000026 R053000039 R053000027 R053000019 R053000020 D042100045 R053000038 Concentration f PFOS PFOS ug/mL a r % Ree 16.7 20.5 26.4 14.3 17.8 24.5 27.3 3.58 12.1 17.2 18.0 56.2 27.4 29.5 39.3 11.4 35.4 38.1 29.1 38.5 31.4 33.6 70.5 55.8 54.5 67.1 62.3 49.1 60.2 37.2 51.3 60.9 60.1 264 220 49.2 73.0 82.4 175 73.5 220 148 66.0 134 . 317 317 132 139 123 284 183 55.9 76.2 163 PFOSA - Perfliinrooctonesulfonamide PFOSAA --Periluomoctanesulfonamidoacetate ElFOSF, - Narrow Range N-Ethyl Perfluoroootanesulfonamido ethyl alcohol M55*-C8FI7S02N((H)CH2C00) PFOSEA --Perfuorooclane sulfonyl ethylamide Corrected PFOS 1.00 (0 00492 ug ml.) to incl new LOQ is 0.00394 ug/mL. LAC02/19'01 * CCVs were ou t data may be biased low. Dale Entered/By: Dale Verified/ By: Purity Entered/Verified: 04/17 00,04.20/00. 04.24/0,0/425/00, 05/04/00,05/05'00, 06 01 00.09/01/00,09/18/00,11/06/00,03/07/01,0322/01 CSH/MMH/LAC 0223/01 KJH ' 0420/01 I.AC 02/19/01 LAC RSD Std. Dev. MS/MSD RPD 39.8 7.18 33.8 11.4 80.1 66.0 53.6 87.2 PFOSA Purity Correction F a c to r Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown TInlrnnwn Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA . NA - NA NA NA NA NA NA NA NA ? NA NA NA NA NA NA NA NA NA NA NA NA Analytical Report: FACT-TOX-001 L R N -U 2103 PFOSA Dilution Factor I 1 1 1 1 l 1 1 1 1 1 1 10 10 1 1 1 1 10 10 10 1 10 10 10 10 10 PFOSA Cone. ug/mL 201 209 338 293 181 231 252 125 180 365 393 268 324 489 485 404 279 283 415 323 615 275 382 662 305 223 363 247 331 270 231 474 343 203 430 105 120 305 517 746 577 112 109 203 637 103 159 224 106 125 Filena roe R041000104 R041000105 R041000106 R041000107 R041000108 R041000112 R041000113 R041000114 R041000115 R041000116 D03300087 D03300088 D03300089 D03300090 D03300091 D03300094 D03300095 D03300096 D03300097 D03300098 D03300101 D03300102 D03300103 D03300104 D03300105 D03300108 D03300109 D03300110 D033001I1 D03300112 D03300115 D03300116 D03300117 DQ3300118 D03300119 D042000047 D042000048 D033000105 A041800068 A041800069 A04IROOO70 D010227020 D010227021 D042000055 A041800075 D042000057 D010227022 D010227023 19042000058 D042000059 Concentration of PFOSA ug/mL or % Rec 0.201 0.209 0.338 0.293 0.181 0.231 0.252 0.125 0.180 0.365 0,393 0.268 0.324 0.489 0.485 0.404 0.279 0.283 0.323 0.615 0.275 0.382 0.662 0.305 0.223 0.363 0.247 0.331 0.270 0.231 0.343 0.203 0.430 1.05 1.20 0.305 0.517 0.746 0 477 1.12 1.09 2.03 0.637 1.59 2.24 1.25 PFOSA ug/mL RSD Std. Dev. MS/MSD RPD 0.237 31.6 0.0751 0.366 0.0824 0.357 1.10 0.536 3MEnvironmental Laboratory Page 221 3M M edical D epartm ent Study: T6316.1 AiviuifF uyoy/.i Covante# 6329-212 Study: Product Numbet(Tesl Substance): Matrix: Method/Revision: Analytical Equipment System Number Instrument Software/Version: Filename R-Squared Value: Slope: Y-Intetcept Dates of Extraction/Analyst: Dates o f Analysis/Analyst: 104 Week Dietary Carcinogenicity Study with Narrow Range (98. I S ) N-Ethyl Periluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 & ETS-8-5.1 Amelia 062498, Soup 020199, Ruby 100699 Masslyux 3.3 & 3.4 See Below See Attachments See Attachments See Attachments 2/25/00 RWW 03/22/00,03 30/00,04 10/00,04/18 00,04 20/00, 04/21'00, 05/01/00,0530/00,08/18/00, 08/21/00, 08/23/00,02/27/01 CSH/MMH/IAS Date of Data Reduction Analyst: 04'12/00,04 13/00,04 19 00.04 20'00,04-21'00, 04 25 00, 05 03'00,0531/00,0821/00,0822/00, 0825/00, 03/13/01 IAS/MMR/HOJ Sample Data W E E K 53 RA T SER A ioiT.712!.l ________________________________________________________________________ lot Unknown/SD013 Gruup Dose Group 3 Mid Dose 30.0 mg/kg Group 4 Mid-High Dose 100 mg/kg Sample * C90841M C90RS0M C90854M C90855M C90856M C908S9M C90873M C90879M C90881M C90896M C91255F C9I258F C91264F C91269F C91270F C91274F C91289F C91294F C91297F C91305F C90902M C90908M C90914M C909I8M C90923M C90926M C90927M C90934M C90936M C90944M C90946M C90950M C9095IM C90956M C90957M C9I314F C9I319F C9I323F C91326F C91334F C9I346F C91347F C91352F C91356F C91359F C91363F C9I367F C91371F C91372F C91373F PFOSAA Purity Correction Factor Unknown Unknown Unknown TTnlrfmwn Unknown Unknown Unknown Unknown Unknown Unknown Unknown t Inlrnown Unknown Unknown Unknown 1'nVnnwn Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown 1InVnnwn Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA KA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOSAA Dilution F a c to r 10 10 10 to 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 100 10 10 100 10 10 10 10 10 10 10 100 100 10 100 10 10 100 10 10 10 100 100 too 10 10 too 100 10 10 PFOSAA Cone. Filename 431 323 749 600 321 419 621 417 235 682 678 306 317 508 457 430 310 347 435 431 227 527.9 590.7 152 738 502.6 596.2 468.3 532.2 511.9 492.5 220 118 396.0 99.4 837 702 201 647 655 672 152 215 223 825 818 230 197 978 958 A042100052 A042100053 A042100054 A042100055 A042100056 A042100060 A042100061 A042100062 A042100063 A042I00064 A042100068 A042100069 A042100070 A042I00071 A042100072 A04200076 A042100077 A042100078 A042100079 A042I00080 D082100023 D04200003I D042000032 D082100027 D042000033 D042000034 D042000035 D042000039 D042000040 D042000041 D042000042 D082100028 D082100029 D042000043 D082100030 D042000047 D042000048 D082300020 D042000049 D042000050 D042000051 D08230002I D082300022 D082100031 D042000056 D042000057 D082300023 DO82300024 D042000058 D042000059 Concentration of PFOSAA ug/mL o r % Ree 4.31 3.23 7.49 6.00 3.21 4.19 6.21 4.17 2.35 6.82 6.78 3.06 3.17 5.08 4.57 4.30 3.10 3.47 4.35 4.31 22.7 5.28 5.91 15.2 7.4 5.03 5.96 4.68 5.32 5.12 4.92 22.0 11.8 3.96 994 837 7.02 20.1 6.47 6.55 6.72 15.2 21.5 22.3 8.25 8.18 23.0 19.7 9.78 9.58 PFOSAA RSD Std. Dev. MS/MSD RPD 35.9 4.80 1.72 27.0 4.22 1.14 69.2 9.0 6.23 51.3 12.8 6.59 EtFOSE-OH Purity Correction Fa c to r Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown PFOS = Periluorooclanesulfonate PFOSA = Perfluorooctanesulfonamide + Recovery confirmed high with 08/21/00 analysis. LAC 09/18/00 Corrected PFOS LOO (0.00492 un'ml.) to include 'hi correction factors PFOSAA = Periluorooctanesulfonamidoacetate EtFOSE 3 Narrow Range N-Ethyl Periluorooctanesulfonamido ethyl alcohol new LOQ is 0.00394 ug/mL. LAC 02/19/01 * CCVs were out data may be biased low. M556 = C8F17S02N((H)CH2C00) PFOSEA - Perfuorooctane sulfonyl ethylamide Date Entered/By: Date Verified/By: Purity Entered/Verified: 04.17 00, 04.20 00, 04.24,0, 0 4 25 00, 05'04'00,05'05 00, 06/01/00, 09 01/00,09/18 (>0, 11 06/00, 03/07'01.03/22/01 CSH/MMH/LAC 02/23/01 KJH / 04 3001 LAC . 02 19/01 LAC Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA ? NA NA NA NA NA NA NA NA NA NA NA NA Analytical Report: FACT-TOX-001 L R N -U 2103 EtFOSE-OH Dilution Factor 1 t 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 EtFOSE-OH Cone. 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 24.1 0.00 26.6 0.00 22.9 23.7 23.1 24.5 22.0 32.8 31.8 27.4 31.2 23.5 24.0 23.7 29.0 28.1 31.6 25.6 3.77 14.6 10.1 7.15 6.10 18.1 22.7 24.0 12.5 20.8 15.7 28.3 23.6 39.6 14.4 13.4 36.9 40.7 15.6 15.7 Filename R041000104 R.041001D5 R041000106 R041000107 R041000108 R041000112 R041000113 R0410001I4 R041000115 R041000116 D03300087 D03300088 D03300089 D03300090 D0330009I D03300094 D03300095 D03300096 D03300097 D03300098 D0330010I D03300102 D03300103 D03300104 D03300105 D03300108 D03300109 D03300IIO D03300111 D03300112 A041800058 A04I800059 A041800060 A041800061 A041800062 A041800066 A041800067 D033000105 A041800068 A041800069 A041800070 D010227027 D010227028 A 0 4 1800074 A 0 4 1800075 A 0 4 1800076 D010227029 D010227030 A 0 4 1800077 A04I800078 Concentration of EtFOSE-OH ug/m Lor % Ree <-LOQ(0.00977 ug/mL) 'LOQ(0.00977 ug'niL) * <LOQ(0.00977 ug/mL) <LOQ(0.00977 ug/mL) <LOQ(0.00977 ug/mL) * <LOQ(0.00977 ug/mL) * <LOQ(0.00977 ug/mL) * <LOQ(0.00977 ug/mL) * <LOQ(0.00977 ug/mL) * <LOQ(0.00977 uE/mL) * <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) 0.0266 <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) 0.0328 0.0318 0.0274 0.0312 <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/tnL) <LOQ (0.0248 ug/mL) 0.0290 0.0281 0.0316 0.0256 <LOQ (0.00493 ug/mL) 0.0146 0.0101 0.00715 0.00610 0.0181 0.0227 <LOQ (0.0248 ug/mL) 0.0125 0.0208 00147 0.0283 0.0236 0.0396 0.0144 0.0184 0.0369 0.0407 0.0156 0.0157 EtFOSE-OH <LOO 0.0258 0.0215 0.0231 RSD Std. Dev. MS/MSD RPD NA NA 9.76 0.00252 46.2 0.00992 41.7 0.00963 3M Environmental Laboratory Page 222 3M M edical D epartm ent Study: T6316.1 A M D T # UyZ5y7.1 Covance# 6329-212 Study: Product NumbeifTest Substance): Matrix: Melhod'Revision: Analytical Equipment System Number Instrument Software/Venion: Filename: R-Squared Value: Slope: 104 Week Dietary Carcinogenicity Study with Narrow Range (98.I%)N-Ethyl ftrfluorooclanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 &ETS-8-5.1 Amelia 062498, Soup 020199, Ruby 100699 Masstynx 3.3 & 3.4 See Below See Attachments See Attachments Y-Inlercept Dales of Extraction/Analyst See Attachments 2-25/00 RWW Dales of Analysis/Analyst Dale o f Data Reducbon/Analyst: 03/22/00, 03-30/00,04/10/00,04/18/00,04/20/00, 04/21/00,05 01.00,05/3000,08 1800, 08/21 '00, 08/23/00,02/27/01 CSK'MMH/IAS 04/12 00, 04 13 00,04/19 00,04,70 00,0431/00, 04/25/00,05'03-00,05/31 00,08/21/00, 08/2200, 08/25/00,03/13/01 IA&'MMH/HOJ Sample Data W E E K S3 R A T SERA IoiNBll3047.80 _ _____________________ _________________________________________________ lot 529 Duse Sample # M556 Purity Correction Fa c to r Surrogate Verified M554 Dilution Factor M554 Cane. F ilen a me Concentra lian ofM 5 ug/mL o r % Ree MSS RSD Std. Dev. MS/MSD RTD PFOSEA Purity Correction Fa c to r Group 3 Mid Dose 30.0 mg/ltg C90841M C90850M C90854M C90855M C90856M C90859M C90873M C90879M C90881M C90896M C9125F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA 10 517 A042100052 5.17 10 356 A042100053 3.56 10 529 A042100054 5.29 10 346 A042100055 3.46 10 417 A042100056 4.17 10 528 A042100060 5.28 10 357 A042100061 3.57 10 242 A042100062 2.42 10 381 A042100063 3.81 10 324 A042100064 3.24 10 407 A042100068 4.07 24.3 4.00 0.970 Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown C91258F C91264F C91269F Unknown Unknown Unknown NA NA NA 10 264 A042100069 2.64 10 391 A042100070 3.91 10 $45 A04210OO71 5.45 Unknown Unknown Unknown C91270F C91274F C9I289F C91294F C91297F C91305F Unknown Unknown Unknown Unknown I TnVnown Unknown NA NA NA NA NA NA 10 468 A042100072 4.68 10 396 A042100076 3.96 10 321 A042100077 3.21 10 425 A042100078 4.25 10 430 A042100079 4.30 10 451 A042100080 4.51 18.8 4.10 0.771 Unknown Unknown Unknown Unknown Unknown Unknown Group 4 C90902M Unknown NA 100 224 D082100024 22.4 Unknown Mid-High Dose 100 mg/kg C90908M C90914M C90918M C90923M C90926M Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA 10 761 D042000031 7.6 10 877 42000032 8.8 urn 201 D08210027 20.1 10 604 D042000033 6.0 10 579.9 D042000034 5.80 Unknown Unknown Unknown Unknown Unknown C90927M C90934M C90936M Unknown Unknown Unknown NA NA NA 10 901 D042000035 9,0 10 787 D042000039 7.9 10 624.6 D042000040 6.25 Unknown Unknown Unknown C90944M C90946M C90950M C90951M C90956M Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA 10 10 100 100 10 762 32.7 149 164 645.7 D042000041 D042000042 DO82100028 DO82100029 D042000043 7.6 5.33 14.9 16.4 6.46 Unknown Unknown Unknown Unknown 52.7 Unknown C909S7M C91314F C91319F C91323F C91326F C91334F . C91346F C91347F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA 100 116 DO82100030 11.6 10 697 D042000047 6.97 10 761 D042000048 7.6! 100 198 D082300020 19.8 10 574 D042000049 5.74 10 927 D042000050 9.27 10 648 D042000051 6.48 100 147 D082300021 14.7 10.4 5.48 Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown C91352F C91356F C91359F Unknown Unknown Unknown NA NA NA 100 178 D082300022 17.8 100 258 D082t00031 25.8 10 708 D042000056 7.08 Unknown Unknown Unknown C91363F C91367F C91371F C91372F 91373F Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA 10 835 D042000057 8.35 100 176 82300023 17.6 100 251 D082300024 25.1 10 901 D042000058 9.01 !0 723 DQ4200059 7.23 55.5 12.6 6.98 Unknown Unknown Unknown Unknown Unknown PFOS = Pcrfluorooclenesuifonale + Recovery confirmed high with 08,21/00 analysis. LAC09/18/00 PFOSA = Perfluorooctanesulfonamide Corrected PFOS LOQ (0.00492 ug mL) to include sld correction factors PFOSAA = Periluorooctanesulfonamidoacetate new LOQ is 0.00394 ug/mL LAC 02/19/01 ElFOSE = Narrow Range N-Ethyl Perfluorooclanesulfonamido ethyl alcohol * CCVs were o u t data may be biased low. M556 =C8F17S02N((H)CH2C00) PFOSEA = Perfuorooctane sulfonyl elhylamide Date Entered/By: DBte Verified' By: Purity Entered/Verified: 04.17/00, 04 20/00, 04/24/0, 0 4/25/00,05 04/00, 05 05 00,06 01/00, 09/01'00, 09/18 00,11 06'00,03/07/01,03,'2201 CSH/MMH/LAC 0223/01 KJH ' 0430/01 LAC 0219/01 LAC Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Analytical Report: FACT-TOX-001 L R N -U 2103 PFOSEA Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 I 1 I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 I 1 I 1 I PFOSEA Cone. 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 17.8 0.00 0.00 13.1 0.00 0.00 0.00 0.00 0.00 0.00 15.0 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 2.52 0.00 0.00 0.00 5.60 0.00 0.00 0.00 Filena me R04100104 R04100105 R04100106 R04100107 R04I00108 R04100112 R04100113 R04100114 R04I00115 R04100116 D03300087 D03300088 D03300089 D03300090 D03300091 D03300094 D03300095 D03300096 D03300097 D03300098 D03300101 D03300102 D03300103 D03300104 D03300105 D03300108 D03300I09 D03300I10 3300111 D03300112 A041800058 A041800059 A 0 4 1800060 A 0 4 1800061 A 0 4 1800062 A 0 4 1800066 A041800067 D03300105 A041800068 A 0 4 1800069 A 0 4 1800070 D010227027 D010227028 A 0 4 1800074 A041800075 A 0 4 1800076 10227029 D010227030 A041800077 A041800078 Concentration of PFOSEA ug/mL or % Ree LOQ (0.0492 ug/mL) LOQ (0.0492 ug'mL) LOQ (0.0492 ug'mL) LOQ (0.0492 ug'mL) LOQ (0.0492 ug/mL) LOQ (0.0492 ug'mL) LOQ (0.0492 ug/mL) LOQ (0.0492 ug'mL) LOQ (0.0492 ug/mL) LOO (0.0492 ug'mL) LOQ (0.0247 ug/mL) LOQ (0.0247 ug/mL) LOQ (0.0247 ug/mL) LOQ (0.0247 ug/mL) LOQ (0.0247 ug/mL) LOQ (0.0247 ug/mL) LOQ (0.0247 ug/mL) LOQ (0.0247 ug/mL) LOQ (0.0247 ug/mL) LOQ (0.0247 ug/mL) LOQ (0.0247 ug/mL) LOQ (0.0247 ug/mL) LOQ (0.0247 ug/mL) LOQ (0.0247 ug'mL) LOQ (0.0247 ug/mL) LOQ (0.0247 ug/mL) LOQ (0.0247 ug'mL) LOQ (0.0247 ug'mL) LOQ (0.0247 ug/mL) LOQ (0.0247 ug/mL) LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug'mL) <LOQ (0.00492 ug'mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) LOQ (0.00492 ug'mL) <LOQ (0.0247 ug'mL) <LOQ (0.00492 ug'mL) <LOQ (0.00492 ug'mL) <LOQ (0.00492 ug'mL) <LOQ (0.00999 ug'mL) <LOQ (0.00999 ug/mL) <LOQ (0.00492 ug/mL) LOQ (0.00492 ug'mL) <LOQ (0.00492 ug'mL) <LOQ (0.00999 ug/mL) <LOQ (0.00999 ug/tnL) <LOQ (0.00492 ug/mL) LOQ (0.00492 ugmL) PFOSEA RSD Std. Dev. MS/MSD RPD <LOQ NA NA <LOQ NA NA <LOQ NA NA LOQ NA NA 3MEnvironmental Laboratory Page 223 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Study: ProductNumber(Tesl Substance): 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Fferiluorooclanesulfonamklo Ethanol in Rats T-6316 (EtFOSE-OH) Method-Revision: Analytical Equipment System Number Instrument Software-Version: Filename: R-Squared Value: Slope: Y-Intercept Dates o f Extraction/Analyst: Dates of Analysis'Analyst: Date ofData Reduction-Analyst Rat Serum ETS-8-4.1 & ETS-8-5.1 Amelia 062498, Soup 020199, Ruby 100699 Masslynx 3.3 & 3.4 See Attachments See Attachments See Attachments See Attachments 2.-75/00 RWW ' 0372-00, 0370/00, 04/10/00,04.18 00,04 20.00,04 21-00,05 01 00,05/30/00, 08 18/00, 0821/00,08/23/00,0727/01 CSH-MMH/IAS 04 12 00, 04/13/00, 04/19'00, 04-20/00,0421/00,04 25/00, 05'03'00, 05-31/00, 0821/00, 0822/00, 0825 00,03/13/01 IAS/MMH/HOJ Sample Data W EEK 53 RAT SERA Group Date Group 3 Mid Dose 30.0 mg/kg S a m p le # C90841M C90850M C90854M C90855M C90856M C90859M C90873M C90879M C90881M C90896M C91255F C91258F C91264F C91269F C91270F C91274F C91289F C91294F C91297F C91305F Concen tra tien f PFOS ug/mL a r % Ree 16.7 20.5 26.4 14.3 L7.8 24.5 27.3 3.58 12 1 17.2 56.2 27.4 29.5 39.3 11.4 35.4 38.1 29.1 38.5 31.4 Mean PFOS ug/mL 18.0 33.6 RSD Std. Dev. MS/MSD RPD 39.8 7.18 33.8 11.4 Concentration of PFOSA ug/mL or % Ree 0.201 0.209 0.338 0.293 0.181 0.231 0.252 0.125 0.180 0.365 0.393 0.268 0.324 0.489 0.485 0.404 0.279 0.283 0.415 0.323 Mean PFOSA ug/mL RSD Std. Dev. MS/MSD RPD 0.237 31.6 0.0751 0.366 22.5 0.0824 Concentratlan f PFOSAA ug/mL ar % Ree 4.31 3.23 7.49 6.00 3.21 4.19 6.21 4.17 2.35 6.82 6.78 3.06 3.17 5.08 4.57 4.30 3.10 3.47 4.35 4.31 Graup 4 Mid-High Dose 100 mg/kg C90902M C90908M C90914M C90918M C90923M C90926M C90927M C90934M C90936M - C90944M C90946M C90950M C9091M C90956M C90957M C913I4F C913I9F C91323F C91326F C91334F C91346F C91347F C91352F C91356F C91359F C91363F C91367F C91371F C91372F CPn^SF 70.5 0.615 22.7 55.8 0.275 5.28 54.5 0.382 5.91 67.1 0.662 15.2 62.3 0.305 7.4 49.1 0.223 5.03 60.2 0.363 5.96 37.2 0.247 4.68 51.3 0.331 5.32 60.9 0.270 5.12 60.1 0.231 4.92 264 0.474 22.0 220 0.343 11.8 49.2 80.1 0.203 38.7 3.96 73.0 82.4 66.0 0.430 0.357 0.138 9.94 175 1.05 8.37 73.5 1.20 7.02 220 0.31 20.1 148 0.517 6.47 66.0 0.746 6.55 134 . 0.577 6.72 317 1.12 15.2 317 1.09 21.5 132 2.03 22.3 t39 0.637 8.25 123 1.03 8.18 284 1.59 23.0 183 2.24 19.7 55.9 53.6 1.06 48.9 9.78 76.2 163 87.2 1.25 1.095 0.536 9.58 PFOS = Pertluorooctanesullonate PFOSA - Periluorooctanesulfonamide PFOSAA - PerfluorooctanesulIbnamidoBcelale + Recovery confirmed high with 08-21/00 analysis. LAC 09/18/00 Corrected PFUS LOQ (0.00492 ug'mL) to include std correction (actors new LOQ is 0.00394 ug/mL LAC 02/19/01 EtFOSE = Narrow Range N-Ethyl Perfiuorooctanesulfonamido ethyl alcohol * CCVs were o u t data may be biased low. MJ56 = C8F17S02N((H)CH2C00) PFOSEA = Perfuorooctane sulfonyl ethylamide Date Entered/By: Date Verified/ By: Purity EnteiedVerified: 04/17'00, 0420/00, 0424/0, 0.4 25/00, 05 04'00,05 05-00, 06 Ot-'OO, 09-01/00, 09 18/00,11.06/00,03/07-01,03/22 01 CSH MMH'LAC 0223/01 KJH/0470/01 LAC . 02/19/01 LAC Mean PFOSAA ug/mL 4.80 4.22 9.0 RSD Std. Dev. MS/MSD RPD 35.9 1.72 27.0 1.14 69.2 6.23 51.3 6.5S Concentration af EtFOSE-OH ug/mL a r % Ree <LOQ(0.00977 ug/mL) <LOQ(0.00977 ug/mL) <LOQ(0.00977 ug/mL) <LOQ(0.00977 ug/mL) <LOQ(0.00977 ug/mL) <LOQ(0.00977 ug/mL) <LOQ(0.009?7 ug/mL) <LOQ(0.00977 ug/mL) <LOQ(0.00977 ug/mL) <LOQ(0.00977 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug'mL) 0.0266 <LOQ (0.0248 ug'mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) 0.0328 0.0318 0.0274 0.0312 <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug'mL) <LOQ (0.0248 ug/mL) 0.0290 0.0281 0.0316 0.0256 <LOQ (0.00493 ug/mL) 0.0146 0.0101 0.0072 0.0061 0.0181 0.0227 <LOQ (0.0248 ug/mL) 0.0125 0.0208 0.0157 0.0283 0.0236 0.0396 0.0144 0.0184 0.0369 0.0407 0.0156 0.0157 * * * * * * Mean EtFOSE-OH ug/mL <LOO 0.0258 0.0215 0.0231 RSD Std. Dev. MS/MSD RPD NA NA 9.76 0.00252 46.2 0.00992 41.7 u.mnro Analytical Report: FACT-TOX-001 LRN-U2103 Concentration a f M556 ug/mL a r % Ree 5.17 3.56 5.29 3.46 4.17 5.28 3.57 2.42 3.81 3.24 4.07 2.64 3.91 5.45 4.68 3.96 3.21 4.25 4.30 4.51 22.4 7.6 8.8 20.1 6.0 5.80 9.0 7.9 6.25 7.6 5.33 14.9 16.4 6.46 116 6.97 7.61 19.3 5.74 9.27 6.48 14.7 17.8 25.8 7.08 8.35 17.6 25.1 9.01 7.23 Mean M556 ug/mL 4.00 4.10 10.4 14.6 RSD Std. Dev. MS/MSD RPD 24.3 0.970 18.8 0.771 52.7 5.48 55.5 6.98 Cencentratton of PFOSEA ug/mL or % Ree <LOQ (0.0492 ug/mL) <LOQ (0.0492 ug'mL) <LOQ (0.0492 ug/mL) <LOQ (0.0492 ug/mL) <LOQ (0.0492 ug/mL) <LOQ (0.0492 ug/mL) <LOQ (0.0492 ug/mL) <LOQ (0.0492 ug/mL) <LOQ (0.0492 ug/mL) <LOQ (0.0492 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug'mL) <LOQ (0.0247 ug/mL) <LOQ (0.0247 ug/mL) <I.OQ (0.0247 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ue/mU <LOQ (0.00492 ug'mL) <LOQ (0.00492 ug'mL) <LOQ (0.0247 ugmL) <LOQ (0.00492 ug'mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ugmL) <LOQ (0.00999 ug'mL) <LOQ (0.00999 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug'mL) <LOQ (0.00492 ug/mL) <LOQ (0.00999 ug/mL) <LOQ (0.00999 ug/mL) <LOQ (0.00492 ug'mL) <LOy (0.00492 ug'mL) Mean PFOSEA ug/mL RSD Std. Dev. MS/MSD RPD <LO0 NA NA <LOQ NA NA <LOQ NA NA <LOQ NA NA 3MEnvironmental Laboratory Page 224 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product Number(Test Substance): Method/Re vision: Analytical Equipment System Number Instrument Software/Version: Filename: R-Squaied Value: Slope: Y-Intercept: Dates o f Extraction/Analyst Dates o f Analysis/Analyst: Dale of Data Reduction/Analyst Sample D ita 104 Week Dietary Carcinogenicity Study with Narrow Range <98.1%) N-Elhyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 & ETS-8-5.1 Amelia 062498, Davey 070799 Masslynx 3.3 & 3.4 See Attachments See Attachments See Attachments 02/07/00,02/08/00,02/09/00 SAL/RWW 02/18/00,03/13/00,4/18/00,4/19/00,06/19/00,06/20/00,08/16/00,08/23/00 MMH/IAS/CSH 02/21/00,03/16/00,4/19/00,4/20/00,06/20/00,06/21/00,08/18/00,08/25/00,04/11/01 MMH/IAS/HOJ Bex 00-009 WEEK 105 RAT SERA____________________________________ lot 171 G ro up Dose Method Blk Matrix Blk QC-250 ppb Group 1 Control 0.0 mg/kg Group 1 Control 0.0 mg/kg Sample # 020700-H20 Btk-5 020700-H20 Blk-6 0208(H)-H20 Blk-I 020800-H20 Blk-2 020900-H20 Blk-5 020900-H20 Blk-6 020700-RBS Blk-5 020700-RBS Blk-6 020800-RBS Blk-1 020800-RBS-Blk-2 020800-RTS Blk-1 020800-RTS-Blk-2 020900-RBS Blk-5 020900-RBS-Blk-6 020900-RTS Blk-5 020900-RTS-Blk-6 020700-RTS-MS-5 020700-RTS-MSD-5 020700-RTS-MS-5 020700-RTS-MSD-5 020700-RTS-MS-6 020700-RTS-MSD-6 0207(KI-RTS-MS-6 0207fH)-RTS-MSD-6 020800-RTS-MS-1 020800-RTS- MSD-1 020800-RTS-MS-1 020800-RTS-MSD-1 020800-RTS-MS-2 020800-RTS-MSD-2 0208(H)-RTS-MS-2 020800-RTS-MSD-2 C90778M-MS-5 C90778M-MSD-6 020900-RTS-MS-5 020900-RTS-MSD-6 020900-RTS-MS-5 020900-RTS-MSD-6 C90712M C907I6M C90722M C90724M C90726M C90728M C90735M C90742M C90743M C90747M C90750M C90758M C90765M C90778M C9I127F C91131F C9I138F C91144F C9I148F C91157F C91159F C91166F C91172F C91176F C91I83F C91188F C91190F Extraction VoL 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 J 1 1 1 1 1 1 1 1 Surrogate Verified NA NA NA NA NA NA NA NA X NA X NA NA NA NA Confirmed Hieh NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOS Std Correction Factor 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0 .9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 PFOS Purity Correction Factor 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA 0.8640 0.8640 0.8640 0.864 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 PFOS Dilution Factor 1 1 1 1 I 1 1 1 1 1 1 1 1 1 1 1 1 1 NA NA 1 1 NA NA 1 1 NA NA 1 NA NA 4 1 1 NA NA 1 1 1 1 1 1 1 1 1 l l I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 PFOS Cone. ng/mL 0.00 0.00 0(H) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.760 0.230 0.00 0.(H) 0.00 0.00 300 3(H) NA NA 297 249 NA NA 198 206 NA NA 2(H) 190 NA NA 343 345 239 249 NA NA 3.62 0.00 8.49 14.5 3.36 16.4 2.65 5.40 1.48 8.06 62.9 2.53 1.01 13.4 51.6 42.7 11.9 108 27.0 21.4 41.5 21.4 10.8 0.00 23.6 69.9 0.00 Filename D082300049 D082300050 D081600020 D03I500025 A062000005 A062000019 D082300051 D082300052 A031500006 D031500026 A031500007 D031500027 A062000006 A062000020 A062000007 A062IHHHI2I A022600017 A022600018 NA NA A0226000I9 A022600020 NA NA A021800017 D081600027 NA NA A021800018 D081600023 NA NA A062000054 A062000055 A201800019 A021800020 NA NA D03IS00G43 DO315O0O57 D031500058 A021800039 D031500044 A021800040 D031500061 D0315Q0064 D031500045 D03I500065 A021800026 D03I500047 D031500066 A02I80Q058 A021800047 A 0 2 I 800048 A021800059 A021800030 A021800051 A021800031 A021800052 A021800032 A021800053 D031500074 A021800055 A021800033 D031500054 Concentration of PFOS ug/mL or % Ree <LCQ (0.00394 ug/mL) <LCQ (0.00394 ue/mL) <LCQ (0.00394 ug/mL) <LCO (0.00394 ug/mL) <LCQ (0.00394 ug/mL) <LOO (0.00394 ue/mL) <LCQ (0.00394 ug/mL) <LOO (0.00394 ue/mL) <L0Q (0.00394 ug/mL) <LCQ (0.00394 ue/mL) <LOQ (0.00394 ug/mL) <LOQ (0.00394 ue/mL) 0.00 0.00 0.00 0.00 12m 12m NA NA 120% . io m NA NA 80% 83% NA NA 81% 77% NA NA 72% 73% 97% 101% NA NA <LOQ((MH)394 ug/mL) <LOQ (0.00394 ug/mL) 0.00680 0.0116 cLOQ (0.00394 ug/mL) 0.0131 <IX>3 (0.(H)394 Ug/mL) O.IH1433 <LOQ (0.IH1394 ug/mL) 0.00646 0.0504 <LOQ (0.00394 ug/mL) <LOQ (0.00394 ug/mL) 0.0107 0.0413 0.0342 0.00951 0.0868 0.0217 0.0171 0.0333 0.0171 0.00865 <1.03 (0.00394 ug/mL) .0189 0.0560 <LOQ (0.00394 Ug/mL) Group 2 C90781M 1 NA 0.9275 0.8640 Low Dose 3.00 mg/lcg C90782M C90783M C90785M 1 1 1 NA 0.9275 0.8640 NA 0.9275 0.8640 NA 0.9275 0.8640 C90787M 1 NA 0.9275 0.8640 C90788M 1 NA 0.9275 0.8640 C90791M 1 NA 0.9275 0.R640 C90794M 1 NA 0.9275 0.8640 C90799M 1 NA 0.9275 0.8640 C90804M 1 NA 0.9275 0.8640 C90809M 1 NA 0.9275 0.8640 C90810M 1 NA 0.9275 0.8640 C9081IM 1 NA 0.9275 0.8640 C90812M 1 NA 0.9275 0.8640 C90815M 1 NA 0.9275 0.8640 C90823M 1 NA 0.9275 0.8640 C90829M 1 NA 0.9275 0.8640 C90830M 1 NA 0.9275 0.8640 C90832M 1 NA 0.9275 0.8640 C90835M 1 NA 0.9275 0.8640 C90838M 1 NA 0.9275 0.8640 C90840M 1 NA 0.9275 0.8640 Group 2 C91197F 1 NA 0.9275 0.8640 Low Dose C91201F 1 NA 0.9275 0.8640 3.00 mg/kg C9I207F 1 NA 0.9275 0.8640 C9I2I6F 1 E E 0.8640 C91220F 1 NA 0.9275 0.8640 C91221F 1 NA 0.9275 0.8640 C91227F 1 NA 0.9275 0.8640 C91232F 1 NA 0.9275 0.8640 C91235F 1 NA 0.9275 0.8640 C91236F t NA 0.9275 0.8640 C91242F 1 NA 0.9275 0.8640 C91243F 1 NA 0.9275 0.8640 A= CCVs analyzed bracketing these data were within criteria but had peak areas slightly above the valid linear range. LAC 03/03/01 E = Lost during extraction, no sample remaining to reextract. 1 1 to 1 10 10 15 10 1 1 15 1 1 1 1 10 10 50 10 10 1 1 10 10 15 E IS 10 50 15 80 50 10 10 102 A021800081 506 A021800060 IS9 A031500027 83.0 A021800064 158 A031500028 460 A03I500029 157 A031500026 273 A031500033 627 A021800082 398 A021800067 382 A031500023 177 A021800068 379 A021800085 218 A021800086 408 A021800087 108 A031500035 177 A031500036 114 R041800049 109 A031500040 36.6 A031500041 229 A021800074 268 A02I800089 198 A031500042 187 A03I500043 49 A031500022 EE 401 A031500021 119 A03I500048 103 R041800051 384 A031500020 156 R041800050 92.3 R041800052 372 A031500055 141 A031500056 0.0819 0.405 1.52 0.0665 1.26 3.69 1.89 2.19 0.502 0.319 4.59 0.142 0.304 0.175 0.327 0.864 1.42 4.56 0.872 0.293 0.184 0.215 1.59 1.50 5.89 E 4.82 0.955 4.12 462 9.98 3.70 2.98 1.13 . PFOS = Perfluorooctanesulfonate Corrected PFOS LOQ (0.00492 ug/mL) to include std correction factors PFOSA - Perfluorooctanesulfonamide new LOQ is 0.00394 ug/mL LAC 02/19/01 PFOSAA * Perfluorooctanesulfonamidoacelale EtFOSE " Narrow Range N-Elhyl Perfluorooctanesulfonamido ethyl alcohol M556 -C8F17S02N((H)CH2C00) PFOSEA Perfuorooclane sulfonyl elhylamide Dale Entered/By: Date Verified/By: Purity Entered/Verified: 03/06/tM), 03/I0AH), 03/20/00, 03/21/00, 4/17/00, 5/16/00,06/22/00,06/23/00, 06/26/00,09/05/00,10/17/00, 04/13/01 LAC/CSH 4/17/01 mmh 4/30/01 hoj /04/30/01 LAC 02/19/01 LAC PFOS ug/mL <LOO <LOO <LOO <LOO <LOO <LOQ <LOQ <LQ 121% NA 110% NA 82% NA 79% NA 72% 99% NA 0.(H)936 0.0271 1.18 3.75 RSD Std. Dev. MS/MSD RPD NA NA NA NA NA NA NA NA 0% NA 17% NA 4% NA 5% NA 1% 4% NA 131 0.0123 87.2 0.0237 120 1.41 70.7 2.65 3MEnvironmental Laboratory Page 225 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product Numbei(Test Substance): Matrix: Method/Revision: 104 Week Dietaiy Carcinogenicity Study with Natrow Range (98.1 /.) N-Elhyl Perfluorooctanesulfonamido Ethanol in T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 & ETS-8-5.1 Analytical Equipment System Number Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Inlercept: Amelia 062498, Davey 070799 Masslynx 3.3 & 3.4 See Below See Attachments See Attachments See Attachments Dales of Extraction/Analyst Dales of Analysis/Analyst Date of Data Reduction/Analyst 02/07/00,02/08/00,02/09/00 SAL/RWW 02/18/00, 03/15/00, 4/18/00, 4/19/00,06/19/00, 06/20/00,08/16/00,08/23/00 MMH/IAS/CSH 02/21/00,03/16/00,4/19/00,4/20/00,06/20/00,06/21/00,08/18/00,08/25/00,04/11/01 MMH/IAS/HOJ Sample Data Box 00-009 WEEK 105 RAT SERA lolL-15709 Group Dose S a m p le # PFOSA Purity CorrectloD Facter Surrogate Verified PFOSA Dilution Feeler PFOSA Cene. ng/mL Filename Concentration of PFOSA ug/mL or % Ree Method Blk Matrix Blk QC-250ppb 020700-H20 Blk-5 020700-H20 Blk-6 020800-H20 Blk-1 020800-H20 Blk-2 020900-H20 Blk-5 020900-H20 Blk-6 020700-RBS Blk-5 020700-RBS Blk-6 020800-RBS Blk-i 020800-RBS-Blk-2 020800-RTS Blk-1 020800-RTS-Blk-2 020900-RBS Blk-5 020900-RBS-Blk-6 020900-RTS Blk-5 020900-RTS-Blk-6 020700-RTS-MS-5 020700-RTS-MSD-5 020700-RTS-MS-5 020700-RTS-MSD-5 020700-RTS-MS-6 020700-RTS-MSD-6 020700-RTS-MS-6 020700-RTS-MSD-6 020800-RTS-MS-l 020800-RTS-MSD-l 020800-RTS-MS-l 020800-RTS-MSD-l 020800-RTS-MS-2 020800-RTS-MSD-2 020800-RTS-MS-2 020800-RTS-MSD-2 C90778M-MS-5 C90778M-MSD-6 020900-RTS-MS-5 020900-RTS-MSD-6 020900-RTS-MS-5 020900-RTS-MSD-6 Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA 2nd Antlysis OK NA NA NA NA NA X NA X NA NA NA NA Confirmed High NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA 1 1 1 1 1 1 1 1 1 1 I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 NA NA 1 1 NA NA NA NA 0.000 0.000 0.000 0.920 0.000 0.000 0.000 0.000 0.790 0.710 0.980 0.790 0.000 0.000 0.000 0.000 349 340 305 310 354 346 318 308 230 272 NA NA 229 259 NA NA 342 341 265 257 NA NA D0816000I6 D0816000I7 D081600020 A021800I10 A062000005 A062000019 D081600018 D0815000I9 A021800004 A 0 2I8 00111 A021800005 A 02I800I12 A062000006 A062000020 A062000007 A062000021 A0225000I7 A022500018 D082300057 D082300058 A022500019 A022500020 D082300059 D082300060 A021800017 D08I600027 NA NA A021800018 D081600023 NA NA D081600024 DOS1600025 A2018000I9 A021800020 NA NA <LOQ (0.00493 ug/mL) <LOO (0.00493 ue/mU cIjOQ (0.00493 ug/mL) <LOO (0.00493 ue/mL) <LOQ (0.00493 ug/mL) <LOO (0.00493 ue/mU <LOQ (0.00493 ug/mL) <LOO (0.00493 ue/mU <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOO (0.00493 ue/mL) <LOQ (0.00493 ug/mL) <LOO (0.00493 ue/mL) <LOQ (0.00493 ug/mL) <LOO (0.00493 ue/mD 14154 137% 123% 125% 143% 140% 128% 124% 93% 110% NA NA 93% 105% NA NA 72% 72% 107% 104% NA NA 2nd 2nd 2nd 2nd Group 1 Control 0.0 mg/kg C90712M Unknown NA 0.770 A021800023 <LOQ (0.00493 ug/mL) C907I6M Unknown NA 0.940 A021800037 <LOQ (0.00493 ug/mL) C90722M Unknown NA 1 0.800 A021800038 <LOQ (0.00493 ug/mL) C90724M Unknown NA 1 0.960 A021800039 <LOQ (0.00493 ug/mL) C90726M Unknown NA 1 0.830 A021800024 <LOQ (0.00493 ug/mL) C90728M Unknown NA 1 0.930 A021800040 <LOQ (0.00493 ug/mL) C90735M Unknown NA 1 0.800 A021800041 <LOQ (0.00493 ug/mL) C90742M Unknown NA 1 0.960 A021800044 <LOQ (0.00493 ug/mL) C90743M Unknown NA 1 0.990 A021800025 <LOQ (0.00493 ug/mL) C90747M Unknown NA 1 0.950 A021800045 <LOQ (0.00493 ug/mL) C90750M Unknown NA 1 0.770 A021800026 <LOQ (0.00493 ug/mL) C90758M Unknown NA 1 0.670 A021800027 <LOQ (0.00493 ug/mL) C90765M Unknown NA 1 0.620 A021800046 <LOQ (0.00493 ug/mL) C90778M Unknown NA 1 0.960 A021800058 <LOQ (0.00493 ug/mL) Group 1 Control 0.0 mg/kg C91127F Unknown NA 1 0.9(H) A021800047 <LOQ (0.00493 ug/mL) C91131F Unknown NA 1 0.930 A021800048 <LOQ (0.00493 Ug/mL) C91138F Unknown NA 1 0.790 A021800059 <LOQ (0.IKI493 ug/mL) C91I44F Unknown NA 1.55 A021800030 ri-OQ (0.00493 ug/mL) C91I48F Unknown NA 1 1.05 A021800051 <LOQ (0.00493 ug/mL) C91157F Unknown NA 1 1.08 A021800031 <LOQ (0.00493 ug/mL) C91159F Unknown NA l 0.740 A021800052 <LOQ (0.00493 ug/mL) C91166F Unknown NA 1 0.770 A02I800032 <LOQ (0.00493 Ug/mL) C91172F Unknown NA 1 0.770 A021800053 <LOQ (0.00493 ug/mL) C9I176F Unknown NA 1 0.750 A021800054 <LOQ (0.00493 ug/ml.) C91183F Unknown NA 1 0.860 A02I800055 <LOQ (0.00493 ug/ml.) C91I88F Unknown NA 1 0.860 A021800033 <LOQ (0.00493 ug/ml.) C91I90F Unknown NA 1 0.920 A021800034 <LOQ (0.00493 ug/ml-) Groiqi 2 Low Dose 3.00mg/kg C9078IM Unknown NA 1 6.70 A021800081 0.00670 C90782M Unknown NA 1 12.8 A021800060 0.0128 C90783M Unknown NA l 30 4 A<>21800061 1) 1)304 C90785M Unknown NA 1 21.7 A021800064 0.0217 C90787M Unknown NA 1 12.5 A021800065 0.0125 C90788M Unknown NA 1 395 A021800100 0.0395 C9079IM Unknown NA 1 13.9 A021800101 0.0139 C90794M Unknown NA 1 37.4 A021800066 0.0374 C90799M Unknown NA 1 9.00 A021800082 0.00900 C90804M Unknown NA 1 7.28 A021800067 0.00728 C90809M Unknown NA 1 33.9 A02I800I02 0.0339 C90810M Unknown NA 1 21.3 A021800068 0.0213 C9081IM Unknown NA 1 2.70 A021800085 <LOQ (4.93 ng/mL) C90812M Unknown NA 1 5.90 A021800086 0.00590 C90815M Unknown NA 1 5.15 A02I800087 0.00515 C90823M Unknown NA 1 6.67 A021800088 0.00667 C90829M Unknown NA 1 22.7 A021800071 0.0227 C90830M Unknown NA 1 37.0 A021800072 0.0370 C90832M Unknown NA 1 31.4 A021800073 0.0314 C90835M Unknown NA 1 19.6 A021800103 0.0196 C90838M Unknown NA 1 11.5 A021800074 0.0115 C90840M Unknown NA 1 5.74 A021800089 0.00574 Group 2 Low Dose 3.00 mg/kg C91197F Unknown NA 1 17.0 A021800092 0.0170 C91201F Unknown NA 1 13.3 A021800093 0.0133 C91207F Unknown NA 1 49,2 A021800075 0.0492 C91216F Unknown E EE E E C91220F Unknown NA 1 50.4 A021800106 0.0504 C9122IF Unknown NA 1 9.43 A02I800094 0.00943 C91227F Unknown NA 1 16.6 A021800095 0.0166 C91232F Unknown NA l 253 A021800078 0.253 C91235F Unknown NA 1 309 A021800079 0.309 C9I236F Unknown NA 1 129 A021800096 0.129 C9I242F Unknown NA 1 62.1 A021800099 0.0621 C9I243F Unknown NA 1 22.0 A021800080 0.0220 A= CCVs analyzed bracketing these data were within criteria but had peak areas slightly above the valir E = Lost during extraction, no sample remaining to reexUacL PFOS = Perfluorooctanesulfonale PFOSA - Periluorooctanesulfooamide PFOSAA - Periluorooctanesulfonamidoacetale Corrected PFOS LOQ (0 (KI492 ug/mL) to include std correction factors new LOQ is 0.00394 ug/mL. LAC 02/19/01 EtFOSE - Narrow Range N-Ethyl Periluorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2C00) PFOSEA - Perfuorooclane sulfonyl ethylamide Average PFOSA <LOO <LOO <LOO <LOO <LOQ <LOO <LOO <LOO 139% 124% 141% 126% 101% NA 99% NA 72% 105% NA <LOQ <LOQ 0.0187 0.0846 Dale Entered/By: Dale Verified/By: Purity Entered/Verified: 03/06/00,03/10/00,03/20/00,03/21/00,4/17/00,5/16/00,06/22/00,06/23/00,06/26/00.09/05/00,10/17/00,04/13/01 LAC/CSH 4/17/01 mmh 4/30/01 hoj/04/30/01 LAC 02/19/01 LAC RSD Std. Dev. MS/MSD RPD NA NA NA NA NA NA NA NA 3% 2% 2% 3% 17% NA 12% NA 0% 3% NA NA NA NA NA 64.0 0.0119 123 0.104 3MEnvironmental Laboratory Page 226 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product NumbeifTest Substance): Matrix: Method'Revision: Analytic! Equipment System Number 104 Week Dietary Carcinogenicity Study with Natrow Range (98.1%) N-F.thyl Perfluorooctanesuifonamido Ethanol in Rata T-6316 (ElFOSE-OH) Rat Serum ETS-8-4.1 &ETS-8-5.I . Amelia 062498, Davey 070799 Instrument Software/Version: Filename: .-Squared Value: Slope: Y-Intercept: Maaslynx 3.3 & 3.4 See Below See Attachments See Attachments See Attachments Dales of Extrection/Analyst Dales of Analysis/Analyst Dale of Data Reduction/Analyst Sam ple D ata 02/07/00.02/08/00,02/09/00 SAL/RWW 02/18/00,03/15/00, 4/18/00,4/19/00, 06/19/00, 06/20/00.08/16/00,08/23/00 MMH/IAS/CSH 02/21/tX), 03/16/00, 4/19/00, 4/20/00, 06/20/00, 06/21/00,08/18/00, 08/25/00, 04/11/01 MMH/IAS/HOJ Box 0 0 -0 0 9 W E E K IP S R A T S E R A __________ lotT-7121.1 Dose Method Blk Matrix Blk QC-250 ppb Simple # 020700-H20 Blk-5 020700-H20 Blk-6 020800-H20 Blk-I 020800-H20 Blk-2 020900-H20 Blk-5 020900-H20 Blk-6 020700-RBS Blk-5 020700-RBS Blk-6 020800-RBS Btk-1 020800-RBS-Blk-2 020800-RTS Blk-1 020800-RTS-Blk-2 020900-RBS Blk-5 020900-RBS-Blk-6 020900-RTS Blk-5 020900-RTS-Blk-6 020700-RTS-MS-5 020700-RTS-MSD-5 020700.RTS-MS-5 020700-RTS-MSD-5 020700-RTS-MS-6 020700-RTS-MSD-6 020700-RTS-MS-6 020700-RTS-MSD-6 020800-RTS-MS-l 020800-RTS-MSD-1 020800-RTS-MS-1 020800-RTS-MSD-l 020800-RTS-MS-2 020800-RTS-MSD-2 020800-RTS-MS-2 020800-RTS-MSD-2 C90778M-MS-5 C90778M-MSD-6 020900-RTS-MS-5 020900-RTS-MSD-6 020900-RTS-MS-5 020900-RTS-MSD-6 PFOSAA Purity Correction Factor Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Surrogate Verified NA NA 2nd Analysis OR NA NA NA NA NA X NA X NA NA NA NA Confirmed Hieh NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOSAA Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 NA NA 1 1 NA NA 1 1 NA NA 1 1 NA NA . 4 1 1 1 1 PFOSAA Cone. ng/mL 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 IMMI 0.00 0.00 0.00 0.00 310 306 NA NA 312 305 NA NA 281 259 NA NA 296 247 NA NA 338 333 334 357 307 313 Filename D08I600016 D081600017 A0218CMHMI3 A021800110 A062000005 A062000019 D081600018 D081600019 A021800004 A021800111 A021800005 A021800112 A062000006 A062000020 A062000007 A062000021 A022500017 A0225000I8 NA NA A022600019 A022600020 NA NA A02I800017 D081600027 NA NA A021800018 D081600023 NA NA A062100054 A062100055 A021800019 A021800020 D03I500039 D031500040 Concentra tien f PFOSAA ug/mL or % Ree <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mLl <LOQ (0.00493 ug/mL) <LOO 0.00493 ue/mL) <LOQ (0.0248 ug/mL) <LOO (0.0248 ue/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ue/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ue/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ue/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 UB/mLl 125% 123% NA NA 126% 123% NA NA 113% 105% NA NA 119% 100% NA NA 71% 70% 135% 144% 124% 126% A A A A A' 2nd 2nd Group 1 Control 0.0 mg/kg C90712M C90716M C90722M C90724M C90726M C90728M C90735M C90742M C90743M C90747M C90750M C90758M C90765M C90778M Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA NA NA NA 1 2.52 A02I800023 <LOQ (0.00493 ug/mL) 1 0.00 A02I800037 <LOQ (0.00493 ug/mL) 1 0.00 A02I800038 <LOQ (0.00493 ug/mL) 1 0.00 A021800039 <LQQ (0.00493 ug/mL) 1 0.00 A021800024 <LOQ (0.00493 ug/mL) 1 0.00 A021800040 <LOQ (0.00493 ug/mL) 1 0.00 A021800041 <LOQ (0.00493 ug/mL) 1 0.00 A021800044 <LOQ (0.00493 ug/mL) 1 0.00 A021800025 <LOQ (0.00493 ug/mL) 1 0.00 A021800045 <LOQ (0.00493 ug/mL) 1 0.00 A021800026 <LOQ (0.00493 ug/mL) 1 (MM) A021800027 'L O Q (0.00493 ug/mL) 1 t).(M) A021800046 <LOQ (0.00493 ug/mL) 1 0(H) A021800058 <LOQ (0.00493 ue/mL) Group 1 Control 0.0 mg/kg C91I27F C91I31F C91I38F C91144F C91148F C91157F C9I159F C91166F C91172F C9II76F C91I83F C91188F C91I90F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown L'nknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA NA NA 1 0(H) A021800047 <LOQ (0.(M)493 ug/mL) 1 0.00 A021800048 <1.00(0.00493 ug/mL) 1 0.00 A021800059 <LOQ (0.1MI493 ug/mL) 1 0.00 A021800030 <LOQ (0.00493 ug/mL) 1 0.00 A021800051 <LOQ (0.00493 ug/mL) 1 0.00 A021800031 <LOQ (0.00493 ug/mL) 1 2.87 A021800052 <LOQ (0.00493 ug/mL) 1 0.00 A021800032 <LOQ (0.00493 ug/mL) 1 0.00 A021800053 <LOQ (0.00493 ug/mL) 1 0.00 A02I800054 <LOQ (0.00493 ug/mL) 1 0.00 A021800055 <LOQ (0.(M)493 ug/mL) 1 0.00 A021800033 <LOQ (0.00493 ug/mL) 1 3.68 A02I800034 <LOQ (0.00493 ug/mL) G roup! Low Dose 3.00 mg/lcg C90781M C90782M C907S3M C90785M C90787M Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA 1 141 R041800017 0.141 1 538 A021800060 0.538 1 642 A021800061 0.642 1 189 A021800064 0.189 1 289 A021800065 0.289 Group 2 Low Dose 3.00 mg/kg C90788M C9079IM C90794M C90799M C90804M C90809M C90810M C90811M C908I2M C908I5M C90823M C90829M C90830M C90832M C90835M C90838M C90840M C91197F C91201F C9I207F C9I2I6F C9I220F C91221F C9I227F C9I232F C91235F C91236F C91242F C91243F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA 10 NA to NA 1 NA 1 NA 1 NA 10 NA 1 NA 1 NA 1 NA 1 NA 1 NA 1 NA 1 NA . 10 NA 1 NA 1 NA 1 NA 1 NA I NA 10 EE NA 10 NA 1 NA 1 NA 10 NA 10 NA 10 NA 10 NA 1 84.5 A031500029 80.7 AQ21800101 670 A021800066 212 R041800021 214 A02I800067 93.6 A031500034 764 A02I8OOO6 8 105 R041800024 617 R041900025 278 R041900026 174 R041800027 475 RQ4I900028 579 R041900031 156 A031500040 684 A021800103 769 R041900033 685 R041900034 327 A021800092 368 A021800093 63.1 A03I500044 EE 130 A03I500047 380 A021800094 609 A021800095 360 A031500050 439 A031500051 272 A031500054 137 A031500055 896 R041900046 0.845 0.807 0.670 0.212 0.214 0.936 0.764 0.105 0.617 0.278 0.174 0.475 0.579 1.56 0.684 0.769 0.685 0.327 0.368 0.631 E 1.30 0.380 0.609 3.60 4.39 2.72 1.37 0.896 A - CCVs analyzed bracketing these data were within criteria but had peak areas slightly above the valid linear range. LAC 05/03/01 PFOSAA Uf/mL <LOO <LOO <LOQ <LOO <LOQ <LOQ <LOQ <LOO 124% NA124% NA 109% NA 110% NA 70% 139% 125% <LOQ <L0Q 0.553 1.51 PFOS - Perfluorooctanesulfonate PFOSA - Perfluorooclanesulfonamide PFOSAA = Peifluorooclanesulfonamidoacelale F.iFOSF. = Narrow Range N-Ethyl Perfluorooctanesuifonamido ethyl alcohol M556 = C8F17S02N((H)CH2C00) PFOSEA - Perfuorooctane sulfonyl ethylamide Corrected PFOS LOQ (0.00492 ug/mL) to include sld correction factors new LOQ is 0.00394 ug/mL LAC 02/19/01 Date Entered/By: Date Verified/ By: Purity Entered/Verified: 03/06AH), 03/10/00,03/20/00, 03/21/00, 4/17/00, 5/16/00,06/22/00, 06/23/00, 06/26/00,09/05/00.10/17/iH), 04/13/01 LAC/CSH 4/17/01 tttmh 4/30/01 h o j/04/30/01 LAC 02/19/01 LAC RSD Sld. Dev. MS/MSD RPD NA NA NA NA NA NA NA NA 2% NA 2% NA 8% NA 18% NA 1% 7% 2% NA NA NA NA 62.4 0.345 94.1 1.42 3MEnvironmental Laboratory Page 227 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product Number(Test Substance): Matrix: MeIhod/Revision: Analytical Equipment System Number Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Intercepl: 104 Week Dietary Carcinogenicity Study with Narrow Range (98.154) N-Ethyl Perfluorooclanesulfonsmido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 & ETS-8-S.I Amelia 062498, Davey 070799 Masstynx 3.3 & 3.4 See Below See Attachments See Attachments See Attachments Dates of Extraction/Analyst: Dales of Analysts/Analysl Date ofData Reduction/Analyst Sample Data 02/07/00,02/08/00,02/09/00 SAL/RWW 02/18/00,03/15/00,4/18/00,4/19/00,06/19/00,06/20/00,08/16/00,08/23/00 MMH/1AS/CSH 02/21/00.03/16/00.4/I9AM), 4/20/00,06/20/00, 06/21/00, 08/18/00,08/25/00,04/11/01 MMH/IAS/HOJ Box 0 0 -0 0 9 WEEK 105 RAT SERA____________________ lotUnknown/SDO 13 Dose Method Blk Matrix Blk QC-250ppb Group 1 Control 0.0 mg/kg Sample U 020700-H20 Blk-S 020700-H20 Blk-6 020800-H20 Blk-I 020800-H20 Blk-2 020900-H20 Blk-5 020900-H20 Blk-6 020700-RBS Blk-5 020700-RBS Blk-6 0208(H)-RBS Blk-I 020800-RBS-Blk-2 020800-RTS Blk-I 020800-RTS-Blk-2 020900-RBS Blk-5 020900-RBS-B9k-6 020900-RTS Blk-5 020900-RTS-Blk-6 020700-RTS-MS-5 020700-RTS-MSD-5 020700-RTS-MS-5 020700-RTS-MSD-5 020700-RTS-MS-6 020700-RTS-MSD-6 020700-RTS-MS-6 020700-RTS-MSD-6 020800-RTS-MS-1 020800-RTS-MSD-I 020800-RTS-MS-1 0208(H)-RTS-MSD-1 0208(H)-RTS-MS-2 020800-RTS-MSD-2 020800-RTS-MS-2 020800-RTS-MSD-2 C90778M-MS-5 C90778M-MSD-6 020900-RTS-MS-5 020900-RTS-MSD-6 020900-RTS-MS-5 020900-RTS-MSD-6 C907I2M C907I6M C90722M C90724M C90726M C90728M C90735M C90742M C90743M C90747M C90750M C90758M C90765M C90778M EtFOSE-OH Purity Correction F a c to r Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown . Surrogate Verified NA NA 2nd Analysis OK NA NA NA NA NA X NA X NA NA NA NA Confirmed Hieb NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA . NA NA NA NA EtFOSE-OH Dilutten Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 NA NA 1 1 NA NA 1 1 1 NA NA 4 4 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 EtFOSE-OH Cone. ng/mL 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.(H> 0.00 0.00 0.00 0.00 83.8 69.2 NA NA 82.2 65.0 NA NA 51.8 63.2 80.6 NA 53.2 62.8 93.2 NA 582 606 64.5 71.1 92.9 97.0 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 Filename D0816000I6 D0816000I7 D081600020 A02I8OOI10 A062000(H)5 A062000019 DOS1600018 D081600019 A021800004 A021800111 A021800005 A 021800I12 A062000006 A062000020 A062000007 A062000021 A022500017 A022500018 NA NA A0225000I9 A022500020 NA NA A021800017 D08I600027 D03I500037 NA A021800018 D081600023 D031500038 NA A062100054 A062100055 A021800019 A021800020 D031500039 D031500040 A021800023 A021800037 A021800038 A021800039 A021800024 A02I800040 A 0 2 I 800041 A021800044 A021800025 A021800045 A021800026 A021800027 A021800046 A021800058 Concentration of EtFOSE-OH ug/mL o r % Ree <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) 'LOQ (0.00977 ug/mL) <LOO (0.00977 uE/mL) <LOQ (0.0248 ug/mL) <LO0 (0.0248 ug/rnL) <LOQ (0.00977 ug/mL) <LOO (0.00977 UE/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 UE/mL) <LOQ (0.(H)977 ug/mL) -LOQ (0.00977 uc/mL) -LOQ (0.0248 ug/mL) <LOO 0.0248 ue/mLl <LOQ (0.0248 ug/mL). <LOO (0.0248 ue/mL) 3454 2854 NA NA 3354 2654 NA NA 2154 2554 3254 2nd NA 2154 2554 3854 2nd NA 12254 12754 2654 2954 3754 2nd 3954 2nd <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) -LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) -LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) Group 1 Control 0.0 mg/kg C9II27F C91I31F C9I138F C9I144F C9I148F C91157F C91159F C91I66F C91I72F C9II76F C9I183F C9I188F C9I190F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA NA NA 1 0.00 A02I800047 <LOQ (0.00977 ug/mL) 1 (UHI A021800048 <LOQ (0.00977 ug/mL) 1 0.00 A021800059 <LOQ (0,(H)977 ug/mL) 1 2.54 A021800030 <LOQ (0.00977 ug/mL) 1 0(H) A021800051 <LOQ (0.00977 ug/mL) 1 0.00 A02180003I -LOQ (0.00977 ug/mL) 1 0.00 A02I8OO052 <LOQ (0.00977 ug/mL) 1 0.00 A021800032 <LOQ (0.00977 ug/mL) 0.00 A02I800053 -LOQ (0.00977 ug/mL) 1 0.00 A021800054 <LOQ (0.00977 ug/mL) 1 0.00 A021800055 <LOQ (0.00977 ug/mL) 1 0.00 A021800033 <LOQ (0.00977 ug/ml.) 1 0.00 A021800034 <LOQ (0.00977 ug/mL) Group 2 I-ow Dose 3.00 mg/kg C90781M C90782M C90783M C90785M C90787M C90788M C9079IM C90794M C90799M C90804M C90809M C90810M C90811M C90812M C90815M C90823M C90829M C90830M C90832M C90835M C90838M C90840M Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA 1 0.00 A0218IMH18I <LOQ (0.00977 ug/mL) 1 0.00 A02I800060 <LOQ (0.00977 ug/mL) 1 2.81 A021800061 <LOQ(0.00977ug/mL) 1 0.00 A0218<HM>64 <LOQ (0.00977 ug/mL) 1 0.00 A021800065 <LOQ (0.00977 ug/mL) 1 2.19 A021800100 -LOQ (0.00977 ug/ml.) 1 0.00 A021800101 -LOQ (0.00977 ug/mL) 1 0.00 A021800066 <LOQ (0.00977 ug/mL) 1 0.00 A021800082 -LOQ (0.00977 ug/mL) 1 0.00 A02!800067 -LOQ (0.00977 ug/mL) 1 2.45 A02I800I02 -LOQ (0.0097? ug/mL) 1 1.89 A02I800068 -LOQ (0.00977 ug/mL) 1 (UK) A021800085 -LOQ (0.00977 ug/mL) 1 0.00 A021800086 -LOQ (0.00977 ug/mL) 1 0.00 A021800087 <LOQ (0.00977 ug/mL) 1 l).(H) A02I800088 -LOQ (0.00977 ug/mL) (UHI A02I800071 <LOQ (0.00977 ug/mL) 1 2.76 A021800072 -LOQ (0,(H)977 ug/mL) 1 0.00 A021800073 <LOQ (0.00977 ug/mL) 1 0.00 A021800103 -LOQ (0,(H)977 ug/mL) 1 2.50 A021800074 -LOQ (0.00977 ug/mL) 1 0.00 A021800089 -LOQ (0.00977 ug/mL) Group 2 Low Dose 3.00 mg/kg C91I97F C9120IF C91207F C912I6F C9I220F C9I221F C9I227F C91232F C91235F C91236F C91242F I C91243F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA E NA NA NA NA NA NA NA NA 1 0.00 A021800092 -LOQ (0.00977 ug/mL) I 0.00 A021800093 -LOQ (0.00977 ug/mt.) 1 0.00 A021800075 -LOQ (0.00977 ug/mL) F. E E E 1 2.40 A02I800I06 -LOQ (0.00977 ug/mL) 1 0.00 A021800094 -LOQ (0.00977 ug/mL) 1 O.(H) A021800095 -LOQ (0.00977 ug/mL) 1 7.15 A021800078 -LOQ (0.00977 ug/mL) 1 7.45 A021800079 -LOQ (0.00977 ug/mL) 1 4.03 A021800096 -LOQ (0.00977 ug/mL) 1 3.07 A021800099 -LOQ (0.00977 ug/mL) 1 0.00 A021800080 <IX)Q (0.00977 ug/mL) A= CCVs analyzed bracketing these data were within criteria but had peak areas slightly above the valid linear range. LAC 05/03/01 E = Lost during extraction, no sample remaining to reextract. PFOS - Perfluorooctanesulfonate Corrected PFOS LOQ (0.00492 ug/mL) to include std correction (actors PFOSA - Perfluorooctanesulfonamide PFOSAA = Periluorooctanesulfonamidoacetate new LOQ is 0.00394 ug/mL. LAC 02/19/01 EtFOSE = Narrow Range N-Ethyl Periluorooclanesulfonamido ethyl alcohol M556 = C8FI7S02N((H)CH2COO) PFOSEA = Perfumooctane sulfonyl ethylamide EtFOSE-OH -LOO -LOQ -LOQ -LOO -LOQ -LOO -LOO -LOO 3154 NA 3054 NA 2354 3254 2354 3854 12554 2754 38V. -LOO -LOQ -LOQ -LOQ Date Entered/By: Date Verified/ By: Purity Entered/Verified: 03/06/00,03/10/00, 03/20/00,03/71/00,4/17/00, 5/16/00, 06/22/00, 06/23/00.06/26/00, 09/05/00, 10/17/00,04/13/01 LAC/CSH 4/17/01mmh 4/30A11 hoj/04/30/01 LAC 02/19/01 LAC RSD Std. Dev. MS/MSD RPD NA NA NA NA NA NA NA NA 1954 NA 2354 NA 20V. NA 1754 NA 454 10V. 454 NA NA NA NA NA NA NA NA 3MEnvironmental Laboratory Page 228 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product NumbeifTest Substance): Matrix: Method/Revision: 104 Week Dietary Carcinogenicity Study with Narrow Range (98 !/.) N-Ethyl Perfluorooclanesulfonamido Ethanol in Rats T-6316 (EtFOSE*OH) Rat Serum ETS-8-4.1 &ETS-8-5.1 Analytical Equipment System Number Instrument Softwtre/Version: Filename: Amelia 062498, Davey 070799 Masslynx 3.3 & 3.4 See Below - R-Squared Value: Slope: See Attachments See Attachments Y-IntercepL Dates of Extraction/Analyst See Attachments 02/07/00,02/08/00,02/09/00 SAL/RWW Dates o f Analysis/Analysl: Date of Data Reduction/AnalysC 02/18/00,03/15/00,4/18/tH), 4/19/00,06/19/00,06/20/00,08/16/00,08/23/00 MMH/IAS/CSH 02/21/00,03/IG/00,4/19/00,4/20/00,06/20/00,06/21/00,08/18/00,08/25/00,04/11/01 MMH/1AS/HOJ Sample Data Box (MMX WEEK 105 RAT SERA lotN BI 13047-80 Group Dose Method Blk Matrix Blk QC-250 ppb Sample * 020700-H20 Blk-5 020700-H20 Blk-6 020800-H20 Blk-1 020800-H20 Blk-2 020900-H20 Blk-5 020900-H20 Blk-6 020700-RBS Blk-5 020700-RBS Blk-6 020800-RBS Blk-I 020800-RBS-Blk-2 020800-RTSBtk-l 0208(K)-RTS-Blk-2 020900-RBS Blk-5 020900-RBS-Blk-6 020900-RTS Blk-5 020900-RTS-Blk-6 020700-RTS-MS-5 M556 Purity C e r re c tl e n Factor Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA Surrogate Verified NA NA 2nd Anelysis OK NA NA NA NA NA X NA X NA NA NA NA Confirmed High NA M556 Dilution Feetnr 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 M556 Cone. ng/mL 0.190 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.69 0.00 0.00 0(H) 0.0900 0.00 380 Filename D0816IX10I6 D081600017 D081600020 D031500025 A061900005 A06190(H) 19 D08I600018 D0816000I9 A0315(X)006 D031500026 A031500007 D031500027 A031500007 D031500027 A061900007 A061900021 A0225000I6 Concentration of M556 ug/mL or % Ree <LOQ (0.00977 ug/mL) <LOO (0.00977 uc/mU 'L O Q (0.00977 ug/mL) 'L O Q (0.(H)494 ug/mU <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.(M)977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) <LOQ 0.00497 ug/mL) <LOO 0.00497 ug/mL) <I.OQ (0.00494 ug/mL) <LOO (0.00494 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/ml.) 153% A A A A A Average M556 'LOQ 'LOQ -LOQ <LOQ <LOO <LOO <LOO <LOQ 020700-RTS-MSD-5 020700-RTS-MS-5 020700-RTS-MSD-5 020700-RTS-MS-6 020700-RTS-MSD-6 020700-RTS-MS-6 020700-RTS-MSD-6 020800-RTS-MS-1 020800-RTS-MSD-1 NA NA NA NA NA NA NA NA NA NA 1 381 A022500017 153% 153% NA 1 345 D082300057 139% 2nd NA 1 359 D082300058 145% 2nd 142% NA 1 363 A022500018 146% NA 1 352 A022500019 142% 144% NA 1 354 D0823(XX)59 143% 2nd NA 1 350 D082300060 141% 2ml 142% NA 1 249 A021800017 100% NA 1 252 D081600027 102% A 101% 020800-RTS-MS-1 020800-RTS-MSD-i 020800-RTS-MS-2 02080(bRTS-MSD-2 NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA 1 247 A02I80OO18 100% NA 1 230 D08I600023 93% A 96% . 020800-RTS-MS-2 020800-RTS-MSD-2 C90778M-MS-5 C90778M-MSD-6 020900-RTS-MS-5 NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA 445 A062000054 93% NA 409 A062000055 86% NA 1 340 A02180(H)19 137% NA 90% 020900-RTS-MSD-6 020900-RTS-MS-5 020900-RTS-MSD-C NA NA NA NA 1 347 A021800020 139% 138% NA 1 324 D031500039 131% 2nd NA 318 D031500040 127% 2nd 129% Group 1 Control 0.0 mg/kg C90712M C90716M C90722M C90724M C90726M Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA 0.600 0.380 0.00 0.00 0.00 D03I500043 D031500057 D031500058 D031500059 D031500044 <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) 'L O Q (0.00494 ug/mL) 'L O Q (0.00494 ug/mL) <LOQ (0.00494 ug/mL) C90728M C90735M Unknown Unknown NA NA 0.00 D031500060 <LOQ (0.00494 ug/mL) 0.00 D031500061 <LOQ (0.00494 ug/mL) C90742M Unknown NA 1 0.00 D031500064 <LOQ (0.00494 ug/mL) C90743M Unknown NA 1 0.00 D031500045 <LOQ (0.00494 ug/mL) C90747M Unknown NA 1 0.00 D031500065 ' LOQ (0.00494 ug/mL) C90750M Unknown NA 1 0.00 D0315(XX>46 <LOQ (0.00494 ug/mL) C90758M Unknown NA 1 0.00 D031500047 'L O Q (0.00494 ug/mL) C90765M Unknown NA 1 0.00 D031500066 'L O Q (t).(KI494 ug/ntL) C90778M Unknown NA 1 0.00 D031500078 'L O Q (0.00494 ug/mL) 'LOQ Group 1 Control 0.0 mg/kg C9I127F Unknown NA 1 0.00 D031500067 'U 3 Q (0.00494 ug/mL) C9I131F Unknown NA 1 0.00 D031500068 'L O Q (0.00494 ug/mL) C9I138F Unknown NA 1 0.00 D031500079 <LOQ (0.00494 ug/mL) C91144F Unknown NA 1 0.00 D031500050 'L O Q (0.00494 ug/mL) C91I48F Unknown NA 1 0.00 D03I50007I 'L O Q (0.(H)494 ug/mL) C91I57F Unknown NA 1 0.00 D03I50005I <LOQ (0.00494 ug/mL) C91I59F Unknown NA 1 0.00 D031500072 <LOQ (0.00494 ug/mL) C91I66F Unknown NA 1 0.00 D03I500052 <LOQ (0.00494 ug/mL) C9I172F Unknown NA I 0.00 D031500073 <LOQ (0.00494 ug/mL) C9I176F Unknown NA I 0.00 D031500074 'L O Q (0.00494 ug/mL) Group 2 C9I183F Unknown NA 1 0.00 D031500075 <LOQ (0.00494 ug/mL) C9I188F Unknown NA 1 0.00 D031500053 <LOQ (0.00494 ug/mL) C9I190F Unknown NA 1 0.00 D031500054 cLOQ (0.00494 ug/mL) <LOQ C90781M Unknown NA 1 44.5 A0218(KH)81 0.0445 Low Dose 3.00 Ttig/lcg C90782M Unknown NA 1 123 A021800060 0.123 C90783M Unknown NA 1 264 A02I8(HM)6I 0 264 C90785M Unknown NA 1 36.2 A()218(XH>64 0.0362 C90787M Unknown NA 1 76.8 A021800065 0.0768 C90788M Unknown NA 1 534 A021800KI0 0.534 C90791M Unknown NA 1 195 A02I80010I 0.195 C90794M Unknown NA 1 217 A021800066 0.217 C90799M Unknown NA 1 161 A021800082 0.161 C90804M Unknown NA 1 21.5 A021800067 0.0215 C90809M Unknown NA 1 255 A021800102 0.255 C908I0M Unknown NA 1 55.8 A02I800068 0.0558 C908I1M Unknown NA 1 91.6 A021800085 0.0916 C908I2M Unknown NA 1 61.0 A021800086 0.0610 C90815M Unknown NA 1 112 A021800087 0.112 C90823M Unknown NA 1 175 A02I800088 0.175 C90829M Unknown NA 1 145 A021800071 0.145 C90830M Unknown NA 1 276 A021800072 0.276 C90832M Unknown NA 1 122 A021800073 0.122 C90835M Unknown NA 1 49.9 A02I800103 0.0499 C90838M Unknown NA 1 95.0 A021800074 0.0950 C90840M Unknown NA 1 88.8 A021800089 0.0888 0.145 Group 2 Low Dose C9I197F Unknown NA 1 285 A021800092 0.285 C9I20IF Unknown NA 1 200 A021800093 0.2(H) 3.00 mg/kg C91207F Unknown NA 1 3(H) A0218(MX)75 0.300 C91216F Unknown E EE E E C91220F Unknown NA 1 355 A021800106 0.355 C9122IF Unknown NA 1 118 A0218(HH)94 0.118 C91227F Unknown NA 1 164 A02180HI95 0.164 C9I232F C9I235F C9I236F Unknown Unknown Unknown NA 10 159 A031500050 1.59 NA 10 190 A03150005I 1.90 NA 1(1 143 A031500054 1.43 C91242F C91243F Unknown Unknown NA 10 98.0 A031500055 0.980 NA 1 166 A021800080 0.166 0.680 A" CCVs analyzed bracketing these data were within criteria but had peak areas slightly above the valic E = lo st during extraction, no sample remaining to reextract range. LAC 05/03/01 PFOS - Perfluorooctanesulfonate Corrected PFOS LOQ (0.00492 ug/mL) to include std correction factors PFOSA = PerfluoTooclanesulfonamide PFOSAA - Perfluorooclanesulfonamidoacetate new LOQ is 0.00394 ug/mL. LAC02/I9/0I EtFOSE - Narrow Range N-Ethyl Perfluorooclanesulfonamido ethyl alcohol M556 = C8FI7S02N((II)CH2C00) PFOSEA = Perfuorooctane sulfonyl ethylamide Dale Enlered/By: Dale Verified/By: Purity Enlered/Verified: 03/06/00,03/10/00,03/20/00,03/21/00,4/17/00,5/16/00,06/22/00,06/23/00,06/26/00.09/05/00, 10/17/00,04/13/01 LAC/CSH 4/17/01 mmh 4/30/01 hoj / 04/30/01 LAC . 02/19/01 LAC RSD Std. Dev. MS/MSD RPD NA NA NA NA NA NA NA NA 0% 4% 3% 1% 1% NA 7% NA 8% 1% 3% NA NA NA NA 79.4 0.115 98.0 0.667 3MEnvironmental Laboratory Page 229 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product Number(Test Substance): Matrix: Method/Revision: Analytical Equipment System Number Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Intercept Dates of Extraction/Analyst Dates of Analysis/Analyst: Date of Data Reduction/Analysl: 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 &ETS-8-5.I Amelia 062498, Davey 070799 Masslynx 3.3 & 3.4 See Below See Attachments See Attachments See Attachments 02/07/00,02/08/00,02/09/00 SAL/RWW 02/18/00,03/15/00,4/18/00,4/19/00,06/19/00,06/20/00,08/16/00,08/23/00 MMH/1AS/CSH 02/21/00, 03/16/00,4/19/00, 4/20/00, 06/20/00,06/21/00,08/18/00, 08/25/00, 04/11/01 MMH/IAS/HOJ Sample Data Box 00-009 WEEK 105 RAT SERA lot 529 Dose Method Btk Matrix Blk QC-250 ppb Group 1 Control 0.0 mg/kg S a m p le # 020700-H20 BIk-5 020700-H20 Btk-6 020800-H20 Blk-I 020800-H20 Blk-2 020900-H20 Blk-5 020900-H20 Blk-6 020700-RBS Blk-5 020700-RBS Blk-6 020800-RBSBIk-1 020800-RBS-Blk-2 020800-RTS Blk-1 0208t)-RTS-Blk-2 020900-RBS Blk-5 020900-RBS-Blk-6 0209(K).RTS Blk-5 020900-RTS-Blk-6 020700-RTS-MS-5 020700-RTS-MSD-5 020700-RTS-MS-5 020700-RTS-MSD-5 020700-RTS-MS-6 020700-RTS-MSD-6 020700-RTS-MS-6 020700-RTS-MSD-6 020800-RTS-MS-l 020800-RTS-MSD-I 020800-RTS-MS-l 0208(H)-RTS-MSD-1 020800-RTS-MS-2 020800-RTS-MSD-2 020800-RTS-MS-2 020800-RTS-MSD-2 C90778M-MS-5 C90778M-MSD-6 020900-RTS-MS-5 0209(K)-RTS-MSD-6 0209(M)-RTS-MS-5 020900-RTS-MSD-6 C90712M C90716M C90722M C90724M C90726M C90728M C90735M C90742M C90743M C90747M C90750M C90758M C90765M C90778M PFOSEA Purity Correction Factor Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA NA 2nd Analysis OK NA NA NA NA NA X NA X NA NA NA NA Confirmed Hieh NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOSEA Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 .1 1 1 1 NA NA 1 1 NA NA 1 1 1 NA 1 1 1 NA 1 1 1 1 1 1 1 1 1 PFOSEA Cone. ng/mL 0.00 0.120 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 196 186 NA NA 196 150 NA NA 114 161 105 NA 115 138 112 NA 398 416 150 150 142 141 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 Filename D081600016 D081600017 D08I600020 A021800110 A061900005 A061900019 D081600018 D08I600019 A0218<HHH)4 A021800111 A021800005 A021800112 A061900006 A061900020 A06I900007 A061900021 A022600017 A022600018 NA NA A0226000I9 A022600020 NA NA A021800017 D081600027 D031500037 NA A021800018 D081600023 D031500038 NA A062000054 A062(KHM)55 A02I800019 A021800020 D031500039 D031500040 A021K00023 A02I800037 A02I800038 A021800039 A02I800024 A021800040 Al)21800041 A021800044 A021800025 A021800045 A021800026 A021800027 A021800046 A02I800058 Concentration of PFOSEA ug/mL e r % Ree <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mD <LOQ (0.00492 ug/mL) <LOQ (0.00492 ue/mL) <LOQ (0.00492 ug/mL) <LOO (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LO0 (0.00492 ue/mL) <LOQ (0.00492 ug/mL) <LOO 0.00492 ue/mH " LOQ (0.00492 ug/mL) <LOO (0.00492 ug/mL) <LOQ(0.(H)492 ug/mL) <LOQ (0.00492 ue/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ue/mL) 79% 75% NA NA 79% 60% NA NA 46% 65% 42% NA 46% 56% 45% NA 83% 87% 61% 60% 57% 56% <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.(H>492 ug/mL) <LOQ (0.00492 Ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.(H)492 ug/mL) <LOQ (0.00492 ug/mL) 2nd 2nd 2nd 2nd Group 1 Control 0.0 mg/kg Group 2 Low Dose 3.00 mg/kg Group 2 Low Dose 3.00 mg/kg C91127F C9I131F C9I138F C91144F C91I48F C91157F C91I59F C91166F C91172F C91176F C9I183F C91188F C91190F C9078IM C90782M C90783M C9078SM C90787M C90788M C90791M C90794M C90799M C90804M C90809M C90810M C90811M C90812M C90815M C90823M C90829M C90830M C90832M C90835M C90838M C90840M C9I197F C91201F C91207F C91216F C91220F C91221F C91227F C9I232F C9I235F C91236F C91242F C91243F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA E NA NA NA NA NA NA NA NA 1 1 1 1 1 1 1 1 1 1 1 1 .1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 I 1 1 1 1 E 1 1 1 1 1 1 1 1 ().() 0.00 0.00 0.00 0.00 0.1) 0.00 0.00 0.00 0.00 0.(M) 3.03 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 l).(K) 0.00 O.00 0.00 0.00 0.00 0.00 0.00 <MH) 0.00 0(H) E 0.(K) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 A021800047 A021800048 A021800059 A021800030 A021800051 A021800031 A021800052 A021800032 A021800053 A021800054 A021800055 A021800033 A021800034 A021800081 A021800060 A021800061 A021800064 A021800065 A021800100 A021800I01 A021800066 A021800082 A021800067 A021800102 A021800068 A021800085 A021800086 A02I800087 A02I800088 A021800071 A021800072 A02180(K)73 A021800103 A021801)074 A021800089 A021800092 A021800093 A021800075 E A02I800I06 A02I800094 A021800095 A021800078 A021800079 A021800096 A021800099 A021800080 <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <IjOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <l-OQ (0.00492 ug/mL) <tX>Q (0.00492 ug/mL) <LOQ (0.00492 Ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/ml-j <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <IjOQ (0.(H)492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <IX>Q (0.(K>492 ug/mL) <1X)Q (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <1jOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <I.OQ (0.00492 ug/mL) <LOQ (0.1M1492 ug/mL) <LOQ (0.00492 ug/mL) <l-OQ (0.00492 ug/mL) <I.OQ (0.00492 ug/mL) <IX)Q (0.00492 ug/mL) <LOQ (0.00492 ug/mL) E <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <IX>Q (0.00492 ug/mL) <1jOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <IX>Q (0.00492 ug/mL) <LOQ (0.00492 ug/mL) A - CCVs analyzed bracketing these data were within criteria but had peak areas slightly above the valid linear range. LAC 05/03/01 E - Lost during extraction, no sample remaining to reextncL PFOS = Perfluorooctanesulfonate PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluomoctanesulfonamidoacetate Corrected PFOS LOQ (0.00492 ug/mL) to include std correction factors new LOO is 0.00394 ug/mL. LAC 02/19/01 ElFOSE - Narrow Range N-Ethyl Periluorooclanesutfonamido ethyl alcohol M556 = C8FI7S02N((H)CH2COO) PFOSEA - Perfuorooctane sulfonyl elhylamide PFOSEA <LOQ <i-oo <LOQ <LOO <LOO <LOO <LOQ <LOO 77% NA 70% NA 55% 42% 51% 45% 85% 60% 57% <LOQ ^LOQ <LOQ <LOQ Date Entered/By: Date Verified/ By: Purity Entered/Verified: 03/06/00,03/10/00,03/20/00,03/21/00,4/17/00, 5/16/00, 06/22/00,06/23/1), OG/26/00, 09/05/00, 10/17/00,04/13/01 LAC/CSH 4/17/01 mmh 4/30/01 hoj / 04/30/01 LAC 02/19/01 LAC RSD Sid. Dev, MS/MSD RPD NA NA NA NA NA NA NA NA 5% NA 27% NA 34% NA 18% NA 4% 1% 2% NA NA NA NA NA NA NA NA 3MEnvironmental Laboratory Page 230 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product Numbci(Tesl SubsUncc): Matrix: Method/R*vision: Analytical Equipment System Number Instrument Soihvare/Version: Filename: 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Periluorooctanesulfonamido Ethanol in Rats T-63l6(EtFOSE-OH) Rat Serum ETS-8-4.1 & ETS-8-5.1 Amelia 062498. Davey 070799 Masslynx 3.3 & 3.4 See Attachments R-Squared Value: Slope: See Attachments See Attachments Y-Inlercept Dales of Extraction/Analyst: See Attachments 02/07/00,02/08/00,02/09/00 SAL/RWW . Dales ofAnalysia/Analyst: Date of Data Reduction/Analyst: Sample Data 02/18/00, 03/15/00, 4/18/00. 4/19/00,06/19/00, 06/20/00,08/16/00.08/23/00 MMJI IAS/CSH 02/21/00,03/16/00,4/19/00,4/20/00,06/20/00,06/21/00,08/18/00,08/25/00,04/11/01 MMH/IAS/HOJ WEEK 105 RAT SERA Group Dose Method Btk Matrix Blk QC-250 ppb S a m p le # 020700-H20 Blk-5 020700-H20 Blk-6 020800-H20 Blk-I 020800-H20 Blk-2 020900-H20 Blk-5 020900-H20 Blk-6 020700-RBS Blk-5 020700-RBS Blk-6 020800-RBS Blk-I 020800-RBS-Blk-2 020800-RTS Blk-I 020800-RTS-Blk-2 020900-RBS Blk-5 020900-RBS-Blk-6 020900-RTS Blk-5 020900-RTS-Blk-6 020700-RTS-MS-5 Cencentratton f PFOS ug/mL e r % Ree <LOQ (0.00394 ug/mL) <LOQ (0.00394 ug/mL) <LOQ (0.00394 ug/mL) <LOO (0.00394 ug/mL) <LOQ (0.00394 ug/mL) <LOQ (0.00394 ug/mL) <LOQ (0.00394 ug/mL) <LOQ (0.00394 ug/mL) <LOQ (0.00394 ug/mL) <LOO (0.00394 ug/mL) <LOQ (0.00394 ug/mL) <LOQ (0.00394 ug/mL) 0.00 0.00 0.00 0.00 121% Average PFOS ug/mL <LOQ <LOQ <LOQ <LOO <LOQ <LOO <LOO <LOQ RSD Std. Dev. MS/MSD RPD NA NA NA NA NA NA NA NA Concentration of PFOSA ug/mL e r % Ree <LOQ (0.00493 ug/mL) <LOQ (0.00493 Ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOO (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOO (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.(M)493 ug/mL) <LOQ (0.00493 ug/mL) 141% Average PFOSA UR/mL <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ RSD Std. Dev. MS/MSD RPD NA NA NA NA NA NA NA NA 020700-RTS-MSD-5 020700-RTS-MS-5 020700-RTS-MSD-5 020700-RTS-MS-6 020700-RTS-MSD-6 020700-RTS-MS-6 020700-RTS-MSD-6 020800-RTS-MS-1 020800-RTS-MSD-1 020800-RTS-MS-l 020800-RTS-MSD-l 020800-RTS-MS-2 121% NA NA 120% 101% NA NA 80% 83% NA NA 81% 121% NA 110% NA 82% NA 0% NA 17% NA 4% NA 137% 123% 125% 143% 140% 128% 124% 93% 110% NA NA 93% 139% 2nd 2nd 124% 141% 2nd 2nd 126% 101% NA 3% 2% 2% 3% 17% NA Group 1 Control 0.0 mg/kg Group 1 Control 0 .0 mg/kg 020800-RTS-MSD-2 020800-RTS-MS-2 020800-RTS-MSD-2 C90778M-MS-5 C90778M-MSD-6 020900-RTS-MS-5 020900-RTS-MSD-6 020900-RTS-MS-5 020900-RTS-MSD-6 C907I2M C907I6M C90722M C90724M C90726M C90728M C90735M C90742M C90743M C90747M C90750M C90758M C90765M C90778M C91I27F C9113IF C9I138F C9I144F C91148F C91I57F 77% NA NA 72% 73% 97% 101% NA NA <LOQ (0.00394 ug/mL) <LOQ (0.00394 ug/mL) 0.01 0.0116 <LOQ (0.00394 ug/mL) 0.0131 <LOQ (0.00394 ug/mL) 0.00 <LOQ (0.00394 ug/mL) 0.01 0.0504 <LOQ (0.00394 ug/mL) <LOQ (0.00394 ug/mL) 0.0107 0.0413 0.0342 0.0095 0.087 0.0217 0.0171 79% NA 72% 99% NA 0.00936 5% NA 1% 4% NA 131 0.0123 105% NA NA 72% 72% 107% 104% NA NA <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 UR/mL) <LOQ (0,(K)493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug'mL) 99% NA 72% 105% NA <LOQ 12% NA 0% 3% NA NA NA C91I59F C91166F 0.0333 0.0171 <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) Group 2 Low Dose 3.00mg/kg C9I172F C9I176F C91183F C9I188F C91190F C90781M C90782M C90783M C90785M C90787M 0.0086 <LOQ (0.00394 ug/mL) 0.0189 0.0560 <LOQ (0.00394 UR/mL) 0.0819 0.405 1.52 0.0665 1.26 0.0271 87.2 0.0237 <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/ml.) <LOQ (0.00493 UR/mL) 0.00670 0.0128 (10304 0.0217 0.0125 <LOQ NA NA C90788M C9079IM C90794M C90799M C90804M C90809M C908I0M C908I1M 3.69 1.89 2.19 0.502 0.319 4.59 0.142 0.304 0.0395 0.0139 0.0374 0.00900 0.00728 0.0339 0.0213 <LOQ (4.93 ng/mL) C908I2M C908I5M C90823M C90829M C90830M 0.175 0.327 0.86 1.42 4.56 0.00590 0.00515 0.00667 0.0227 0.0370 C90832M C90835M 0.87 0.29 0.0314 0.0196 C90838M C90840M 0.184 0.215 120 1.18 1.41 0.0115 0.00574 0.0187 64.0 0.0119 Group 2 Low Dose 3.00 mg/kg C91I97F C9120IF C9I207F C9I2I6F C9I220F C9I221F C91227F C91232F C91235F C9I236F C91242F C9I243F 1.59 0.0170 1.50 0.0133 5.89 0.0492 EE 4.82 0.0504 0.96 0.00943 4.12 0.0166 4.62 0.253 9.98 0.309 3.70 0.129 2.98 70.7 0.0621 1.13 3.75 2.65 0.0220 0.U846 122.5058 0.1037 A= CCVs analyzed bracketing these data were within criteria but had peak areas slightly above the valid linear range. LAC 05/03/01 E = Lost during extraction, no sample remaining to reextract PFOS = Perfluorooctanesulfonate Corrected PFOS LOQ (0.00492 ug/mL) to include sld correction factors PFOSA = l'erfluorooctaneaulfonamide new LOQ is 0.00394 ug/mL. LAC 02/19/01 PFOSAA = Periluorooclanesulfonamidoacelale ElFOSE - Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2COO) PFOSFA = Perfuorooctane sulfonyl ethylamide Concentra tien e f PFOSAA ug/mL or % Ree LOQ (0.00493 ug/mL) A LOO (0.00493 UR/mL) A <LOQ (0.00493 ug/mL) <LOO (0.00493 ue/mL) <1.00(0.0248 ug/mL) <LOQ (0.02*8 UR/mL) LOQ (0.00493 ug/mL) <LOO (0.00493 ue/mL) <LOQ (0.(H)493 ug/mL) A A <LOO (0.00493 ue/mLI <LOQ (0.00493 ug/mL) <LOQ (0.00493 ua/mL) <LOQ (0.0248 ug/mL) <LOO (0.0248 UR/mL) LOQ (0.0248 ug/mL) >:LOO (0.0248 ue/mL) 125% 123% NA NA 126% 123% NA NA 113% 105% A NA NA 119% 100% A NA NA 71% 70% 135% 144% 124% 126% 2nd 2nd <LOQ (0.00493 ug/rnL) <LOQ (0.00493 ug/rnL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/ml.) <LOQ (0.00493 ug/mL) <1>Q (0.00493 ug/mL) <l-OQ (0.00493 ug/mL) <I-OQ (0.00493 ug/mL) <I-OQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <IjOQ (0.00493 ug/mL) <l-OQ (0.00493 ug/mL) <l-OQ (0.00493 ug/rnL) 0.141 0.538 O642 0.189 0.289 0 84 0.81 0.670 0.212 0.214 0.94 0.764 0.105 0.617 0.278 0.174 0.475 0.579 1.56 0.684 0.769 0.685 0.327 0.368 0.63 E 1.30 0.380 0.609 3.60 4.39 2.72 1.37 0.896 PFOSAA ug/ml. <100 <LOO <LOQ <IXK> <LOO <LOO <LOQ <LO0 124% NA 124% NA 109% NA 110% NA 70% 139% 125% <1-00 <LOQ 0.553 1.51 Date Entered/By: Dale Verified/By: Purity Entered/Verified: 03/06/00.03/10/0, 03/20/00,03/21/00,4/17/(81,5/16/00,06/22/00,06/23/00.06/26/00,09/05/00,10/17/00.04/13/01 IAC/CSH 4/17/01 mmh 4/30/01 hoj/04/30/01 IAC 02/19/01 LAC RSD Std. Dev. MS/MSD RPD NA NA NA NA NA NA NA NA 2% NA 2% NA 8% NA 18% NA 1% 7% 2% NA NA NA NA 62.4 0.345 94 1.42 3MEnvironmental Laboratory Page 231 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product Numbei(Tesl Substance): Matrix: Method'Re vision: Analytical Equipment System Number Instrument Soflware/Version: Filename: R-Squaied Value: Slope: Y-Intercept Dales of Extrachon'Analyst: Dales of Analysis/Analyst: Date ofData Reduction'Analysl: Sample Data 104 Week Dietaty Carcinogenicity Study with Narrow Range (98.I%)N-Elhyl Perfluorooctanesulfonamido Ethanol in Rata T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 &ETS-8-5.1 Amelia 062498, Davey 070799 Maaslynx 3.3 & 3.4 See Below See Attachments See Attachments See Attachments 02/07/00,02/08/00.02/09/00 SAL/RWW 02/18/00,03/15/00,4/18/00,4/19/00,06/19/00,06/20/00,08/16/00,08/23/00 MMH/IAS'CSH 02/21/00,03/16/00,4/19/00,4/20/00,06/20/00,06/21/00,08/18/00,08/25/00,04/11/0! MMH/1ASHOJ Box 00-009 WEEK 105 RAT SERA Group Sample 1 Concentration RSD Concentra ttan Dose of EtFOSE-OH EtFOSE-OH Std. Dev. of M5S6 U(/raL o r % Ree MS/MSD RPD ug/mL or % Ree Method Blk 020700-1120 Blk-5 <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) A 020700-H20 Blk-6 <LOO (0.00977 ue/mL) <LOQ NA <LQQ (0.00977 ug/mL) A 020800-H20 Blk-I <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) A 020800-H20 Blk-2 <LOO (0.00977 ue/mL) <LOO NA <LOQ (0.00494 ug/mL) 020900-H20 Blk-5 <LOQ (0.0248 ug/mL) <LOQ (0.00494 ug/mL) 020900-H20 Blk-6 <LOO (0.0248 ug/mL) <LOO NA <LOQ (0.00494 ug/mL) Matrix Blk 020700-RBS Blk-5 <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) A 0207(H)-RBS Blk-6 <LOO (0.00977 uc/mU <LOQ NA <LOQ (0.00977 ug/mL) A 020800-RBS Blk-1 <LOQ (0.00977 ug/mL) <LOQ (0.00494 ug/mL) 020800-RBS-Blk-2 <LOO (0.00977 ug/mL) <LOO NA <IXX5(0.(H)494 ug/mL) 020800-RTS Blk-I <LOQ (0.00977 ug/mL) <LOQ 0.<H)497 ug/mL) 020800-RTS-Blk-2 <LOO (0.00977 ug/mLl <LOQ NA <LO0 0.00497 ug/mL) 0209(H)-RBS Blk-5 <LOQ (0.0248 ug/mL) <LOQ (0.00494 ug/mL) 020900-RBS-Blk-6 <LOO (0.0248 ug/mL) <LOQ NA <LOQ (0.00494 ue/mL) 020900-RTS Blk-5 <LOQ (0.0248 ug/mL) <LOQ (0.00494 ug/mL) QC-250ppb 020900-RTS-Blk-6 020700-RTS-MS-5 <LOO (0.0248 ug/mL) 34% <LOQ NA <LOQ (0.00494 ue/mL) 153% 020700-RTS-MSD-5 28% 31% 19% 153% 020700-RTS-MS-5 NA 139% 2nd 020700-RTS-MSD-5 NA NA NA 145% 2nd 020700-RTS-MS-6 33% 146% 020700-RTS-MSD-6 26% 30% 23% 142% 020700-RTS-MS-6 NA 143% 2nd 020700-RTS-MSD-6 NA NA NA 141% 2nd 020800-RTS-MS-1 21% 100% 020800-RTS-MSD-1 25% 23% 20% 102% A 020800-RTS-MS-1 32% 2nd NA 020800-RTS-MSD-1 NA 32% NA NA 020800-RTS-MS-2 21% 100% 020800-RTS-MSD-2 020800-RTS-MS-2 25% 23% 38% 2nd 17% 93% A NA 020800-RTS-MSD-2 NA 38% NA NA C90778M-MS-5 122% 93% C90778M-MSD-6 127% 125% 4% 86% 0209(H)-RTS-MS-5 26% 137% 020900-RTS-MSD-6 29% 27% 10% 139% t)209(H)-RTS-MS-5 37% 2nd 131% 2nd 0209(H)-RTS-MSD-6 39% 2nd 38% 4% 127% 2nd Group 1 C90712M <LOQ (0.00977 ug/mL) <LOQ (0,(H)494 ug/mL) Control 0.0 mg/kg C90716M C90722M <LOQ (0.(H>977 ug/mL) <LOQ (0.(H)977 ug/mL) <LOQ (0,(H)494 ug/mL) <LOQ (0.00494 ug/mL) C90724M <LOQ (0.(H77 ug/mL) <LOQ (0.00494 ug/mL) C90726M <LOQ (0.00977 ug/mL) <LOQ (0.00494 ug/mL) C90728M <LOQ (0.00977 ug/mL) <LQQ (0.<H>494 ug/mL) C90735M <LOQ (0.00977 ug'mL) <LOQ (0.lH)494 ug/mL) C90742M <LOQ (0.00977 ug/mL) <LOQ (0.00494 ug/ml.) C90743M <LOQ (0.00977 ug/mL) <LOQ (0.00494 ug/mL) C90747M <LOQ (0.00977 ug/mL) <LOQ (0.00494 og/mL) C9O750M <LOQ (0.00977 ug/mL) <LOQ (0.00494 ug/mL) C90758M <LOQ (0.00977 ug/mL) <LOQ (0.00494 ug/mL) C90765M <LOQ (0.00977 ug/mL) NA <LOQ (0.00494 ug/mL) C90778M <LOQ (0.00977 ug/mL) <LOQ NA <LOQ (0.00494 ug/mL) Group 1 C91I27F <LOQ (0.00977 ug/mL) <LOQ (0.00494 ug/mL) Control 0 .0 mg/kg C91I3IF C91I38F <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) C91144F <LOQ (0.00977 ug/mL) <LOQ (0.00494 ug/mL) C91148F <LOQ (0.00977 ug/mL) <LOQ (0.00494 ug/mL) C9I157F <LOQ (0.00977 ug'mL) <LOQ (0.00494 ug/mL) C9I159F <LOQ (0.00977 ug/mL) <LOQ (0.00494 ug/mL) C9I166F <LOQ (0.00977 ug/mL) <LOQ (0.(H)494 ug/mL) C9I172F <LOQ (0.00977 ug/mL) <LOQ (0.00494 ug/mL) C91176F <LOQ (0.00977 ug/mL) <LOQ (0.00494 ug/mL) C91183F <LOQ (0.(H)977 ug/mL) <LOQ (0.00494 ug/mL) C91I88F <LOQ (0.00977 ug/mL) NA <LOQ <0.00494 ug/mL) C91I90F <LOQ (0.00977 ug/mL) <LOQ NA <LOQ (0.00494 ug/rnL) Group 2 Low Dose 3.00 mg/kg C90781M C90782M C90783M C90785M <LOQ (0.00977 ug/mL) <-LOQ (0.(K)977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) 0.0445 0.123 0.264 0.0362 C90787M <LOQ (0.00977 ug/mL) 0.0768 C90788M C9079IM <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) 0.534 0.195 C90794M <LOQ (0.00977 ug/mL) 0.217 C90799M <LOQ(0.00977 ug/mL) 0.161 C90804M <LOQ((MH)977 ug/mL) 0.0215 C90809M <LOQ (0.00977 ug/mL) 0.255 C908I0M <LOQ (0.00977 ug/mL) 0.0558 C908I1M <LOQ (0.00977 ug/mL) 0.0916 C908I2M <LOQ (0.00977 ug/mL) 0.0610 C90815M <LOQ (0.00977 ug/mL) 0.112 C90823M <LOQ (0.00977 ug/mL) 0.175 C90829M <LOQ (0.00977 ug/mL) 0.145 C90830M <LOQ (0.00977 ug/mL) 0.276 C90832M <LOQ (0.00977 ug/ml.) 0.122 C90835M <LOQ (0.00977 ug/mL) 0.0499 C90838M <LOQ (t).(H)977 ug/mL) NA 0.0950 C90840M <LOQ ((MHI977 ug/mL) 'L O Q NA 0.0888 Group 2 C91197F <LOQ (0.00977 ug/mL) 0.285 Low Dose C9120IF <LOQ (0,(K)977 ug/mL) 0.2(H) 3.00 mg/kg C91207F <LOQ (0.(K)977 ug/mL) 0.3(H) C91216F E E C91220F <LOQ (0.00977 ug/mL) 0.355 C9122IF <LOQ (0.00977 ug'mL) 0.118 C91227F <LOQ (0.00977 ug/mL) 0.164 C9I232F <LOQ (0.00977 ug/mL) 1.59 C9I235F <LOQ (0.00977 ug/mL) 1.90 C9I236F <LOQ (0.00977 ug/mL) 1.43 C9I242F C9I243F <LOQ (0.H1977 ug/mL) <LOQ (0.00977 ug/ml.) <l o q : NA NA 0.980 0.166 CCVs analyzed bracketing these data were within criteria but had peak areas slightly above the valid linear range. LAC 05/03/1H E = Lost during extraction, no sample remaining to reextract. Average MS56 <LOQ <LOQ <LOQ <LOO <LOQ <LOQ <LOQ <LOQ 153% 142% 144% 142% 101% NA 96% NA 90% 138% 129% LOQ <LOQ 0.145 0.680 PFOS Perfluorooctanesullonate PFOSA = Periluorooclanesulfonamide PFOSAA = Pertluorooclanesulfonamidoacelale EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamjdo ethyl alcohol M556 = C8F17S02N((H)CH2COO) PFOSEA - Perfuorooclane sulfonyl ethylamide Corrected PFOS LOQ (0.00492 ug/mL) to include sld correction factors new LOQ is 0.00394 ug/mL LAC 02/19/01 RSD Std. Dev. MS/MSD RPD NA NA NA NA NA NA NA NA 0% 4% 3% 1% 1% NA 7% NA 8% 1% 3% NA NA NA NA 79.4 0.115 98 0.667 Concentra lien of PFOSEA u|/m L or % Ree <I-OQ (0.00492 ug'mL) <LOQ (0.00492 ug'mL) <LOQ ((MKI492 ug'mL) <LOO (0.00492 ue/mLl <LOQ (0.00492 ug/mL) <LOO (0.00492 ug'mL) <LOQ (0.00492 ug/mL) <LOO (0.00492 ue/mL) <LOQ (0.(H)492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOO (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mU <LOQ (0.00492 ugmL) <LOO (0.00492 ug/mL) 79% 75% NA NA 79% 60% NA NA 46% 65% 42% 2nd NA 46% 56% 45% 2nd NA 83% 87% 61% 60% 57% 2nd 56% 2nd <LOQ (0.00492 ug/ml.) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/ml.) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ(0.(H)492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0,(H)492 ug/mL) <LOQ (0.1HI492 ug/mL) <LOQ((MH)492 ug/mL) <LOQ (0.00492 ug/mL) <IGQ (0.00492 ug/mL) <I.OQ (0.00492 ug/mL) <LOQ (0.(HI492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0,(H)492 ug/mL) <LOQ (0.04)492 ug/mL) <LOQ(0.(H)492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <l-OQ (0.(H)492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug'mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug'mL) <LOQ (0.00492 ug/mL) <LOQ (0.1HI492 ug/ml.) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.IM1492 ug/ml.) <LOQ (0.(K)492 ug'mL) LOQ (0.00492 ug/ml.) 'L O Q (0,(H)492 ug'mL) 'L O Q (0.00492 ug/ml.) <I.OQ (0.IKI492 ug/mL) <LOQ (0.00492 ug/ml.) ' LOQ (0.00492 ug/mL) <LOQ (0.HI492 ug/ml.) <LOQ (0.00492 ug/ml.) <LOQ (0.(M)492 ug/mL) K <LOQ(0.(H)492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ(0.(H)492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 uc'mL) PFOSEA 'L O O <LOO <L00 'L O O <LOO <LOO 'L O O <LOO 77% NA 70% NA 55% 42% 51% 45% 85% 60% 57% <LOQ <LOQ <LOQ <LOQ Date Entered/By: Date Verified/ By: Purity Entered/Verifed: 03/06/00,03/10/00, 03/20/00,03/21/00, 4/17/00. 5/16/00, 06/22/00.06/23/00,06/26AK), 09/05/00, 10/17/00.04/13/01 LAC/CSH 4/17/01 mmh 4/30/01 ho; / 04/30/01 LAC 02/19/01 LAC RSD Std. Dev. MS/MSD RPD NA NA NA NA NA NA NA NA 5% NA 27% NA 34% NA 18% NA 4% t% 2% NA NA NA NA NA NA NA NA 3MEnvironmental Laboratory Page 232 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product Number(T#st Substance): 104 W eek D ietary Carcinogenicity Study with N arrow Range (98.1% ) N -Ethyl Perfluorooctanesulfonam ido E thanol in Rats T-6316 (EtFOSE-OH) Matrix: Rat Serum M ethod/R evision: ETS-8-4.1 & ETS-8-5.I Analytical Equipment System Number: Amelia 062498, Davey 070799 Instrument Software/Version: M asslynx 3.3 & 3.4 Filename: See Below R-Squared Value: See Attachments Slope: See Attachments Y -lntercept: See Attachments Dates o f Extraction/Analyst: 02/07/00, 02/08/00, 02/09/00, 2/24/00 RW W , SAL Dates o f Analysis/Analyst: 0 2/18AM), 02/25/00, 03/27/00, 0 6 /01/00,06/19/00, 06/20/00, 08/02/00, 08/16/00, 08/23/00 M M H /IA S Date o f Data Reduction/Analyst: 02/21/00, 02/29/00, 02/29/00, 06/06/00, 06/02/00, 06/20/00, 06/26/00, 08/03/tK), 08/18/00, 08/25/(H) M M H /IA S/H O J Sample Data Box 00-009 WEEK 105 RAT SERA lot 171 G roup Dose G roup 3 M id Dose 30.0 mg/kg S am p le ff C90842M C90844M C90850M E x trac tio n Voi. 1 1 1 Surrogate Verified NA NA NA PFOS Std C o rrec tio n Factor 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 PFOS Purity C o rrec tio n Factor 0.8640 0.8640 0.8640 PFOS D ilu tio n F a c to r 500 50 50 PFOS Cone. ng/m L 102 115 273 F ilenam e A 060100050 A04()60(X)39 A040600040 C o n cen tratio n of PFOS ug/mL or % Ree 40.7 4 61 11.0 C90851M C90854M C90855M C908S6M C90858M C90860M C90864M 1 NA 0 .9 2 7 5 0.8640 50 224 A04060004I 8.98 1 NA 0 .9 2 7 5 0.8640 50 683 A040600042 27.3 1 NA 0 .9 2 7 5 0 .8 6 4 0 50 483 A040600046 19.4 1 NA 0 .9 2 7 5 0.8640 50 112 A040600047 4.49 1 NA 0 .9 2 7 5 0.8640 50 670 A 040600048 26.9 1 NA 0 .9 2 7 5 0.8640 500 208 A0601(H)102 83.2 1 NA 0 .9 2 7 5 0.8640 50 667 A040600050 26.7 C90865M C90867M C90869M C90871M C9088IM C90882M C90883M C90884M 1 NA 0 .9 2 7 5 0 .8 6 4 0 50 402 A0406(HH)54 16.1 1 NA 0 .9 2 7 5 0 .8 6 4 0 500 122 A 060100051 48.9 1 NA 0 .9 2 7 5 0 .8 6 4 0 50 155 A040600056 6.22 1 NA 0 .9 2 7 5 0.8640 50 420 A 040600062 16.8 1 NA 0 .9 2 7 5 0.8640 50 460 A 040600063 18 4 1 NA 0.9275 0.8640 50 592 A040600064 23.7 1 NA 0.9275 0.8640 50 374 A 040600057 15.0 1 NA 0.9275 0.8640 50 391 A040600065 15.7 C90885M C90889M C90893M C90900M 1 NA 0.9275 0.8640 50 623 A040600058 24.9 1 NA 0.9275 0.8640 50 159 A040600066 6 .3 5 1 NA 0.9275 0.8640 50 578 A040600071 23.2 1 NA 0.9275 0 .8 6 4 0 50 387 A040600070 15.5 G roup 3 M id Dose 30.0 mg/kg C91252F C91253F C9I254F 1 NA 0 .9 2 7 5 0 .8 6 4 0 100 577 A 040600014 46.2 1 NA 0 .9 2 7 5 0 .8 6 4 0 100 674 A040600015 54.0 1 NA 0 .9 2 7 5 0.8640 1000 119 A 060100049 95.5 C91256F 1 NA 0 .9 2 7 5 0.8640 100 823 A 0406000I7 66.0 C91264F 1 NA 0 .9 2 7 5 0.8640 100 571 A0406(XH)18 45.7 C91278F C91279F C91286F 1 NA 0.9275 0.8640 1000 138 A0601D0100 no 1 NA 0 .9 2 7 5 0 .8 6 4 0 1(H) 139 A 040600023 11.2 1 NA 0 .9 2 7 5 0 .8 6 4 0 1(H) 868 A 040600024 69.5 C91292F 1 NA 0 .9 2 7 5 0.8640 100 210 A040600025 16.9 C91294F C91295F C91301F C91303F 1 NA 0 .9 2 7 5 0.8640 100 774 A0406(HH)26 62.0 1 NA 0 .9 2 7 5 0.8640 1(H) 185 A040XK)30 14.8 1 NA 0 .9 2 7 5 0 .8 6 4 0 1(H) 753 A 04060003I 60.4 1 NA 0 .9 2 7 5 0 .8 6 4 0 5(H) 128 A060100101 51.4 C91307F 1 NA 0 .9 2 7 5 0.8640 100 883 A040600033 70.8 C91310F 1 NA 0 .9 2 7 5 0.8640 1(H) 665 A040600034 53.3 PFO S = Perfluorooctanesulfonate PFOSA = Pertluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonamidoacetate EtFO SE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2C00) PFO SEA " Perfuorooctane sulfonyl ethylamide Date Entered/By: D ate V erified/ By: Purity Entered/Verified: 03/06/00, 0 3 /1 0 /0 0 ,0 3 /2 0 /0 0 , 03/21/00, 04/16/00, 05/16/00, 06/12/00, 06/22/00, 06/23/00,06/26/00, 08/15/00, 09/05/00, 10/17/00 LAC/CSH 4/30/01 h o j / 04/30/01 LAC 02/19/01 LAC PFOS RSD Std. Dev. M S/M SD RPD 80.0 22.0 17.6 49.7 55.2 27.4 ' 3MEnvironmental Laboratory Page 233 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product N umbeifTest Substance): 104 W eek Dietary C arcinogenicity Study with N arrow Range (98.1% )N -E thy) Perduorooctanesuifonam ido Eithanol in Rats T-6316 (EtFOSE-OH) Matrix: Rat Serum M ethod/Revision: ETS-8-4.1 & ETS-8-5.1 Analytical Equipment System Number: Amelia 062498, Davey 070799 Instrument Soflware/Version: M asslynx 3.3 & 3.4 Filen am e: See Below R-Squared Value: Slope: Y -lntercept: Dates o f Extraction/Analyst: See Attachments See Attachments See Attachments 02/07/00, 02/08/00, 02/09/00, 2/24/00 RWW, SAL Dates o f Analysis/Analyst: 02/18/00, 02/25/00, 03/27/00,06/01/00, 06/19/00, 06/20/00, 08/02/00, 08/16/0), 08/23/00 MMH/IAS Date o f Data Reduction/Analyst: Sample Data 02/21/00, 0 2 /29/00,02/29/00, 06/0(5/00, 06/02/00, 06/20/00, 06/26/00, 08/03/(0, 08/18/00, 08/25/00 M M H /IA S/H O J Box 00-009 WEEK 105 RAT SERA lo tL -1 5 7 0 9 Dose Group 3 M id Dose 30.0 mg/kg Group 3 M id Dose 30.0 mg/kg Sample # C90842M C90844M C90850M C90851M C90854M C90855M C90856M C90858M C90860M C90864M C90865M C90867M C90869M C90871M C90881M C90882M C90883M C90884M C90885M C90889M C90893M C90900M C91252F C9I253F C91254F C91256F C91264F C91278F C91279F C91286F C91292F C91294F C9I295F C9I301F C91303F C91307F C91310F PFOSA Purity Correction Factor Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA ' NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOSA Dilution Factor 1 1 1 1 1 10 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 10 1 1 1 1 1 1 1 1 1 PFOSA Cone. D g /m L 196 155 187 83.7 287 34.6 223 217 338 272 238 430 258 343 536 482 436 232 414 315 459 296 369 484 380 572 340 71.7 206 497 447 542 306 263 368 536 401 Filename A060100052 A060100053 A060100056 A ('6(11(KM)17 A<'60100057 A ('40600080 A( '60100105 A ('60100107 A( 60100108 A( 60100058 1X81600040 A< 60100059 A (60100109 A (60100110 A f60100060 A f60100063 AC60I00022 AC6 0 100064 DC81600041 A C60100!11 All 60100065 A060100066 AO60100114 A 060100I15 A 060100116 A 060100117 D081600044 A0227(XH)24 A0G01(KK)71 A 060100118 A0601(M)I21 A050KKM172 A0501000IS A050100122 A0SO1OO123 A0 50100073 AO SOI (NX) 16 Concentration o f PFOSA ug /m L or % Ree 0 .1 9 6 0.155 0.187 0.0837 0.287 0.346 0.223 0.217 0.338 0.272 0.238 0.430 0.258 0.343 0.536 0.482 0.436 0.232 0.414 0 .3 1 5 0.459 0.296 0.369 0.484 0.380 0.572 0 .3 4 0 0 .7 1 7 0.206 0 .4 9 7 0 .4 4 7 0 .5 4 2 0.306 0 .2 6 3 0 .3 6 8 0.536 0.401 Average PFOSA 0.306 0.429 PFOS = Perfluorooctanesulfonate PFOSA = Perfluorooctanesulfonamide PFOSAA = Periluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonam ido ethyl alcohol M 556 - C8F17SO2N((H)CH2CO0) PFOSEA = Perfuorooctane sulfonyl ethyiamide Date Entered/By: D ate V erified/ By: Purity Entered/Verified: 03/06/00, 03/10/00, 03/20/00, 03/21/00, 04/16/00, 05/16/00, 06/12/00, 06/22/00, 06/23/00, 06/26/00, 0 8 /15AM), 09/05/00, 10/17/00 LAC/CSH 4/30/01 hoj / 0 4 /3 0 /0 1 LAC 02/19/01 LAC RSD Std. Dev. MS/MSD RPD 37.9 0.116 30.9 0.133 3MEnvironmental Laboratory Page 234 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product NumberfTest Substance): M a tr ix : M eth o d /R ev isio n : Analytical Equipment System N um ber Instrument Soflware/Version: Filename: R-Squared Value: Slope: Y-Intercept: Dates o f Extraction/Analyst: Dates o f Analysis/Analyst: 104 W eek D ietary Carcinogenicity Study w ith Narrow Range (98.1% ) N -Ethyl Perfluorooctanesulfonam ido E thanol in Rats T -6 3 16 (EtFOSE-OH) Rat Serum ETS-8-4.1 & ETS-8-5.1 Amelia 062498, Davey 070799 M asslynx 3.3 & 3.4 See Below See Attachments See Attachments See Attachments 02/07/00, 02/08/00, 02/09/00, 2/24/00 RW W , SAL * 02/18/00, 02/25/00, 03/27/00, 06/01/00, 06/19/00, 06/20/00, 08/02/00, 08/16/00 08/23/00 M M H /IA S Date o f Data Reduction/Analyst: Sample Data WEEK 105 RAT SERA 02/21/00, 02/29/00, 02/29/00, 06/06/00, 06/02/00, 06/20/00, 06/26/00, 0 8 /0 3 / , 08/18/00, 08/25/00 M M H /IA S/H O J Box 00-009 lot T-7121.1 Sam ple # PFOSAA Purity C o rrec tio n Factor G roup 3 M id Dose 30.0 mg/kg C90842M C90844M C90850M C90851M Unknown Unknown Unknown Unknown C90854M C90855M C90856M Unknown Unknown Unknown C90858M Unknown C90860M Unknown C90864M Unknown C90865M Unknown C90867M Unknown C90869M Unknown C90871M Unknown C90881M Unknown C90882M Unknown C90883M C90884M C90885M Unknown Unknown Unknown C90889M Unknown C90893M C909)M Unknown Unknown G roup 3 M id Dose C91252F C91253F Unknown Unknown 30.0 mg/kg C91254F Unknown C91256F Unknown C91264F Unknown C9I278F Unknown C9I279F Unknown C91286F C91292F C91294F Unknown Unknown Unknown C91295F Unknown C91301F Unknown C91303F C91307F Unknown Unknown C91310F Unknown PFOS " Perfluorooctanesulfonate PFOSA = Perfluorooctanesulfonamide PFOSAA = Periluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M 556 = C8F17S02N((H)CH2C00) PFOSEA = Perfuorooctane sulfonyl ethylamide Surrogate V erified Confirm ed High NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOSAA D ilution Factor 10 10 10 10 10 10 10 10 to 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 100 10 10 10 10 10 10 in 10 10 PFOSAA Cone. ng/m L 187 132 308 98.4 715 828 509 379 376 355 166 287 455 330 472 390 435 2% 605 652 481 647 373 733 646 791 316 95.9 334 932 525 781 614 349 524 721 614 Filenam e A040600072 A040600073 A040600074 A040600078 A040600079 A040600080 A040600081 A040600082 A040600086 A040600087 A040600088 A0406(XM)89 A040600090 A040600094 A040600095 A040600096 A040600097 A040G00098 A040600102 A040600103 A 040600104 A040600105 A0227(XX)17 A 0227000I8 A022700019 A0227(KX)20 A022700021 A060100103 A0227(XK)25 A0227(XX)26 A0227(KX)27 A0227(XX)28 A022700031 A022700032 A022700033 A022700034 A0227(XX)35 C o n cen tratio n of PFOSAA ug/mL o r % Ree 1.87 1 '12 3.08 0.984 7.15 8.::8 5 .0 9 3.79 3.76 3 .5 5 1 .0 6 2 .8 7 4 .5 5 3 .3 0 4.72 3 .5 0 4.35 2 .9 6 6.05 6.52 4.81 6.47 3 .7 3 7.33 6.46 7.91 3.16 9 59 3.34 9.32 5.25 7.81 6.14 3.49 5.24 7.21 6 .1 4 A verage PFOSAA ug/m L 4 .1 4 6 .1 4 Date Entered/By: D ate V erified/ By: Purity Entered/Verified: 03/06/00, 03/10/00, 03/20/00, 03/21/00, 04/16/00, 05/16/00, 06/12/00, 06/22/00, 06/23/00, 06/26/00, 08/15/00, 09/05/00, 10/17/00 L A C 'C SH 4/30/01 h o j / 04/30/01 LAC 02/19/01 LAC RSD Std. Dev. M S/M SD RPD 46.4 1.92 34.2 2 .1 0 3MEnvironmental Laboratory Page 235 3M M edical D epartm ent Study: T6316.1 A M D,,T # 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product Number(Test Substance): 104 W eek Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfiuoroootancsulfonamido Ethanol iri Rats T-6316 (EtFOSE-OH) Matrix: Rat Serum Method/Revision: ETS-8-4.1 &ETS-8-5.1 Analytical Equipment System Number: Amelia 062498, Davey 070799 Instrument Software/Version: M asslynx 3.3 & 3.4 Filename: See Below R-Squared Value: See Attachments Slope: See Attachments Y-Inlercept: See Attachments Dates o f Extraction/Analyst: 02/07/00, 02/08/00, 02/09/00, 2/24/00 RWW, SAL Dates o f Analysis/Analyst: 02/18/00, 02/25/00, 03/27/00, 06/01/00, 06/19/00, 06/20/00, 08/02/4X), 08/16/00, 08/23/00 MMH/1AS Date o f Data Reduction/Analyst: 02/21/00, 02/29/00, 02/29/00, 06/06/00, 06/02/00, 06/20/00, 06/26/4X1, 08/03/00, 08/18/00 08/25/4X1 M M H/IAS/HOJ Sample Data Box 00-009 WEEK 105 RAT SERA Dose Sample It Group 3 M id Duse 30.0 mg/kg C90842M C90844M C90850M C90851M C90S54M C90855M C90856M C90858M C90860M C90864M C90865M C90867M C90869M lot Unknown/SD013 EtFOSE-OH Purity Correction Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA EtFOSE-OH Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 EtFOSE-OH 5 .1 5 1.89 5 .1 3 .8 2 1.90 3 . 37 3.76 3.30 4.90 10.3 5.47 6.66 6.06 Filename A080200017 A080200018 A080200019 A080200020 A08020002I A0802<XM)24 A08G200025 A080200026 A080200027 A080200028 A080200031 A080200032 A080200033 Concentration o f EtFOSE-OH ug/niL or % Ree 0.00515 <LOQ (0.(X)493 ug/mL) 0.4X1510 <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.4X1493 ug/mL) <LO Q (3.4X1493 ug/mL) <LO Q (0.(X)493 ug/m L) 0.0103 0.00547 <1.4X1666 0.00606 C90871M C90881M C90882M C90883M Unknown Unknown Unknown Unknown NA NA NA NA 1 2.60 A080200034 <LO Q (0.4X1493 ug/m L) 9.89 A080200035 0.4K1989 1 18.2 A080200038 0.0182 1 1.86 A 080200039 <LOQ (0.00493 ug/m L) Group 3 M id Dose 30.0 mg/kg C90884M C90885M C90889M C90893M C90900M C91252F C91253F C9I254F C91256F C9I264F C91278F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA 1 3.89 A080200040 <LOQ (0.00493 ug/mL) 1 15.2 A080200041 0.0152 1 7.71 A08()2(XX)42 0.00771 1 10.6 A 080200045 0.0106 1 4.68 A 080200046 <LO Q (0.(X)493 ug/m L) 1 8.42 A080200047 0.00842 1 8 56 A08020(X)48 0.(X)856 1 21.3 A080200049 0 .0 2 1 3 1 5.64 A080200052 0.00564 1 5.17 A 080200053 0.4X1517 1 17.8 A 080200054 0.0178 C91279F C91286F C9I292F C9I294F C91295F C91301F C91303F C91307F C91310F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA 2nd Analysis OK NA NA 1 1.90 A08020<M)55 <I.O Q (0.00493 ug/m L) 1 6.46 A080200056 (1.4X1646 1 15.3 A080200059 0.0153 1 12.8 A080200060 0.0128 1 0 .5 7 0 A08020(X)61 <LO Q (41.4X1493 ug/m L) 1 6.03 A0802(XM)62 <1.00603 1 9.21 D 081600046 0.1X1921 1 12.8 A 080200066 0.0128 1 ! 1.36 A0802(XM)67 <LOQ (0.04)493 ug/mL) PFOS = Perilucirooctanesulfonate PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonam idoacetate EtFOSE = Narrow Range N-Ethyl Perfiuorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2C00) PFOSEA Perfuorooctane suifonyl ethylamide Average EtFOSE-OH (>.<X)912 0.0108 RSD Std. Dev. MS/MSD RPD 47.2 0.00430 48.4 0.4X1522 Date Entered/By: Date V erified/ By: Purity Entered/Verified: <>3/06/<X), 03/10/00, 03/20/00, 0 3 /2 1 /0 0 ,0 4 /1 6 /0 0 ,0 5 /1 6 /0 0 , 06/12/00, 06'2 2/00, 06/23/00, 06/26/(H), 08/15/00, 09/0:i/(K>, 10/17/00 LAC/CSH 4/30/01 hoj / 04/30/01 LAC 02/19/01 LAC 3MEnvironmental Laboratory Page 236 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 LRN-U2103 Study: Product Number(Test Substance): 104 W eek D ietary Carcinogenicity Study w ith N arrow Range (98.1% ) N -Ethyl Peril jorooctanesulfonam ido E thanol in Rats T-6316 (EtFOSE-OH) M atrix: Rat Serum M ethod/R evision: ETS-8-4.1 &ETS-8-5.1 Analytical Equipment System Number: Amelia 062498, Davey 070799 Instrument Software/Version: M asslynx 3.3 & 3.4 Filen am e: See Below R-Squared Value: Slope: See Attachments See Attachments Y-Intercept: Dates o f Extraction/Analyst: See Attachments 02/07/00, 02/08/00, 02/09/00, 2/24/00 RW W , SAL D ates o f A nalysis/Analyst: 0 2 /1 8 /0 0 ,0 2 /2 5 /0 0 , 03/27/00, 06/01/00, 06/19/00, 06/20/00, 08A)2/(X), 08/16/00, 08/::3 '(H) M MH/IAS D ate o f D ata Reduction/Analyst: 02/21/tX), 02/29/00, 02/29/00, 06/06/00, 06/02/00, 06/20/00, 06/26/00, 08/03/00, 08/18/00, 08/25/00 M M H /lA S/H O J Sample Data Box 00-009 WEEK 105 RAT SERA lot NB I I 3047-80 Group Dose Group 3 M id Dose Sample # C90842M C90844M M556 Purity Correction Factor Unknown Unknown Surrogate Verified Confirmed High NA M556 Dilution Factor 10 10 M556 Cone. n g /m L 254 116.0 Filename A0225IXX174 A022500075 Concentration o f M556 ug/mL or % Ree 2 .5 4 1.160 30.0 mg/kg C90850M C9085IM C90854M C90855M C90856M Unknown Unknown Unknown Unknown Unknown NA - 10 NA 10 NA 10 NA 10 N A 10 214 A 022500076 169 A 022500079 187 A 022500080 162 A022500081 278 A022500082 2 .1 4 1.69 1.87 1.62 2 .7 8 C90858M Unknown NA 10 610 A022500083 6 .1 0 C90860M Unknown NA 10 264 A 022500086 2 .6 4 C90864M Unknown NA 10 228 A022500087 2 .2 8 C90865M Unknown NA 10 337 A022500088 3 .3 7 C90867M Unknown NA 10 208 A0225(XH)89 2.08 C90869M Unknown NA 10 270 A0225(XX)90 2.70 C90871M Unknown NA 10 192 A 022500093 1.92 C90881M Unknown NA 10 378 A022500094 3.78 C90882M C90883M C90884M Unknown Unknown Unknown NA NA NA 10 294 A022500095 2.94 10 534 A0225(XK)96 5.34 10 334 A0225(XX)97 3.34 C90885M Unknown NA 10 284 A()22500i(X) 2 .8 4 C90889M Unknown NA 10 440 A022500I0I 4.40 C90893M Unknown NA 10 252 A022500102 2.52 C909(X)M Unknown NA 10 286 A022500103 2.86 Group 3 C91252F Unknown NA 10 385 A 0227000I7 3 .8 5 M id Dose C91253F Unknown NA 10 474 A022700018 4.74 30.0 mg/kg C9I254F C9I256F C91264F Unknown Unknown Unknown NA NA NA 10 324 A022700019 3 .2 4 10 291 A022700020 2.91 10 178 A022700021 1.78 C91278F Unknown NA to 323 A022700024 3.23 C91279F Unknown NA 10 176 A022700025 1 .7 6 C91286F C9I292F Unknown Unknown NA NA 10 312 A0227(XX)26 3 .1 2 10 470 A0227(XK)27 4.70 C9I294F Unknown NA 10 346 A022700028 3.46 C9I295F Unknown NA 10 209 A022700031 2.09 C91301F Unknown NA 10 348 A022700032 3.48 C91303F Unknown NA 10 381 A 022700033 3.81 C91307F Unknown NA 10 125 A022700034 1.25 C9I310F Unknown NA 10 181 A022700035 1.81 PFOS = Perfluorooctanesulfonate PFOSA = Perfluorooctanesulfonam ide PFOSAA = Perfluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M 556 = C 8 F 17S02N ((H )C H 2C O O ) PFOSEA = Perfuorooctane sulfonyl ethylamide Date Entered/By: Date V erified/ By: Purity Entered/Verified: 03/06/00, 03/10/00, 03/20/00.03/21/(8), 0 4 /16/00,05/16/00, 06/12/00, 06/22/00,06/23/00, 06/26/00, 08/15/00, 09/05/00, 10/17/00 LAC/CSK 4/30/01 h o j / 04/30/01 LAC 02/19/01 LAC Average M556 RSD Std. Dev. MS/MSD RPD 41.7 2.86 1.191 3.02 35.7 1.08 3M Environmental Laboratory Page 237 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product Number(Tesl Substance): 104 W eek Dietary Carcinogenicity Study with-Narrow Range (98.1%) N-Ethyl PerfluorooctanesUlfonamido Ethanol in Rats T-6316 (EtFOSE-OH) M ethod/Revision: Analytical Equipment System N um ber Instrument Software/Version: F i le n a m e : R-Squared Value: Slope: Y-lntercept: Dates o f Extraction/Analyst: Rat Serum ETS-8-4.1 & ETS-8-5.1 Amelia 062498, Davey 070799 M asslynx 3.3 & 3.4 See Below See Attachments See Attachments See Attachments 02/07/00, 02/08/00, 02/09/00, 2/24/<X) RW W, SAL Dates o f Analysis/Amlyst: 02/18/00, 02/25/00, 03/27/00, 06/01/00, 06/19/00, 06/20/00, 08/02/00, 08/16/00, 08/23/00 M M H /IA S Date o f Data Reduction/Analyst: 02/21/00, 02/29/00, 02/29/00, 06/06/00, 06/02/00, 06/20/00, 06/26/00, 08/03/00, 08/18/00, 08/25/00 M M H /lA S/H O J Sample Data Box 00-009 WEEK 105 RAT SERA lot 529 G roup Dose Sam ple # PFOSEA Purity C o rrec tio n Factor Surrogate Verified PFOSEA D ilu tio n Factor PFOSEA F ilenam e C o n cen tratio n o f PFOSEA ug/m L o r % Ree A verage PFOSEA ug/m L G roup 3 M id Dose 30.0 mg/kg C90842M C90844M C90850M C90851M C90854M C90855M C90856M C90858M C90860M C90864M C90865M Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA 1 0.00 A0802000I7 <LOQ (0.00452 ug/mL) 1 0.00 A080200018 <LOQ (0.00492 ug/mL) 1 0.03(H) A080200019 <LOQ (0.00492 ug/mL) 1 0(H) A080200020 <LO Q (0.(H)492 ug/inL) 1 1.04 A080200021 <LOQ (0.00492 ug/mL) 1 0.210 A080200024 <LOQ (0.00492 ug/mL) l 0.00 A 080200025 <LO Q (0.(X)492 ug/m L) 1 1.44 A080200026 <LO Q (0.00492 ug/inL) 1 0.00 A0802(HX)27 <LO Q (0.00492 ug/rnL) 1 0.00 A 080200028 <LOQ (<).(X)492 ug/inL) 1 0.00 A080200031 <LOQ (0.(K)492 ug/rnL) C90867M C90869M C9087IM C9088IM C90882M C90883M C90884M C90885M Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA 0.00 /,080200032 <LO Q (0.01)492 ug/rnL) 1 0.00 /.0802(HK)33 <LO Q (0.00492 ug/rnL) 1 0.00 A080200034 cLO Q (0.00492 ug/rnL) 1 0.00 A 080200035 <LOQ (0.00492 ug/rnL) 1 2.88 A080200038 <LO Q (0,(X)492 ug/m L) 1 0.00 A080200039 <LOQ (0.00492 ug/mL) 1 0.00 A080200040 <LOQ (0.00492 ug/mL) 1 0.0800 fi 080200041 <LOQ (0.0049 2 ug/m L) C90889M C90893M C90900M Unknown Unknown Unknown NA NA NA 1 4.85 A 080200042 <LO Q (0.0049.2 ug/m L) 1 0.480 080200045 <LO Q (0.<X)49.2 ug/m L) 1 0.00 A0802(HX)46 <LO Q (0.(X)492 ug/m L) <LOQ G roup 3 M id Dose 30.0 mg/kg C91252F C91253F C9I254F C91256F C91264F C91278F C91279F C91286F C91292F C91294F C91295F C9130IF C91303F C91307F C913I0F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA NA 2nd Analysis OK NA NA 1 1 1 1 1 1 1 1 1 1 1 1 1 1 0.00 0 .0 0 0 .0 0 0.00 0.710 0.320 0 .0 0 0.640 0.190 O.(H) 0.00 0.00 0.00 1.19 0 .0 0 080200047 080200048 080200049 080200052 080200053 080200054 080200055 080200056 A080200059 . A080200060 A080200061 A0H0200062 D0816KX146 A080200066 A0802(XH)67 <LOQ (0.0049.2 ug/mL) <I.OQ (0.00492 ug/mL) <LO Q (0.(X)492 ug/m L) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LC>Q (0.(H)492 ug/m L) <LOQ (0.00492 ug/mL) <LO Q (0.00493. ug/m L ) <LOQ (0.00492 ug/mL) <LO Q (0.(X)492 ug/m L) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ PFOS = Perfluorooctanesulfonate PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonam idoacelate EtFOSE = Narrow Range N-Ethyl PerfluorooctanesUlfonamido ethyl alcohol M556 = C8F17S02N((H)CH2C00) PFOSEA = Perfuorooctane sulfonyl ethylamide Date Entered/By: Date V erified/ By: Purity Entered/Verified: 03/06/IH), 03/10/00, 03/20/00, 03/21/00, 04/16/00, 05/16/00, 06/12/00, 06/22/00, 06/23/00, 06/26/00, 08/15/00, 09/05/00, 10/17/00 LAC/C SH 4/30/01 hoj / 04/30/01 LAC 02/19/01 LAC RSD Std. Dev. M S/M SD RPD NA NA NA NA 3MEnvironmental Laboratory Page 238 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product Numbcr(Te8t Substance): Matrix: M eth o d /R ev isio n : Analytical Equipment System Number: Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Intercept: Dates o f Extraction/Analyst: Dates o f Analysis/Analyst: Date o f Data Reduction/Analyst: Sample Data 104 W eek D ietary Carcinogenicity Study with N arrow Range (98.1% ) N -Ethyl Perfluorooctunesulfonam ido E thanol in Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 & E T S-8-5.1 Amelia 062498, Davey 070799 M asslynx 3.3 & 3.4 See Attachments See Attachments See Attachments See Attachments 02/07/00, 02/08/00, 02/09/00, 2/24/00 RW W , SAL 0 2 /1 8 /0 0 ,0 2 /2 5 /0 0 , 03/27/00, 0 6 /01/00,06/19/00, 06/20/00, 08/02/00, 08/16/00, 08/23/00 ICMH/IAS 02/21/00, 02/29/00, 02/29/00, 06/06/00, 06/02/00, 06/20/00, 06/26/00, 08/03/00, 08/18/00, C8/25/00 M M H /IA S/H O J WEEK 105 RAT SERA Dose Sample it Group 3 M id Dose 30.0 mg/kg Group 3 M id Dose 30.0 mg/kg PFO S = Pe rfiuorooctanesul fonate C90842M C90844M C90850M C90851M C90854M C90855M C90856M C90858M C90860M C90864M C90865M C90867M C90869M C90871M C90881M C90882M C90883M C90884M C90885M C90889M C90893M C90900M C9I252F C91253F C91254F C91256F C9I264F C91278F C91279F C91286F C91292F C9I294F C91295F C91301F C91303F C91307F C91310F Concentration of PFOS ug/mL or % Ree 40.7 4.61 11.0 8.98 27.3 19.4 4.49 26.9 83.2 26.7 16.1 48.9 6.22 16.8 18.4 23.7 15.0 15.7 24.9 6.35 23.2 15.5 46.2 54.0 95.5 66.0 45.7 110 11.2 69.5 16.9 62.0 14.8 60.4 51.4 70.8 53.3 Average PFOS 22.0 55.2 RSD Std. Dev. MS/MSDRPD 80.0 176 49.7 27.4 Concentration or PFOSA ug/mL or % Ree 0.196 0.155 0.187 0 .0 8 3 7 0 .2 8 7 0.34590(H) 0 .2 2 3 0 .2 1 7 0.338 0 .2 7 2 0 .2 3 8 0 .4 3 0 0.258 0.343 0 .5 3 6 0 .4 8 2 0.436 0.232 0.414 0.315 0.459 0 .2 9 6 0.369 0.484 0.380 0.572 0.340 0.7173000 0.206 0.497 0.447 0.542 0.306 0.263 0.368 0.536 0.401 PFOSA RSD Std. Dev. MS/MSD RPD 0 306 37.9 0.116 0.429 30.9 0.133 PFOSA = Perfluorooctanesulfonamide PFOSAA * Perfluorooctanesulfonam idoacetate EtFOSE = Narrow Range N-Ethyl Perlluorooctanesulfonamido ethyl alcohol M 556 = C 8 F 17S 0 2 N ((H )C H 2 C 0 0 ) PFOSEA = Perfuorooctane sulfonyl ethylamide Concentration of PFOSAA ug/mL or % Ree 1.87 3 .0 8 0.984 7 .1 5 8 .2 8 5.09 3.79 3.76 3.55 1.66 2.87 4.55 3.30 4.72 3.90 4.35 2.96 6.05 6.52 4.81 6.47 3.73 7.33 6.46 7.91 3.16 9.59 3.34 9.32 5 .2 5 7.81 6 14 3 .4 9 5.24 7.21 6 .1 4 Average PFOSAA RSD Std. Dev. MS/MSD RPD 46.4 4.14 1.92 34.2 6.14 2.10 Date Entered/By: D ate V erified/ By: Purity Enlered/Verified: 03/06/00, 03/10/00, 03/20/K, 03/21/00, 04/16 /0 0 ,0 5 /1 6 /0 0 , 06/12/00, 06/22/00, 06/23/(X), 06/26/00, 08/15/00, 09/05/00, 10/17/00 LAC/C SH 4/30/01 h o j / 04/30/01 LAC 02/19/01 LAC 3MEnvironmental Laboratory Page 239 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product Number(Test Substance): 104 W eek D ietary C arcinogenicity Study w ith N arrow Range (98.1% ) N -Ethyl Perfluorooctanesilfonam ido E thanol in Rats T-63l6(EtFO SE-O H) M atrix: Rat Serum M elh o d /R ev isio n : Analytical Equipment System Number: Instrument Software/Version: Filen am e: ETS-8-4.1 & ETS-8-5.1 Amelia 062498, Davey 070799 M asslynx 3.3 & 3.4 See Below R-Squared Value: See Attachments Slope: See Attachments Y-Intercept: See Attachments Dates o f Extraction/Analyst: Dates o f Analysis/Analyst: 02/07/00, 02/08/00, 02/09/00, 2/24/tK) RW W , SAL 02/18/00, 02/25/00, 03/27/00, 0 6 /01/00,06/19/00, 06/20/00, 08/02/00, 08/16/00, 08/23/00 M M P/IA S Date o f Data Reduction/Analyst: 0 2 /2 1 /0 0 ,0 2 /2 9 /0 0 ,0 2 /2 9 /0 0 , 06/06/00, 06/02/00, 06/20/00, 06/26/00, 08/03/00, 08/18/00, 08/25/00 M M H/IAS/HOJ Sample Data Box 00-009 W EEK 105 RAT SERA G roup Dose Sam ple # C o n cen tratio n ofEtFO SE-O H ug/m L o r % Ree Average EtFO SE-O H ug/m L RSD Std. Dev. M S/M SD RPD C o n cen tratio n of M556 ug/m L or % Ree Average M556 ug/m L RSD Std. Dev. M S/M SD RPD G roup 3 M id Dose 30.0 mg/kg G roup 3 M id Dose 30.0 mg/kg C90842M C90844M C90850M C90851M C90854M C90855M C90856M C90858M C90860M C90864M C90865M C90867M C90869M C90871M C90881M C90882M C90883M C90884M C90885M C90889M C90893M C90900M C91252F C91253F C91254F C91256F C91264F C91278F C91279F C91286F C9I292F C9I294F C91295F C91301F C91303F C91307F C9I3I0F 0.00515 <LOQ (0.00493 ug/mL) 0.00510 <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LO Q (.1493 ug/mL) 0 .0 1 0 3 0.00547 0.(8)666 0.00606 <LOQ (0.00493 ug/mL) 0.00989 0.0182 <LOQ (0.00493 ug/mL) <LOQ (0.(8)493 ug/m L) 0.0152 0.(8)771 0.0106 <LOQ (0.00493 ug/mL) 0.0 0842 0.(8)856 0 .0 2 1 3 0.(8)564 0.00517 0 .0 1 7 8 <LOQ (0.00493 ug/mL) (1.(8)646 0.0153 0.0128 <LOQ (0.00493 ug/mL) 0.00603 0.00921 0 .0 1 2 8 <LOQ (0.00493 ug/mL) O.OO9I2 0 .0 1 0 8 47.2 0 .0 0 4 3 0 48.4 0.00522 2 .54 1.160 2 .14 1.69 1.87 1.62 2.78 6 .10 2.64 2 .28 3 .37 2 .08 2 .70 1.92 3 .78 2.94 5.34 3 .34 2 .84 4 .40 2 .52 2 .86 3 .85 4 .74 3 .24 2 .91 1.78 3 .23 1.76 3 .12 4 .70 3.46 2 .09 3 .48 3 .81 1.25 1.8t 41.7 2.86 1.191 35.7 3.02 1.08 PFOS = Periluorooctanesulfonate PFOSA = Perfluorooctanesulfonam ide PFOSAA = Perfluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M 556 = C8F17SO2N((H)CH2CO0) PFOSEA = Perfuorooctane sulfonyl ethylamide Date Entered/By: D ate V erified/ By: Purity Entered/Verified: 03/06/00, 03/10/00, 03/20/00, 03/21/00, 04/16/00, 05/16/00, 06/12/00, 06/22/00, 06/23A8), 06/26/00, 08/15/00,09/05/00, 10/17/00 LAC/CSH 4/30/01 h o j/ 04/30/01 LAC 02/19/01 LAC C o n c en tra tio n of PFOSEA ug/m L o r % Ree <LO Q (0.(8)492 ug/m l.) <LOQ (0.(8)492 ug/mL) <LO Q (0.(8)492 ug/m L) <1.0Q (0.(8)492 ug/m L) <LOQ (0.(8)492 ug/m L) <LOQ (0.(8)492 ug/m L) <LO Q (0.(8)492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/ml.) <LOQ (0.(8)492 ug/m L) <LO Q (0.(8)492 ug/m L) <LO Q (0.(8)492 ug/m l.) <LO Q (0.(8)492 ug/m L) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.(8)492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.(8)492 ug/m L) <LO Q (0.(8)492 ug/m L) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <].O Q (0.(8)492 ug/m L) <LOQ (0.(8)492 ug/m L) <LO Q (0.(8)492 ug/m L) <I.O Q (0.(8)492 ug/m L) <!.O Q (0.(8)492 ug/m L) <!.OQ (0.00492 ug/mL) <LOQ (0.(8)492 ug/mL) <J.O Q (0.(8)492 ug/mL) <I.O Q (0.(8)492 ug/m l.) <LOQ (0.(8)492 ug/m L) <I.O Q (0.(8)492 ug/m L) <I.OQ (0.00492 ug/mL) <I.OQ (0.00492 ug/mL) < lO Q (0.00492 ug/mL) A verage PFOSEA ug/m L <LOQ <LOQ RSD S td. Dev. M S/M SD RPD NA NA NA NA 3M Environmental Laboratory Page 240 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 LRN-U2103 S tu d y : Product NumberfTest Substance): Matrix: Melhod/Revision: Analytical Equipment System Number: Instrument Software/Version: F il e n a m e : R-Squared Value: Slope: Y-Intercept: Dates o f Extraction/Analyst: D ates o f Analysis/Analyst: 104 W eek D ietary C arcinogenicity Study with N arrow Range (98.1%) N -Ethyl Perflucrooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 & ETS-8-5.1 Soup 020199, Davey 070799 Masslynx 3.3 & 3.4 See Below See Attachments See Attachments See Attachments 02/07/00, 02/08/00, 02/09/00 RWW, SAL 02/18/00, 2/28/00, 03/27/00, 05/31/00, 06/19/00, 06/20/00, 08/03/00, 08/16/00, 08/23/CO MMH/IAS Date o f Data Reduction/Analyst: Sample Data W E E K 105 R A T SER A 02/21/00, 02/29/00, 3/02/00, 06/02/00, 06/20/00, 06/21/00, 08/07/00, 08/18/00, 08/25/(0 MMH/IAS/HOJ Box 00-009 lo ti7 \ G ro u p Dose Sam ple ft E x tra c tio n V o i. mL Surrogate Verified PFO S Std C o rrection Factor PFOS Purity C o rrectio n Factor PFOS Dilution Factor PFOS Cone. n g/m L G roup 4 C90904M 1 NA 0.9275 0 .8 6 4 0 200 417 Mid-High Dose C90908M 1 NA 0.9275 0 .8 6 4 0 200 443 100 mg/kg C90910M 1 NA 0.9275 0 .8 6 4 0 50 786 C90911M 1 NA 0.9275 0 .8 6 4 0 200 911 C90916M 1 NA 0.9275 0.8640 200 551 C90926M 1 NA 0.9275 0.8640 200 384 C90927M 1 NA 0.9275 0.8640 50 548 C90928M 1 NA 0.9275 0.8640 200 791 C90933M 1 NA 0.9275 0.8640 200 286 C90944M 1 NA 0.9275 0.8640 200 848 C90947M 1 NA 0.9275 0.8640 200 899 C90948M 1 NA 0.9275 0.8640 200 323 C90953M 1 NA 0.9275 0.8640 50 324 C90955M 1 NA 0.9275 0.8640 200 400 C90956M C90965M C90968M 1 NA 0.9275 0.8640 200 822 1 NA 0.9275 0.8640 200 857 l NA 0.9275 0.8640 200 626 G roup 4 C91315F 1 NA 0.9275 0 8640 200 762 Mid-High Dose C91324F 1 NA 0.9275 0.8640 200 829 100 m g/kg C91327F 1 NA 0.9275 0.8640 20 612 C91332F 1 NA 0.9275 0.8640 500 627 C9I335F C91336F C91338F l NA 0.9275 0.8640 200 621 1 NA 0.9275 0.8640 500 504 1 NA 0.9275 0.8640 200 875 C91340F 1 NA 0.9275 0.8640 500 628 C91341F C91342F 1 NA 0.9275 0.8640 200 474 1 NA 0.9275 0 8640 200 761 C91356F l NA 0.9275 0.8640 20 386 C91357F 1 NA 0.9275 0.8640 500 500 C91360F 1 NA 0.9275 0.8640 200 881 C91361F 1 NA 0.9275 0.8640 200 815 C91362F 1 NA 0.9275 0.8640 200 158 C91372F 1 NA 0.9275 0.8640 200 367 C91376F C91378F C91380F 1 NA 0.9275 0.8640 200 831 1 NA 0.9275 0.8640 200 682 1 NA 0.9275 0.8640 200 648 G roup 6 C91047M 1 NA 0.9275 0.8640 1 231 M id-High Dose Recovery C91054M C91056M 1 NA 0.9275 0.8640 1 >7.7 1 NA 0.9275 0.8640 5 293 100 mg/kg C91060M 1 NA 0.9275 0.8640 1 177 C91065M 1 NA 0.9275 0.8640 1 0.00 C91070M 1 NA 0.9275 0.8640 1 64.1 C91071M 1 NA 0.9275 0.8640 1 4.80 C91072M 1 NA 0.9275 0.8640 l 56.6 C91073M 1 NA 0.9275 0.8640 1 0.00 C91076M 1 NA 0.9275 0.8640 1 739 G roup 6 C91451F 1 NA 0.9275 0.8640 10 526 Mid-High Dose C91453F 1 NA 0.9275 0 .8 6 4 0 10 >10 Recovery C91455F 1 NA 0.9275 0 .8 6 4 0 10 739 100 mg/kg C91459F 1 NA 0.9275 0 .8 6 4 0 1 0.410 C91462F 1 NA 0.9275 0 .8 6 4 0 10 576 C91467F C91473F C91479F 1 NA 0.9275 .0.8640 1 25.8 1 NA 0.9275 0 .8 6 4 0 10 479 l NA 0.9275 0 .8 6 4 0 1 (1.00 C91480F C91485F 1 NA 0.9275 0 .8 6 4 0 1 9.0 1 NA 0.9275 0 .8 6 4 0 10 443 C91487F C91488F 1 NA 0.9275 0 .8 6 4 0 1 i:.20 1 NA 0.9275 0 .8 6 4 0 10 519 PFO S = Perfluorooctanesulfonate Corrected PFOS LOQ (0.0247 ug/m L) to include std correction factors PFO SA Pcriluorooctanesulfonamidc new LOQ is 0.0198 ug/mL. LAC 02/19/01 PFOSAA Perfluorooctanesulfonamidoacetate A data is above tlie upper lim it o f quantitation and is provided as an estimate. E tF O S E = N arrow R ange N -Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 - C8F17S02N((H)CH2C00) PFOSEA = Perfuorooctane sulfonyl ethylamide Filenam e D062000016 D062000017 A053100106 D062000018 D062000019 D062000020 A 053100108 D062000023 D062000024 D062000025 D062000026 D062000027 A053100I13 D062000030 D062000031 D062000032 D062000033 D062000034 D062000037 D062000065 D081600030 D062000040 D 081600031 D062000044 D 081600032 D062000046 D062000047 D062000048 D 0 8 1600033 D062000052 D062000053 D062000054 [>062000055 D062000058 D062000059 D062000060 A 053100082 A053100072 A 0 5 3 100060 A053100074 A053100075 A053100078 A053100079 A 0 5 3 100080 A053100081 A053100085 A053100040 A053100043 A053100044 A053100089 A053100046 A053100093 AOS3100050 A053I00095 A053100096 A053100051 A 0 5 3 100101 A053100052 C o n c e n tra tio n of PFOS ng/mL or % Ree ' 66.9 71.0 31.5 46 88.4 61.6 2 2 .0 127 45.8 136 144 51.7 13.0 64.1 132 137 100 122 133 9.81 251 A 99.5 202 A 140 252 A 76.0 122 6.18 200 A 141 131 25.3 58.8 133 109 104 0.185 0.0222 1.18 0.142 <LOQ (0.0198 ug/mL) 0 .0 5 1 4 <LOQ (0.0198 ug/mL) 0.0454 <LOO (0.0198 ug/mL) 0.592 5.02 1.68 5 .92 <LOQ (0.0198 ug/mL) 4 .61 0.0207 3 .84 <LOQ (0.0198 ug/mL) 0.0553 3 .55 <LOQ (0.0198 ug/mL) 4 .16 Average PFOS ug/m L 84.6 122 0.227 2 .41 Date Entered/By: D ate Verified/ By: Purity Entered/Verified: 03/06/00, 03/10/00, 03/20/00, 03/21/00, 4/15/00, 5/16/00, 06/13/00, 6/15/00, 6/19/00, 06/22/00, 06/23/00, 06/26/00, 08/15/00, 09/05/00, 10/17/00 LAC/CSH 04/30/01 h o j / 04/30/01 LAC 02/19/01 LAC RSD Std. Dev. MS/MSD RPD 5 3 .6 45.4 57.9 70.5 166 0.377 . 96.3 2.32 3MEnvironmental Laboratory Page 241 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 LRN-U2103 Study: Product N um ber(Test Substance): M atr ix : Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Filename: R-Squared Value: 104 W eek D ietary C arcinogenicity Study with Narrow Range (98.1%) N-Etliyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum _ ETS-8-4.1 & ETS-8-5.1 * Soup 020199. Davey 070799 Masslynx 3.3 & 3.4 See Below See Attachments Slope: Y-Inlercept: Dates o f Extraction/Analyst: Dates o f Aitalysis/Analyst: See Attachments See Attachments 02/07/00, 02/08/00, 02/09/00 RW W , SAL 02/18/00, 2/28/00, 03/27/00, 05/31/00, 06/19/00, 06/20/00, 08/03/00, 08/16/00, 08/23/00 MMH/IAS Date o f Data Reduction/Analyst: Sample Data W E E K 105 R A T SERA 02/21/00, 02/29/00, 3/02/00, 06/02/00, 06/20/00, 06/21/00, 08/07/00, 08/18/(0, 08/25/00 MMH/IAS/HOI Box 00-009 lot L-15709 G roup Dose G roup 4 M id-High Dose lO O m g /k g G roup 4 Mid-High Dose 100 mg/lcg Sample # C90904M C90908M C909I0M C909I1M C90916M C90926M C90927M C90928M C90933M C90944M C90947M C90948M C90953M C9955M C90956M C90965M C90968M C91315F C91324F C91327F C91332F C91335F C9I336F C91338F C91340F C91341F C91342F C91356F C91357F C9I360F C91361F C91362F C91372F C91376F C91378F C91380F PFOSA Purity C o rrection Factor Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOSA Dilution Factor 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 PFOSA Cone. ng/m L 56.8 60.6 184 60.7 61.2 33.0 109 97.9 59.3 56.0 68.5 27.7 57.2 61.4 39.0 94.9 63.8 89.8 191 102 136 205 107 171 72.1 138 82.6 34.5 201 185 116 72.0 161 193 117 89.1 F ilen am e A022700090 A022700091 A022700094 A022700054 4022700055 4 022700095 4022700096 4022700097 4022700098 4022700056 4022700059 A022700060 4022700101 A022700102 A022700061 A022700062 A022700103 A022700077 A022700080 A022700081 A022700082 A022700083 A022700084 AD22700087 AD22700088 A322700089 A322700063 A322700066 AJ22700067 AJ22700068 A022700069 A 122700070 A022700073 A022700074 A022700075 A022700076 C o n c e n tra tio n of PFOSA ug/mL or % Ree 0.568 0.606 1.84 0.607 0.612 0.330 1.09 0.979 0.593 0.5CO 0.685 0.277 0.572 0.614 0.390 0.949 0.638 0.898 1.91 1.02 1.36 2.05 1.07 1.71 0.721 1.38 0.826 0.345 2.01 1.85 1.16 0.720 1.61 1.93 1.17 0.891 * A verage PFOSA ug/m L 0.701 1.30 G roup 6 C91047M Unknown NA 1 0.00 A062000022 <LOQ (0.00493 ug/mL) Mid-High Dose C91054M Unknown NA 1 0.00 A062000023 <LOQ (0.00493 ug/mL) Recovery C91056M Unknown NA 1 0.00 A062000026 <LOQ (0.00493 ug/mL) lO O m g /k g C91060M Unknown NA 1 0.00 A062000027 <LOQ (0.00493 ug/mL) C91065M C91070M Unknown Unknown NA l 0.00 A062000028 <LOQ (0.00493 ug/mL) NA 1 0.00 A062000029 <LOQ (0.00493 ug/mL) C91071M Unknown NA 1 0.00 A062000030 <LOQ (0.00493 ug/mL) C91072M Unknown NA 1 0.00 A062000033 <LOQ (0.00493 ug/mL) C91073M Unknown NA 1 0.00 A062000034 <LOQ (0.00493 ug/mL) C91076M Unknown NA 1 0.00 A062000035 <LOQ (0.00493 ug/mL) G roup 6 C91451F Unknown NA 1 2.07 A062000036 <LOQ (0.00493 ug'm L) Mid-High Dose C91453F Unknown NA 1 0.00 A062000037 <LOQ (0.00493 Ug/mL) Recovery C91455F Unknown NA 1 0.00 A062000040 <LOQ (0.00493 ug'mL) lO O m g /k g C91459F Unknown NA I 0.00 A062000041 <LOQ (0.00493 ug'mL) C9I462F Unknown NA l 0.00 A062000042 <LOQ (0.00493 ug'm L) C9I467F C91473F Unknown Unknown NA 1 0.00 A062000043 <LOQ (0.00493 ug'mL) NA 1 0 .0 0 A62000044 <LOQ (0.00493 ug'mL) C91479F Unknown NA l 0.00 A(>62000047 <LOQ (0.00493 u g'm L ) C91480F C91485F Unknown Unknown NA 1 0.00 A(>62000048 <LOQ (0.00493 ug'm L) NA 1 0.00 A (62000049 <LOQ (0.00493 ug'm L) C91487F Unknown NA l 0.00 AC62000050 <LOQ (0.00493 ug'mL) C91488F Unknown NA 1 0.00 AC62000051 <LOQ (0.00493 ug'm L) PFOS = Perfluorooctanesulfonate Corrected PFOS LOQ (0.0247 ug/mL) to include std correction factors PFOSA - Perfluorooctanesulfonamide new LOQ is 0.0198 ug/mL. LAC 02/19/01 PFOSAA = Perfluorooctanesulfonamidoacetate A - data is above the upper limit o f quantitation and is provided as an estimate. EtFOSE = N arrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2C00) PFOSEA = Perfuorooctane sulfonyl ethylamide <LOQ <LOQ Date Entered/By: D ate V erified/ By: Purity Entered/Verified: 03/06/00, 03/10/00, 03/20/00, 03/21/00, 4/15/0, 5/16/00, 06/13/00, 6/15/00, 6/19/00, 06/22/00, 06/23/30, 06/26/00, 08/15/00, 09/05/00, 10/17/00 LAC/CSH 04/30/01 hoj / 04/30/01 LAC 02/19/01 LAC rsd Std. Dev. M S/M SD RPD 51.9 0.363 39.5 0.512 NA NA NA NA 3MEnvironmental Laboratory Page 242 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 LRN-U2103 Study: Product Number(Test Substance): Matrix: M ethod/Revision: Analytical Equipment System Number: Instrument Software/Version: Filename: R-Squarcd Value: Slope: Y -lntercept: Dates o f Extraction/Analyst: Dates o f Analysis/Analyst: 104 W eek D ietary Carcinogenicity Study w ith Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamidc Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 & ETS-8-5.1 Soup 020199, Davey 070799 Masslynx 3.3 & 3.4 See Below See Attachments See Attachments See Attachments 02/07/00, 02/08/00, 02/09/00 RWW, SAL 02/18/00, 2/28/00, 03/27/00, 05/31/00, 06/19/00, 06/20/00, 08/03/00, 08/16/00, 38/23/00 MMH/1AS Date o f Data Reduction/Analyst: Sample Data W E E K 105 R A T SER A 02/21/00, 02/29/00, 3/02/00, 06/02/00, 06/20/00, 06/21/00, 08/07/00, 08/18/00, 38/25/00 MMH/IAS/HOJ Box 00-009 lot T-7121 l G roup Dose G roup 4 M id-High Dose 100 mg/kg Sample # C90904M C90908M C90910M C90911M C90916M C90926M C90927M C90928M C90933M C90944M C90947M C90948M C90953M C90955M C90956M C90965M C90968M PFOSAA Purity Correction F a c to r Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate V erified 2nd Analysis OK NA NA . NA 2nd Analysis OK NA NA NA NA NA 2nd Analysis OK 2nd Analysis OK NA NA 2nd Analysis OK 2nd Analysis OK NA PFOSAA D ilation Factor 50 50 50 50 50 10 50 50 50 50 50 50 50 50 50 50 50 PFOSAA Cone. n g/m L 132 154 671 475 177 119 193 329 134 279 174 84 112 207 71.0 251 173 Filenam e D081600055 A022800018 A022800019 A022700038 D 081600058 D 081600038 A022800021 A022800024 A022800025 A022700040 D081600059 D 081600060 A022800026 A022800027 D 081600061 D081600062 A022800028 C o n cen tratio n of PFOSAA ug/mL o r % Ree 6.58 7.68 33.6 23.7 8.84 1.19 9.64 16.5 * 6.59 14.0 8 71 4 19 5.58 10.3 355 12.6 8.63 G roup 4 C91315F Unknown NA 20 510 D062000061 10.2 Mid-High Dose C91324F Unknown NA 20 570 D062000062 11.4 100 mg/kg C91327F Unknown NA 20 941 D062000065 18.3 C91332F Unknown NA 20 922 D062000066 18.4 C91335F Unknown NA 20 498 D062000067 10.0 C91336F Unknown NA 20 559 D062000068 11.2 C91338F Unknown NA 20 529 D062000069 106 C91340F Unknown NA 20 553 D062000072 111 C91341F Unknown NA 20 555 D062000073 11 1 C91342F Unknown NA 20 596 D062000074 119 C91356F Unknown NA 10 602 A05310029 6.02 C91357F Unknown NA 20 562 D062000076 112 C91360F Unknown NA 20 688 D062000079 13 8 C91361F Unknown NA 10 776 A 05310032 7.76 C91362F Unknown NA 20 624 D062QOOQ8l 12 5 C91372F Unknown NA 20 670 D062000082 134 C91376F Unknown NA 20 648 D062000083 13.0 C91378F Unknown NA 20 515 D062000086 103 C91380F Unknown NA 20 646 D062000087 12.9 Group 6 C91047M Mid-High Dose C91054M Recovery C91056M 100 mg/kg C91060M C91065M C91070M C91071M C91072M C91073M C91076M G roup 6 C91451F Mid-High Dose C91453F Recovery C91455F 100 mg/kg C91459F C91462F C91467F C91473F C91479F C91480F C91485F C91487F C91488F PFOS = Perfluorooctanesulfonate Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA 1 0.00 A062000022 NA 1 0.00 A062000023 NA 1 0.00 A062100026 NA 1 0.00 A062100027 NA 1 0.00 A062I00028 NA l 0.00 *062100029 NA 1 0.00 *062100030 NA 1 0.00 *062100033 NA 1 0.00 *062100034 NA 1 0.00 *062100035 NA 1 26.1 *062100036 NA 1 0.00 A062100037 NA 1 0.00 *062100040 NA l 0.00 A062100041 NA 1 0.00 A062100042 NA 1 0.00 A062100043 NA 1 0.00 A 062100044 NA l 0.00 A062100047 NA l 0.00 A062100048 NA 0.00 A062100049 NA 1 0.00 A062100050 NA 1 0.00 A062100051 Corrected PFOS LOQ (0.0247 ug/mL) to include std correction factors <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) 0.0261 <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mb) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) PFOSA = Perfluorooctanesulfonamide new LOQ is 0.0198 ug/mL. LAC 02/19/01 PFOSAA = Perfluorooctanesulfonamidoacetate A - data is above the upper limit o f quantitation and is provided as an estimate. EtFOSE = N arrow R ange N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2C00) PFOSEA = Perfuorooclane sulfonyl ethylamide A verage PFOSAA ug/m L 10.7 11.9 <LOQ <LOQ Date Entered/By: D ate V erified/ By: Purity Entercd/Verified: 03/06/00, 03/10/00, 03/20/00, 03/21/00, 4/15/00, 5/16/00, 06/13/00. 6/15/00, 6/19/00, 06/22/00, 06/23/00, 06/26/00, 08/15/00, 09/05/00, 10/17/00 LAC/CSH 04/30/01 h o j / 04/30/01 LAC 02/19/01 LAC RSD Std. Dev. MS/MSD RPD 74.1 7.93 25.4 3.02 NA NA NA NA 3MEnvironmental Laboratory Page 243 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 S tu d y : Product Number(Tesl Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Intercept: Dates o f Extraction/Analyst: Dates o f Analysis/Analyst: 104 W eek D ietary C arcinogenicity Study w ith N arrow Range (98.1%) N-Ethyl Perfluorocctanesulfonamido Ethanol h Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 & ETS-8-5.1 Soup 020199, Davey 070799 Masslynx 3.3 & 3.4 See Below See Attachments See Attachments See Attachments 02/07/00, 02/08/00, 02/09/00 RWW, SAL 02/18/00, 2/28/00, 03/27/00, 05/31/00, 06/19/00, 06/20/00, 08/03/00, 08/16/00, 08/23/00 MMH/IAS D ate o f D ata R eduction/Analyst: Sample Data 02/21/00, 02/29/00, 3/02/00, 06/02/00, 06/20/00, 06/21/00, 08/07/00, 08/18/00, 08/25/00 MMH/IAS/HOJ Box 00-009 W E E K 105 R A T SE R A lot Unknown/SD013 G roup Sample # EtFO SE-O H P urity Dose C o rrection Factor G roup 4 C90904M Unknown Mid-High Dose C90908M Unknown 100 mg/kg C90910M Unknown C90911M Unknown C909I6M Unknown C90926M Unknown C90927M Unknown C90928M Unknown C90933M Unknown C90944M Unknown C90947M Unknown C90948M Unknown C90953M Unknown C90955M Unknown C90956M Unknown C90965M Unknown C90968M Unknown G roup 4 C91315F Unknown M id-High Dose C91324F Unknown 100 mg/kg C91327F Unknown C91332F Unknown C91335F Unknown C91336F Unknown C91338F Unknown C91340F Unknown C91341F Unknown C91342F Unknown C91356F Unknown C91357F Unknown C91360F Unknown C91361F Unknown C91362F Unknown C91372F Unknown C91376F Unknown C91378F Unknown C91380F Unknown G roup 6 C91047M Unknown Mid-High Dose C91054M Unknown Recovery C91056M Unknown 100 mg/kg C91060M Unknown C91065M Unknown C91070M Unknown C91071M Unknown C91072M Unknown C91073M Unknown C91076M Unknown G roup 6 C9145IF Unknown Mid-High Dose C91453F Unknown Recovery C91455F Unknown 100 mg/kg C91459F Unknown C91462F C91467F C91473F C91479F Unknown Unknown Unknown Unknown C91480F C91485F Unknown Unknown C91487F C91488F Unknown Unknown PFOS = Periluorooctanesulfonate PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2C00) PFOSEA = Perfuorooctane sulfonyl ethylamide Sarrogate EtFOSE-OH E tF O S E -O H F ilen am e Verified Dilution Cone. Factor n g/m L NA 1 8.52 A080300017 NA 1 12.6 A080300018 NA 1 81.6 A080300019 NA 1 4.19 A080300020 2nd Analysis OK NA l 1 22.1 0.440 D081600053 A080300024 NA 1 16.4 A080300025 2nd Analysis OK 1 22.7 D081600054 NA l 11.2 A080300027 NA 1 11.6 A080300028 NA 1 7.73 A080300031 NA 1 6.26 A080300032 NA 1 21.7 AQ8Q300033 NA 1 15.4 A080300034 NA 1 1.28 A080300035 NA 1 19.7 A080300038 NA 1 16.4 A080300039 2nd Analysis OK NA 1 1 67.2 DO81600047 34.4 A080300041 NA 1 29.0 A080300042 NA 1 31.2 A080300045 NA 1 56.2 A080300046 NA 1 30.0 A080300047 NA 1 27.4 A080300048 NA 1 10.1 A080300049 NA . NA 1 43.6 A080300052 1 33.7 A080300053 NA 1 17.8 A080300054 NA 1 33.5 A080300055 NA 1 57.3 A080300056 2nd Analysis OK I 45.9 D0816OOO48 NA 2nd Analysis OK NA 1 1 1 17.0 A080300060 46.7 D081600051 40.8 A080300062 2nd Analysis OK NA 1 1 42.4 [>081600052 27.0 A080300066 NA - 1 0.00 A062100022 NA 1 0.00 A062100023 NA 1 0.00 A062100026 NA 1 0.00 A062100027 NA 1 0.00 A062100028 NA 1 0.00 A062100029 NA l 0.00 A062100030 NA 1 0.00 A062100033 NA 1 0.00 A 062100034 NA 1 0.00 A062100035 NA 1 0.0800 A062100036 NA 1 0.00 A062100037 NA 1 0.00 A062100040 NA 1 0.00 A062100041 NA 1 0.00 A062100042 NA 1 0.00 A062100043 NA l 0.00 A062100044 NA 1 0.00 A 062100047 NA l 0.00 A062100048 NA l 0.00 A062100049 NA 1 0.00 A062100050 NA 1 0.00 A 062100051 Corrected PFOS LOQ (0.0247 ug/m L) to include std correction factors new LOQ is 0.0198 ug/mL. LAC 02/19/01 A - data is above the upper limit o f quantitation and is provided ns an estimate. C o n cen tratio n (if EtFO SE-O H ug/mL o r % Ree <LOQ (0.00977 ug/mL) 0 .0 1 2 6 00816 <LOQ (0.00977 ug/mL) 0 0221 <LOQ (0.00977 ug/mL) 0 .0 1 6 4 0 .0 2 2 7 0.0112 0.0116 <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) 0.0217 0.0154 <LOQ (0.00977 ug/mL) 0.0197 0.0164 0.0672 0.0344 0 .0 2 9 0 0.0312 0.0562 0.0300 0.0274 0.0101 0.0436 - 0.0337 0.0178 0.0335 0.0573 0.0459* 0.0170 0.0467 0.0408 0.0424 0.0270 <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ' (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) Date Entered/By: Date V erified/ By: Purity Entered/Verified: 03/06/00, 03/10/00, 03/20/00, 03/21/00, 4/15/00, 5/16/00, 06/13/00, 6/15/00, 6/19/00, 06/22/00, 06/23/00, 06/26/00, 18/15/00, 09/05/00, 10/17/00 LAC/CSH 04/30/01 h o j / 04/30/01 LAC 02/19/01 LAC Average E tF O S E -O H ug/m L 0 .0 1 8 2 0.0364 <LOQ <LOQ RSD Std. Dev. M S/M SD RPD 93.3 0 .0 1 7 0 40.0 0.0145 NA NA NA NA 3MEnvironmental Laboratory Page 244 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covane* 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product N um bcrtTest Substance): M atr ix : 104 W eek Dietary C arcinogenicity Study w ith N arrow Range (98.1%) N -Elhyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Filename: ETS-8-4.1 & ETS-8-5.1 Soup 020199, Davey 070799 M asslynx 3.3 & 3.4 See Below R-Squared Value: Slope: Y-Intercept: Dates o f Extraction/Analyst: Dates o f Analysis/Analyst: See Attachments See Attachments See Attachments 02/07/00, 02/08/00, 02/09/00 RWW, SAL 02/18/00, 2/28/00, 03/27/00, 05/31/00, 06/19/00, 06/20/00, 08/03/00, 08/16/00, 08/23/00 MMH/IAS Date o f Data Reduction/Analyst: Sample Data W E E K 105 R A T SER A 02/21/00, 02/29/00, 3/02/00, 06/02/00, 06/20/00, 06/21/00, 08/07/00, 08/18/00, 08/25/00 MMH/IAS/HOJ Box 00-009 lotNB113047-80 G ro u p Dose G roup 4 Mid-High Dose 100 mg/kg Sample # C90904M C90908M C90910M C90911M C90916M C90926M C90927M C90928M C90933M C90944M C90947M C90948M C90953M C90955M C90956M C90965M C90968M M556 Purity C o rrection Factor Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA NA NA NA NA NA NA . NA NA NA NA NA NA NA NA NA NA M556 Dilution Factor 10 10 50 10 10 10 10 10 10 10 10 10 10 10 10 10 10 M556 Cone. ug/m L 646 766 295 610 599 641 824 694 899 410 416 538 401 871 345 421 627 F ilen am e A022700090 A022700091 A0228000J9 A022700054 A022700055 A022700095 A022700096 A022700097 A022700098 A022700056 A022700059 A022700060 A022700101 A022700102 A022700061 A022700062 A022700103 C o n c e n tra tio n of M556 ug/mL o r % Ree 6.46 7.66 14.8 6.10 5.99 6.41 8.24 6.94 8.99 4.10 4.16 5.38* 4.01 8.71 3.45 4.21 6.27 G roup 4 Mid-High Dose 100 mg/kg C91315F C91324F C91327F C91332F C91335F C91336F C91338F C91340F C91341F C91342F C91356F C91357F C91360F C91361F C91362F C91372F C91376F C91378F C91380F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA 10 635 A022700077 6.35 10 421 A022700080 4.21 10 320 A022700081 3.20 20 288 A022800048 5.76 10 570 A022700083 5.70 10 753 A022700084 7.53 10 608 A022700087 6.08 10 388 A022700088 3.88 10 505 A022700089 5.05 10 618 A022700063 6.18 10 210 A022700066 2.10 10 625 A022700067 6.25 10 460 A022700068 4.60 10 305 A022700069 3.05 10 512 A022700070 5.12 10 606 A022700073 6.06 10 620 A022700074 6.20 10 376 A022700075 3.76 10 512 A022700076 5.12 G roup 6 Mid-High Dose Recovery C91047M C91054M C91056M Unknown Unknown Unknown NA NA NA 1 0.0600 A 061900022 <LOQ (0.00494 ug/m L) 1 0.00 A061900023 <LOQ (0.00494 ug/mL) l 0.00 A061900026 <LOQ (0.00494 ug/mL) 100 mg/kg C91060M C91065M C91070M C91071M Unknown Unknown Unknown Unknown NA NA NA NA 1 0.270 A061900027 <LOQ (0.00494 ug/mL) 1 0.00 A 061900028 <LOQ (0.00494 ug'mL) 1 0.00 A 061900029 <LOQ (0.00494 ug/mL) l 0.00 A061900030 <LOQ (0.00494 Ug/mL) C91072M C91073M C91076M Unknown Unknown Unknown NA NA NA l 4.41 A061900033 <LOQ (0.00494 ug/mL) 1 0.00 A061900034 <LOQ (0.00494 Ug/mL) 1 0.00 A061900035 <LOQ (0.00494 ug/mL) G roup 6 Mid-High Dose Recovery 100 mg/kg C9I451F C91453F C91455F C91459F C91462F C91467F C91473F C91479F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA NA NA NA NA NA NA NA 1 55.3 A061900036 <LOQ (0.00494 ug/mL) 1 1.97 A061900037 <LOQ (0.00494 ug/mL) 1 0.350 A 061900040 <LOQ (0.00494 ug/mL) l 0.00 A061900041 <LOQ (0.00494 ug/mL) l 1.87 A 061900042 <LOQ (0.00494 ug/mL) 1 0.00 A 061900043 <LOQ (0.00494 ug/mL) 1 0.3SO A 061900044 <LOQ (0.00494 ug/mL) 1 0.00 A 061900047 <LOQ (0.00494 ug/mL) C91480F C91485F C91487F C91488F Unknown Unknown Unknown Unknown NA NA NA NA 1 0.00 A061900048 <LOQ (0.00494 ug/mL) 1 2.75 A 061900049 <LOQ (0.00494 ug/mL) 1 0.00 A061900050 <LOO (0.00494 ug/mL) 1 0.00 A 061900051 <LOC> (0.00494 ug/mL) PFOS = Perfluorooctanesulfonate PFOSA = Perfluorooctanesulfonamide Corrected PFOS LOQ (0.0247 ug/mL) to include std correction factors new LOQ is 0.0198 ug/mL. LAC 02/19/01 PFOSAA = Perfluorooctanesulfonamidoacetate A data is above the upper lim it o f quantitation and is provided as an estimate. EtFOSE = N arrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2C00) PFOSEA = Perfiiorooctane sulfonyl ethylamide A verage M556 ug/m L 6.58 5.06 <LOQ <LOQ Date Entered/By: D ate V erified/ By: Purity Entered/Verified: 03/06/00, 03/10/00, 03/20/00, 03/21/00, 4/15/00, 5/16/00, 06/13/00, 6/15/00, 6/19/00, 06/22/00, 06/23/00, 36/26/00, 08/15/00, 09/05/00, 10/17/00 LAC/CSH 04/30/01 h o j/ 04/30/01 LAC 02/19/01 LAC RSD Std. Dev. M S/M SD RPD 41.2 2.71 27.5 1.39 NA NA NA NA 3MEnvironmental Laboratory Page 245 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product Number(Test Substance): M atr ix : Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Filename: R -Squared Value: Slope: Y-Intercept: Dates o f Extraction/Analyst: Dates o f Analysis^ Analyst: D ate o f D ata Reduction/Analyst: Sample Data W E E K 105 R A T S ER A 104 W eek Dietary Carcinogenicity Study with N arrow R ange (98.1%) N-Ethyl Perflvorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 &ETS-8-5.1 Soup 020199, Davey 070799 M asslynx 3.3 & 3.4 See Below See Attachments See Attachments See Attachments 02/07/00, 02/08/00, 02/09/00 RWW, SAL 02/18/00, 2/28/00, 03/27/00, 05/31/00, 06/19/00, 06/20/00, 08/03/00, 08/16/00, 08/23/00 MMH/IAS 02/21/00, 02/29/00, 3/02/00, 06/02/00, 06/20/00, 06/21/00, 08/07/00, 08/18/00, 08/25/00 MMH/1AS/HOJ Box 00-009 lot 529 G roup Dose Sample # PFOSEA Purity C o rrection Factor Surrogate Verified PFOSEA D ilation Factor PFOSEA Cone. ng/m L F ilen am e Group 4 C90904M Unknown NA 1 0.00 A080300017 Mid-High Dose C90908M Unknown NA 1 0.00 A080300I8 100 mg/kg C90910M Unknown NA I 0.00 A080300019 C909UM Unknown NA 1 2.76 A080300020 C90916M Unknown 2nd Analysis OK 1 0.00 D081600Q53 C90926M Unknown NA l 0.00 A080300024 C90927M Unknown NA 1 0.00 A080300025 C90928M Unknown 2nd Analysis OK 1 0.450 D081600054 C90933M Unknown NA 1 0.00 A080300027 C90944M Unknown NA 1 0.00 A080300028 C90947M C90948M Unknown Unknown NA NA I 0.00 A080300031 1 0.00 A080300032 C90953M Unknown NA 1 0.00 A080300033 C90955M C90956M Unknown Unknown NA NA 11 0.00 A080300034 0.00 A080300035 C90965M Unknown NA 1 3.75 A080300038 C90968M Unknown NA 1 0.00 A080300039 G roup 4 C91315F Unknown 2nd Analysis OK 1 0.00 D081600047 Mid-High Dose C91324F Unknown NA 1 4.02 A080300041 100 mg/kg C91327F C91332F C91335F Unknown Unknown Unknown NA NA NA 1 6.88 A080300042 1 0.00 A080300045 1 1.85 A080300046 C91336F Unknown NA 1 0.320 A080300047 C91338F C91340F U n b io w n Unknown NA NA 1 0.00 A080300048 1 0.00 A080300049 C91341F Unknown NA 1 0.00 A080300052 C91342F Unknown NA 1 0.00 A080300053 C91356F Unknown NA 1 1.72 A080300054 C9I357F Unknown NA 1 0.00 A080300055 C91360F Unknown NA 1 2.40 A080300Q56 C91361F C91362F Unknown Unknown 2nd Analysis OK NA 1 1 1.61 D 081600048 0.00 A080300060 C91372F Unknown 2nd Analysis OK 1 0.610 D081600051 C91376F C91378F C91380F Unknown Unknown Unknown NA 2nd Analysis OK NA 1 1 1 6.20 A080300062 1.04 D081600052 0.00 A080300066 G roup 6 C91047M Unknown NA 1 0.00 A061900022 Mid-High Dose C91054M Unknown NA 1 0.00 A061900023 Recovery C91056M Unknown NA 1 0.00 A061900026 100 mg/kg C91060M Unknown NA 1 0.00 A061900027 C91065M C91070M Unknown Unknown NA NA 0.00 A061900028 l 0.600 A061900029 C91071M Unknown NA 1 0.00 A061900030 C91072M Unknown NA 1 0.00 A061900033 C91073M C91076M Unknown Unknown NA NA 1 0.00 A 061900034 1 0.00 A061900035 Group 6 C91451F Unknown NA 1 0.00 A061900036 Mid-High Dose Recovery C91453F C91455F Unknown Unknown NA NA 1 0.00 A061900037 1 0.00 A 061900040 100 mg/kg C91459F Unknown NA 1 0.00 A061900041 C91462F Unknown NA 1 0.00 A061900042 C91467F Unknown NA 1 0.00 A 061900043 C91473F C91479F Unknown Unknown NA NA 1 0.00 A061900044 1 0.00 A061900047 C91480F Unknown NA 1 0.00 A061900048 C91485F Unknown NA 1 0.00 A 061900049 C91487F C91488F Unknown Unknown NA NA 1 0.00 A 061900050 l 0.00 A061900051 PFOS = Perfluorooctanesulfonatc Corrected PFOS LOQ (0.0247 ug/mL) to include std correction factors PFOSA = Perfluorooctanesulfonamide new LOQ is 0.0198 ug/mL. LAC 02/19/01 PFOSAA = Perfluorooctancsulfonamidoacetate A - data is above the upper limit o f quantitation and is provided at an estimate. EtFOSE = Narrow Range N -Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2C00) PFOSEA = Perfuorooctane sulfonyl ethylamide C o n c e n tra tio n of PFOSEA ug/m L o r % Ree <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (3.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ <0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) (1.00688 <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (('.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (C.00492 ug/mL) <LOQ (C.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) 0.00620 <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0 00492 ug/mL) <LOQ (0 00492 ug/mL) <LOQ (0 00492 ug/mL) <LOQ (0 00492 ug/mL) <LOQ (0 00492 ug/mL) <LOQ (0 00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) Date Entered/By: D ate V erified/ By: Purity Entered/Verified: 03/06/00, 03/10/00, 03/20/00, 03/21/00, 4/15/00, 5/16/00, 06/13/00, 6/15/00, 6/19/00, 06/22/00, 06/23/00, 06/26/00, 08/15/00, 09/05/00, 10/17/00 LAC/CSH 04/30/01 h o j / 04/30/01 LAC 02/19/01 LAC A verage PFOSEA ug/m L <LOQ <LOQ <LOQ <LOQ RSD Std. Dev. M S/M SD RPD NA NA NA . NA NA NA NA NA 3MEnvironmental Laboratory Page 246 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product N um bcr(Tesl Substance): M atr ix : Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Intercept: Dates orExtraction/Analyst: Dates o f Analysis/Analyst: 104 W eek D ietary C arcinogenicity Study with N arrow Range (98.1% ) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 & ETS-8-5.1 Soup 020199, Davey 070799 Masslynx 3.3 & 3.4 See Attachments See Attachments See Attachments See Attachments 02/07/00, 02/08/00, 02/09/00 RWW, SAL 02/18/00, 2/28/00, 03/27/00, 05/31/00, 06/19/00, 06/20/00, 08/03/00, 08/16/00, 08/23/00 MMH/IAS Date o f Data Reduction/Analyst: Sample Data W E E K 105 R A T SERA 02/21/00, 02/29/00, 3/02/00, 06/02/00, 06/20/00, 06/21/00, 08/07/00, 08/18/00, 08/25/00 MMH/IAS/HOJ G roup Dose Sample # C o n cen tratio n of PFOS ug/mL o r % Ree Average PFOS ug/m L RSD Std- Dev. MS/MSD RPD Concentration of PFOSA ug/mL or % Ree A verage PFOSA ug/m L G roup 4 M id-High Dose C90904M C90908M 66.9 71.0 0.568 0.606 ]00m g/kg C90910M C90911M C90916M 31.5 146 88.4 1.84 0.607 0.612 C90926M C90927M 61.61 22.0 0.330 1.09 C90928M 127 0.979 C90933M C90944M 45.8 136 0.593 0.560 C90947M 144 0.685 C90948M C90953M 51.7 13.0 0.277 0.572 C90955M C90956M C90965M C90968M 64.1 132 137 100 53.6 84.6 45.4 0.614 0.390 0.949 0.638 0.701 G roup 4 C91315F 122 0.898 Mid-High Dose lO O m g /k g C91324F C91327F 133 9 .81 1.91 1.02 C91332F C91335F 251 A 99.5 1.36 2 .05 C91336F 202 A 1.07 C91338F 140 1.71 C91340F 252 A 0.721 C91341F 76.0 1.38 C91342F 122 0.826 C91356F 6.18 0.345 C91357F C9136QF 200 A 141 2 .01 1.85 C91361F 131 1.16 C91362F 25.3 0.720 C91372F 58.8 1.61 C91376F C91378F 133 109 1.93 57.9 1.17 C91380F 104 122 70.5 0.891 1.30 G ronp 6 C91047M 0.185 <LOQ (0.00493 ug/mL) M id-High Dose Recovery lO O m g /k g C91054M C91056M C91060M 0.0222 1.18 0.142 <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) C91065M C91070M C91071M C91072M C91073M C9I076M <LOQ (0.0198 ug/mL) 0.0514 <LOQ (0.0198 ug/mL) 0 .0 4 5 4 <LOQ (0.0198 ug/mL) 0.592 0.227 166 0.377 <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ G roup 6 Mid-High Dose C91451F C91453F 5.02 1.68 <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) Recovery l OOmg/kg C91455F C91459F 5 .92 <LOQ (0.0198 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) C91462F 4.61 <LOQ (0.00493 ug/mL) C91467F C91473F C91479F 0.0207 3 .8 4 <LOQ (0.0198 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) <LOQ (0.00493 ug/mL) C91480F C91485F 0.0553 3 .55 <LOQ (0.00493 Ug/mL) <LOQ (0.00493 ug/mL) C9I487F <LOQ (0.0198 ug/raL) 96.3 <LOQ (0.00493 ug/mL) C91488F 4.16 2.41 2 .32 <LOQ (0.00493 ug/mL) <LOQ PFOS = Pcrfluorooctanesulfonatc Corrected PFOS LOQ (0.0247 ug/mL) to include std correction factors PFOSA = Perfluorooctanesulfonamide PFOSAA = Pcrfluorooctanesulfonamidoacetatc new LOQ is 0.0198 ug/mL. LAC 02/19/01 A - d ata is above the upper lim it o f quantitation and is provided as air estimate. EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 C8F17S02N((H)CH2C00) PFOSEA = Perfiiorooctane sulfonyl ethylamide RSD Std, Dev. MS/MSD RPD 51.9 0.363 39.5 0.S12 NA NA NA NA C o n c e n tra tio n of PFOSAA ug/mL or % Ree 6 .5 8 7 .6 8 33.6 2 3 .7 8.8 1.19 9.64 16.5 6 .6 9 14.0 . 8.7 4 . 19 5 .58 10.3 3 .55 12.6 8.63 10.2 11.4 18.8 18.4 10.0 11.2 10.6 11.1 11.1 11.9 6 .02 11.2 138 7 .7 6 12.5 13.4 13.0 10.3 12.9 <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0,0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) 0.03 <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0348 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) <LOQ (0.0248 ug/mL) Date Entcred/By: Date V erified/ By: Purity Entered/Verified: 03/06/00, 03/10/00, 03/20/00, 03/21/00, 4/15/00, 5/16/00, 06/13/00, 6/15/00, 6/19/00, 06/22/00, 06/23/00, 06/26/00, 08/15/00, 09/05/00, 10/17/00 LA G C SH 04/30/01 h o j/ 04/30/01 LAC 02/19/01 LAC Average PFOSAA ug/m L RSD Std. Dev. MS/MSD RPD 74.1 10.7 7.93 25.4 11.9 3.02 <LOQ NA NA <LOQ I NA NA 1 3MEnvironmental Laboratory Page 247 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product N um ber(Test Substance): Matrix: Mcthod/Revision: Analytical Equipment System Number: Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Intercept: Dates o f Extraction/Analyst: D ates o f Analysis/Analyst: 104 W eek Dietary Carcinogenicity Study w ith N arrow Range (98.1%) N -Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Serum ETS-8-4.1 & ETS-8-5.1 Soup 020199, Davey 070799 Masslynx 3.3 & 3.4 See Below See Attachments See Attachments See Attachments 02/07/00, 02/08/00, 02/09/00 RWW, SAL 02/18/00, 2/28/00, 03/27/00, 05/31/00, 06/19/00,06/20/00, 08/03/00, 08/16/00, 08/23/00 MMH/IAS Date o f Data Reduction/Analyst: Sample Data W E E K 105 R A T SERA 02/21/00, 02/29/00, 3/02/00, 06/02/00, 06/20/00, 06/21/00, 08/07/00, 08/18/00, 08/25/00 MMH/IAS/HOJ Box 00-009 G roup Sample # C o n c e n tra tio n Dose of EtFO SE-O H ug/m L o r / Ree Group 4 C90904M <LOQ (0.00977 ug/mL) Mid-High Dose C90908M 0.0126 . 100 mg/kg C90910M 0.0816 C90911M <LOQ (0.00977 ug/mL) C90916M 0.0221 C90926M <LOQ (0.00977 ug/mL) C90927M 0.0164 C90928M 0.0227 C90933M 0.0112 C90944M 0.0116 C90947M <LOQ (0.00977 ug/mL) C90948M <LOQ (0.00977 ug/mL) C90953M 0.0217 C90955M 0.0154 C90956M <LOQ (0.00977 ug/mL) C90965M 0.0197 C90968M 0.0164 Group 4 C91315F 0.0672 Mid-High Dose C91324F 0.0344 100 mg/kg C91327F 0.0290 C91332F 0.0312 C91335F 0.0562 C91336F 0.0300 C91338F 0.0274 C91340F 0.0101 C91341F 0.0436 C91342F 0 .0 3 3 7 C91356F 0 .0 1 7 8 C91357F 0 .0 3 3 5 C91360F 0 .0 5 7 3 C91361F 0 .0 4 5 9 C91362F 0.0170 C91372F 0.0467 C91376F 0 .0 4 0 8 C91378F 0.0424 C91380F 0.0270 G roup 6 C91047M <LOQ (0.00977 ug/mL) M id-High Dose C91054M <LOQ (0.00977 ug/mL) Recovery C9I056M <LOQ (0.00977 ug/mL) 100 mg/kg C91060M C91065M C91070M <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) C9107IM <LOQ (0.00977 ug/mL) C91072M <LOQ (0.00977 ug/mL) C91073M <LOQ (0.00977 ug/mL) C91076M <LOQ (0.00977 ug/mL) Group 6 C91451F <LOQ (0.00977 ug/mL) Mid-High Dose C91453F <LOQ (0.00977 ug/mL) Recovery C91455F <LOQ (0.00977 ug/mL) 100 mg/kg C91459F <LOQ (0.00977 ug/mL) C91462F C91467F C9I473F C91479F C91480F <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) <LOQ (0.00977 ug/mL) C91485F <LOQ (0.00977 ug/mL) C91487F <LOQ (0.00977 ug/mL) C91488F <LOQ (0.00977 ug/mL) PFOS = Perfluorooctanesulfonate PFOSA = Perfluorooctanesulfonamide PFOSAA = Periluorooctanesuifonaniidoacetale EtFOSE = N arrow Range N -Ethyl Pcrfluorooctanesulfonamido ethyl alcohol M556 = C8Fl7S02N((H)CH2COO) PFOSEA = Perfuorooctane sulfonyl ethylamide A verage E tF O S E -O H ug/m L 0 .0 1 8 2 0 .0 3 6 4 <LOQ <LOQ RSD Std. Dev. MS/MSD RPD Concentration of M556 ug/m L o r */ Ree Average M 556 ug/m L RSD Std. Dev. MS/MSD RPD 6.46 7.66 14.8 6.10 5.99 6.41 8.24 6.94 8.99 4.10 4.16 5.38 4.01 8.71 3.45 93.3 0.0170 4.21 41.18 6.27 6.58 2.71 6.35 4.21 3.20 5.76 5.70 7.53 6.08 3.88 5.05 6.18 2.10 6.25 4.60 3.05 5.12 6.06 6.20 40.0 0.0145 3.76 27.5 5.12 5.06 1.39 <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) NA <LOQ (0.00494 ug/mL) NA NA <LOQ (0.00494 ug/mL) <LOQ NA <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) <LOQ (0.00494 ug/mL) NA <LOQ (0.00494 ug/mL) NA <LOQ (0.00494 ug/mL) <LOQ NA NA Corrected PFOS LOQ (0.0247 ug/m L) to include std correction factors new LOQ is 0.0198 ug/mL. LAC 02/19/01 A - data is above the upper lim it o f quantitation and is provided as an estimate. C o n c e n tra tio n of PFOSEA ug/mL or % Ree <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) 0.00688 <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) 0.00620 <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) <LOQ (0.00492 ug/mL) Date Entered/By: D ate V erified/ By: Purity Entered/Verified: 03/06/00, 03/10/00, 03/20/00, 03/21/00, 4/15/00, 5/16/00, 06/13/00, 6/15/00, 6/19/00, 06/22/00, 06/23/00, 06/26/00, 08/15/00, 09/05/00, 10/17/00 LAC/CSH 04/30/01 h o j / 04/30/01 LAC 02/19/01 LAC Average PFOSEA ug/m L <LOQ <LOQ <LOQ <LOQ RSD Std. Dev. MS/MSD RPD NA NA NA NA NA NA NA NA 3MEnvironmental Laboratory Page 248 3M M edical D epartm ent Study: T6316.1 Study: Product Number(Test Substance): Matrix: MelhodRevision: Analytical Equipment System Number Instrument Softwere/Version: Date of Extrschon/Analyst: Date of Analysts/Analyst Date of Data Reduction/Analysl: Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol inRau T-63I6 (EtFOSE-OH) Rat Liver FACT-M-t.O & FACT-M-2.0 reworked using ETS-8-7.0 Chick 080697, Madeline 041098, and Amelia 062498 MassLyax 2.3 and 3.1 0579/98 and06'01/98 RWW'OK/LAC 06/03'98, 06 05/98,06/12/98,06/14/98,07/09/98,09'02/98 HOJ/KJH/MEE 0275 00,03']4 00,03-15 00,03/16/00,1179/00,12/10/00 MMH'IAS Covance 6329-212 Filename: R-Squared Value: Slope: Y-lntereept See Attachments See Attachments See Attachments See Attachments Analytical Report: FACT-TOX-001 PFOS 06/03/98 Lot 193 06/05/98 Lot 193 06/12/98 Lot 193 06/14/98 Lot 193 PFOSA 06/03/98 Lot L-2353 06/05/98 Lot L-2353 0612/98 U t L-2353 07/09/98 U t L-2353 09/02/98 U t L-2353 PFOSAA 06/03/98 U I6 1 7 06/05,98 U t 617 06/1298 U t617 07/0998 U t 617 09/0298 U t 617 EtFOSE 06/0398 U t 936 06/05/98 U t 936 06/1298 U t 936 07/0998 U t 936 09/0298 U t 936 L R N -U 2103 W EEK 4 RAT LIV ER REW O RK G reup Sample # Duse Initial W t 8 Tutnl Maas uf Liver Method Blk H 20 Blk-1 1.0000 NA H20 Blk-2 1.0000 NA Matrix Blk Rabbit Liver Blk-1 1.0080 40.13 Rabbit Liver Blk-2 1.0080 40.13 QC - lOOppb C907I9M-MS* 1.0248 NA C90719M-MSD 1.0248 NA Group 1 C90719M* 1.0248 NA Control C90725M 1.0364 NA 0.0 mg/kg C90732M 1.0333 NA C90753M 0.9999 NA C90775M 1.0586 NA C91135F 1.0124 NA C91143F 1.0380 NA C91165F 1.0375 NA C91169F 1.0477 NA C91171F 1.0064 NA Group 2 C90789M 1.0591 NA 1nw Dose C908I4M 1.0572 NA 3.0 mg/kg C908I7M 1.0460 NA C90833M 1.0438 NA C90834M 1.0749 NA C9U98F 1.0532 NA C9I205F 1.0651 NA C91222F 1.0183 NA C91230F 1.0433 NA C9I237F 1.0467 NA Group 3 C90846M 1.0108 NA Mid Dose C90853M 1.0440 NA 30.0 mg/kg C90866M 1.0389 NA C90890M 1.0258 NA C90891M 1.0173 NA C91251F 1.0048 NA C91272F 1.0564 NA C91285F 1.0113 NA C91287F 1.0695 NA C91291F 0.9961 NA Group 4 C90935M 0.9603 NA Mid-High Dose C90939M 1.0444 NA 100 mgkg C90942M 1.0119 NA C90961M 1.0621 NA C90966M 1.0166 NA C91316F 1.0324 NA C91317F 0.9882 NA C91333F 1.0133 NA C91345F C91350F 1.0724 1.0509 NA NA Group 5 C90984M 1.0062 NA High Dose C9I005M 1.0225 NA 300 mg/kg C9I024M 1.0121 NA C91033M 1.0339 NA C9I037M 1.027$ NA C9I423F 1.0131 NA C9I427F 1.0217 NA C91430F 1.0191 NA C91443F 1.0106 NA C91448F 1.0130 NA PFOS Perfluorooctanesulfbnete PFOSAc fkrfluorooctanesulfonamide PFOSAA - Perfluorooctanesulfonoinidoacetate EtFOSE - Narrow Range N-Ethyl Perfluorooctanesulfonainido ethyl alcohol Date Entered/Analyst 0573/00,0670/00, 08/15/00 CSHLAC 12/05/00 KJH Date Verified'Analyst U'05/00 KJH, 12/06/00 HOJ Purity Entered/Verified: 1276/00 LAC PFOS Std Curreetton Fa c to r 0.9275 0.9275 0.9275 0.9275 NA NA 0.927 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.927$ 0.927$ 0.927$ 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.927$ 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.927$ 0.927$ 0.9275 0.9275 0.9275 0.9275 0.927$ 0.927$ 0.927$ 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 Lot 193 __________ ___________________________________ ___ ___________ _______________________________Lot L-2353 PFOS Purity Correction Factor Unknown Unknown Unknown Unknown NA NA PFOS Cone. 12.4 0.00 8.66 0.00 1043 1032 PFOS Dilution Factor 1 1 1 1 1 1 Filetta me 60398014 61298056 60398015 61298057 60398042 60398123 PFOS Cale. Cone. It*'* 11.5 0.00 7.97 0.00 233 223 Concentration of PFOS u i/f or % Ree. <LOQ (0.0552 ug/g) <LOO(O.OHO utt/e) <LOO (0.0552 ug/g) <LOO (0.0110 ug/g) 196% 187% PFOS u*/f <LOQ <LOQ 192% RSD Std. Dev. MS/MSD RPD NA NA 5% PFOSA Purity C o r r e c ti o n Unknown Unknown Unknown Unknown NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown 804 1 60398122 723 1 60398043 1091 1 60398044 723 1 60398045 963 1 60398046 221 1 60398050 284 1 60398051 631 1 60398052 454 1 60398053 453 1 60398054 728 647 980 670 844 203 254 564 402 418 0.728 0.647 0.980 0.670 0.844 0.203 0.254 0.564 0.402 0.418 0.774 0.368 17.8 0.138 39.0 0.144 Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown 145 100 60598112 120 100 60598113 132 100 60598114 169 100 60598115 12658 10487 11723 15011 12.7 10.5 11.7 15.0 Unknown Unknown Unknown 13.5 Unknown Unknown Unknown 140 100 60598116 125 1O0 60598119 12069 11027 12.1 11.0 12.4 1.67 Unknown Unknown Unknown Unknown Unknown Unknown 110 1O0 60598120 146 too 60598121 106 100 60598122 152 1O0 60598123 9588 13282 9412 13426 9.59 13.3 9.41 13.4 Unknown Unknown 17.1 Unknown 11.3 1.94 Unknown Unknown 141 500 61498027 64520 64.5 Unknown Unknown Unknown Unknown 194 500 61498028 249 500 61498029 243 500 61498030 86362 110931 109767 86.4 111 110 Unknown Unknown 21.2 Unknown Unknown Unknown 239 500 61498031 215 500 61498034 108824 99018 109 99.0 96.1 20.4 Unknown Unknown Unknown Unknown Unknown 277 500 61498035 200 500 61498036 319 500 61498037 121385 91929 138167 121 91 9 138 Unknown Unknown 21.0 Unknown Unknown 325 500 61498038 151495 151 120 25.3 Unknown Unknown 66.4 2000 M061298067 128159 128 Unknown Unknown Unknown Unknown 94.2 2000 MO61298068 167259 111 2000 M061298069 202805 151 2000 M061298070 263867 167 203 264 Unknown Unknown 26.8 Unknown Unknown Unknown 127 2000 M061298071 231647 94.2 2000 M061298072 169257 232 169 199 53.2 Unknown Unknown Unknown Unknown 223 2000 M061298074 419299 121 2000 M061298075 220960 419 221 Unknown Unknown Unknown 141 2000 M061298076 243655 244 52.8 Unknown Unknown 52.5 2000 M061298077 92724 92.7 229 121 Unknown Unknown 41.6 5000 M061298078 191685 192 Unknown Unknown 86.4 5000 M061298081 391682 392 Unknown Unknown 144 5000 M061298082 661557 662 Unknown Unknown 154 5000 M06I298083 691925 692 41.7 Unknown Unknown 124 5000 M06I298084 559479 559 499 208 Unknown Unknown 122 5000 M06I298085 557635 558 Unknown Unknown Unknown 83.7 5000 M06I298088 379688 107 5000 M061298089 488915 380 439 Unknown Unknown Unknown Unknown 178 5000 M061298090 816358 162 5000 M06I298091 740764 816 741 30.1 Unknown 597 180 Unknown + CCVs not within criteria due to carryover, estimated results. * Below LOQ, tentative numbers. ++ Above the linear range o f the curve, data are estimated. Samples were mislabeled during the extraction or analysis. A deviation was written and sample data switched. PFOSA Com. .00 0.00 0.00 0.00 130 145 9.19 10.2 18.4 10.5 25.2 2.23 23.0 31.6 14.4 13.6 520 320 $07 900 721 670 676 663 794 756 80.5 53.1 74.4 74.6 67.1 59.6 78.3 48.2 59.5 70.1 94.6 69.3 88.3 139 97.0 75.4 107 92.8 95.3 53.0 1.37 6.32 12.7 13.6 11.8 15.7 13.6 16.5 14.8 12.0 PFOSA Dilution Factor 1 1 1 1 1 1 1 1 1 I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 too too 100 100 100 100 100 100 100 100 too 100 100 100 100 100 100 100 100 100 1000 1000 1000 1000 tooo 1000 1000 1000 1000 1000 Filettaroe 60398014 61298056 60398015 61298057 60398042 60398123 60398122 60398043 60398044 60398045 60398046 60398050 60398051 60398052 60398053 60398054 60598098 60598099 60598100 60598101 60598102 60598105 60598106 60S98107 60598108 60598109 M090298049 M090298050 M090298051 M090298052 M090298053 M090298057 M090298058 M090298059 M090298060 M090298061 M07099813 M07099814 M07099815 M07099816 M07099817 M07099820 M07099821 M07099822 M07099823 M07099824 7099827 7099828 7099829 7099830 7099831 7099834 7099835 7099836 7099837 7099838 PFOSA Cak. Com. 0.00 0.00 0.00 0.00 121 132 8.97 9.86 17.8 10.5 23.8 2.20 22.1 30.4 13.8 13.5 491 302 485 863 670 636 635 651 761 722 7961 5083 7159 7276 6598 5934 7413 4761 5566 7036 9841 6639 8722 13084 9543 7302 10851 9162 8889 5043 1362 6181 12528 13154 11465 15517 18156 16152 14645 11836 Co M c n tr n ti o ii of PFOSA u f /t o r % Ree. <LOQ (0.0121 ug/g) <LOO (0.00604 ug/g) <LOQ (0.0121 ug/g) <LOO (0.00604 ue/e) 100% 110% 0.00897 <LOQ (0.0121 ug/g) 0.0178 <LOO (0.0121 ug/c) 0.0238 <LOO (0.0121 ug/g) 0.0221 0.0304 0.0138 0.0135 0.491 0.302 0.485 0.863 0.670 0.636 0.635 0.651 0.761 0.722 7.96 .0 8 7.16 7.28 6.60 5.93 7.41 4.76 5.57 7.04 9.84 6.64 8.72 13.1 9.54 7.30 10.9 9 16 8.89 5.04 1.36 6.18 12.5 13.2 11.5 15.5 18.2 16.2 14.6 11.8 * * * PFOSA <LOO <LOQ 105% 0.0150 0.0184 0.562 0 681 6.82 6 14 9.57 8.25 8.94 15.3 RSD Std. Dev. MS/MSD RPD NA NA 9% 49.9 0.00746 43.7 0.00804 37.8 0.212 8.39 0.0572 15.9 1.08 17.6 1.08 24.4 2.33 26.5 2.19 56.5 5.05 15.1 2.31 Corrected PFOS LOQs(0.0595 & 0.0119 ug/g) to include std correction factors new LOQs are 0.0552 & 0.0110 ug/g. LAC 02/19'01 3MEnvironmental Laboratory Page 249 3M M edical D epartm ent Study: T6316.1 Study: Product Number(Test Substance): Matrix: MethodRevision: Analytical Equipment System Number Instrument Software/Version: Date of Extraction/Analyst Date o f Analysia/Analyst: Date of Data Reduction/Analyst Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98.154) N-Ethyl Perfluorooctanesulfoniimido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Liver Filename: FACT-M-1.0 & FACT-M-2.0 reworked using ETS-8-7.0 Chick 080697, Madeline 041098, and Amelia 062498 MassLynx 2.3 and 3.1 R-Squared Value: Slope: Y-Intcrcept 05/29/98 and 06/01 *98 RWW/OK/LAC 06 03 98, 06/05/98,0 6 'I2 9 8 , 06/14/98,07/0998,09/0298 HOJ/KJH/MEE 0225/00, 03'14'00,03 15 00,03/16/00,11/29/00,12/10/00 MMH/IAS See Attachments See Attachments See Attachments See Attachments W EEK 4 RAT L IV E R R E W O R K Lot617 Group Duse Method Blk Matrix Blk QC - lOOppb Sample It H20 Blk-I H20 BIk-2 Rabbit Liver Blk-I Rabbit Liver Blk-2 C9 0 7 |9 M -M SA C907I9M-MSD PFOSAA Purity Correction Factor Unknown Unknown Unknown Unknown NA NA PFOSAA Cane. 3.85 0.00 0.00 0.00 187 191 Control Group 1 C90719MA C90725M C90732M C90753M C90775M C91135F C91143F C91165F C91169F C91171F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown 52.7 109 147 151 232 11.5 80.9 167 83.7 116 Group 2 Low Dose 3.0 mg/kg C90789M C90814M C90817M C90833M C90834M C91I98F C91205F C91222F C91230F C91237F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown 221 205 193 203 272 809 293 396 221 421 Group 3 Mid Dose 30.0 mg/kg C90846M C90853M C90866M C90890M C90891M C9125IF C91272F C91285F C91287F C91291F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown 989 525 529 403 608 462 991 260 440 1020 Grotq>4 Mid-High Dose 100 mg/kg C90935M C90939M C90942M C90961M C90966M C91316F C913I7F C91333F C91345F C91350F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown 486 384 335 936 579 509 531 543 792 337 Greup 5 High Dose 300 mg/kg C90984M C91005M C91024M C91033M C91037M C9I423F C9I427F C9I430F C91443F C91448F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown 79.7 62.1 94.6 120 81.8 85.0 32.3 30.2 151 108 PFOS = Perfluorooclanesulfonate PFOSA r Perfluorooctanesulfonanude PFOSAA1 Perfluorooctanesulfonamidoacetate ElFOSE 3 Narrow Range N-Ethyl Perfluorooclanesulfonamido ethyl alcohol Dale Entered/Analyst: 05/23/00,06/20/00,08/15.'00 CSRLAC 12/05/00 KJH Dale Verified/Analyst: 12/05/00 KJH, 12/06/00 HOJ Purity EnteredVerified: 12/26/00 LAC Corrected PFOS LOQs (0.0595 & 0.0119 ug/g) to include std correction factors new LOQs are 0.0552 & 0.0110 ug/g. LAC 02/19/01 PFOSAA M utton Fnctor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 10 10 10 50 10 10 10 10 10 10 100 100 100 100 100 100 100 100 100 100 100 100 100 too too too 100 100 100 100 1000 1000 1000 1000 1000 100O 1000 1000 1000 1000 ___________________________ ________________________________________ L ot936 Filename 60398014 61298056 60398015 61298057 60398042 60398123 60398122 60393043 60398044 60398045 60398046 60398050 PFOSAA Calc. Cane. *1% 3.85 0.00 0.00 0.00 131 134 51.5 105 143 151 219 11.3 Concentrattan e f PFOSAA u t/f r % Ree. <LOO (0.0633 ug/g) < L O O (0 .l2 7 u g /g ) <LOQ (0.0633 ug/g) <LOQ (0.127 ug/g) 103V. 106V. 0.0515 0.105 0.143 0.151 0.219 <LOQ (0.0633 ug/g) PFOSAA ug/f <LOQ <LOQ 104% 0.134 RSD Std. Dev. MS/MSD RPD NA NA 3% 46.1 0.0617 EtFOSE Purity Correction Factor Unknown Unknown Unknown Unknown NA NA Unknown Unknown Unknown Unknown Unknown Unknown 60398051 60398052 60398053 60398054 77.9 161 79.8 115 0.0779 0.161 0.0798 0.115 0.0995 39.2 0.0390 Unknown Unknown Unknown Unknown 60598140 60598141 2087 1940 2.09 1.94 Unknown Unknown 60598142 60598129 60598144 1846 9732 2528 1.85 9.73 2.53 Unknown 94.4 Unknown 3.63 3.42 Unknown 60598147 60598148 60598149 7681 2751 3893 7.68 2.75 3.89 Unknown Unknown Unknown 60598150 60598151 2123 4020 2.12 4.02 52.7 Unknown 4.09 2.16 Unknown 90298049 90298050 90298051 97855 50290 50940 97.9 * 50.3 + 50.9 + Unknown Unknown Unknown 90298052 90298053 39263 59731 39.3 + 59.7 + 59.6 37.9 Unknown 22.6 Unknown 90298057 90298058 46022 93774 46.0 * 93.8 + Unknown Unknown 90298059 90298060 90298061 25750 41154 102446 25.8 + 41.2 + 102 * 61.8 Unknown 55.1 Unknown 34.1 Unknown M07099813 M07099814 M07099815 50589 36794 33108 50.6 36.8 33.1 Unknown Unknown Unknown M07099816 M07099817 88123 56911 88.1 56.9 41.2 Unknown 53.1 21.9 Unknown M07099820 M07099821 M07099822 M07099823 M07099824 49348 53684 53610 73837 32106 49.3 53.7 53.6 73.8 32.1 Unknown Unknown Unknown 28.3 Unknown 52.5 14.9 Unknown M07099827 M07099828 M07099829 M07099830 M07099831 M07099834 M07099835 M07099836 M07099837 M07099838 79219 60714 93469 115688 79582 83911 31653 29614 149030 106357 79.2 60.7 93.5 116 79.6 85.7 83.9 31.7 * 29.6 * 149 106 80.1 Unknown Unknown Unknown 23.8 Unknown 20.4 Unknown Unknown Unknown Unknown 63.5 Unknown 50.9 Unknown + CCVs not within criteria due to carryover, estimated results. * Below LOQ, tentative numbers. ++ Above the linear range of the curve, data are estimated. ' Samples were mislabeled during the extraction or analysis. A deviation was written and sample data switched. EtFOSE Com. 32.5 0.00 0.00 0.00 194 133 0.00 0.00 0.00 30.7 0.00 0.00 0.00 0.00 0.00 0.00 23.5 0.00 0.00 0.00 0.00 0.00 0.00 69.2 0.00 0.00 128 45.7 64.0 117 79.6 51.3 49.1 44.8 41.9 33.9 656 167 328 449 432 640 267 154 124 247 375 496 1127 1045 551 926 1459 753 364 371 EtFOSE Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 l 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 I 1 1 I 1 l 1 1 Analytical Report: FACT-TOX-001 L R N -U 2103 Filename 60398014 61298056 60398015 61298057 60398042 60398123 60398122 60398043 60398044 60398045 60398046 60398050 60398051 60398052 60398053 60398054 60598098 60598099 60598100 60598101 60598102 60598105 60598106 60598107 60598108 60598109 90298064 90298065 90298066 90298067 90298068 90298072 90298073 90298074 90298075 90298076 90298079 90298080 90298081 90298082 90298083 90298087 90298088 90298089 90298090 90298091 90298094 90298095 90298096 90298097 90298098 90298102 90298103 90298104 90298105 90298106 EtFOSE Calc. Cone. 32.5 0.00 0.00 0.00 189 129 0.00 0.00 0.00 30.7 0.00 0.00 0.00 0.00 0.00 0.00 22.2 0.00 0.00 0.00 0.00 0.00 0.00 68.0 0.00 0.00 128 45.7 64.0 117 79.6 51.3 49.1 44.8 41.9 33.9 683 NA 324 422 425 620 270 NA NA 235 372 486 1113 1011 536 914 1428 739 361 366 Concentration of EtFOSE ut/* or % Ree. <LOQ (0.0596 ug/g) <LOQ (0.119 ug/g) <LOO (0.0596 uc/ci <LOO (0.119 ue/e) 158% 109% <LOO 0.0596 up/cl <LOO (0.0596 uv/s-l <LOQ (0.0596 ug'g) <LOQ (0.0596 ug/g) <LOQ (0.0596 ue/s> <LOQ (0.0596 ug/g) <LOQ (0.0596 ug/g) <LOQ (0.0596 ug/g) <LOQ (0.0596 ug/g) <LOQ (0.0596 ug/g) <LOQ (0.119 ug/g) <LOQ (0.119 ug/g) <LOQ (0.119 ug/g) <LOQ (0.119 ug/g) <LOQ (0.119 ug/g) <LOQ (0.119 ug/g) <LOO (0.119 u/el <LOO (0.119 u*/1 <LOO (0.119 uc/fl <LOQ (0.119 ug/R) 0.128 0.0457 0.0640 0.117 0.0796 0.0513 0.0491 0.0448 0.0419 0.0339 0.683 NA 0.324 0.422 0.425 0.620 0.270 NA NA 0.235 0.372 0.486 1.11 1.01 0.536 0.914 1.43 0 739 0.361 0.366 ++ *+ ++ EtFOSE <LOO <LOQ 133% <LOQ <LOQ <LOQ <LOQ 0.0870 0.0442 0.464 0.375 0.704 0.762 RSD Std. Dev. MS/MSD RPD NA NA 37% NA NA NA NA NA NA NA NA 40.4 0.0351 15.4 0.00682 33.1 0.154 56.7 0.213 47.5 0.335 58.2 0.443 3MEnvironmental Laboratory Page 250 3M M edical D epartm ent Study: T6316.1 c~0"n;e~~;212 Study: Product Numbei(Tesl Substance): Matrix: Method/Revision: Analytical Equipment System Number Instrument Software/Version: Date of Extraction/Analyst: Date of Analysis/Analyst Date orData Rcduction/Analyst: Sam ple D ata 104 Week Dietary Carcinogenicity Study nith Narrow Range (98.1V) N-Ethyl Perfluorooctanesulfonatrtido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Liver FACT-M-1.0 & FACT-M-2.0 reworked using ETS-8-7.0 Chick 080697, Madeline 041098, and Amelia 062498 MassLynx 2.3 and 3.1 Filename: R-Squired Value: Slope: Y-Intercept: See Attachments See Attachments See Attachments See Attachments 05/29/98 and 06/01/98 RWW-OIOLAC 06 03/98, 06/05/98, 06/12/98, 06/14 98,07/09:98,09/02/98 HOJ/KJH/MEE 02 25'00, 03/14'00, 03 15/00, 03 16/00. 1|/29'00, 12/10/00 MMH1AS WEEK 4 RAT LIVER REWORK Group Dose Sample # PFOS Cale. Cone. Concentration of PFOS u t/c o r % Ree. Method Blk K 20 Blk-1 11.5 <LOO (0.0552 uc/et H 20 Blk-2 0.00 <LOQ (0 0110 ur/r) Matrix Blk Rabbit Liver Blk-1 7.97 <LOQ (0.0552 ug/g) Rabbit Liver Blk-2 0.00 <LOQ (0.0110 ur/r) Q C- lOOppb C90719M-MS* C90719M-MSD 233 223 196% 187% C90719M' 728 0.728 Control C90725M 647 0.647 Group 1 C90732M 980 O.980 C90753M 670 0.670 C90775M 844 0.844 C91135F 203 0.203 C91143F 254 0.254 C91165F 564 0.564 C91169F C91171F 402 418 0.402 0.418 Group 2 C90789M 12658 12.7 Low Dose C90814M 10487 10.5 3.0 mg/kg C90817M 11723 11.7 C90833M 15011 15.0 C90834M 12069 12.1 C91198F 11027 11.0 C91205F 9588 9.59 C91222F 13282 13.3 C91230F 9412 9.41 C91237F 13426 13.4 Group 3 C90846M 64520 64.5 Mid Dose C90853M 86362 864 30.0 mg/kg C90866M 110931 111 C90890M 109767 110 C9089IM 108824 109 C9I251F 99018 99.0 C91272F 121385 121 C91285F 91929 91.9 C91287F 138167 138 C91291F 151495 151 Group 4 C90935M 128159 128 Mid-High Dose C90939M 167259 167 100 mg/kg C90942M 202805 203 C90961M 263867 264 C90966M 231647 232 C9I316F 169257 169 C9I317F C91333F 419299 220960 419 221 C91345F C91350F 243655 92724 244 92.7 Group 5 C90984M 191685 192 High Dose 300 mgkg C91005M C91024M 391682 661557 392 662 C91033M 691925 692 C91037M 559479 559 C91423F 557635 558 C9I427F 379688 380 C91430F 488915 489 C91443F C91448F 816358 740764 816 741 PFOS = Perfluorooctaacsulfonatc * PFOSA - Periluorooctanesulfonamide PFOSAA = Pcriluorooctanesulfonamidoacetale ElFOSE - Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol Date EnteredAnalyst 0523/00,06/20/00,08/15/00 CSK/TAC 12'05/00 KJH Dale Verified/Analyst 12.05/00 IUH, 12/06/00 HOJ Purity Enlered'Verified: 12/26/00 LAC Corrected PFOS LOQs (0.0595 & 0.0119 ug/g) to include std correction factors new LOQs are 0.0552 & 0.0110 ug/g. LAC 02'19/01 PFOS <LOO <LOQ 192% 0.774 0.368 12.4 11.3 96.1 120 199 229 499 597 RSD Std Dev. MS/MSDRPD NA NA 5% 17.8 0.138 39.0 0.144 13.5 1.67 17.1 1.94 21.2 20.4 21.0 25.3 26.8 53.2 52.8 121 41.7 208 30.1 180 PFOSA Concentra tion RSD PFOSAA Calc. Cone. 0.00 of PFOSA ug/g or % Roc. <LOQ (0.0121 ug/g) PFOSA S td Dev. MS/MSD RPD Calc. Cone. "*' 3.85 0.00 <LOO (0.00604 ur/r) <LOQ NA 0.00 0.00 <LOQ (0.0121 ug/g) 0.00 0.00 <LOQ (0.00604 ur/r) <LOQ NA 0.00 121 100% 132 110% 105% 131 9% 134 8.97 0.00897 51.5 9.86 <LOQ (0.0121 ug/g) 105 17.8 0.0178 143 10.5 <LOQ (0.0121 ug/g) 49.9 151 23.8 0.0238 0.0150 0.00746 219 2.20 <LOO (0.0121 ur/r 11.3 22.1 0.0221 77.9 30.4 0.0304 161 13.8 0.0138 43.7 79.8 13.5 0.0135 0.0184 0.00804 115 491 0.491 2087 302 0.302 485 0.485 863 0.863 670 0.670 636 0.636 0.562 37.8 0.212 1940 1846 9732 2528 7681 635 0.635 2751 651 0.651 3893 761 0.761 722 0.722 0.681 8.39 0.0572 2123 4020 7961 7.96 97855 5083 7159 5.08 7.16 50290 50940 7276 6598 5934 7413 7.28 6.60 5.93 7.41 15.9 39263 6.82 1.08 59731 46022 93774 4761 4.76 25750 5566 7036 5.57 7.04 17.6 41154 6.14 1.08 102446 9841 9.84 50589 6639 6.64 36794 8722 8.72 33108 13084 9543 7302 10851 9162 13.1 9.54 7.30 10.9 9.16 24.4 88123 9.57 2.33 56911 49348 53634 53610 8889 8.89 5043 5.04 26.5 73837 8.25 2.19 32106 1362 1.36 * 79219 6181 6.18 * 60714 12528 12.5 * 93469 13154 13.2 56.5 115688 11465 15517 11.5 15.5 8.94 5.05 79582 83911 18156 18.2 31653 16152 16.2 29614 14645 11836 14.6 11.8 15.1 149030 15.3 2.31 106357 * CCV'snot within criteria due to carryover, estimated results. * Below LOQ, tentative numbers. ++ Above the linear range o f the curve, data are estimated ASamples were mislabeled during the extraction or analysis. A deviation was written and sample data switched . Concentration of PFOSAA Uf/ | or % Ree. <LOQ (0.0633 ug/g) <LOQ (0.127 ur/r) <LOQ (0.0633 ug/g) <LOQ (0.127 ur/r) 103% 106% 0.0515 0.105 0.143 0.151 0.219 <LOO (0.0633 ur/r) 0.0779 0.161 0.0798 0.115 2.09 1.94 1.85 9.73 2.53 7.68 2.75 3.89 2.12 4.02 97.9 50.3 50.9 39.3 59.7 46.0 93.8 25.8 41.2 102 50.6 36.8 33.1 88.1 56.9 49.3 53.7 536 73.8 32.1 79.2 60.7 93.5 116 79.6 83.9 31.7 29.6 149 106 + + + + + + + + + . - PFOSAA <LOQ <LOQ 104% 0.134 0.0995 3.63 4.09 59.6 61.8 53.1 52.5 85.7 80.1 Analytical Report: FACT-TOX-001 L R N -U 2103 RSD Std. Dev. MS/MSDRPD NA NA 3% 46.1 0.0617 39.2 0.0390 94.4 3.42 52.7 2.16 37.9 22.6 55.1 34.1 41.2 21.9 28.3 14.9 23.8 20.4 63.5 50.9 EtF O S E Calc. Cone. 32.5 0.00 0.00 0.00 189 129 0.00 0.00 0.00 30.7 0.00 0.00 0.00 0.00 0.00 0.00 22.2 0.00 0.00 0.00 0.00 0.00 0.00 68.0 0.00 0.00 128 45.7 64.0 117 79.6 51.3 49.1 44.8 41.9 33.9 683 NA 324 422 425 620 270 NA NA 235 372 486 1113 1011 536 914 1428 739 361 366 Concentration o f EtFOSE u c/t or % Ree. <LOQ (0.0596 ug/g) <LOQ (0.119 ur/r) <LOQ (0.0596 ug/g) <LOO (0.119 ur/r) 158% 109% <LOQ (0.0596 ug/g) <LOQ (0.0596 ug/g) <LOQ (0.0596 ug/g) <LOQ (0.0596 ug/g) <LOO (0.0596 ur/r) <LOQ (0.0596 ug/g) <LOQ (0.0596 ug/g) <LOQ (0.0596 ug/g) <LOQ (0.0596 ug/g) <LOQ (0.0596 ug/g) <LOQ (0.119 ug/g) <LOQ (0.119 ug/g) <LOQ (0.119 ug/g) <LOQ (0.119 ug/g) <LOQ (0.119 ur/r) <LOO (0.119 up/p1 <LOQ (0.119 ug/g) <LOQ (0.119 ug/g) <LOO (0.119 uc/el <LOQ (0.119 ur/r) 0.128 0.0457 0.0640 0.117 0.0796 0.0513 0.0491 0.0448 0.0419 0.0339 0.683 NA 0.324 0.422 0.425 0.620 0.270 NA NA 0.235 0.372 0.486 111 1.01 0.536 0.914 1.43 0.739 0.361 0.366 ++ ++ +* Mean EtFOSE <LOQ <LOQ 133% <LOO <LOQ <LOQ <LOQ 0.0870 0.0442 0.464 0.375 0.704 0.762 RSD Std. Dev. MS/MSD RPD NA NA 37% NA NA NA NA NA NA NA NA 40.4 0.0351 15.4 0.00682 33.1 0.154 56.7 0.213 47.5 0.335 58.2 0.443 3MEnvironmental Laboratory Page 251 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product Number(Test Substance): Matrix: Method/Revision: Analytical Equipment System Num ber Instrument Software/Version: Date o f Extraction/Analyst: Date o f Analysis/Analyst: Date o f Data Reduction/Analyst: Sample Data 06/14/98 Lot 193 06/18/98.12/29/98 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesuifonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Liver FACT-M-1.0 & FACT-M-2.0 reworked using ETS-8-7.0 Filename: See List to Right Filenames Chick 080697 and Madeline 041098 M assLynx2.3 and 3.1 R-Squared Value: See Attachments Slope: See Attachments Blks Grp 1 06/01/98 RWW/OK 06/12/98,06/14/98,06/18/98,09/02/98 HOJ/KJH/LAC Y-Intercept: See Attachments Grp 5 MS, MSD 03/16/00, 11/29/00,12/01/00, 12/10/00 IAS/MMH/KJH 06/12/98 Lot L-2353 09/02/98 Lot L-2353 06/12/98 Lot 617 06/18/98 Lot 617 PFOS PFOSA M06189834-35& 60-61 A90298002-3 & 116-117 06189852-57, 122998069-W 298019-31 61498013-24 122998041-52 61298127-128 61298127-128 06/12/98 Lot 936 09/02/98 Lot 936 PFOSAA M06189834-35 & 60-61 06189845-57 122998055-66 61298127-128 EtFOSE Dilutions A90298002-3 & 1/1,1/1,1/1, 1/1 90298019-31 1/1,1/1,1/1, LI need 1:10 dii. 1/10000, 1/100, 1/1000, 1/10 90298110-111 need 1:5 dii, 1/1, I/l, 1/1 W EEK 8 RAT LIVER REWORK Group Sample # Initial Wt. Total Mass Dose g o f Liver g Method Blk H 20 Blk-1 1.0000 NA H 20 Blk-2 1.0000 NA Matrix Blk Rabbit Liver Blk-1 1.0080 40.13 Rabbit Liver Blk-2 1.0080 40.13 QC -100 ppb C907I7M-MS 1.0248 NA C90717M-MSD 1.0248 NA Group 1 C90717M 1.0455 NA Control C90718M 1.0268 NA 0.0 mg/kg C90737M 1.0434 NA C90756M 1.0089 NA C90769M 1.0083 NA C91126F 1.0205 NA C9I140F 1.0265 NA C91145F 1.0128 NA C91162F 1.0160 NA C9I163F 1.0162 NA Group 5 . C90971M 1.0129 NA High Dose C90972M 1.0204 NA 300 mg/kg C90988M 1.0108 NA C90996M 1.0128 NA C91017M 1.0116 NA C91393F 1.0247 NA C91394F 1.0126 NA C9I404F 1.0149 NA C91415F 1.0244 NA C91438F 1.0230 NA PFOS = Perfluorooctanesulfonate PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonamidoacelate EtFOSE = Narrow Range N-Ethyl Perfiuorooctanesulfonamido ethyl alcohol PFOS Std Correction Factor 0.9275 0.9275 0.9275 0.9275 NA NA 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 Lot 193 PFOS Purity Correction Factor Unknown Unknown Unknown Unknown NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown PFOS Cone. ng/g 0.00 47.4 0.00 33.1 1153 959 313 222 307 218 124 270 383 558 1198 605 137 122 136 97.3 90.6 96.5 103 112 116 157 PFOS Dilution Factor PFOS Calc. Cone, ng/g Filename 1 0.00 61298056 1 43.9 122998002 1 0.00 61298057 1 30.4 122998003 1 -1584 61298127 1 -1773 61298128 10 2776 122998073 10 2004 122998072 10 2731 122998071 10 2002 122998070 10 1144 122998069 1 245 6189852 1 346 6189853 1 511 6189854 1 1094 6189855 1 552 6189856 . 10000 10000 1250280 1111564 61498013 61498014 10000 1249941 61498015 10000 890777 61498016 10000 830679 61498017 10000 10000 10000 10000 10000 873644 945819 1027570 1054710 1423345 61498020 61498021 61498022 61498023 61498024 * Data above the linear calibration range, estimated value. ' + CC V's failed, data entered as estimated ' ' confirmed low on 90298 ++ Qualitative data only. Concentration Mean of PFOS PFOS ug/g or % Ree. <LOQ (0.0110 ug/g) ug/g <LOQ (0.112 ug/g) <LOQ <LOQ (0.0110 ug/g) <LOQ (0.112 ug/g) < LOQ -1331% -1490% * -1410% 2.78 + 2.00 + 2.73 + 2.00 + 1.14 + 2.13 0.245 0.346 0.511 1.09 * 0.552 0.549 1250 1112 1250 891 831 1067 874 946 1028 1055 1423 1065 RSD Std. Dev. MS/MSD RPD NA NA 11% 31.3 0.668 59.8 0.328 18.5 197 20.0 213 Date Entered/Analyst: Date Verified/Analyst: Purity Entered/Verified: 4/13/00, 5/24/00 CSH 12/12/00 MMH 12/28/00 hoj (list a!22998a) 12/26/00 LAC Corrected PFOS LOQs (0.0119 & 0.0121 ug/g) to include std correction factors new LOQs are 0.0110 & 0.112 ug/g. LAC 02/19/01 ETS-8-7.0 Excel 97 3MEnvironmental Laboratory Lvr Week 8 Rework TOX-001-liver2l2-10O.xls Page 252 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Product Number(Test Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Date o f Extraction/Analyst: Date o f Analysis/Analyst: Date o f Data Reduction/Analyst: Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Liver FACT-M-l.O & FACT-M-2.0 reworked using ETS-8-7.0 Filename: See List to Right Chick 080697 and Madeline 041098 R-Squared Value: See Attachments MassLynx 2.3 and 3.1 Slope: See Attachments 06/01/98 RWW/OK Y-Intercept: See Attachments 06/12/98,06/14/98,06/18/98,09/02/98 HOJ/KJH/LAC 03/16/00,11/29/00, 12/01/00, 12/10/00 IAS/MMH/KJH W EEK 8 RAT LIVER REWORK L o tL -2 3 5 3 Group Sample * PFOSA Purity Dose Correction Factor M ethod Blk H 20 Blk-1 Unknown H 20 Blk-2 Unknown Matrix Blk Rabbit Liver Blk-1 Unknown Rabbit Liver Blk-2 Unknown QC -100 ppb C90717M-MS C90717M-MSD NA NA Group 1 C90717M Unknown Control 0.0 mg/kg C907I8M C90737M Unknown Unknown C90756M Unknown C90769M C91126F C91140F Unknown Unknown Unknown C91145F Unknown C91162F C91163F Unknown Unknown Group 5 High Dose C90971M C90972M Unknown Unknown 300 mg/kg C90988M Unknown C90996M Unknown C91017M Unknown C9I393F Unknown C9I394F C9I404F C91415F C91438F Unknown Unknown Unknown Unknown PFOS = Perfluorooctanesulfonate PFOSA = Perfluorooctanesuffnnamide PFOSAA - Perfluorooctanesulfonamidoacetale EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol PFOSA Cone. ng/g 0.0 66.3 0.0 41.8 83.4 65.4 33.8 19.6 35.2 31.1 10.1 104 10.4 12.7 35.0 15.2 196 191 191 211 185 154 142 174 142 177 PFOSA Dilution Factor I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 100 100 100 100 100 100 100 100 100 100 PFOSA Filename Concentration Mean Calc. Cone, ng/g of PFOSA ug/g or % Ree. PFOSA ug/g 0.00 61298056 <LOQ (0.0119 ug/g) 66.3 122998002 0.0663 + 0.0391 0.00 61298057 <LOQ (0.0119 ug/g) 41.4 t2298003 0.0414 + 0.0267 48.4 61298127 40% 30.8 61298128 26% * 33% 32.4 90298019 0.0324 <LOQ (0.0302 ug/g) 90298020 <LOQ (0.0302 ug/g) 33.7 90298021 0.0337 <LOQ (0.0302 ug/g) 90298022 <LOQ (0.0302 ug/g) <LOO (0.0302 ug/g) 90298023 <LOQ (0.0302 ug/g) 0.0313 <LOQ (0.0302 ug/g) 90298027 <LOQ (0.0302 ug/g) <LOQ (0.0302 ug/g) 90298028 <LOQ (0.0302 ug/g) <LOQ (0.0302 ug/g) 90298029 <LOQ (0.0302 ug/g) 34.4 90298030 0.0344 <LUQ (0.0302 ug/g) 90298031 <LOQ (0.0302 ug/g) 0.0310 19353 12298045 19.4 + 18747 18897 20877 12298044 12298043 12298042 18.7 + 18.9 + 20.9 + 18323 14999 14071 12298041 12298052 12298051 18.3 + 19.2 15.0 + 14.1 + 17148 12298050 17.1 + 13844 12298049 13.8 + 17272 12298048 17.3 + 15.5 * Data above the linear calibration range, estimated value. + CCVs failed, data entered as estimated "' confirmed low on 90298 ++ Qualitative data only. Date Entered/Analyst: Date Verified/Analyst: Purity Entered/Verified: 4/13/00, 5/24/00 CSH 12/12/00 MMH 12/28/00 hoj (list al22998a) 12/26/00 LAC Corrected PFOS LOQs (0.0119 & 0.0121 ug/g) to include std correction factors new LOQs are 0.0110 & 0.112 ug/g. LAC 02/19/01 RSD Std. Dev. M S/M SD R P D NA NA 44% 5.21 0.00163 6.09 0.00189 5.13 0.987 10.7 1.65 Analytical Report: FACT-TOX-001 . LRN-U2103 ETS-8-7.0 Excel 97 3MEnvironmental Laboratory Lvt Week 8 Rework TOX-OO1-liver212-1OO xls ' 5/31/2001 Page 253 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 . LRN-U2103 Study: Product NumberfTest Substance): Matrix: Method/Revision: Analytical Equipment System Number Instrument Software/Version: Date o f Extraction/Analyst: Date o f Analysis/Analyst: Date o f Data Reduction/Analyst: Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfiuorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Liver FACT-M-1.0 & FACT-M-2.0 reworked using ETS-8-7.0 Filename: See List to Right Chick 080697 and Madeline 041098 R-Squared Value: See Attachments MassLynx 2.3 and 3.1 Slope: See Attachments 06/01/98 RWW/OK Y-lntercept: See Attachments 06/12/98,06/14/98,06/18/98,09/02/98 HOJ/KJH/LAC 03/16/00,11/29/00,12/01/00,12/10/00 IAS/MMH/KJH W EEK8 RATLIVER L o t6 l7 Group Dose Method Blk Matrix Blk QC -100 ppb Sample # H 2 0 Blk-1 H 2 0 Blk-2 Rabbit Liver Blk-1 Rabbit Liver Blk-2 C90717M-MS C90717M-MSD PFOSAA Purity Correction Factor Unknown Unknown Unknown Unknown NA NA PFOSAA Cone, nt i l 27.2 0.00 13.0 0.00 88.6 97.6 Group 1 Control 0.0 mg/kg C90717M C90718M C90737M C90756M C90769M C91126F C91140F C91145F C91162F C91163F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown 76.0 90.4 156 118 3.13 15 6 1.74 40.6 195 79.4 Group 5 High Dose 300 mg/kg C90971M C90972M C90988M C90996M C91017M C91393F C9I394F C91404F C91415F C91438F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown 512 594 478 480 384 306 272 375 293 439 PFOS = Perfluorooctanesulfonate PFOSA = Perfluorooctanesulfonamide PFOSAA - Perfluorooclanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol PFOSAA Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 PFOSAA Calc. Cone, ng/g 27.2 0.00 12.9 0.00 12.3 21.0 72.7 88.1 149 117 3.10 15.2 1.70 40.1 192 78.1 505667 581791 473002 473865 379557 298858 268201 369672 286207 429003 Filename 61898 34 S001206005 6189835 sOO1206006 61298127 61298128 6189845 6189846 6189847 6189848 6189849 6189852 61898 53 6189854 6189855 6189856 122998059 122998058 122998057 122998056 122998055 122998066 122998065 122998064 122998063 122998062 Concentration Mean RSD o f PFOSAA PFOSAA Std. Dev. ug/g or % Ree. ug/g MS/MSD RPD <LOQ (0.633 ug/g) <LOQ (0.633 ug/g) <LOQ NA <LOQ (0.633 ug/g) <LOQ (0.633 ug/g) <LOQ NA 10% + 17% + 13% 52% 0.0727 0.0881 0.149 0.117 35.8 <LOQ (0.633 ug/g) 0.0980 0.0351 <LOQ (0.633 ug/g) <LOQ (0.633 ug/g) <LOQ (0.633 ug/g) 0.192 61.1 0.0781 0.0920 0.0561 . 506 + 582 + 473 + 474 + 15.1 380 + 433 72.7 299 + 268 + 370 + +286 + 429 330 20.3 67.2 * Data above the linear calibration range, estimated value. + CCV's failed, data entered as estimated ` ` confirmed low on 90298 Qualitative data only. Date Entered/Analyst: Date Verified/Analyst: Purity Entered/Verified: 4/13/00,5/24/00 CSH 12/12/00 MMH 12/26/00 LAC Corrected PFOS LOQs (0.0119 & 0.0121 ug/g) to include std correction factors new LOQs are 0.0110 & 0.112 ug/g. LAC 02/19/01 Lot936 EtFOSE Purity Correction Factor Unknown Unknown Unknown Unknown NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown EtFOSE Cone. ng/g 2.44 0.00 46.5 30.3 0.00 0.00 0.00 0.00 39.2 0.00 0.00 0.00 0.00 0.00 892 816 805 347 650 EtFOSE Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 10 10 1 10 1 1 10 10 1 1 EtFOSE Calc. Cone, ng/g 2.44 0.00 0.00 0.00 45.4 29.5 0.00 0.00 0.00 0.00 38.8 0.00 0.00 0.00 0.00 0.00 0.00 0.00 883 0.00 807 786 0.00 0.00 339 636 Filename 90298002 90298003 90298110 90298111 90298019 90298020 90298021 90298022 90298023 90298027 90298028 90298029 90298030 90298031 90298036 90298038 90298042 90298045 90298046 Concentration o f EtFOSE ug/g nr / Ree. <LOQ (0.0298 ug/g) 0.00 <LOQ (0.0298 ug/g) 0.00 38% 25% <LOQ (0.0298 ug/g) <LOQ (0.0298 ug/g) <LOO (0.0298 ue/g) <LOQ (0.0298 ug/g) 0.0388 <LOQ (0.0298 ug/g) <LOQ (0.0298 ug/g) <LOQ (0.0298 ug/g) <LOQ (0.0298 ug/g) <LOQ (0.0298 ug/g) 0.00 0.00 0.883 0.00 0.807 0.786 0.00 0.00 0.339 0.636 ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ +4++ Mean EtFOSE ug/g <LOQ <LOQ 31% 0.0316 <LOQ 0.338 0.352 RSD Std. Dev. MS/MSD RPD NA NA 42% 12.7 0.00402 NA NA 137 0.463 102 0.359 ETS-8-7.0 Excel 97 ' 3MEnvironmental Laboratory Lvr Week 8 Rework TOX-001-liver212-10O.xls 5/31/2001 Page 254 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 LRN-U2103 Study: Product Number(Test Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Date o f Extraction/Analyst: Date o f Analysis/Analyst: Date o f Data Reduction/Analyst: Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Liver FACT-M-1.0 & FACT-M-2 0 reworked using ETS-8-7.0 Chick 080697 and Madeline 041098 Filename: See Attachments MassLynx 2.3 and 3 1 R-Squared Value: See Attachments 06/01/98 RWW/OK Slope: See Attachments 06/12/98,06/14/98,06/18/98,09/02/98 HOJ/KJH/LAC Y-Intercept: See Attachments 03/16/00, 11/29/00, 12/01/00, 12/10/00 IAS/MMH/KJH W EEKS RAT LIVER REWORK Group Sample # PFOS Concentration Mean Dose Calc. Cone, o f PFOS PFOS ng/g ug/g or */ Ree. ug/g Method Blk H 2 0 Blk-1 0.00 < LO Q (0.0U 0 ug/g) H 2 0 Blk-2 43.9 <LOQ (0.112 ug/g) <LOQ Matrix Blk Rabbit Liver Blk-1 0.00 <LOQ (0.0110 ug/g) Rabbit Liver Blk-2 30.4 <LOQ (0.112 ug/g) < LOQ QC - 100 ppb C90717M-MS C90717M-MSD -1584 -1773 -1331% -1490% -1410% Group 1 C90717M 2776 2.78 + Control C90718M 2004 2.00 + 0.0 mg/kg C90737M 2731 2.73 + C90756M C90769M 2002 1144 2.00 + 1.14 4- 2.13 C91126F 245 0.245 C91140F 346 0.346 C91145F 511 0.511 C91162F 1094 1.09 C91163F 552 0.552 0.549 Group 5 C90971M 1250280 1250 High Dose C90972M 1111564 1112 300 mg/kg C90988M 1249941 1250 C90996M 890777 891 C91017M 830679 831 1067 C91393F 873644 874 C91394F 945819 946 C91404F 1027570 1028 C91415F 1054710 1055 C91438F 1423345 1423 1065 PFOS = Perfluorooctanesulfonate PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol RSD Std. Dev. MS/MSD RPD NA NA 11% 31.3 0.668 59.8 0.328 18.5 197 20 0 213 PFOSA Concentration Mean Calc. Cone, ng/g o f PFOSA ug/g or % Ree. PFOSA ug/g 0.00 <LOQ (0.0119 ug/g) 66.3 0.0663 + 0.0391 0.00 <LOQ (0.0119 ug/g) 41.4 0.0414 + 0.0267 48.4 40% * 30.8 26% * 33% 32.4 0.0324 <LOQ (0.0302 ug/g) <LOQ (0.0302 ug/g) 33.7 0.0337 <LOQ (0.0302 ug/g) <LOQ (0.0302 ug/g) <LOQ (0.0302 ug/g) <LOQ (0.0302 ug/g) 0.0313 <LOQ (0.0302 ug/g) <LOQ (0.0302 ug/g) <LOQ (0.0302 ug/g) <LOQ (0.0302 ug/g) <LOQ (0.0302 ug/g) <LOQ (0.0302 ug/g) 34.4 0.0344 <LOQ (0.0302 ug/g) <LOQ (0.0302 ug/g) 0.0310 19353 19.4 + 18747 18.7 + 18897 18.9 + 20877 20.9 + 18323 18.3 + 19.2 14999 15.0 + 14071 14.1 + 17148 17.1 + 13844 17272 +13.8 + 17.3 15.5 * Data above the linear calibration range, estimated value. + C CV s (ailed, data entered as estimated **confirmcd low on 90298 ++ Qualitative data only. Date Entered/Analyst: Date Verified/Analyst: Purity Entered/Verified: 4/13/00, 5/24/00 CSH 12/12/00 MMH 12/28/00 hoj (list al22998a) 12/26/00 LAC Corrected PFOS LOQs (0.0119 & 0.0121 ug/g) to include std correction factors new LOQs are 0.0110 & 0 .112 ug/g. LAC 02/19/01 RSD Std. Dev. MS/MSD RPD NA NA 44% 5.21 0.00163 6.09 0.00189 5.13 0.99 10.7 1.65 PFOSAA Calc. Cone, ng/g 27.2 0.00 12.9 0.00 12.3 21.0 72.7 88.1 149 117 3.10 15.2 1.70 40.1 192 78.1 505667 581791 473002 473865 379557 298858 268201 369672 286207 429003 Concentration Mean of PFOSAA PFOSAA ug/g or % Ree. <LOQ (0.633 ug/g) ug/g <LOO (0.633 ug/g) <LOQ <LOQ (0.633 ug/g) <LOQ (0.633 ug/g) <LOQ 10% + 17% + 13% 0.0727 0.088 0.149 0.117 <LOQ (0.633 ug/g) 0.0980 <LOQ (0.633 ug/g) <LOQ (0.633 ug/g) <LOQ (0.633 ug/g) 0.192 0.0781 0.0920 506 + 582 + 473 + 474 + 380 + 483 299 + 268 + 370 + +286 + 429 330 RSD Std. Dev. MS/MSD RPD NA NA 52% 35.8 0.0351 61.1 0.0561 15.1 72.7 20.3 67.2 EtFOSE Calc. Cone, ng/g 2.44 0.00 0.00 0.00 45.4 29.5 0.00 0.00 0.00 0.00 38.8 0.00 0.00 0.00 0.00 0.00 0.00 0.00 883 0.00 807 786 0.00 0.00 339 636 Concentration o f EtFOSE ug/g or % Ree. <LOQ (0.0298 ug/g) 0.00 <LOQ (0.0298 ug/g) 0.00 38% 25% <LOQ (0.0298 ug/g) <LOQ (0.0298 ug/g) <LOQ (0.0298 ug/g) <LOQ (0.0298 ug/g) 0.0388 <LOQ (0.0298 ug/g) <LOQ (0.0298 ug/g) <LOQ (0.0298 ug/g) <LOQ (0.0298 ug/g) <LOQ (0.0298 ug/g) 0.00 0.00 0.883 0.00 0.807 0.786 0.00 0.00 0.339 0.636 ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ ++ + -t++ Mean EtFOSE ug/g <LOQ <LOO 31% 0.0316 <LOQ 0.338 0.352 RSD Std. Dev. MS/M SD RPD NA NA 42% 12.7 0.00402 NA NA 137 0.463 102 0.359 ETS-8-7.0 Excel 97 3MEnvironmental Laboratory ' Lvr Week 8 Rework TOX-001-liver212-100.xls ' 5/31/2001 Page 255 3M M edical D epartm ent Study: T6316.1 rt.Ul/1tt U7U7M Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product NumberfTest Substance): M ethod/R evision: Analytical Equipment System N um ber Instrument Software/Version: Date o f Extraction/Analyst: Date o f Analysis/Analyst: D ate o f D ata Reduction'A nalyst: Sample Data 104 W eek D ietary Carcinogenicity Study w ith N arrow Range (98 1%) N -Ethyl Perfluorooctanesulfonamido E thanol in Rats T-6316 (EtFOSE-OH) Rat Liver Filenam e: See List to Right FACT-M-1.0 & FACT-M-2.0 reworked using ETS-8-7.0 R-Squared Value: See Attachments Chick 080698, Amelia 062498, Madeline 041098, and Soup 020199 Slope: See Attachments M assL ynx 2.3 and 3.1 Y-Intercept: See Attachments 0 6 /0 2 /9 8 ,0 1 /1 4 /9 9 ,0 1 /1 7 /9 9 RW W/1AS/SAH 06/25/98, 06/26/98, 12/14/98, 01/18/99, 02/16/99, 02/18/99 HOJ/KJH/MEE/DRB 04/05/00, 11/30/00, 12/01/00, 12/05/00, 12'07/00, 0 1 /0 2 0 1 CSH /M M H /K JH PFOS PFOSA 1214/98 Lot 193 06/26/98 Lot L-2353 01/18/99 Lot 171 1 2 14/98 L ot L-2353 0 2 1 6 /9 9 Lot 171 0 2 1 8 /9 9 L ot Unknow n 0 2 1 8 /9 9 Lot 171 PFOSAA EtFOSE 06/26/98 Lot 617 06/25/98 Lot 936 1214/98 Lot 617 0218/99 Lot Unknown 0218/99 Lot Unknown WEEK 14 RAT LIVER REWORK Group Dose Sample # Initial Wt. S M ethod Blk Matrix Blk QC - lOOppb QC - 250 ppb QC - 750 ppb Group 1 Control 0.0 mg/kg Group 2 Low Dose 3.0 mg/kg Group 3 M id Dose 30.0 mg/kg Group 4 M id-High Dose 100 mg/kg H 2 0 Blk-I H 2 0 Blk-2 Rabbit L iver Blk-1 Rabbit Liver Blk-2 C90768M-MS C90768M-MSD C90780M-MS C90780M-MSD C91174F-M S C 91174F -M SD C90731M C90746M C90748M C90768M C90780M C91129F C91155F C9I160F C91174F C91181F C90797M C90807M C90818M C90831M C90836M C91I92F C91223F C91233F C91241F C91248F C90843M C90852M C90863M C90877M C90880M C91281F C91288F C91293F C91299F C91304F C90905M C90907M C90917M C90921M r90960M C91329F C91337F C91355F C91370F C91379F 1.0000 1.0000 1.0080 1.0080 1.0214 1.0214 1.0166 1.0166 1.0123 1.0123 1.0133 1.0226 1.0072 1.0214 1.0166 1.0264 1.0156 1 .0 1 0 3 1 .0 1 2 3 1.0251 1.0060 1 .0 2 5 8 1 .0 0 8 5 1.0231 1 .0 1 5 5 1 .0 0 4 7 1 .0 0 6 2 1 .0 2 5 7 1 .0 0 9 3 1.0031 1 .0 2 1 4 1 .0 1 0 5 1.0349 1.0019 1 .0 0 1 8 1.0201 1 .0 2 1 0 1.0016 1 .0 1 7 3 1 .0 2 7 7 1.0099 1.0123 1.0104 1.0378 1 074T 1.0016 1.0180 1.0081 1.0150 1.0090 Total Mass K NA NA 40.13 40 .1 3 NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOS Std Correction Factor 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 NA NA NA NA NA NA 0 .9 2 7 5 0.9275 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0.9275 . 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0.9275 0 .9 2 7 5 0.9275 0.9275 0 9' 75 0.9275 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 0 .9 2 7 5 PFOS = Perfluorooctanesulfonate PFOSA = Perfluorooctanesulfonam ide . PFOSAA = Perfluorooctanesulfonam idoacetate EtFOSE = N arrow Range N -Ethyl Perfluorooctanesulfonam ido ethyl alcohol Date Entered/Analyst: Date Verified/Analyst: Purity Entered/Verified: 5/24/00, 1207/00, 1214/00 CSH/KJH/LAC 1228/00 HOJ 1226/00 LAC PFOS Purity Correction Factor 0.8640 0.8640 0.8640 0.8640 NA NA NA NA NA NA 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 f) 8640 0.8640 0.8640 0.8640 0.8640 0.8640 PFOS Cone. ng/g 0.00 0.00 0.00 0.00 867 1023 88.9 98.3 140 151 348 425 504 383 286 133 155 175 76.6 97.0 230 231 247 210 266 214 235 289 195 256 26.3 72.0 26.1 96.2 33.9 87.2 85.8 70.9 148 54.1 523 686 469 407 4(75 328 377 313 823 273 PFOS Dilution Factor 1 1 1 1 1 1 10 10 10 10 4 4 4 4 4 4 4 4 4 4 125 125 125 125 125 125 125 125 125 125 2000 2000 2000 2000 2000 2000 2000 2000 2000 2000 1000 1000 1000 1000 inno 1000 lOOO 1000 1000 1000 Filename M011899013 S021899003 M011899014 S021899004 M121498109 M 1 2 14 9 8 1 1 0 M021699036 M021699037 S02189901S S021899016 M0U 899025 M011899026 M011899027 M011899028 M011899029 M011899032 M011899033 M011899034 M011899035 MOI 1899036 M011899039 M011899040 MOI 1899041 MOI 1899042 M11899043 MO11899046 MO11 899047 MO11899048 M 0II899O 49 M 0 II8 9 9 O 5 O MOI 1899053 M01I899054 M01I899055 M0I1899O56 M011899057 MOI 1899060 M01I899061 M01I899062 M01I899063 M011899064 M021699022 M021699023 M021699024 M021699025 M(V>1600076 M021699029 M021699030 M 0 2 1699 031 M021699032 M021699033 PFOS Calc. Cone. ng/g 0.00 0.00 0.00 0.00 -351 -199 -27.0 65.3 1136 1245 1100 1332 1603 1200 901 417 489 555 243 303 22950 22597 24494 20514 26220 21300 23437 28206 19334 25542 41221 114260 40451 153905 54251 137003 134654 113467 233295 84401 415193 543101 372033 314243 71*01 A 262314 296535 248810 649710 216709 Concentration or PFOS ug/g or % Ree. <LOO (0.0496 ue/e) <LOQ (0.0248 ue/e) <LOQ (0.0496 ug/g) <LOQ (0.0248 ug/g) -295% -167% -9% 22% 126% 138% 1.10 1.33 1.60 1.20 0.901 - 0.417 0.489 0.555 0.243 0.303 23.0 22.6 24.5 20.5 26.2 21.3 23.4 28.2 19.3 25.5 41.2 114 40.5 154 54.3 137 T 135 + 113 + 233 + 84.4 + 415 543 372 314 317 262 297 249 650 217 Mean PFOS g/g <LOQ <LOQ -231% 6% 132% 1.23 0 .4 0 2 23.4 23.6 80 8 141 392 335 + Bracketed bya CCV a t-30% difference, data may be biased low. LAC 0219/01 R eportd below th e L0Q . + f PFOSAA MS/M SD not fully bracketed. LA C 1214/00 4 * + EtFOSE MS/M SD reported, on ly a 4 point curve c ould be generated. L A C 1214/00 E = Sam ple went to dryness after the initial analysis. N o extract rem aining for analysis. ff Q ualitative data only, based on M S/M SD results. RSD Std Dev MS/MSD RPD NA NA 55% 481% 9% 21.4 0.262 32.1 0.129 9 .1 6 2 .1 4 14.8 3.48 63.0 5(7 9 39.8 56.0 24.0 94.1 53.3 178 Lot L-2353 or Unknown PFOSA Purity Correction Factor Unknown Unknown Unknown Unknown NA NA NA NA NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown I Inknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown PFOSA Cone. ng/g 0.00 NA 0.00 NA 102 90.3 NA NA NA NA 54.4 0.00 E 2 .7 4 36.5 6 .6 0 9 .7 5 29.9 2 .4 4 0.00 133 111 89.7 134 98.3 194 171 183 180 182 68.2 91.3 58.2 101 OR * 87.6 66.2 73.7 90.9 87.5 183 158 153 172 177 127 160 142 143 167 PFOSA Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 10 10 10 10 io 10 10 10 10 10 100 100 100 100 11717 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 PFOSA Calc. Cone, ng/g 0.00 NA 0.00 NA 97.3 85.8 NA NA NA NA 53.7 0.00 E 2 .6 8 35.9 6 .4 3 9.60 29.6 2.41 0.00 1319 1084 889 1305 968 1927 1697 1786 1781 1815 6672 9036 5626 10096 QRAft 8589 6480 7359 8935 8512 18099 15579 15150 16600 17258 12659 15721 14058 14066 16522 Filename Concentration of PFOSA ug/g or % Ree. M062698057 <LOQ (0.00604 ug/g) NA NA M062698058 <LOO (0.00604 ue/e) NA NA M121498109 81% M I21498110 71% NA NA NA NA NA NA M121498014 0.0537 M 121498015 <LO Q (0.0121 ug/g) M 121498016 M121498017 M121498021 M 121498022 M121498023 M 121498024 M 12I498025 M 12I498060 M121498061 M121498062 M12I498063 M121498064 M 121498068 M121498069 M 121498070 M 12149807I M 121498072 M 062698067 M062698068 M 062698069 M062698070 M 062698074 M062698075 M 062698076 M062698077 M062698078 M121498092 M 121498093 M 12I498094 M 121498095 M 214S8096 M121498100 M 21498101 M121498102 M 121498103 M 121498104 <LO Q (0.0121 ug/g) 0.0359 <LO Q (0.0121 ug/g) <LO Q (0.0121 ug/g) 0.0296 <LOQ (0.0121 ug/g) <LO Q (0.0121 ug/g) 1.32 1.08 0.889 1.31 0 .9 6 8 1.93 1.70 1.79 1.78 1.82 6 .6 7 9 .0 4 5 .6 3 10.1 OR4 8 .5 9 6.48 7 .3 6 8 .9 4 8.51 18.1 15.6 15.2 16.6 57.3 12.7 15.7 14.1 14.1 16.5 C orrected PF O S LO Qs (0.0619 & 0.0309 ug/g) to include std correction factors new LOQs are 0.0496 & 0.0248 ug/g. LAC 0219/01 Mean PFOSA <LOQ <LOQ 76% NA NA RSD Std Dev MS/MSD RPD NA NA 13% NA 0.0284 71.1 0 .0 2 0 2 0.0156 50.2 0.00784 17.5 1.11 0.194 4.61 1.80 0.0831 O 7.98 1.03 7.28 \r. i 7,", 10.4 14.6 1.52 3MEnvironmental Laboratory Page 256 3M M edical D epartm ent Study: T6316.1 nirii# wyia?/.i Covance# 6329-212 Analytical Report: FACT-TOX-001 L R N -U 2103 Study: Product NumbeifTest Substance): M a tr ix : M ethod/Revision: Analytical Equipment System N um ber Instrument Software/Version: Date o f Extraction/Analyst: Date o f Analysis/Analyst: Date o f Data Reduction/Analyst: Sample Data 104 W eek D ietary Carcinogenicity Study with N arrow Range (98.1/ ) N -Ethyl Perfluorooctanesulfonamido Ethanol in Rats T -6 3 16 (EtFO SE-O H ) Rat Liver Filename: FACT-M -1.0 & FACT-M-2.0 R-Squared V alue: Chick 080698, Amelia 062498, Madeline 041098, and Soup 020199 Slope: M assLynx 2.3 and 3.1 Y-Intercept: 5/11/98,6/2/98,01/14/99 RWW/IAS/SAH 6/5/98, 12/14/98, 01/18/99, 02/16/99, 02/18/99 HOJ/KJH/M EE/DRB 12/22/98, 01/20/99, 0 2 2 2 /9 9 , 3/23/00 H O J/K JIl'D RB /M M H See Attachments See Attachments See Attachments See Attachments WEEK 1 4 RAT LIVER_____________ Lot 617 o r Unknown G roup Dose Sam ple # PFOSAA Purity C orrection F a c to r M ethod Blk H 2 0 Blk-1 Unknown H 20 Blk-2 Unknown Matrix Blk R abbit L iv er Blk-1 Unknown Rabbit Liver Blk-2 Unknown QC - 100 ppb C90768M-MS NA C90768M-MSD NA QC - 250 ppb C90780M-MS NA C90780M-MSD NA QC - 750 ppb C91174F-M S NA C91174F-M SD NA C90731M Unknown Control 0.0 mg/kg C90746M C90748M Unknown Unknown C90768M Unknown C90780M Unknown C91129F Unknown C91155F Unknown C91160F Unknown C91174F Unknown C91181F Unknown G roup 2 C90797M Unknown Low Dose C90807M Unknown 3.0 m e/ke C90818M Unknown C90831M Unknown C90836M Unknown C91192F Unknown C91223F Unknown C91233F Unknown C91241F Unknown C91248F Unknown G roup 3 C90843M Unknown M id Dose C90852M Unknown 30.0 mg/kg C90863M Unknown C90877M Unknown C90880M Unknown Unknown C91288F Unknown C91293F Unknown C91299F Unknown C91304F Unknown G roup 4 C90905M Unknown M id-High Dose C90907M Unknown 100 m e/ke C90917M Unknown C90921M Unknown C90960M TInknown C91329F Unknown C91337F Unknown C91355F Unknown C91370F Unknown C91379F Unknown PFOSAA Cone. ng/g 0.00 NA 0.00 NA 115 153 NA NA 905 1315 174 143 E 211 29.0 76.4 94.9 69.1 232 21.8 238 145 180 203 175 218 326 262 232 303 7.58 202 116 358 326 53.8 140 128 302 134 953 749 619 1209 612 404 800 641 510 640 PFOS = Perfluorooctanesulfonate PFOSA = Perfluorooctanesulfonam ide . PFOSAA = Perfluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Pcrfluorooctanesulfonam ido ethyl alcohol Date Entered/Analyst: Date Verified/Analyst: Purity Entered/Verified; 5/24/00, 1207/00, 1214/00 CSH/KJH/LAC 1228/00 HOJ 1226/00 LAC PFOSAA D ilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 10 10 10 10 10 10 10 10 10 10 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 Filenam e M121498003 NA M I21498004 PFOSAA Calc. Cone, ng/g 0.00 NA 0.00 C o n c en tra tio n of PFO SA A ug/g o r % R ee. <LOQ (0.0633 ug/g) NA <LOQ (0.0633 ug/g) PFOSAA g/g <LOQ RSD S td Dev M S/M SD RPD NA NA NA NA <LOQ NA M121498109 M 121498110 NA NA S021899017 -93.9 -56.6 NA NA 665 -74% -45% NA NA 74% ++ ++ -59% NA 50% NA S021899018 1070 119% 97% 47% M 121498014 M121498015 172 140 0.172 0.140 E M 121498016 M121498017 M121498021 M I21498022 EE 206 0.206 28.5 <LO 0 (0.0633 ue/b) 74.5 0.0745 93.4 0.0934 0.145 42.0 0 .0 6 1 1 M121498023 68.4 0.0684 M12I498024 M121498025 229 0.229 21.3 <LOQ (0.0633 ug/g) 0.106 66.1 0.0699 M 121498060 2363 2 .3 6 M121498061 1414 1.41 M 121498062 M121498063 M 121498064 M 121498068 M 121498069 M 121498070 M121498071 M 121498072 M062698067 1786 1984 1719 2168 3240 2556 2295 3023 742 1.79 1.98 1.72 2.17 3.24 2 .5 6 2 .2 9 3.02 0.742 1.85 2 .6 6 * 18.9 0.351 17.4 0.462 M062698068 20013 20.0 M 062698069 M062698070 M062698071 M062698074 M062698075 M 062698076 M062698077 M062698078 11226 35706 32557 5269 13748 12775 29678 13073 11.2 35.7 32.6 20.0 5.27 * 13.7 12.8 29.7 13.1 14.9 72.8 14 6 60.0 8 .9 5 M 121498092 M 121498093 M121498094 M 121498095 Ml 21498096 M121498100 M121498101 M121498102 M121498103 M 12I498104 94336 73968 61232 116449 59712 40356 78625 63619 50197 63386 94.3 74.0 61.2 116.4 59 7 40.4 78.6 63.6 50.2 63.4 29.7 1.1 24.1 24.6 59.2 14.6 N ote: PFO S data m ay be biased high b a sed on the M S /M SD recoveries. + B racketed by a CCV a t -30% difference, data m ay be b iased low. L A C 0 2 1 9 /0 1 * Reportd below the LOQ <-+ PFOSAA M S/M SD not fully bracketed. LAC 1 2 14/00 ++* EtFO SE M S/M SD reported, only a 4 point curve c ould be generated. LAC 1 2 1 4 /0 0 E = Sam ple went to dryness after the initial analysis. N o extract rem aining for analysis. # Qualitative d ata only, based on M S/M SD results. Lot 936 or Unknown EtFOSE Purity C o rrectio n Factor Unknown Unknown Unknown Unknown NA NA NA NA NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown I Inknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown E tF O S E Cone. ng/g 0.00 NA 0.00 NA NA NA NA NA 516 480 0.00 0.00 0.00 0.00 0.00 0 .0 0 0.00 0 .0 0 0 .0 0 0 .0 0 NA NA NA NA NA NA NA NA NA NA 234 177 325 146 168 152 142 171 117 170 NA NA NA NA NA NA NA NA NA NA C orrected PFO S LO Q s (0.0619 & 0.0309 ug/g) to include std correction factors n ew L O Q s a re `0.0496 & 0.0248 ug/g. LAC 0219/01 E tF O S E D ilution Factor 1 1 1 1 1 1 1 1 10 10 1 1 1 1 l I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 F ilenam e A062598002 NA A062598003 NA NA NA NA NA S021899015 S021899016 A062598034 A062598035 A062598036 A062598037 A062598038 A062598041 A062598042 A062598043 A062598044 A062598045 NA NA NA NA NA NA NA NA NA NA A062598076 A062598077 A062598078 A062598079 Af)fi7S9808n A062598083 A062598084 A062598085 A062598086 A062598087 NA NA NA NA NA NA NA NA NA NA E tF O S E Calc. Cone, ng/g 0.00 NA 0.00 NA NA NA NA NA 5102 4739 0.00 0.00 0.00 0.00 0.00 0.00 0 .0 0 0.00 0.00 0.00 NA NA NA NA NA NA NA NA NA NA 229 175 314 146 167 149 139 171 115 165 NA NA NA NA NA NA NA NA NA NA C o ncentration o r EtFOSE ug/g o r % Ree. <LOQ (0.0596 ug/g) NA <LOO (0.0596 ue/el NA NA NA NA NA 567% 527% +++ +++ <LOO (0.0596 ue/el <LOO (0.0596 ue/el <LOO (0.0596 ue/el <LOO (0.0596 ue/el <LOQ (0.0596 ue/ b) <LOO (0.0596 ue/ b1 <LOO (0.0596 ub/e) <LOO (0.0596 ue/ bI ff <LOO (0.0596 ue/ b) <LOQ (0.0596 ug/g) # NA # NA NA NA NA NA NA NA NA 0.229 0 .1 7 5 0 .3 1 4 0.146 n 167 0.149 0.139 0.171 0 .1 1 5 0.165 NA NA NA NA NA NA NA NA NA # # ft tt # n # * it # # # # # `# # E tF O S E <LOQ <LOO NA NA 547% <LOQ <LOQ NA NA nw 0 .1 4 8 NA NA RSD S td Dev M S/M SD RPD NA NA NA NA 7% NA NA NA NA NA NA 0.0224 NA 3MEnvironmental Laboratory Page 257 3M M edical D epartm ent Study: T6316.1 Caomvadncte##069322599-72.1i2 Analytical Report: FACT-TOX-001 . LRN-U2103 Study: Product Number(Test Substance): M a tr ix : M ethod/Revision: Analytical Equipment System Number: Instrument Software/Version: Date o f Extraction/Analyst: Date o f A nalysisAnalyst: Date o f Data Reduction/Analyst: Sample Data 104 W eek D ietary Carcinogenicity Study w ith N arrow Range (98.1% ) N -Ethyl Perfluorooctanesulfonamido E thanol in Rats T -6 3 16 (EtFOSE-OH) Rat Liver Filename: See List to Right FA C T-M -1.0 & FA CT-M -2 0 rew orked using ETS-8-7.0 R-Squared Value: SeeA ttachm ents Chick 080698, Amelia 062498, M adeline 041098, and Soup 020199 Slope: SeeA ttachm ents M assL ynx 2.3 and 3.1 Y-lnterwpt: SeeA ttachm ents 06/02/98,01/14/99,01/17/99 RWW/IAS/SAH 06/25/98, 06/26/98, 12/14/98, 01/18/99, 0 2 /1 6 /9 9 ,0 2 /1 8 /9 9 HOJ/K JI1/MEE/DRB 04/05/00, 11/30/00, 12/01/00, 12/05/00, 12/07/00,01/02/01 CSH /M M H /K JH WEEK 14 RAT LIVER REWORK Group Dose Sample H PFOS Calc. Cone. Dg/g M ethod Blk H 2 0 Blk-1 0.00 H 2 0 Blk-2 0.00 Matrix Blk Rabbit L iv er Blk-1 0.00 Rabbit Liver Blk-2 0.00 Q C - lOOppb C90768M-MS -351 C90768M-MSD -199 QC - 250 ppb C90780M -M S -27 C90780M-MSD 65 QC - 750 ppb C 91I74F-M S 1136 C91174F-M SD 1245 Group 1 C90731M 1100 Control C90746M 1332 0.0 mg/kg C90748M 1603 C90768M 1200 C90780M 901 C91129F 417 C91155F 489 C91160F 555 C9I174F 243 C91181F 303 Group 2 C90797M 22950 Low Dose C90807M 22597 3.0 m g/kg C90818M 24494 C 9083IM 20514 C90836M 26220 C91192F C91223F 21300 23437 C91233F 28206 C91241F 19334 C91248F 25542 Group 3 C90843M 41221 M id Dose 30.0 mg/kg C90852M C90863M 114260 40451 C90877M 153905 C90880M 54251 C91281F C91288F 137003 134654 C91293F 113467 C91299F 233295 C91304F 84401 Group 4 M id-High Dose C90905M C90907M 415193 543101 100 mg/kg C90917M C90921M C90960M C91329F C91337F 372033 314243 316914 262314 296535 C91355F C91370F 248810 649710 C91379F 216709 Concentration of PFOS ug/g or % Ree. <LOQ (0.0496 Ug/g) <LOQ (0.0248 ug/g) <LOQ (0.0496 ug/g) <LOQ (0.0248 ug/g) -295% -167% -9% 22% 126% 138% 1.10 1.33 1.60 1.20 0.90 0.417 0.489 0.555 0.243 0.303 23.0 22.6 24.5 20.5 26.2 21.3 23.4 28.2 19.3 25.5 41.2 114 40.5 * 154 54 * 132 135 + 113 + 233 + 84 + 415 543 372 314 317 262 297 249 650 217 Mean PFOS Ug/g <LOQ <LOQ -231% 6% 132% 1.23 0.402 23.4 23.6 80.8 141 392 335 PFOS = PerOuorooctanesulfonate PFOSA = Perfluorooctanesulfonam ide PFOSAA Perfluorooctanesulfonam idoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol . Date Entered/Analyst: Date Verified/Analyst: Purity Entered/Verified: 5/24/00, 12/07/00, 12/14/00 CSH /K JH /LAC 12/28/00 HOJ 12/26/00 LAC RSD Std Dev MS/MSD RPD NA NA 55% 481% 9% 21.4 0.262 32.1 0.129 9.16 2.14 14.8 3.48 63.0 50.9 39.8 56.0 24.0 94.1 53.3 178 PFOSA Calc. Cone, ng/g 0.00 NA 0.00 NA 97.3 85.8 Concentration of PFOSA ug/g or % Ree. <LO O (0.00604 ug/g) NA <LOQ (0.00604 ug/g) NA 81% 71% Mean PFOSA ur/r <LOO <LOQ 76% RSD Std Dev MS/MSD RPD NA NA 13% NA NA NA NA NA NA NA NA NA NA NA NA 53.7 0.0537 0.00 <LOQ (0.0121 ug/g) EE 2.68 <LOQ (0.0121 ug/g) 71.1 35.9 0.0359 0.0284 0.0202 6.43 <LOQ (0.0121 ug/g) 9.60 <LOQ (0.0121 ug/g) 29.6 0.0296 2.41 <LO Q (0.0121 ug/g) 50.2 0.00 <LO Q (0.0121 ug/g) 0.0156 0.00784 1319 1.32 1084 1.08 889 0.889 1305 1 31 17.5 968 0 968 1.11 0.194 1927 1.93 1697 1.70 1786 1.79 1781 1.78 461 1815 1.82 1.80 0.0831 6672 6.67 9036 9.04 5626 5.63 10096 10.1 24.2 9840 9.84 8.25 2.00 8589 8 59 6480 6.48 7359 7.36 8935 8.94 12.9 8512 8.51 7.98 1.03 18099 18.1 15579 15.6 15150 15.2 16600 17258 16.6 17.3 7.28 16.5 t 7f1 12659 12.7 15721 15.7 14058 14.1 14066 14 1 10.4 16522 16.5 14.6 1.52 Note: PFOS data m a y be biased hig h based on the M S/M SD recoveries. + Bracketed by a C C V at -30% difference, data m ay be biased low. LAC 02/19/01 * Reportd below the LOQ ++ PFOSAA M S/M SD not fully bracketed. LAC 12/14/00 +++ EtFOSE M S/M SD reported, o nly a 4 point curve could be generated. LA C 12/14/00 E = Sample w ent to dryness after the initial analysis. N o extract rem aining for analysis. tt Qualitative data only, based on M S /M SD results. C orrected PFO S LO Qs (0.0619 & 0.0309 ug/g) to include std correction factors new LO Qs are 0.0496 & 0.0248 ug/'g. LAC 02/19/01 ' PFOSAA Calc. Cone, ng/g 0.00 NA 0.00 NA -94 -57 NA NA 665 1070 172 140 E 206 28.5 74.5 93.4 68.4 229 21.3 2363 1414 1786 1984 1719 2168 3240 2556 2295 3023 742 20013 11226 35706 32557 5269 13748 12775 29678 13073 94336 73968 61232 116449 <07n 40356 78625 63619 50197 63386 Concentration of PFOSAA ug/g or % Ree. <LOO (0.0633 ug/g) NA <LOQ (0.0633 ug/g) NA -74% ++ -45% ++ NA NA 74% 119% 0.172 0.140 E 0.206 <LOQ (0.0633 ug/g) 0.0745 0.0934 0.0684 0.229 <LOQ (0.0633 ug/g) 2.36 1.41 1.79 1.98 1.72 2.17 3 .2 4 2.56 2.29 3 .0 2 0.742 * 20.0 11.2 35.7 32.6 5.27 * 13.7 12.8 29.7 13.1 94.3 74.0 61.2 116 59.7 40.4 78.6 63.6 50.2 63.4 Mean PFOSAA ttR/R <LOQ <LOQ -59% NA 97% 0.145 0.106 1.85 2 .6 6 m o 14.9 S. 59.2 RSD Std Dev MS/MSD RPD NA NA 50% NA 47% 42.0 0.0611 66.1 0 .0 6 9 9 18.9 0.351 17.4 0 .4 6 2 72.8 li X 60.0 8.95 29.7 24.! 24.6 14.6 EtFOSE Calc. Cone, ng/g 0.00 NA 0.00 NA NA NA NA NA 5102 4739 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 NA NA NA NA NA NA NA NA NA NA 229 175 314 146 !67 149 139 171 l\5 165 NA NA NA NA NA NA NA NA NA NA Concentration of EtFOSE ug/g or % Ree. <LOO (0.0596 ug/g) ft NA ft <LOQ (0.0596 ug/g) ft NA ft NA ft N A ft NA NA 567% 527% ft ft +++ +++ <LOQ (0.0596 ug/g) ft <LOQ (0.0596 ug/g) ft <LOQ (0.0596 ug/g) ft <LOQ (0.0596 ug/g) ft <LOQ (0.0596 ug/g) ft <LOQ (0.0596 ug/g) ft <LOQ (0.0596 ug/g) ft <LOO (0.0596 ug/g) <LOO (0.0596 ug/g) it <LOQ (0.0596 ug/g) ft NA ft NA ft NA ft N A ' ft NA ft NA tt N A ft NA ft NA tt NA ft 0.229 0 .1 7 5 tt ft 0.314 tt 0.146 ft 0.167 If 0.149 ft 0.139 ft 0.171 tt 0.115 ft 0 .1 6 5 ft NA ft NA ft NA ft NA tt NA tf NA ft NA ft NA tt NA tt NA tt Mean EtFOSE ur/r <LOQ <LOQ NA NA 547% <LOQ <LOQ NA NA 0.206 0.148 NA NA RSD Std Dev MS/MSD RPD NA NA NA NA 7% NA NA NA NA NA NA NA NA 32.8 0.0677 15.1 0.0224 NA NA ' NA NA 3MEnvironmental Laboratory Page 258 3M M edical D epartm ent Study: T6316.1 A M U I ff u y zsy /.l C ovance# 6329-212 Study: Product Number(Test Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Date of Extraction/Analyst: Date of Analysis/Analyst: Date of Data Reduction/Analyst: Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Liver ETS-8-6.0 & ETS-8-7.0 Filename: See Below Davey 070799 R-Squared Value: See Attachments MassLynx 3.3, 3.4 Slope: See Attachments 2/29/00 SAL Y-Intercept: See Attachments 05/08/00, 05/24/00, 08/21/00, 08/23/00 IAS/HOJ/MMH 05/09/00, 05/25/00, 08/22/00, 08/28/00 IAS/MMH/HOJ Analytical Report: FACT-TOX-001 L R N -U 2103 WEEK 53 RAT LIVER Group Dose Sample # Initial Wt. g Method Blk Matrix Blk QC - 250 ppb Group 1 Control 0.0 mg/kg Group 1 Control 0.0 mg/kg RBL02290-H20 Blk-5 RBL02290-H20 BIk-6 RBL02290-Liver BIk-5 RBL02290-Liver BIk-6 C90714M-250 ppb-MS-5-1 C90714M-250 ppb-MS-5-2 C90714M C90751M C90752M C90754M C90767M C91121F C91122F C91124F C91133F C91152F 1.0000 1.0000 1.0000 1.0000 1.0093 1.0093 1.0093 1.0033 0.9994 0.9912 0.9845 0.9972 1.0073 1.0079 0.9918 1.0162 Group 4 Low Dose 3.0 mg/kg Group 4 Low Dose 3.0 mg/kg C90902M C90918M C90950M C90951M C90957M C91323F C91347F C91352F C91367F C91371F 0.9925 1.0022 0.9878 1.0037 0.9880 0.9939 0.9917 0.9983 0.9908 0.9903 FFOS - rcifiuuiuucuuicsulfuuaie PFOSA = Perfluorooctanesulfonamide PFOSAA Perfluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2C00) PFOSEA = Perfuorooctane sulfonyl ethylamide Date Entered/Analyst: 05/15/00, 06/12/00, 09/03/00 CSH/LAC Date Verified/Analyst: 06/05/00. 06/06/00 CSH: 02/26/01 hoj Purity Entered/Verified: 02/16/01 LAC Conected PFOS LOQ (0.0613 ug/g) to include std correction factors new LOQ is 0.0491 ug/g. LAC 02/19/01 Lot 171 Total Mass PFOS Std PFOS Purity Surrogate PFOS PFOS PFOS Filename of Liver Correction Correction Verified Cone. Dilution Calc. Cone. g Factor Factor NA 0.9275 0.8640 ng/g Factor ng/g NA 2.15 1 1.72 A082100016 NA 0.9275 0.8640 NA 0.00 1 0.00 A082100017 40.13 0.9275 0.8640 NA 0.00 1 0.00 A082100018 40.13 0.9275 0.8640 NA 3.16 1 2.53 A082100019 NA NA NA Confirmed low 1239 1 528 D050800019 NA NA NA Confirmed low 1006 1 298 D050800020 NA 0.9275. 0.8640 NA 706 1 560 D050800023 NA 0.9275 0.8640 NA 473 1 378 D050800024 NA 0.9275 0.8640 NA 993 1 796 D050800025 NA 0.9275 0.8640 NA 857 1 693 D050800026 NA 0.9275 0.8640 NA 526 1 428 D050800027 NA 0.9275 0.8640 NA 374 1 301 D050800030 NA 0.9275 0.8640 NA 383 1 305 D050800031 NA 0.9275 0.8640 NA 539 1 429 D050800032 NA 0.9275 0.8640 NA 0.9275 0.8640 NA 668 1 NA 474 1 540 D050800033 374 D050800034 NA 0.9275 0.8640 NA 739 1000 596825 D050800037 NA 0.9275 0.8640 NA 548 1000 437941 D050800038 NA 0.9275 0.8640 NA 0.9275 ft 8640 NA 1138 1000 923568 D050800039 NA 875 1000 AQR^m 00^0800040 NA 0.9275 0.8640 NA 1008 1000 817501 D050800041 NA 0.9275 0.8640 NA 820 1000 661438 D050800044 NA 0.9275 0.8640 NA 0.9275 0.8640 NA 1065 1000 860688 D050800045 NA 959 1000 770046 D050800046 NA 0.9275 0.8640 NA 0.9275 0.8640 NA 776 1000 627330 D050800047 NA 678 1000 548628 D050800048 * High recovery was confirmed on 8/21/00, data was not entered because it was outside the calibration range. 4/20/01 mmh Concentration Mean of PFOS ug/g or % Ree. <LOQ (0.00491 ug/g) PFOS ug/g <LOQ (0.00491 ug/g) <LOQ <LOQ (0.00491 ug/g) <LOQ (0.00491 ug/g) <LOQ 177% * 100% 138% 0.560 0.378 0.796 0.693 0.428 0.571 0.301 0.305 0.429 0.540 0.374 0.390 597 438 924 699 818 695 661 861 770 627 549 694 . RSD Std Dev MS/MSD RPD NA NA NA NA 56% 30.7 0.175 25.5 0.0993 I"? *1 189 17.7 123 ETS-8-7.0 3M E nvironm ental Laboratory I vr W e p lf c l i i/inni Page 259 3M M edical D epartm ent Study: T6316.1 AJVlJUlff U VZ3y /.l Covance# 6329-212 Study: Product Number(Test Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Date of Extraction/Analyst: Date of Analysis/Analyst: Date of Data Reduction/Analyst: Sample Data 104 W eek Dietary Carcinogenicity Study with N arrow Range (98.1% ) N -Ethyl Perfluorooctanesulfonam ido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Liver ETS-8-6.0 & ETS-8-7.0 Filename: See Below Davey 070799 R-Squared Value: See Attachments MassLynx 3.3, 3.4 Slope: See Attachments 2/29/00 SAL 05/08/00,05/24/00, 08/21/00, 08/23/00IAS/HOJ/MMH Y-Intercept: See Attachments 05/09/00, 05/25/00, 08/22/00, 08/28/00 IAS/MMH/HOJ Analytical Report: FACT-TOX-001 . LRN-U2103 WEEK 53 RAT LIVER Group Dose Sample # Method Blk Matrix Blk QC - 250 ppb Group 1 Control 0.0 mg/kg Group 1 Control 0.0 mg/kg Group 4 Low Dose 3.0 mg/kg Group 4 Low Dose 3.0 mg/kg RBL02290-H20 BIk-5 RBL02290-H20 Blk-6 RBL02290-Liver Blk-5 RBL02290-Liver BIk-6 C90714M-250 ppb-MS-5-1 C90714M-250 ppb-MS-5-2 C90714M C90751M C90752M C90754M C90767M C91121F C91122F C91124F C91133F C91152F C90902M C90918M C90950M C90951M C90957M C91323F C91347F C91352F C91367F C91371F Lot L-15709 PFOSA Purity Correction Factor Unknown Unknown Unknown Unknown NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2C00) . PFOSEA = Perfuorooctane sulfonyl ethylamide Date Entered/Analyst: 05/15/00, 06/12/00, 09/03/00 CSH/LAC Date Verified/Analyst: 06/05/00. 06/06/00 CSH: 02/26/01 hoj Purity Entered/Verified: 02/16/01 LAC Corrected PFOS LOQ (0.0613 ug/g) to include std correction factors new LOQ is 0.0491 ug/g. LAC 02/19/01 Surrogate Verified NA NA NA NA Confirmed Low Confirmed Low NA NA NA NA NA NA NA NA NA NA NA NA NA NA 2nd Analysis OK NA 2nd Analysis OK Confirmed High High, Not Confirmed High, Not Confirmed PFOSA Cone. ng/g 0.00 0.00 2.58 0.00 233 288 0.710 35.5 11.7 18.1 19.3 12.5 5.41 25.5 15.8 9.87 296 196 289 716 404 236 216 219 264 3 19 PFOSA Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 100 100 100 mo 100 100 100 100 100 100 PFOSA Calc. Cone. ng/g 0.00 0.00 2.58 0.00 230 285 0.703 35.4 11.7 18.3 19.6 12.5 5.37 25.3 15.9 9.71 29822 19579 29280 714R1 40923 23731 21786 21911 26678 32243 Filename D050800004 D050800017 D050800005 D0508000I8 D050800019 D050800020 A082100024 A082100025 A082100026 A082100027 A082100028 A082100031 A082100032 A082100033 A082100034 A082100035 D052400040 D052400041 D052400042 nns'Mnnru'; D052400047 D052400048 D052400049 D052400050 A082300016 A082300017 Concentration of PFOSA ug/g or % Ree. <LOQ (0.0123 ug/g) <LOQ (0.0123 ug/g) <LOQ (0.0123 ug/g) <LOQ (0.0123 ug/g) 77% 95% <LOO (0.00614 ue/e) 0.0354 0.0117 0.0183 0.0196 0.0125 <LOQ (0.00614 ug/g) 0.0253 0.0159 0.00971 29.8 19.6 29.3 -n <; 40.9 23.7 21.8 21.9 26.7 32.2 Mean PFOSA Ug/g <LOQ <LOQ 86% 0.0182 0.0139 28.2 25.3 RSD Std Dev MS/MSD RPD NA NA NA NA 21% 55.1 0.0100 48.7 0.00677 -n n 8.44 17.3 4.37 ETS-8-7.0 3MEnvironmental Laboratory I v r W*ek ^3 Page 260 3M M edical D epartm ent Study: T6316.1 A M J J 'l f IW2 5 9 7 .1 Covance# 6329-212 Study: Product Number(Test Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Date of Extraction/Analyst: Date of Analysis/Analyst: Date of Data Reduction/Analyst: Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Liver ETS-8-6.0 & ETS-8-7.0 Filename: See Below Davey 070799 R-Squared Value: See Attachments MassLynx 3.3, 3.4 Slope: See Attachments 2/29/00 SAL Y-Intercept: See Attachments 05/08/00, 05/24/00, 08/21/00,08/23/00 1AS/HOJ/MMH 05/09/00, 05/25/00, 08/22/00,08/28/00 IAS/MMH/HOJ Analytical Report: FACT-TOX-001 LRN-U2103 WEEK 53 RAT LIVER LotT-7121.1 Group Sample # PFOSAA Purity Dose Correction Factor Method Blk RBL02290-H20 Blk-5 Unknown Matrix Blk RBL02290-H20 Blk-6 RBL02290-Liver BIk-5 Unknown Unknown RBL02290-Liver Blk-6 Unknown QC - 250 ppb C90714M-250 ppb-MS-5-1 C90714M-250 ppb-MS-5-2 NA NA Group 1 C90714M Unknown Control C90751M Unknown 0.0 mg/kg C90752M Unknown C90754M C90767M Unknown Unknown Group 1 C91121F Unknown Control C91122F Unknown 0.0 mg/kg C91124F C91133F C91152F Unknown Unknown Unknown Group 4 C90902M Unknown Low Dose C90918M Unknown 3.0 mg/kg C90950M C9095IM Unknown Unknown C90957M Unknown Group 4 C91323F Unknown Low Dose C91347F Unknown 3.0 mg/kg C91352F Unknown C91367F Unknown C91371F Unknown pFOS ~ Perfluorooctanesulfonate PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol MS56 = C8F 17S02N((H)CH2COO) PFOSEA = Perfuorooctane sulfonyl ethylamide Date Entered/Analyst: 05/15/00, 06/12/00, 09/03/00 CSH/LAC Date Verified/Analyst: 06/05/00. 06/06/00 CSH: 02/26/01 hoj Purity Entered/Verified: 02/16/01 LAC Corrected PFOS LOQ (0.0613 ug/g) to include std correction factors new LOQ is 0.0491 ug/g. LAC 02/19/01 Surrogate Verified NA NA NA NA Confirmed Low Confirmed Low NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOSAA Cone. ng/g 0.00 0.00 0.00 0.00 339 370 8.54 48.7 8.27 44.0 4.96 8.95 4.04 61.6 25.5 16.0 803 402 677 286 600 491 409 451 457 558 PFOSAA Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 100 100 100 100 100 100 100 100 100 100 PFOSAA Calc. Cone. ng/g 0.00 0.00 0.00 0.00 327 359 8.46 48.6 8.27 44.4 5.04 8.98 4.01 61.1 25.7 15.7 80884 40068 68551 2847<; 60700 49362 41192 45161 46121 56329 Filename D050800004 D050800017 D050800005 D050800018 D050800019 D050800020 D050800023 D050800024 D050800025 D050800026 D050800027 D050800030 D050800031 D050800032 D050800033 D050800034 D050800051 D050800052 D050800053 nofngfWKa D050800055 D050800058 D050800059 D050800060 D050800061 D050800062 Concentration of PFOSAA ug/g or % Rec. <LOQ (0.0307 ue/a) <LOQ (0.0307 ug/g) <LOQ (0.0307 ug/g) <LOQ (0.0307 ug/g) 109% 120% <LOQ (0.0307 ug/g) 0.0486 <LOQ (0.0307 ug/g) 0.0444 <LOQ (0.0307 ug/g) <LOQ (0.0307 ug/g) <LOO (0.0307 ue/a) <LOQ (0.0307 ug/g) <LOQ (0.0307 ue/a) <LOQ (0.0307 ug/g) 80.9 40.1 68.6 o < 60.7 49.4 41.2 45.2 46.1 56.3 Mean PFOSAA " g/g <LOQ <LOQ 114% <LOQ <LOQ 55.7 47.6 RSD Std Dev MS/MSD RPD NA NA NA NA 9% NA NA NA NA 38.2 21.3 11.9 5.67 ETS-8-7.0 3MEnvironmental Laboratory Lvr Week 53 5 /3 1/2001 Page 261 3M M edical D epartm ent Study: T6316.1 A M D Iff U9Z597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 . LRN-U2103 Study: Product Num ber(Test Substance): M atrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Date of Extraction/Analyst: Date of Analysis/Analyst: Date of Data Reduction/Analyst: Sample Data 104 W eek Dietary C arcinogenicity Study w ith N arro w R ange (98.1% ) N -E thyl Perfluorooctanesulfonam ido E thanol in Rats T -6 316(E tF O S E -O H ) Rat Liver ETS-8-6.0& ETS-8-7.0 Filename: See Below Davey 070799 R-Squared Value: See Attachments MassLynx 3.3,3.4 Slope: See Attachments 2/29/00 SAL Y-Intercept: See Attachments 05/08/00, 05/24/00, 08/21/00, 08/23/00IAS/HOJ/MMH 05/09/00, 05/25/00, 08/22/00, 08/28/00 IAS/MMH/HOJ WEEK 53 RAT LIVER lot Unknown Group Dose Sample # EtFOSE Purity Correction Factor Method Blk Matrix Blk RBL02290-H20 Blk-5 RBL02290-H20 Blk-6 RBL02290-Liver Blk-5 Unknown Unknown Unknown QC - 250 ppb RBL02290-Liver Blk-6 C90714M-250 ppb-MS-5-1 C90714M-250 ppb-MS-5-2 Unknown NA NA Group 1 Control 0.0 mg/kg . Group 1 Control 0.0 mg/kg C90714M C90751M C90752M C90754M C90767M C91121F C91122F C91124F C91133F C91152F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Group 4 Low Dose 3.0 mg/kg Group 4 Low Dose 3.0 mg/kg C90902M C90918M C90950M C90951M C90957M C91323F C91347F C91352F C91367F C91371F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown PFOS = Periluorcoctanesulfonate PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2COO) PFOSEA = Perfuorooctane sulfonyl ethylamide Date Entered/Analyst: Date Verified/Analyst: 05/15/00, 06/12/00, 09/03/00 CSH/LAC 06/05/00. 06/06/00 CSH: 02/26/01 hoj Purity Entered/Verified: 02/16/01 LAC Corrected PFOS LOQ (0.0613 ug/g) to include std correction factors new LOQ is 0.0491 ug/g. LAC 02/19/01 Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA ' NA NA NA EtFOSE Cone. ng/g NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR EtFOSE Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 EtFOSE Calc. Cone. ng/g NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR Filename NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA. NA NA NA NA NA NA Concentration of EtFOSE ug/g or Vo Rec. NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR. NR NR NR NR NR NR Mean EtFOSE ug/g NR NR NR NR NR NR NR RSD Std Dev MS/MSD RPD NA NA NA NA NA NA NA NA NA NA NA NA NA ETS-8-7.0 3MEnvironmental Laboratory Lvr W eek 53 5/31/2001 Page 262 3M M edical D epartm ent Study: T6316.1 Aiviu i w v y s y /.i C ovance# 6329-212 Study: Product Number(Test Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Date of Extraction/Analyst: Date of Analysis/Analyst: Date of Data Reduction/Analyst: Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Liver ETS-8-6.0 & ETS-8-7.0 Filename: See Below Davey 070799 R-Squared VaSee Attachments MassLynx 3.3, 3.4 Slope: See Attachments 2/29/00 SAL Y-Intercept: See Attachments 05/08/00, 05/24/00,08/21/00, 08/23/00 IAS/HOJ/MMH 05/09/00,05/25/00,08/22/00, 08/28/00IAS/MMH/HOJ Analytical Report: FACT-TOX-001 L R N -U 2103 WEEK S3 RAT LIVER Group Dose Sample # Method Blk Matrix Blk QC - 250 ppb Group 1 Control 0.0 mg/kg Group 1 Control 0.0 mg/kg Group 4 Low Dose 3.0 mg/kg Group 4 Low Dose 3.0 mg/kg RBL02290-H20 Blk-5 RBL02290-H20 Blk-6 RBL02290-Liver Blk-5 RBL02290-Liver Blk-6 C90714M-250 ppb-MS-5-1 C907I4M-250 ppb-MS-5-2 C90714M C90751M C90752M C90754M C90767M C9I121F C91122F C91124F C91133F C91152F C90902M C90918M C90950M C90951M C90957M C91323F C91347F C91352F C91367F C91371F Lot NB113047-80 M556 Purity Correction Factor Unknown Unknown Unknown Unknown NA NA Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonamidoacetate . EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2C00) PFOSEA = Perfuorooctane sulfonyl ethylamide Date Entered/Analyst: 05/15/00, 06/12/00, 09/03/00 CSH/LAC Date Verified/Analyst: 06/05/00. 06/06/00 CSH: 02/26/01 hoj Purity Entered/Verified: 02/16/01 LAC Corrected PFOS LOQ (0.0613 ug/g) to include std correction factors new LOQ is 0.0491 ug/g. LAC 02/19/01 . Surrogate Verified NA NA NA NA Confirmed Low Confirmed Low NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA M556 Cone. ng/g 0.00 0.00 0.00 0.00 296 336 0.00 37.4 0.00 29.0 8.62 5.14 0.00 10.9 8.22 7.79 860 591 546 409 522 395 297 292 307 510 M556 Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 100 100 100 100 100 100 100 100 100 100 M556 Calc. Cone, "g/g 0.00 0.00 0.00 0.00 294 333 0.00 37.3 0.00 29.3 8.76 5.15 0.00 10.8 8.29 7.67 86649 58978 55321 40710 52862 39739 29927 29267 30992 51513 Filename D050800004 D050800017 D050800005 D050800018 D050800019 D050800020 D050800023 D050800024 D050800025 D050800026 D050800027 D050800030 D050800031 D050800032 D050800033 D050800034 D050800051 D050800052 D050800053 nosnsnon-a D050800055 D050800058 D050800059 D050800060 D050800061 D050800062 Concentration of M556 ug/g or % Ree. <LOQ (0.0308 ug/g) <LOQ (0.0308 ug/g) <LOQ (0.0308 ug/g) <LOQ (0.0308 ug/g) 98% 112% <LOQ (0.0308 ug/g) 0.0373 <LOQ (0.0308 ug/g) <LOO (0.0308 ug/g) <LOQ (0.0308 ug/g) <LOQ (0.0308 ug/g) <LOG (0.0308 ug/e) <LOQ (0.0308 ug/g) <LOQ (0.0308 ug/g) <LOQ (0.0308 ug/g) 86.6 59.0 55.3 40 7 52.9 39.7 29.9 29.3 31.0 51.5 Mean M556 ug/g <LOQ <LOQ 105% <LOQ <LOQ 58.9 36.3 RSD Std Dev MS/MSD RPD NA NA NA NA 13% NA NA NA NA -VO O 17.0 26.2 9.51 E T S -8 -7 .0 3MEnvironmental Laboratory Lvr Week 53 Page 263 3M M edical D epartm ent Study: T6316.1 A M DT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 LRN-U2103 Study: Product Number(Test Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Date of Extraction/Analyst: Date of Analysis/Analyst: Date o f Data Reduction/Analyst: Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Liver ETS-8-6.0 & ETS-8-7.0 Filename: See Below Davey 070799 R-Squared Value: See Attachments MassLynx 3.3, 3.4 Slope: See Attachments 2/29/00 SAL Y-Intercept: See Attachments 05/08/00, 05/24/00,08/21/00, 08/23/00 IAS/HOJ/MMH 05/09/00, 05/25/00,08/22/00, 08/28/00 IAS/MMH/HOJ W E E K 53 RAT L IV E R lot 529 Group Dose Sample # PFOSEA Purity Correction Factor Method Blk Matrix Blk RBL02290-H20 Blk-5 RBL02290-H20 Blk-6 RBL02290-Liver Blk-5 Unknown Unknown Unknown QC - 250 ppb RBL02290-Liver Blk-6 C90714M-250 ppb-MS-5-I C90714M-250 ppb-MS-5-2 Unknown NA NA Group 1 . Control 0.0 mg/kg Group 1 Control 0.0 mg/kg C90714M C90751M C90752M C90754M C90767M C91121F C91122F C91124F C91133F C91152F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Group 4 Low Dose 3.0 mg/kg C90902M C90918M C90950M Unknown Unknown Unknown Group 4 Low Dose 3.0 mg/kg C90951M C90957M C91323F C91347F C91352F C91367F C91371F Unknown Unknown Unknown Unknown Unknown Unknown Unknown PFOS = PerHuorooctanesulfcnate PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2C00) PFOSEA = Perfuorooctane sulfonyl ethylamide Date Entered/Analyst: Date Verified/Analyst: 05/15/00, 06/12/00, 09/03/00 CSH/LAC 06/05/00. 06/06/00 CSH: 02/26/01 hoj Purity Entered/Verified: 02/16/01 LAC Corrected PFOS LOQ (0.0613 ug/g) to include std correction factors new LOQ is 0.0491 ug/g. LAC 02/19/01 Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOSEA Cone. ng/g NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR PFOSEA Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 PFOSEA Calc. Cone. ng/g NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NF. NR NR NR NR NR NR Filename NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Concentration of PFOSEA ug/g or % Rec. NR NR NR NR NR NR NR NR NR NR NR NR NR ' NR NR NR NR NR NR XTD NR NR NR NR NR NR Mean PFOSEA " g/g NR NR NR NR NR NR NR RSD Std Dev MS/MSD RPD NA NA NA NA NA NA NA NA NA NA ETS-8-7.0 3MEnvironmental Laboratory L vr W eek 53 5/31/2001 Page 264 3M M edical D epartm ent Study: T6316.1 A M DT# 092597.1 Covance# 6329-212 Analytical Report: FACT-TOX-001 LRN-U2103 Study: Product Number(Test Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Date of Extraction/Analyst: Date of Analysis/Analyst: Date of Data Reduction/Analyst: Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Liver ETS-8-6.0 & ETS-8-7.0 Filename: See Below Davey 070799 R-Squared See Attachments MassLynx 3.3,3.4 Slope: See Attachments 2/29/00 SAL Y-Intercept See Attachments 05/08/00, 05/24/00, 08/21/00, 08/23/00 IAS/HOJ/MMH 05/09/00, 05/25/00,08/22/00, 08/28/00IAS/MMH/HOJ WEEK 53 RAT LIVER Group Dose Sample # Method Blk Matrix Blk QC - 250 ppb Group 1 Control 0.0 mg/kg Group 1 Control 0.0 mg/kg Group 4 Low Dose 3.0 mg/kg Group 4 Low Dose 3.0 mg/kg RBL02290-H20 Blk-5 RBL02290-H20 Blk-6 RBL02290-Liver Blk-5 RBL02290-Liver Blk-6 C90714M-250 ppb-MS-5-1 C90714M-250 ppb-MS-5-2 C90714M C90751M C90752M C90754M C90767M C91121F C91122F C91124F C91133F C91152F C90902M C90918M C90950M C90951M C90957M C91323F C91347F C91352F C91367F C91371F Concentration ofPFOS ug/g or % Ree. <LOQ (0.00491 ug/g) <LOQ (0.00491 ug/g) <LOQ (0.00491 ug/g) <LOQ (0.00491 ug/g) 177% 100% 0.560 0.378 0.796 0.693 0.428 0.301 0.305 0.429 0.540 0.374 597 438 924 699 818 661 861 770 627 549 PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 = C8F17SO2N((H)CH2C00) . PFOSEA = Perfuorooctane sulfonyl ethylamide Date Entered/Analyst: 05/15/00, 06/12/00, 09/03/00 CSH/LAC Date Verified/Analyst: 06/05/00. 06/06/00 CSH: 02/26/01 hoj Purity Entered/Verified: 02/16/01 LAC Mean RSD Concentration Mean RSD Concentration Mean PFOS Std Dev of PFOSA PFOSA Std Dev of PFOSAA PFOSAA ug/g MS/MSD RPD ug/g or % Ree. ug/g MS/MSD RPD ug/g or % Ree. ug/g NA <LOQ (0.0123 ug/g) NA <LOQ (0.0307 ug/g) <LOQ NA <LOQ (0.0123 ug/g) <LOQ NA <LOQ (0.0307 ug/g) <LOQ NA <LOQ (0.0123 ug/g) NA <LOQ (0.0307 ug/g) <LOQ NA <LOQ (0.0123 ug/g) <LOQ NA <LOQ (0.0307 ug/g) <LOQ * 77% 109% 138% 56% 95% 86% 21% 120% 114% <LOQ (0.00614 ug/g) <LOQ (0.0307 ug/g) 0.0354 0.05 0.0117 <LOQ (0.0307 ug/g) 30.7 0.0183 55.1 0.04 0.571 0.175 0.0196 0.0182 0.0100 <LOQ (0.0307 ug/g) <LOQ 0.0125 <LOQ (0.0307 ug/g) <LOQ (0.00614 ug/g) <LOQ (0.0307 ug/g) 0.0253 <LOO (0.0307 ue/e) 0.390 25.5 0.0993 0.0159 0.00971 0.0139 48.7 0.00677 <LOQ (0.0307 ug/g) <LOQ (0.0307 ug/g) <LOQ 29.8 80.9 19.6 40.1 29.3 27.2 7.1.5 68.6 29.9 TO 695 189 40.9 28.2 8.44 60.7 55.7 23.7 49.4 21.8 41.2 21.9 45.2 17.7 694 123 26.7 17.3 32.2 25.3 4.37 46.1 56.3 47.6 * High lecovciy was eoufiniieu on 8/21/00, data was not entered because it was outside the calibration range. 4/20/01 mmh RSD Std Dev MS/MSD RPD NA NA NA NA 9% NA NA NA NA JO . 21.3 11.9 5.67 ETS-8-7.0 3MEnvironmental Laboratory Lvr W eek 53 5/31/2001 Page 265 3M M edical D epartm ent Study: T6316.1 A iviuiff u ysy/ .i Covance# 6329-212 Study: Product Num ber(Test Substance): M atrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Date o f Extraction/Analyst: Date o f Analysis/Analyst: Date o f Data Reduction/Analyst: Sample Data 104 W eek D ietary Carcinogenicity Study w ith N arrow Range (98.1% ) N -Ethyl Perfluorooctanesulfonam ido Ethanol in Rats T -6 3 16 (EtFOSE-OH) Rat Liver ETS-8-6.0 & ETS-8-7.0 Filename: See Below Davey 070799 R-Squared Value: See Attachments MassLynx 3.3,3.4 Slope: See Attachments 2/29/00 SAL Y-Intercept: See Attachments 05/08/00, 05/24/00,08/21/00,08/23/00IAS/HOJ/MMH 05/09/00, 05/25/00,08/22/00, 08/28/00 IAS/MMH/HOJ WEEK 53 RAT LIVER Group Sample # Concentration Dose of EtFOSE ug/g or % Rec. Method Blk RBL02290-H20 Blk-5 NR Matrix Blk QC - 250 ppb RBL02290-H20 Blk-6 RBL02290-Liver Blk-5 RBL02290-Liver BIk-6 C90714M-250 ppb-MS-5-1 C90714M-250 ppb-MS-5-2 NR NR NR NR NR Group 1 Control 0.0 mg/kg C90714M C90751M C90752M C90754M NR NR NR NR Group 1 Control 0.0 mg/kg C90767M C91121F C9U22F C91124F NR NR NR NR C91133F C91152F NR NR Group 4 Low Dose 3.0 mg/kg Group 4 Low Dose 3.0 mg/kg C90902M C90918M C90950M C90951M C90957M C91323F C91347F C91352F NR NR NR NR NR NR NR NR C91367F C91371F NR NR PFOS - Perfluorooctanesulfonate PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 = C8F17S02N((H)CH2C00) PFOSEA = Periuorooctane sulfonyl ethylamide Date Entered/Analyst: Date Verified/Analyst: 05/15/00, 06/12/00, 09/03/00 CSH/LAC 06/05/00. 06/06/00 CSH: 02/26/01 hoj Purity Entered/Verified: 02/16/01 LAC Corrected PFOS LOQ (0.0613 ug/g) to include std correction factors new LOQ is 0.0491 ug/g. LAC 02/19/01 Mean EtFOSE ug/g NR NR NR NR NR NR NR RSD Std Dev MS/MSD RPD NA NA NA NA NA NA NA NA NA NA NA Concentration of M556 ug/g or % Rec. <LOO (0.0308 ug/g) <LOQ (0.0308 ug/g) <LOQ (0.0308 ug/g) <LOQ (0.0308 ug/g) 98% 112% <LOQ (0.0308 ug/g) 0.0373 <LOQ (0.0308 ug/g) <LOQ (0.0308 ug/g) <LOQ (0.0308 ug/g) <LOQ (0.0308 ug/g) <LOQ (0.0308 ug/g) <LOQ (0.0308 ug/g) <LOQ (0.0308 ug/g) <LOQ (0.0308 ug/g) 86.6 59.0 55.3 40 7 52.9 39.7 29.9 29.3 31.0 51.5 Mean M556 ug/g <LOQ <LOQ 105% <LOQ <LOQ 58.9 36.3 RSD Std Dev MS/MSD RPD NA NA NA NA 13% NA NA NA NA 28.8 17.0 26.2 9.51 Analytical Report: FACT-TOX-001 L R N -U 2103 Concentration of PFOSEA ug/g or % Rec. NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR \m NR NR NR NR NR NR Mean PFOSEA ug/g NR NR NR NR NR NR NR RSD Std Dev MS/MSD RPD NA NA NA NA NA NA NA NA NA NA NA ETS-8-7.0 3MEnvironmental Laboratory I.vrW eekS3 / i t /' ru n Page 266 3M M edical D epartm ent Study: T6316.1 CWeofExtraction/Analyat DateofAnalyai^Ajietyat DoleofUHi Sample Data WEEK185 RATLIVER AMDT# 092597.1 Covine*# 6329-212 104WeekDietaryCKcmogrok.it> Surly withNa T-HI(EtroSE-OH) * Range(96 IS)N*Elhyl PerfUeoeoocteieeulfoQKneloElheaol m ETS-8-6.0ft ETS-l-7.0 Amelie062498. Devey070799 MauLyn* 33 011400. 0116/00,Oi-l.tiOl RWW'SAL'KJS . 04/24/00.04/15/00, 0426/00,06 D042600013 AOJCI00004 AO2IOOOI9 AJM00M A03M00Q17 <LOQ(0024Sug <LOQ(0.0243ug <LOQ(00245ug D042600030 A032700024 A0J2700023 A032700026 DM2600036 D042600037 A032700029 A03270003I D042800043 :LOQ(0.0245ug/g) A032700039 A0J2700O6I PPOSAA" Periluorooctaneeulloanuioecetate EtFDSC- NarrowRangeN-Elhyl Perfluorooclaaeeulftranatoethyli MSS6* C6FI 7SO2N((H)CH2CO0) PFlaLA- PerfborooctancauIRmyletbyIemale OIWOI ho, Punty Enhevd/Vended. ' ' 7WI'f -lu* Hdcorrectiontoa n g LAC0219/01 A0I0322021 A022900080 A01500063 A022900032 A0BI500067 A022900033 A08I50007I A032700076 A022900049 A022900061 AO04000JI A022900023 A022900024 A022900023 A022900026 AD!1300044 ' A022900030 AO12900031 concentnuoon7x<f1*dJloci0J/|5/0jeahenUei L Analytical Report: FACT-TOX-001 L R N -U 2103 3MEnvironmental Laboratory Page 267 3M M edical D epartm ent Study: T6316.1 Malhod/Revaioo Analytic*! Equipment SystemNu Instrument SoftwaruVoiion DaleofE*tncbun/Analyst DateofAnalysa,Analyst Dateof Data Redin.'boQ/Analyst Sample Data 104Week Dietary Caroofenicity StudyunthNanowRange(g I-.)N-Elhyl PcrfVuoroos-tanesuliooinudoEthanol a flab T-6314(BFOSE-OH) ETS-8-60AETS-1-70 Amelia062496, Davay070790 MassLym3 3 0-14/00,0--16-00, 03'1501 RWWSAUKJS 02CI'Oft.02:9'00,OiOIOO,03/03,00.03*l,00,03/27.00,04/:4'00,04/25-00,04/26/00,O'lS,l,03-22/01 mmh/mee/ias-sah 02:800, 01/0100.0j,0j/00. 0106/00, 041700, O4C4O0, M-25/00,04/26-00, W07/00,081700,01/23/01 AS/MEE-MMH/ADV Analytical Report: FACT-TOX-001 L R N -U 2103 DaleEntered'Analyst. DaleVenfiedAnalyst PurityEnteued'Venlled 01 1400,03 1600,01 1700,04/2700,05 1700,05 !g'00. 09 Ot'OO,012601,04 1901 LAC2CSH 03 09.01 hoj 02110! LAC 3MEnvironmental Laboratory Page 268 3M M edical D epartm ent Study: T6316.1 Study ' ProductNmnbcrfTeat Subitanee7 MethodRevoion Analytical Equipment SyrtetnNumber DMeafEtttactettVAlmiyit DaleofAmdyue/Amlya Dateof Dt Reduction/Analyit Sample Data 104Wok DieOfyCafnaopeniedySeedywithNarour Rart*eiM|%)N-Edtyll T-6J6 \EiOSE-OHI ETS-8-60* ETS--70 Aimba06249&. Efcvey070799 0114/00,02/16-00,03/15/01 RWW/SAL/KJS M l -00,01-2900, 030I-00, 03-03/00, 03-04/00,03/27-00,04-24-00, 04/25 01IS/00.03-0! 00, 0303.-00, 03/06/00, 04/17/00,04/24/00,0125/00, 04,26 AMDT# 092597.1 Covane# 6329-212 WMH/MEE/IAS-SA3 IAVMEEMMH/ADV Analytical Report: FACT-TOX-001 L R N -U 2103 M350- C8PI7S02N((H)CH:COO) PROSEA- ratomacaat lulftmyla DateEntendAnaJyet DateYcnAedAaatyil Punt) EnteredYenVi CorrectedPROSLOQ(00306 u*/|)to Deludeltd correct*beton newLOQu 00243u*/* LACO'19/O! 3MEnvironmental Laboratory LAC/CSH Page 269 3M M edical D epartm ent Study: T6316.1 Covtnce# 6329.212 Product NimTe*tSubstancei Methnd/Rcvuioii Instrument Softwarw/Vcsstoa. DleofExmcbaa/Analyst DaleofAnalysis/Analyst Dde of Data Reduction/Analyst SampleData ICWed DietaryCarcnoyerucjiyStudymthNarrowR siaO il*.)N-EchytPenTu. T-4316(EtFOS&OH) HT5-8-60ETS-8.70 Aurelia06249|, Davcy070799 MusLyra3.3 02/14/00,021111/00,03/15/01 FWW/SAL/KJS 0211/00,02/29,00, 03/01/00,03/03/00,03/04/00, 03/2700, 04/24/00,1 021100,03/01/00,03/03/00, 03/06/00, 04/17/00, 04/24/00.0415/00, 04.1 ,04/26/00,08/15,00,031201 MMH/MEE1AS/SAH .04,27/00,08/17/00,0313/01 lAS'MEE'MMH'ADV 1004312,00013 WEEK10$ RATLIVER Creap RBL021400-WBk-2 RRI.02l600.WRIk-4 RBL03150l-WBk-2 PRL02I400-LBH.: HR103l5Ol*LBk>? RTL03150l-LBk-2 C907I6M-MS-2 C90722M-MSD-2 C907I2M-MSD-S CW7M6FMMW C9II57R-MSD-5 RTL03ISOI-LivirUSD PTOSCa Parky CarrartWa Facme Unknnam Unknown NA Unknown NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA 2nd Analysis OK 2odAnalysisOK NA C907I6M-I C90716M-2 C90722M-1 C90722M-2 C90724M CW24M-B1-J C90726M-B1-6 C90735M C90742M C9074JM CW74TM C90750M C90758M C90763M CW778M C91157P-8lk-5 C9II59P Unknown Uoknown Unknown Unknown Unknown Unknown Unknown Lktknoutr Unknown Uokturwu Unknown Unknown Unknown Unknown 1 Connned High NA LowDose 3.0tli*fc* LowDoaa SOnyti C90782M C90783M C907B5M C90787M C907SBM C90791M C90794M C90799M CW8MM C90809M C9O8I0M C908I1M C908I2M C908I5M C90823M C90829M C90B30M C90835M C90838M C90B4OU C91227F C91232F C9I235F C9I236F C91241F am Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Utknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Utknown Unknown Contened High NA PFOSEA 000 NA 000 000 NA 374 294 274 PROSEA DUm Parlar \ NA J NA NA 1 1 1 240 NA NA 1 1 1 1 1 1 1 1 1 E 000 " ------ ef PROSEA PROSEA trl! <LOQ 0307u*/g AOJOIOOOO <LDQ 030?up* O.On A03040000 NA A022IOOOO. <LOQ(00307u*/g 0.0(1 0.00 AOfOIOOOCM <LOQ<0030?afg NA z 2 241 M3 2 NA E E E NA z A0221000I AO22101X11 NA A030400016 AI23040Q01 L% A08I5000I7 NA z A022I00045 <LOQ(0.0307y*/g <LOQ(O0307u*/g A022I00022 <LOQ(0.0307u*/g A022I00023 <LQ<3<PQ3Q7up* A022I00024 <LOQ(00307US's A022I00025 <LOQ(00307u*/j A022I00026 <LQQ(aO307ne'# <LOQ(00307 up* A022100050 <LQQ(00307up* <LOQ(0.0307up* <LOQ(0.0307up*) A02210003I <LOQ(00307u*/*) <LOQ(00307up*) <LOQ(00307u*/*: <LOQ(0.0307up* <LOQ(00307 li*/*) A022I00033 <LOQ(00307u*/*) <LOQ(0.0307up*) A022I00037 <LOQ(0.0307up*) A032700064 <LOQ(00613 up1*) <LOQ(0.0307up*) <LOQ(00307u*/*> <LOQ(0.0307 u*/*> A022100058 <LOQ(00307 it*/*) <LOQ(00307u*/|) <LOQ(00307u*/g) A022I00040 <100(0.0307 it*/*) <LOQ(00307 ii*/*) <LOQ(0.0307u*/*) <LOQ(00307u*/|) <100(0.0307 u*/*) A022100073 <LOQ(00307li*/*) <LOQ(0.030?U*/*) <LOQ(00307U*/*) A022I00078 <LOQ(00307u*/g) AD32700089 <LOQ(006)311*/*) <LOQ(0.0613U*/*) A022100079 <LOQ(00307up*) A022IQ0065 <LO0(a.O0?u*(l ) A0" 100080 <100(0.0307 u*/*) A03270009I <LOQ(00613 h*/*) A022I0008I <LO0(00307u*/g) A022I00066 <LOQ(00307u*/*) A022I00067 <LOQ(00307 U*/*) A022I00068 <LOQ(0.0307u*/*> AO22100071 <LOQ(0.0307u*<*) <LOQ(00307U*/*) A022I00085 <LOQ(0.0307upg) A022I00086 <LOQ(0.0307ii*/*) 0292 A0221000E7 <LOQ(0.0307u*/*) <LOQ(0.0307u*/*) AOZ2IOOOS9 <LOQ030307up*) <LOQ(00307u*/*) <LOQ(00307u*/*) A022100092 A032700095 <LOQ(0.0613u*/g) A022100093 <LOQ(003C7u*/*) <LOQ(00307it*/*) A022I0010I <LOQ(0.0307u*/*) <LOQ(0.0307u*/g) AO22100095 <LOQ(0.0307u*/*) A02210C096 <LOQ(0.0307a*/*) <LOO(00307Uc/cl ___ 2 2 _ . USD SMDev NA NA EtPOSE- NarrowRange\-Ethy! FertiucrooctenmulfooMidoethylalcohol M566-CBFI7S02N((H)CH2COO) PROSEA- Peetborooctoncsulfonyl ethytamale DmeEntered/Analyst 03/1400,03 1/ 00,03 1700,04,2) 00,05/]700 05 ] DateVenflad/Analyst 03/09/01 turj PuntyEnterwd/Venfled. 02/19/01 LAC . Corrected PPOSLOQ(00306u*/g)tomtlujeHdcorrectionlcteas LAC-CSH Analytical Report: FACT-TOX-001 LRN-U2103 3MEnvironmental Laboratory Page 270 3M M edical D epartm ent Study: T6316.1 Instruirait Softwate/Vefnoo Ont offctneton/AnelyK DeleofDalaReducboiVAnalyst. SwfkDita r-6JI6(ElFOS-Off) ETS-8-6.0AETS-8-7I K>,0M6/W.03/|5I RWW/SAL.KJS O, 02/29'00, OJ'OI'jO,03/03/00,Ol'MDO, l/H/00,04/24/00, 04/25/00,04/26/W,08 "5,03] 'M, 0)/030,03/06't)0l04 17/00, WEEK185 RATLIVER Sa^bg Control RBL021400-WRB.7 RBL021600-WBIt.A RBL03I50I-WBIk-2 RBL02I400-LBD;-? RBL02l600-IJ3lk-6 RBL03130I-LBB1.2 RTL031501-1 Bit.' C90716M-MS-7 C90722M-MSD-7 C907I2M-MSD.5 C90726M-MSIV6 C9II57F-MSD.5 RTL03150l-bver MSD C907I2M-BB.6 C90716M-) CW752M-) C90722M-2 C90724M C90726M-BB-5 C90728M C90735I4 C907S0M C907S864 C90765M C9077BM C91I48F C91157F-Blk-5 CTII57F.B&.6 I SIS ow 16.27 327 Z 286 z z Ei 130 Z y CavatiraSee 4PFOS gler %Rer. <LOQ(00245u/ 1 M 'LOG uso D a MS/MSBRPI) NA <LOO(00745ue/a 'LOQ NA 'LOQ(0 Odi 1tln/n NA 'LOQ(00245U/J 'LOO NA 'LCO/O0745i6 fJA 'LOQ100613hit/ 'LOQ NA 001627 'LOQ NA " ih 100% 22% S% 83% 30% 103% 100% 7% 78% 45% " 14)% 7% 96S ,05% ,8% 'LOQ(0.0245ug/g) 'LOQ(Q0245ug/g) 005 ofS 'LOQ(00245 ug'g) 'LOQ(00245 ug/g) S Si JOreglg C91I72P SilH F C90782M C907B3M C90785M C90787M C90788M 223* 'LOQ(00245ug'g) 205 0 00650 0,78 ;* o` m Cale. Caer. Ut OW f PFOSA ag/ar % Iter. 'LOQ(00)23 ug/g <LOQ,00l23ug'g NA OW 06TO NA NA ^74 3U III >T 353 NA oS vi ODO SA 'LOQ(0 0123ug'g 'LOO(0(1171 nolo LOQ(00123 ug'g '100/0 006141./ NA NA 47% 107% 116% 86%* ss NA 'LOQ(0.0123 ug'g) 'LOQ(00123 ug/g) 'LOQ(0.0123 ug/g) LOQ(00123 ug/g) <LOQ(0.012J ug'g) <LOQ(00123 ug/g) <LO?(O.OI2J ug/g) 'LOQ(0.0123 ug/g) <LOQ(00123 ug/g) 'LOQ (00123ug'g) 'LOQ(0.0123 ug/gl 'LOQ(00123 ug/g) 'LOQ(0.0123 ug/g) 'LOO(00123 u') 'LOQ (0.0123 ug'g) *LCQ(0t>t2J ug'g) LOQ(00123 ug/g) ".00(9011) uglg) LOQ(00121 ug/g) 'LOQ(0.0123ug/g) 'LOO room >() <LOQ(00123 ug/g) 'LOQ(ODI23 ug/g) 'LOQ(00123 ug/g) 'LOQ(00123 ug/g) PFOSA Wl <LOO 'LOO NA NA NA 102% 105% 120% 107% 114% NA 'LOO SUD MSMSDRPD NA NA NA NA NA NA NA 18% 3% 7% isa 5% NA ii aTPFOSAA PFOSAA <LOQ(00307ug/g a <LOQ(0.0123ug'g OM IOO NA NA 'LOQ(00307ug/g 'LOQ (00123 ug/g) 'LOO NA NA NA NA NA 3 nrr- ^1 T% 93% S : S% 93% <9<i ,00% S i !S% ,38% NA NA NA 'LOQ(0.0613ug/g) <LOQ(0.0615ug'g) 000 'LOO(00107il/) 'LOQ (00307ug/g) <LOQ(00615ug/g) 'LOQ(0.0615ug'g) 'LOQ(0.0307ug'g) ow 'LOQ(00307ug/g) 'LOQ (00615 ug/g) NA 0 'LOQ(0.0307ug'g) 'LOQ(00307 ug/g) 00 'LOQ(00307ug/g) 'LOQ(000615ug/g) *000 LOQ(00307ug/g) <LOQ(0 0615 ug'g) 'LOQ (00615 ug'g) 0.00 'LOQ(00615ug/g) 'LOQ (00307 ug/g) E NA :'Z 0 970 LowDo C90799M C908D4M C90809M C90B1DM WI5M C90823M C90829M C90830M C90832M C90B3SM C90SJSM C9O840M C9120IF C91235F PFOS- perfiuorooLtanesitl PPOSAA" Pcrfhi'uuo'tani ElFOSE" NarrowRangeN-Ediyl Pe M556C8FI?S02N((H)CH2COO) PFOSEA Pofisorooctin* sulfcmyl etfc DateEntered/Artelyit 03.14/00.0 DataVerifiedAnalyst. 03/W'Ol lie Pimty Entered/Venfled. 0219/01 L ss i 1990 26030 32SSO 71153 20899 2 "" [S S Si Z ri? m 0: [)4 199 756 Si 326 71 2 209 L25 208 710 HE iVn 1010 101 S 0167 614 0611 671 9671 884 (1888 U6 un 0.386. [S j7 VM m 0744 0*2 >w 525 510 in 137 'T ' 0764 0.976 0.869 u3.3 z Im " Senile m reeatretted )/15'01, inalyzcdi '22'01.andthf PFOslooccotratioiireporta cm LAC03060) LU - !wLOQisO0245ug'g LAC02 NA NA 37.8 oV 22 z ElFCst Cale. Catte. 000 0.00 NA 000 OW NA Z Si 16 267 ,C7 244 z i eS ^ " e (0.0614 ug/g 'LOQ (0.121 ug'g u< A <LOQ(0 0614 ug/g 'LOQ(O23ug'g) . NA 124% 57% 81% NA 'LOQ (00614 ug/g ' LOQ(00614ug/g 'LOQ(99614ug/g .... 0 <WQ(0O6li ug`g 721 00721 'LOQ(0 0614ug/g) 0.00 'LOQ(0 0614ug/g 'LOQ(0.0614 ug'g 'LOQ (00614ug/g) B 'LOQ (00614ug/g) LOQ(00614ug/g) y TM ! ' "" 1 733 892 0.00 'LOQ (00614ug/g) 00791 Si 'LOQ(00614 ug'g) i 'LOQ(00614ug/g) '1 (Vi '01)614in*/i <LOQ(00614 ug/g) 'LOOIO0614u/d) <LOQ(0 0614 ug'g) LOQ(0 0614 ug/g) 'LOQ(O06l4iig>g) <LOQ(00614 ug'g) 'LOQ (0.0614ug'g) 0 LOQ(00614ug/g) i w 'LOQ(0.0614ug'g) *3.6 " <LOQ(00614 ug'g) 'LOQ (00614ug/g) o.w 'LOQ(00614 ug/g) 20.1 o.w <LOQ100614 ug/g) UU4 ------ 00110--------- 'I DAIO0614ii/i*t 98 5 00985 101 0 101 OW 'LOQ (0.0614 ug/g) OW <LOQ(0.0614ug'g) 'LOO100614 u/>) LOQ(0.0614ug'g) S " 'LOO100614u/el ifo 0 0 0766 002,0 1 Analytical Report: FACT-TOX-001 LRN-U2103 RBL021400-WBIk-| RB321400-WBlk-2 RBL0216OO-WBIk.5 RBL02t600-WBlk-< C91157F-MSD-5 C90712M-BB1-5 C90712M-BK-6 C90716M-1 C90716M-2 C90722M-1 C90722M-2 C9Q724M C90726M-Blk-S C90?26M-BIk-6 C90735M C90742M C90743M C90750M C90758M C90765M C90778M C907SIM C90782M C90783M C90785M C90787M CW7B8M C90791M C90794M C90799M C90804M C9009M C908I0M C9Q812M C90815M C90B29M C90B30M C90835M C90838M CT0840M <LQQ(00308 ug/g) 'LOQ (0.0308 <LOQ(0 0308 ug/g) 'LOQ (0.0308 ug/g) <LOQ(003011 <LOQ(0 0308ug/g) 'LOO 10.03 'LOO (0.03 'LOO (00308 ug/g) LOQ(0.0308u 'LOQ(00308 u 'LOQ(0 0308 eLOQ(0.030Bu, : LOQ(0.0308 u 'LOQ(0.03( 'LOQ (0 061 'LOQlO.OMugfg) 'LOQ(0.0308ug/g) 'LOQ(00108m ' LOQ(0.0308u, 'LOQ(0.0308U, 'LOQ(0.0308u, 'LOQ(0 0308 u, ;LOQ(0.0308 ug 'LOQ(0.0307ug/g) 'LOQ(0.0307ug/g) 'LOQ(00307ug/g <LOQ(0.0307ug/g) <LOQ(0.0307 'LOQ(0.0307ug/g) 'LOQ(00307ug/g) 'LOQ(00307ugg) 'LOQ(00307ug/g) 'LOQ(0.0307ug/g) 'LOQ(0.0307 ug/g) 'LOQ(0.0307 ug/g) 'LOQ(0.0307ug/g) 'LOQ(00307ug/g) ;LOQ(0.0307ug/g) 'LOQ(00307ug/g) 'LOQ(00307ug/g) 'LOO(00613 'LOQ(00307ug/g) 'LOQ(0.0307ug/g) 'LOQ(00613 ug/g) 'LOQ(0.0307ug/g) 'LOQ(00307ug/g) ' LOQ(00307 'LOQ(0.0307ug/g) 'LOQ(00307ug/g) 'LOQ(0.0307ug/g) 'LOQ(00107ug/g) 'LOQ(0.0307ug/g) 'LOQ(0.0307ug/g) .LOQ( ostri ug-g) LOQ(00307ug/g) 'LOQ(0.0307ug/g) 'LOQ(00307ug/g) 'LOQ(0.0307ug/g) 'LOQ (00307 i 'LOQ(00307ug/g) 'LOQ(0.0307ug/g) 'LOQ(006)3 'LOQ(0.0307 'LOQ(0.0307 'LOQ(0 0307ug/g) 'LOQ(00307ug/g) 'LOQ(0.0307ug/g) 'LOQ(00307ug'g) 'LOQ(0.0307ug/g) 'LOQ(0.0307ug/g) 'LOQ(0.0307ug/g) 'LOQ(00307ug/g) 'LOQ(00307 ug/g) 'LOQ(0.0307ug/g) 'LOQ(00613 ug/g) 'LOQ(00307ug/g) 'LOQ(0.0307ug/g) 'LOQ(0.0307 ug/g) 'LOQ(0 0307ug/g) 'LOQ(0 0307ug/g) 'LOQ(00307ug/g) Lj0^00307u^ 3M Environmental Laboratory Page 271 3M M edical D epartm ent Study: T6316.1 A M U lff 11925^7.1 Covance# 6329-212 Study: Product Number(Test Substance): M a tr ix : M ethod'R evision: Analytical Equipment System N um ber Instrum ent Software/Version: Date o f Extraction/Analyst: D ate o f Analysis'A nalyst: Date o f Data Reduction/Analyst: Sample Data 104 Week D ietary C arcinogenicity Study with N arrow Range (98.1% ) N -Ethyl Perfluorooctanesulfonainido E thanol in Rats T -6316 (EtFOSE-OH) Rat Liver ETS-8-6.0 & ETS-8-7.0 Amelia 062498, Davey 070799 M assLynx 3.3 02/14/00, 02/16/00 RWW/SAL 02/21/00, 02/29/00, 03/01/00, 03/03/00, 03/04/00, 07/28/00, 08/15/00 MM H /M EE/IA S 0 2 /28/00,03/01/00, 03/03/00, 03/06/00, 07/31/00, 08/17/00 IAS/M M H W E E K 105 R AT L IV E R Sample it Initial Wt. Total Maas Dose g ofLiver g Group 3 C90842M 0.9962 NA M id Dose C90844M 1.0160 NA 30.0 mg/kg C90850M 0.9930 NA C9085IM 1.0565 NA C90854M 0 .9 8 7 2 NA C90855M 0.9921 NA C90856M 1.0485 NA C90858M 1.0156 NA C90860M 1.0070 NA C90864M 1.0137 NA C90865M 1.0105 NA C90867M 0.9923 NA C90869M 1.1355 NA C90871M 1.0511 NA C90881M 1.0129 NA C90882M 0.9909 NA C90883M 0.9926 NA C90884M 0.9874 NA C9088SM 1.0068 NA C90889M 1.0299 NA C90893M 1.0178 NA C90900M 1.0072 NA Group 3 C9I252F 1.1046 NA M id Dose C91253F 1.0730 NA 30.0 mg/kg C91254F 0.9834 NA C9I256F 0 .9 9 6 3 NA C91264F 1.0678 NA C91278F C91279F 1.1455 1.0120 NA NA C91286F 1.0412 NA C91292F 1.0162 NA C91294F 1.0046 NA C91295F 1.0159 NA C91301F 1.1103 NA C91303F 0 .9 9 0 8 NA C91307F 1.0083 NA C91310F 1.0132 NA PF O S = Pertiorooctanesullonatc PFOSA = Perfluorooctanesulfonamide PFOSAA - Perfluorooctanesulfonam idoacetate EtFOSE = Narrow Range N -Ethyl Perfluorooctanesulfonam ido ethyl alcohol M 556 - C8F17S02N((H)CH2C00) PFOSEA = Perfuorooctane sulfonyl ethylam ide Date Entered/Analyst: 03/14/00, 03/16/00, 03/17/00,08/15/00, 09/03/00 LAC D ate Verified/A nalyst: 03/09/01 hoj P u rity Entered/V erified: 02/19/01 LAC PFOS Std Correction Factor 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 L ot 171 PFOS Purity Correction Factor 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0 .8 6 4 0 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0 .8 6 4 0 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0 .8 6 4 0 0.8640 0.8640 0.8640 Q.8640 0 .8 6 4 0 0 .8 6 4 0 Surrogate Verified NA NA NA NA NA NA NA NA Low, Not Confirmed NA NA NA NA NA NA NA NA Low, Not Confirmed NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOS Cone. ng/g 975 268 287 796 1104 458 106 836 424 774 469 635 298 595 267 492 239 376 642 232 371 165 437 270 533 403 381 663 100 592 124 294 56.0 235 411 141 319 Filename: R-Squared Value: Slope: Y-Intereept: See Below See Attachments See Attachments See Attachments Box 00-012, 00-013 Analytical Report: FACT-TOX-001 LRN-U2103 PFOS Dilution Factor 200 200 200 200 200 200 200 200 1000 200 200 200 200 200 200 200 200 200 200 200 200 200 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 PFOS Calc. Cone, ng/g 156858 42289 46376 120793 179256 73931 16276 131992 337224 122357 74361 102548 42001 90688 42229 79628 38587 61036 102254 36130 58405 26321 158371 100973 217110 161881 143127 231922 39747 227867 48865 117280 22079 84658 166184 56102 Filename A030300037 A030300038 A030300039 A030300040 A030300041 A030300044 A030300045 A030300046 A 081500088 A03030048 A03030051 A03030052 A03030053 A03030054 A03030055 A03030058 A03030059 A 0 8 1500091 A03030060 A03030061 A03030062 A03030065 A030300017 A030300018 A030300019 A030300020 A030300023 A030300024 A030300016 A030300025 A030300026 A030300027 A030300030 A030300031 A030300034 A030300033 arvjrtirw ivi Concentration o f PFOS ug/g or % Ree. 157 42.3 46.4 121 179 73.9 16.3 132 337 122 74.4 103 42.0 90.7 42.2 79.6 38.6 61.0 102 36.1 58.4 26.3 158 101 217 162 143 232 39.7 228 48.9 117 22.1 84.7 166 56.1 126 PFOS "g/g RSD Std Dev m s /m s d r p d 78.1 90.1 70.3 5 4 .0 127 5J 3MEnvironmental Laboratory Page 272 3M M edical D epartm ent Study: T6316.1 amdt#os2597.i Covance# 6329-212 Study: Product N um ber(T est Substance): M atrix: M ethod/R evision: Analytical Equipment System N um ber Instrument Software/Version: Date o f Extraction/Analyst: Date o f Analysis/Analyst: Date o f Data Reduction/Analyst: Sample Data 104 W eek D ietary Carcinogenicity Study with N arrow Range (98.1% ) N-Ethyl Perfluorooctanesulfonam ido E thanol in Rats T-6316 (EtFOSE-OH) Rat Liver ETS-8-6.0 & ETS-8-7.0 Filename: Amelia 062498, Davey 070799 R-Squared Value: M assLynx 3.3 Slope: 02/14/00,02/16/00 RWW/SAL Y -I n te rc e p t: 02/21/00, 02/29/00, 03/01/00, 03/03/00, 03/04/00, 07/28/00, 08/15/00 MMfLMEE/IAS 02/28/00, 03/01/00, 03/03/00, 03/06/00, 07/31/00, 08/17/00 IAS/M MH W E E K 105 R A T L IV E R ________________ lotL-15709 Dose S a m p le ti PFOSA Purity C o rrectio n Surrogate Verified F a c to r G roup 3 M id Dose 30.0 mg/kg C90842M C90844M C90850M C90851M Unknown Unknown Unknown Unknown NA NA NA NA C90854M Unknown NA C90855M Unknown NA C90856M Unknown NA C90858M Unknown NA C90860M Unknown NA C90864M Unknown NA C90865M Unknown NA C90867M Unknown NA C90869M Unknown NA C90871M Unknown NA C90881M Unknown NA C90882M Unknown NA C90883M Unknown NA C90884M C90885M Unknown Unknown High. Not Confirmed NA C90889M Unknown NA C90893M Unknown NA G roup 3 M id Dose 30.0 mg/kg C90900M C91252F C91253F C9I254F Unknown Unknown Unknown Unknown NA NA NA NA C91256F C91264F Unknown Unknown NA NA C91278F Unknown NA C91279F C91286F Unknown Unknown NA NA C91292F Unknown NA C91294F Unknown NA C91295F Unknown NA C9I301F C91303F Unknown Unknown NA NA C91307F Unknown NA C91310F Unknown NA r r S = Periiuoroocianesunonale PFOSA = Perfluorooclanesulfonamide PFOSAA = Perfluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Elhyl Perfluorooctanesulfonam ido ethyl alcohol M 556 =*C 8F 17S 02N ((H )C H 2 C 0 0 ) PFOSEA = Perfuorooctane sulfonyl elhvlamide Date Entered/Analyst: 03/14/00,03/16/00, 03/17/00, 08/15/00, 09/03/00 LAC Date Verified/Analyst: 03/09/01 hoj Purity Entered/Verified: 02/19/01 LAC PFOSA Cone. " g /s 366 188 323 361 472 518 435 314 633 478 224 271 313 454 324 371 270 53.6 424 338 354 334 386 387 452 382 334 513 236 497 354 377 166 309 330 297 266 PFOSA D ilution F a c to r 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 200 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 PFOSA Calc Cone, ng/g 7349 3696 6514 6828 9569 10434 8293 6178 12569 9434 4441 5466 5521 8631 6403 7493 5439 10849 8430 6567 6949 6625 6992 7206 9190 7676 6251 8954 4670 9554 6960 7509 3266 5559 6664 5896 5242 Filenam e A030300087 A030300088 A030300089 A030300090 A030300093 A030300094 A030300095 A030300096 A030300097 A030300100 A0303Q0101 A 030 3 0 0 I0 2 A030300103 A03O3OO1O4 A030300107 A030300108 A030300109 A 081500091 A 030300110 A 030300111 A030300U4 A030300115 A030300067 A030300068 A030300069 A030300072 A030300073 A030300074 A030300066 A030300075 A030300076 A030300079 A030300080 A030300081 A030300082 A030300083 A030300086 See Below See Attachments See Attachments See Attachments Box 00-012, 00-013 C o n cen tratio n of PFOSA ug/g o r % Ree. 7 .3 5 3 .7 0 6.51 6 .8 3 9 .5 7 10.4 8.29 6.18 12.6 9.43 4 .4 4 5 .4 7 5 .5 2 8.63 6.40 7.49 5 .4 4 10.8 8.43 6.57 6 .9 5 6 .6 2 6 .9 9 7.21 9.19 7.68 6.25 8.95 4 .6 7 9 .5 5 6 .9 6 7.51 3.27 5.56 6.66 5 .9 0 5 .2 4 PFOSA ug/g 7.44 6 .7 7 RSD StdD ev M S/M SD R PD 29.1 2 .1 7 25.4 1 72 Analytical Report: FACT-TOX-001 L R N -U 2103 lotT-712M PFOSAA Purity C o rrec tio n Factor Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown t Intnr.u'n Surrogate V erified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOSAA ng/g 291 354 506 362 180 977 545 471 583 550 241 253 705 620 350 420 295 839 866 802 430 488 282 430 408 533 271 699 239 911 351 471 261 248 422 356 337 PFOSAA D ilution Factor 20 20 20 20 200 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 PFOSAA Calc. Cone, ng/g 5840 6967 10194 6845 36513 19689 10390 9279 11573 10854 4761 5093 12412 11794 6916 8486 5935 17002 17198 15569 8459 9694 5114 8009 8292 10693 5070 12207 4729 17499 6906 9383 5143 4470 8525 7067 6C57 F ilen am e A030300087 A030300088 A030300089 A030300090 A030300041 A030300094 A030300095 A030300096 A030300097 A030300100 A 0 30300I01 A030300102 A030300103 A030300104 A030300107 A 030300I08 A030300109 A 081500092 A 030300110 A 030300111 A 0303001I4 A030300115 A030300067 A030300068 A030300069 . A030300072 A030300073 A030300074 A030300066 A030300075 A030300076 A030300079 A030300080 A030300081 A030300082 A030300083 A03030003C C o n c en tra tio n of PFOSAA ug/g o r % Ree. 5 .8 4 6.97 10.2 6 .8 5 36.5 19.7 10.4 9 .2 8 11.6 10.9 4.76 5.09 12.4 11.8 6 .9 2 8.49 5 .9 4 17.0 17.2 15.6 8 .4 6 9.69 5.11 8.01 8 .2 9 10.7 5 .0 7 12.2 4 .7 3 17.5 6.91 9.38 5 .1 4 4 .4 7 8 .5 2 7 .0 7 . PFOSAA 11.4 /. RSD Std Dev M S/M SD R PD 6 .9 5 3.48 PT.S.7 n 3M E nvironm ental Laboratory Page 273 3M M edical D epartm ent Study: T6316.1 A M D T# 092597.1 Covance# 6329-212 Study: Product N um berfT est Substance): Matrix: M ethod/R evision: Analytical Equipment System Number Instrument Software/Version: Date o f Extraction/Analyst: D ate o f A nalysis''Analyst: D ate o f D ata R eduction/Analyst: Sample Data W E E K 105 R A T L IV E R Group Dose Sample ft Group 3 M id Dose 30.0 mg/kg Group 3 M id Dose 30.0 mg/kg C90842M C90844M C9O 850M C90851M C90854M C90855M C90856M C90858M C90860M C90864M C90865M C90867M C90869M C90871M C90881M C90882M C90883M C90884M C90885M C90889M C90893M C90900M C91252F C91253F C91254F C91256F C91264F C9I278F C91279F C91286F C91292F C91294F C91295F C91301F C91303F C91307F C91310F 104 W eek Dietary C arcinogenicity Study w ith Narrow Range (98.1% ) N -Elhyl Pertluorooctanesulfonam ido E thanol in Rats T-6316 (EtFOSE-OH) Rat Liver ETS-8-6.0 & ETS-8-7.0 F i le n a m e : Amelia 062498, Davey 070799 R-Squared Value: M assLynx 3.3 Slope: 02/14/00,02/16/00 RWW/SAL Y -I n te rc e p t: 0 2 /21/00, 01/29/00, 03/01/00, 0 3 /03/00,03/04/00, 07/28/00, 08/15/00 M M H/M EE/1AS 02/28/00, 03/01/00, 03/03/00, 03/06/00, 07/31/00, 08/17/00 IAS/M M H See Below See Attachments See Attachments See Attachments lotU nknow n EtFOSE Purity Correction Factor Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA EtFOSE Cone. HR/K 95.0 16.8 39.1 167 39.1 96.3 34.5 66.2 80.5 76.3 137 80.6 86.0 51.3 58.8 153 48.4 72.4 219 49.2 81.3 0.00 84.1 112 96.9 97.8 111 147 24.1 111 154 138 9.69 66.0 120 89 1 33.7 EtFOSE Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 EtFOSE Calc. Cone, ng/g 95.3 16.6 39.3 158 39.6 97.0 32.9 65.2 80.0 75.2 135 81.2 75.7 48.8 58.0 155 48.8 73.3 218 47.7 79.9 0.00 76.2 105 98.5 98.1 104 129 23.8 107 151 137 9.54 59.4 122 88.4 33.3 Filename A 0728000I7 A072800018 A072800019 A072800020 A072800021 A072800024 A07280Q025 A072800026 A072800027 A072800028 A072800031 A072800032 A072800033 A072800034 A072800035 A072800038 A072800039 A072800040 A072800041 A072800042 A072800045 A072800046 A072800047 A072800048 A072800049 A072800052 A072800Q53 A072800054 A072800055 A072800056 A072800059 A072800060 A072800061 A072800062 A072800063 A072800066 A072800067 _____ Concentration of EtFOSE ug/g or % Ree. 0.0953 <LO Q (0 .0614 ug/g) <LOO (0.0614 u e /rl 0.158 <LOQ (0.0614 ug/g) 0.0970 <LOQ (0.0614 ug/g) 0.0652 0.0800 0.0752 0 .1 3 5 0.0812 0.0757 <LOQ (0.0614 ug/g) <LOO (0.0614 up/ pI 0 .1 5 5 <LOO (0.0614 up/ pI 0.0733 0.218 <LOQ (0.0614 ug/g) 0.0799 <LOQ (0.0614 ue/ b) 0.0762 0 .1 0 5 0.0985 0 .0 9 8 1 0.104 0 129 <LOO (0.0614 up/ pI 0.107 0.151 0.137 <LOQ (0.0614 ug/g) 0.0594 0.122 0.0884 <LOQ (0.0614 ug/g) PFOSA = Perfluorooctanesulfonamide PFOSAA * Perlluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonam ido ethyl alcohol M 556 = C8F17S02N((H)CH2CCX)) PFOSEA = Perfuorooctane sulfonyl ethylamide Date Entered/Analyst: 03/14/00,03/16/00,03/17/00,08/15/00,09/03/00 LAC D ate V erified/A nalyst: 03/09/01 hoj Purity Entered/V erified: 02/19/01 LAC Mean EtFOSE ug/g 0.0883 0.103 Analytical Report: FACT-TOX-001 LRN-U2103 RSD Std Dev MS/MSD RPD 47.1 0.0415 26.9 0 .0 2 7 6 lo tN B113047-80 M556 Purity Correction Factor Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown ' Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA M556 ng/g 541 345 421 614 797 427 255 590 778 597 399 312 453 545 326 520 264 729 618 413 393 272 537 455 770 512 357 584 226 523 479 517 150 415 620 268 254 M556 Dilution Factor 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 M556 Calc. Cone, ng/g 10857 6798 8480 11631 16151 8603 4869 11618 15449 11779 7888 6286 7985 10364 6427 10500 5327 14760 12272 8025 7724 5398 9729 8473 15661 10275 6689 10199 4468 10051 9421 10286 2961 7474 12522 5325 5CC6 Filename A030300087 A030300088 A030300089 A030300090 A030300093 A030300094 A030300095 A030300096 A030300097 A0303OOIOO A03030010I A030300I02 A030300103 A030300104 A030300I07 A 030300108 A030300109 A081500092 A 030300110 A 030300111 A 030300114 A030300115 A030300067 A030300068 A030300069 A03030072 A030300073 A030300074 A030300066 A030300075 A030300076 A030300079 A030300080 A030300081 A030300082 A030300083 AC3C30CCS6 Concentration o f M556 ug/g or % Ree. 10.9 6.80 8 .4 8 11.6 16.2 8.60 4 .8 7 11.6 15.4 11.8 7.89 6.29 7.99 10.4 6 .4 3 10.5 5 .3 3 14.8 12.3 8 .0 3 7.72 5 .4 0 9.73 8 .4 7 15.7 10.3 6.69 10.2 4 .4 7 10.1 9.42 10.3 2.96 7 .4 7 12.5 5.32 5.01 M556 Ug/g 9.51 8.57 RSD Std Dev MS/MSD RPD 34.6 3.29 38.8 i.Ji 3MEnvironmental Laboratory Page 274 3M M edical D epartm ent Study: T6316.1 A M D T# 092597.1 Covance# 6329-212 Study: Product N um berfTest Substance): Method y'Re vision: Analytical Equipment System Number: Instrum ent Soflw are/V ereion: Date o f Extraction/Analyst: Date o f Analysis/Analyst: Date o f Data Reduction/Analyst: Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesuifonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Liver Filen am e: See Below ETS-8-6.0 & ETS-8-7.0 R-Squared ValuSee Attachments A m elia 062498, D avey 070799 Slope: See Attachments M assLynx 3.3 Y-Intercept: See Attachments 02/14/00, 02/16/00 RWW/SAL Box 00-012, 00-013 02/21/00, 02/29/00, 03/01/00, 03/03/00, 03/04/00, 07/28/00, 08/15/00 M M H /M EE/IA S 02/28/00, 03/01/00, 03/03/00, 03/06/00, 07/31/00, 08/17/00 IAS/M M H WEEK 105 RAT LIVER lot 529 Group Sample # PFOSEA Purity Surrogate Dose Correction Verified Factor Group 3 C90842M Unknown NA M id Dose C90844M Unknown NA 30.0 mg/kg C90850M C90851M Unknown Unknown NA NA C90854M Unknown NA C90855M Unknown NA C90856M Unknown NA C90858M Unknown NA C90860M Unknown NA C90864M Unknown NA C90865M Unknown NA C90867M Unknown NA C90869M Unknown NA C90871M Unknown NA C9088IM Unknown NA C90882M Unknown NA C90883M Unknown NA C90884M Unknown NA C90885M Unknown NA C90889M Unknown NA C90893M Unknown NA Group 3 C90900M C91252F Unknown Unknown NA NA M id Dose C91253F Unknown NA 30.0 mg/kg C9I254F Unknown NA C91256F Unknown NA C91264F Unknown NA C91278F Unknown NA C91279F Unknown NA C91286F C91292F Unknown Unknown NA NA C91294F Unknown NA C91295F Unknown NA C91301F Unknown NA C91303F Unknown NA C91307F Unknown NA C91310F Unknown NA PFOS = Perlluorooctanesulfonate PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonamidoacetate EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonatnido ethyl alcohol M556 = C8F17S02N((H)CH2C00) PFOSEA = Perfuorooctane sulfonyl ethylamide D ate Entered/A nalyst: 0 3 /1 4 /0 0 ,0 3 /1 6 /0 0 ,0 3 /1 7 /0 0 ,0 8 /1 5 /0 0 ,0 9 /0 3 /0 0 LAC D ate Verified/A nalyst: 03/09/01 hoj Purity Entered/V erified: 02/19/01 LAC PFOSEA Cone. ng/g 0.00 0.00 0.00 0.00 2.94 2.53 3.93 16.0 0.00 0.00 0.00 0.00 0 .7 8 0 3.64 6.14 0.00 0.00 0.180 329 0.00 3.43 0.00 1.03 0 .2 3 0 0.00 . 0.00 4.13 2.91 0.00 3.35 0.00 2.55 0.00 3.18 0.00 16.8 0.00 PFOSEA Dilution Factor 1 I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 PFOSEA Calc. Cone, ng/g 0.00 0.00 0.00 0.00 2.98 2.55 3.75 15.7 0.00 0.00 0.00 0.00 0.687 3.46 6.06 0.00 0.00 0.182 3.27 0.00 3.37 0.00 0.932 0.214 0.00 0.00 3.87 2 .5 4 0.00 3 .2 2 0.00 2.54 0.00 2.86 0.00 16.6 0.00 Filename A072800017 A072800018 A072800019 A072800020 A072800021 A072800024 A072800025 A072800026 A072800027 A072800028 A072800031 A072800032 A072800033 A072800034 A072800035 A072800038 A072800039 A072800040 A072800041 A072800042 A072800045 A072800046 A072800047 A072800048 A072800049 A072800052 A072800053 A072800054 A072800055 A072800056 A072800059 A072800060 A072800061 A072800062 A072800063 A072800066 A072800067 C o n cen tratio n o f PFOSEA ug/g or % Ree. <LOQ (0.0307 ug/g) <LOQ (0.0307 ub/ b! <LOQ (0.0307 ug/g) <LOQ (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LOQ (0.0307 ug/g) <LOQ (0.0307 ug/g) <LOQ (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <L O Q (0.0307 ug/g) <LOQ (0.0307 ug/g) <LOQ (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LOQ (0.0307 ug/g) <LO Q (0.0307 ub/b) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ub/ bI <LOQ (0.0307 ug/g) <LOQ (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LOQ (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) < L O O 0.0307 ub/ b) Mean PFOSEA Ug/g <LOQ < r.o n RSD Std Dev MS/MSDRPD NA NA NA NA Analytical Report: FACT-TOX-001 L R N -U 2103 FTS-R-7 0 3MEnvironmental Laboratory Page 275 3M M edical D epartm ent Study: T6316.1 AM D T# 092597.1 Covance# 6329-212 Study: Product Number(Test Substance): Matrix: M ethod/R evision: Analytical Equipment System N um ber Instrum ent Softw are/Version: Date o f Extraction/Analyst: Date o f Analysis/Analyst: Date o f Data Reduction/Analyst: Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Liver F ile n a m e : See Attachments ETS-8-6.Q & ETS-8-7.0 R-Squared Value: See Attachments Amelia 062498. Davey 070799 Slope: See Attachments Mas8Lynx 3.3 Y -I n te rc e p t : See Attachments 02/14/00,02/16/00 RWW/SAL 02/21/00, 02/29/00, 03/01/00, 03/03/00, 03/04/00, 07/28/00, 08/15/00 MMFLMEE/1AS 02/28/00, 03/01/00, 03/03/00, 03/06/00, 07/31/00, 08/17/00 IAS/MMH W E E K 105 R A T L IV E R G roup Dose S a m p le tt PFOS Calc. Cone, C o n c en tra tio n of PFOS ng/g u g/g o r % Ree. Group 3 C90842M 156858 157 M id Dose 30.0 mg/kg C90844M C90850M 42289 46376 42.3 46.4 C9085IM 120793 121 C90854M 179256 179 C90855M 73931 73.9 C90856M 16276 16.3 C90858M 131992 132 C90860M 337224 337 C90864M 122357 122 C90865M 74361 74.4 C90867M 102548 103 C90869M 42001 42.0 C 9087IM 90688 91 C90881M 42229 42.2 C90882M 79628 79.6 C90883M 38587 38.6 C90884M 61036 61.0 C90885M 102254 102 C90889M 36130 36.1 C90893M 58405 58.4 C90900M 26321 26.3 Group 3 C91252F 158371 158 M id Dose C91253F 100973 101 30.0 mg/kg C9I254F 217110 217 C91256F C91264F 161881 143127 162 143 C91278F 231922 232 C91279F 39747 39.7 C91286F 227867 228 C9I292F 48865 48.9 C91294F 117280 117 C91295F 22079 22.1 C91301F 84658 84.7 C91303F 166184 166 C91307F 56102 56.1 C91310F 126168 126 P rO s = Pertluorooctanesultonate PFOSA = Perfluorooctanesulfonamide PFOSAA = Perfluorooctanesulfonam idoacetate EtFOSE = Narrow Range N-Ethyl perfluorooctanesulfonamido ethyl alcohol M 556 = C 8 F 17 S 0 2 N ((H )C H 2 C 0 0 ) PFOSEA = Perfuorooctane sulfonyl ethylam ide Date Entered/Analyst: 03/14/00, 03/16/00, 03/17/00, 08/15/00,09/03/00 LAC Date V erified/Analyst: 03/09/01 hoj Purity Entered/V erified: 02/19/01 L A C M ean PFOS Ug/g 90.1 127 RSD S td Dev M S/M SD RPD 78.1 70.3 54.0 68.5 PFOSA Calc. Cone, ng/g 7349 3696 6514 6828 9569 10434 8293 6178 12569 9434 4441 5466 5521 8631 6403 7493 5439 10849 8430 6567 6949 6625 6992 7206 9190 7676 6251 8954 4670 9554 6960 7509 3266 5559 6664 5896 5242 C o ncentration of PFOSA ug/g or % Ree. 7.35 3 .7 0 6.51 6.83 9 .5 7 10.4 8 .2 9 6.18 12.6 9.43 4 .4 4 5 .4 7 5 .5 2 8.63 6.40 7.49 5 .4 4 10.8 8.43 6.57 6.95 6 .6 2 6 .9 9 7.21 9.19 7.68 6 .2 5 8.95 4.67 9.55 6.96 7.51 3 .2 7 5 .5 6 6.66 5.90 5.24- PFOSA UR/R 7.44 6.77 RSD Std Dev M S/M SD RPD 29.1 2.17 25.4 1.72 PFOSAA Calc. Cone, ng/g 5840 6967 10194 6845 36513 19689 10390 9279 11573 10854 4761 5093 12412 11794 6916 8486 5935 17002 17198 15569 8459 9694 5114 8009 8292 10693. 5070 12207 - 4729 17499 6906 9383 5143 4470 8525 7067 6657 C o n cen tratio n of PFOSAA ug/g o r % Ree. 5.84 6 .9 7 10.2 6 .8 5 36.5 19.7 10.4 9.28 11.6 10.9 4 .7 6 5.09 12.4 11.8 6.92 8.49 5 .9 4 17.0 17.2 15.6 8.46 9.69 5.11 8.01 8.29 10,7 5 .0 7 12.2 4 .7 3 17.5 6.91 9.38 5 .1 4 4.47 8.52 7 .0 7 6 .6 6 M ean PFOSAA Ug/g 11.4 7 OS RSD Std Dev M S/M SD RPD 60.8 6 .9 5 43.6 3.4? Analytical Report: FACT-TOX-001 L R N -U 2103 E tF O S E Calc. Cone. "R/R 95.3 16.6 39.3 158 39.6 97.0 32.9 65.2 80.0 75.2 135 81.2 75.7 48.8 58.0 155 48.8 73.3 218 47.7 79.9 0 .0 0 76.2 105 98.5 98.1 104 129 23.8 107 151 137 9 .5 4 59.4 122 88.4 23.3 C o n c en tra tio n ofEtFO SE ug/g o r % Ree. 0 .0 9 5 3 <LO Q (0.0614 ug/g) <LOQ (0.0614 ug/g) 0.158 <LOQ (0.0614 ug/g) 0.0970 <LOQ (0.0614 ug/g) 0.0652 0 .0 8 0 0 0 .0 7 5 2 0 .1 3 5 0.0812 0 .0 7 5 7 <LO Q (0.0614 ug/g) <LO O (0.0614 ub/ pI 0 .1 5 5 <LOQ (0.0614 ug/g) 0 .0 7 3 3 0 .2 1 8 <LO Q (0.0614 ug/g) 0.0799 <LOO (0.0614 ug/e) 0.0762 0 .1 0 5 0 .0 9 8 5 0.0981 0 .1 0 4 0.129 <LO Q (0.0614 ug/g) 0.107 0.151 0 .1 3 7 <LO Q (0.0614 ug/g) 0 .0 5 9 4 0.122 0.0884 <LCQ (0.0014 ug/g) M ean E tF O S E ug/g RSD Std Dev M S/M SD RPD 0 .0 8 8 3 47.1 0.0415 0 .1 0 2 8 26.9 O.C/2' 3M Environmental Laboratory Page 276 3M M edical D epartm ent Study: T6316.1 A M D T# 092597.1 Covance# 6329-212 Study: Product Number(Test Substance): M a tr ix : Method/Revjsion: Analytical Equipment System Number: Instrum ent Softw are/Version: Date o f Extraction/Analyst: Date o f Analysis/Analyst: Date o f D ata Reduction/Analyst: Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE-OH) Rat Liver ETS-8-6 0 & ETS-8-7.0 A m elia 062498, Davey 070799 MassLynx 3 3 02/14/00,02/16/00 RWW/SAL F i le n a m e : R-Squared Value: Slope: Y-Intercept: See Below See Attachments See Attachments See Attachments Box 00-012, 00-013 02/21/00, 02/29/00, 03/01/00, 03/03/00, 03/04/00, 07/28/00, 08/15/00 M M Il/M E E /IA S 02/28/00, 03/01/00, O3/O3/O0, 03/06/00, 07/31/00, 08/17/00 IAS/M M H W EEK 105 R AT L IV E R Group Dose Sample If Group 3 C90842M Mid Dose C90844M 30.0 mg/kg C90850M C908 51M C90854M C90855M C90856M C90858M C90860M C90864M C90865M C90867M C90869M C90871M C90881M C90882M C90883M C90884M C9088 5M C90889M C90893M C90900M Group 3 C91252F Mid Dose C91253F 30.0 mg/kg C91254F C9I256F C91264F C91278F C91279F C91286F C91292F C9I294F C91295F C91301F C91303F C91307F C91310F PFOS - Periluorooctanesulfonate M556 Calc. Cone. "g/R 10857 6798 8480 11631 16151 8603 4869 11618 15449 11779 7888 6286 7985 10364 6427 10500 5327 14760 12272 8025 7724 5398 9729 8473 15661 . 10275 6689 10199 4468 10051 9421 10286 2961 7474 12522 5325 5006 Concentration of M556 ug/g of % Re10.9 6,80 8 ,4 8 11.6 16.2 8 ,6 0 4.87 11.6 15.4 11-8 7 89 6,29 7,99 10.4 643 10.5 5 33 14.76 12.3 8,03 772 5 ,4 0 9,73 8,47 15.7 10.3 6 ,6 9 10.2 4,47 10.1 9.42 10.3 2.96 7,47 12-5 5,32 5,01 PFOSA = Perfluorooctanesulfonamide PFOSAA *=Perfluorooctanesulfonam idoacetate EtFOSE = N arrow Range N -Ethyl Perfluorooctanesulfonam ido ethyl alcohol M556 = C8F17S02N((H)CH2C00) PFOSEA = Perfuorooctane sulfonyl ethylamide Date Entered/Analyst: 03/14/00, 03/16/00,03/17/00, 08/15/00, 09/03/00 LAC Date Verified/Analyst: 03/09/01 hoj Purity Entered/V erified: 0 2 '19/01 LA C M556 "R/R 9.51 8 .5 7 RSD Std Dev MS/MSD RPD 34.6 3.29 38.8 3.33 PFOSEA Calc. Cone, ng/g 0.00 0.00 0.00 0.00 2 .9 8 2 .5 5 3 .7 5 15.7 0.00 0.00 0.00 0.00 0.687 3.46 6.06 0.00 0.00 0.182 3 .2 7 0.00 3.37 0.00 0.932 0.214 0.00 0.00 3.87 2.54 0.00 3.22 0.00 2.54 0.00 2.86 0.00 166 n rtn Concentration or PFOSEA ug/g or % Ree. <LO Q (0.0307 ug/g) <LOQ (0.0307 ug/g) <LOQ (0.0307 ug/g) <LOQ (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LOQ (0.0307 ug/g) <LOQ (0.0307 ug/g) <2.0Q (0.0307 ug/g) <LOQ (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.Q3O7 ug/g) <LOQ (0.0307 ug/g) <LO Q (0.0307 ug/g) <LOQ (0.0307 ug/g) <LOQ (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LOQ (0.0307 ug/g) <LO Q (0.0307 ug/g) <LOQ (0.0307 ug/g) <LOQ (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LOQ (0.0307 ug/g) <LOQ (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) <LOQ (0.0307 ug/g) <LOQ (0 0307 ug/g) <LO Q (0.0307 ug/g) <LO Q (0.0307 ug/g) ^ L C Q (0.0307 ug'g) Mean PFOSEA Ug/g <LOO <.O Q RSD Std Dev MS/MSD RPD NA NA NA NA Analytical Report: FACT-TOX-001 L R N -U 2103 3MEnvironmental Laboratory Page 277 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Study: Product NumbeifTest Substance): Matrix: Me thod' Re vi sion: Analytical Equipment System Number Instrument Software/Version: Date o f Extraction/Analyst Date o f Analysis/Analyst: Date o f Data Reduction/Analyst: Sample Data f04 Week Dietary Carcinogenicity Study with Narrow Range (98. IV.) N-Ethy! Perfluorooclanesulfonatmdo Ethanol in Rata T-6316 (EtFOSE-OH) Rat Liver ETS-8-6.0 & ETS-8-7.0 Soup 020199, Amelia 062498 MassLynx 3.3 02/14/00,02/16/00,03/15/01 RWW'SAL'KJS 02/21/00,02'29/00,03'01 '00.03/03/00,03-04/00, 4/28/00,08/01/00,08'14 00,0815 00, 03/22/01 MMH MEE/IAS 02/28-DO, 03/01/00.03 3/00.03/06/00,5 3/00, 54/00, 0802/00,08/15 00.08/17 00.0323/01 IASMMH Filename: See Below R-Squared Value: See Attachments Slope: See Attachments Y-Intercept See Attachments Bex 00-012,00-013 WEEK 105 RAT LIVER _________ ___________________ Lot 171 Dote Group 4 Mid-High Dose 100 mg/kg Group 4 Mid-High Dose 100 mg/kg C90904M C90908M C909I0M C909I1M C90916M C90926M C90927M C90928M C90933M C90944M C90947M C90948M C90953M C90955M C90956M C90965M C90968M C91315F C91324F C91327F C9I332F C91335F C9I336F Initial W t 8 1.0750 1.0601 1.0130 0.9883 0.9913 1.0448 1.0776 1.0152 1.0884 0.9935 1.0069 0.9872 1.0290 1.0011 1.0111 0.9962 1.(563 0.9933 0.9989 0.9827 1.1502 1.1177 1.0214 Tatal Mass of Liver X NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOS Std Correction Factor 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 1.0000 0.9275 0.9275 0.9275 0.9275 1.0000 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 0.9275 PFOS Purity Correction Factor 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 1.0000 0.8640 0.8640 0.8640 0.8640 1.0000 0.8640 0.8640 0.8640 0.8640 0.8640 0.8640 0.3640 0.3640 Surrogate Verified NA NA NA NA NA NA NA NA NA High, Not Confirmed NA NA NA NA High, Not Confirmed NA NA NA NA NA NA NA NA PFOS Cene. o%l* 867 829 250 886 584 313 70.6 796 416 561 742 460 155 663 407 857 642 570 635 778 542 614 841 PFOS Dilution Fa c to r 500 500 500 1000 500 500 500 1000 500 1000 500 500 500 500 500 1000 1000 500 1000 50 1000 500 500 PFOS Cak- Cette, ng/g 323257 313374 98979 718021 236132 120112 26240 628332 153299 565043 295355 186556 60324 265167 201182 689313 445034 230009 509159 31737 377842 220157 329837 Filename A030I0004I A030100044 A030100045 A041200037 A03010004 A030100048 A030100051 A041200038 A030100053 A010322030 A030I00055 A0301000S8 A030100059 A030100060 A010322035 A041200040 A041200041 A030100016 A041200029 A030I00093 A041200030 A030100020 A030100023 Cencentratien of PFOS Uf/f e r % Ree. 323 313 99.0 718 236 120 26.2 628 153 565 295 187 60.3 265 201 689 445 230 509 31.7 378 220 330 C91338F 0.9986 NA 0.9275 0.8640 NA 851 500 341389 A030100024 341 C91340F 1.0204 NA 0.9275 0.8640 NA 738 1000 579769 A041200031 580 C91341F 1.0345 NA 0.927S 0.8640 NA 626 500 242581 A030I00026 243 C91342F 1.0056 NA 0.9275 0.8640 NA 891 500 355109 A030100027 355 C9I356F 1.0115 NA 0.9275 0.8640 NA 214 250 42389 A041200045 42.4 C91357F C91360F C91361F C91362F C91372F C91376F C91378F C91380F 0.9988 1.0132 0.9998 1.0130 0.9926 1.0544 1.0032 0.9840 NA 0.9275 0.8640 NA 0.9275 0.8640 NA 0.9275 0.8640 NA 0.9275 0.8640 NA 0.9275 0.8640 NA 0.9275 0.8640 NA 0.9275 0.8640 NA 0.9275 0.8640 NA 481 500 192963 A030100031 193 NA 522 500 206612 A030100032 207 NA 889 . 1000 712319 A04120032 712 NA 220 500 86896 A030100034 86.9 NA 639 500 257883 A030I00037 258 NA 668 500 253932 AQ3010003R 254 NA 853 500 340658 A03010039 341 NA 797 500 324616 A030100040 325 Greup 6 C91047M 0.9884 NA 0.9275 0.8640 NA 251 10 2034 A08I500102 2.03 Mid-High Dose C9I054M 1.0156 NA 0.9275 0.8640 NA 251 1 198 A042800044 0.198 Recovery C9I056M 1.0019 NA 0.9275 0.8640 Low, not Confirmed 131 100 10494 A081500105 10.5 100 mg/kg C9I060M C91065M C91070M C9107IM 1.0062 0.9918 0.9943 0.9973 NA 0.9275 0.8640 NA 0.9275 0.8640 NA 0.9275 0.8640 NA 0.9275 . 0.8640 NA 252 10 2006 A081500106 2.01 NA 45.2 1 36.5 AO428OO017 0,0365 NA 254 1 205 A042800018 0.205 NA 51.2 1 41 1 Aru'/anrvno nim i Greup 6 Mid-High Dose Recovery 100 mg/kg C91072M C91073M C91076M C91451F C91453F C91455F C91459F C91462F C91467F C91473F C91479F C91480F C91485F C9I487F C9I488F 0.9986 1.0016 1.0102 1.0161 1.0133 1.0117 1.0140 1.0082 1.0130 0.9879 1.0018 0.9882 0.9812 1.0175 1.0101 NA 0.9275 0 8640 NA 479 NA 0.9275 0.8640 NA 104 NA 0.9275 0.8640 High. Not Confirmed 633 NA 0.9275 0.8640 Low. not Confirmed 195 NA 0.9275 0.8640 NA 572 NA 0.9275 0.8640 Low, not Confirmed 237 NA 0.9275 0.8640 NA 62.6 NA 0.9275 0.8640 Low. not Confirmed 221 NA 0.9275 0.8640 NA 174 NA 0.9275 0.8640 Low, not Confirmed 171 NA 0.9275 0.8640 NA 25.8 NA 0.9275 0.8640 NA 183 NA 0.9275 0.8640 low , not Confirmed 253 NA 0.9275 0.8640 NA 79.7 NA 0.9275 0.8640 Low, not Confirmed 143 I 384 A042S00022 1 83.1 A042S00023 10 5025 A010322065 100 15396 A030400022 10 4525 A081500107 100 18803 A030400024 1 49.4 A042800030 100 17533 A030400026 1 137 A042300032 100 13901 A030400030 20.7 A0i'?fWW. 1 149 A042800037 50 10329 A081500108 I 62.8 A042800039 100 . 11369 A030400037 0.384 0.0831 5.02 15.4 4.53 18.8 0.0494 17.5 0.137 13.9 0.149 10.3 0.0628 11.4 PFOS = Perfluorooctaneaulfonale tt Value estimated, above the range o f the calibration curve. LAC 03/14/01 PFOSA " Periluorooctaneaulfonamide * Data may be biased high as CCVs weren't within criteria. LAC 03/14/01 PFOSAA - Perfluorooctanesulfonamidoaceiate . EtFOSE Narrow Range N-Elhyl Perttuorooclanesulfcnamido ethyl alcohol A * Sample was extracted 03/15/01, analyzed 03/22/01, and the PFOS concentration reported from 03/15/01 extraction. LAC 03/26/01 M5S6 - C8FI7S02N{(H)CH2COO) . PFOSEA Perfuorooctane sulfonyl ethylamide Date Entered'Analyst: 03 14 00,03/16/00,03/17 00, 05 05 00,05 18/00, 0815 00, 08/21/00,09 03/00, 03 26 01 LAC'CSH/MMH Dale VerifiedAnalyst: O3 O9,01 boj Purity Entered'Verified: 02/19/01 LAC Corrected PFOS LOQ (0.0306 ugg) to include sid correction factors new LOQ is 0.0245 ugg. LAC 02/19.01 Analytical Report: FACT-TOX-001 L R N -U 2103 PFOS RSD Std Dev MS/MSD RPD A A 313 70.4 220 57.7 297 171 164 2.05 3 36 99.0 7.69 7.62 3MEnvironmental Laboratory Page 278 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Study: Product NumbetfTest Substance): Matrix: Method/Revision: Analytical Equipment System Number Instrument Software/Version: Date ofExtraction;Analyst Oste o f Analysis/Analyst Dale o f Data Reduction/Analyst Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98. !*/) N-Ethyl Periluorooclanesulfonamido Ethanol in Rats T-6316 (EtFOSE*0H) Rat Liver Filenaine: See Below ETS-8-6.0 & ETS-8-7.0 R-Squared Value: See Attachments Soup 020199, Amelia 062498 Slope: SeeAttachments MassLynx 3.3 Y-lntercept SeeAttachments 02/14/00, 02/16/00, 03/15/01 RWW/SAL'KJS Box00-012, 00-013 02/21/00,02/29/00, 03 '01/00,03/03/00, 03/0400,4.2800,0801/00,08/14/00,08/15/00,03/22/01 MMH/MEE/IAS 02/28/00,0301/00,03/03/00,03/0600, 5/3/00, 5/4/00, 08/0200,08 15/00, 08/17/00,03/2301 1AS/MMH WEEK1QS RAT LIVER ____ lotH5709 ______________________________________________ ________________ _______ lotT-7121.l Group Dose Group 4 Mid-High Dose 100 mglcg Group 4 Mid-High Dose 100 mg/kg Group 6 Mid-High Dose Recovery 100 mglcg Groins 6 Mid-High Dose Recovery 100 mg/kg Sample V C90904M C90908M C90910M C909I1M C909I6M C90926M C90927M C90928M C90933M C90944M C90947M C90948M C90953M C90955M C90956M C90965M C90968M C91315F C91324F C91327F C91332F C9I335F C91336F C91338F C91340F C9I34IF C9I342F C9I356F C91357F C91360F C9136IF C9I362F C9I372F C91376F C91378F C91380F C91047M C91054M C91056M C91060M C91065M C91070M C9I071M tyto/2M C91073M C91076M C91451F C91453F C914S5F C91459F C91462F C91467F C91473F C91479F C91480F C9I485F C91487F PFOSA Purity Correction Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOSA Cone. ng/g 316 316 251 367 353 84.9 249 358 288 299 198 186 206 291 176 407 384 254 324 209 392 325 305 361 329 316 338 125 336 364 446 220 386 344 380 303 2.14 2.50 43.0 1.84 2.72 1.78 2.52 2.67 0.85 1.76 1.66 1.31 2.46 0.380 2.51 2.71 2.30 1 62 0.870 2,21 0.910 PFOSA Dilution Factor 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 SO 50 50 50 50 50 50 50 50 50 50 1 1 1 1 1 1 1 1 I 1 1 1 1 1 1 1 1 l 1 1 PFOSA Calc. Cene. n*/* 14679 14920 12376 18544 17812 4061 11539 17644 13218 15070 9823 9411 10031 14511 8680 20448 16616 12800 16226 10627 17062 14551 14949 18058 16126 15274 16810 6157 16831 17955 22322 10883 19454 16296 18952 15385 2.17 2.46 42.9 1.83 2.74 1.79 2.53 2.67 0.849 1.74 1.63 1.29 2.43 0.375 2.49 2.68 2.33 1.62 0.880 2.25 0.894 2.94 Filename A030100066 A030100067 A030100068 A030I00069 A030I00072 A030100073 A030100074 A030I00075 A030100076 A030100079 A030100080 A030100081 A030I00082 A 0 3 0 100083 A030100086 A030100087 A030100088 A030100089 A030100090 A030100093 A030100094 A030100095 A030100096 A030100097 A030100IOO A030I00I01 A030I00102 A030100103 A030100104 A030100107 A030100I08 A030100109 A030I001IO A030100111 A030100114 A030100115 A042800043 A04280044 A042800015 A042800016 A042800017 A042800018 A042800019 A042B00022 A042800023 A042800024 A042800025 A042800026 A042800029 A042800030 A042800031 A042800032 A042800033 A042800036 A042800037 A042800038 A042800039 A042800040 Concentration of PFOSA ug/g or % Ree. 14.7 14.9 12.4 18.5 17.8 4.06 11.5 17.6 13.2 15.1 9.82 941 10.0 14.5 8.68 20.4 16.6 12.8 16.2 10.6 17.1 14.6 14.9 18.1 16.1 15.3 16.8 6.16 16.8 18.0 22.3 10.9 19.5 16.3 19.0 15.4 <LOQ (0.00614 ug/g) <LOQ (0.00614 ug/g) 0.0429 <LOQ (0.00614 ug/g) <LOO (0.00614 up/el <LOO(0.00614 ue/e) <LOQ(0.00614 ug/g) IDO (0.00614 up/pi <LOO (0.00614 ue/e) <100(0.00614 ue/e) <LOO (0.00614 ue/e) <LOQ (0.00614 ue/e) <LOO (0.00614 ue/e) <LOQ(0.00614 ue/e) <LOQ (0.00614 ue/e) <LOO (0.00614 ue/e) <LOO (0.00614 ub/b) <IOO (0.00614 .e/) <LOO (0.00614 ue/e) <LOO(0.006UueVi <LOQ (0.00614 ug/g) <LOQ (0.00614 ug/g) PFOSA "*/ 13.5 15.6 <LOQ <LOQ RSD Sid Dev MS/MSD RPD 31.3 4.23 23.1 3.61 NA NA NA NA PFOSAA Purity C o r r e c li e n Fa c to r Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown PFOS = Perfluorooctanesulfooate tt Value estimated, above the range of the calibration curve. LAC 03/1401 PFOSA Periluorooctanesulfonamide * Data may be biased high as CCVs weren'twithincriteria. LAC03/14/01 PFOSAA Perfluorooctanesulfonaiiudoacelale EtFOSE - Narrow Range N-Ethyl Rerfluorooctanesulfonamido ethyl elcohol A = Sample was reextracted 03/15/01, analyzed 032201, and the PFOS concentration repotted from 03/15/01 extraction. LAC 0326/01 M556 = C8F17SO2N((H)CH2CO0) PFOSEA = Perfuorooctane sulfonyl elhylamide Dale Entered/Analyst 03/14/00, 03/16/00, 03/17/00,05/05/00, 05/1M 3, 08 1 5/00, 0821/00,09/03/00,03 26/01 LAC/CSH/MMH Date VeriRed/Analysi: 03/09/01 hoj Purity Entered/Veritied: 0219/01 LAC Corrected PFOS LOQ (0.0306 ug g) to include std correction factors new LOQ is 0.0245 ug g. LAC 0219/01 Surrogate Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA PFOSAA Cone. n/| 459 392 909 696 475 37.3 333 819 403 457 358 226 377 548 95.5 1031 622 314 564 758 585 408 402 418 537 524 673 349 413 577 631 608 840 $78 604 604 217 19.8 74.7 44.8 28.6 19.0 411 30.0 21.8 20.3 0.00 0.00 0.00 0.00 0.00 0.00 0.00 C.OC 11.1 7.07 0.00 . 13.1 PFOSAA Dilution F a c to r 50 50 50 50 50 $0 $0 50 50 50 50 50 50 $0 $0 $0 50 50 50 $0 50 $0 50 50 50 50 50 0 50 50 50 $0 50 50 50 $0 l 1 1 1 l 1 ! 1 I 1 1 1 1 1 1 1 1 1 1 1 Analytical Report: FACT-TOX-001 L R N -U 2103 PFOSAA Calc. Cone, n/* 21358 18476 44847 35222 239*8 1784 15462 40328 18511 23008 17773 11445 18340 27358 4725 51758 26905 15794 28252 38590 25423 18251 19676 20954 26299 25334 33469 17230 20686 28490 31554 30022 42332 27417 30114 30712 220 19.5 74.5 44.5 28.9 19.1 12 S 30.1 21.8 20.1 0.00 0.00 0.00 0.00 0.00 0.00 0.00 . 11.2 7.21 0.00 12.9 Filename A030100066 A030100067 A030100068 A030I00069 A030I00072 A030100073 A030I00074 A030100075 AO3O10OO76 A030100079 A030100080 A03Q100081 A030I00082 A030100083 A030100086 A030100087 A030100088 A030100089 A030100090 A030100093 A030100094 A030100095 A030100096 A030I00097 A030100100 A030100101 A030100102 A030100103 A030100104 A030100107 A030100108 A030100109 A030100110 A030100111 A030I00114 A030100115 A042800043 A042800044 A042800015 A042800016 A042R00017 A042800018 A042800022 A042800023 A042800024 A042800025 A042800026 A042800029 A042800030 A042800031 A042800032 A042800033 480WJ6 A042800037 A042800038 A042800039 A042800040 Cencentratien of PFOSAA ug/g or % Ree. 21.4 18.5 44.8 35.2 23.9 1.78 15.5 40.3 18.5 23.0 17.8 11.4 18.3 27.4 4.72 51.8 26.9 15.8 28.3 38.6 25.4 18.3 19.7 21.0 26.3 25.3 33.5 17.2 20.7 28.5 31.6 30.0 42.3 27.4 30.1 30.7 0.220 0.0195 0.0745 0.0445 0.0289 0.0191 ".ii: 0.0301 0.0218 0.0201 <LOQ (0.0123 ug/g) <LOQ (0.0123 Ug/g) <LOO (0.0123 ub/b) <LOQ (0.0123 ug/g) <LOQ (0.0123 ug/g) <LOQ (0.0123 ug/g) <LOQ (0.0123 ug/g) <LOQ (0.0123 ug/g) <LOQ (0.0123 ug/g) <LOQ (0.0123 ug/g) <LOQ (0.0123 ug/g) <LOQ(0.0123 ug/g) PFOSAA >*/ 23.6 26.9 0.0522 <LOQ RSD Std Dev MS/MSD RPD 56.5 13.3 7.08 118 0.0614 NA NA 3MEnvironmental Laboratory Page 279 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Study: Product NumbeflTest Substance): Matrix: Meth o d R e vision: Analytical Equipment System Number Instrument Softwatc/Vcrrion: Date ofExtraction/Analyst: Data of Analysis/Analyst: Date of Data Reduction/Analyst: Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Etbyl Perfluorooctanesulfonamido Ethanol in Rats T-6316 (EtFOSE*OH) Rat Liver Filename: See Below ETS-8-6.0 & ETS-8-7.0 R-Squared Value: See Attachments Soup 020199, Amelia 062498 Slope: See Attachments MassLynx 3.3 Y-Intarcept See Attachments 02/14/00, 02/16/00,03.1S/0! RWW'SALKJS Box 00-012, 00-013 02/21/00, 02 79/00, 03/01 00, 03 03/00, 03/04/00, 4.78/00,08/01/00,08/14/00, 08/15/00,0372/01 MMH/MEE/LAS 02 28.00,03/01/00, 03/03/00,03WOO, 57/00,5/4/00, 08/02/00. 08/15/00,08.17/00, 0323/01 IAS/MMH WEEK IQS RAT LIVER lotUnknown ___________ ______________________________ Greup Dare Group 4 Sample f C90904M EtFOSE Purity Correction Factor Unknown Surrogate Verified NA EtFOSE Cene. 1*/ 469 EtFOSE Dilution Fa c to r l EtFOSE Calc. Cone. n*'* 437 Filename A080100017 Concentratlen o f EtFOSE ug/g or % Ree. 0.437 EtFOSE Uf/t RSD Std Dev MS/MSD RPD Mid-High Dose C90908M Unknown NA 293 1 276 A0801000I8 0.276 100 mg/kg C90910M Unknown NA 833 1 823 A080I00019 0.823 C90911M Unknown NA 464 1 470 A080I00020 0.470 C90916M Unknown NA 331 1 334 A080100021 0.334 C90926M Unknown NA 0.00 1 0.00 A080100024 <LOO (0.0614 ue/e) C90927M Unknown NA 313 l 291 A080100025 0.291 C90928M Unknown NA 314 l 309 A080100026 0.309 C90933M Unknown NA 363 l 334 A080100027 0.334 C90944M Unknown NA 321 1 323 A080I00028 0.323 C90947M Unknown NA 310 1 308 A080I0003I 0.308 C90948M Unknown NA 232 1 235 A080I00032 0.235 C90953M Unknown NA 213 l 207 AQ8010033 0.207 C90955M Unknown NA 466 1 466 A080100034 0.466 C90956M Unknown NA 314 1 310 A080I00035 0.310 C90965M Unknown NA 1020 1 1024 A080I00038 1.02 57.8 Group 4 Mid-High Dose C90968M C91315F C91324F Unknown Unknown Unknown NA NA NA 594 439 377 1 514 AOSOI00039 0.514 0.395 0.229 1 442 A080I00040 0.442 2 755 AQ815Q0Q98 0.755 100 mg/kg C91327F Unknown NA 274 l 279 A080100042 0.279 C91332F Unknown NA 496 1 432 A080100045 0.432 C91335F Unknown NA 776 2 1389 A08I500099 1.39 C91336F Unknown NA 479 1 469 A080100047 0.469 C91338F Unknown NA 916 1 917 A080I00048 0.917 C91340F Unknown NA 416 1 408 A080100049 0.408 C9I341F Unknown NA 746 1 721 A080100052 0.721 C9I342F Unknown NA 782 1 777 A080100053 0.777 C91356F Unknown NA 184 1 182 A080I00054 0.182 C91357F Unknown NA 842 l 843 A080100055 0.843 C91360F Unknown NA 611 10 6034 A081500100 6.034 C91361F Unknown NA 1106 1 1106 A080100059 1.11 n C9I362F Unknown NA 213 1 211 A080100060 0.211 C91372F Unknown NA 518 l 522 A080I00061 0.522 C91376F Unknown NA 774 1 734 A080I00062 0.734 C91378F C91380F Unknown Unknown NA NA 1062 549 2 2117 A030400085 2.12 * 131 1 557 A080100066 0.557 0.994 1.30 Group 4 C91047M Unknown NA 0.00 1 0.00 A081400028 LOQ (0.0614 ug/g) Mid-High Dose C91054M Unknown NA 0.00 1 0.00 A081400029 LOQ (0.0614 ug/g) Recovery C91056M Unknown NA 0.00 1 0.00 A081400030 LOO (0.0614 ue/c) 100 mg/kg C9I060M Unknown NA 0.00 C91065M Unknown NA 0.00 C91070M Unknown NA 0.00 C91071M Unknown NA 0.00 1 0.00 A081400031 LOQ (0.0614 ug/g) 1 0.00 A081400034 LOQ (0.0614 ug/g) 1 0.00 A081400035 LOQ (0.0614 ug/g) 1 0.00 A08I400036 LOO (0.0614 ue/e) Wxnuwn ISA u.uu I 0.00 A081400037 LOO (0.0614 ueV) C91073M Unknown NA 0.00 1 0.00 A08I400038 LOO (0.0614 ue/e) NA C91076M Unknown NA 0.00 1 0.00 A081400041 LOO (0.0614 ue/e) <LOO NA Group 6 C91451F Unknown NA 0.00 1 0.00 A081400042 LOO (0.0614 ue/e) Mid-High Dose C91453F Unknown NA 0.00 1 0.00 A081400043 LOO (0.0614 uv,VI Recovery C91455F Unknown NA 0.00 1 0.00 A081400044 LOO (0.0614 ue/e) 100 mg/kg C91459F Unknown NA 0.00 C91462F Unknown NA 0.00 C91467F Unknown NA 0.00 1 0.00 A08I400045 LOO (0.0614 ue/e) 1 0.00 A081400048 LOO (0.0614 ue/e) 1 0.00 A081400049 LOO (0.0614 ue/e) C91473F Unknown NA 0.00 1 0.00 A081400050 <LOO (0.0614 ueV) C91479F Cyi4HUP C91485F C91487F Unknown Unknown Unknown Unknown Unknown NA NA NA 0.00 0.00 0.00 1 0.00 A081400027 LOO (0.0614 ue/g) 1 0.00 A08I400051 <LOQ (0.0614 ug/g) 0.00 A081400052 <LOQ (0.0614 ug/g) 1 0.00 A081400055 <LOQ (0.0614 ug/g) NA 1 0.00 A0814000S6 .LOQ (0.0614 u*/r) <LOQ NA PFOS = Perfluorooctanesulfonate AValue estimated, above the range o f the calibration curve. LAC 03/14/01 PFOSA Perfluorooctanesulfonamide * Data may be biased high as CCVs weren'twithin criteria. LAC 03/14^01 PFOSAA = Perfluorooctanesulfonaimdoacctata A - Sample was reextractad 03/15/01, analyzed 0372/01, and the PFOS concentration reported from 03/15/01 extraction. LAC 0376/01 ElFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonamido ethyl alcohol M556 = C8FI 7SQ2N((H)CH2COO). PFOSEA = Perfuorooctane sulfony! ethylamide Data Entered/Analyst: 03/14/00,03'I6/00, 03/17'00,05/05/00,05'18/00,08/15 '00, 087 1 00, 09/03'00, 0376/01 LAC'CSH/MMH Data Verified/Analyst 03 09/01 hoj Purity EnteretWerified: 02/19/01 LAC lotNB113047-80 M556 Purity Correction Fa c to r Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown 1mVnnwn Unblown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Surroga te Verified NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Corrected PFOS LOQ (0.0306 ug/g) to include std correction factors new LOQ is 0.0245 ug/g. LAC 02/19/01 Analytical Report: FACT-TOX-001 L R N -U 2103 M55* Cene. /* 623 633 619 648 642 177 500 626 553 547 351 510 420 727 188 887.7 866.6 457 655 193 740 552 553 614 636 542 839 228 536 07 889 480 789 717 475 656 2.70 3.18 0.00 0.00 0.00 0.00 000 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.36 000 4.62 1.21 2.96 M556 Dilution F a c to r 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 $0 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 l 1 1 1 I 1 1 1 1 1 1 1 1 1 1 1 1 1 1 M556 Calc. Cene, ng/f 28960 29855 30567 32781 3239 8469 23216 30818 25401 27552 17406 25822 20389 36299 9313 44554 37472 22980 32766 9807 32164 24677 27071 30744 31154 26187 41708 11248 26842 25014 44467 23712 39723 33977 23656 33352 2.73 3 13 0.00 0.00 0.00 0.00 0 00 0.00 0.00 0.00 0.00 0.00 0,00 0.00 0.00 0.00 0.00 1.36 0.00 4.71 1.19 2.93 Filename A030100066 A030100067 A030100068 A030100069 A030100072 A030100073 A030100074 A030100075 A030100076 A030100079 A030100080 A030100081 A030100082 A030I00083 A0301000S6 A030100087 A030100088 A030100089 A030100090 A030100093 A030100094 A030I00095 A030100096 A030100097 A030100100 A03010010I A030IO0IO2 A030I00103 A030100104 A030100107 A030100108 A030100109 A030I00110 A030100111 A030100I14 A030100115 A081400028 A081400029 A0428000I5 A042800016 A042800017 A042800018 "'-'Win A0428D0022 A042800023 A042800024 A04280002S A042800026 A04280Q029 A042800030 A042800031 A042800032 A042800033 mii14iiuii77 A081400051 A08I400052 A081400055 A081400056 Cencentratien of MS54 ug/g o r % Ree. 29.0 29.9 30.6 32.8 32.4 8.47 23.2 30.8 25.4 27.6 17.4 25.8 20.4 36.3 9.31 44.6 37.5 23.0 32.8 9.81 32.2 24.7 27.1 30.7 31.2 26.2 41.7 11.2 26.8 25.0 44.5 23.7 39.7 34.0 23.7 33.4 <LOQ (0.00615 ug/g) <LOQ (0.00615 ug/g) <LOQ (0.123 ug/g) <LOQ (0.123 ug/g) <LOQ (0.123 ug/g) <LOQ(0.123 ug/g) <LOQ (0.123 ug/g) LOLM0.UU6IS u/e) LOQ (0.0061S ug/g) <LOO (0.00615 ue/e) <LOQ (0.00615 ug/g) <LOQ(0.006!5ue/R) MSS4 27.1 28.5 <LOO <LOQ RSD Std Dev MS/MSD RPD 34.7 941 8.86 NA NA 3MEnvironmental Laboratory Page 280 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Study: Product NumbeifTest Substance): Matrix: Meth odR e vision: Analytical Equipment System Number Instrument Software/Venion: Date o f Extraction'Analyst Date o f Analysis'Analyst Date o f Data Reduction/Analyst: Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1H) N-Ethyl Periluorooclanesutfonamido Ethanol in Rats T-63I6 (EtFOSE-OH) Rat Liver Filename: See Below ETS-8-6.0&ETS-8-7.0 R-Squared Value: See Attachments SoupO20l99,Amelii062498 Slope: See Attachments MossLynx 3 3 Y-Intercept: See Attachments 02/14/00.02 16/00,03/15/01 RWW/SAlVKJS Box 00-012, 00-013 02/21/00.0229/00,03/01/00,03/03/00, 03/04/00, 4 28/00, 08/01/00.08/14/00, 08/15/00, 03/22/01 MMH/MEE/1AS 02 28/00,03.01/00, 03/03/00,03'06/00, 5'3'00, 5'4'00,08'02'00, 08/15/00,08/17/00, 0323/01 IAS/MMH WEEK 105 RAT LIVER _______ lot 529 Sample # PFOSEA Purity Surrogate PFOSEA PFOSEA PFOSEA Filena me Ceneentratlen RSD Date CorreeOan Verified Cene. Dilutlen Calc. Cone. ofPFOSEA PFOSEA Std Dev Fictar */* Factor n*/f ug/g o r % Ree. u*/* MS/MSD RPD Group 4 Mid-High Dose 100 mg'ltg C909O4M C90908M C909I0M C90911M C90916M Unknown Unknown Unknown Unknown Unknown NA 0.00 1 0.00 A080100017 <LOQ (0.0123 ug/g) NA 21.7 1 20.5 A080100018 0.0205 NA 34.1 1 33.7 A080I00019 0.0337 NA 0.00 1 0.00 A080100020 <LOQ (0.0123 ug/g) NA 2.39 1 2.41 A080I00021 <LOQ(0.0123 ug/g) C90926M Unknown NA 50.4 1 48.3 A080100024 0.0483 C90927M Unknown NA 3.75 1 3.48 A080100025 <LOQ (0.0123 ug/g) C90928M C90933M C90944M Unknown Unknown Unknown NA 31.1 1 30.7 A030100026 0.0307 NA 31.7 l 29.1 A080I00027 0.0291 NA 54.4 1 54.8 A080I00028 0.0548 C90947M C90948M C90953M Unknown Unknown Unknown NA 0.00 1 0.00 A080I0003I <LOQ (0.0123 ug/g) NA 26.0 1 26.3 A080100032 0.0263 NA 0.00 0.00 A080100033 <LOQ (0.0123 ug/g) C90955M Unknown NA 0.00 0.00 A080100034 <LOQ (0.0123 ug/g) C90956M Unknown NA 117 115 A080100035 0.115 C90965M Unknown NA 235 1 236 A080100038 0.236 139 Group 4 C90968M C91315F Unknown Unknown NA 3.03 1 2.62 A080100039 <LOQ (0.0123 ur/r) 0.0408 0.0566 NA 57.8 1 58.1 A080100040 0.0581 Mid-High Dose 1 0 0 mg'ltg C91324F C91327F Unknown Unknown NA 32.7 NA 32.7 32.7 A080100041 33.3 A080100042 0.0327 0.0333 C91332F Unknown NA 2.34 2.03 A080100045 <LOQ (0.0123 ug/g) C91335F Unknown NA 4.61 4.12 A080100046 <LOQ (0.0123 ug/g) C91336F Unknown NA 10.7 1 I0.S A080100047 <LOQ (0.0123 ug/g) C91338F Unknown NA 13.0 1 13.0 A080100048 0.0130 C91340F Unknown NA 24.9 24.4 A080100049 0.0244 C9134IF Unknown NA 10.7 1 10.3 A080100052 <LOQ (0.0123 ug/g) C91342F Unknown NA 10.9 10.8 A080100053 <LOQ (0.0123 ug/g) C9I356F Unknown NA 56.7 56.0 A080100054 0.0560 C9I357F Unknown NA 11.5 1 11.5 A080100055 <1.00(0.0123 ur/c) C9I360F C9136IF Unknown Unknown NA 25.6 1 25.2 A080100056 0.0252 NA 23.2 l 23.2 A080100059 0.0232 C91362F Unknown NA 2.86 1 2.82 A080100060 <LOQ (0.0123 ug/g) C91372F Unknown NA 26.6 26.8 A080100061 0.0268 C91376F C9I378F C91380F Unknown Unknown Unknown NA 25.6 24.3 A080100062 0.0243 NA 28.7 1 28.6 A080I00063 0.0286 57.6 NA 25.6 l 26.0 A080100066 0.0260 0.0241 0.0139 Group 6 C9I047M Unknown NA 0.00 1 0.00 A0428OQO43 <lO O (0.0307 u/*\ Mid-High Dose C91054M Unknown NA 0.00 1 0.00 A042800044 <LOQ (0.0307 ug/g) Recovery 100 mg'ltg C910S6M C91060M C91065M Unknown Unknown Unknown NA 0.00 0.00 A042800015 <LOQ (0.0307 ug/g) NA 0.00 0.00 A042800016 <1.00 (0.0307 uv/v) NA 0.00 1 0.00 A042800017 <LOO (0.0307 ufi/el Group 6 Mid-High Dose Recovery 100 mg/fcg C91070M C91071M C9I072M C9I073M C91076M C91451F C9I453F C91455F C91459F C91462F Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown Unknown NA 0.00 1 NA . 0.00 1 NA 0.00 1 NA 0.00 1 NA 0.00 NA 0.00 NA 0.00 1 NA 0.00 1 NA 0.00 1 NA 0.00 1 0.00 A0428000I8 <LOO (0.0307 u r /il 0.00 A0428000I9 < 1 0 0 (0 0707 ue/ei 0.00 A042800022 <LOQ (0.0307 ug'g) 0.00 A042800023 <LOQ (0.0307 ug/g) 0.00 A042800024 <LOO (0.0307 ur/r) <LOO 0.00 A042800025 <LOQ (0.0307 ug/g) 0.00 A0428OO026 <LOQ (0.0307 ug'g) 0.00 A0428OOO29 <LOQ (0.0307 ug/g) 0.00 A042800030 <LOQ (0.0307 ug/g) 0.00 A042800031 <LOQ (0.0307 ug/g) NA NA C91467F Unknown NA 0.00 1 0.00 A042800032 <LOQ (0.0307 ug/g) C91473F C91479F C9I480F C91485F Unknown Unknown Unknown Unknown NA 0.00 0.00 A042800033 <LOQ (0.0307 ug/g) NA non 0.00 A04280003S <!(>0!u<nr!? NA 0.00 1 0.00 A042800037 <LOQ (0.0307 ug/g) NA 0.00 1 0.00 A042800038 <LOO (0.0307 uff/pi C91487F C91488F Unknown Unknown NA 0.00 l 0.00 A042800039 <1.00(0.0307 uv/pi NA NA 0.00 l 0.00 A042800040 <LOQ (0.0307 ug/g) <LOQ NA PFOS = Perfluorooctanesulfonate # Value estimated, above the range o f the calibration curve. LAC 03/14/01 PFOSA - Perfluorooctanesulfonamide ** Data may be biased high osCCVs weren't within criteria. LAC 03/14/01 PFOSAA * Periluorooctanesulfonamidoacetate A = Sample was reextracled 03 15 01, analyzed 0322/01, and the PFOS concentration reported from 03/15/01 extraction. LAC 03/26/01 EtFOSE = Narrow Range N-Ethyl Perfluorooctanesulfonairrido ethyl alcohol M556 = C8FI7S02N{(H)CH2COO). PFOSEA Perfuorooctane sulfonyl ethyiamide Date Entered/Analyst 03/14/00,03/16/00, 03 17'00.05/05/00,05/18/00, 08/15/00, 0821 '00,09/03/00,03/26/01 LAC/CSH'MMH Date VerifiedAnalyst 03/09/01 hoj Purity Entered'Verified: 02 19/01 LAC Corrected PFOS LOQ (0.0306 ug'g) to include sld correction factors new LOQ is 0.0245 ug/g. LAC 02 19/01 Analytical Report: FACT-TOX-001 L R N -U 2103 3MEnvironmental Laboratory Page 281 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Study: Product Number(Test SubsUnce): Matrix: Me(hod/Revision: Analytical Equipment System Number Instrument Software/Version: Dale orExtraction'Analyst Date o f Analysia/Analyst: Date o f Data Reduction/Analyst Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98.1%) N-Ethyl PerfluorooctanesuKonamido Ethanol in Rata T-6316 (EtFOSE-OH) Rat Liver Filename: ETS-8-6.0 & ETS-8-7.0 R-Squared Value: Soup 020199. Amelia 062498 Slope: MassLynx 3.3 Y-Iutcrcept 02.14,00,02.16/00,03/15/01 RWW/SAL/KJS 0221 '00, 02 29/00, 03/01'00,03/03/00,03/04/00, 4/28/00,08'01/00, 0814/00,08/15/00, 03/22/01 MMH/MEE/IAS 02 28 00,03 O IW 03 03/00,03/06/00,52/00,5/4/00, 0 8 '0 2 '0 0 , 08 1500,08/17/00.0323/01 IAS/MMH See Attachments See Attachments See Attachments See Attachments WEEK IPS RAT LIVER G roup Duse Group 4 Mid-High Dose 100 mg/kg Sample $ C90904M C90908M C909I0M C909I1M C90916M C90926M C90927M C90928M C90933M C90944M C90947M C90948M C90953M C90955M C90956M C90965M C90968M C91315F C91324F PFOS Calc. Cone. 3232S7 313374 98979 718021 236132 120112 2624(1 628332 153299 565043 295355 186556 60324 265167 201182 689313 445034 230009 509159 Concentration of PFOS ug/g or % Rec. 323 313 99.0 718 236 120 26.2 628 153 565 295 187 60.3 265 201 689 445 230 509 A A PFOS Of/* 313 RSD Std Dev MS/MSD RFD 70.4 220 PFOSA Cale. Cune. n*/* 14679 14920 12376 18544 17812 4061 11539 17644 13218 15070 9823 9411 10031 14511 8680 20448 16616 12800 16226 Concentra Hon of PFOSA ug/g e r % Rec. 14.7 14.9 124 18.5 17.8 4.06 11.5 17.6 13.2 15.1 9.82 9.41 10.0 14.5 8.68 20.4 16.6 12.8 16.2 PFOSA u*/* RSD Std Dev MS/MSD RPD 31.3 13.5 4.23 C91327F C91332F 31737 377842 31.7 378 10627 17062 10.6 17.1 C91335F C9I336F C9I338F C91340F C91341F C91342F C91356F C91357F 220157 329837 341389 579769 242581 355109 42389 192963 220 330 341 580 243 355 42.4 193 14551 14949 18058 16126 15274 16810 6157 16831 14.6 14.9 18.1 16.1 15.3 16.8 6.2 16.8 C9t360F C91361F 206612 712319 207 712 17955 22322 18.0 22.3 C91362F 86896 86.9 - 10883 10.9 C91372F C9I376F C9I378F C91380F 257883 253932 340658 324616 258 254 341 325 19454 19.5 16296 16.3 57.7 18952 19.0 23.1 297 171 15385 15.4 15.6 3.61 Group 6 C91047M Mid-High Dose C9I054M Recovery 100 mg/kg C9I056M C91060M C91065M C91070M C91071M CViU/M C91073M C91076M C91451F C9I453F C91455F C9H59F C91462F C91467F C9I473F C9I479F C9I480F C9H85F C91487F C91488F PFOS - Perfluorooclancsulfonate 2034 198 10494 2006 36.5 205 4M 384 83.1 5024.960 15396 4525 18803 49.4 17533 137 13901 20.7 149 10328.5* 62.8 11369 2.03 2.17 <LOO (0.00614 ue/e) 0.198 2.46 <LOO (0.00614 ue/e) 10.5 42.9 0.0429 2.01 1.83 <LOQ (0.00614 ug/g) 0.0365 2.74 <LOO (0.00614 ue/el 0.205 1.79 <LOQ (0.00614 ue/e) 0.04 M 2.53 <LOQ (0.00614 ue/e) 0.384 2.67 <L0Q(O 00614 ug/g) 0.0831 164 0.849 <LOQ (0.00614 ug/g) 5.024960 nu 205 3.36 1.74 <LOQ (0.00614 ue/e) 15.4 1.63 <LOQ (0.00614 ug/g) 4.53 1.29 <LOQ (0.00614 ug/g) 18.8 2.43 <LOQ (0.00614 ug/g) 0.0494 0.37 <LOQ (0.00614 ug/g) 17.5 2.49 <LOQ(0.00614 ug/g) 0.137 2.68 <LOQ (0.00614 ug/g) 13.9 2.33 <LOQ (0.00614 ug/g) <LOQ (0.0245 ug/g) 1.62 <LOO (0.00614 ue/e) 0.149 0.880 <LOQ (000614 ug/g) 10.33 2.25 <LOO (000614 ue/el 0.0628 11.4 99.0 0.894 <LOO (0.00614 ue'e) 7.62 2.94 <LOQ (0.00614 ug/g) 8 Value estimated, above the range of the calibration curve. LAC 03/14/01 <LOQ <LOQ NA NA NA NA PFOSA = Pcrfluorooctanesulfooamide PFOSAA " Perfluorooclanesulfonamideacetale ** Data may be biased high as CCVs weren't within criteria. LAC03/14/01 A = Sample was reextracted 03/15/01, analyzed 0322/01, and the PFOS concentration reported from 03/15/01 extraction. LAC 0326/01 ElFQSE - Narrow Range N-Ethyl Perfluorooctaatanlfonamido ethyl alcohol M556 = C8F17SO2N((H)CH2CO0) PFOSEA - Perfuorooctane sulfonyl ethylamide Date Entered/Anal 03/14/00,03.16/00, 03/17/00, 05/05 00,05/18/00,08 15/00,0821 00,09 03'00, 0326/01 LAC'CSH/MMH Date Verified/Ana 03/09/01 hoj Purity EntereAVer02.19/01 LAC PFOSAA Calc. Cone. ng/g 21358 18476 44847 35222 23948 1784 15462 40328 18511 23008 17773 11445 18340 27358 4725 51758 26905 15794 28252 38590 25423 18251 19676 20954 26299 25334 33469 17230 20686 28490 31554 30022 42332 27417 30114 30712 220 19.5 74.5 44.5 28.9 19.1 43.8 30.1 21.8 20.1 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 11.2 7.21 0.00 12.9 Corrected PFOS LOQ (0.0306 ug'g) to include std correction factors new LOQ is 0.0245 ug/g. LAC02/19'01 Concentration of PFOSAA ug/g or % Rec. 21.4 18.5 44.8 35.2 23.9 1.78 15.5 40.3 18.5 23.0 17.8 11.4 18.3 27.4 4.72 51.8 26.9 15.8 28.3 38.6 25.4 18.3 19.7 21.0 26.3 25.3 33.5 17.2 20.7 28.5 31.6 30.0 42.3 27.4 30.1 30.7 0.22Q 0.0195 0 0745 0.0445 0.0289 0.0191 0.0438 0.0301 0.0218 0.0201 <LOO (0.0123 ue/el <LOQ(0.0I23 ug/g) <LOOf0.0123 ue/el <LOO (0.0123 ue/el <LOQ (0.0123 ug/g) <LOQ (0.0123 ug/g) <LOQ (0.0123 ug/g) ''LCX; 10.012.3 ue/el <LOQ (0.0123 ug/g) <LOQ (0.0123 ug/g) <LOQ (0.0123 ug/g) <LOQ (0.0123 ug/g) Mean PFOSAA ug/g 23.6 26.9 0.0522 <LOQ RSD Std Dev MS/MSD RPD 56.5 13.3 26.3 7.08 118 0.0614 NA NA Analytical Report: FACT-TOX-001 L R N -U 2103 EtF O S E Calc. Cdc. n*/* 437 276 823 470 334 0.00 291 309 334 323 308 235 207 466 310 1024 514 442 755 279 432 1389 469 917 408 721 777 182 843 6034 1106 211 522 734 211? 557 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 Concentration f EtFOSE EtFOSE ug/g o r % Rec. ug/* 0.437 0.276 0.823 0.470 0.334 <LOQ (0.0614 ug/g) 0.291 0.309 0.334 0.323 0.308 0.235 0.207 0.466 0.310 1.02 0.514 0.395 0.442 0.755 0.279 0.432 1.389 0.469 0.917 0.408 0.721 0.777 0.182 0.843 6.03 1.11 ft 0.211 0.522 0.734 2.12 * 0.557 0.994 <LOQ (0.0614 ug/g) <LOO (0.0614 ue/p) <LOO (0.0614 ue/el <LOO (0.0614 ue/el <LOO (0.0614 ue/el <LOO (0.0614 ue/el -LOQ (0.C14 ug'g) <LOO (0.0614 ue/el <LOQ (0.0614 ug/g) <LOO (0.0614 ue/el <LOQ <LOQ (0.0614 ug/g) <LOQ (0.0614 ug/g) <LOQ (0.0614 ug/g) <LOQ (0.0614 ug/g) <LOQ (0.0614 ug/g) <LOQ (0.0614 ug/g) <LOQ (0.0614 ug/g) < L u u I0.U614 ue/e) <LOO <0.0614 ue/e\ <LOO (0.0614 ue/el <LOO (0.0614 ue/e) . <LOQ (0.0614 ug/g) <LOQ RSD Std Dev MS/MSD RPD 57.8 0.229 131.0 1.303 NA NA NA NA 3MEnvironmental Laboratory Page 282 3M M edical D epartm ent Study: T6316.1 AMDT# 092597.1 Covance# 6329-212 Study: Product Number(Tesl Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Soflwmre/Version: Date o f Extraction/Analyst: Date o f Analysis/Analyst: Dale of Data Reducaon/Analyst Sample Data 104 Week Dietary Carcinogenicity Study with Narrow Range (98. I*/.) N-Ethyi Perfluorooctanesulfonamido Ethanol in Rats T-63I6 (EtFOSE-OH) Rat Liver Filename: See Attachments ETS-B-6.0 & ETS-8-7.0 R-SquaredValue: See Attachments Soup 020199, Amelia 062498 Slope: See Attachments MassLynx 3.3 Y-Intercept See Attachments 02/14/00,02/16/00,03/|5-X)X RWW/SAL/KJS Box 004312,00-013 02/21/00,02/29/00, 03/01/00,03/03/00, 03'04 '00, 4/28/(0,08/01/00,08/14/00, 08.15/00,03/22/01 MMH/MEEIAS 02/28.00, 03/01/00, 03/03/00, 03/06/00, 5/3/00, 5/4/00,08/02/00, 08/15/00,08/17/00, 03,23/01 IAS/MMH WEEK 105 RAT LIVER `ST Sample# MS54 Calc. Cane. n/l CsDcentntten f M554 Ug/g or % Ree. M554 <*/ RSD Std Dev MS/MSD RPD PFOSEA C ak. Cane, o*/* C e p e e n tr a ti e ti of PFOSEA ug/g ar % Ree. PFOSEA ug/g RSD Std Dev MS/MSD RPD Group 4 Mid-High Dose 100 tng/ltg C909MM C90908M C90910M C909I1M C909I6M C90926M 28960 29855 30567 32781 32395 8469 29.0 299 30.6 32.8 32.4 8,47 0.00 <LOQ (0.0123 ug/g) 20.5 0.0205 33.7 0.0337 0.00 <LOO (0.0123 ue/p) 2.41 <JXX) (0.0123 up/p) 48.3 0.0483 C90927M 23216 23.2 3.48 <LOQ (0.0123 ug/g) C90928M 30318 30.8 30.7 0.0307 C90933M 25401 25.4 29.1 0.0291 C90944M 27552 27.6 54.8 0.0548 C90947M C90948M 17406 25822 17.4 25.8 0.00 <LOO (0.0123 up/p) 26.3 0.0263 C90953M 20389 20.4 0.00 <LOQ (0.0123 ug/g) C90955M 36299 36.3 000 <LOQ (0.0123 ug/g) C90956M 9313 9.31 115 0.115 C90965M 44554 44.6 34.7 236 0.236 139 Group 4 Mid-High Dose 100 mgltg C90968M C91315F C91324F C91327F C91332F C91335F 37472 22980 32766 9807 32164 24677 37,5 27.1 9.4 23.0 32.8 9.81 32-2 24.7 2.62 <LOQ (0.0123 UE/g) 0.0408 58.1 0.0581 32.7 0.0327 33.3 0.0333 2.03 <LOQ (0.0123 ug/g) 4.12 <1.00 (0.0123 up/p) 0.0566 C9I336F 27071 27.1 10.5 <LOQ (0.0123 ug/g) C91338F 30744 30.7 13.0 0.0130 C91340F 31154 31.2 24.4 0.024* C91341F C91342F 26187 41708 26.2 41.7 10.3 <LOO (0.0123 up/p) 10.8 <LOQ (0.0123 ug'g) C9I356F 11248 11.2 56.0 0.0560 C9I357F 26342 26.8 11.5 <LOQ(0.0123 ug/g) C9I360F 25014 25.0 25.2 0.0252 C9I361F C9I362F C91372F C91376F C91378F C9I380F 44467 23712 39723 33977 23656 33352 . 44.5 23.7 39.7 34.0 23.7 33.4 31.1 28.5 8.86 23.2 0.0232 2.82 <LOQ (0.0123 ug'g) 26.8 0.0268 24.3 0.0243 28.6 0.0286 26.0 0.0260 0.0241 57.6 0.0139 Group 6 C91047M 2.73 <LOO (0.00615 ub/b) 0.00 <LOO (0.0307 us:) Mid-High Dose Recovery C91054M C91056M 3.13 <LOO (0.00615 ub/b) 0.00 <LOQ (0.123 ug/g) 0.00 <LOO (0.0307 up/p) 0.00 <LOQ (0.0307 ug/g) lOOmg/kg Group 6 Mid-High Dose Recovery 100 mg/kg C91060M C9I065M C9I070M C91071M C91072M C91073M C91076M C91451F C91453F C91455F C91459F C9I42F 0.00 <LOO (0.123 ub/b) 0.00 <LOO (0.123 ub/b) 0.00 <LOQ (0.123 ug'g) 000 <LOO (0.123 u*/p) 000 <LOQ(0 123 ug/g) 0.00 <LOQ(O.I23 ug/g) 0.00 <LOO (O.I23ue/e> <LOO 0.00 <LOQ (0.123 ug/g) 0.00 <LOQ (0.123 ug/g) 0.00 <LOQ (0.123 ug/g) 0.00 <LOQ (0.123 ug/g) 0.00 <LOQ (0.123 ug/g) NA NA 0.00 <LOQ (0.0307 ug/g) 0.00 <LOQ <0.0307 ug/g) 0.00 <LOQ (0.0307 ug/g) 0.00 <1.00 (0.0307 up/p) 0.00 <1.00 (0.0307 up/p) 0.00 < 100(0.0307 up/p) 0.00 <LOO (0.0307 ug'B) <LOO 0.00 < 100(0.0307 up/p) 0.00 < 100(0.0307 up/p) 0.00 <IOO (0.0307 up/p) 0.00 <IOO (0.0307 up/p) 0.00 <1 OO (0.0307 up/p) NA NA C91467F C91473F C91479F 0.00 <LOQ (0.123 ug/g) 0.00 <LOQ (0.123 ug/g) 1.36 <1 o n (0.00615 up/p) 0.00 <LOQ (0.0307 ug/g) 0.00 < 100(0.0307 up/p) 0.00 <1 <vin? C91480F C91485F C91487F C9I488F 0.00 4,71 1.19 2.93 <LOQ (0.00615 ug/g) <LOO (0.00615 ub/b) <1.00 (0.00615 uf/p) <LOQ (0.00615 ug/g) <LOQ NA NA 0.00 <LOQ (0.0307 ug/g) 0.00 <LOQ (0.0307 ug/g) 0.00 <LOO (0.0307 up/p) 0.00 <LOQ (0.0307 ug/g) <LOQ NA NA PFOS = Perfluorooctenesulfonate # Value estimated, above the range fthe calibration curve LAC 03/14/01 PFOSA - Perfluorooctanesulfonanride ' Data may be biased high as CCVs weren't within criteria. LAC 03/14/01 PFOSAA = Perfluorooclanesulfonamidoacttate EtFOSE - Narrow Range N-Ethyl Perfluorooctanesulfonamido = Sample was reextracted 03/15/01, analyzed 03/22/01, and the PFOS cone miration reported from 03/15/01 extraction. LAC 03 26/01 M556 = C8F17SO2N((H)CH2C0O) PFOSEA = Perfuorooctane sulfonyl etbylatnide . Date Entered/Analyst 03:14/00, 03'16/l)0,03/17/00,05/05/00,05/18/00,08/15/00,08/21/00,09/03/00,03/26/01 LAC/CSH/MMH Date Verified'Analysl: 03/09/01 hoj Purity Entered'Verified: 02/19/01 LAC Corrected PFOS LOQ (0.0306 ug'g) to include std correction factors new LOQ is 0 0245 ug'g. LAC02/19/01 Analytical Report: FACT-TOX-001 L R N -U 2103 3MEnvironmental Laboratory Page 283 3M M edical D epartm ent Study: T6316.1 3M Medical Department Study: T-6316.1 Appendix F: Example Calculations Analytical Report: FACT-TOX-001 L R N -U 2103 Analytical Report: FACT TOX-001 LRN-U2103 Formula Used for Sera Analyses in Study FACT TOX-001 A R (ng/m L) x D F x SC x P F x FV (m L) x 1.0 p g Reported Concentration (pg/mL) EV (mL) 1000 ng Calculation Used for Group 2, Week 105, Animal ID C90783M, determination of PFOS 189.2 ng/m L x 10 x 0.9275 x 0.8640 x 1 m L x 1.0 p g 1 mL 1000 ng = 1.52 pg/mL AR-- Analytical result from M assLynx summary DF-- Dilution factor SC-- PFOS salt correction constant (0.9275) PF-- Purity correction factor FV-- Final extract volume (1.0 mL unless otherwise noted) EV -- Volume o f sera extracted Formula Used for Liver Analyses in Study FACT TOX-001 A R (ng/g) x 3 c u r v e (1) x S C x P F x D F x 1.0 p g = Reported Concentration (pg/g) 5 sample 1000 ng (1) d curve is assum ed to be: 1 g liver 5 m L H 20 Calculation Used for Group 2, Week 105, Animal ID C90783M, determination of PFOS 4 88.16 ng/g x l g / 5 m L x 0.9275 x 0.8640 x 20 x 1.0 p g = 7.91 pg/g 0.9895 g/ 5 mL 1000 ng AR-- Analytical result from MassLynx summary d curve-- Density o f the liver standard curve, assumed to be lg liver/ 5 ml w ater d sam ple-- D ensity o f the liver sam ple (g sam ple/ 5 m L H 20 ) SC-- PFOS salt correction constant (0.9275) PF-- Purity correction factor DF-- Dilution factor 3MEnvironmental Laboratory Page 284 3M M edical D epartm ent Study: T6316.1 3M Medical Department Study: T-6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Analytical Report: FACLTRTNO-UX2-010013 Appendix G: Interim Certificates of Analysis 3MEnvironmental Laboratory Page 285 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Centre Analytical Laboratories, Inc. L 3048 Research Drive State College, PA 16801 Phone:(814)231-8032 Fax: (814) 231-1253 or (814) 231-1580 INTERIM CERTIFICATE OFANALYSIS Revision 1(9/7/00) Centre Analytical Laboratories COA Reference #: 023-018B 3M Product: PFOS,Lotl71 Reference#: SD-009 Purity: 86.4%_________________ Test Name Specifications Purity1 R esult 86.4% Appearance Identification NMR Metals (ICP/MS) 1. Calcium 2. Magnesium 3. Sodium 4. Potassium2 5. Nickel 6. Iron 7. Manganese Total % Impurity (NMR) Total % Impurity (LC/MS) Total % Impurity (GC/MS) Related Compounds POAA Residual Solvents (TGA) Purity by DSC Inorganic Anions (IC) 1. Chloride 2. Fluoride 3. Bromide 4. Nitrate 5. Nitrite 6. Phosphate 7. Sulfate4 Organic A cid s5(IC) 1. TFA 2. PFPA 3. HFBA 4. NFPA Elemental Analysis*1: 1. Carbon 2. Hydrogen 3. Nitrogen 4. Sulfur 5. Fluorine White Crystalline Powder 1. Theoretical V alue = 17.8% 2. Theoretical Value = 0% 3. Theoretical Value = 0% 4 . Theoretical Value = 5.95% 5. Theoretical Value = 60% Conforms Positive 1. 0.017 wt./wt.% 2. 0.007 wt./wt.% 3. 1.355 wt./wt.% 4 . 6.552 wt./wt.% 5. 0.003 wt./wt.% 6. 0.004 wt./wt.% 7. <0.001 wt./wt.% 1.00 wt./wt.% 10.60 wt./wt.% None Detected 0.30 wt./wt.% None Detected Not Applicable3 1. <0.015 wt./wt.% 2 . 0 .2 7 w t.A v t.% 3. <0.040 wt./wt.% 4 . <0.009 wt./wt.% 5. <0.006 wt.Avt.% 6. <0.007 wt.Avt.% 7 . 8.82 wt.Avt.% 1. <0.1 wt.Avt.% 2 . <0.1 wt.Avt.% 3 . <0.1 wt.Avt.% 4 . <0.25 wt.Avt.% 1. 12.08 wt.Avt.% 2. 0.794 wt.Avt.% 3. 1.61 wt.Avt.% 4 . 10.1 wt.Avt.% 5 . 50.4 wt.Avt.% C O A 023-018B 3MEnvironmental Laboratory Page 1 o f 3 Page 286 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Centre Analytical Laboratories, Inc. 3048 Research Drive Phone: (814) 231-8032 State College, PA 16801 Fax: (814) 231-1253 or (814) 231-1580 INTERIM CERTIFICATE OFANALYSIS C e n tre A nalytical L a b o ra to rie s C O A R eferen ce it: 023-018B D ate o f L ast A nalysis: 08/31/00 Expiration D ate: 08/31/01 Storage Conditions: Frozen <-10C R e-assessm ent D ate: 08/31/01 'Purity = 100% - (sum o f m etal im purities, 1.39% +LC/M S im purities, 10.60% +Inorganic Fluoride, 0.27% +N M R im purities, 1.00%+ POAA, 0.30%) Total im purity from all tests = 13.56% Purity = 100% -13.56% = 86.4% fy Potassium is expected in this salt form and is therefore not considered an im purity. 3P u rity b y D S C is g en era lly n o t applicable to m a teria ls o f lo w purity. N o en d o th erm w as observed for this sample. . 4S ulfu r in th e sam p le appears to b e converted to SO4 an d h en ce d etected u sin g the inorganic anion method conditions. The anion result agrees w ell w ith the sulfur determ ination in the elem ental analysis, lending confidence to this interpretation. B ased on the resu lts, th e SO4 is n o t considered an im purity. 5T F A HFBA NFPA PFPA Trifluoroacetic acid Heptafluorobutyric acid N onofluoropentanoic acid Pentafluoropropanoic acid "T heoretical v alu e calculations b ased on th e em p irical form ula, C gFi7S 03'K + (M W = 538) This w ork w as conducted under EPA G ood Laboratory Practice Standards (40 C FR 160). C O A 023-018B 3MEnvironmental Laboratory Page 2 of 3 Page 287 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Centre Analytical Laboratories, Inc. 3048 Research Drive State College, PA 16801 Phone: (814) 231-8032 Fax: (814) 231-1253 or (814) 231-1580 INTERIM CERTIFICATE OFANALYSIS Centre Analytical Laboratories COA Reference #: 023-018B LC/MS Purity Profile: Impurity C4 C5 C6 C7 Total wt./wt. % 1.03 1.56 6.38 1.63 10.60 Note: The C4 and C6 values were calculated using the C4 and C6 standard calibration curves, respectively. The C5 value was calculated using the average response factors from the C4 and C6 standard curves. Likewise, the C7 value was calculated using the average response factors from the C6 and C8 standard curves. C Prepared By f/a /' . Date lytical Laboratories Reviewed By: ? /f/m Date Laboratory Manager, Centre Analytical Laboratories COA023-018B 3M E nvironm ental Laboratory Page 3 of 3 Page 288 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 i i Centre Analytical Laboratories, Inc 3 0 4 8 R esearch D rive Phone: (814) 23 1-8 032 S tate C ollege, PA 16801 Fax: (814) 231 -12 53 or (814) 231 -1580 INTERIM CERTIFICATE OFANALYSIS Centre Analytical Laboratories COA Reference #: 023-022-2 3M Product: EtFOSE-OH Test Control Reference #: TCR-00017-52 Purity: 97.4% P urity1 Test Name Appearance Identification NMR Metals (ICP/MS) 1. Calcium 2. Magnesium 3. Sodium 4. Potassium 5. Nickel . 6. Iron 7. Manganese Total % Impurity (NMR) Total % Impurity (LC/MS) Total % Impurity (GC/MS) Related Compounds - POAA Residual Solvents (TGA) Purity by DSC Inorganic Anions (IC) 1. Chloride 2. Fluoride 3. Bromide 4. Nitrate 5. Nitrite 6. Phosphate 7. Sulfate . Organic Acids2(IC) 1. TFA 2. PFPA 3. HFBA 4. NFPA Elemental Analysis2: 1. Carbon 2. Hydrogen 3. Nitrogen 4. Sulfur 5. Fluorine <,. Specifications - ...,..... , .....,,....;iiff; i],i', i;i i.; Yellow-white, waxy solid Result 97.4% Conforms , - .: , 1 , i ii , ll ' V '/ * 1 1 'ji ' ,,; (.../>< ..-> 1. :/!!t- !:: :!< . : ' . . : / i ' 1 ', V ' : : . : 1 S' t : . I ; :1 - -- i 1 *. V tj '' r1 ( 1- ' ' ' I1 . .... .-,X - y :: i ": : - Positive 1. <0.001 wt./wt.% 2. <0.001 wt./wt.% 3. <0.001 wt./wt.% 4. <0.001 wt./wt.% 5. <0.001 wt./wt.% 6. <0.001 wt./wt.% 7. <0.001 wt./wt.% 1.26 wt./wt.% None Quantified 1.29 wt./wt.% 0.10wt./wt.% None Detected 90.3 wt./wt.%. 1. <0.015 wt./wt.% 2. <0.005 wt./wt.% 3. <0.040 wt./wt.% 4. < 0.009 wt./wt.% 5. <0.006 wt./wt.% 6. <0.007 wt./wt.% 7. <0.154 wt./wt.% 1. <0.1 wt./wt.% 2. <0.1 wt./wt.% 3. <0.1 wt./wt.% 4. <0.25 wt./wt.% 1. Theoretical Value = 25.2% v 1. 25.04 wt./wt.% 2. Theoretical Value = 1.75% 2. 1.69 wt./wt.% 3. Theoretical Value = 2.45% 4. Theoretical Value = 5.60% 3. 2.61 wt./wt.% 4. 8.88wt./wt.% 5. Theoretical Value = 56.6% 5. 56.8 wt./wt.% C O A 023-022-2 3MEnvironmental Laboratory Page 1 o f3 Page 289 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Centre Analytical Laboratories, Inc. 3 0 4 8 R esearch D rive Phone: (814) 23 1-8 032 S tate C o llege, PA 16801 Fax: (814) 23 1-1 253 or (814) 23 1 -1 5 8 0 INTERIM CERTIFICATE OFANALYSIS Centre Analytical Laboratories COA Reference #: 023-022-2 3M Product: EtFOSE-OH Test Control Reference #: TCR-00017-52 D ate o f Last Analysis: 11/26/00 Expiration D ate: 11/26/01 Storage Conditions: <-10 C R e-assessm ent Date: 11/26/01 1P u rity = 100% - (total N M R im purities, 1.26% + G C/M S im purities, 1.29 + PO A A , 2T F A HFBA NFPA PFPA Total impurity from all tests = 2.65% Purity = 100% - 2.65% = 97.4% Trifluoroacetic acid Heptafluorobutyric acid Nonafluoropentanoic acid Pentafluoropropanoic acid th e o r e tic a l value calculations based on the em pirical form ula, C 12H 10F 17N O 3S (M W =571) t: C O A 023-022-2 3MEnvironmental Laboratory Page 2 of 3 Page 290 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Centre Analytical Laboratories, Inc. 3 0 4 8 R esearch D rive S tate C o llege, PA 16801 Phone: (814) 231-8032 Fax: (814) 23 1-1 253 or (814) 23 1 -1 5 8 0 n INTERIM CERTIFICATE OFANALYSIS Centre Analytical Laboratories COA Reference #: 023-022-2 3M Product: EtFOSE-OH Test Control Reference #: TCR-00017-52 GC/MS Purity Profile Peak# 1 2 Total Retention Time (m in ) 13.934 17.307 - Identity PFOSDEA Cl - % Im purity 0.36 0.93 1.29 i This w ork was conducted under EPA Good Laboratory Practice Standards (40 CFR 160). Prepared By: nd S. Bell Scientist Centre A nalytic# Laboratories R eview ed By: l A jL /W John Flaherty Laboratory M anager Centre Analytical Laboratories C O A 023-022-2 3MEnvironmental Laboratory D ate D ate Page 3 o f3 Page 291 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 LRN-U2103 Centre Analytical Laboratories, Inc. 3 0 4 8 R esearch D rive Phone: (814) 231-8032 S ta te C ollege, PA 16801 Fax: (814) 231-1253 or (814) 2 3 1-1 580 INTERIM CERTIFICATE OFANALYSIS Centre Analytical Laboratories COA Reference #: 023-022-1 3M Product: EtFOSE-OH Test Control Reference #: SD-013 Purity: 88.9% P u rity 1 Test Name Appearance Identification NMR Metals (ICP/MS) 1. Calcium 2. Magnesium 3. Sodium 4. Potassium 5. Nickel 6. Iron 7. Manganese Total % Impurity (NMR) Total % Impurity (LC/MS) Total % Impurity (GC/MS) Related Compounds - POAA Residual Solvents (TGA) Purity by DSC Inorganic Anions (IC) 1. Chloride 2. Fluoride 3. Bromide 4. Nitrate 5. Nitrite 6. Phosphate 7. Sulfate Organic Acids'1(IC) 1. TFA 2. PFPA 3. HFBA 4. NFPA Elemental Analysis'*: 1. Carbon 2. Hydrogen 3. Nitrogen 4. Sulfur 5. Fluorine Specifications 1! Yellow-white, waxy solid " :T : y ..... ! , , . 4- ` , .1 ,_______ b___!!___!_____ ' 1 : h 'rV ' ' ' 7i i" ; ; ' 1, ' i1 '; J i , 1* ' ;' .,. ` - `- ` . ; ; i`' , 4- >' ~. ' ' . - .fr i i,, * - '' ( '''-':.!`:'L.\1bt"-;`..ii,:?.-v;-.-i'::j,;=:; 2. ` 1> v:: '< v ' - .. " >` '* 1i '' {': t it 1 'i ' :>: :; . < - 1. , ! `' 7 -- ,. ! ?1 . '1 , M,v , , "*' i <<)' 1. Theoretical Value = 25.2% 2. Theoretical Value = 1.75% 3. Theoretical Value = 2.45% 4. Theoretical Value = 5.60% 5. Theoretical Value = 56.6% Result 88.9% Conforms Positive 1. <0.001 wt./wt.% 2. <0.001 wt./wt.% 3. <0.001 wt./wt.% 4. 0.002 wt./wt.% 5. <0.001 wt./wt.% 6. <0.001 wt./wt.% 7. <0.001 wt./wt.% 0.90 wt./wt.% None Quantified 10.21 wt./wt.% 0.03 wt./wt.% None Detected 87.6 wt./wt.%. 1. <0.015 wt./wt.% 2. <0.005 wt./wt.% 3. <0.040 wt./wt.% 4. <0.009 wt./wt.% 5. <0.006 wt./wt.% 6. <0.007 wt./wt.% 7. <0.040 wt./wt.% 1. <0.1 wt./wt.% 2. <0.1 wt./wt.% 3. <0.1 wt./wt.% 4. <0.25 wt./wt.% 1. 24.42 wt./wt.% 2. 1.78wt./wt.% 3. 2.72 wt./wt.% 4. 9.34 wt./wt.% 5. 58.4 wt./wt.% C O A 023-022-1 3MEnvironmental Laboratory Page 1 o f3 Page 292 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Centre Analytical Laboratories, Ine. 3 0 4 8 R esearch Drive S tate C ollege, PA 16801 Phone: (814)231-8032 Fax: (814) 231-1253 or (814) 23 1-1580 o t INTERIM CERTIFICATE OFANALYSIS Centre Analytical Laboratories COA Reference #: 023-022-1 . 3M Product: EtFOSE-OH Test Control Reference #: SD-013 D ate o f Last Analysis: 11/26/00 Expiration Date: 11/26/01 Storage Conditions: <-10 C Re-assessm ent Date: 11/26/01 'Purity = 100% - (total metal impurities, 0.002% + total N M R impurities, 0.90% + GC/MS impurities, 10.21 + POAA, 0.03%) Total impurity from all tests = 11.14% Purity = 100% - 11.14% = 88.9% 2T F A HFBA NFPA PFPA Trifluoroacetic acid Heptafluorobutyric acid Nonafluoropentanoic acid Pentafluoropropanoic acid th e o r e tic a l value calculations based on the empirical formula, C 12H 10F 17N O 3S (M W =571) * C O A 023-022-1 3MEnvironmental Laboratory Page 2 o f 3 Page 293 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Centre Analytical Laboratories, Inc 3 0 4 8 R esearch Drive Phone: (814) 231-8032 S tate C ollege, PA 16801 Fax: (814) 231-1253 or (814) 23 1-1 580 i INTERIM CERTIFICATE OFANALYSIS Centre Analytical Laboratories COA Reference #: 023-022-1 3M Product: EtFOSE-OH Test Control Reference #: SD-013 GC/MS Purity Profile Peak# 1 2 3 4 5 6 7 8 9 10 11 12 13 Total Retention Time (m in ) 6.163 8.011 8.206 9.065 9.844 13.93 14.238 15.130 15.52 15.941 16.379 16.801 17.222 - Identity Unknown Unknown Unknown Unknown Unknown Unknown Unknown C2 C3 C4 C5 C6 C7 - ' % Im parity 0.12 0.23 0.51 0.21 0.34 0.62 0.11 0.11 1.11 1.55 1.07 3.30 0.93 10.21 This work was conducted under EPA Good Laboratory Practice Standards (40 CFR 160). Prepared By: id S. B ell Scientist Centre Analyse iratories Reviewed By: fY ) John Flaherty Laboratory Manager Centre Analytical Laboratories CO A023-022-1 3MEnvironmental Laboratory D ate D ate Page 3 o f3 Page 294 3M M edical D ep artm ent Study: T 6 3 1 6 .1________ ______________________ _________A nalytical R eport: FA C T -T O X -001 L R N -U 2103 ANALYTICAL REPO RT STUDY TITLE PURITY DETERMINATION OF SAMPLE LOTS Sample # TCR-00065-022 DATA REQUIREM ENTS Test Article Characterization STUDY DIRECTOR Kevin Lloyd T H IS IS AN EXACT COPY OF THE ORIGINAL DOCUMENT" BY. & L . -DATE Jo , ANALYTICAL REPO RT CO M PLETIO N D ATE October 25,2000 PERFORM ING LA BO RATORY / TESTIN G FA C ILITIES 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 B ox 33331 St. Paul, MN 55133-3331 PROTECT IDENTIFICATION Centre Study Number: 023-045 Total Pages: 15 3MEnvironmental Laboratory Page 295 3M M edical D epartm ent Study: T6316.1 Analytical Report: FACT-TOX-001 , LRN-U2103 Centre Study No.: 023-045 GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT Centre Study Num ber 023-045, entitled "Purity Determ ination o f Sam ple Lots o f PFO S, Sample # TCR-00065-022" conducted for 3M Environmental Laboratory, was performed in compliance with US EPA Good Laboratory Practice Standards (40 CFR Part 160) by Centre Analytical Laboratories, Inc. with the following exceptions: The automated data collection systems used in this study were not fully com pliant with 21 CFR 58.130 (e). Study Director Centre Analytical Laboratories, Inc. D ate 3M Environmental Technology and Safety Services D ate lo/as/eo Centre Analytical Laboratories, Inc. 3MEnvironmental Laboratory Page 2 o f 15 Page 296 3M M edical D epartm eniSiudy: T6316 1 Analytical Report: FACT-TOX-001 L R N -U 2103 Centre Study No.: 023-045 QUALITYASSURANCE STATEMENT Centre Study Number 023-045, entitled "Purity Determination of Sample Lots of PFOS, Sample # TCR-00065-022" was reviewed by Centre Analytical Laboratories' Quality Assurance Unit. All reviewed 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 Date Inspected 10/19/00 Date Reported to Study Director and Centre Management Date Reported to Stionsor Management 10/25/00 10/25/00 2. Raw Data Review 10/19/00 10/25/00 10/25/00 3. Report Review 10/24/00 10/25/00 10/25/00 William Spare Quality Assurance Officer / o'/ S '/o D ate 'T H IS IS AN EXACT COPY OF THE O RIGINAL D O C U M E N T" BY. -DATE Centre Analytical Laboratories, Inc. 3MEnvironmental Laboratory Page 3 of 15 Page 297 2M M edfiaLD fipam eii udiB E616J. Analytical Report: FACT-TOX-001 L R N -U 2103 Centre Study No.: 023-045 CERTIFICATION OF AUTHENTICITY This report, for Centre Study Number 023-045, is a true and complete representation of the raw data for the study. Submitted by: Centre Analytical Laboratories, Inc. 3048 Research Drive State College, PA 16801 (814) 231-8032 Study Director, Centre: Kevin Lloyd Study Director Centre Analytical Laboratories, Inc Centre Analytical Laboratories, Inc. Facility Management: Date Centre Analytical Laboratories, Inc. 8Y'-----& ---- ----- DATEJO/S'//*, Centre Analytical Laboratories, Inc. 3MEnvironmental Laboratory Page 4 o f 15 Page 298 w *0- LRN-U2103 Centre Study No.: 023-045 STUDY IDENTIFICATION PURITY DETERMINATION OF SAMPLE LOTS OF PFOS Sample # TCR-00065-022 TYPE OF STUDY: TEST SYSTEM: TEST ARTICLE: SPONSOR: STUDY DIRECTOR: TESTING FA C m TIES: ANALYTICAL PHASE TIMETABLE: Characterization Not Applicable PFOS, Test Control Reference # TCR-00065-022 3M Environmental Technology and Safety Services Building 2-3E-09 PO Box 33331 St. Paul, M N 55133-3331 Kevin Lloyd C en t Analytical Laboratories, Inc. Phone: (814) 231-8032 Centre Analytical Laboratories, Inc. (Centre) 3048 Research D riv e State College, PA 16801 Phone:814-231-8032 Study Initiation Date: Analytical Start Date: Analytical Termination Date: 09/28/00 10/05/00 10/24/00 "THIS IS AN EXACT COPY OF \cil&S'/cOTHE ORIGINAL DOCUMENT" RY STL nATP Centre Analytical Laboratories, Inc. 3M E nvironm ental Laboratory Page 5 o f 15 Page 299 3M M edical U e p ^ a e n h i M y T6316 1 Analytical Report: FACT-TOX-001 L R N -U 2103 Centre Study No.: 023-045 PROJECT PERSONNEL The Study Director for this project was Kevin Lloyd at Centre Analytical Laboratories, Inc. The following personnel from Centre Analytical Laboratories, Inc., were associated with various phases of the study: Name Gerry Shero David S. Bell Emily R. Stauffer Mark Ammerman Title Scientist Scientist Scientist Sample Custodian THE ORIGINAL DOCUMENT" BY. - ^ T - hatc lo /A /k o Centre Analytical Laboratories, Inc. 3MEnvironmental Laboratory Page 6 o f 15 Page 300 ------ --------------------- A nalytical R eport: FA C T -T O X -001 L R N -U 2103 Centre Study No.: 023-045 TABLE OF CONTENTS Page TITLE PAGE.............................................................................. 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 1.0 SUMMARY.................................................................................................................... 8 2.0 INTRODUCTION.............................................................................................................. 8 3.0 TEST SYSTEM................................................................................................................. 8 4.0 TEST ARTICLE................................................................................................................. 8 5.0 EXPERIMENTAL PROCEDURES................................................................................. 9 6.0 RESULTS AND DISCUSSION.......................................................................................10 8.0 CIRCUMSTANCES THAT MAY HAVE AFFECTED THE DATA......................10 9.0 RETENTION OF DATA AND SAMPLES................................................................ 10 Table I. Results From LC/MS for TCR-00065-022............................................................ 11 Figure 1. PFOS Calibration Standard (C100500-4) at 269pg/L......................................... 12 Figure 2. PFOS Calibration Standard (C100500-2) at 539pg/L......................................... 13 Figure 3. PFOS (TCR-00065-022) at 250pg/L, ESI Negative Ion M ode........................ 14 Appendix A: Study Protocol 00P-023-045: PURITY D ETER M IN A TIO N O F SAMPLE LOTS OF PFOS, Sample # TCR-00065-022, Including Amendment 1...........15 IS AN EXACT COPY O P THE ORIGINAL DOCUMENT" BY-----2 2 ------ D A T E i a j d Centre Analytical Laboratories, Inc. 3MEnvironmental Laboratory Page 7 o f 15 Page 301 3M IM i r i i a n b a f t m -- ^udijn T r i f l Analytical Report: FACT-TOX-001 LRN-U2103 Centre Study No.: 023-045 1.0 SUMMARY from sampled TCR-O006S20ii, was determined from the LC/MS test data to be,88.`0frpure as compared with the PFOS control (TCR-00017-046,97.9% purity). 2.0 INTRODUCTION This report details the results of the analysis of PFOS, Test Control Reference# TCR00065-022. The test was analysis by liquid chromatography - mass spectrometry (LC/MS). The LC/MS was conducted at Centre. The study was initiated on September 28,2000 when the Study Director signed protocol number 00P-023-045. The analytical start date was October 5,2000, and the experimental termination date was October 9,2000. 3.0 TEST SYSTEM There is no test system associated with this characterization study, therefore the GLP requirement for test system description, justification, and identification do not apply. The route of administration, levels and frequency of administration also do not apply to characterization studies. 4.0 TEST ARTICLE 'T H IS IS A N EXACT COPY O F THE O RIG INA L D O C U M EN T" BY S T (l n atc I o fe e , The test article was PFOS, Test Control Reference# TCR-00065-022. 3M Environmental Laboratory supplied the test article and it was logged at Centre Analytical Laboratories, Inc. as follows: Compound PFOS TCR-00065-022 Lot or NB Number Centre Control No. 00-023-068 Purity TBD Date Received 10/05/00 The sample received was a white, crystalline solid. It was received under frozen conditions and was stored in a temperature-monitored freezer kept at <-10C. Centre Analytical Laboratories, Inc. 3MEnvironmental Laboratory Page 8 of 15 Page 302 3M ^^dfc^^epartm enti^tw dy^Ti631>1 Analytical Report: FACT-TOX-001 LRN-U2103 Centre Study No.: 023-045 The analytical/control standard PFOS was: Control Article Lot Number PFOS TCR-00017-046 Centre Control No. 00-023-042 Expiration Purity Date 97.9% 8/31/2001 The chemical and physical data for PFOS is as follows. Common Name: Molecular weight: CAS Number Structure: PFOS 499 (C8F17SO3') 2795-39-3 O II CgFnS O--O" K+ II O Note: the neutral molecule and standard form that the PFOS (anion) is derived from is potassium perfluorooctane sulfonate (C8F17SO3K), molecular weight 538. 5.0 EXPERIMENTAL PROCEDURES LC/MS Spectral Analysis PFOS sample TCR-00065-022 was analyzed for purity using liquid chromatography/mass spectrometry (LC/MS). The sample was analyzed according to the following procedure. The sample was prepared at about 250 pg/mL in methanol and analyzed by LC/MS using a Hewlett-Packard 1100 HPLC system interfaced with a Hewlett-Packard 1100 mass selective detector. The mass spectrometer was run in negative ionization mode using electrospray ionization (ESI) using Selective Ionization Monitoring for ion m/z 499. The liquid chromatography system was operated in reversed-phase mode using a C l8 silica-based column. Each resulting chromatogram was calculated against the analytical control article (TCR00017-046) calibration curve. "THIS IS AN EXACT COPY OF THE ORIGINAL DOCUMENT Centre Analytical Laboratories, Inc. 3MEnvironmental Laboratory Page 9 o f 15 Page 303 3 M M e d ic a l^ e p a rtm e n fc ^ tu d y --^ 6 3 1 # '1 Analytical Report: FACT-TOX-001 L R N -U 2103 Centre Study No.: 023-045 6.0 RESULTS AND DISCUSSION LC/MS Spectral Analysis Responses were observed for the PFOS sample in negative ion mode using an ESI interface. Quantitation was performed using SIM mode, m/z 499, and PFOS was detected at 7.8 minutes. TH-PFOS was used as the internal standard, m/z 427, and was detected at 7.5 minutes. The total percent purity, calculated against the analytical control article (TCR-00017-046) calibration curve was determined to be 88.0% from the average of three replicate analyses. 8.0 CIRCUMSTANCES THAT MAY HAVE AFFECTED THE DATA Electronic records are not fully compliant with 21 CFR 11, "Electronic records; Electronic Signature." However, approved SOPs were in place and all instrumentation used in this study was fully calibrated and operational. All original raw data were printed as hard copies and fully audited by quality assurance. Verified exact copies and the electronic data will be stored in the archives at Centre Analytical Laboratories. Original raw data will be returned to the Sponsor. 9.0 RETENTION OF DATAAND SAMPLES When the final report is final, 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 of temperature logs will be submitted. Exact copies of all raw data, as well as a signed copy of the final analytical report and all original facility-specific raw data, will be retained in the Centre A nalytical Laboratories, Inc. archives for the period of time specified in 40 CFR Part 160. Retained samples of reference substances are archived by the sponsor. 'THIS IS AN EXACT COPY OF THE ORIGINAL DOCUMENT" BY. - S fc DATE J o /3 S 7 q^ Centre Analytical Laboratories, Inc. 3MEnvironmental Laboratory Page 10 of 15 Page 304 3M M edical Department. Study: T6316.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Centre Study No.: 023-045 Table L Results From LC/MS Of TCR-00065-022, ESI Negative mode 3M ID TCR-00065-022 TCR-00065-022 TCR-00065-022 Standard Standard Standard Standard Standard Standard Standard Standard Standard CCV Retention Time (min) 7.79 7.80 7.80 7.69 7.73 7.77 7.79 7.79 7.77 7.78 7.78 7.78 7.81 Mass 499 499 499 499 499 499 499 499 499 499 499 499 499 Value Determined Ug/L Hg/L 250 219 250 220 250 220 Average = 11 100* 11 17* 54 60 54 50 108 101 269 284 539 562 808 831 1078 1205 269 278 Standards Average = Std Dev = % Recovery 88.0 88.0 88.0 88.0 * * 110 93 94 105 104 103 112 103 103 7 * First two injections during instrument warm up, not reported. CCV = standard in run used to check calibration (C100500-4 at 269pg/L) "THIS IS AN E X A C T C O W O f THE ORIGINAL DO CUM ENT STZ. ,,DfiTE.isicc> BY. Centre Analytical Laboratories, Inc. 3MEnvironmental Laboratory Page 11 o f 15 Page 305 3M Medical DopartmontnStwdyiJ63Ji61 Analytical Report: FACT-TOX-001 L R N -U 2103 Centre Study No.: 023-045 Figure 1. PFOS Calibration Standard (C100500-4) at 269jng/L Sample Name:C100500-4 Sample Info: Data file :C:\HPCHEM\1\DATA\100600\10060022 .D ' 1 Instrument 1 Mon, 23. Oct. 2000 00:12:06 pm Page 1 cff 1 'T H IS IS A N EXACT COPY OF THE ORIGINAL DOCUMENT" >v lo / jiT /t*c ) Centre Analytical Laboratories, Inc. 3MEnvironmental Laboratory Page 12 o f 15 Page 306 3 M M edicai n epartm ent Study: T63161 Analytical Report: FACT-TOX-001 LRN-U2103 Centre Study No.: 023-045 Figure 2. PFOS Calibration Standard (C100500-3) at 539fig/L Sample Name:C100500-3 Sample Info-. Data file :C:\HPCHEM\1\DATA\100600\10060015.D ^^Injection Date \ Acq Operator Instrument Dilution ' 10/6/2000 1:13:21 PM GS G* W Instrument 1 1 Seq Line Vial No. Inj. No. Inj . Voi. : : : : Acq. Method PFOS.M . Analysis Method :\HPCHEM\1\METHODS\100600.M Last Changed 10/9/2000 01:45:43 pm (modified after loading) Analysis for PFOS MSo r n i , (V)WUWWBUWS.Ui W E S; N*a, SIM. 60000 70900 60000 50000 40000 30000 20000 10000 0 n i 1 1 r MSU1 4UU. blCMWa.f:<W. / ( 1WWU\1WSWIi.U) L 1 13 IS 1 5 il _flar 200000 150000 100000 50000- 2 Compound Name TH-PFOS PFOS Amount 500.0 499.8 4 R.T. 7.57 7.80 Area 770327 2238071 L ------------ 2------,___ -- ________ DIE Signal MSDl 427, EIC-426.7:42 MSD1 499, EIC*49B.7:49 r' *** End of Report *** Instrument 1 Mon, 9. Oct. 2000 01:46:00 pm Page 1 of 1 THI; IS AN EXACT COPY OF THE ORIGINAL DOCUMENT Centre Analytical Laboratories, Inc. 3MEnvironmental Laboratory Page 13 o f 15 Page 307 caiD epartfflent^iudy:< iiT 6216i1 Analytical Report: FA C T-TOX-001 L R N -U 2103 Centre Study No.: 023-045 Figure 3. PFOS (TCR-00065-022) at 250ng/L, ESI Negative Ion M ode Sample Name:L29092-1 Sample Info:C100500-8 Data file :C :\HPCHEM\1\DATA\100600\10060019 .D Injection Date Acq Operator Instrument Dilution 10/ 6/2000 GS ti. V.I-- Instrument 1 1 2:20:49 PM Seq Line Vial No. Inj. No. Inj. Voi. -> 1 17 21 1 5 til n .................................. - ---------------. . . . -- *** End of Report *** Instrument 1 Mon, 23. Oct. 2000 00:10:19 pm Page 1 of 1 Centre Analytical Laboratories, Inc. 3MEnvironmental Laboratory THE ORIGINAL DOCUMENT" BV. -DATE lokSr/oO Page 14 of 15 Page 308 3M M edical D ep artm en t Study: T63-16.1 Analytical Report: FACT-TOX-001 L R N -U 2103 Centre Study No.: 023-045 APPENDIX A Study Protocol Purity Determination of Sample Lots of PFOS Including Amendment 1 I n o 10 Ml* C A M LI U U r T O F THE ORIGINAL DOCUMENT BY. _2IL .DATE lo /jtsrA Centre Analytical Laboratories, Inc. 3MEnvironmental Laboratory Page 15 o f 15 Page 309 3M M edical D epartm ent Study: T6316.1 3M Medical Department Study: T-6316.1 Appendix H: Report Signature Page Analytical Report: FACT-TOX-001 L R N -U 2103 Analytical Report: FACT TOX-001 LRN-U2103 John L. Butenhoff, Ph.D., Study Director Date Tt Marvin T. Case, D.V.M., Ph.D., Sponsor Representative Date /3l/o( Kristen J. Hansen, Ph.D., Principal Analytical Investigator Date William K. Reagen, Ph.D., Laboratory Manager Date 3M Environmental Laboratory Page 310