Document qdkDmZzKjOoXk47ajZVXbed7K

P-1 <OE>. Surface Protection Solutions 4417 Lancaster Pike, BMP23-2236 Wilmington, DE 19805 rh r:. r -C, ciMMarsi - DuPont ; ., Malinowski - DuPont OS JU:! -3 KJ: 3U 9^ May 30, 2008 Attn: Jim Willis (phone 202-564-0104) Document Control Office (7407M) United States Environmental Protection Agency (EPA) Office o f Pollution Prevention and Toxics (OPPT) EPA East, Room 6248 1200 Pennsylvania Avenue, N. W. Washington, D. C. 20460 .pcn Dear Jim, As part o f DuPont's voluntary sharing o f information on our biodegradation research with EPA, enclosed is a Company Sanitized copy o f the final study report for a two-year aerobic soil biodegradation research study conducted by Wildlife International (Project No. 112E-108) for DuPont. We would like to meet with you and discuss the study and our interpretation o f the results. We will follow up in the near future to schedule time. We plan to publish this work and anticipate submitting a manuscript this summer. Thank you for offering to wait to post this to the Docket until publication. We don't think this will be necessary, however we can discuss it further when we meet. Please contact me if you have any questions regarding the study. 63100000010/S Robert C. Buck Tel. 302 892 8935; Email robert.c.buck@usa.dupont.com Company Sanitized 'lZO ZJt P-2 Company Sanitized. Does not contain TSCA CBI. p r-p ---t\ is--p 08 JL*r! -? r.M!Q:3t [ ]: TRANSFORMATION POTENTIAL IN AEROBIC AND ANAEROBIC SOILS WILDLIFE INTERNATIONAL, LTD. PROJECT NO. : 112E-108 Organisation for Economic Cooperation and Development OECD Guideline 307 AUTHORS: Edward C. Schaefer Joel Stenzel Raymond L. Van Hoven STUDY INITIATION DATE: March 10, 2005 STUDY COMPLETION DATE: March 17, 2008 Submitted to: E.I. du Pont de Nemours and Company Wilmington, Delaware 19898 USA . Wildlife International, Ltd. 8598 Commerce Drive Easton, Maryland 21601 USA 1 (410) 822-8600 Page 1 o f 298 Com pany Sanitized es r~nn c:> II cn 3 / Z 0M P-3 Company Sanitized. Does not contain TSCA CBI. Wildlife International, Ltd, ProjectNo.; 1I2E-208 2- GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT SPONSOR: E.I. du Pont de Nemours and Company TITLE: ^ Transformation Potential in Aerobic and Anaerobic Soils WILDLIFE INTERNATIONAL, LTD. PROJECT NO.: I12E-108 STUDY COMPLETION DATE: March 17, 2008 This study was conducted in compliance with Good Laboratory Practice Standards as published by the U.S. Environmental Protection Agency in 40 CFR Part 792 and OECD Principles of Good Laboratory Practice (ENV/MC/CHEM (98) 17), with the following exceptions: Periodic analyses of well water for potential contaminants were performed using a certified laboratory' and standard U.S. Environmental Protection Agency analytical methods. The characterization of the test substance, and the stability of the test substance under the conditions of storage at the test site, were not determined in accordance with Good Laboratory Practice Standards. Original documentation for the preparation of two combined stocks were not maintained. Documentation of the stocks preparation was re-created from the information on die stock label. STUDY DIRECTOR: Edward C. Schaeid Director of Biodegradation 17 rn/U-ctt U #? DATE b9stn8 ynCfmoO Company Sanitized. Does not contain TSCA CBI. Wildlife International, Ltd. Project No.: 112E-108 -3 - QUALITY ASSURANCE STATEMENT This study was examined for compliance with Good Laboratory Practice Standards as published by the U.S. Environmental Protection Agency in 40 CFR Part 792 and OECD Principles of Good Laboratory Practice (ENV/MC/CHEM (98) 17). The dates of all inspections and audits and the dates that any findings were reported to the Study Director and Laboratory Management were as follows: ACTIVITY: Protocol Stock Solution Preparation DATE CONDUCTED: March 1,2005 March 15,2005 DATE REPORTED TO: STUDY DIRECTOR: MANAGEMENT: March 1,2005 March 11,2005 March 15,2005 March 16,2005 Headspace Sampling March 24,2005 March 24,2005 April 13, 2005 Stock Solution Preparation April 19, 2005 April 19,2005 April 22, 2005 Analytical Data Day 0 Analyses October 10-26,2005 October 26,2005 November 8, 2005 Analytical Data Week 1 Analyses October 10-28, 2005 October 28,2005 November 21,2005 Analytical Data - Week 2 Analyses October 10Novembcr 1,2005 November 1,2005 November 21,2005 Analytical Data - Month 1 Analyses October 0November 1,2005 November 1,2005 November 21,2005 Analytical Data - Month 2 Analyses October 10November 1,2005 November 1, 2005 November 21, 2005 Analytical Data - Month 4 Analyses October 10November 2, 2005 November 2, 2005 December 1,2005 Soil Moisture Determination and Dosing Data October 10December 2,2005 December 2,2005 August 30, 2006 Oxygen Measurement October 17, 2005 October 17, 2005 October 19, 2005 Dosing Viability Controls October 17,2005 October 17,2005 September 26, 2006 Microbial Biomass Sample Processing . October 18, 2005 October 18,2005 November 3, 2006 P-5 Company Sanitized. Does not contain TSCA CBI. Wildlife International, Ltd, Project No.: 112E-108 ACTIVITY: Analytical Sample Processing (6-month) Month 6 Analytical Data Analytical Draft Report 9 and 12 Month Analytical Data and Tables Biological Data and Draft Report Data and Draft Report (including 15,18 and 24 month analytical data) Final Report -4 - QUALITY ASSURANCE STATEMENT (continued) DATE CONDUCTED: DATE REPORTED TO: STUDY DIRECTOR: MANAGEMENT: October 20,2005 November 14-17,2005 November 17-22, 2005 August 21-25 and 28, 2006 October 23 November 9, 2006 October 24 November 2, 2007 October 20, 2005 November 17, 2005 November 22, 2005 August 29, 2006 November 9, 2006 November 2,2007 October 24, 2005 November 28, 2005 December 1, 2005 October 3, 2006 December 18, 2006 November 20,2007 March 17,2008 March 17,2008 March 17, 2008 All inspections were study-based unless otherwise noted. Linda R. Mitchell Director of Regulatory and Ecotox Operations / 7 M/huJ 0C& DATE P-6 Company Sanitized. Does not contain TSCA CBI. Wildlife International, Ltd. Project No.: 112E-108 -5 REPORT APPROVAL SPONSOR: E.I. du Pont de Nemours and Company TITLE: J Transformation Potential in Aerobic and Anaerobic Soils WILDLIFE INTERNATIONAL, LTD. PROJECT NO. : 112E-108 STUDY DIRECTOR: Edward C. Schagrer Director of Biodegradation /7 DATE Q-eoj MANAGEMENT: lUn-rs D , \^ros?e/ Heiuy O. Krueger, Ph.D. ' Director of Aquatic Toxicology/Terrestrial Plants and Insects 3 DATE Willard B. Nixon, Ph? Director of Chemistry DATE Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. 6- - TABLE OF CONTENTS Title Page......................................................................... Good Laboratory Practice Compliance Statement...... Quality Assurance Statement........................................ Report Approval.............................................................. Table of Contents........................................................... Study Information........................................................... Introduction..................................................................... O b je c tiv e ......................................................................... ? Experimental D esign...................................................... Materials and M ethods................................................... Test Substance.......................................................... Measured Analytes................................................... Internal Standards..................................................... Test Soils................................................................... Test Apparatus and Conditions............................... Soil Pre-Incubation................................................... Preparation o f the Test Chambers.......................... Maintenance of Test Chambers............................... Sampling and M easurements.................................. Quality Criteria......................................................... . Viability Assessments............................................. . Results............................................................................. . Test Conditions......................................................... Characterization of Soils.......................................... Sample Processing and Analyses............................ Headspace Analyses.......................................... Soil Analyses...................................................... Stock and Calibration Standard Preparation.... Calibration Curves and Limits of Quantitation. References p.7 Project No.: 112E-108 ...1 ...2 ...3 ...5 ...6 16 17 17 17 18 18 18 21 22 23 23 23 24 25 25 26 26 26 27 27 27 27 29 31 34 p.8 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project no .: 112E-108 -7- TABLE OF CONTENTS .. - Continued - TABLES Table 1. Frequency of Measurements..............................................................................................................35 Table 2. Test Chamber Headspace Oxygen Content..................................................................................... 36 Table 3. Selected Soil Properties..................................................................................................................... 37 Table 4. Soil Viability by Glucose Mineralization:Alfisol...........................................................................38 Table 5. Soil Viability by Glucose Mineralization :Inceptisol..................................................................... 38 Table 6. Soil Viability by Glucose Mineralization:Ultisol...........................................................................39 Table 7. Soil Viability by Glucose Mineralization:Mollisol....................................................................... 39 Table 8. Soil Microbial Biom ass..................................................................................................................... 40 Table 9. Typical GC/MS Operational Parameters for Analysis of 8-2 FTOH in Headspace Gas.............42 Table 10. Typical LC/MS/MS Operational Parameters for Analysis of 8-2 FTA, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA in Soil Extracts........................................................................ 43 Table 11. Typical LC/MS/MS Operational Parameters for Analysis of 8-2 FTOH in Soil Extracts........44 Table 12. Typical LC/MS/MS Operational Parameters for Analysis of 7-3 Acid and 7-2 sFTOH in Soil E x tra c ts ............................................................................................................................................... 45 FIGURES Figure 1. Method flowchart for the analysis o f 8-2 FTOH in the headspace of soil test chambers.........46 Figure 2. Method flowchart for the analysis o f 8-2 FTOH, 7-2 sFTOH, 8-2 FTA, 7-3 Acid, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA in soil extracts............................................................. 47 Figure 3. Representative ion chromatogram for 8-2 FTOH in a low-level (25.0 ng a.i./mL) calibration standard by GC/MS.................................................................................................. 48 P-9 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -8 - TABLE OF CONTENTS - Continued - Project No.: 112E-108 Figure 4. Representative ion chromatogram for 8-2 FTOH in a high-level (500 ng a.i./mL) calibration standard by GC/M S......................................................................................................49 Figure 5. Representative ion chromatogram for 8-2 FTOH in a low-level (10.0 ng a.i./mL) calibration standard by LC/MS/MS................................................................................................50 Figure 6. Representative ion chromatogram for 8-2 FTOH in a high-level (1000 ng a.i./mT.) calibration standard by LC/MS/MS................................................................................................51 Figure 7. Representative ion chromatogram for 7-2 sFTOH in a low-level (5.00 ng a.i./mL) calibration standard by LC/MS/MS................................................................................................52 Figure 8. Representative ion chromatogram for 7-2 sFTOH in a high-level (250 ng a.i./mL) calibration standard by LC/MS/MS................................................................................................53 Figure 9. Representative ion chromatogram for 8-2 FTA in a low-level (0.100 ng a.i./mL) combined PFCA calibration standards by LC/MS/MS..................................................................................54 Figure 10. Representative ion chromatogram for 8-2 FTA in a high-level (5.00 ng a.i./mL) combined PFCA calibration standards by LC/MS/MS..................................................................................55 Figure 11. Representative ion chromatogram for 7-3 Acid in a low-level (0.100 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS.................................................................................... 56 Figure 12. Representative ion chromatogram for 7-3 Acid in a high-level (5.00 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS....................................................................................57 Figure 13. Representative ion chromatogram for 8-2 FTUA in a low-level (0.100 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS................................................................. 58 Figure 14. Representative ion chromatogram for 8-2 FTUA in a high-level (5.00 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS................................................................. 59 Figure 15. Representative ion chromatogram for PFOA in a low-level (0.100 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS................................................................. 60 Figure 16. Representative ion chromatogram for PFOA in a high-level (5.00 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS................................................................. 61 Figure 17. Representative ion chromatogram for PFNA in a low-level (0.100 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS......................................... 62 Company Sanitized. Does not contain TSCA CB1. W ildlife International, Ltd. Project No.: 112E-108 -9 - TABLE OF CONTENTS - Continued - Figure 18. Representative ion chromatogram for PFNA in a high-level (5.00 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS.................................................................. 63 Figure 19. Representative ion chromatogram for PFDA in a low-level (0.100 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS.................................................................. 64 Figure 20. Representative ion chromatogram for PFDA in a high-level (5.00 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS.................................................................. 65 Figure 21. Representative ion chromatogram for PFUA in a low-level (0.100 ng a.i./mL) combined PFCA calibration standard by GC/MS ........................................................................66 Figure 22. Representative ion chromatogram for PFUA in a high-level (5.00 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS.................................................................................... 67 Figure 23. Representative calibration curve for 8-2 FTOH by G C /M S........................................................ 68 Figure 24. Representative calibration curve for 8-2 FTOH by LC/MS/MS...................................................69 Figure 25. Representative calibration curve for 7-2 sFTOH by LC/MS/MS.................................................70 Figure 26. Representative calibration curve for 8-2 FTA by LC/M S/M S.....................................................71 Figure 27. Representative calibration curve for 7-3 Acid by LC /M S/M S.................................................... 72 Figure 28. Representative calibration curve for 8-2 FTUA by LC/M S/M S..................................................73 Figure 29. Representative calibration curve for PFOA by LC/MS/MS .-....................................................... 74 Figure 30. Representative calibration curve for PFNA by LC/MS/MS......................................................... 75 Figure 31. Representative calibration curve for PFDA by LC /M S/M S........................................................ 76 Figure 32. Representative calibration curve for PFUA by LC/MS/MS......................................................... 77 Figure 33. Representative ion chromatogram for 8-2 FTOH in the sampled headspace (Ci8 cartridge extract) from a Day 0 untreated control soil by GC/MS ............................................................. 78 Figure 34. Representative ion chromatogram for 8-2 FTOH in the soil extract from a Day 0 untreated control soil by LC/MS/MS..........................................................................................79 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 - 10TABLE OF CONTENTS - Continued - Figure 35. Representative ion chromatogram for 7-2 sFTOH in the soil extract from a Day 0 untreated control soil by LC/M S/M S............................................................................................80 Figure 36. Representative ion chromatogram for 8-2 FTA in the soil extract from a Day 0 . untreated control soil by LC/M S/M S............................................................................................81 Figure 37. Representative ion chromatogram for 7-3 Acid in the soil extract from a Day 0 untreated control soil by LC/M S/M S......... a............................................................................... 82 Figure 38. Representative ion chromatogram for 8-2 FTUA in the soil extract from a Day 0 untreated control soil by LC/M S/M S............................................................................................83 Figure 39. Representative ion chromatogram for PFOA in the soil extract from a Day 0 untreated control soil by LC/MS/MS.............................................................................................................84 Figure 40. Representative ion chromatogram for PFNA in the soil extract from a Day 0 untreated control soil by LC/MS/MS............................................................................................................85 Figure 41. Representative ion chromatogram for PFDA in the soil extract from a Day 0 untreated control soil by LC/MS/MS................ '............................................................................................86 Figure 42. Representative ion chromatogram for PFUA in the soil extract from a Day 0 untreated control soil by LC/MS/MS............................................................................................................ 87 Figure 43. Representative ion chromatograms for 8-2 FTOH in the sampled headspace (Cig cartridge extract) from a Month 24 untreated control soil by GC/M S.......................................................88 Figure 44. Representative ion chromatogram for 8-2 FTOH in the soil extract from a Month 24 untreated control soil by LC/M S/M S........................................................................................... 89 Figure 45. Representative ion chromatogram for 7-2 sFTOH in the soil extract from a Month 24 untreated control soil by LC/M S/M S..................... ;..................................................................... 90 Figure 46. Representative ion chromatogram for 8-2 FTA in the soil extract from a Month 24 untreated control soil by LC/M S/M S............................................................................................91 Figure 47. Representative ion chromatogram for 7-3 Acid in the soil extract from a Month 24 untreated control soil by LC/M S/M S........................................................................................... 92 Figure 48. Representative ion chromatogram for 8-2 FTUA in the soil extract from a Month 24 untreated control soil by LC/MS/MS........................................................................................ 93 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -11 TABLE OF CONTENTS - Continued - Figure 49. Representative ion chromatogram for PFOA in the soil extract from a Month 24 untreated control soil by LC/M S/M S.............................................................................................94 Figure 50. Representative ion chromatogram for PFNA in the soil extract from a Month 24 untreated control soil by LC/M S/M S.............................................................................................95 Figure 51. Representative ion chromatogram for PFDA in the soil extract from a Month 24 untreated control soil by LC/M S/M S.............................................................................................96 Figure 52. Representative ion chromatogram for PFUA in the soil extract from a Month 24 untreated control soil by LC/M S/M S.............................................................................................97 Figure 53. Representative ion chromatograms for 8-2 FTOH in the sampled headspace (C18 cartridge extract) from a Day 0 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by GC/MS................................. ....................................................................................98 Figure 54. Representative ion chromatogram for 8-2 FTOH in the soil extract from a Day 0 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS............... 99 Figure 55. Representative ion chromatogram for 8-2 FTA in the soil extract from a Day 0 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS............. 100 Figure 56. Representative ion chromatogram for 8-2 FTUA in the soil extract from a Day 0 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS............. 101 Figure 57. Representative ion chromatogram for PFOA in the soil extract from a Day 0 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS.............102 Figure 58. Representative ion chromatogram for PFNA in the soil extract from a Day 0 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS.............103 Figure 59. Representative ion chromatogram for PFDA in the soil extract from a Day 0 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS.............104 Figure 60. Representative ion chromatogram for PFUA in the soil extract from a Day 0 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS.............105 Figure 61. Representative ion chromatograms for 8-2 FTOH in the sampled headspace (Ci8cartridge extract) from a Month 12 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by GC/MS............................................................................................................... 106 Company Sanitized. Does not contain TSCA CB1. W ildlife International, Ltd. Project No.: 112E-108 -12TABLE OF CONTENTS - Continued - Figure 62. Representative ion chromatogram for 8-2 FTOH in the soil extract from a Month 12 fortified (250 pg 8-2 FTOH/kg and 10.0 fig PFCAs/kg) control soil by LC/MS/MS.............107 Figure 63. Representative ion chromatogram for 8-2 FTA in the soil extract from a Month 12 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS.............108 Figure 64. Representative ion chromatogram for 8-2 FTUA in the soil extract from a Month 12 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS.............109 Figure 65. Representative ion chromatogram for PFOA in the soil extract from a Month 12 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS.............110 Figure 66. Representative ion chromatogram for PFNA in the soil extract from a Month 12 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS.............I l l Figure 67. Representative ion chromatogram for PFDA in the soil extract from a Month 12 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS.............112 Figure 68. Representative ion chromatogram for PFUA in the soil extract from a Month 12 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS.............113 Figure 69 Representative ion chromatograms for 8-2 FTOH in the sampled headspace (Qg cartridge extract) from a Day 0 sterile soil treated with 200 mg/kg H-26634 by GC/MS...................... 114 Figure 70. Representative ion chromatogram for 8-2 FTOH in the soil extract from a Day 0 sterile soil treated with 200 mg/kg H-26634 by LC/M S/M S............................................................... 115 Figure 71. Representative ion chromatogram for 8-2 FTA in the soil extract from a Day 0 sterile soil treated with 200 mg/kg Q ^by LC/M S/M S.................................................................116 Figure 72. Representative ion chromatogram for 8-2 FTUA in the soil extract from a Day 0 sterile soil treated with 200 mg/kgQ J b y LC/M S/M S.................................................................117 Figure 73. Representative ion chromatogram for PFOA in the soil extract from a Day 0 sterile soil treated with 200 mg/kg_ J y LC/M S/M S................................................................ 118 Figure 74. Representative ion chromatogram for PFNA in the soil extract from a Day 0 sterile soil treated with 200 mg/kg ^ by LC/M S/M S............................................................... 119 Figure 75. Representative ion chromatogram for PFDA in the soil extract from a Day 0 sterile soil treated with 200 mg/kg' J b y LC/MS/MS.............................................................. 120 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -13 TABLE OF CONTENTS - Continued - Figure 76. Representative ion chromatogram for PFUA in the soil extract from a Day 0 sterile soil treated with 200 mg/kg [_ 3 by LC/MS/MS................................................................. 121 Figure 77. Representative ion chromatograms for 8-2 FTOH in the sampled headspace (Cig cartridge extract) from a Month 12 sterile soil treated with 200 mg/kg J b y GC/MS................122 Figure 78. Representative ion chromatogram for 8-2 FTOH in the soil extract from a Month 12 sterile soil treated with 200 mg/kg Jby LC/MS/MS................................................................ 123 Figure 79. Representative ion chromatogram for 8-2 FTA in the soil extract from a Month 12 sterile soil treated with 200 mg/kgC 3 by LC/MS/MS................................................................. 124 Figure 80. Representative ion chromatogram for 8-2 FTUA in the soil extract from a Month 12 sterile soil treated with 200 m g/kg 3 by LC/MS/MS...................................................................125 Figure 81. Representative ion chromatogram for PFOA in the soil extract from a Month 12 sterile soil treated with 200 mg/kg 3 ^ y LC/MS/MS..................................................................126 Figure 82. Representative ion chromatogram for PFNA in the soil extract from a Month 12 sterile soil treated with 200 m g/kg^ 3 by LC/MS/MS................................................................... 127 Figure 83. Representative ion chromatogram for PFDA in the soil extract from a Month 12 sterile soil treated with 200 m g/kg^ ])by LC/MS/MS................................................................. 128 Figure 84. Representative ion chromatogram for PFUA in the soil extract from a Month 12 sterile soij treated with 200 mg/kg Q 3by LC/MS/MS..................................................................129 Figure 85. Representative ion chromatograms for 8-2 FTOH in the sampled headspace (C18 cartridge extract) from a Day 0 live soil treated with 200 mg/kg by G C /M S..........................130 Figure 86. Representative ion chromatogram for 8-2 FTOH in the soil extract from a Day 0 live soil treated with 200 m g/kg 3^y LC/MS/MS..................................................................131 Figure 87. Representative ion chromatogram for 7-2 sFTOH in the soil extract from a Day 0 live soil treated with 200 mg/kgQ 3by LC/MS/MS...................................................................132 Figure 88. Representative ion chromatogram for 8-2 FTA in the soil extract from a Day 0 live soil treated with 200 m g/kg j)by LC/MS/MS..................................................................133 JFigure 89. Representative ion chromatogram for 7-3 Acid in the soil extract from a Day 0 live soil treated with 200 mg/kg by LC/MS/MS.................................................. 134 Company Sanitized. Does not contain TSCA CBI. x International, Ltd. Project No.: 112E-108 - 14TABLE OF CONTENTS - Continued - Figure 90. Representative ion chromatogram for 8-2 FTUA in the soil extract from a Day 0 live soil treated with 200 mg/kg *3by LC/MS/MS................................................................ 135 Figure 91. Representative ion chromatogram for PFOA in the soil extract from a Day 0 live soil treated with 200 mg/kg [ ^by LC/MS/MS.................... 136 Figure 92. Representative ion chromatogram for PFNA in the soil extract from a Day 0 live soil treated with 200 mg/kg[ ^by LC/MS/MS................................................................ 137 Figure 93. Representative ion chromatogram for PFDA in the soil extract from a Day 0 live soil treated with 200 m g / k g "3 by LC/MS/MS............................................................... 138 Figure 94. Representative ion chromatogram for PFUA in the soil extract from a Day 0 live soil treated with 200 m g /k ^ ~0by LC/MS/MS........................................ ........................139 Figure 95. Representative ion chromatograms for 8-2 FTOH in the sampled headspace (Ci8 cartridge extract) from a Month 24 live soil treated with 200 m g/kgf GC/M S................... 140 Figure 96. Representative ion chromatogram for 8-2 FTOH in the soil extract from a Month 24 live soil treated with 200 mg/kg [ ^ by LC/MS/MS............................................................... 141 Figure 97. Representative ion chromatogram for 7-2 sFTOH in the soil extract from a Month 24 live soil treated with 200 mg/kg 3 by LC/MS/M s ............................................................... 142 Figure 98. Representative ion chromatogram for 8-2 FTA in the soil extract from a Month 24 live soil treated with 200 m g/kg^' ' ^yL O M S /M iS ............................................................... 143 Figure 99. Representative ion chromatogram for 7-3 Acid in the soil extract from a Month 24 live soil treated with 200 mg/kg )jy LC/MS/MS................................................................144 Figure 100. Representative ion chromatogram for 8-2 FTUA in the soil extract from a Month 24 live soil treated with 200 m g/kg ]) by LC/MS/MS...............................................................145 Figure 101. Representative ion chromatogram for PFOA in the soil extract from a Month 24 live soil treated with 200 mg/kg Jb y LC/MS/MS...............................................................146 Figure 102. Representative ion chromatogram for PFNA in the soil extract from a Month 24 live soil treated with 200 mg/kg Q }by LC/MS/MS...........>................................................. 147 Figure 103. Representative ion chromatogram for PFDA in the soil extract from a Month 24 live soil treated with 200 mg/kg Q Joy LC/MS/MS............................................................ 148 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 - 15 - TABLE OF CONTENTS - Continued - Figure 104. Representative ion chromatogram for PFUA in the soil extract from a Month 24 live soil treated with 200 mg/kgfy _3by LC/MS/MS..................................................... APPENDICES Appendix I. Measured Concentration o f Selected Analytes (pg/kg Soil Dry W eight)................ Appendix II. Measured Concentration of Selected Analytes (pmol/kg Soil Dry W eight)........... Appendix III. Example Calculations................................................................................................... Appendix IV. Duration of Incubation................................................................................................. 149 150 223 296 298 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -16- STUDY INFORMATION Study Initiation Date: Experimental Start Date: Experimental Termination Date: Study Completion Date: 10 March 2005 11 March 2005 07 September 2007 17 March 2008 p. 17 Project]*,, m s -io s Study Director: Sponsor: Sponsor Representatives: Study Personnel: Edward C. Schaefer E.I. du Pont de Nemours and Company William Berti and Bogdan Szostek Edward C. Schaefer, B.S., Director of Biodegradation Raymond L. Van Hoven, Ph.D., Scientist, Chemistry Joel I. Stenzel, B.S., Senior Chemist R. Scott Flaggs, B.S., Biologist, Biodegradation Abul Siddiqui, B.S., Scientist, Biodegradation Frank Lezotte, B.S., Senior Chemist, Chemistry David L. Weiss, M.S., Chemist, Chemistry William Schutt, B.S., Chemist, Chemistry John R. Murrell, B.S., Senior Chemist Willard B. Nixon, Ph.D., Director o f Chemistry Henry O. Krueger, Ph.D., Director of Aquatic Toxicology/Terrestrial Plants and Insects Molly E. Matthews, Biologist, Biodegradation Jon A. MacGregor, B.S., Scientist Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -17- INTRODUCTION This report describes a laboratory research study conducted to assess aerobic and anaerobic transformation o f Din soil systems. This study was conducted by Wildlife International, Ltd. for E.I. du Pont de Nemours and Company at the Wildlife International, Ltd. research facility in Easton, Maryland. The raw data generated by Wildlife International, Ltd. and the original final report final report will be archived by the study sponsor. A certified copy will be retained under Project Number 112E-108 in the archives located at on the Wildlife International, Ltd. site. OBJECTIVE The objective of the research study was to assess the potential for transformation of the test substance in aerobic and anaerobic soils. EXPERIMENTAL DESIGN The test was conducted with four test soils under aerobic conditions. The study was initially designed to set-up to also include four soils under anaerobic conditions, however a check of the system indicated that the test chamber closures did not exclude air. The systems initially started under anaerobic conditions up to and including month 6 are included in this report because they were extracted and analyzed as planned. Four groups were established for each soil type and condition (aerobic or anaerobic): (1) untreated (control) live soil; (2) 200 mg test substance/kg dw treated live soil; (3) 200 mg test substance/kg dw treated sterile soil; (4) 250 pg 8-2 telomer B alcohol/kg dw treated sterile soil; 10 pg 8-2 telomer B acid /kg dw; 10 pg 8-2 unsaturated telomer B acid/kg dw; and 10 pg perfluorooctanoic acid/kg dw, heptadecafluorononaoic acid, nonadecafluorodecanoic acid, and perfluoroundecanoic acid at 10 pg/kg dw all added to sterile soil. The test systems reported here were incubated in sealed containers at approximately 20C for at approximately 24 months. Two incubation chambers from each of the groups were removed at appropriate time intervals and the soil samples were extracted and analyzed for potential metabolites. In addition to the day zero samples, eight samplings were performed with all of the groups. Three additional sampling intervals were performed with only the untreated control (1) and 200 mg test substance/kg dw treated live soil (2) groups. Company Sanitized. Does not contain TSCA CBI. Wildlife InternationalLtd. ProjectNo.: 112E-108 - 18- Additional untreated and test substance treated soil chambers were prepared for use as matrix fortification samples, biomass determinations, viability controls and to monitor aerobic conditions as necessary. The test groups were prepared using 25 grams (dry weight equivalent) of soil. While this amount o f soil is less than the 50 to 200 grams specified in the OECD 307 guideline, it was chosen to allow for 1) the extraction of the entire test chamber contents and internal surfaces; 2) sufficient headspace to minimize the need for active aeration which could result in a loss of potential transformation products. METHODS AND MATERIALS The test system and study conditions are based on the OECD Guideline for Testing of Chemicals, Guideline 307, Aerobic and Anaerobic Transformation in Soil (1). As this guideline is designed for low molecular weight substances, but not for polymers, adaptations o f the method may be necessary for feasibility reasons. Nevertheless, the study was carried out in such a way that the recommendations given in the guideline were followed as closely as possible. Test Substance The following substance was used in this study: rot ) Date received: 2 November 2004 f' Wildlife International Ltd. ID: 6918 1 Measured Analytes Name: 8-2 Telomer B Acid, 8-2 Fluorotelomer Acid Synonym used in Report: 8-2 FTA CAS Name: Decanoic acid, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro-(8CI,9CI) CAS Number: 27854-31-5 Molecular Weight: 478.1 g/mole ID: H-26210 Date received: 1 September 2004 . Expiration/reanalysis date: 12 October 2007 Purity: 97%; 3% 2H-Hexadecafluoro-2-Decanoic Acid Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 - 19- Description: Solid Wildlife International Ltd. ID: 6826 Name: 8-2 Telomer B Alcohol, 8-2 Fluorotelomer Alcohol Synonym used in Report: 8-2 FTOH CAS Name: 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro- (7CI, 8CI, 9CI) CAS Number: 678-39-7 Molecular Weight: 464.11 g/mole ID: H-24691 Date received: 1 September 2004 Expiration/reanalysis date: 12 October 2007 Purity: 99.2% Description: Solid Wildlife International Ltd. ID: 6828 Name: 8-2 Unsaturated Telomer B Acid, 8-2 Fluorotelomer Unsaturated Acid Synonym used in Report: 8-2 FTUA CAS Name: 2-Decenoic acid, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-hexadecafluoro- (9CI) CAS Number: 70887-84-2 Molecular Weight: 458.1 g/mole ID: H-26211 Date received: 1 September 2004 Expiration/reanalysis date: 12 October 2007 Purity: 98%; 0.5% 8-2 FTOH; 1.5% unknown Description: Solid Wildlife International Ltd. ID: 6829 Name: N-Perfluorooctanoic Acid Synonym used in Report: PFOA CAS Name: Octanoic acid, pentadecafluoro- (8CI, 9CI) CAS Number: 335-67-1 Molecular Weight: 414.07 g/mole ID: H-24749 Date received: 10 September 2004 Expiration/reanalysis date: 12 October 2007 Purity: 99.2% Description: Solid Wildlife International Ltd. ID: 6849 Name: Heptadecafluorononaoic Acid, Perfluorononanoic Acid Synonym used in Report: PFNA CAS Name: Nonanoic acid, heptadecafluoro-(8CI, 9CI) CAS Number: 375-95-1 Molecular Weight: 464.08 g/mole ID: H7568 Date received: 30 November 2004 Expiration/reanalysis date: 12 October 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -20- Purity: 99+% Description: Solid Wildlife International Ltd. ID: 6944 , Name: Nonadecafluorodecanoic Acid, Perfluorodecanoic Acid Synonym used in Report: PFDA CAS Name: Decanoic acid, nonadecafluoro (6CI, 7CI, 8CI, 9CI) CAS Number: 335-76-2 Molecular Weight: 514.08 g/mole ED: R11K Date received: 30 November 2004 Expiration/reanalysis date: 12 October 2007 Purity: 99+% Description: Solid Wildlife International Ltd. ID: 6943 Name: Perfluoroundecanoic Acid, Perfluoroundecanoic Acid Synonym used in Report: PFUA CAS Name: Undecanoic acid, heneicosafluoro-,ammonium salt (9CI) CAS Number: 4234-23-5 Molecular Weight: 564.09 g/mole ID: Q30G Date received: 30 November 2004 Expiration/reanalysis date: 12 October 2007 Purity: 99+% Description: Solid Wildlife International Ltd. ID: 6945 Name: 2H, 2H, 3H, 3H Pentadecafluoro-Decanoic acid Synonym used in Report: 7-3 Acid CAS Name: Decanoic acid, 4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-pentadecafluoro- CAS Number: 812-70-4 . Molecular Weight: 442.12 g/mole ID :26833 Date received: 20 April 2006 Expiration/reanalysis date: Not provided Purity: Not provided Description: Solid Wildlife International Ltd. ID: 7592 Name: 1-Perfluoro heptyl ethanol, 7-2 Secondary Fluorotelomer Alcohol Synonym used in Report: 7-2 sFTOH CAS Name: Not provided CAS Number: Not provided Molecular Weight: 414.11 g/mole ID :27497 Lot: 72SFTOHGA05 Company Sanitized. Does not contain TSCA CBI. Wildlife International, Ltd. -21 - Date received: 20 April 2006 Expiration/reanalysis date: Not provided Purity: Not provided Description: Liquid Wildlife International Ltd. ID: 7593 Internal Standards Name: N-Perfluorooctanoic Acid [l,2-di-13C] Synonym used in Report: 2-13CPFOA CAS Name: NA CAS Number: NA ID: H-25617 Dates received: 1 September 2004 and 20 April 2006 Expiration/reanalysis date: 12 October 2007 and 31 January 2007 Purity: 96.4% (not given for WIL 7591) Description: Solid Wildlife International Ltd. ID: 6827, 7591 Standard Reanalysis Date: August 2007 Purity: Confirmed Expiration Date: August 2010 Name: ID, ID, 2D, 2D, 3-13C-Heptadecafluorodecanol Synonym used in Report: HDFD CAS Name: NA CAS Number: NA ID: H-25433 Dates received: 10 September 2004 and 20 April 2006 Expiration/reanalysis date: 12 October 2007 Purity: 100% (not given for WIL 7590) Description: Solid Wildlife International Ltd. IDs: 6850, 7590 p. 22 Project No.: 112E-108 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -22- Test Soils Four freshly collected United States (U.S.) soils were used to evaluate the test substance under aerobic and anaerobic conditions. The soils were collected from each of the following soil orders: Soil O rder Percent of US Land* Alfisol 13 Mollisol . 25 Inceptisol 16 Ultisol 13 Percent o f total land in the U S, from Foth, H.D. 1990. Fundamentals o f Soil Science 8 ed. John W iley & Sons, N ew York) The soils were processed between 6 and 22 days after collection. Processing included removing vegetation, larger soil fauna, stones and passing the soil through a 2 mm sieve. The soil used in the sterile groups was sterilized by cobalt irradiation. The soils were stored in the dark at 4 2 C. Characterization of the soils was conducted by Agvise Laboratories (Northwood, North Dakota, USA). The following is a list of the minimum physicochemical properties of the soil. Texture (i.e., percentage of sand, silt and clay) (NUT.02.06) pH (NUT.02.05) Organic carbon (NUT.20.20) Bulk density (NUT.02.10) Field moisture capacity (% moisture at 1/3 bar) Cation exchange capacity (NUT.02.03) The percent moisture and water holding capacity (ISO 14240-2; Annex A) of each of the soil types was determined. In addition, the microbial biomass (ISO 14240-2; fumigation-extraction) o f a live sample of each soil type was determined. The soil microbial biomass was determined at the beginning of the test prior to adding the test substance and in test and control soil samples at 4, 6 and 12 months using the fumigation-extraction method. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -23 - Test Apparatus and Conditions The test chambers were 250 mL glass serum bottles (Wheaton, Milleville NJ). The chambers were sealed with butyl rubber septa (Wheaton, Milleville NJ) that were covered with aluminum foil and aluminum crimp caps (Wheaton, Milleville NJ). The test chambers were identified by project number, test substance ID, test concentration, and unique identifier and incubated statically at approximately 20 2C. Soil Pre-Incubation The soil moisture of each test soil content was adjusted to 40 to 60% o f water holding capacity (which is equivalent to a pF of between 2.0 and 2.5, or from 0.1 to 0.33 bar). The test soil then was allowed to warm to the test temperature for at least 2 days. A pre-incubation period of at least 7 days for the aerobic soils and at least 14 days for the anaerobic soils was performed under the appropriate conditions (i.e. temperature, soil moisture content, aerobic or anaerobic). Approximately 25 grams dry weight equivalent of test soil was added to the test chambers. Sterile soil treatments were dosed at approximately 200 mg/kg (dw) with both chloramphenicol (Aldrich, 98%, CAS 56-75 7) and cycloheximide (Sigma, min. 94%, CAS 66-81-9) to inhibit microbial growth. The chambers to be incubated under aerobic conditions were sealed with aluminum foil-lined septa and incubated. The chambers to be incubated under anaerobic conditions were flushed with anaerobic mixed gas, sealed with aluminum foil-lined septa and incubated. The soil moisture content was maintained in the optimal microbial growth range of 40 to 60% water holding capacity (WHC). The soil moisture content o f each chamber was checked and adjusted, if necessary, once during the pre-incubation period by weighing the test vessels. Sterile-filtered demineralized water (degassed sterile-filtered demineralized water for the anaerobic soils) was added as necessary to compensate for water losses. Preparation of the Test Chambers The soil moisture content was checked and adjusted, if necessary, prior to the addition of the test substance. Sterile-filtered demineralized water (degassed sterile-filtered demineralized water for the anaerobic soils) was added as necessary to compensate for water. Anaerobic treatments and controls were prepared within an anaerobic environment and stored in a temperature controlled room. The test substance was applied to the soil within the test chambers as described below. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -24- Background Blank Control: Soils with no test substance added was tested in duplicate to check for background concentrations of analytes (see Sampling and Measurements). The entire bottle was extracted after a sample of the headspace had been taken. Tffst Substance: The test substance dosed treatments were prepared by dosing approximately 25 grams (dry weight equivalent) of soil with sufficient test substance to deliver 200 mg/kg dry weight. The test substance was administered by direct weight addition. The test chambers were sealed with septum lined with aluminum foil, mixed and incubated. The entire bottle was extracted after a sample of the headspace had been taken. Abiotic Controls: The abiotic controls were prepared by dosing approximately 25 grams (dry weight equivalent) of 6Co-sterilized soil with sufficient test substance to deliver 200 mg/kg dry weight. The test substance was administered by direct weight addition. The entire bottle was extracted after a sample of the headspace had been taken. Spike Recovery Controls: The spike recovery controls were prepared by dosing approximately 25 grams (dry weight equivalent) of Co-sterilized soil with appropriate volumes of 8-2 FTOH stock (250 )ig/mT. in ethanol) and fluorinated acid stocks (10 pg/mL in water). The stocks were injected directly into the soil using a glass microsyringe. The test chambers were immediately sealed with septum lined with aluminum foil and the contents of the chambers were mixed. The entire bottle was extracted after a sample of the headspace had been taken. Viability Controls (untreated!: The metabolic activity of untreated test soil was assessed on a monthly basis. Duplicate incubation chambers for each test soil and condition (aerobic and anaerobic) were dosed at approximately 100 mg/kg dw with a combination of radiolabeled and non-labelled glucose. The evolved 14C 0 2 (aerobic and anaerobic conditions) and 14OELt (anaerobic conditions) was measured and the percent biodegradation calculated. Aerobic Controls (Treated!: The aerobic controls were prepared by dosing approximately 25 grams (dry weight equivalent) of soil with sufficient test substance to deliver 200 mg/kg dry weight. The test substance was administered by direct weight addition. The test chambers were sealed with septum lined with aluminum foil, mixed and incubated. The oxygen content of a sacrificial chamber was measured at monthly intervals. Maintenance of Test Chambers The soil moisture content was maintained in the optimal microbial growth range of 40 to 60% water holding capacity (WHC; a pF of between 2.0 and 2.5, or from 0.1 to 0.33 bar). The soil moisture content was initially checked and adjusted, if necessary, at 1 to 2 week intervals by weighing the test vessels but was changed to monthly intervals based on the observed weight losses. Adding sterile-filtered demineralized water (degassed sterile-filtered demineralized water for the anaerobic soils) compensated for water losses. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -25 - The oxygen content in the headspace of two aerobic control chambers was assessed on a monthly basis to ensure aerobic conditions. If the mean measured oxygen content within the control chambers was less than 19%, aerobic test chambers was aerated with filter-sterilized, oil-free air. Test chambers did not have to be opened to add water or for monitoring purposes. Soil moisture content was adjusted by injecting the appropriate amount of sterile water through the septa and onto soil. The headspace oxygen content was measured by inserting the probe of an oxygen analyzer through the septa and into the headspace of the aerobic control chamber. Sampling and Measurements Duplicate chambers from each of the control, treated and spike recovery soils were extracted and analyzed. Sampling intervals were at 0, 1 and 2 weeks and 1, 2, 4, 6, 9 12, 15, 18 and 24 months for aerobic. Potential volatile transformation products in the headspace of the soils chambers were collected using a C l8 cartridge. At each sampling time prior to opening the test vessel, the septum was pierced using a needle connected to a C l8 cartridge and syringe. A 20-mL volume of headspace gas from within the chamber was pulled through the C l8 cartridge using the attached syringe. The Cl 8 was subsequently extracted with ACN and analyzed. Sample extracts were stored at -10C or lower if analysis is delayed more than 24 hours. Extracts were analyzed for: 1. 8-2 FTOH 2. 8-2 FTA 3. 8-2 FTUA 4. PFOA 5. PFNA 6. PFDA 7. PFUA 8. 7-2 sFTOH 9. 7-3 Acid Quality Criteria Recovery for a given sampling time point should range between 70 to 120% for the analysis of the 8-2 FTOH, 8-2 FTA, 8-2 FTUA, PFNA, PFDA, PFUA, and PFOA from the spike recovery control samples. These ranges should be interpreted as targets and should not be used as criteria for acceptance o f the test. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -26- Viability Assessments On a monthly basis, duplicate incubation chambers for each test soil and condition were dosed with 1 mL of the stock solution containing both radiolabelled and non-labelled forms of d-glucose which resulted in a concentration of approximately 3000 mg/kg dw. The headspace of each of the aerobic test chambers was continuously purged at an air-flow rate of approximately 1 bubble per second. The air exiting the test chambers was be passed through a series of gas washing bottles with at least one containing approximately 100 mL of 1.5 N KOH. The headspace of each of the anaerobic chambers was continuously purged with a flow of nitrogen and passed through a gas collection system consisting of two sets of C 0 2 traps and a combustion apparatus. The displaced gases initially passed through one empty bottle followed by two bottles each containing approximately 100 mL of 1.5N KOH (C 02 trapping solution) followed by another empty bottle. The gas was combined with a flow of oxygen and channeled through a quartz column that was packed with cupric oxide and maintained at approximately 800C in a tube furnace to combust methane to C 0 2. The gas exiting the combustion column was passed through an empty bottle followed by two additional C 0 2 traps. The C 02 traps connected to the aerobic chambers and the 1st C 0 2 trap in each set (before and after furnace) of the anaerobic mineralization apparatus were removed for analysis and replaced at least weekly. Three replicate 1 mL aliquots of C 0 2 trapping solution were analyzed for radioactivity by liquid scintillation counting (LSC; Packard Tri-Carb Liquid Scintillation Counter). The assessment was terminated when 50% of the initial activity was recovered as mineralization products or after 28 days. RESULTS Test Conditions Room temperatures during the acclimation period for all four soils ranged from 18 to 22 C. Temperatures recorded during the test for all four soils ranged from 17 to 25 C. Incubation temperatures outside of the range 18 to 22 C were observed three times over the duration of the study. The frequency of measurements performed on the test soils is presented in Table 1. The moisture contents of the soils were adjusted as needed based on soil moisture content determinations. Each vessel required water additions at least once during the initial 12-month test period, but no additions were required for shorter incubation times. The maximum amounts of water added to any vessel over 12 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -27- and 24 month periods were 1.2 and 3.9 mL, respectively. The oxygen content in the headspace of the two aerobic control chambers used to assess aerobic conditions is presented in Table 2. Characterization of Soils The test soils were characterized before the start o f acclimation, and the results are presented in Table 3. The results of the viability assessments are presented in Tables 4-7. The results of microbial biomass determinations performed at the start of the test, during the test, and at the end o f the test are presented in Table 8. Sample Processing and Analysis Soil chambers were either processed immediately upon receipt or removed from frozen storage and prepared for analysis of the candidate analytes 8-2 FTOH, 7-2 sFTOH, 8-2 FTA, 7-3 Acid, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA. Headspace Analyses Prior to opening the soil chambers, a 20-mL volume o f headspace gas was sampled from each chamber for 8-2 FTOH using a gas-tight syringe (Becton Dickinson, 10 mL with Luer-LokTM tip), hypodermic needle (Becton Dickinson, 18G 154) and a C]8 cartridge (600 mg, Alltech Maxi-Clean). Each sampled C!8 cartridge was extracted with 10 mL of acetonitrile (Burdick & Jackson, HPLC-Grade, CAS No. 75-05-8). The extracts were fortified with 100 pL of a 0.100 mg HDFD/mL internal standard in acetonitrile to yield an internal standard concentration of 100 ng/mL in each extract. The fortifications were performed using a gas-tight syringe (Hamilton 81000 Series). An aliquot o f each sample extract was transferred into a glass autosampler vial, sealed and analyzed for 8-2 FTOH by GC/MS. A method outline and typical instrumental conditions for analysis of 8-2 FTOH in the headspace of the soil chambers are provided in Figure 1 and Table 9, respectively. Soil Analyses Following headspace sampling, the crimp seal from each soil chamber was removed and the aluminum foil liner was placed inside the test vessel. A 125-milliliter aliquot of acetonitrile extraction solvent (measured with a graduated cylinder) followed by a 10-milliliter aliquot of 200 mM sodium hydroxide (measured with a serological pipette and prepared with Aldrich, Lot No. 14227TO NaOH or Fisher, Lot No. 926471 and Burdick & Jackson HPLC-Grade reagent water, CAS Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -28- No. 7732-18-5) were added to each test vessel containing the soil sample. The acetonitrile extraction solvent contained 100 ng/mL of HDFD internal standard and was prepared by fortifying four liters of acetonitrile measured with a graduated cylinder with 400 pL of a 1.00 mg HDFD/mL primary stock' in isopropyl alcohol (Burdick & Jackson, HPLC-Grade, CAS No. 67-63-0) and a gas-tight syringe. The vessels were re-sealed and placed onto a gyratory shaker table (New Brunswick Scientific, Model G10) set for 250 rpm for three hours at room temperature. The vessels were removed from the gyratory table and allowed to settle for several minutes at ambient temperature. Using a volumetric pipette, a 10-mL aliquot o f the extract from each vessel was transferred into a separate polypropylene centrifuge tube (Nalgene, 50-mL polypropylene Oak Ridge type, Catalog No. 3119-0050) containing 25 milligrams of ENVI-Carb (Supelco, 120/400). The test vessel, including the remainder of the extract, was replaced into frozen storage (operating range -10 to -20C). The extract aliquots were centrifuged (Sorvall RC5BPlus fitted with Sorvall SS-34 rotor) for 10 minutes at 12000 rpm (17000 g) and 20 degrees C. An aliquot of supernatant was diluted with reagent water containing 1.00 ng/mL of 2-13C PFOA internal standard and in the proportions 1 part extract: 3 parts dilution water and the diluted extract was analyzed for 8-2 FTA, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA by HPLC tandem mass spectrometry (LC/MS/MS). The dilutions were performed directly in HPLC autosampler vials using calibrated micropipettes. The dilution water was freshly prepared by fortifying 100 mL of reagent water with 100 pL o f a 2-13C PFOA secondary stock in acetonitrile using a borosilicate glass, Class A volumetric flask and either a gas-tight syringe or calibrated micropipettes. A second aliquot of supernatant was diluted with reagent water containing 1.00 ng/mL of HDFD internal standard and in the proportions 1 part extract: 1 part dilution water and the diluted extract was analyzed for 8-2 FTOH by LC/MS/MS. The dilutions were performed directly in HPLC autosampler vials using calibrated micropipettes. The dilution water was freshly prepared by fortifying 100 mL of reagent water with 100 pL of a HDFD secondary stock in acetonitrile using a borosilicate glass, Class A volumetric flask and gas-tight syringe. The remainder of the soil extract supernatant was decanted into glass scintillation vials (Fisher, 20-mL disposable, Catalog No. 03-337 7) and placed in frozen storage. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -29- At the request of the Sponsor, two additional analytes, 7-2 sFTOH and 7-3 Acid, were screened for in selected stored soil extracts collected prior to the Month 18 sampling interval using LC/MS/MS. The earlier sampling intervals included Day 0 and Months 2, 6, 9, 12 and 15. 7-2 sFTOH and 7-3 Acid were also screened for in soil extracts generated concurrent with the Months 18 and 24 sampling intervals. The soil treatments selected for the screen included one untreated control soil replicate and the live treated soil replicates in each o f the four soil types. Three different sample preparation regimes were used. For concurrent analyses of 7-2 sFTOH and 7-3 Acid, an aliquot of soil extract was diluted with reagent water containing 100 ng/mL of HDFD internal standard and 1.00 ng/mL of 2-13C PFOA internal standard in the proportions 1 part extract: 3 parts dilution water. This preparation was used for Month 18 and batch analyses on the earlier sampling intervals, except Day 0. For 7-2 sFTOH analyses only, an aliquot o f soil extract was diluted with reagent water containing 1.00 ng/mL of HDFD internal standard and in the proportion of 1 part extract: 3 part dilution water. For 7-3 Acid analyses only, an aliquot o f soil extract was diluted with reagent water containing 1.00 ng/mL o f 2-13C PFOA internal standard and in the proportions 1 part extract: 3 parts dilution water. The latter two preparations were used for processing Day 0 and Month 24 samples where re-analyses due to instrumental or sample stability issues were required (e.g. 7-2 sFTOH stability in the dilutions was suspect). Each o f the dilution solvents in reagent water was freshly prepared before use. A method outline for the analysis 8-2 FTOH, 7-2 sFTOH, 8-2 FTA, 7-3 Acid, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA in soil extracts by LC/MS/MS is presented in Figure 2. Typical instrumental conditions for LC/MS/MS analysis of 8-2 FTA, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA are provided in Table 10. Typical instrumental conditions for LC/MS/MS analysis of 8-2 FTOH are provided in Table 11. Typical instrumental conditions for LC/MS/MS analysis o f 7-2 sFTOH and 7-3 Acid are provided in Table 12. Stock and Calibration Standard Preparation Individual component primary stock solutions (1.00 mg/mL) were prepared for each analyte and internal standard from the neat materials using an analytical balance and volumetric glassware. Individual component secondary stock solutions (100, 10.0, 1.00 and 0.100 pg/mL) were also prepared by serial dilution. The 8-2 FTA, 7-3 Acid, 8-2 FTUA, PFOA, PFNA, PFDA, PFUA, 2-13C PFOA and HDFD (for 24 month interval only) primary stock solutions were prepared in acetonitrile. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -30- The 8-2 FTOH, 7-2 sFTOH and HDFD (except as noted for the 24 month interval) primary stock solutions were prepared in isopropyl alcohol. All secondary stocks were serially diluted with acetonitrile. The 100-pg/mL HDFD secondary stock solution was used to fortify the internal standard into soil extraction solvent, calibration standards containing 8-2 FTOH and 7-2 sFTOH and dilution solvents for analyses o f soil extracts for these analytes. For GC/MS analyses of 8-2 FTOH in the headspace gas of soil test chambers, 8-2 FTOH calibration standards in acetonitrile (25.0, 50.0, 100, 250 and 500 ng 8-2 FTOH/mL) and each fortified at 100 pg HDFD/mL internal standard, were prepared from the appropriate individual component stocks. Representative ion chromatograms for 8-2 FTOH calibration standards by GC/MS are presented in Figures 3 and 4. For LC/MS/MS analyses of 8-2 FTOH in soil extracts, 8-2 FTOH calibration standards in 50: 50 (v/v) acetonitrile: reagent water (10.0, 25.0, 50.0, 100, 250 500 and 1000 ng 8-2 FTOH/mL) and each fortified at 100 pg HDFD/mL internal standard, were prepared from the appropriate individual component stocks. Representative ion chromatograms for 8-2 FTOH calibration standards by LC/MS/MS are presented in Figures 5 and 6. For 8-2 FTA, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA analyses of soil extracts, a 100[ig/mT. -combined stock of 8-2 FTA, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA in acetonitrile was prepared from the individual component primary stocks. Secondary combined acid stocks in acetonitrile (10.0, 1.00 and 0.100 pg/mL) were prepared by serial dilution from the 100 pg/mL combined stock solution. Combined 8-2 FTA, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA calibration standards in 25: 75 (v/v) acetonitrile: reagent water (0.100, 0.250, 0.500, 0.750 and 1.00 ng/mT.) and each fortified with 0.75 ng 2-13C PFOA/mL internal standard were prepared from the 0.100-pg/mL combined stock. A 5.00ng/mL combined 8-2 FTA, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA calibration standard in 25: 75 (v/v) acetonitrile: reagent water was prepared from the 1.00 11g/mT. combined stock. All stock and calibration standards were stored under refrigerated (-4 degrees C) conditions when not in use. For 7-3 Acid and 7-2 sFTOH analyses of Months 2, 6, 9, 12, 15, 18 and 24 (7-3 Acid only) soil extracts, two sets o f combined stocks were prepared. A 10-pg/mL combined stock o f 8-2 FTA, Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -31 - 7-3 Acid, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA in acetonitrile was prepared from the individual component primary stocks. Secondary combined stocks in acetonitrile (1.00 and 0.100 pg/mL) were prepared by serial dilution from the 10.0-pg/mL combined stock. A 10.0-pg/mL combined stock of 8-2 FTOH and 7-2 sFTOH in acetonitrile was prepared from the individual component primary stocks. Calibration standards in 25: 75 (v/v) acetonitrile: reagent water containing 0.75 ng 2-13C PFOA/mL and 100 ng HDFD/mL internal standards were prepared from the 0.100 and 1.00-pg/mL combined perfluorinated carboxylic acid (PFCA) and 10.0-pg/mL combined telomer alcohol stock solutions, respectively. The nominal concentrations of 7-3 Acid and 7-2 sFTOH in the calibration standard set (7-3 Acid/7-2 sFTOH) were 0.100/5.00, 0.250/10.0, 0.500/25.0, 0.750/35.0, 1.00/50.0 and 5.00/250 ng/mL. Due to stability concerns, fresh preparations of 7-2 sFTOH calibration standards were prepared from the 10.0-pg/mL combined stock of 8-2 FTOH and 7-2 sFTOH in acetonitrile for analyses o f 7-2 sFTOH in Month 24 soil extracts. The nominal concentrations of 7-2 sFTOH were as specified above. For 7-3 Acid analyses of Day 0 soil extracts, a combined calibration standard for set for 7-3 Acid and 7-2 sFTOH only was prepared as described above from individual component 7-3 Acid (0.100 and 1.00-ng/mL) and 7-2 sFTOH (10.0-ng/mL) secondary stock solutions. Only 7-3 Acid results were reported from this standard set due to a delay in instrumental analyses. For 7-2 sFTOH analyses, another set of standards was freshly prepared from the 10.0-pg/mL 7-2 sFTOH secondary stock solution. Representative ion chromatograms for 7-2 sFTOH, 8-2 FTA, 7-3 Acid, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA calibration standards by LC/MS/MS are presented in Figures 7-22. Calibration Curves and Limits of Quantitation Calibration standard sets for a given analysis were injected at the beginning and end o f each analytical sequence with one calibration standard injected after a maximum of every five study samples. For 8-2 FTOH analyses in the headspace o f test vessels by GC/MS, linear regression equations were generated using adjusted peak areas (for the internal standard response ratio) versus the respective concentration of the calibration standards. The concentration of 8-2 FTOH in the sampled headspace o f the soil test vessels was determined by substituting the peak area response ratios obtained for the samples into the applicable linear regression equation. The concentrations were converted to a mass basis using the appropriate volumes, weights and unit conversion factors. A representative calibration curve for 8-2 FTOH analyses by GC/MS is presented in Figure 23. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -32- For soil extract analyses of 8-2 FTOH, 7-2 sFTOH, 8-2 FTA,7-3 Acid, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA by LC/MS/MS, weighted linear regression equations were generated using peak area response ratios (analyte:intemal standard) versus the respective concentration ratios (analyte:intemal standard) of the calibration standards. The concentration of each analyte in the samples was determined by substituting the peak area response ratios obtained for the samples into the applicable linear regression equation. Representative calibration curves for 8-2 FTOH, 7-2 sFTOH, 8-2 FTA, 7-3 Acid, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA analyses by LC/MS/MS are presented in Figures 24-32, respectively. The limits of quantitation (LOQ) for these analyses were defined on a low-level standard equivalent basis and were calculated for 8-2 FTOH in the sampled headspace and for each analyte in soil as the product of the low-level standard concentration and the dilution factor of the untreated control samples. The LOQ for 8-2 FTOH in a 20 mL headspace gas aliquot was 12.5 ng/mL sampled headspace gas, or 0.250 pg for a 20-mL sample. The LOQ was 2.0 pg/kg for soil analyses of 8-2 FTA, 7-3 Acid, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA. The LOQs for soil analyses of 8-2 FTOH and 7-2 sFTOH were 100 and 100 pg/kg, respectively. Statistical derivation of the limits of detection (LOD) was completed for all analytes with the exception of 7-3 Acid and 7-2 sFTOH during method verification trials. The calculation for each analyte was based on three times the concentration equivalent of the standard deviation of five replicate analyses of a reagent blank. Method verification trials and derivation of statistical LODs for 7-3 Acid and 7-2 sFTOH was outside the scope of the study. Measured concentrations of the analytes are presented in mg/kg soil dry weight and pmol/kg soil dry weight in Appendix I and II, respectively. Measured concentrations of 7-2 sFTOH and 7-3 Acid in the untreated soils were less than the LOQ and are not presented. Example calculations are presented in Appendix III. Representative chromatograms are presented for each of the four treatment groups in aerobic alfisol soil. Similar chromatographic characteristics were evident for the aerobic ultisol, mollisol and inceptisol soils. Representative ion chromatograms for 8-2 FTOH by GC/MS in the sampled headspace of untreated control, fortified control, sterile and live samples treated with J from Day 0 of the test are presented in Figures 33, 53, 69 and 85, respectively. Representative ion chromatograms for Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -33 - 8-2 FTOH in the sampled headspace of untreated control and live samples treated with" Month 24 of the test are presented in Figures 43 and 95, respectively. om Representative ion chromatograms for 8-2 FTOH by GC/MS in the sampled headspace of fortified control and sterile samples treated withC from Month 12 of the test are presented in Figures 61 and 77, respectively. Representative ion chromatograms for 8-2 FTOH, 7-2 sFTOH, 8-2 FTA, 7-3 Acid, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA by LC/MS/MS in soil extracts from untreated control samples from Day 0 and Month 24 of the test are presented in Figures 34-42 and 44-52, respectively. Representative ion chromatograms for 8-2 FTOH, 8-2 FTA, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA by LC/MS/MS in soil extracts from fortified control samples from Day 0 and Month 12 of the test are presented in Figures 54-60 and 62-68, respectively. Representative ion chromatograms for 8-2 FTOH, 8-2 FTA, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA by LC/MS/MS in soil extracts from sterile samples treated with L 3frm Day 0 and Month 12 of the test are presented in Figures 70-76 and 78-84, respectively. Representative ion chromatograms for 8-2 FTOH, 7-2 sFTOH, 8-2 FTA, 7-3 Acid, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA by LC/MS/MS in soil extracts from live samples treated with Jfrom Day 0 and Month 24 of the test are presented in Figures 86-94 and 96-104, respectively. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -34REFERENCE Project No.: 112E-108 1 Organisation for Economic Cooperation and Development. April 2002. A ero b ic an d A n aerobic Transform ation in Soil. OECD Guideline 307. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -35 - Table 1 Frequency of Measurements1 Interval Activity Biomass Soil moisture Headspace Soil Analytical oxygen metabolic interval content activity Day 0 ' Week 1 V V V V Week 2 V V Week 4 VVVV Week 6 Month 2 V VVVV Month 3 VVV Month 4 V V V V V Month 5 VVV Month 6 V V V V V Month 7 VVV Month 8 VVV Month 9 VVVV Month 10 VVV Month 11 VVV Month 12 V V V V V Month 15 VV Month 18 V VV Month 21 V Month 23 V Month 24 V VV 'Additional chambers for the measurement of biomass and headspace oxygen content beyond the initial 12 month test period were not prepared at the start of the study. Company Sanitized. Does not contain TSCA CBI. ,W ildlife International Ltd Project No.: 112E-108 Interval Month 1 Month 2 Month 3 Month 4 Month 5 Month 6 Month 7 Month 8 Month 9 Month 10 Month 11 Month 12 -36- Table 2 Test Chamber Headspace Oxygen Content Alfisol 20.8 21.0 20.9 20.8 20.8 20.9 20.8 20.8 20.8 20.9 20.8 20.9 Average Oxygen Content (%) Inceptisol Mollisol 20.8 20.7 20.9 20.7 20.9 20.6 20.8 20.8 20.7 20.7 20.9 20.7 20.7 20.8 20.8 20.9 20.8 20.8 20.9 20.8 20.8 20.8 20.9 20.8 Ultisol 20.8 20.7 20.6 20.8 20.8 20.8 20.7 " 20.8 20.8 20.9 20.8 20.8 ' Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd Project No.: 112E-108 -37Table 3 Soil label Texture class Alfisol Inceptsol Ultisol Mollisol Sandy loam Loam Sandy loam Sandy clay loam 1- cation exchange capacity ^-^pH^^j^ljo^wateyatr Selected Soil Properties Organic carbon content % 1.4 2,0 2.9 2.1 Sand Silt Clay % 65 24 11 45 32 23 55 31 14 59 18 23 CEC1 meq/100 g 7.8 16.9 7.9 17.7 Water holding capacity pH2 % 5.8 54.5 6.6 43.3 4.8 59.3 6.9 63.2 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -38- Table 4 Soil Viability by Glucose Mineralization: Alfisol Month Glucose Mineralization Rate Aerobic Anaerobic 1 1.83 1.81 2 1.79 2.68 3 2.45 7.34 4 2.73 7.36 5 2.54 4.17 6 2.60 3.00 7 3.99 NA 8 3.79 NA 9 7.57 NA 10 2.64 NA 11 2.39 NA 12 2.00 NA 15 1.64 NA 18 1.81 NA 24 1.81 NA '- (percent biodegradation/elapsec time in days) x 100 ` Table 5 Soil Viability by Glucose Mineralization: Inceptisol Month Glucose Mineralization Rate1 Aerobic Anaerobic 1 2.48 1.95 2 4.15 3.89 3 8.60 8.44 4 8.90 7.76 5 8.29 3.34 6 8.97 3.02 7 9.50 NA 8 9.47 NA 9 10.46 NA 10 8.91 NA 11 8.50 NA 12 8.04 NA 15 8.14 NA 18 8.06 NA 24 8.90 NA (percent biodegradation/elapsec time in days) x 100 p. 40 Company Sanitized. Does not contain TSCA CBI. ,W ildlife International Ltd. Project No.: 112E-108 -39- Table 6 Soil Viability by Glucose Mineralization: Ultisol Month Glucose Mineralization Rate1 Aerobic Anaerobic 1 2.23 2.22 2 2.56 2.39 3 1.67 2.86 4 1.95 4.22 5 4.04 5.41 6 2.46 3.80 7 3.79 NA 8 7.33 NA 9 7.37 NA 10 8.83 NA 11 2.99 NA 12 3.61 NA 15 8.19 NA 18 2.37 NA 24 3.65 NA '- (percent biodegradation/elapsed time in days) x 100 Table 7 Soil Viability by Glucose Mineralization: Mollisol Month Glucose Mineralization Rate1 Aerobic Anaerobic 1 2.36 1.85 2 2.54 2.99 3 1.72 2.57 4 3.63 3.99 5 4.06 4.82 6 3.66 4.16 7 3.74 NA 8 3.95 NA 9 3.60 NA 10 7.51 NA 11 2.73 NA 12 1.78 NA 15 3.59 NA 18 2.11 NA 24 1.81 NA *- (percent biodegradation/elapsed time in days) x 100 p. 41 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -40- Table 8 Soil Microbial Biomass (pg/g) (ISO 14240-2; fumigation-extraction) ALFISOL INCEPTISOL _____Aerobic____________ Anaerobic_____ Aerobic Anaerobic Treated Untreated Treated Untreated______ Treated Untreated Treated Untreated Post Inc. - 244 - 128 Month 4 317 323 435 287 Month 6 680 279 593 645 Month 12 769 675 NA NA - 131 - 132 138 109 184 106 432 483 423 467 504 564 NA NA p. 42 Company Sanitized. Does not contain TSCA CBI. _______W ildlife International, Ltd. Project No.: 112E-108 -41 - Table 8 (continued) Soil Microbial Biomass (pg/g) (ISO 14240-2; fumigation-extraction) Post, Inc. Month 4 Month 6 Month 12 MOLLISOL Aerobic ________Anaerobic_____ Treated Untreated Treated Untreated - 190 - 53 216 218 218 205 243 259 267 270 714 734 NA NA ULTISOL ______ Aerobic____________ Anaerobic Treated Untreated Treated Untreated - 312 - 54 36 31 26 34 486 194 500 407 565 570 NA NA NA - Not analyzed p. 43 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -42Table 9 Typical GC/MS Operational Parameters for Analysis of 8-2 FTOH in Headspace Gas Instrument: Detector: Analytical Column: Injector Temperature: Oven Temperature Profile: Hewlett-Packard Model 5890 Series II Gas Chromatograph (GC) Hewlett-Packard Model 5971 Mass Selective Detector Phenomenex Zebron ZB-5 (30 m x 0.25 mm, 0.25-pm film thickness). 150C Initial temperature: 50C Initial hold time: 2.00 minute Ramo: Rate CC/minutei 20.00 50.00 Final Temoerature CCI 100 300 Detector Temperature: Carrier Gas: Septum Purge: Split Vent: Injection Volume: Data Acquisition Mode: Final hold time: 3.00 minute 280C Helium, ~1 mL/min; CHP = ~14 psi Helium, ~5 mL/min ~40 mL/min 2 pL (2 stops w/ 10 pL syringe), splitless SIM Acquisition Ions: Component 8-2 FTOH Quantitation 31 m/z Confirmation 95 m/z Peak Retention Times: HDFD 33 m/z 98 m/z 8-2 FTOH: Approximately 5.0 minutes HDFD: Approximately 5.0 minutes Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -43 - Table 10 Typical LC/MS/MS Operational Parameters for Analysis of 8-2 FTA, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA in Soil Extracts Instrument: Analytical Column: Column Temperature: Mobile Phase: Gradient Elution Profile: Injection Volume: Monitored Ion Transitions: PFOA 2-13 PFOA (internal standard) 8-2 FTA 8-2 FTUA PFNA PFDA PFUA LC/MS/MS Analog Parameters: Agilent Technologies 1100 Series High Performance Liquid Chromatograph with an Applied Biosystems/MDS SCIEX API 3000 LC Mass Spectrometer equipped with a Perkin-Elmer Turbo IonSpray source. Operated in the negative ion multiple reaction-monitoring mode. Zorbax RX-C8 (150 mm x 2.1 mm, 3-pm particle size) 40C A: 0.1% Formic Acid in Reagent Water B: Acetonitrile Time /mint 0.00 1.00 8.00 9.00 9.10 14.00 15.00 20.00 Flow Rate /uL/minl 250 250 250 250 250 250 250 250 Percent A 70.0 70.0 15.0 15.0 5.0 5.0 70.0 70.0 Percent B 30.0 30.0 85.0 85.0 95.0 95.0 30.0 30.0 50.0 pL Ql 413.0 amu 415.0 amu 477.0 amu 457.0 amu 463.0 amu 513.0 amu 563.0 amu Q3 369.0 amu 370.0 amu 393.0 amu 393.0 amu 419.0 amu 469.0 amu 519.0 amu Dwell Time 250 msec 250 msec 250 msec 250 msec 250 msec 250 msec 250 msec Retention Time 9.82 min 9.82 min 12.2 min 12.3 min 10.6 min 11.2 min 11.8 min IS =-4500 TEM = 400 DP = -10 FP = -140 EP = -10 CE = -15 CXP = -25 CUR = 8 CAD = 4 NEB = 12 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -44Table 11 Typical LC/MS/MS Operational Parameters for Analysis of 8-2 FTOH in Soil Extracts Instrument: Analytical Column: Guard Column: Column Temperature: Mobile Phase: Isocratic Profile: Injection Volume: Monitored Ion Transitions: 8-2 FTOH HDFD (internal standard) LC/MS/MS Analog Parameters: Agilent Technologies 1100 Series High Performance Liquid Chromatograph with an Applied Biosystems/MDS SCIEX API 3000 LC Mass Spectrometer equipped with a Perkin-Elmer Turbo IonSpray source. Operated in the negative ion multiple reaction-monitoring mode. THERMO EC Betasil C-18 (50 mm x 2.1 mm, 5-pm particle size) Javelin Betasil C-18 (20 mm x 2.1 mm) 40C A: 0.15% Acetic Acid in Reagent Water B: Acetonitrile Time (min') 0.00 6-00 Flow Rate CuL/mm) 250 250 Percent A Percent B 30.0 70.0 30.0 70.0 25.0 pL Q1 523.1 amu 528.1 amu IS = -4500 TEM = 450 DP = -25 FP = -250 EP = -10 Q3 58.9 amu 58.9 amu Dwell Time 500 msec 500 msec Retention Time 4.18 min 4.15 min CE = -50 CXP = -10 NEB = 12 CUR = 7 CAD = 6 p. 46 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project n o .: 112E-108 -45 Table 12 Typical LC/MS/MS Operational Parameters for Analysis of 7-3 Acid and 7-2 sFTOH in Soil Extracts Instrument: Analytical Column: Column Temperature: Mobile Phase: Gradient Elution Profile: Injection Volume: Reported Ion Transitions: 7-3 Acid 2-13 PFOA (internal standard) 7-2 sFTOH HDFD (internal standard) LC/MS/MS Analog Parameters: Agilent Technologies 1100 Series High Performance Liquid Chromatograph with an Applied Biosystems/MDS SCIEX API 3000 LC Mass Spectrometer equipped with a Perkin-Elmer Turbo IonSpray source. Operated in the negative ion multiple reaction-monitoring mode. Zorbax RX-C8 (150 mm x 2.1 mm, 3-pm particle size) 40C A: 0.15% Acetic Acid in Reagent Water B: Acetonitrile/ 0.15% Acetic Acid Time ("min) 0.00 1.00 1.01 7.00 12.00 13.00 20.00 Flow Rate (uL/min) 250 250 250 250 250 250 250 Percent A Percent B 95.0 5.0 95.0 50.0 70.0 30.0 15.0 85.0 15.0 85.0 95.0 5.0 95.0 5.0 50.0 pL Q1 441.0 amu 415.0 amu 473.0 amu 528.0 amu Q3 337.0 amu 370.0 amu 59.0 amu 59.0 amu Dwell Time 50 msec 50 msec 50 msec 50 msec Retention Time 11.6 min 10.0 min 11.9 min 12.1 min IS = -4500 TEM = 400 EP = -10 CUR = 7 CAD = 6 NEB = 132 7-3 Acid/ 2-13 PFOA DP = -40 FP = -350 CE = -15 CXP = -11 7-2 sFTOH/ HDFD -25 -250 -50 -10 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -46- Project No.: 112E-108 Method flowchart for the analysis of 8-2 FTOH in the headspace of soil test chambers For each sample, fit a C]8 cartridge between the end of an appropriate volume syringe and a hypodermic needle. I With the plunger fully depressed, insert the needle of the disposable syringe through the septum of the sample and pull a full syringe volume. Remove needle, expel headspace air and repeat. i Detach C18 cartridge and place in appropriate holder. Attach the barrel of a 10 mL disposable syringe to Cj8 cartridge and use a volumetric pipette to transfer acetonitrile extraction solvent into the syringe barrel. Insert the syringe plunger into the barrel and inject the acetonitrile through the C,8cartridge into a 20-cc glass scintillation vial. Fortify the extract to contain 100 ng/mL ID, ID, 2D, 2D, 3-13C Heptadecafluoro Decanol internal standard. I Pipette an aliquot of the extract directly into an autosampler vial. Cap vial and submit for GC/MS analysis of 8-2 FTOH. All sample vials not analyzed immediately are place in refrigerated storage. I Store the remaining trap extract in scintillation vials under frozen conditions. Figure 1. Method flowchart for the analysis of 8-2 FTOH in the headspace o f soil test chambers. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -47- p. 48 Projectno.:iheios Method flowchart for the analysis of 8-2 FTOH, 7-2 sFTOH, 8-2 FTA, 7-3 Acid, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA in soil extracts For each sample vessel, remove crimp seal and place foil liner into the vessel. Using a graduated cylinder, measure and transfer 125 milliliters of extraction solvent into each sample vessel. The extraction solvent consists of 100 ng/mL ID, ID, 2D, 2D, 3-13C Heptadecafluoro Decanol internal standard in acetonitrile. Add a 10-mL aliquot of 200 mM NaOH into each sample. 4 Re-crimp each sample vessel with a new aluminum crimp cap and the original septum. Extract the samples for approximately three hours using a gyratory shaker table set for 250 rpm. 4 Allow suspended material in extracts to settle. Remove a 10-mL aliquot of the extract using a serological pipette and transfer into a separate 50-mL plastic centrifuge tube preloaded with approximately 25 mg of Envi-CarbTM. Centrifuge samples at a setting of 12000 rpm for 10 minutes. Transfer extract supernatant for each sample into a separate labeled scintillation vial. 4 For 8-2 FTOH analyses, pipette an aliquot o f the extract supernatant (or diluted extract, if applicable) with reagent water fortified with 100 ng/mL ID, ID, 2D, 2D, 3-13C Heptadecafluoro Decanol (HDFD) internal standard to produce a final solution composition of 1:1 (v/v) extract: water. For 7-2 sFTOH analyses, pipette an aliquot of the extract supernatant (or diluted extract, if applicable) with reagent water fortified with 100 ng/mL HDFD to produce a final solution composition of 1:3 (v/v) extractiwater. Perform dilution directly in an autosampler vial, cap and vortex. Submit for HPLC/MS/MS analysis of telomer alcohols. All sample vials not analyzed immediately, place in refrigerated storage. 4 For PFCA analyses of each sample, dilute an appropriate volume o f the extract supernatant (or diluted extract, if applicable) with reagent water fortified with 1.00 ng/mL N-Perfluorooctanoic Acid, [1,2 di13C] internal standard to produce a final solution composition of 1:3 extract: water. Perform dilution directly in an autosampler vial, cap and vortex. Submit for HPLC/MS/MS analysis o f PFCAs. All sample vials not analyzed immediately, place in refrigerated storage. 4 Re-crimp each sample vessel with a new aluminum crimp cap and the original septum. Store sample vessels and extract scintillation vials under frozen conditions. Figure 2. Method flowchart for the analysis of 8-2 FTOH, 7-2 sFTOH, 8-2 FTA, 7-3 Acid, 8-2 FTUA, PFOA, PFNA, PFDA and PFUA by LC/MS/MS in soil extracts. p. 49 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -48- Wildlife International, Ltd. GC-MS#2 MSD Serial No. 3118A02483 File: Operator: T:\DATA\ALFI025\0101005.D DW Date Acquired: 20 Apr 106 5:41 pm Instrument: GCMS#1 Sample Name: TA-30 Misc Info: 25.0 ug a.i./L Vial Number : 1 Figure 3. Representative ion chromatograms for 8-2 FTOH in a low-level (25.0 ng a.i./mL) calibration standard by GC/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd, Project No.: 112E-108 -49- Wildlife International, Ltd. GC-MS#2 MSD Serial No. 3118A02483 File: T:\DATA\ALFI025\0501009.D Operator: DW Date Acquired: 20 Apr 106 7:03 pm Instrument: GCMS#1 Sample Name: TA-34 Misc Info: 500 ug a.i./L Vial Number : 5 Figure 4. Representative ion chromatograms for 8-2 FTOH in a high-level (500 ng a.i./mL) calibration standard by GC/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -50- Project No.: 112E-108 Figure 5 Representative ion chromatogram for 8-2 FTOH in a low-level (10.0 ng a.i./mL) calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI W ildlife International, Ltd -51 - Project No.: 112E-108 Figure 6. Representative ion chromatogram for 8-2 FTOH in a high-level (1000 ng a.i./mL) calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -52 - Project No.: 112E-108 Figure 7. Representative ion chromatograms for 7-2 sFTOH in a low-level (5.00 ng a.i./mL) calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd -53- Project No.: 112E-108 Figure 8. Representative ion chromatograms for 7-2 sFTOH in a high-level (250 ng a.i./mL) calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBi. W ildlife International, Ltd. -54- Project No.: 112E-108 Figure 9. Representative ion chromatogram for 8-2 FTA in a low-level (0.100 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBi. W ildlife International, Ltd. -55 - I W.FWWtWl"fto k Nun* *6-2(5)' **<**) *47709a0i ` c ---.....Cenm* *1MMT Amdrtiov S e ttle Indax: 33 S a ^ la Type: Standard C a c u m cio n : 5 .0 0 ug C a lc u lacad Cone: 4 . 1 5 0 ug BunchiI ' 'Mediti ad; Er o e. A lg o ritb i sin g Pacte) e Thru*hol e a Threshold AdJ. I MrTOWLMBJl 3Dad* 29*422*42J*42a425a*- 23*422a*- project no.: 112E-108 MIB.O 8009. 70OE. 600. 30CD. 200. Figure 10. Representative ion chromatogram for 8-2 FTA in a high-level (5.00 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. Wildlife InternationalLtd. -56- Project No.: 112E-108 Figure 11. Representative ion chromatogram for 7-3 Acid in a low-level (0.100 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -57- Project No.: 112E-108 Figure 12. Representative ion chromatogram for 7-3 Acid in a high-level (5.00 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. ,W ildlife International, Ltd -58- Project No.: 112E-108 Figure 13. Representative ion chromatogram for 8-2 FTUA in a low-level (0.100 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd -59- Project No.: 112E-108 Figure 14. Representative ion chromatogram for 8-2 FTUA in a high-level (5.00 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. ,W ildlife International, Ltd -60- Project No.: 112E-108 Figure 15. Representative ion chromatogram for PFOA in a low-level (0.100 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd, -61 - ProjectNo.: 112E-108 Figure 16. Representative ion chromatogram for PFOA in a high-level (5.00 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. ,W ildlife International, Ltd I s*npwNm "ample.WT" 'UampielD 'ILiUMuB'l' hh M i m M 1 lbULAfcir Peek Name X-SAdd" Mu*(as)'`463A '4190 nir " Cerniw r *LCMS-1S' A rroaton:- Sattpl Index: 1C ic p le Type: Standard Concent r a t l i n : 0.100 ug a . i . / L C a lc u la te d Cer.e: O.OSOS1C ug a . i . / k g ic q . Cate: 0 4 /2 1 /2 0 0 K edltled: F re e . Alge I Bunching Fi He -62- Project No.: 112E-108 Figure 17. Representative ion chromatogram for PFNA in a low-level (0.100 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd -63 - Project No.: 112E-108 Figure 18. Representative ion chromatogram for PFNA in a high-level (5.00 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -64- Project No.: 112E-108 Figure 19. Representative ion chromatogram for PFDA in a low-level (0.100 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI W ildlife International, Ltd -65 - Project No.: 112E-108 Figure 20. Representative ion chromatogram for PFDA in a high-level (5.00 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. .W ildlife International, Ltd -66- Comma TCMS-18' Anrowen aiapla Inda.-.: in S a a p lt Types Standard Is d itle d . N: Pros. Algorithm: Analyst C T h raa h eld : 25.41 3 8*4 36*4 3 4M 3.2M 30M 2 4M 2.2M Project No.: 112E-108 12M 8000.0 8000 0 4000.0 2000.0- o.o-L i 9 10 11 Figure 21. Representative ion chromatogram for PFUA in a low-level (0.100 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd -67- Project No.: 112E-108 Figure 22. Representative ion chromatogram for PFUA in a high-level (5.00 ng a.i./mL) combined PFCA calibration standard by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -68 - p. 69 Project No.: 112E-108 IS Adjusted Peak Area Counts Concentration (fig 8-2 FTOH/L) Figure 23. Representative calibration curve for 8-2 FTOH by GC/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd -69- Project No.: 112E-108 Figure 24. Representative calibration curve for 8-2 FTOH by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. .W ildlife International, Ltd -70- Project No.: 112E-108 Figure 25. Representative calibration curve for 7-2 sFTOH by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd -71 - Project No.: 112E-108 A nalv te A r e a / IS A re a Figure 26. Representative calibration curve for 8-2 FTA by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -72- Project No.: 112E-108 Figure 27. Representative calibration curve for 7-3 Acid by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd -73 - Project No.: 112E-108 A na l v t e A r e a / IS A re a Figure 28. Representative calibration curve for 8-2 FTUA by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -74- Project No.: 112E-108 042006_M12_TELALAE.ndb (PFOA C-8): "Linear" Regression ("1 / x" weighting): y = 1.12 x + 0.0538 (r = 0.9985) X n a l v t e A rea / IS A re a 1-5 2.0 ' 2.5 ' ' 3C ' ' 315 ' ' 40 ' 4 .5 ' ' ' 5.0 ' 5 5 ' ' 6.'o _____________________ Analyte Cone. / IS Cone. Figure 29. Representative calibration curve for PFOA by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd -75 - Project No.: 112E-108 An alvte A re a / IS A re a 042006_M12_TELALAE.rdb (C-9 Add): "Linear" Regression {"1 / x" weighting): y = 1.34 x + -0.00636 (r = 0.9991) 9.0 8.5 8.0 7.5 7.0 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0 0.5 0.0 0.5 1.0 1.5 2 0 2.5 3.0 3.5 4.0 4.5 5.0 5 5 6.0 6.5 Analyte Cone. / IS Cone.__________________________ ______ Figure 30. Representative calibration curve for PFNA by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. Wildlife International, Ltd. -76- Project No.: 112E-108 An alvte A re a / IS A re a 042006_M12_TELALAE.rdb (C-10 Acid): `lin e a r Regression ("1 /x" weighting): y= 1.4 x + -0.0404 (r = 0.9996) 9.5 9.0 8.5 8.0 7.5 7.0 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0 0.5, o.oK 0.5 1.0 1 5 2.0 2 5 3.0 3.5 4.0 ______ Analyte Cone. / IS Cone. 4.5 5.0 ' 5 5 : 6.'o' ' ' 6 5 ` Figure 31. Representative calibration curve for PFDA by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd -77- Project No.: 112E-108 042006_M12_TELALAErdb(C-11 Acid): "Lineai' Regressen ("1 /x" weighting): y= 1.29 x + 0.0743 (r = 0.9994) A n a lv te A r e a / IS A re a Figure 32. Representative calibration curve for PFUA by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -78- Wildlife International, Ltd. GC-MS#2 MSD Serial No. 3118A02483 File: Operator: C:\HPCHEM\l\DATA\ALFI005\0701011.D fj1 Date Acquired: 30 Apr 105 4:10 pm Instrument: GCMS#2 Sample Name: Misc Info: 1570-TEX Vial Number : 7 Figure 33. Representative ion chromatograms for 8-2 FTOH in the sampled headspace (C,gcartridge extract) from a Day 0 untreated control soil by GC/MS. 8-2 FTOH was not present (no peak at 5.0 min). Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -79- Project No.: 112E-108 Figure 34. Representative ion chromatogram for 8-2 FTOH in the soil extract from a Day 0 untreated control soil by LC/MS/MS. 8-2 FTOH was not present (no peak at 4.18 min). Company Sanitized. Does not contain TSCA CBI. Wildlife International, Ltd. -80- Project No.: 112E-108 Figure 35. Representative ion chromatogram for 7-2 sFTOH in the soil extract from a Day 0 untreated control soil by LC/MS/MS. 7-2 sFTOH was not present (no peak at 11.9 min). Company Sanitized. Does not contain TSCA CBI W ildlife International, Ltd. -81 - Project n o .: i u e - ios r ^u U S S S im DOF Samps ID '15717 Ffa.*04210$_DQ_TELALAE.<> PMk Nam: *9-2 (Sr Maee<ee). `477.OW3.0 wmt` S a a pClea n Innadnet x":ll2E-10S.11D4 #.H 0-(UTCr A n w w e o n - S aaple Type: C e n cen tiitica: B lank 0.00 ug a .i ./ L 1 00*4 C a lc u la te d Cone: N/A Acq. Date: 0 4 /2 1 /0 5 0 1 : 10:04 PM 9600.00 nodi tied : Bunching fa c to r: N oise T hreshold: A rea T hreshold: Nun. Smooths : RT window: t x p e c t e d RT: Sep. W idth: Sep. H eight: Exp. Peek R atio Exp. A di R atio Exp. v a l. R atio U se R e la tiv RT No 2 4 .0 6 120.21 3 0 .0 12.2 0 .2 0 0 .0 1 5 .0 0 4 .0 0 3 .0 0 No cps epa sun 9000 00 9500.00 9000 00 7500.00 700000 I n t . Type: A rea: H eight: S t a r t Tiise: End T ine: No Peak N/A N/A N/A N/A in eps sun 4600 00 9000 00 $900000 I! li| 2500.00 2000.00 1500.00 1000.00 900 00 I: 000 Printing Date: Friday, April 22,2005 9.04 \ 10.74 __ I W . 7JOT3 8.13 10 39 ' A , . . . . ____ _ . ____ _ T 9'7 ~ -r- ^ T3 * 15 16 17 IS IS __ _ _Ta.in . . . __________________________________________ _ Figure 36. Representative ion chromatogram for 8-2 FTA in the soil extract from a Day 0 untreated control soil by LC/MS/MS. 8-2 FTA was not present (no peak at 12.2 min). Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -82- Project No.: 112E-108 Figure 37. Representative ion chromatogram for 7-3 Acid in the soil extract from a Day 0 untreated control soil by LC/MS/MS. 7-3 Acid was not present (no peak at 11.6 min). Company Sanitized. Does not contain TSCA CBI W ildlife International, Ltd *S*mpta_006- $*m p4 ID ' T O * Fie: TO 105_D0jr6LA LA E wr PM k Mem*. *B-J (U r *4X7.0003 0 amu* Commant *11 -IO 0.100.1 ICH^TC)* Ann t o r ** sa ap l* Index: S u p U Type: : C oncentration: : C a lc u la te d Cone: i Acq. D ote: | Acq. T ine: 14 B lank 0 .0 0 N/A W /21 /0 5 0 3 :1 0 :3 4 u a .i./L PM 1 00*5 B 50*4 | M odified: , Bunching F acto r: N o is e T h r e s h o ld : 1A re T h re sh o ld ; 1Mu*. Sm ooths: ] k t Window: : E x p e c te d RT: .S e p . W idth: [ Sep. H eight: 1Exp. Peak R eno | Exp. A d). R atio ; Exp. V al. Raeic ( U se R e l a t i v e P.T Ho 2 0 1 .9 3 1 0 0 9 .6 4 3 0 .C 1 2 .3 0 .2 0 0 .0 1 5 .0 0 4 .0 0 3 .0 0 No epa eps see m in 900*4 1 50*4 6.00*4 790*4 7 00*4 ! In t. Type: i R e t e n t i o n T1m : A rea: {H eight; , S ta r t Ti m : i End Ti m : No Peak N/A N/A N/A N/A N/A eps m in tain 6 60*4 6 00*4 5: j $.00*4 Ii S 4.50*4 4 00*4 3.60*4 3.00*4 2.60*4 200*4 -83 - Project No.: 112E-108 1 000 ' Printing Date: Friday, April 22,2005 i '3 ____________ __ 604 a.fr! _7.w SJS 10.16 11,10 12.67-, 1 3 .4 2 ,13.05 > _ _________ ^ 3 4 51 T ' V ~ 10 11 12 13 14 1 1 I ? _________________________ T o r*, non______________________________________ __ _____ Figure 38. Representative ion chromatogram for 8-2 FTUA in the soil extract from a Day 0 untreated control soil by LC/MS/MS. . 8-2 FTUA was not present (no peak at 12.3 min). Company Sanitized. Does not contain TSCA CBI. .W ildlife International, Ltd [| S*mp>* N * w : -&mp>*_00r SanvN IO : ^5 7 tT "H a: 'M 2 ia 5 '"Do' TELALAE.wHT || PM k Name: *PFOA C -T '413.04309.0 Knu* "" j C i r n w n t `t12E-108.10e,11CKVTCr Annotation: " i s u f i Indue: i!i S a ha fpll* T iympae 14 fBt l al annl ik I C o n centration: c .o o ug a . i . /L 1.00*5 , j C a lc u la te d Cone: KVA ' Acq. D ate: Acq. T in e: 04/21/0S 0 7 :1 0 :0 4 PM 9.50*4 ; M odified: ! Bunching f a c to r : I N oise T hresh o ld : ' A rea T hreshold: : Nun. Saooths: | NT Window: . E x p e c te d NT: 1 Sep. W idth: Sep. H eight: Exp. Peak R atio: Exp. Ad}, ftacio: Exp. V al. R atio: Use R e l a t i v e RT: No 1 1 8 3 .7 7 9 4 8 .6 4 1 3 0 .0 9 .8 2 0 .2 0 0 .0 1 5 .0 0 4 .0 0 3 .0 0 No cps cps sec in 9.00*4 8.50*4 ! 8X0*4 j 7X0*4 7.00*4 ^ In t. Type: R eten tio n T iae: A rea: N eighs: S ta rt T iae: End T l*K : No P eak H/A N/A N /A N/A N /A ln i c o u n ts cps in in 6.50*4 j .00*4 | } 'S !j- 4X0*4 4.00*43.50*4 3.00*4 2.50*4 2.00*4 -84- 5000.00! 000 Project No.: 112E-108 Figure 39. Representative ion chromatogram for PFOA in the soil extract from a Day 0 untreated control soil by LC/MS/MS. PFOA was not present (no peak at 9.82 min). Company Sanitized. Does not contain TSCA CBI W ildlife International, Ltd Project No.: 112E-108 -85 - 71TS S5: S rtl.l0 .-t5 7 0 - H >: -l2iui.00.TE LLE . li PM k N am : *C-e M f Me*<*>: -63.0M1BJD imu" I C nm w c*1l2E -t0e.1(.11H W T Cr AnnoWion." i! S u ^ l i I n d e x : ` S a w p le T y p e: il C o n e e n t r e t i e r : C alc u lated Cone: 14 81*k 0 .0 0 ug N/A a .i 1.00*5 . 0 50*4 : K o dified: Bunching F a c to r: N ois* T h resh o ld : A re* T h resh o ld : Hu m . S a o o t h i : RT w indow : E x p ec te d RT: Sep. W idth: Sep. H eight: Exp. Peak R a tio : Exp. Ad}. R atio : Exp. V al. R atio: U se R e la tiv e RT: NO l 1 9 2 .8 5 9 6 4 .2 5 1 3 0 .0 1 0 .6 0 .2 0 0 .0 1 5 .0 0 4 .0 0 1 .0 0 Ho : T o t. Type: R e te n tio n Tit**: 1 A rea: , H eight: | S ta r t Ti m : ! End Ti m : HO P eak N/A M/A N/A M/A N/A cps cps sec w in w in c o u n ts cps w in 9.00*4 8.50*4 8.00*4 750*4 7.00*4 6.30*4 6.00*4 5 5** 5 4.50*4- 4 00*4 3 50*4 3.00*4 2.50*4 1 50*4 1.00*4 3000.00 OOO Printing Date: Friday, April 22,2005 5~SL. 3 * . , f i* 5.83!-. 66-.0W1 -A*3>4 7.66 3 l 0 . 2 > J f l I t 1250 1353 Figure 40. Representative ion chromatogram for PFNA in the soil extract from a Day 0 untreated control soil by LC/MS/MS. PFNA was not present (no peak at 10.6 min) Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -86- Project No.: 112E-108 I SewpieMem* *Srapl*..gOr Semple 10'`l&fT >4* "042105'DO 'TELALRE.wtfT I. PeetNeme-C-IOAdd- U w |n ) -S13.0a8.0amu* "~ j Comment*112E>108.10B,110-<inCr AnnokSbon " . Sample Index: 14 Sample Typ: Blank C oncentration: 0.00. 1191.1./L 100*5. - C a lc u la te d Cone: n/ a Aeq. D ate: Acq. T lx: 04/21/05 0 1 :1 0 :0 4 PH 9.90*4 M odified: - bunching F acto r: j N oise T hreshold: ! A res Threshold: 11 Pint, sm o o th s: !| RT Window: ': E x p ec te d ST: I Sep. W idth: : Sep. Heighc: . Cxp. Peak R atio: Exp. Ad). R atio: Exp. V al. R atio: Use R e la tiv e RT: Ho J 167.30 SS e.S O l 3 0 .0 11.2 C.20 c.01 S.00 4 .0 0 3 .0 0 No cps cps sec min 9.00*4 8.50*4 8.00*4 7.50*4 7.00*4 i, l n t . T ype: R e te n tio n Time: A rea: l| H e ig h t: ; S tart T iw : End Time: Me Peak n /a n/A N/A N/A N/A 6J0*4 ] 6.00*4 ; 5, 1 I6.00*4 < 4SOM ) 4.00*4-1 350*4 ! 250*4 j 2.00*4 1.00*4 500000 i 000 Printing Date: Friday, April 22,2005 _2.08 3.18 .SJ3.4J56.85 8.01 AS7 7.77.7J7 0.81 X>M 1 1 2 2 ,11.80 13.a0.13J* ___ 2* 48 8 7 6 5 10 11 72 15 14 IS 18 IT ' 18 " ' Figure 41. Representative ion chromatogram for PFDA in the soil extract from a Day 0 untreated control soil by LC/MS/MS. PFDA was not present (no peak at 11.2 min). Company Sanitized. Does not contain TSCA CBI W ildlife International, Ltd -87- I--.^ 7 = 7 - -- T * 1" CTTr Fie W2l0S_00_TELALA6tr PeekNeme: *C-11 Aenf *5 0 0018.0 am* I S n pCl et nInmd l x*:112E-1C0.140.t10-<UTCr S a ^ le Typ: Blank Cooc e n t r t io n : 0 .0 0 ug C a lc u la te d Cor H/A Acq. Dite: 04/21/05 I Acq. Ti m : 0 7 :1 0 :0 4 PK A m M ten** 00a5 | JON j < M ediiied: i. Bunching f a c t o r : !i H ois* T h re sh o ld : I' Area T h re s h o ld : '< mm. S a e o th s : j RT Window: expected kt: 9ep. W idth: Sep. H eight: Exp. peak R a tio : Exp. Ad3 . R a tio : ;! Exp. V a l. R a tio : ! Ose R e la tiv e RT Mo 1 114.03 570.16 1 3 0 .0 u .< 0.20 C.01 5 .0 0 4 .0 0 3.00 DON SOn ] Xr.t. T ype: He Peak Retention T ine: H/A SOee H eight: S tart T iae: End T ia e : !i H/A H/A H/A l Project No.: 112E-108 ,00e4 2.00* i 1.D0H ! i 900000 : 000 - -- Printing Date: Friday, April 22,2005 ~4 S ! 7 837 8.01 BJ1 730 0.70 40 .si. m i lc e is a o n jB 10 "TT 12 14 is" 1 17 10 10 Figure 42. Representative ion chromatogram for PFUA in the soil extract from a Day 0 untreated control soil by LC/MS/MS. PFUA was not present (no peak at 11.8 min). Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -88- Project No.: 112E-108 W i l d l i f e I n t e r n a t i o n a l , L t d . Q C ^M S#2 M S I) S e r i a l No;. F I Xe ; p e r tea ts X.:/\CMST\ 1 \m T A \A I -HZ;4- 1 :Vt>.,61010 . 0 o ft .... . b $ t e A c q u ir e d : I S A> 103f 3:B pari In s tru m e n t: tSBM'S#! ' " Sam ple Name: 15S2VTEJX: M ia c ln e .i V ia l Num ber : 6 '' 3 .1 1 S A 0 2 4 S 3 Figure 43. Representative ion chromatograms for 8-2 FTOH in the sampled headspace (C18cartridge extract) from a Month 24 untreated control soil by GC/MS. 8-2 FTOH was not present (no peak at 5.0 min). Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -89- Project No.: 112E-108 Figure 44. Representative ion chromatogram for 8-2 FTOH in the soil extract from a Month 24 untreated control soil by LC/MS/MS. 8-2 FTOH was not present (no peak at 4.18 min). Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -90- Project No.: 112E-108 Figure 45. Representative ion chromatogram for 7-2 sFTOH in the soil extract from a Month 24 untreated control soil by LC/MS/MS. 7-2 sFTOH was not present (no peak at 11.9 min). Company Sanitized. Does not contain TSCA CBi. W ildlife International, Ltd. -91 - Project No.: 112E-108 Figure 46. Representative ion chromatogram for 8-2 FTA in the soil extract from a Month 24 untreated control soil by LC/MS/MS. Trace 8-2 FTA at 12.3 min was <LOQ. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -92- Project No.: 112E-108 Figure 47. Representative ion chromatogram for 7-3 Acid in the soil extract from a Month 24 untreated control soil by LC/MS/MS. 7-3 Acid was not present (no peak at 11.6 min). Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -93 - Project No.: 112E-108 Figure 48. Representative ion chromatogram for 8-2 FTUA in the soil extract from a Month 24 untreated control soil by LC/MS/MS. 8-2 FTUA was not present (no peak at 12.3 min). Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -94- Project No.: 112E-108 Figure 49. Representative ion chromatogram for PFOA in the soil extract from a Month 24 untreated control soil by LC/MS/MS. Trace PFOA at 9.91 min was <LOQ. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -95 - Project No.: 112E-108 Figure 50. Representative ion chromatogram for PFNA in the soil extract from a Month 24 untreated control soil by LC/MS/MS. Trace PFNA at 10.7 min was <LOQ. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -96- Project No.: 112E-108 Figure 51. Representative ion chromatogram for PFDA in the soil extract from a Month 24 untreated control soil by LC/MS/MS. Trace PFDA at 11.4 min was <LOQ. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -97- Project No.: 112E-108 Figure 52. Representative ion chromatogram for PFUA in the soil extract from a Month 24 untreated control soil by LC/MS/MS. Trace PFUA at 12.0 min was <LOQ. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 -98- Wildlife International, Ltd. GC-MS#2 MSD Serial No. 3118A02483 File: C:\HPCHEM\1\DATA\ALFI005\0801012.D Operator: fjl Date Acquired: 30 Apr 105 Instrument: GCMS#2 Sample Name: 4:29 pm 1719-TEX Mise Info: Vial Number : 8 Figure 53. Representative ion chromatograms for 8-2 FTOH in the sampled headspace (Ci8 cartridge extract) from a Day 0 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by GC/MS. - 8-2 FTOH was not present (no peak at 5.0 min). Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -99- p. 100 Project No.: 112E-108 Figure 54. Representative ion chromatogram for 8-2 FTOH in the soil extract from a Day 0 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS. p 101 Company Sanitized. Does not contain TSCA CBI W ildlife International, Ltd. -100- 00T Semple *D: *17W Fie 'O4210S_D0.TELALAE.wifr Peek Heme *a-2<Sr Mb u (m ):'477.0093.0 amu* CowoL-ttJ6-l06,10e.110-(SPtKEr Aiw wMon" i. S a l a l e In d e x : Saeple Typ: IS i CC oa nl ccuelna ttreadc i Cono :r .c : 7 .7 S 1 9 ug * Acq. D ate: Aeq. Tim e: 0 4 /2 1 /OS 0 7 :3 1 :2 7 PH M odified: I Bunching r a c to r : B oise T hreshold: | A rea T h resh o ld : Bus. Smooths: XT W indow: | E x p e c te d XT: i; S e p . W id th : T Sep. H eight: Exp. Peak R a tio : Exp. Adj . R a tio : ;> E x p . v a l . R a t i o : > Use R e la tiv e RT: No 1 2 4 .0 6 1 2 0 .3 1 1 3 0 .C 1 2 .2 0 .2 0 0 .0 1 S.OO 4 .0 0 3 .0 0 He 9000 00 8500 CO 9000 00 7600.00 7000 00 I n t. Type: R e te n tio n T isie: A rea: H eight: S t a r t Ti m Base To Base 12.2 ain 1S075. counts 2931.21603 epa 1 2 .4 4000.00 3500DO - ii 3000-00 Ii i1 j| 2500.00-I : 2000.00 \ 1500.00 ; 1000.00 ! 12.23 0 X ---------- . ------- -- 0 * 702 5 .X 6.7B 10.06, Project No.: 112E-108 Figure 55 Representative ion chromatogram for 8-2 FTA in the soil extract from a Day 0 fortified (250 jig 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -101 - Project No.: 112E-108 Figure 56 Representative ion chromatogram for 8-2 FTUA in the soil extract from a Day 0 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS p. 103 Company Sanitized. Does not contain TSCA CBI W ildlife International, Ltd. Project No.: 112E-108 - 102- I Sampte N am : 5emp<*_OOB* i ^ t o l D i - l f i r Fite: *042106J30_TEtALeiWr P w k Heme *PFOA C-F Uaaa4*s) *413 0068.0 eexT C m iM it *112E-108.l08.110-(SPIKEr Annotetav" Sample Index: IS Sample T ype: C oncentration; c= 1 0 .0 1.00*5 C a lc u la te d Cone: 9.1702 uq a .i ./ k q Aeq. D ate: Acq. Time: 0 4 /2 1 /0 5 . 0 7 :3 1 :2 7 PM 8.50*4 | M odified: ' Punching F a c to r: M oise T h re sh o ld : ' A rea T hreshold: : Hum. S m o o th s: ! RT Window: ! E x p ec te d RT: Sep. w idth: 1Sep. H eight: ! Exp. Peak R atio: 1 Exp. A d] R a tio : i Exp. V al. R a tio : 1 Use R e la tiv e RT: No 1 189.77 948.84 1 3 0 .0 9 .8 2 0 .2 0 0 .0 1 5 .0 0 3 .0 0 NO <=P epa sec m in 8.00*4 8 50*4 8 .0 0 t 7 50*4 700*4 ! In t. Type: Pase To E tse j! R e te n tio n T im e : 9 .8 1 min !! A re : 170080. counts l H e i g h t: 28273.54469 epa ! S t e r t Time: 9 .8 7 min End T im e: 1 0 .0 min 860*4 j ) 6.00*4 j I :.. 5.50*4 | ^ 5.00*4 j 4.00*4 3.30*4 i 3.00*4 2J0M 2.00*4 1J0*4 1.00*4 5000.00 0.00 - 8.62 3 4 r 7 8 8 10 ___________________ Time, r 12 13 14 15 ' 18 17* 18 Figure 57. Representative ion chromatogram for PFOA in the soil extract from a Day 0 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. ,W ildlife International, Ltd - 103 - Project No.: 112E-108 Figure 58. Representative ion chromatogram for PFNA in the soil extract from a Day 0 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 104- p 105 Project No.: 112E-108 Figure 59. Representative ion chromatogram for PFDA in the soil extract from a Day 0 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -105 - I Sam Niw: 'wipf_00r 6anli 1D.`1>ir F4*. *042105 00 TELALAE.Mfr~ Peek Name *C-11 K f *<): *5*3.0/519.0 mu' ~~ Cwiwwnc*112E-10e.10e.110K8PIKr AmoMon:*- :: S a e p le I n d e x : IS S tap le Type: C oncentration: QC 10.0 Uf a .i ./ L *"11 OQeS-j !| C a lc u la t e d C one: 9 .1 8 9 4 u g a . l . / k g i; AAceqq.. B a te : 0047:/2311/:0257 W *.S0e4- Bunching T ac to r: Noi T h resh o ld : i Ar T h resh o ld : Hun. Sneoth: AT Window: E x p e c te d AT: S e p . width.: | Sep. H eight: | Exp. Peak R atio: ! Exp. A d). R atio: Exp. V al. R atio: ; O R e la tiv e RT: 1 114.03 5 7 0 .1 6 1 3 0 .0 1 1 .0 0 .2 0 0 .0 ] 5 .0 0 4 .0 0 3 .0 0 No ep Bin in t. Type: R etention Tu A rea: i H eight : ' S t a r t Tiate: End T in e : Ease To Base 1 1 .8 Bin 198870. count 32316.82269 cps 11.6 Bin 1 2 .0 Bin 0.00*4 ' 8 50*4 8.00*4 760*47.00*4 j t ^ 5.00*4 p. 106 Project No.: 112E-108 2 00*4 ] 5000 00000 11.81 t.OI 031 7 08 7 0 9 3 5 0.79 11.5 7 . , ^ *123913.91 .1306 7 8 10 11 12 13 14 15 18 17 " ie 19 Figure 60. Representative ion chromatogram for PFUA in the soil extract from a Day 0 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. p. 107 Project No.: 112E-108 - 106- Wildlife International, Ltd. GC-MS#2 MSD Serial No. 3118A02483 File: T:\DATA\ALFI025\0801012.D Operator: DW Date Acquired: 20 Apr 106 8:04 pm Instrument: GCMS#1 Sample Name: 1735-TEX Misc Info: 112E-108,109,110 Vial Number : 8 Figure 61. Representative ion chromatograms for 8-2 FTOH in the sampled headspace (Cjs cartridge extract) from a Month 12 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by GC/MS. 8-2 FTOH was not present (no peak at 5.0 min). Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 107- p. 108 Project No.: 112E-108 Figure 62. Representative ion chromatogram for 8-2 FTOH in the soil extract from a Month 12 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS. Trace 8-2 FTOH at 3.98 min was <LOQ. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -108- p. 109 Project No.: 112E-108 Figure 63. Representative ion chromatogram for 8-2 FTA in the soil extract from a Month 12 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI W ildlife International, Ltd. - 109 - p. 110 Project No.: 112E-108 Figure 64. Representative ion chromatogram for 8-2 FTUA in the soil extract from a Month 12 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. .W ildlife International, Ltd - 110- p. 111 Project No.: 112E-108 Figure 65. Representative ion chromatogram for PFOA in the soil extract from a Month 12 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS. . Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - Ill - p. 112 Project No.: 112E-108 Figure 66. Representative ion chromatogram for PFNA in the soil extract from a Month 12 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 112- p. 113 Project No.: 112E-108 Figure 67. Representative ion chromatogram for PFDA in the soil extract from a Month 12 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 113 - p. 114 Project No.: 112E-108 Figure 68. . Representative ion chromatogram for PFUA in the soil extract from a Month 12 fortified (250 pg 8-2 FTOH/kg and 10.0 pg PFCAs/kg) control soil by LC/MS/MS. p. 115 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 - 114- Wildlife International, Ltd. GC-MS#2 MSD Serial No. 3118A02483 File: C:\HPCHEM\1 \DATA\ALFI 005\1201020.D Operator: fj 1 Date Acquired; 30 Apr 105 Instrument: GCMS#2 7:04 pm Sample Name: 1665-TEX Misc Info: Vial Number : 12 Figure 69. Representative ion chromatograms for 8-2 FTOH in the sampled headspace (Cj8cartridge extract) from a Day 0 sterile soil treated with 200 mg/kg(_ }by GC/MS. 8-2 FTOH was not present (no peak at 5.0 min). Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 115 - p. 116 Project No.: 112E-108 Figure 70. Representative ion chromatogram for 8-2 FTOH in the soil extract from a Day 0 sterile soil treated with 200 mg/kgQ J b y LC/MS/MS. Trace 8-2 FTOH at 4.09 min was <LOD. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 116- I SajrgXe'Nsir. " en(ijj14- SamplelO l e e r ' Fie `042105 DCTEtALAE.wWr Peak Mane: *9-2 i r Meea1ee}.*477.Qra930em' ~" Conenent *112E-106-* Awtetnon." Seaple Index: 20 Seaple Type: unknown C o n c en tra tio n : W/A IJW C eleuleted Cone: 0.0000 ug e .i./k g , Aeq. Date: 04/23/0$ . Acq. Tu n : 09:18:31 PR00.00 Bunching T a s te r : H eist Threshold: Area Threshold: Hu. Sm ooths: ' ST Window: S sp ected RT: , Sep. Width: ' Sep. H eight: Lxp. Teak R a tio : Exp. Adj. R atio : Exp. V al. R atio : Use R e la tiv e RT: 120.31 30.0 0.01 5.00 4.00 3.00 ops sec 9000.00 9500.00 9000.00 7900.X } 7Q00.X j I n t. Type: R ese ctio n Tia Area: H eight: S t a r t Time: Sne Tine: Ho Peak OSCO- I: 00.001 p. 117 Project No.: 112E-108 2000.00 1S00.M m oo 04 : T25 Printing Date: Friday, A p ril 22 ,2 0 0 5 . il 10.99 ^ y S g __ _ _ S 9 7 9 9 10 ' 11 12 13 14 IS 19 17 ' 1* ' 19 Figure 71. Representative ion chromatogram for 8-2 FTA in the soil extract from a Day 0 sterile soil treated with 200 mg/kg by LC/MS/MS. 8-2 FTA was not present (no peak at 12.2 min). Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. p. 118 Project No.: 112E-108 - 117- r i f ' Ssmpis Nam: S#mpi*_CH' Sampto 1C 'I M S ' Fie *042106jW.JteukLAESSr* ;[ P M k N*m*- *9-2 < u r Mee*<**) '457 00 9 3 .0 emu* : H Carrwnanc *112E-1C9-* A nnonaon ** S a n p lt Index: 20 S eaple Type: Unknown C on cen tratio n : H/A 1.00*5 - C a lc u la te d Cone: 0.0000 ug a . i . / k q Acq. D ate: A cq. Tim e: 0 4 /2 1 /0 5 0 9 : 1 8 :3 1 PH 950*4 !i M o d if ie d : ! B u n c h in g r e c t o r : |! N o is e T h r e s h o l d : : A re a T h r e s h o l d : jl Nu b . S m o o th s : l! AT W indow : ' E x p e c te d RT: ' Sep. W idth: Sep. H eight: Exp. Peak A atio : Exp. A dj. R atio : >j E x p . V a l . R a t i o : ij U se R e l a t i v e RT: No 1 2 0 1 .9 3 1 0 0 9 .6 4 1 3 0 .0 1 2 .3 0 .2 0 0 .0 1 S.OO 4 .0 0 3 .0 0 No cps cps sec Bin 900s4 4.50*4 4.00*4 7.50e4 7.00*4 - ij X n t. T y p e : R e te n tio n T ine: | A rea: 1 H e i g h t : 1 S t a r t T i e : i| End T iB e : No P e s l N/A N/A N/A N/A N/A Bin c o u n ts cps Bin Bin 4.50*4 9.00*4- 5 5.00*4 : j 4.50*4 - 3.50*4 j 3.00*4 I I2.50*4 -j 2.00*4-j 1.50*4 j i aoo Printing Date: Friday, April 22,2005 23 75 iF" "i77-S? 812 9.79 10.12 116 n J6 13-33. 13-93 6 7 9 9 "tO 11 12 13 14 19 ___Time, min____________ _ Figure 72. Representative ion chromatogram for 8-2 FTUA in the soil extract from a Day 0 sterile soil treated with 200 mg/kg by LC/MS/MS. 8-2 FTUA was not present (no peak at 12.3 min). Company Sanitized. Does not contain TSCA CBI ,W ildlife International Ltd. - 118- p. 119 Project No.: 112E-108 Figure 73. Representative ion chromatogram for PFOA in the soil extract from a Day 0 sterile soil treated with 200 mg/kg(_ "]by LC/MS/MS. Trace PFOA at 9.81 min was <LOQ. Company Sanitized. Does not contain TSCA CBI. ,W ildlife International Ltd. p. 120 Project No.: 112E-108 - 119- SampaNam* *Sm/iY SamphTS^fSr 'V ii' -042105 DOTEl AEw Peak Nam* 'C 4 Add* hha^aa): `4630M15 0a> ` "" ~ Comment *1T2-tC6-` Aiwotaton ~ Saaple In d ex : 20 s u p l t Type: Unknown C oncentration: N/A 1 00*5 C a lc u la te d Core: 0.0000 ug 4 . 1 . /k g Acg. D ate: Acq. Ti m : 0 4 /2 1 /0 5 09:18:31 m 9.50*4 M odified: Aunehing P a sto r: N oise Thxcataold: Area T h resh o ld : N w . Sm ooths: IT Window: E x p e c te d RT: Sep. W idth: Sap. H eight: Exp. Peak R atio: la p . Ad}. R atio : Exp. V al. R atio: Uae R e la tiv e IT : 19 2 .e` 9 6 4 .2S 3 0 .0 10.6 0 .2 0 0 .0 1 5 .0 0 4 .0 0 3 .0 0 No cpi cps 9 00*4 8.50*4 8.00*4 7 50*4 7.00*4 R eten tio n Ti m : H eight: S t a r t Ti m : End T ina: No Peak N/A H/A N/A N/A in epa in in e 30*4 8 00*4 5 500*4 ' OOM 4A M 3.50*4 3 00*4 250*4 - 2AM 1 50*4 : 1 00*4 500000- Printing Date: Friday, Aprii 22,2005 12 a _ S* . ,___ iD - O j0;8* . 0.82 13 0 , 13.72____ ____________ ______ _____ f 5 * 1 11 12 13 M*" 16 17 11 i l Figure 74. Representative ion chromatogram for PFNA in the soil extract from a Day 0 sterile soil treated with 200 mg/kgC Jby LC/MS/MS. PFNA was not present (no peak at 10.6 min). p. 121 Company Sanitized. Does not contain TSCA CBl W ildlife International, Ltd. Project No.: 112E-108 -120- T SenvieNaine'^Senptt OW Sampiell Reek Not : *C-10Ac*r Meet*) -513.O46S.0 *< Comment '112E-106-" AmoMen-** Sawpi* In d ex : 20 S n p t t T y p e: Unknown C o n c en tra tio n : M/A C a lc u lated Cone: 0.35761 ug * . : . / k g I Acq. S a t : 04/21/0$ Acq. T ia e : 0 9 :1 8 :3 1 PM M odified: Punching Facto r: Sola T hreshold: Area T hreshold: Ituw. Sw ooths: RT Window: E x p ected RT: Sap. w idth: Sep. H eight: Exp. Peak P atio Exp. A d;. P atio Exp. V al. R atio Use R e la tiv e RT 167.30 3 6 .$ 0 3 0 .0 11.2 0.20 0.01 $.00 4.00 3.00 No cps cps sec win 9.00e4 ; a.S0e4 | I7.50*4 J 7 00*4 | K i t To Rase R eten tio n Ti m : 1 1 .2 win A re a: 7192.7 counts H eight: 1226.09099 cps S ta rt Tine: 11.1 win End Time: 11.3 win 0.50*4 j 0.00*4 1 t 5 j j 5.00*4 " 490*4 4 00*4 3 90*4 : 2.00*4 | 1.60*4 | ' 1.00*4 * ! sooo o o ' I ___ :i Printing Date: Friday, April 22,2005 2 ' *" 4 ___________ __________ 57 00 " a 3 1230 13 > 3__________ . _______ 10 11 12 13 14 15 16 17 10 9 Figure 75. Representative ion chromatogram for PFDA in the soil extract from a Day 0 sterile soil treated with 200 mg/kg^ ^ p y LC/MS/MS. Trace PFDA at 11.2 min was <LOQ. Company Sanitized. Does not contain TSCA CBI ,W ildlife International Ltd. p. 122 Project No.: 112E-108 - 121 - 1''~ S am j * & m '* 3 M * 3 t 014* "simpW O:*1085* F: *042109 DO T D oAESt ' F**fc Nam*' `C-11 Aa f Ma--( . . ) *553.0610.0 amu* S a a pClaemImnadnrx*1: 136-10*-2*0 AnneMan-** Saapl* Typ: Unknown C oncentration: X/A 00*5 C a l c u l a t e d C e n e: 0 .0 8 2 9 4 0 U9 a . i . / k q Acq. D ata: Acq. T i*e: 0 4 /2 1 /0 5 0 9 :1 8 :3 1 PH 1.90*4 M odiliaC : :: B u n c h in g F a c t o r : [ N o ia* T h r e s h o ld : Ara* T h resh o ld : Ik a. Soootha: ' RT Window: E x p ec te d RT: Sep. W idth: 5p. H eight: Exp. Peak R a tio : . E x p . AO3. R a tio : Exp. V al. R a tio : ' Uaa R e l a t i v e RT: Ko 114.03 S I C .15 1 3 C .0 1 1 .8 C . 20 0.01 5 .0 0 4 .0 0 3 .0 0 Mo cps epa sac M in I n t. Type: l a t a n t i m Tiata: H eight: ' S ta rt T iae: . End Ti *m : Rasa To Baa* 11.1 Min 35*70.4 c o u n ts 5 : . l l t 4 t epa 1 1 .7 Min 12.0 Min 9.00*4 - 8 50*4-' 900*4 1 i 7.50*4 ! ! 9 50*4 i 8.00*4 5.00*4- 4-50*4; 4.00*4 I3.60*4 4 300d4J ! 50*4 200*4 1.50*4 100*4 OOO Printing Date: Friday, April 22,2005 Ma a nsa. *r40> 1262 13.42-1 3 J3 Figure 76. Representative ion chromatogram for PFUA in the soil extract from a Day 0 sterile soil treated with 200 mg/kg "]by LC/MS/MS. Trace PFUA at 11.8 min was <LOD. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. p. 123 Project No.: 112E-108 -122 - Wildlife International, Ltd. GC-MS#2 MSD Serial No. 3118A02483 File: T:\DATA\ALFI025\1301021.D Operator: DW Date Acquired: 20 Apr 10S 11:09 pm Instrument: GCMS#1 Sample Name: 1682-TEX Misc Info: 112E-108 Vial Number : 13 Figure 77. Representative ion chromatograms for 8-2 FTOH in the sampled headspace (C]8 cartridge extract) from a Month 12 sterile soil treated with 200 mg/kgC Jby GC/MS. Company Sanitized. Does not contain TSCA CBI W ildlife International, Ltd. - 123 - p. 124 Project No.: 112E-108 Figure 78. Representative ion chromatogram for 8-2 FTOH in the soil extract from a Month 12 sterile soil treated with 200 mg/kgC 7 by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI W ildlife International, Ltd. - 124- p. 125 Project No.: 112E-108 Figure 79. Representative ion chromatogram for 8-2 FTA in the soil extract from a Month 12 sterile soil treated with 200 mg/kg_ 3 by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd - 125 - Project No.: 112E-108 Figure 80. Representative ion chromatogram for 8-2 FTUA in the soil extract from a Month 12 sterile soil treated with 200 mg/kg Jby LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 126- p. 127 Project No.: 112E-108 Figure 81. Representative ion chromatogram for PFOA in the soil extract from a Month 12 sterile soil treated with 200 mg/kg__ ")oy LC/MS/MS. Company Sanitized. Does not contain TSCA CBl. W ildlife International, Ltd. - 127- p. 128 Project No.: 112E-108 Figure 82. Representative ion chromatogram for PFNA in the soil extract from a Month 12 sterile soil treated with 200 mg/kg^ by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI .W ildlife International, Ltd -128- p. 129 Project No.: 112E-108 Figure 83. Representative ion chromatogram for PFDA in the soil extract from a Month 12 sterile soil treated with 200 mg/kgC Jb y LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd -129- Project No.: 112E-108 Figure 84. JRepresentative ion chromatogram for PFUA in the soil extract from a Month 12 sterile soil treated with 200 mg/kg by LC/MS/MS. p. 131 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. Project No.: 112E-108 - 130- Wildlife International, Ltd. GC-MS#2 MSD Serial No. 3118A02483 File: C:\HPCHEM\1\DATA\ALFI005\1001014.D Operator: fjl Date Acquired: 30 Apr 105 5:06 pm Instrument: GCMS#2 Sample Name: 1593-TEX Misc Info: ' Vial Number : 10 Figure 85. Representative ion chromatograms for 8-2 FTOH in the sampled headspace (Ci8cartridge extract) from a Day 0 live soil treated with 200 mg/kg(_ ^ b y GC/MS. 8-2 FTOH is not present (no peak at 5.0 min). Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -131 - p. 132 Project No.: 112E-108 Figure 86. Representative ion chromatogram for 8-2 FTOH in the soil extract from a Day 0 live soil treated with 200 m g / k g Q b y LC/MS/MS. Trace 8-2 FTOH at 3.93 min was <LOD. Company Sanitized. Does not contain TSCA CBI. Wildlife International, Ltd. -132- p. 133 Project No.: 112E-108 Figure 87. Representative ion chromatogram for 7-2 sFTOH in the soil extract from a Day 0 live soil treated with 200 mg/kgjT Joy LC/MS/MS. Trace 7-2 sFTOH at 11.9 min was <LOQ. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. I Sample Name:'Sampi* Oil* Sample ID:'1563* FI 'O42U_D0_TElALA T Peek to rn * l - J (S r U n t i l ) ' **77.00830 emu* Comment *112E-105-" j S u p l i Index: 17 S aaple Type: Unkn C oncentration: H/A | Calculate! Cone: < 0 I Aeq. Dace: 0 4 /2 1 /0 5 * A cq. Ti m : 05:14:1 I M odified: : B u n c h in g f a c t o r :: N oiaa T h re s h o ld :: i< A re a T h r e s h o ld : ij Mum. Sm o o th s: I- RT Window: E x p e c te d BT: , Sep. W idth: jj S e p . H e i g h t : | E xp. Pea): R a tio : ij E x p . A d}. R a tio : '! E xp. v a l . R a tio : ' Use R e l a t i v e RT: NO 1 2 4 .0 6 120.31 1 3 0 .0 1 2 .2 0 .2 0 0.01 5 .0 0 4 .0 0 3 .0 0 No cps cps sec m in 8000 00 50000 000.00 7500.00 ' i 7000.00 I In t. Type: . R e te n tio n Ti m : A rea: H eight: S ta r t Tuee: End Time: Base To Base 12.2 Bin 73.81 count! 142.09353 epa 12.1 n in 12.4 Bin 5600.00 | 5000.00 , j j 600000 | ~ *50000 4000.00 3600.00* 3000.00 ] jj 1500.00' 100000 500.00 - 133 - p. 134 Project No.: 112E-108 Figure 88. ' Representative ion chromatogram for 8-2 FTA in the soil extract from a Day 0 live soil treated with 200 mg/kg(j ^by LC/MS/MS. Trace 8-2 FTA at 12.2 min was <LOD. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 134- p. 135 Project No.: 112E-108 Figure 89. Representative ion chromatogram for 7-3 Acid in the soil extract from a Day 0 live soil treated with 200 mg/kg' JJby LC/MS/MS. 7-3 Acid is not present (no peak at 11.6 min). Company Sanitized. Does not contain TSCA CBI. W ildlife InternationalLtd. p. 136 Project No.: 112E-108 - 135 - SainptaNama: "Sampt# O'M* SwnptotO:`iSo* Fii.;tM2106.00_TELALAE wrfr Pn K Hans: *6-2(Uf ktte#(a*).*437.0383.0 i W Cemmant *112E-106-* Annotaten " j] S a a v l* I n d e x : 17 |] S u p l i T y p e: Unknown j! C o n c e n t r a tio n : N/A j C a lc u la te d Cone: 0.0000 ug a .i./k g I COOS' |i A cq . D o t e j A eg . Ti m : 04/21/05 0 0 :1 4 :1 PH 8.30*4 -j M odified: Bunching F a c to r: 'N o ra* T h resh o ld : X rtt T hreshold: Num. S tao o th e : | AT Window: E x p e c te d AT: Sep. W idth: Sep. H eight: Exp. Peak R atio : Exp. A d). R atio: Exp. vl. R atio : U se R e l a t i v e AT: No 1* 2 0 1 .9 3 1009.64 1 3 0 .0 1 2 .3 0 .2 0 0.01 S .0 0 4 .0 0 3 .0 0 Ko cps cp* sec n in 9 00*4 -j 30*4 2 730*4 7.00*4 In t. Type: R e te n tio n Titae: A rea: H eight: S t a r t Ti m : End T in e : No Peak N/A n/ a N/A n/A N/A Bin c o u n ts cp* m in n in 6.30*4 I. ^ 5.00*4 , 3 50*4 | 3.00*4 j 2.50*4 [ I 2.00*4 | 1.00*4 I j500000 0.00 - ..................... ..... 23 4 ~5 B7 *9 10 11 12 13 14 15 1 ta. win Figure 90. Representative ion chromatogram for 8-2 FTUA in the soil extract from a Day 0 live soil treated with 200 mg/kg(( Jby LC/MS/MS. 8-2 FTUA was not present (no peak at 12.3 min). Company Sanitized. Does not contain TSCA CBI W ildlife International, Ltd. - 136- I Sempts Herrn:$*B*l*_0ir Sanpt* ID;'1583' Me: TM210SJ P**k NtttM- *PFOA C-T M**<#*): *413.0/389.0 amu* CammanC ` 1121-1 Oft-' A nnoM en:- S ama ppll*e TI nydpe x : Un1k7nown C oncentration: N/A C a lc u la te d Cone: C.6S38S uq a . i . / k q Acq. D ate: Acq. Tim*: 0 1 /2 1 /0 5 0 8 :1 4 :1 8 PH 0*4 < M odified: Eunehinq F a c to r: N oise T h resh o ld : A rea T hresh o ld : Mum. S m o o th s: FT Window: E x p e c te d RT: Sep. W idth: Sep. H eiqht: Exp. Peek R atio Exp. AdJ. R atio Exp. VaL. R a tio Use R e l a t i v e RT 1 8 9 .7 7 9 4 8 .8 4 3 0 .0 9 .8 2 0 .2 0 0 .0 1 5 .0 0 4 .0 0 3 .0 0 No epa CP. sec in 9.00*4 ' 6.S0*4 8.00*4 ' 7.50*4 7.00*4 In c. Type: R e te n tio n Time: A rea: H eight: S t a r t Time: End Time: Rase To la se 9 .8 3 min 14347. 2460.59297 cps 9 .7 0 1 0 .0 6.50*4 600*4 fr. 5.90*4 5O0M * 4.50*4-. i 4.00*4 - i j 3.50*4 3.00*4 2.50*4 2.00*4 1 S04 5000.00 ; 0.00 ` 5070 p. 137 Project No.: 112E-108 12 13 14 15 18 17 18 IS Figure 91. Representative ion chromatogram for PFOA in the soil extract from a Day 0 live soil treated with 200 m g/kgf _^by LC/MS/MS. Trace PFOA at 9.83 min was <LOQ. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -137- Ttempi* Nam*- `tempi P n k Nam*. "C-B A otf Comment *112E-tOB-' Oil* Sample ID.*1593* F4*.*04210S_00_TEUMA.w M*M(**): '483.0M19.0aimT Sam ple In d e x : 1? S n p lt Type: Unknown C oncentration: N/A C a lc u la te d Cone: 0.J792S Aeq. D ata: 0 1 /2 1 /0 ! Acq. Tim e: 08:11:11 j M odified: : Bunching F a c to r: N oise T h resh o ld : A rea T h resh o ld : Mum. S m o o th s: RT W indow : E x p e c te d RT: Sep. W idth: 1 S e p . H e i g h t: >; e x p . P eak R a t i o : 'i E x p . A d } . R a t i o : -J E x p . V a l . R a t i o : U se R e l a t i v e RT: No 1 1 9 2 .8 5 6 4 .2 5 3 0 .0 10.6 0.20 0.01 5 .0 0 4 .0 0 3 .0 0 No 900*4 J In t. Type: R etention ` A rea: , H e i g h t: : S ta r t Tu n : \ End Time: E ase To Base 1 0 .6 min 5541.0 c o u n ts 984.41642 cps 1 0 .4 a m 1 0 .7 a in p. 138 Project No.: 112E-108 3.50*4 j 3.00*4 ] 2.50*4 ! 2.00*4- 5000.00 000 Figure 92. Representative ion chromatoeram for PFNA in the soil extract from a Day 0 live soil treated with 200 mg/kg _J b y LC/MS/MS. Trace PFNA at 10.6 min was <LOD. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -138- MtU.tM_TKLALAE.Si p. 139 Project No.: 112E-108 li KT Hindovi 1tspaettd AT: ||*p. Widch: || S*p. Migtic: 30.0 11-2 0 .2 0 *0.01 liSup. Ad}. >*: .00 ,!Cap. Vj, A*tlc: 3.00 in Jteitn tio n Tli Art*: . tight: i7.90*4 i 7.00*4 f 130* ' 3.00*4 1JM 1.00*4 9000.00 4& I7 09 *14 IS " 17 ' 19 S ' Figure 93. Representative ion chromatogram for PFDA in the soil extract from a Day 0 live soil treated with 200 mg/kg_ J b y LC/MS/MS. Trace PFDA at 11.2 min was <LOQ. Company Sanitized. Does not contain TSCA CBI, W ildlife International, Ltd. p. 140 Project No.: 112E-108 - 139- I SampI* Nam:-SengM* S ii* Pa k Nam' "C-1 f Adid" S * n * tetO .`1S03* FU*: "042106 DO TELALAEwtr *903 0 5 1 0 .0 amu* t a a pCiocrmImndnetx"1: 12E-106-*17 AnneM tc n ~ Saaple Type: C o n centration: Unknown N/A 1 OOaS- C a lc u lated Cone: 0.0000 ug a .i./k g Acq. D ate: Acq. T ine: 0 4 /2 1 /0 5 0 8 :1 4 :1 8 PK 9.50e4 . M odified: bunching f a c to r : N oise T h resh o ld : A rea T h resh o ld : Nun. Sm ooths: ! RT Window: E xpected RT: Sap. W idth: Sep. H eight: Bxp. Peak R a tio : Bxp. A dj. R a tio : Bxp. V al. R a tio : Use A a l a t i v a RT: Mo 1 1 1 4 .0 3 5 1 0 .IS 1 3 0 .0 1 1 .8 0 .2 0 0 .0 1 5 .0 0 4 .0 0 3 .0 0 Ho eps cps sec sun S.00e4 6.50a4 6.00*4 7.50*4 7.00*4 X nt. Type: ! R e te n tio n Tim e: A rea: ! h eig h t: : S t a r t Tima: ' End T i m : No Peak V/A N/A N/A N/A K/A m id cps m in 6.50*4 6.004 j, S 4.50*4 j ti I 4 004 - S .0 M 2.50*4 2.00*4 1.50*4 1.00*4 600000 j 0.00 ^ -------- ---------- ---------- ----------,---- 12 3 4 5 --------------------- , - , ------ 1--------- ,----------r ------ --------------------- -----------,--------, ------------------ -- 6 7 5 9 10 11 12 13 14 15 16 17 16 19 . Tima,win ____________________________ Figure 94. Representative ion chromatogram for PFUA in the soil extract from a Day 0 live soil treated with 200 mg/kg_ ^ by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. .W ildlife International, Ltd - 140- p. 141 Project No.: 112E-108 Figure 95. Representative ion chromatograms for 8-2 FTOH in the sampled headspace (Cis cartridge extract) from a Month 24 live soil treated with 200 mg/kg(j Jb y GC/MS. Company Sanitized. Does not contain TSCA CBI. .W ildlife International, L td - 141 - p. 142 Project No.: 112E-108 Figure 96. Representative ion chromatogram for 8-2 FTOH in the soil extract from a Month 24 live soil treated with 200 mg/kgt J b y LC/MS/MS. Trace 8-2 FTOH at 3.96 min was <LOQ. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 142- p. 143 Project No.: 112E-108 Figure 97. Representative ion chromatogram for 7-2 sFTOH in the soil extract from a Month 24 live soil treated with 200 mg/kg by LC/MS/MS. Trace 7-2 sFTOH at 11.9 min was <LOQ. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 143 - p. 144 Project No.: 112E-108 Figure 98. Representative ion chromatogram for 8-2 FTA in the soil extract from a Month 24 live soil treated with 200 mg/kg Jby LC/MS/MS. Trace 8-2 FTA at 12.3 min was <LOQ. Company Sanitized. Does not contain TSCA CBI W ildlife International, Ltd. - 144- p. 145 Project No.: 112E-108 Figure 99. Representative ion chromatogram for 7-3 Acid in the soil extract from a Month 24 live soil treated with 200 mg/kg J b y LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 145 - p. 146 Project No.: 112E-108 Figure 100. Representative ion chromatogram for 8-2 FTUA in the soil extract from a Month 24 live soil treated with 200 mg/k^Q ^ by LC/MS/MS. Trace 8-2 FTUA at 12.3 min was <LOQ. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 146- p. 147 Project No.: 112E-108 Figure 101. Representative ion chromatogram for PFOA in the soil extract from a Month 24 live soil treated with 200 mg/kg _Jby LC/MS/MS. Note: Secondary dilution required and reported for PFOA. Original analysis was over calibration range. Company Sanitized. Does not contain TSCA CBI W ildlife International, Ltd. - 147- p. 148 Project No.: 112E-108 Figure 102. Representative ion chromatoeram for PFNA in the soil extract from a Month 24 live soil treated with 200 mg/kgC T3by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 148- p. 149 Project No.: 112E-108 Figure 103. Representative ion chromatogram for PFDA in the soil extract from a Month 24 live soil treated with 200 mg/kgC J y LC/MS/MS. Company Sanitized. Does not contain TSCA CBI W ildlife International, Ltd. - 149- p. 150 Project No.: 112E-108 Figure 104. Representative ion chromatogram for PFUA in the soil extract from a Month 24 live soil treated with 200 mg/kg ]by LC/MS/MS. Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. p. 151 Project No.: 112E-108 - 150 Appendix I Measured Concentration of Selected Analytes (pg/kg Soil Dry Weight) Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -151 - p. 152 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFOA (pg/kg) in Soils Treated with f 3 Soil Type Ultisol Sample Interval Day 0 Weekl Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Aerobic Live Sterile <LOQ <LOQ 17.8 19.1 32.0 36.5 57.8 61.4 122.1 150.0 269.7 373.8 376.4 441.1 487.0 558.6 367.7 344.1 340.1 362.6 410.7 328.7 365.9 329.1 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 2.0 <LOQ 2.4 <LOQ 2.2 <LOQ 4.9 <LOQ 7.8 <LOQ <LOQ <LOQ Anaerobic Live Sterile <LOQ <LOQ 21.7 22.7 26.8 23.9 51.5 40.3 70.0 73.3 114.7 133.5 148.6 104.7 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 2.5 <LOQ 2.8 <LOQ LOD = limit o f detection (0.206 pg/kg) LOQ = limit o f quantitation (2.0 |ig/kg) Thursday, N ovem ber 08, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -152- p. 153 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFOA (jig/kg) in Soils Treated with J Sample Soil Type________ Interval Mollisol DayO Week 1 Week 2 Week4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Aerobic Live Sterile <LOQ <LOQ 15.4 15.1 17.8 18.0 21.7 20.2 31.8 30.3 46.0 58.6 74.7 74.4 92.5 69.3 103.8 94.0 98.5 247.9 126.9 118.8 229.3 207.5 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 2.9 <LOQ 3.2 2.3 3.4 3.3 3.0 3.1 LOD = limit of detection (0.206 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) Anaerobic Live Sterile <LOQ <LOQ 14.7 15.1 18.8 18.1 20.2 22.3 42.8 43.2 78.5 61.5 117.4 91.0 . <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 2.7 <LOQ 3.6 2.4 Thursday, N ovem ber OS, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 153 - p. 154 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFOA in Soils Treated with Soil Type Sample Interval Aerobic Live Sterile Alfisoi -- DayO Week 1 Week2 Week4 . Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month IS Month 24 <LOQ <LOQ 8.5 8.2 11.4 11.0 14.9 15.8 23.2 25.0 32.0 33.1 58.4 52.5 97.9 93.7 65.4 84.2 133.1 103.5 194.4 155.9 196.5 190,7 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 3.3 <LOQ <LOQ <LOQ LOD = limit o f detection (0.206 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) Anaerobic Live Sterile <LOQ <LOQ 9.4 10.9 14.1 15.4 19.7 19.8 17.9 31.1 90.0 77.8 99,3 83.5 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 2.0 <LOQ 2.2 <LOQ Friday, O ctober 22, 2Q7 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 154- p. 155 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFOA (jrg/kg) in Soils Treated with ^ Soil Type Inceotisol 1Sample Interval . Day 0 Week 1 Week 2 Week 4 Month2 Month 4 Months Month 9 Month 12 Month 15 Month 18 Month 24 Aerobic Anaerobic Live Sterile______ Live Sterile <LOQ <LOQ 18.9 20.8 28.6 29.0 55.7 54.7 122.2 97.7 190.4 189.4 264.7 250.4 288.5 339.5 367.8 350.0 402.3 385.3 422.5 446.5 530.9 554.1 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 2.1 <LOQ 2.8 <LOQ 4.4 <LOQ 5.6 3.0 6.2 2.8 4.2 2.5 <LOQ <LOQ 20.9 17.7 26.5 26.8 75.5 48.1 138.0 144.3 284.5 302.6 327.0 347.1 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 5.0 <LOQ 7.6 <LOQ LOD = limit of detection (0.206 pg/kg) LOQ = limit o f quantitation (2.0 pg/kg) Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -155 - p. 156 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTUA Qig/kg) in Soils Treated w ith ^ 3 Sample Aerobic Anaerobic Soil Type________ Interval____________Live Sterile______ Live Sterile Ultisol . Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month IS Month 24 <LOD <LOQ <LOQ <LOQ 2.1 2.5 4.0 3.2 6.3 6.7 12.3 12.7 12.1 19.3 30.9 19.7 6.0 7.6 11.3 13.5 15.6 6.4 15.6 32.3 <LOD <LOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD <LOQ cLOQ <LOQ CLOQ CLOQ CLOQ cLOQ cLOQ cLOQ CLOQ cLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD LOD = limit o f detection (0.119 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. ---------------------------------------------------------------------------------------------------------------------------------------------------------------------------------j --------------------------------------------------------------- -156- p. 157 Project No.: 112E-108 Wildlife International, Ltd, Project Number 112E-108 Measured Concentrations of 8-2 FTUA (fig/kg) in Soils Treated w ith ^ Soil Type Mollisol Sample Interval Day 0 Week 1 Week2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month IS Month 24 Aerobic Live Sterile CLOQ <LOQ <LOD <LOD <LOD <LOD <LOQ <LOQ cLOQ cLOQ CLOQ CLOQ CLOD cLOQ CLOQ cLOQ <LOQ cLOQ CLOD CLOD CLOQ CLOQ 3.0 cLOQ CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOQ CLOQ CLOD CLOD LOD = limit o f detection (0.119 pg/kg) LOQ = limit o f quantitation (2.0 ig/kg) Anaerobic Live Sterile cL O Q CLOQ CLOQ cLOQ CLOD CLOD CLOD cLOQ cLOQ CLOQ CLOQ CLOQ cLOQ CLOQ CLOD CLOD cLOQ cLOD CLOD CLOD cLOD CLOD CLOD cLOD CLOD CLOQ CLOD CLOD Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 157- p. 158 Project No.: 112E-108 Wildlife International, Ltd, Project Number 112E-108 Measured Concentrations of 8-2 FTUA (fig/kg) in Soils Treated w ith^ ~2 Soil Type Alfisol Sample Interval Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Aerobic Live Sterile <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOQ <LOQ <LOD <LOD <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOD <LOD <LOD -CLOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOQ Anaerobic Live Sterile <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOQ <LOD <LOQ 3.9 2.2 2.3 <LOQ <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOQ LOD = limit o f detection (0.119 gg/kg) LOQ = limit o f quantitation (2.0 gg/kg) Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBi. W ildlife International, Ltd. - 158- p. 159 Project No.-: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTUA (fig/kg) in Soils Treated with (f Soil Type Incentisol Sample Interval Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Aerobic Live Sterile <LOQ <LOQ <LOD <LOD <LOQ <LOQ 5.9 5.0 25.2 12.3 77.7 88.9 164.0 160.4 192.1 161.0 209.5 206.9 225.6 '25C2'i.11 256.2 242.7 248.5 239.0 <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOD 2.7 <LOQ 2.2 <LOQ <LOQ <LOQ Anaerobic Live Sterile <LOD <LOD <LOD <LOD <LOD <LOQ 7.7 <LOQ 5.6 5.5 13.0 13.0 15.4 10.0 <LOD CLOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOQ LOD = limit o f detection (0.119 pg/kg) LOQ = limit o f quantitation (2.0 pg/kg) Friday, October 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -159- p. 160 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTA (fig/kg) in Soils Treated with. ^ S oil Type Ultisol Sam ple In terval Day 0 W eek 1 W eek 2 W eek 4 M onth 2 M onth 4 M onth 6 M onth 9 M o n th 12 M o n th 15 M o n th 18 M onth 24 A erobic L ive S terile <LOD <LOD <LOQ <LOQ 3.8 3.7 6.2 4.7 8.6 8.5 9.7 8.0 10.1 19 0 19.7 12.0 3.0 4.4 4.3 3.8 6.7 2.9 4.7 5.2 <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOD <LOD <LOD <LOD 2.0 A naerobic L ive S terile <LOD <LOD <LOD <LOD <LOD <LOQ <LOD <LOD <LOD <LOD <LOD <LOQ <LOQ <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD -CLOD <LOD CLOD <LOD -CLOD <LOD <LOD LOD = limit of detection (0.503 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) F riday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 160- p. 161 Project No.: 112E-108 Wildlife International, Ltd. Project Number 11ZE-108 Measured Concentrations of 8-2 FTA (pg/kg) in Soils Treated withC Soil Type Mollisol Sample Interval DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Aerobic U v e Sterile cLOD <LOQ <LOQ <LOD <LOD CLOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOQ 2.3 <LOD <LOD <LOD <LOD <LOQ CLOQ <LOD <LOD <LOD <LOD <LOD <LOD CLOD cL O D CLOD CLOD CLOD cL O D CLOD cLOD CLOD CLOD CLOD cLOD LOD = limit of detection (0.503 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) Anaerobic Live Sterile CLOD CLOD CLOD <LOD CLOD CLOD <LOD cLOD cLOD cL O D cL O D cLOD CLOD CLOD CLOD cLOD CLOD cL O D CLOD cL O D CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD Friday, October 12 ,2 0 0 7 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 161 - p. 162 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTA (jig/kg) in Soils Treated with Soil Type Alfisol Sam ple Interval Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month IS Month 24 Aerobic Live Sterile <LOD <LOD <LOD <LOD <LOD <LOD <L0D <LOD <LOD CLOD <LOD <LOD CLOD <LOD CLOD <LOD CLOD cLOD CLOD CLOD CLOD CLOD cLOQ CLOQ cLOD CLOD cL O D CLOD CLOD CLOD CLOD cL O D CLOD cL O D CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD L O D = limit o f detection (0.503 pgflcg) L O Q = limit of quantitation (2.0 fig/kg) Anaerobic Live Sterile CLOD CLOD CLOD CLOD CLOD CLOD cLOQ cLOQ cLOD CLOD CLOQ cLOQ cLOQ CLOQ cLOD CLOD CLOD cLOD cL O D CLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD cLOQ Fridayt O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 162- p. 163 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-:08 Measured Concentrations of 8-2 FTA (pg/kg) in Soils Treated with. Soil Type InceDtisol Sample Interval Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month IS Month 18 Month 24 Aerobic Live Sterile <LOQ <LOQ CLOD <LOD <LOQ <LOQ 5.5 4.8 18.0 13.0 73.7 75.7 162.8 144.6 163.8 126.8 133.2 140.6 193.0 205.7 213.7 226.5 202.5 221.7 <LOD <LOD <LOD <LOD <LOD CLOD CLOD <LOD CLOD CLOD cLOQ CLOD 2.9 cLOQ 2.8 CLOQ cLOQ cLOQ LOD = limit of detection (0.503 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) Anaerobic Live Sterile CLOD CLOD CLOQ CLOD CLOD CLOD 6.6 <LOQ 2.5 2.6 6.1 5.9 8.5 5.3 CLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOQ . Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 163 - p. 164 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFNA (ng/kg) in Soils Treated witfa^ *3 Soil Type Ultisol Sample Interval Day 0 Week 1 Week 2 Week4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Aerobic Live Sterile Anaerobic Live Sterile <LOQ <LOQ 7.0 7.2 11.5 12.3 17.6 16.7 24.0 21.5 28.0 30.0 28.5 30.7 33.2 30.1 8.6 15.7 23.8 26.2 29.8 24.4 31.0 29.5 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ , 6.5 7.0 9.2 9.5 15.7 13.7 15.4 21.5 23.4 22.4 30.0 25.5 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOD = limit o f detection (0.124 pg/kg) LOQ = limit o f quantitation (2.0 pg/kg) Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBl. W ildlife International, Ltd. -164- p. 165 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFNA (pg/kg) in Soils Trented with J Soil Type Mollisol Sample Interval Day 0 Week 1 Week 2 Week 4 Month. 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Aerobic Live Sterile <LOQ <LOQ 5.8 6.0 5.7 8.3 10.6 12.3 18.1 17.2 22.4 22.5 21.2 20.0 17.3 11.1 19.5 18.4 14.6 25.8 20.7 17.1 25.7 34.7 <LOD <LOD <LOQ <LOQ <LOD <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ Anaerobic Live Sterile <LOQ <LOQ 4.2 4.3 5.8 4.6 4.3 5.9 6.5 8.2 12.1 9.3 16.0 12.1 <LOD <LOD <LOQ <LOQ <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOD = limit o f detection (0.124 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 165- p. 166 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFNA in Soils Treated withC. Soil Type Alfisol S am ple Interval ' Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Aerobic Live Sterile <LOQ <LOQ 3.3 4.0 4.6 3.9 6.6 7.7 10.4 16.2 10.6 13.5 8.9 15.9 17.6 23.3 13.4 17.5 23.1 15.2 15.7 17.7 25.3 22.0 <LOD <LOD <LOQ <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOQ <LOQ <LOQ <LOD <LOQ <LOQ LOD = limit of detection (0.124 pg/kg) LOQ = limit of quantitation (2.0 jig/kg) Anaerobic Live Sterile <LOQ <LOQ <LOQ 2.4 2.7 3.2 4.8 4.9 3.6 6.6 8.9 9.2 11.2 7.9 <LOQ <LOQ <LOQ <LOD <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ F riday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 166- p. 167 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFNA (pg/kg) in Soils Treated with(T T Soil Type Incentisol Sample Interval Day 0 Week 1 Wed: 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Aerobic Live Sterile <LOQ <LOQ 20.3 25.1 29.0 33.4 36.9 35.2 62.2 63.9 59.4 61.9 67.9 79.9 79.9 79.5 71.5 70.7 73.9 74.1 79.2 80.6 96.5 104.2 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOD = limit o f detection (0.124 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) Anaerobic Live Sterile <LQ <LOQ 9.5 7.2 13.1 13.5 34.9 21.8 24.8 26.6 28.7 35.7 34.0 36.1 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ Friday, O ctober 12, 2001 Company Sanitized. Does not contain TSCA CBI. ,W ildlife International Ltd. - 167- p. 168 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFDA (jrg/kg) in Soils Treated w ith j. Soil Type Ultisol Sample Interval Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 M onth 24 Aerobic Live Sterile <LOQ <LOQ 4.6 4.8 7.6 8.4 10.7 11.9 18.0 18.5 26.6 28.2 30.4 35.5 37.9 39.3 9.2 20.9 33.3 34.0 48.1 36.5 50.7 44.3 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOD = limit o f detection (0.114 pg/kg) LOQ = limit o f quantitation (2.0 pg/kg) Anaerobic Live Sterile <LOQ <LOQ 4.8 5.2 6.9 7.3 9.3 8.5 13.2 15.0 25.4 28.4 21.9 19.6 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ Thursday, N ovem ber OS, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 168 - p. 169 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Soil Type Mollisol Measured Concentrations of PFDA (jttg/kg) in Soils Trested with^ J iSample Interval Aerobic U ve Sterile Anaerobic Live Sterile Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ 3.4 3.7 4.7 5.2 6.2 6.2 9.9 10.1 14.6 16.4 17.3 17.6 16.6 12.4 19.7 18.6 14.6 27.7 22.0 21.4 45.4 48.5 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 2.0 <LOQ <LOQ <LOQ <LOQ 2.1 <LOQ <LOQ <LOQ <LOQ 3.7 3.7 5.4 4.7 6.5 6.7 11.0 10.7 17.4 14.2 21.0 17.5 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOD = limit o f detection (0.114 pg/kg) LOQ = limit o f quantitation (2.0 pg/kg) Thursday, N ovem ber 08, 2007 Company Sanitized. Does not contain TSCA CBl. W ildlife International, Ltd. - 169- p. 170 Project No.: 112E-108 Wildlife International, Ltd. Project Number 1 1 2 E-1 0 8 Measured Concentrations of PFDA (jig/kg) in Soils Trested with 3 S am ple Aerobic Anaerobic Soil Type_______Interval_________ L ive Sterile_____ Live Sterile Alfisol DayO Weekl Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month IS Month 18 Month 24 <LOQ <LOQ <LOQ 2.1 2.9 3.0 4.4 4.8 8.1 9.2 8.4 9.8 9.3 12.5 17.1 19.7 12.9 16.1 26.3 15.3 23.3 20.7 37.6 36.8 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ 2.4 3.1 3.6 5.4 5.6 4.8 8.7 12.9 13.2 14.6 12.2 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <l o q <LOQ <LOQ <LOQ LOD = limit o f detection (0.114 pg/kg) LOQ = limit o f quantitation (2.0 pg/kg) Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 170- p. 171 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Soil Type Inceotisol Measured Concentrations ofPFDA (ng/kg) in Soils Treated w iti 3 Sample Interval Aerobic Live Sterile Anaerobic Live Sterile Day 0 Week I Week2 Week4 Month. 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month IS Month 24 <LOQ <LOQ 4.5 5.4 8.1 8.3 15.6 15.6 34.3 29.8 43.5 50.4 52.3 68.8 66.7 57.2 62.0 69.8 62.9 66.0 81.4 77.9 86.7 " 89.6 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 2.1 <LOQ 2.6 <LOQ 3.1 3.1 2.9 2.3 2.3 2.0 <LOQ <LOQ 5.3 4.5 7.5 7.8 20.9 11.5 21.4 22.9 33.7 39.3 47.0 41.0 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 2.7 <LOQ LOD = limit of detection (0.114 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -171 - p. 172 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFUA (jig/kg) in Soils Treated witb(~ Soil Type Ultisol - Sample Interval Day 0 Week 1 Week2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Aerobic Live Sterile <LOQ <LOQ <LOQ <LOQ 3.0 3.3 5.1 4.7 8.5 8.0 13.2 15.0 16.0 16.4 18.8 17.0 3.6 10.5 15.1 15.5 19.2 16.1 22.5 22.7 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ Anaerobic Live Sterile <LOQ <LOQ <LOQ <LOQ 2.7 2.6 4.1 3.9 6.9 8.2 15.5 13.1 18.2 17.6 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ * LOD = limit of detection (0.128 ng/kg) LOQ = limit o f quantitation (2.0 fig/kg) Friday, O ctober 22, 2007 Company Sanitized. Does not contain TSCA CBI. Wildlife International, Ltd. - 172- p. 173 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFUA (fig/kg) in Soils Treated with Soil Type Mollisol Sample Interval DayO Week 1 Week2 Week4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Aerobic Uve Sterile <LOQ <LOQ <LOQ <LOQ <LOQ 2.1 2.7 2.7 6.0 5.7 10.0 10.8 9.5 9.6 8.2 4.6 8.8 8.6 6.1 11.6 10.4 9.2 14.5 21.3 <LOQ <LOQ <LOD <LOD <LOD <LOD <LOQ <LOQ <LOQ <LOD <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ Anaerobic Live Sterile <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 2.0 2.5 3.5 6.0 4.7 6.8 5.5 <LOQ <LOQ <LOQ <LOQ <LOD <LOD <LOQ <LOQ <LOD <LOD <LOQ <LOQ <LOQ <LOD LOD = limit of detection (0.128 (ig/kg) LOQ = limit o f quantitation (2.0 pg/kg) Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. .W ildlife International, L td - 173- p. 174 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFUA (pg/kg) in Soils Treated withf_ 3 Sample Soil Type________ Interval Alfisol DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Aerobic Live Sterile <LOD <LOD <LOQ cL O Q <LOQ CLOQ 2.0 2.3 4.6 6.1 4.1 6.2 3.2 6.2 7.3 11.3 7.6 9.2 13.5 5.8 7.0 7.2 14.4 10.1 <LOD CLOD <L0Q cLOQ CLOD CLOD CLOD CLOD <LOD CLOD <LOQ CLOD CLOD CLOQ cLOQ CLOD CLOQ CLOQ Anaerobic Live Sterile CLOD CLOD CLOQ cL O Q CLOQ CLOQ cLOQ cLOQ cLOQ 3.0 3.1 3.3 4.5 3.5 cLOD CLOD cLOD CLOD cL O Q cL O Q cL O D cLOD cL O Q CLOD CLOD CLOD CLOQ CLOQ LOP = limit o f detection (0.128 pg/kg) LOQ = limit o f quantitation (2.0 pg/kg) Fridayt O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. Wildlife InternationalLtd. -174- p. 175 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFUA ( in Soils Treated with Sample Aerobic Anaerobic Soil Type________ Interval___________ Live Sterile______ Live Sterile InceDtisol Day 0 Week 1 Week2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ 2.4 3.9 4.3 7.1 6.0 19.0 19.8 18.7 18.8 20.8 28.0 29.4 28.2 25.9 29.3 26.1 25.7 34.9 33.0 40.5 45.3 <LOQ <LOQ <LOQ <LOQ <LOD <LOD <LOD <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ CLOQ <LOQ <LOD <LOD cLOQ <LOQ 3.4 3.5 9.6 6.3 14.1 14.2 17.1 19.1 22.2 21.1 <LOD <LOD cLOD CLOD cL O D cLOQ cLOQ CLOD cLOQ CLOQ cLOQ CLOD CLOQ cLOQ LOD = limit o f detection (0.128 ng/kg) LOQ = limit of quantitation (2.0 pg/kg) Friday, O ctober 12, 2907 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 175 - p. 176 project no : 112E-ios Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTOH (pg/kg) in Soils Treated w ith D Sample Soil Type________ Interval_______ Aerobic Live Sterile Ultisol DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month IS Month 18 Month 24 <LOD <LOD CLOD CLOD cLOQ cLOQ CLOD CLOD CLOQ cL O Q cLOQ cLOQ CLOQ CLOQ cLOQ cLOQ CLOQ CLOD CLOQ cLOQ <LOQ <LOQ CLOD CLOD <LOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD cLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD CLOD Anaerobic Live Sterile cLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD cLOD cLOD CLOD CLOD cLOD CLOD <LOD CLOD cL O D CLOD cL O D CLOD cLOD CLOD cL O D cLOD cL O D CLOD LOD = limit o f detection (22.3 pg/kg) LOQ = limit of quantitation (100 pg/kg) M onday, O ctober IS , 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 176- p. 177 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 5Measured Concentrations of 8-2 FTOH g/kg) in Soils Treated w ith f Soil Type Mollisol Sample Interval DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month IS Month IS Month 24 Aerobic Live Sterile <LOD <LOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD <LOD CLOD CLOD CLOD CLOD CLOD <LOD CLOD CLOD CLOQ CLOD <LOD <LOD CLOD CLOD CLOD CLOD CLOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD LOD = limit of detection (22.3 jig/kg) LOQ = limit o f quantitation (100 ;ig/kg) Anaerobic Live Sterile CLOD CLOD cLOQ CLOQ CLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD cLOD CLOD cLOD CLOD cLOD CLOD CLOD cLOD CLOD CLOD M onday, O ctober IS , 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 177- p. 178 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTOH (fig/kg) in Soils Treated withQ Sample Aerobic Anaerobic Soil Type________ Interval___________ Live Sterile______ Live Sterile Alfisol DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 CLOD <LOD CLOD CLOD cLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD cLOD CLOD CLOD <LOD <LOD CLOD CLOD cLOQ CLOD cL O D cL O D cLOD CLOD cL O D CLOD CLOD cLOD cL O D CLOD CLOD CLOD CLOD CLOD CLOD cL O D <LOD cL O D CLOD CLOD CLOD cL O D CLOD cLOD CLOD CLOD CLOD cLOQ cLOD CLOD CLOD cL O D cLOD CLOD CLOD cLOD cLOD CLOD CLOD CLOD <LOD CLOD CLOD CLOD CLOD LOD = limit o f detection (22.3 |ig/kg) LOQ = limit o f quantitation (100 pg/kg) M onday, O ctober IS , 207 Company Sanitized. Does not contain TSCA CBl. W ildlife International, Ltd. - 178- p. 179 Project No.: 112E-108 Wildlife International, Ltd. Project Number 1 12E-108 Measured Concentrations of 8-2 FTOH (pg/kg) in Soils Treated with ^ ~1 Soil Type InceDtisol Sample Interval Day 0 Week 1 Week 2 Week 4 Month2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Aerobic Uve Sterile <LOD <LOD <L0D <LOD <LOD <LOD <L0Q <LOQ 174 125 148 138 <LOQ 140 100 <LOQ 131 165 173 121 <LOQ <LOQ <LOQ <LOQ <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOD <LOD <LOD <LOD <LOD <LOD <LOD LOD = limit o f detection (22.3 pg/kg) LOQ = limit of quantitation (100 pg/kg) Anaerobic Live Sterile <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOD <LOD <LOD <L0D <LOD <LOD <LOD <LOQ <LOD <LOD <LOD <LOD <LOD M onday, O ctober IS , 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 179- p. 180 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTOH Qtg/L) in Headspaces Gases from Chambers Treated with jf^ 1 Sample Aerobic Anaerobic Soil Type________ Interval____________Live Sterile______ Live Sterile Ultisol DayO Week 1 Week 2 Week 4 Month2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOQ = limit of quantitation (12.5 pg/L of headspace) <LOQ <LOQ <LOQ <LOQ <L0Q <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ . M onday, O ctober 15, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 180- p. 181 Project No.: 112E-108 Wildlife InternationalLtd. Project Number 112E-108 Measured Concentrations of 8-2 FTOH (fig/L) in Headspaces Gases from Chambers Treated w ith J Soil Type Sample Interval Aerobic Live Sterile Mollisol . Day 0 Week 1 Week 2 Week 4 Month. 2 Month 4 Month. 6 Mbnth9 Month 12 Month 15 Month IS Month. 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOQ = limit of quantitation (12.5 pg/L of headspace) Anaerobic Live Sterile <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ M onday, O ctober 15, 2907 Company Sanitized. Does not contain TSCA CBI. W^ildlife International, Ltd. -181 - p. 182 project no.: 112E-108 Wildlife InternationalLtd.________________ Project Number 112E-108 Measured Concentrations of 8-2 FTOH (pg/L) in Headspaces Gases from Chambers Treated with Q Sample Soil Type________ Interval_______ Aerobic Live Sterile Alfisol DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOQ = limit of quantitation (12.5 |ig/L of headspace) Anaerobic Sterile <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ M onday, O ctober IS , 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 182- p. 183 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTOH (fig/L) in Headspaces Gases from Chambers Treated with(T Soil Type Sample Interval Aerobic Live Sterile InceDtisol DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOQ = limit ofquantitation (12.5 pg/L ofheadspace) Anaerobic Live Sterile <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ M onday, O ctober IS , 2097 Company Sanitized. Does not contain TSCA CBI. ,W ildlife International Ltd. - 183 - p. 184 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 7-2 s FTOH (pg/kg) in Soils Treated with{^ Sample Aerobic Anaerobic Soil Type________ Interval___________ Live Sterile______ Live Sterile Ultisol Day 0. Month 2 Month 6 Mouth9 Month 12 Month 15 Month IS Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ 133.0 166.1 <LOQ <LOQ <LOQ <LOQ 115.6 <LOQ <LOQ <LOQ <LOQ LOQ = limit of quantitation (100 pg/kg) Thursday, N ovem ber Ob, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 184- p. 185 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 7-2 s FTOH (p.g/kg) in Soils Treated withC ^ Sample Aerobic Anaerobic Soil Type________ Interval___________ Live Sterile______ Live Sterile Mollisol Day 0 Month 2 Month 6 <LOQ <LOQ <LOQ <LOQ a o' oo V1 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <L0Q <LOQ <L0Q <LOQ LOQ = limit of quantitation (100 pg/kg) Thursday, Novem ber OS, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 185 - p. 186 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 7-2 s FTOHQig/kg) in Soils Treated with. ' Sample Soil Type________ Interval Alfisol Day 0 Month 2 Month 6 Month9 Month 12 Month 15 Month 18 Month 24 Aerobic Live Sterile <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ Anaerobic Live Sterile LOQ = limit of quantitation (100 pg/kg) Thursday, N ovem ber 08, 2007 Company Sanitized. Does not contain TSCA CBI. Wildlife International, Ltd. - 186- p. 187 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 7-2 s FTOH (pg/kg) in Soils Treated w ith J Sample Aerobic Anaerobic Soil Type_______ Interval___________ Live Sterile______ Live Sterile Inceutisol Day 0 Month 2 Month 6 Month 9 Month 12 Month IS Month IS Month 24 <LOQ <LOQ <LOQ <LOQ 278.3 278.3 192.8 464.2 193.0 118.9 173.2 182.2 <LOQ <LOQ <LOQ <LOQ LOQ = limit of quantitation (100 pg/kg) Thursday, N ovem ber 08,2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 187- p. 188 projectn o ; i h e ios Wildlife International, Ltd._________________ Project Number 1 1 2 E- 1 0 8 Measured Concentrations of 7-3 A dd (fig/kg) in Soils Treated with ~J Sample Soil Type________ Interval Ultisol Day 0 Month2 Month 6 Month9 Month 12 Month 15 Month 18 Month24 Aerobic Live Sterile <LOQ <LOQ 6.6 9.1 16.3 21.4 31.3 28.7 41.7 33.4 34.1 40.1 27.8 17.0 54.3 56.2 Anaerobic Live__Sterile_ LOQ - limit of quantitation (2.0 ng/kg) W ednesday, M arch 1 2 ,200S Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 188 - p. 189 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 7-3 Acid Qig/kg) in Soils Treated with f 'l Soil Type Mollisol Sample Interval Day 0 Month 2 Month 6 Month 9 Month 12 Month 15 Month 18 Month24 Aerobic Live Sterile <LOQ <LOQ <LOQ <LOQ 2.4 2.7 2.7 2.9 5.0 4.8 6.6 9.0 3.5 3.4 8.9 6.6 LOQ = limit o f quantitation (2.0 ng/kg) Anaerobic Live Sterile W ednesday, M arch 12,2008 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 189- p. 190 Project no.: 112E-108 Wildlife International, Ltd._________________ Project Number B1 1 2 -1 0 8 Measured Concentrations of 7-3 Acid (p.g/kg) in Soils Treated w ith Soil Type Alfisol Sample Internai Day 0 Monili 2 Month6 Mondi 9 Mondi 12 Mondi 15 Month 18 Mondi 24 Aerobic Live Sterile <LOQ <LOQ <LOQ <LOQ 3.2 2.5 3.2 2.5 4.9 6.1 7.6 8.9 8.1 6.4 6.6 7.3 Anaerobic Live Sterile LOQ = limit of quantitation (2.0 |ig/kg) W ednesday, M arch 12,2008 Company Sanitized. Does not contain TSCA CBI. Wildlife International, Ltd. - 190- p. 191 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 7-3 Acid Qig/kg) in Soils Treated with(_ ^ Soil Type Inceotisol ' Sample Interval Day 0 Month2 Month6 Month9 Month 12 Month 15 Month 18 Month24 Aerobic . Anaerobic Live Sterile______ Live Sterile <LOQ <LOQ 16 .7 9.6 67.7 81.6 128.3 153-2 277.0 246.2 260.7 289.7 282.3 2122 3 5 5 .2 321.9 LOQ = limit of quantitation (2.0 pg/kg) W ednesday, M arch 1 2 ,20BS Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 191 - p. 192 Project No.: 112E-108 Wildlife International, Ltd,______________Project Numbers 112E-108,109,110 Measured Concentrations of PFOA (pg/kg) in Untreated and Fortified Soils Sample Untreated Controls Fortified Recoveries Soil Type________ Interval______ Aerobic Anaerobic_____ Aerobic______ Anaerobic Ultisol DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 9.5 7.8 8.6 9.1 9.2 9.2 10.4 10.3 12.0 11.4 10.6 10.4 9.2 10.0 7.4 6.8 95% 7854 86% 91% 92% 92% 104% 103% 120% 114% 106% 104% 92% 100% 74% 68% 9.5 95% 9.2 92% 10.5 105% 11.3 113% 9.2 92% 9.8 98% 9.3 93% 9.0 90% 11.4 114% 10.8 108% 11.4 114% 11.3 113% 11.2 112% 11.5 115% LOD = limit of detection (0.206 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) Friday, O ctober 12, 2007 Page 1 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 192 - p. 193 Project No.: 112E-108 Wildlife International, Ltd. P ro jectN um bersll2E -108,109,I10 Measured Concentrations of PFOA (pg/kg) in Untreated and Fortified Soils Sam ple U ntreated C ontrols F ortified R ecoveries S o il Type______ In terval_____ A erobic A naerobic____ A erobic____ A naerobic Mollisol Day 0 Week 1 Week 2 Week4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOQ <LOD <LOD <LOQ <LOD <LOQ <LOQ <LOQ <LOD <LOD <LOD <LOD <LOD <LOQ LOD = limit of detection (0.206 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) <LOD <LOD <LOD <LOQ <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD 8.9 9.3 9.7 10.0 8.8 9.4 9.1 9.0 10.7 11.2 13.2 12.1 13.1 12.0 11.4 11.6 9.2 10.4 89% 93% 97% 100% 88% 94% 91% 90% 107% 112% 132% 121% 131% 120% 114% 116% 92% 104% 9.3 10.1 8.5 9.6 8.5 8.9 9.5 9.9 12.2 10.9 14.0 13.9 14.5 14.3 93% 101% 83% 96% 85% 89% 95% 99% 122% 109% 140% 139% 143% 143% Friday, O ctober 12, 2007 Page 2 o f4 - Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 193 - p. 194 project n o .: i h e - ios Wildlife International, Ltd.______________ Project Numbers 112E-108,109,110 Measured Concentrations of PFOA Qig/kg) in Untreated and Fortified Soils S oil Type Sam ple In terval U ntreated C ontrols A erobic A naerobic A lfisol DayO Weds; 1 Week 2 Week 4 Month2 Month 4 Month 6 Month 9 Month 12 Month 15 Month IS Month 24 <LOD <LOD <LOD CLOD cL O D CLOD CLOD CLOD cLOD CLOD cL O Q CLOQ CLOD CLOD cL O D CLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD cLOD CLOD CLOD CLOD cL O D cL O D cLOD cLOD CLOD CLOD CLOD CLOD LOD = limit of detection (0.206 pg/kg) LOQ= limit of quantitation (2.0 pg/kg) F o rtified R ecoveries A erobic A naerobic 9.2 8.3 8.9 10.0 9.9 9.4 10.0 10.1 11.0 10.7 10.8 11.5 11.0 11.1 11.5 12.5 9.2 9.3 92% 83% 89% 100% 99% 94% 100% 101% 110% 107% 108% 115% 110% 111% 115% 125% 92% 93% 9.2 8.2 8.7 9.3 9.6 10.0 10.6 10.4 10.4 10.7 11.1 10.9 10.5 11.2 92% 82% 87% 93% 96% 100% 106% 104% 104% 107% 111% 109% 105% 112% F riday, October 12, 2007 Page 3 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 194- p. 195 Project No.: 112E-108 Wildlife International, Ltd. ProjectNumbersll2E-108,109,110 Measured Concentrations of PFOA (fig/kg) in Untreated and Fortified Soils S o il Type Sam ple In terval U ntreated C ontrols A erobic A naerobic Inceotisol Day 0 Week 1 Week2 Week4 Month 2 Month 4 Month 6 Month 9 Month 12 Month L5 Month IS Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOD = limit of detection (0.206 fj.g/kg) LOQ = limit of quantitation (2.0 jig/kg) <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ F ortified R ecoveries A erobic A naerobic 10.4 10.5 12.9 10.1 10.6 10.9 12.4 11.2 11.3 11.7 13.4 10.8 12.1 10.6 14.5 12.4 9.6 9.6 104% 105% 129% 101% 106% 109% 124% 112% 113% 117% 134% 10% 121% 106% 145% 124% 96% 96% 9.7 9.4 10.9 9.8 10.8 10.5 10.7 10.9 11.9 11.1 10.6 11.5 11.3 11.6 97% 94% 109% 98% 108% 105% 107% 109% 119% 111% 106% 115% 113% 116% Friday, O ctober 1 2 ,2 0 0 7 Page 4 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 195 - p. 196 project no .: 112E-108 Wildlife InternationalLtd._____________ Project Numbers 1 1 2 B-1 0 8 ,109,110 Measured Concentrations of 8-2 FTUA (ng/kg) in Untreated and Fortified Soils Sam ple U ntreated C ontrols F ortified R ecoveries S oil Type_______In terval_____ A erobic A naerobic____ A erobic_____A naerobic Ultisol Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month IS Month 24 <LOQ <LOD <LOD CLOD cL O D CLOD cLOD cLOD CLOD CLOD cLOD CLOD cLOD CLOD cLOD CLOD CLOD cLOD cLOD CLOD CLOD cLOD CLOD cLOD CLOD cLOD cL O D cL O D cL O D cLOD CLOD CLOD CLOD CLOD CLOD 7.2 72% 6.5 65% 7.7 77% 7.9 79% 6.9 69% 6.9 69% 7.2 72% 7.2 72% 8.9 89% 8.0 80% 6.5 65% 7.3 73% 2.9 29% 5.4 54% 5.1 51% 4.0 40% 8.0 80% 7.4 74% 7.7 77% 8.7 87% 8.4 84% 8.2 82% 8.2 82% 7.9 79% 9.3 93% 7.6 76% 8.2 82% 8 .0 80% 6.5 65% 7.0 70% LOD = limit of detection (0.119 ng/kg) LOQ = limit of quantitation (2.0 gg/kg) Friday, O ctober 12, 2007 Page J o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 196- p. 197 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 112E-108,109,11 0 Measured Concentrations of 8-2 FTUA (jig/kg) in Untreated and Fortified Soils Sam ple U ntreated C ontrols F ortified R ecoveries S o il Type______ In terval_____ A erobic A naerobic____ A erobic_____Anaerobic M ollisol , Day 0 W eek 1 W eek 2 W eek 4 M onth 2 M onth 4 M onth 6 M onth 9 M onth 12 M onth 15 M o n th 18 M onth 24 <LOD <LOD ' <LOD CLOD CLOD CLOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOQ CLOD CLOD CLOD CLOD CLOD <LOD CLOD CLOD CLOD CLOD <LOD 9.2 9.0 8.1 8.5 9.1 9.5 9.0 9.1 8.8 8.7 10.0 9.4 10.2 8.2 7.8 9.0 5.9 6.3 92% 90% 81% 85% 91% 95% 90% 91% 88% 87% 100% 94% 102% 82% 78% 90% 59% 63% 7.3 8.8 7.7 8.7 7.7 9.8 8.0 8.0 9.7 7.8 9.9 10.7 10.0 8.5 73% 88% 77% 87% 77% 98% 80% 80% 97% 78% 99% 107% 100% 85% LOD = limit of detection (0.119 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) Friday, O ctober 12, 2007 Page 2 o f4 Company Sanitized. Does not contain TSCA CBI. ,W ildlife International Ltd. - 197- p. 198 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 112E-108,109,110 Measured Concentrations of 8-2 FTUA ((ig/kg) in Untreated and Fortified Soils Sam ple U ntreated C ontrols F ortified R ecoveries S o il Type_______In terval_____ A erobic Anaerobic____ A erobic_____A naerobic Alfisol DayO Week 1 Week 2 Week 4 Month. 2 Month 4- Month 6 Month 9 Month 12 Month IS Month IS Month 24 <L0D <LOD <L0D CLOD cL O D CLOD CLOD CLOD cLOD cLOD CLOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD cLOD <LOD cLOD CLOD cLOD cLOD CLOD CLOD cLOD CLOD CLOD cLOD CLOD CLOD cLOD CLOD 8.4 84% 7.7 77% 8.6 86% 9.8 98% 10.5 105% 7.6 76% 7.5 75% 9.2 92% 9.6 96% 9.1 91% 6.6 66% 9.0 90% 8.4 84% 9.0 90% 8.0 80% 11.1 111% 6.2 62% 6.7 67% 8.9 7.5 9.3 9.5 9.2 8.9 8.6 9.4 10.9 10.8 8.1 8.3 10.3 8.3 89% 75% 93% 95% 92% 89% 86% 94% 109% 108% 81% 83% 103% 83% LOD = limit of detection (0.119 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) ,Friday O ctober 12, 2007 Page 3 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 198- p. 199 Project No.: 112E-108 Wildttfe International, Ltd. Project Numbers 1 1 2 E -] 0 8 ,1 0 9 ,1 1 0 Measured Concentrations of 8-2 FTUA (ng/kg) in Untreated and Fortified Soils Sam ple U ntreated C ontrols F ortified R ecoveries S o il Type______ Interval_____ A erobic A naerobic____ A erobic____ Anaerobic InceD tisol DayO Week 1 Week2 Week4 Month 2 Mdnth4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 2+ <LOD CLOD <LOD CLOD CLOD CLOD CLOD CLOD cLOD <LOD CLOD <LOD cLOD CLOD CLOD CLOD cLOD CLOD <L0D <LOD CLOD CLOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD cLOD CLOD 11.0 9.6 10.8 8.3 8.8 9.7 9.4 7.9 8.0 8.9 10.1 8.1 7.0 6.8 7.4 6.4 5.3 5.2 110% 96% 108% 83% 88% 97% 94% 79% 80% 89% 101% 81% 70% 68% 74% 64% 53% 52% 7 .9 79% 8.1 81% 8.3 83% 7.5 75% 8.5 85% 7.8 78% 7.7 77% 8 .2 82% 7.6 76% 8.8 88% 6.6 66% 7.0 70% 6.1 61% 7.1 71% LO D = lim it o f detection (0.119 pg/kg) L O Q = lim it o f quantitation (2.0 pg/kg) Friday, O ctober 12, 2007 Page 4 o f4 Company Sanitized. Does not contain TSCA CBi. W ildlife International, Ltd. -199- p. 200 Projectn 0.: 112E-108 Wildlife International, Ltd._____________ Project Numbers 1 1 2 E-1 0 8 ,109,110 Measured Concentrations of 8-2 FTA (jag/kg) in Untreated and Fortified Soils S o il Type Ultisol Sam ple In terval Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 U ntreated C ontrols A erobic A naerobic <LOD <LOD CLOD CLOD CLOD CLOD cLOD CLOD cLOD CLOD CLOD CLOD CLOD <LOD cL O D CLOD cL O Q cL O Q CLOD <LOD CLOD cL O D cLOD CLOD cL O D cL O D cL O D CLOD CLOD CLOD CLOD CLOD CLOD cLOD c LOD F ortified R ecoveries A erobic A naerobic 6.1 61% 5.8 58% 6.2 62% 6.9 69% 5.4 54% 5.5 55% 5.4 54% 5.3 53% 3.3 33% 2.4 24% 3.4 34% 3.7 37% (1.4 ) (1.4) 4.1 41% (1.7) 6.7 67% 6.6 W>% 7.0 70% 6.9 69% 6.1 61% 6.5 65% 5.3 53% 6.3 63% 7.2 72% 5.1 51% 4.8 48% 4.6 46% 3.5 35% 3.2 32% L O D = lim it o f detection (0.503 pg/kg) L O Q = lim it o f quantitation (2.0 pg/kg) V a lu e s in parentheses a r e < L O Q a n d > = L O D Friday, O ctober 12, 2007 Page 1 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 200- p. 201 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 112E-108.,109>110 Measured Concentrations of 8-2 FTA (pg/kg) in Untreated and Fortified Soils S oil Type Mollisol Sam ple In terval DayO Week 1 Week 2 Week 4 Month 2 Month. 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 U ntreated C ontrols A erobic A naerobic F ortified R ecoveries A erobic A naerobic <LOD <LOD 2.7 <LOD <LOD <LOD <LOQ <LOD <L0D <LOD <LOD <L0D <L0D <LOD <LOD <LOD <LOD <LOQ <L0D <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD 8.7 9.0 8.4 9.0 9.0 8.8 8.3 8.1 7.8 - 7.9 8.4 6.9 6.4 6 .2 5.0 6 .2 2.3 (1.71 87% 90% 84% 90% 90% 88% 83% 81% 78% 79% 84% 69% 64% 62% 50% 62% 23% 7.0 70% 8.7 87% 7.1 71% 7.6 76% 6.4 64% 8.3 83% 6.3 63% 7.0 70% 8.0 80% 7.1 71% 5.8 58% 6.5 65% 5.7 57% 5.2 52% LOD = limit of detection (0.503 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) Values in parentheses are <LOQ and >=LOD Friday, O ctober 12, 2007 Page 2 o f4 Company Sanitized. Does not contain TSCA CBI. .W ildlife International, Ltd -201 - p. 202 Project No.: 112E-108 Wildlife International, Ltd.______________Project Numbers 11ZE-108,109,no Measured Concentrations of 8-2 FTA (pg/kg) in Untreated and Fortified Soils Sam ple U ntreated C ontrols F o rtified R ecoveries S o il Type_______In terval_____ A erobic A naerobic____ A erobic_____A naerobic Alfisol DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOD <LOD <LOD CLOD CLOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD <LOD <LOD <LOD cLOD cLOD CLOD cLOQ cLOD CLOD cL O D CLOD cLOD CLOD cLOD cLOD cLOD CLOD CLOD cLOD CLOQ CLOQ 7.8 7.9 8.4 10.6 8.7 6.8 8.4 7.5 7.0 4.2 6.7 6.0 6.6 5.1 7.7 4.0 3.7 oo 78% 79% 78% 84% 106% 87% 68% 84% 75% 70% 42% 67% 60% 66% 51% 77% 40% 37% 8.8 88% 6.7 67% 8.5 85% 8.4 84% 8.4 84% 8.1 81% 7.7 77% 8.3 83% 8.8 88% 8.3 83% 6.7 67% 6.6 66% 7.3 73% 7.0 70% LOD = limit of detection (0.503 pg/kg) L O Q = lim it o f quantitation (2.0 pg/kg) V alues in parentheses are <L O Q and >=LO D Friday, O ctober 12, 2007 Page 3 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 202- p. 203 Project No.: 112E-108 Wildlife International, Ltd. P roject N um bers 112E -108,109,110 Measured Concentrations of 8-2 FTA (fig/kg) in Untreated and Fortified Soils Sample Untreated Controls Fortified Recoveries Soil Type________ Interval______ Aerobic Anaerobic_____ Aerobic______ Anaerobic InceDtisol DayO Week 1 Week2 - Week 4 Month2 ' Month 4 Month6 Month 9 Month 12 Month 15 Month 18 Month 24 CLOD CLOD <LOD <LOD CLOD CLOD CLOQ CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOQ CLOQ CLOQ CLOD CLOD CLOD cLOQ CLOD CLOD CLOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD 10.7 9.6 9.8 7.6 7.0 8.4 7.1 6.3 5.5 5.8 5.3 4.5 4.3 3.7 3.4 3.4 2.1 (1.81 107% 96% 98% 76% 70% 84% 71% 3% 55% 58% 53% 45% 43% 37% 34% 34% 21% 7.8 78% 7.2 72% 7.0 70% 6.7 7% 7.2 72% 7.6 76% 5.9 59% 6.6 66% 4.8 48% 6.3 63% 3.6 36% 3.4 34% 2.6 26% 3.5 35% LOD = limit ofdetection (0.503 pg/kg) LOQ = limit ofquantitation (2.0 jig/kg) Values in parentheses are <LOQ and >=LOD Friday, O ctober 12, 2007 Page 4 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -203 - p. 204 Project No.: 112E-108 Wildlife International, Ltd. P roject N um bers 112E -108, 109,110 Measured Concentrations of PFNA (fig/kg) in Untreated and Fortified Soils Soil Type Ultisol Sample Untreated Controls Fortified Recoveries Interval______ Aerobic Anaerobic_____ Aerobic Anaerobic Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 9.4 94% 7.8 78% 9.7 97% 9.8 98% 9.5 95% 9.8 98% 10.4 104% 10.1 101% 11.4 114% 11.4 114% 10.3 103% 10.6 106% 7.0 70 % 10.3 103% 7.9 79% 6.7 67 % 10.0 100% 9.9 9 9 % 9.9 99% 10.7 107% .9.7 97% 10.3 103% 10.3 103% 9.6 96% 11.2 112% 11.0 110% 11.6 116% 11.7 117% 10.8 108% 11.6 116% LOD --limit of detection (0.124 jig/kg) LOQ = limit of quantitation (2.0 jig/kg) F riday, O ctober 12, 2607 Page 1 o f4 Company Sanitized. Does not contain TSCA CB1. W ildlife International, Ltd. -204- p. 205 Project No.: 112E-108 Wildlife International, Ltd. _____________ P ro je c t N u m b e rs 112E -108,109,110 Measured Concentrations of PFNA (pg/kg) in Untreated and Fortified Soils Soil Type Mollisol Sample Interval DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Untreated Controls Aerobic Anaerobic <LOD <LOD <LOD CLOD CLOD CLOD CLOD cLOQ <LOD CLOD CLOD CLOD CLOD CLOD cLOQ CLOQ CLOD CLOD CLOD CLOD CLOD CLOD CLOD cL O Q CLOD CLOD CLOD cLOD cLOD CLOD CLOD cLOD CLOD CLOD cLOD LOD = limit of detection (0.124 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) Fortified Recoveries Aerobic Anaerobic 9.4 9.6 9.7 9.7 9.5 9.9 10.2 8.6 10.7 10.6 12.2 11.9 12.0 11.7 10.0 11.2 8.1 8.3 94% 96% 97% 97% 95% 99% 102% 86% 107% 106% 122% 119% 120% 117% 100% 112% 81% 83% 9.6 10.1 8.9 9.8 9.6 9.9 9.3 9.8 10.7 10.1 11.6 12.8 12.2 11.9 96% 101% 89% 98% 96% 99% 93% 98% 107% 101% 116% 128% 122% 119% Friday, O ctober 12, 2007 Page 2 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -205 - p. 206 Project No.: 112E-108 Wildlife International, Ltd. P roject N um bers 1 12E -108,109,110 Measured Concentrations of PFNA (pg/kg) in Untreated and Fortified Soils Sample Untreated Controls Fortified Recoveries Soil Type________ Interval______ Aerobic Anaerobic_____ Aerobic______ Anaerobic Alfisol DayO Week 1 Week 2 Week 4 Month. 2 Month 4 Month 6 Month 9 Month 12 Month IS Month 18 Month 24 <LOD <LOD <LOD <LOD <LOD CLOD cL O D CLOD cLOD CLOD CLOD CLOD CLOQ cL O Q CLOQ CLOQ cLOQ cLOQ CLOD CLOD CLOD cLOD CLOD cLOD CLOD cL O D CLOD CLOD cLOD cLOD CLOD CLOD CLOD CLOQ cL O Q 9.8 9.3 9.4 11.2 10.3 9.1 10.3 10.7 11.3 11.0 10,0 11.4 10.8 11.4 11.3 12.3 8.7 8.6 98% 93% 94% 112% 103% 91% 103% 107% 113% 110% 100% 114% 108% 114% 113% 123% 87% 86% 9.7 8.1 9.4 10.1 9.8 10.1 10.3 10.0 11.0 11.0 10.7 10.7 11.5 10.2 97% 81% 94% 101% 98% 101% 103% 100% 110% 110% 107% 107% 115% 102% LOD = limit of detection (0.124 ng/kg) LOQ = limit of quantitation (2.0 ig/kg) Friday, O ctober 12, 2007 Page 3 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 206- p. 207 project n 0.: 112E-108 Wildlife International, Ltd. P ro ject N um bers 112E -108,109,110 Measured Concentrations of PFNA (ug/kg) in Untreated and Fortified Soils Soil Type Incentisol Sample Interval DayO Weds 1 Weds 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Untreated Controls Aerobic Anaerobic <LOQ <LOQ <LOD <LOD <LOQ <LOQ <LOQ <LOD <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOQ <LOD <LOD CLOD CLOD CLOD cLOQ cLOQ cLOQ cLOQ cLOQ <LOD cLOQ cLOQ cLOQ CLOQ Fortified Recoveries Aerobic Anaerobic 12.4 11.6 13.0 10.6 10.7 10.7 12.5 10.7 11.2 11.9 14.0 10.5 10.4 10.0 13.0 10.9 8.9 8.8 124% iis% 130% 106% 107% 107% 125% 107% 112% 119% 140% 105% 104% 100% 130% 109% 89% 88% 10.2 10.0 10.8 9.8 10.3 10.2 10.1 10.7 11.1 11.1 11.0 10.8 10.1 10.8 102% 100% 108% 98% 103% 102% 101% 107% 111% 111% 110% 108% 101% 108% LOD = limit ofdetection (0.124 ug/kg) LOQ = limit of quantitation (2.0 pg/kg) Friday, O ctober 12, 2007 Page 4 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -207- p. 208 Project No.: 112E-108 WildUfe International, Ltd.__________________ P ro je c t N u m b ers 1 1 2 E -1 0 8 ,1 0 9 ,1 1 0 Measured Concentrations of PFDA (pg/kg) in Untreated and Fortified Soils Soil Type Ultisol Sample Interval DayO Week 1 Week 2 Week4 Month 2 Month 4 Month 6 Month 9 Month 12 Month IS Month IS Month 24 Untreated Controls Fortified Recoveries Aerobic Anaerobic_____ Aerobic______ Anaerobic <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 9.3 93% 7.4 74% 8.9 89% 8.6 86% 8.8 88% 8.9 89% 9.4 94% 9.3 93% 10.9 109% 10.9 109% 9.6 96% 10.0 100% 5.2 52% 9.5 95% 8.4 84% 7.0 70% 9.2 9.1 9.0 9.7 9.4 9.2 9.3 8.0 10.4 10.2 11.0 10.9 9.6 10.4 92% 91% 90% 97% 94% 92% 93% 80% 104% 102% 110% 109% 96% 104% LOD = limit,ofdetection (0.114 pg/kg) LOQ = limit ofquantitation (2.0 pg/kg) F riday, O ctober 12, 2007 Page 1 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -208- p. 209 Project No.: 112E-108 Wildlife International, Ltd. P roject N um bers ]12E-108,109,110 Measured Concentrations of PFDA (pg/kg) in Untreated and Fortified Soils Soil Type Mollisol Sample Interval DayO Week 1 Week 2 Week 4 Month.2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Untreated Controls Aerobic Anaerobic <LOQ <LOQ <LOD <LOD <LOD <LOD <LOQ <LOQ <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOQ <LOD <LOD <LOD <LOD <LOQ <LOQ <LOQ <LOQ <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD LOD = limit ofdetection (0.114 |ig/kg) LOQ = limit ofquantitation(2.0 jig/kg) Fortified Recoveries Aerobic Anaerobic 10.0 10.0 9.8 10.4 9.7 10.1 9.8 8.1 9.9 9.7 11.7 10.9 12.1 11.2 9.2 10.2 7.6 8.0 100% 100% 98% 104% 97% 101% 98% 81% 99% 97% 117% 109% 121% 112% 92% 102% 76% 80% 9.2 9.9 8.2 9.5 9.2 9.3 9.0 9.0 10.4 9.2 11.4 12.1 11.2 10.9 92% 99% 82% 95% 92% 93% 90% 90% 104% 92% 114% 121% 112% 109% Friday, O ctober 12, 2007 Page 2 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -209- p. 210 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers ii2 E -io 8 ,io 9 ,n o Measured Concentrations of PFDA (pg/kg) in Untreated and Fortified Soils Alfisol Sample Interval Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month IS Month 18 Month 24 Untreated Controls F ortified Recoveries Aerobic Anaerobic_____ Aerobic______ Anaerobic cLOD <LOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD <LOD <LOD CLOD CLOD CLOD CLOD CLOQ CLOD <LOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD cLOD CLOD cLOD CLOD cLOD CLOD CLOD CLOD CLOQ 9.3 9.3 9.4 11.0 10.1 8.6 9.0 10.3 11.9 11.2 9.3 10.9 10.7 11.2 10.9 13.3 9.2 9.3 93% 93% 94% 110* 101% 86% 90% 105% 119% 112% 93% 109% 107% 112% 109% 133% 92% 93% 9.2 7.4 8.7 9.3 9.0 9.5 9.7 9.6 11.3 11.4 9.0 9.6 . 11.6 8 .6 92% 74% 57% 93% 90% 95% 97% 96% 113% 114% 90% 96% 116% 86% LOD = limit of detection (0.114 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) F riday, O ctober 12, 2007 Page 3 o f4 Company Sanitized. Does not contain TSCA CBI. Wildlife InternationalLtd. - 210- p. 211 Project No.: 112E-108 Wildlife International, Ltd. P roject N um bers 112E -108,109,110 Measured Concentrations of PFDA (pg/kg) in Untreated and Fortified Soils Soil Type InceDtisol Sample Interval Day 0 Week 1 Week2 Week4 Month 2 Month4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Untreated Controls Aerobic Anaerobic <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <L0Q <LOQ LOD = limit of detection (0.114 (ig/kg) LOQ = limit of quantitation (2.0 pg/kg) Fortified Recoveries Aerobic Anaerobic 13.9 12.4 14.6 11.6 11.3 11.6 12.1 11.5 12.0 13.3 14.1 10.8 10.7 9.2 12.8 10.9 9.5 9.2 139% 124% 146% 116% 113% 116% 121% 113% 120% 133% 141% 108% 107% 92% 128% 109% 95% 92% 9.9 9.7 10.7 9.6 10.8 10.5 10.1 10.7 11.8 12.2 10.8 11.6 9.6 10.6 99% 97% 107% 96% 108% 103% 101% 107% 118% 122% 108% 116% 96% 106% F riday. O ctober 12, 2007 Page 4 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -211 - p. 212 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 112E-108,109,110 Measured Concentrations of PFUA (pg/kg) in Untreated and Fortified Soils Sample Untreated Controls Fortified Recoveries Soil Type________ Interval_______Aerobic Anaerobic_____ Aerobic______ Anaerobic Ultisol DayO Weekl Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month IS Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 8.5 6.9 8.2 8.2 7.6 7.8 8.6 7.4 10.2 10.1 9.2 9.3 4.1 8.4 7.2 6.2 85% 69% 82% 82% 76% 78% 86% 74% 102% 101% 92% 93% 41% 84% 72% 62% 8.5 85% 8.8 88% 8.5 85% 8.4 84% 8.8 88% 8.6 86% 9.1 91% 7.0 70% 9.8 98% 9.5 95% 9.4 94% 9.5 95% 8.8 88% 9.9 99% LOD --limit of detection (0.128 pg/kg) LOQ = limit of quantitation (2.0 gg/kg) Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -212 - p. 213 Project No.: 112E-108 Wildlife International, Ltd. P ro ject N um bers 112E -108,109,110 Measured Concentrations of PFUA (fig/kg) in Untreated and Fortified Soils Soil Type Mollisol Sample Interval DayO Week 1 Week! Week 4 Month 2 Month4 Month6 Month 9 Monti 12 Month 15 Month 18 Month 24 Untreated Controls Aerobic Anaerobic <LOQ <LOQ <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOQ <LOQ <LOQ <LOD <LOD <LOD <LOD <LOD <LOQ <LOQ <LOQ <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD LOD = limit of detection (0.128 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) Fortified Recoveries Aerobic Anaerobic 9.5 9.6 8.7 9.3 9.0 9.2 8.7 6.9 8.4 8.4 10.1 10.1 9.5 8.7 7.4 8.8 6.1 6.3 95% 96% 87% 93% 90% 92% 87% 69% 84% 84% 101% 101% 95% 87% 74% 88% 61% 63% 8.2 82% 8.6 86% 6.7 67% 7.6 76% 6.3 63% 7.1 71% 6.3 63% 8.0 80% 8.5 85% 7.5 75% 9.6 96% 9.4 94% 9.8 98% 7.9 79% Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -213 - p. 214 Project No.: 112E-108 Wildlife International, Ltd. P roject N um bers 112E -108,109,110 Measured Concentrations of PFUA (pg/kg) in Untreated and Fortified Soils Soil Type Alfisol Sample Interval Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 Untreated Controls Aerobic Anaerobic <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD CLOD <LOD <LOD <LOD <LOD <LOQ <LOQ <LOD <LOD <LOD <L0D <LOD <LOD <LOD <LOD CLOD cLOD <LOD <LOD CLOD CLOD CLOD cLOQ CLOQ LOD = limit of detection (0.128 pg/kg) LOQ --limit of quantitation (2.0 pg/kg) F ortified Recoveries Aerobic Anaerobic 9.2 8.7 9.2 10.9 9.4 8.0 7.7 9.4 10.3 9.7 7.5 8.9 8.9 9.3 8.6 12.2 8.7 8.8 92% 87% 92% 109% 94% 80% 77% 94% 103% 97% 73% 89% 89% 93% 86% 122% 87% 88% OO oo 8.3 83% 6.1 61% 8.3 83% 8.6 86% 7.9 79% 7.9 79% 7.0 70% 7.6 76% 88% 9.9 99% 7.4 74% 7.2 72% 9.5 95% 6.7 67% Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -214- p. 215 Project No.: 112E-108 Wildlife International, Ltd. P ro ject N um bers 112E -108,109,110 Measured Concentrations of PFUA (pg/kg) in Untreated and Fortified Soils Soil Type In c e D tiso l Sample Interval Untreated Controls Aerobic Anaerobic Day 0 Week 1 Week 2 Week 4 Month2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 , <L0Q <LOQ <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOQ LOD = limit of detection (0.128 pg/kg) LOQ = limit of quantitation (2.0 pg/kg) Fortified Recoveries Aerobic Anaerobic 12.0 11.2 12.5 10.1 9.2 10.3 9.8 8.9 10.4 11.7 12.2 8.8 8.2 8.3 9.9 . 8.2 7.4 6.9 120% 112% 125% 101% 92% 103% 98% 89% 104% 117% 122% 88% 82% 83% 99% 82% 74% 69% 7.9 7.4 7.9 7.4 7.4 8.7 8.0 8.5 8.7 10.3 6.9 7.3 7.0 8.5 79% 74% 79% 74% 74% 87% 80% 85% 87% 103% 69% 73% 70% 85% Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -215- p. 216 Project No.: 112E-108 Wildlife International, Ltd. P ro je c t N u m b e rs 112E-108.109.no Measured Concentrations of 8-2 FTOH Qig/kg) in Untreated and Fortified Soils Sample Untreated Controls Soil Type________ Interval______ Aerobic Anaerobic Fortified Recoveries Aerobic______ Anaerobic Ultisol DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month IS Month 24 <LOD <LOD <LOD CLOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <L0D <LOD <LOD <LOD <LOD <LOD CLOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD 289 115% 283 113% 244 97% 247 99% 210 84% 208 83% 165 66% 147 59% 1 0 2 41% ( 98 1 39% ( 45 > 18% ( 53 ) 21% ( 41 ) 16% <LOD 0% <LOD 0% <LOD 0% cLOD 0% CLOD 0% 291 116% 288 115% 220 88% 258 103% 249 181 179 155 165 117 ( 87 ) ( 54 ) ( 68 ) 99% 72% 71% 62% 66% 47% 35% 22% 27% LOD = limit of detection (22.3 pg/kg) LOQ = limit of quantitation (100 pg/kg) Values in parentheses are <LOQ and >=LOD M onday, O ctober IS , 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 216- p. 217 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers E- ,1 1 2 1 0 8 1 0 9 ,1 1 0 Measured Concentrations of 8-2 FTOH (pg/kg) in Untreated and Fortified Soils Soil Type Moliisol Sample Interval DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month6 Month 9 Month 12 Month 15 Month 18 Month 24 Untreated Controls Aerobic Anaerobic Fortified Recoveries Aerobic Anaerobic <LOD <LOD CLOD <LOD <L0D <LOD <LOD <LOD <L0D <LOD <LOD <LOD <LOD <L0D <L0D <LOD <L0D CLOD <L0D <LOD CLOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD CLOD <LOD <LOD <LOD <LOD <LOD <LOD 299 120% 261 104% 213 85% 217 87% 194 78% 112 45% 119 48% ( 51 ) 21% ( 63 ) 25% <LOD 0% ( 32 ) 13% <LOD 0% -CLOD 0% <LOD 0% <LOD 0% -CLOD 0% CLOD 0% 266 106% 279 112% 244 98% 273 109% 257 . 103% 243 97% 191 77% 192 77% ( 99 ) 40% 162 65% ( 70 ) 28% ( 46 ) 18% ( 36 ) 14% <LOD 0% LOD - limit of detection (22.3 ng/kg) LOQ = limit of quantitation (100 pg/kg) Values in parentheses are <LOQ and >=LOD M onday, O ctober 15, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -217- p. 218 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 112E-108,109,110 Measured Concentrations of 8-2 FTOH (p.g/kg) in Untreated and Fortified Soils Sample Untreated Controls Fortified Recoveries Soil Type________ Interval______ Aerobic Anaerobic_____ Aerobic______ Anaerobic Alfisoi D ayO Week 1 Week 2 Week 4 Month 2 Month 4 Month Month 9 Month 12 Month 15 Month 18 Month 24 CLOD <LOD <LOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD cLOD CLOD 307 123% 245 98% 210 84% 143 57% 156 6 2 % 142 57% 117 47% 112 45% ( 75 ) 30% ( 79 ) 32% ( 54 ) 22% ( 51 ) 21% CLOD 0% ( 29 ) 12% CLOD 0% cLOD 0% cLOD 0% CLOD 0% 267 107% 254 102% 215 86% 203 81% 205 82% 161 64% 127 51% 143 57% ( 81 1 33% ( 62 1 25% ( 50 ) 20% ( 37 ) 15% cLOD 0% CLOD 0% LOD = limit of detection (22.3 pg/kg) LOQ = limit of quantitation (100 pg/kg) Values in parentheses are <LOQ and >=LOD M onday, October 15, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -218 - p. 219 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 112E-108,109,110 Measured Concentrations of 8-2 FTOH (jig/kg) in Untreated and Fortified Soils Soil Type Inceotisol . Sample Interval Day & Week 1 Week 2 Week 4 Month 2 Month 4 Month6 Month 9 Month 12 Month 15 Month 18 Month 24 Untreated Controls Aerobic Anaerobic F ortified Recoveries Aerobic Anaerobic CLOD <LOD <LOD <LOD <LOD <LOD CLOD CLOD CLOD CLOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD 285 11494 262 305% 267 10794 285 11494 245 9894 234 94% 218 87% 284 114% 201 81% 200 80% 157 6394 186 7496 ( 86 1 34% ( 85 ) 34% ( 55 ) 22% 115 46% CLOD 0% CLOD 0% 287 115% 285 114% 258 103% 260 104% 237 95% 235 94% 230 92% 219 87% 134 54% 165 66% 106 42% 106 42% ( 42 ) 17% ( 37 ) 15% LOD = limit ofdetection (22.3 pg/kg) LOQ = limit of quantitation (100 pg/kg) Values in parentheses are <LOQ and >=LOD M onday, O ctober 15, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -219- p. 220 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 112E-108.109.110 Measured Concentrations of 8-2 FTOH (pg/L) in Headspace Gases from Untreated and Fortified Soils Sample Untreated Controls Fortified Soils Soil Type________ Interval______ Aerobic Anaerobic_____ Aerobic Anaerobic Ultisol Day 0 Week 1 Week2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month IS Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <L0Q <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOQ ~ limit of quantitation (12.5 pg/L of headspace) <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ M onday, O ctober 15, 2007 Page 1 o f4 . Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 220- p. 221 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 112E-108,109,110 Measured Concentrations of 8-2 FTOH (fig/L) in Headspace Gases from Untreated and Fortified Soils Sample Untreated Controls Fortified Soils Soil Type________ Interval______ Aerobic Anaerobic_____ Aerobic Anaerobic M ollisol Day 0 Week 1 Week 2 Week4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOQ = limit of quantitation (12.5 pg/L ofheadspace) ,M onday O ctober IS , 2007 Page 2 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -221 - p. 222 Project No.: 112E-108 Wildlife International, Ltd. P roject N u m b ers 1 12E -108,109,110 Measured Concentrations of 8-2 FTOH Qig/L) in Headspace Gases from Untreated and Fortified Soils Sample Untreated Controls Fortified Soils Soil Type________ Interval______ Aerobic Anaerobic_____ Aerobic Anaerobic Alfisol . Day 0 Week 1 Week 2 Week4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOQ = limit of quantitation (12.5 fig/L of headspace) <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <L0Q <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ M onday, O ctober IS , 2007 Page 2 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -222- p. 223 Project No.: 112E-108 Wildlife International, Ltd. P ro ject N um bers 1 1 2 E -108,109,110 Measured Concentrations of 8-2 FTOH (pg/L) in Headspace Gases from Untreated and Fortified Soils Soil Type Sample Interval Untreated Controls Aerobic Anaerobic InceD tisol Day 0 Week 1 Week2 Week 4 Month 2 Month 4 Months Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOQ = limit of quantitation (12.5 pg/L ofheadspace) Fortified Soils Aerobic Anaerobic <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ ,M onday, O ctober 15 2007 Page 4 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. p. 224 Project No.: 112E-108 -223Appendix II Measured Concentration o f Selected Analytes (gmol/kg Soil Dry Weight) Company Sanitized. Does not contain TSCA CBI. ,W ildlife International Ltd. -224- p. 225 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFOA (ftmol/kg) in Soils Treated with(^ D Soil Type Sample Interval Aerobic Live Sterile Anaerobic Live Sterile Ultisol Day 0 Week 1 Week 2 Week4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month IS Month 24 <LOQ <LOQ 0.043 0.046 0.077 0.088 0.140 0.148 0.295 0.362 0.651 0.903 0.909 1.065 1.176 1.349 0.888 0.831 0.821 0.876 0.992 0.794 0.884 0.795 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 0.005 <LOQ 0.006 <LOQ 0.005 <LOQ 0.012 <LOQ 0.019 <LOQ <LOQ <LOQ <LOQ <LOQ 0.053 0.055 0.065 0.058 0.124 0.097 0.169 0.177 0.277 0.322 0.359 0.253 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 0.006 <LOQ 0.007 <LOQ LOD = limit o f detection (0.0005 pmol/kg) LOQ = limit of quantitation (0.0048 pmol/kg) Thursday, N ovem ber 08, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -225 - p. 226 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFOA (pmol/kg) in Soils Treated with S am ple A erobic Soil Type_______Interval_________ Live Sterile M ollisol Day 0 W eek 1 W eek 2 Week 4 M onth 2 M onth 4 M onth 6 M onth 9 M onth 12 M onth 15 M onth IS M onth 24 <LOQ <LOQ 0.037 0.036 0.043 0 .0 4 4 0.052 0.049 0.077 0.073 0.111 0.142 0.180 0 .1 8 0 0.223 0.167 0.251 0.227 0.238 0.599 0.307 0.287 0.554 0.501 LOD = limit of detection (0.0005 pmol/kg) LOQ = limit of quantitation (0.0048 pmol/kg) <LOQ <LOQ OLOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 0.007 <LOQ 0.008 0.006 0.008 0.008 0.007 0.008 Anaerobic Live Sterile <LOQ <LOQ 0.035 0 .0 3 6 0.045 0.044 0.049 0 .0 5 4 0 .1 0 3 0 .1 0 4 0 .1 8 9 0 .1 4 9 0 .2 8 4 0 .2 2 0 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 0.006 <LOQ 0 .0 0 9 0 .0 0 6 Thursday, N ovem ber Od, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 226- p. 227 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFOA (nmol/kg) in Soils Treated with C 3 Soil Type Sam ple Interval Aerobic Live Sterile Alfisol Day 0 Week 1 Week2 Week4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 O' O' OO 0.020 0.020 0.027 0.026 0.036 0.038 0.056 0.060 0.077 0.080 0.141 0.127 0.236 0.226 0.158 0.203 0.321 0.250 0.469 0.376 0.475 0.460 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 0.008 <LOQ <LOQ <LOQ LOD = limit o f detection (0.0005 pmol/kg) LOQ = limit o f quantitation (0.0048 pmol/kg) Anaerobic Live Sterile <LOQ <LOQ 0.023 0.026 0.034 0.037 0.048 0.048 0.043 0.075 0.217 0.188 0.240 0.202 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 0.005 <LOQ 0.005 <LOQ Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -227- p. 228 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFOA (jrmol/kg) in Soils Treated with Q. 3 Soil Type Sample Interval Aerobic U ve Sterile Incentisol Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 . Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ 0.046 0.050 0.069 0.070 0.135 0.132 0.295 0.236 0.460 0.457 0.639 0.605 0.697 0.820 0.888 0.845 0.972 0.930 1.020 1.078 1.282 1.338 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 0.005 <LOQ 0.007 <LOQ 0.011 <LOQ 0.013 0.007 0.015 0.007 0.010 0.006 LOD = limit o f detection (0.0005 nmol/kg) LOQ = limit o f quantitation (0.0048 pmol/kg) Anaerobic Live Sterile <LOQ <LOQ 0.050 0.043 0.064 0.065 0.182 0.116 0.333 0.349 0.687 0.731 0.790 0.838 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 0.012 <LOQ 0.018 <LOQ Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 228- p. 229 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTUA (innol/kg) in Soils Treated with . Soil Type Sample Interval Aerobic U ve Sterile Ultisol Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOD <LOQ <LOQ <LOQ 0.005 0.006 0.009 0.007 0.014 0.015 0.027 0.028 0.026 0.042 0.067 0.043 0.013 0.017 0.025 0.029 0.034 0.014 0.034 0.071 LOD --limit of detection (0.0003 (imol/kg) LOQ = limit of quantitation (0.0044 pmol/kg) <LOD <LOD <LOD <LOD <LOD <LOD CLOD <LOD <LOD <LOD <LOD <LOD CLOD cLOD CLOD CLOD CLOD CLOD Anaerobic Live Sterile CLOD CLOD cLOD cLOD cLOQ CLOQ cL O Q CLOQ cLOQ cLOQ CLOQ CLOQ cLOQ CLOQ CLOD CLOD CLOD clod CLOD CLOD cLOD CLOD CLOD cLOD cL O D CLOD CLOD CLOD / Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -229- p. 230 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTUA (junol/kg) in Soils Treated with j Soil Type Sam ple Interval Aerobic Live Sterile Moflisol - Day 0 Week 1 Week2 Week 4 Month. 2 Month.4 Month. 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOD <LOD cLOD cLOD cLOQ <LOQ cL O Q <LOQ cLOQ cLOQ <LOD <LOQ cLOQ cLOQ <LOQ cLOQ CLOD <LOD CLOQ <LOQ 0.007 CLOQ LOD = limit o f detection (0.0003 pmol/kg) LOQ = limit o f quantitation (0.0044 pmol/kg) cLOD cLOD cLOD CLOD cLOD <LOD cL O D cLOD cLOD CLOD <LOD CLOD cL O D CLOD CLOQ <LOQ cL O D CLOD Anaerobic Live Sterile cLOQ CLOQ cL O Q CLOQ cLOD CLOD cLOD CLOQ cL O Q cLOQ CLOQ cLOQ cLOQ CLOQ cLOD CLOD cL O Q CLOD cL O D CLOD CLOD CLOD cLOD CLOD CLOD CLOQ CLOD CLOD F riday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -230- p. 231 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTUA (fimol/kg) in Soils Treated with Soil Type Sample Interval Aerobic Live Sterile Alfisol DayO Week 1 Week 2 Week 4 Month. 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month IS Month 24 <LOD <LOD <LOD CLOD CLOD CLOD CLOQ CLOQ CLOQ CLOD CLOD CLOD CLOQ CLOQ CLOQ CLOQ CLOQ CLOQ CLOQ CLOQ CLOQ cLOQ cLOQ cLOQ LOD = limit of detection (0.0003 pmol/kg) LOQ = limit o f quantitation (0.0044 pmol/kg) CLOD CLOD cLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD CLOD <LOD CLOD CLOD CLOD CLOQ cLOQ Anaerobic Live Sterile CLOD CLOD CLOD CLOD CLOD cLOD cLOQ cLOQ cLOD CLOQ 0.008 0.005 0.005 cLOQ CLOD cLOD CLOD cL O D cL O D CLOD CLOD <LOD CLOD CLOD cLOD CLOD CLOQ CLOQ ,Friday October 12, 2607 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -231 - p. 232 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTUA (punol/kg) in Soils Treated with^ 3 Soil Type Sample Interval Aerobic Live Sterile Incentisol Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOD <LOD <LOQ <LOQ 0.013 0.011 0.055 0.027 0.170 0.194 0.358 0.350 0.419 0.352 0.457 0.452 0.492 0.550 0.559 0.530 0.542 0.522 LOD = lirait of detection (0.0003 pmol/kg) LOQ = limit of quantitation (0.0044 pmol/kg) <LOD CLOD CLOD cLOD cLOD cLOD <LOD cLOD CLOD CLOD <LOQ cLOD 0.006 CLOQ 0.005 CLOQ CLOQ CLOQ Anaerobic Live Sterile CLOD CLOD cLOD cLOD CLOD cLOQ 0.017 CLOQ 0.012 0.012 0.028 0.028 0.034 0.022 cLOD CLOD CLOD CLOD <LOD <LOD cLOD <LOD cLOD CLOD cLOD CLOD <LOQ cLOQ F riday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -232 - p. 233 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTA (junol/kg) in Soils Treated wititQ 3 Sample Aerobic Anaerobic S o il Type______ Interval_________ L ive Sterile_____L ive Sterile Ultisol DayO Week 1 Week2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOD <LOD <LOQ <LOQ 0.008 0.008 0.013 0.010 0.018 0.018 0.020 0.017 0.021 0.040 0.041 0.025 0.006 0.009 0.009 0.008 0.014 0.006 0.010 0.011 <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOD <LOD <LOD <LOD 0.004 <LOD <LOD <LOD <LOD <LOD <LOQ <LOD <LOD <LOD <LOD <LOD <LOQ <LOQ <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD CLOD CLOD <LOD CLOD LOD = limit of detection (0.0011 pmol/kg) LOQ = limit o f quantitation (0.0042 pmol/kg) Friday, O ctober 12,2 0 0 7 Company Sanitized. Does not contain TSC'A CBI. W ildlife International, Ltd. -233 - p. 234 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 M easured Concentrations o f 8-2 F T A (ju n o l/kg ) in Soils T reated w ith Q J Soil Type Sample Interval Aerobic Live Sterile Mollisol Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 CLOD <LOQ cLOQ CLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD cL O D CLOD CLOD cL O D cLOQ 0.005 cL O D CLOD CLOD cLOD cL O Q CLOQ LOD = limit o f detection (0.0011 pmol/kg) LOQ = limit o f quantitation (0.0042 pmol/kg) cL O D CLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOD cLOD CLOD CLOD <LOD <LOD <LOD CLOD Anaerobic U ve Sterile CLOD CLOD cL O D CLOD CLOD cLOD CLOD cLOD cL O D CLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD <LOD CLOD CLOD cLOD CLOD CLOD cLOD CLOD cL O D CLOD CLOD Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. ,W ildlife International Ltd. -234- p. 235 Project No.: 112E-108 Wildlife InternationalLtd. Project Number 112E-108 M easured Concentrations o f 8-2 F T A (fim ol/kg) in Soils Treated w ith 1 Soil Type Sample Interval Aerobic Live Sterile Anaerobic Live Sterile Alfisol Day 0 Week 1 Week2 Week4 Mouth2 Monti 4 Month 6 Month? Month 12 Month 15 Month 18 Month 24 CLOD CLOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD cLOQ CLOQ LOD = limit o f detection (0.0011 pmol/kg) LOQ = limit o f quantitation (0.0042 pmol/kg) CLOD CLOD CLOD CLOD cL O D CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD cLOQ CLOQ CLOD CLOD CLOQ CLOQ cLOQ CLOQ cL O D CLOD CLOD CLOD cLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD CLOQ Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 235 - p. 236 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 M easured C oncentrations o f 8-2 F T A (pm ol/kg) in Soils T re ated w ith ^ 3 Sample Aerobic Anaerobic Soil Type________ Interval____________Live Sterile______ Live Sterile InceDtisoI Day 0 Week 1 Week 2 Week4 Month 2 Month 4 Month 6 Month 9 Month 12 Month IS Month 18 Month 24 <LOQ <LOQ <LOD <LOD <LOQ <LOQ 0.011 0.010 0.038 0.027 0.154 0.158 0.341 0.302 0.343 0.265 0.279 0.294 0.404 0.430 0.447 0.474 0.423 0.464 LOD = limit o f detection (0.0011 pmol/kg) LOQ = limit o f quantitation (0.0042 pmol/kg) <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOD 0.006 <LOQ 0.006 <LOQ <LOQ <LOQ <LOD <LOD <LOQ <LOD <LOD <LOD 0.014 <LOQ 0.005 0.005 0.013 0.012 0.018 0.011 <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD CLOD <LOQ Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -236- p. 237 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 M easured Concentrations o f P F N A (pm ol/kg) in Soils Treated Soil Type Sample Interval Aerobic Live Sterile Ultisol DayO Week 1 Week2 Week 4 Month2 Month4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ 0.015 0.016 0.025 0.026 0.038 0.036 0.052 0.046 0.060 0.065 0.061 0.066 0.072 0.065 0.018 0.034 0.051 0.057 0.064 0.053 0.067 0.064 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOD = limit o f detection (0.0003 pmol/kg) LOQ = limit o f quantitation (0.0043 pmol/kg) Anaerobic Live Sterile <LOQ <LOQ 0.014 0.015 0.020 0.020 0.034 0.029 0.033 0.046 0.050 0.048 0.065 0.055 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ ,Friday O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -237- p. 238 Project No.: 112E-108 Wildtife International, Ltd. Project Number 112E-108 M easured Concentrations o f P F N A (fun o l/kg ) in Soils T reated w ith 3 Soil Type Sample Interval Aerobic Live Sterile Mollisol ' Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month6 Month 9 Month 12 Month IS Month 18 Month 24 <LOQ cLOQ 0.013 0.013 0.012 0.018 0.023 0.026 0.039 0.037 0.048 0.048 0.046 0.043 0.037 0.024 0.042 0.040 0.031 0.056 0.045 0.037 0.055 0.075 <LOD <LOD cL O Q CLOQ CLOD cLOD CLOQ cL O Q cLOQ <LOQ CLOQ <LOQ CLOQ cLOQ CLOQ CLOQ cL O Q cLOQ LOD = limit o f detection (0.0003 jimol/kg) LOQ = limit o f quantitation (0.0043 pmol/kg) Anaerobic Live Sterile CLOQ cLOQ 0.009 0.009 0.013 0.010 0.009 0.013 0.014 0.018 0.026 0.020 0.034 0.026 cL O D cL O D cLOQ CLOQ cL O Q cLOD cLOQ cLOQ cL O Q cL O Q cL O Q cL O Q CLOQ CLOQ Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -238 - p. 239 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 M easured Concentrations o f P F N A (junol/kg) in Soils T reated w ith 3 Soil Type Sample Interval Aerobic Live Sterile Anaerobic Live Sterile Alfisol . Day 0 Week 1 Week2 Week4 Month. 2 Month 4 Month 6 Month 9 Month 12 Month 13 Month 18 Month 24 <LOQ <LOQ 0.007 0.009 0.010 0.008 0.014 0.017 0.022 0.035 0.023 0.029 0.019 0.034 0.038 0.050 0.029 0.038 0.050 0.033 0.034 0.038 0.054 0.047 <LOD <LOD <LOQ <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOQ . <LOQ <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ 0.005 0.006 0.007 0.010 0.010 0.008 0.014 0.019 0.020 0.024 0.017 <LOQ <LOQ <LOQ <LOD <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOD = limit o f detection (0.0003 pmol/kg) LOQ = limit o f quantitation (0.0043 pmol/kg) Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -239 - p. 240 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 M easured Concentrations o f P F N A (junol/kg) in Soils T reated w ith Soil Type Sample Interval Aerobic Live Sterile Inceotisol Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Monlh6 . Month 9 Month 12 Month IS Month 1$ Month 24 <LOQ <LOQ 0.044 0.054 0.062 0.072 0.079 0.076 0.134 0.138 0.128 0.133 0.146 0.172 0.172 0.171 0.154 0.152 0.159 0.160 0.171 0.174 0.208 0.224 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOD = limit o f detection (0.0003 pmol/kg) LOQ = limit o f quantitation (0.0043 pmol/kg) Anaerobic Live Sterile <LOQ <LOQ 0.021 0.016 0.028 0.029 0.075 0.047 0.053 0.057 0.062 0.077 0.073 0.078 <LOQ <L0Q <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ Friday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -240- p. 241 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 M easured Concentrations o f P F D A (fim ol/kg ) in Soils T reated w ith 'J Sample Aerobic Anaerobic Soil Type________ Interval__________ Live Sterile______ Live Sterile Ultisol . Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month. 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ 0.009 0.009 0.015 0.016 0.021 0.023 0.035 0.036 0.052 0.055 0.059 0.069 0.074 0.076 0.018 0.041 0.065 0.066 0.093 0.071 0.099 0.086 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOD = limit o f detection (0.0002 pmol/kg) LOQ = limit of quantitation (0.0039 pmol/kg) <LOQ <LOQ 0.009 0.010 0.013 0.014 0.018 0.016 0.026 0.029 0.049 0.055 0.043 0.038 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ Thursday, N ovem ber OS, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -241 - p. 242 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFDA (funol/kg) in Soils Treated with^ 3 Soil Type Sample Interval Aerobic Live Sterile Anaerobic Live Sterile Mollisol ' Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ 0.007 0.007 0.009 0.010 0.012 0.012 0.019 0.020 0.028 0.032 0.034 0.034 0.032 0.024 0.038 0.036 0.028 0.054 0.043 0.042 0.088 0.094 LOD = limit o f detection (0.0002 pmol/kg) LOQ = limit o f quantitation (0.0039 pmol/kg) <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 0.004 <LOQ <LOQ <LOQ <LOQ 0.004 <LOQ <LOQ <LOQ <LOQ 0.007 0.007 0.010 0.009 0.013 0.013 0.021 0.021 0.034 0.028 0.041 0.034 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ Thursday, N ovem ber 08, 2007 Company Sanitized. Does not contain TSCA CB1. ,W ildlife International Ltd. -242- p. 243 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFDA (pmol/kg) in Soils Treated withQ Sample Aerobic Anaerobic Soil Type________ Interval___________ Live Sterile______ Live Sterile Alfisol DayO Weekl Week 2 Week4 Month 2 Month 4 MODth6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ 0.004 0.006 0.006 0.009 0.009 0.016 0.018 0.016 0.019 0.018 0.024 0.033 0.038 0.025 0.031 0.051 0.030 0.045 0.040 0.073 0.071 LOD = limit of detection (0.0002 pmol/kg) LOQ = limit o f quantitation (0.0039 pmol/kg) <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ 0.005 0.006 0.007 0.011 0.011 0.009 0.017 0.025 0.026 0.028 0.024 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ Friday. O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -243 - p. 244 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFDA (fimol/kg) in Soils Treated with J Soil Type Sample Interval Aerobic Live Sterile InceDtisol Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ 0.009 0.010 0.016 0.016 0.030 0.030 0.067 0.058 0.085 0.098 0.102 0.134 0.130 0.111 0.121 0.136 0.122 0.128 0.158 0.151 0.169 0.174 <LOQ <LOQ <120Q <LOQ <LOQ <LOQ <LOQ <LOQ 0.004 <LOQ 0.005 <LOQ 0.006 0.006 0.006 0.005 0.004 0.004 LOD = limit o f detection (0.0002 pmol/kg) LOQ = limit o f quantitation (0.0039 pmol/kg) Anaerobic Live Sterile <LOQ <LOQ 0.010 0.009 0.015 0.015 0.041 0.022 0.042 0.045 0.065 0.076 0.091 0.080 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 0.005 <LOQ F riday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. Wildlife International, Ltd. -244- p. 245 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFUA Qunol/kg) in Soils Treated with Soil Type Sample Interval Aerobic Live Sterile Dltisoi . DayO Week 1 Week2 Week 4 Month2 Month. 4 Month6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ 0.005 0.006 0.009 0.008 0.015 0.014 0.023 0.027 0.028 0.029 0.033 0.030 0.006 0.019 0.027 0.028 0.034 0.029 0.040 0.040 LOD = limit o f detection (0.0002 pmol/kg) LOQ = limit o f quantitation (0.0036 pmol/kg) <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ Anaerobic Live Sterile <LOQ <LOQ <LOQ <LOQ 0.005 0.005 0.007 0.007 0.012 0.015 0.027 0.023 0.032 0.031 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ ' Friday, O ctober 12, 2907 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -245 - p. 246 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFUA Qunol/kg) in Soils Treated withC 3 Sample Aerobic Anaerobic Soil Type________ Interval___________ Live Sterile______ Live Sterile Mollisol DayO Week 1 Week2 Week4 Month.2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ 0.004 0.005 0.005 0.011 0.010 0.018 0.019 0.017 0.017 0.015 0.008 0.016 0.015 0.011 0.020 0.018 0.016 0.026 0.038 LOD - limit ofdetection (0.0002 pmoldsg) LOQ = limit ofquantitation (0.0036 pmol/kg) <LOQ <LOQ <LOD <LOD <LOD <LOD <LOQ <LOQ <LOQ <LOD <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 0.004 0.004 0.006 0.011 0.008 0.012 0.010 <LOQ <LOQ <LOQ <LOQ <LOD <LOD <LOQ <LOQ <LOD <LOD <LOQ <LOQ <LOQ <LOD Friday. O ctober 22, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -246- p. 247 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFUA (junol/kg) in Soils Treated with(_ J Sample Aerobic Anaerobic Soil Type________ Interval___________ Live Sterile______ Live Sterile Alfisol Day 0 Week 1 . ' Week2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOD <LOD <LOQ <LOQ <LOQ <LOQ 0.004 0.004 0.008 0.011 0.007 0.011 0.006 0.011 0.013 0.020 0.014 0.016 0.024 0.010 0.012 0.013 0.025 0.018 LOD = limit o f detection (0.0002 pmol/kg) LOQ = limit o f quantitation (0.0036 pmol/kg) <LOD <LOD <LOQ <LOQ <LOD <LOD cLOD CLOD CLOD CLOD cL O Q CLOD cLOD cLOQ cL O Q cL O D cLOQ CLOQ CLOD CLOD CLOQ cLOQ cL O Q CLOQ cLOQ cL O Q cL O Q 0.005 0.005 0.006 0.008 0.006 cLOD CLOD cLOD cLOD CLOQ CLOQ cLOD CLOD cL O Q CLOD CLOD CLOD cL O Q cL O Q Friday. O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -247- p. 248 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of PFUA (jimol/kg) in Soils Treated w ith J Sample Aerobic Anaerobic Soil Type________ Interval___________ Live Sterile______ Live Sterile Inceotisol Day 0 Week 1 Week 2 Week4 Month 2 Month 4 Monlh6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ 0.004 0.007 0.008 0.013 0.011 0.034 0.035 0.033 0.033 0.037 0.050 0.052 0.050 0.046 0.052 0.046 0.045 0.062 0.058 0.072 0.080 LOD = limit o f detection (0.0002 pmol/kg) LOQ = limit o f quantitation (0.0036 pmol/kg) <LOQ <LOQ <LOQ <LOQ <LOD <LOD <LOD <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOD <LOQ <LOQ 0.006 0.006 0.017 0.011 0.025 0.025 0.030 0.034 0.039 0.037 <LOD <LOD <LOD <LOD <LOD <LOQ <LOQ <LOD <LOQ <LOQ <LOQ <LOD <LOQ <LOQ F riday, O ctober 12, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -248 - p. 249 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTOH (junol/kg) in Soils Treated with 3 Soil Type Sample Interval Aerobic Live Sterile Ultisol Day 0 Week I . Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOD <LOD <LOD <LOD <LOQ <LOQ <LOD <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD CLOD <LOD LOD --limit o f detection (01048 pmol/kg) LOQ = limit o f quantitation. (0.216 pmol/kg) Anaerobic Live Sterile <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD M onday, O ctober IS , 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -249- p. 250 Project No.: 112E-108 Wildlife International, Ltd, Project Number 112E-108 Measured Concentrations of 8-2 FTOH (pmol/kg) in Soils Treated withU 3 Soil Type Sample Interval Aerobic Live Sterile Mollisol Day 0 Week 1 Week2 Week 4 Month 2 Month4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOD <LOD cL O D <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD CLOD cL O D CLOD CLOD CLOD <LOD cL O D CLOD cL O Q CLOD CLOD LOD - limit o f detection (0.048 pmol/kg) LOQ = limit o f quantitation (0.216 uniol/kg) CLOD CLOD CLOD CLOD cLOD CLOD cLOD CLOD CLOD CLOD cLOD CLOD cLOD CLOD <LOD CLOD cLOD CLOD Anaerobic Live Sterile CLOD cL O D cLOQ CLOQ CLOD CLOD cL O D CLOD cLOD CLOD cLOD CLOD cLOD cLOD CLOD cL O D cL O D CLOD cL O D CLOD cLOD cL O D CLOD cL O D cL O D CLOD cLOD CLOD M onday, O ctober IS , 2007 Company Sanitized. Does not contain TSCA CBI. ,W ildlife International Ltd. -250- p. 251 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTOH (pmol/kg) in Soils Treated withQ D Soil Type Sample Interval Aerobic Live Sterile Anaerobic Live Sterile Alfisol Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month L2 Month 15 Month 18 Month 24 <LOD CLOD <LOD <LOD <LOD <LOD <LOD <LOD CLOD CLOD cLOD CLOD cLOD CLOD cLOD CLOD CLOD CLOD cLOD cLOD CLOD CLOD cLOQ CLOD LOD = limit o f detection (0.048 pmol/kg) LOQ = limit o f quantitation (0.216 pmol/kg) CLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD cL O D CLOD <LOD cLOD cLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOQ CLOD cLOD CLOD CLOD CLOD CLOD cLOD CLOD CLOD cLOD CLOD <LOD CLOD cL O D CLOD cL O D cL O D M onday, O ctober IS , 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -251 - p. 252 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTOH (junol/kg) in Soils Treated with(. T Soil Type Sample Interval Aerobic Live Sterile Inceotisol Day 0 Week 1 Week 2 Week 4 ' Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOD <LOD <LOD CLOD CLOD CLOD cLOQ CLOQ 0.374 0.269 0.319 0.297 cLOQ 0.302 0.216 cLOQ 0.282 0.356 0.374 0.261 cLOQ CLOQ cL O Q cLOQ LOD = limit o f detection (0.048 pmol/kg) LOQ = limit o f quantitation (0.216 pmol/kg) <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD <LOQ CLOD cLOD CLOD cL O D CLOD CLOD CLOD Anaerobic Live Sterile CLOD cLOD CLOD CLOD CLOD cLOD cLOQ CLOD cLOQ CLOQ cLOQ CLOQ CLOQ CLOQ CLOD CLOD cL O D cL O D CLOD CLOD CLOD CLOD cLOQ cL O D cL O D CLOD cLOD CLOD M onday, O ctober 15, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -252- p. 253 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTOH (pmol/L) in Headspaces Gases from Chambers Treated with Sample Aerobic Anaerobic Soil Type________ Interval___________ Live Sterile______ Live Sterile Dltisol DayO Week 1 Week2 Week 4 Month. 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month IS Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOQ = limit of quantitation (0.027 {imol/L ofheadspace) M onday, O ctober IS , 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -253 - p. 254 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations,of 8-2 FTOH (pmol/L) in Headspaces Gases from Chambers Treated withC 1 Soil Type Scingile Interval Aerobic Live Sterile MoDisol DayO Week 1 Week 2 Week 4 Month 2 Month4 Month6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOQ = limit of quantitation (0.027 pmol/L ofheadspace) Anaerobic Live Sterile <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ M onday, O ctober IS , 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -254- p. 255 Project No.: 112E-108 Wildlife International, Ltd. P ro je ct N u m b er 112E-108 Measured Concentrations of 8-2 FTOH (pjmol/L) in Headspaces Gases from Chambers Treated w ith 1 Sample Aerobic Anaerobic Soil Type________ Interval___________ Live Sterile______ Live Sterile Alfisol Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOQ = limit o f quantitation (0.027 pmol/L ofheadspace) <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ M onday, O ctober 15, 2007 Company Sanitized. Does not contain TSCA CBI. ,W ildlife International Ltd. -255 - p. 256 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 8-2 FTOH (pmol/L) in Headspaces Gases from Chambers Treated withjj, D Soil Type Sample Interval Aerobic Live Sterile InceotisoL DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 M onth 12 M onth 15 Month IS M onth 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOQ = limit of quantitation (0.027 pmol/L ofheadspace) Anaerobic Live Sterile <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ M onday, O ctober IS , 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -256- p. 257 Project No.: 112E-108 Wildlife InternationalLtd. Project Number 112E-108 Measured Concentrations of 7-2 s FTOH (junol/kg) in Soils Treated with 3 Soil Type Sample Interval Aerobic Live Sterile Ultisol DayO Month 2 Month 6 Month 9 Month 12 Month IS Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ 0.321 0.401 <LOQ <LOQ <LOQ <LOQ 0.279 <LOQ <LOQ <LOQ <LOQ LOQ = limit ofquantitation (0.24 jimol/kg) Anaerobic Live Sterile Thursday, N ovem ber 0 8 2 0 0 7 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -257 - p. 258 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 7-2 s FTOH Qimol/kg) in Soils Treated w ith Sam ple A erobic A naerobic S o il Type_______In terval_________ L ive S terile_____ L ive S terile Mollisol Day 0 M onlli2 M onth 6 M ontli9 M onth 12 M o n th 15 M onth 18 M onth 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOQ = limit of quantitation (0.24 pmol/feg) ' Thursday, N ovem ber 08, 2007 Company Sanitized. Does not contain TSCA CB1. W ildlife International, Ltd. -258 - p. 259 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 7-2 s FTOH (pmol/kg) in Soils Treated with^ S oil Type Sam ple In terval A erobic L ive S terile Alfisol DayO Month 2 Month6 Month 9 Month 12 Month IS Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOQ = limit of quantitatiaDL(0.24 pmol/kg) A naerobic L ive S terile Thursday, N ovem ber 08, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -259 - p. 260 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 7-2 s FTOH Qunol/kg) in Soils Treated with ^ Sam ple A erobic A naerobic S o il Type______ In terval_________ L ive Sterile_____L ive S terile O' O 33 Inceotisol DayO Month 2 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ 0.672 0.672 0.466 1.121 0.466 0.287 0.418 0.440 <LOQ <LOQ <LOQ <LOQ LOQ = limit of quantitation (024 iimol/kg) Thursday, N ovem ber 08, 2007 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 260- p. 261 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 7-3 Acid (p.moI/kg) in Soils Treated withQ ^ Sam ple A erobic A naerobic S o il Type_______In terval_________ L ive Sterile_____ L ive Sterile Ultisol Day 0 Month2 Mondi 6 Month 9 Month 12 Month IS Month 18 Month24 <LOQ <LOQ 0.015 0.021 0.037 0.048 0.071 0.065 0.094 0.076 0.077 0.091 0.063 0.038 0.123 0.127 ' LOQ= limit of quantitation (0.0045 pmol/kg) W ednesday, M arch 12,2008 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -261 - p. 262 Project No.: 112E-108 Wildlife International, Ltd. P roject N um ber 112E-108 Measured Concentrations of 7-3 Acid (pmol/kg) in Soils Treated with ^ Soil Type Sample Interval Aerobic Live Sterile Mollisol Day 0 Month 2 Month 6 Month 9 Month 12 Month IS Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ 0.005 0.006 0.006 0.006 0.011 0.011 0.015 0.020 0.008 0.008 0.020 0.015 LOQ= limit of quantitation (0.0045 pmol/kg) Anaerobic Live Sterile W ednesday, M arch 12,2008 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 262- p. 263 Project No.: 112E-108 Wildlife International, Ltd. Project Number 112E-108 Measured Concentrations of 7-3 Acid (fimol/kg) in Soils Treated w ith 3 S o il Type Sam ple In terval A erobic l iv e S terile A lfisol Day 0 M onth 2 Month 6 Month9 Month 12 Mon* 15 Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ 0.007 0.006 0.007 0.006 0.011 0.014 0.017 0.020 0.018 0.015 0.015 0.016 LOQ= limit of quantitation (0.0045 pmol/kg) A naerobic L ive S terile W ednesday, M arch 12,2008 I 1 Company Sanitized. Does not contain TSCA CB1. W ildlife International, Ltd. -263 - p. 264 Project No.: 112E-108 Wildlife International, Ltd. Project Num ber 112E-108 Measured Concentrations of 7-3 Acid (pmol/kg) in Soils Treated with. 3 Sample Soil Type________ Interval A erobic L ive S terile A naerobic L ive S terile Inceotiso) Day 0 0o tO o Month2 Month 6 Month 9 Month 12 Month 15 Month IS Month24 0.038 0.022 0.153 0.185 0.290 0.347 0.626 0.557 0.590 0.655 0.638 0.480 0.803 0.728 LOQ= limit of quantitation (0.0045 pmol/kg) W ednesday, M arch 12, 2008 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -264- p. 265 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 1 1 2 E-1 0 8 , 109,110 Measured Concentrations of PFOA (pjmoi/kg) in Untreated and Fortified Soils S o il Type Sam ple In terval U ntreated C ontrols A erobic A naerobic Ultisol Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <L0Q <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOD = limit of d&ection (0.0005 p.mol/kg) LOQ = limit of quantitation (0.0048 jimol/kg) F ortified R ecoveries A erobic A naerobic 0.023 0.019 0.021 0.022 0.022 0.022 0.025 0.025 0,029 0.028 0.026 0.025 0.022 0.024 0.018 0.017 95% 78% 85% 91% 92% 92% 104% 103% 120% 114% 106% 104% 92% 100% 74% 68% 0.023 0.022 0.025 0.027 0.022 0.024 0.023 0.022 0.027 0.026 0.027 0.027 0.027 0.028 95% 92% 105% 113% 92% 98% 93% 90% 114% 108% 114% 113% 112% 115% Friday, O ctober 12, 2007 Page 1 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -265 - p. 266 Project No.: 112E-108 Wildlife International, Ltd. P ro je ct N u m b ers 1 12E -108,109;1 10 M easured Concentrations o f P F O A (pm ol/kg) in U ntreated and F o rtifie d Soils Sample Untreated Controls F ortified Recoveries Soil Type________ Interval______ Aerobic Anaerobic_____ Aerobic______ Anaerobic Mollisol . Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOD <LOD <LOD <LOD cLOD CLOD cLOQ CLOQ cLOD CLOD CLOQ CLOD CLOQ cLOQ CLOQ CLOD cLOD CLOD cL O D cLOD CLOQ cLOD CLOD CLOD cLOQ cLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD 0.022 0.022 0.023 0.024 0.021 0.023 0.022 0.022 0.026 0.027 0.032 0.029 0.032 0.029 0.028 0.028 0.022 0.025 89% 93% 97% 100% 88% 94% 91% 90% 107% 112% 132% 121% 131% 120% 114% 116% 92% 104% 0.023 0.024 0.020 0.023 0.020 0.021 0.023 0.024 0.030 0.026 0.034 0.034 0.035 0.035 93% 101% 85% 96% 85% 89% 95% 99% 122% 109% 140% 139% 145% 143% LOD " limit of detection (0.0005 umoi/kg) LOQ = limit of quantitation (0.0048 pmol/kg) Friday, O ctober 12, 2007 Page 2 o f4 Company Sanitized. Does not contain TSCA CB1. W ildlife International, Ltd. - 266- p. 267 Project No.: 112E-108 Wildlife International, Ltd. ProjectNumbersll2E-108,109,110 M easured Concentrations o f P F O A (pm ol/kg) in U ntreated and F o rtifie d Soils Sample Untreated Controls Fortified Recoveries Soil Type________ Interval______ Aerobic Anaerobic_____ Aerobic______ Anaerobic Alfisol Day 0 Week 1 Week 2 Week4 Month2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOD <LOD <LOD CLOD <LOD CLOD CLOD CLOD CLOD CLOD CLOQ <LOQ CLOD CLOD cLOD CLOD CLOD CLOD cLOD CLOD CLOD LO D --limit of detection (0.0005 pmol/kg) LO Q = limit ofquantitation (0.0048 pmol/kg) CLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD 0.022 0.020 0.022 0.024 0.024 0.023 0.024 0.024 0.026 0.026 0.026 0.028 0.027 0.027 0.028 0.030 0.022 0.022 92% 83% 89% 100% 99% 94% 100% 101% 110% 107% 108% 115% 110% 111% 113% 125% 92% 93% 0.022 0.020 0.021 0.022 0.023 0.024 0.025 0.025 0.025 0.026 0.027 0.026 0.025 0.027 92% 82% 87% 93% 96% 100% 106% 104% 104% 107% 111% 109% 105% 112% Friday, O ctober 12, 2607 Page 3 o f4 p. 268 Company Sanitized. Does not contain TSCA CBI. ________W ildlife International, Ltd. project no - 112E-108 -267- WVViMldWllitfjCe Ifnibteerrnrua+MtiUoJnt*a*'l*,, Ltd. ____________ Project Numbers 112E-108,'109,110 M easured Concentrations o f P F O A (pm ol/kg) in U ntreated and F o rtifie d Soils Soil Type Sample Interval Untreated Controls Aerobic Anaerobic Inceotisol Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOD = limit of detection (0.0005 pmol/kg) LOQ = limit of quantitation (0.0048 pmol/kg) Fortified Recoveries Aerobic Anaerobic 0.025 104,4 0.025 lo:% 0.031 129,4 0.024 101% 0.026 106,4 0.026 109,4 0.030* 124,4 0.027 112,4 0.027 113,4 0.028 117,4 0.032 134,4 0.026 108,4 0.029 121,4 0.026 106,4 0.035 145,4 0.030 124,4 0.023 96,4 0.023 96,4 0.023 0.023 0.026 0.024 0.026 0.025 0.026 0.026 0.029 0.027 0.026 0.028 0.027 0.028 97% 94% 109% 98% 108% 105% 107% 109% 119% 111% 106% 115% 113% 116% Friday, O ctober 12, 2007 Page 4 o f 4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -268- p. 269 Project No.: 112E-108 WiIdlife International, Ltd. Project Numbers 112E-108,109,110 Measured Concentrations of 8-2 FTUA (pmol/kg) in Untreated and Fortified Soils Sam ple U ntreated C ontrols F ortified R ecoveries S o il Type__________ In terva l________ A ero b ic A naerobic______ A erobic_______ A naerobic U ltiso l Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month $ Month 12 M onth 15 Month IS Month 24 <LOQ <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <L0D CLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOD LOD = lim it o f detection (0.0003 junol/kg) LOQ = lim it o f quantitation (0.0044 ^mol/kg) CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD ' 0.016 0.014 0.017 0.017 0.015 0.015 0.016 0.016 0.019 0.017 0.014 0.016 0.006 0.012 0.011 0.009 72% 65% 77% 79% 69% 69% 72% 72% 89% 80% 65% 73% 29% 54% 51% 40% 0.017 0.016 0.017 0.019 0.018 0.018 0.018 0.017 0.020 0.017 0.018 0.017 0.014 0.015 80% 74% 77% 87% 84% 82% 82% 79% 93% 76% 82% 80% 65% 70% Friday, O ctober 12 ,2 0 0 7 P age J of.4 p. 270 Company Sanitized. Does not contain TSCA CBI. .W ild life International, L td _____________________________Project no.: m E -io s -269- Wildlife International, Ltd._____________ Project Numbers 112B-108,109,110 Measured Concentrations of 8-2 FTUA (pmol/kg) in Untreated and Fortified Soils S o il Type Sam ple In terval U ntreated C ontrols A erobic A naerobic M ollisol DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 M onth 12 Month IS M onth 18 M onth 24 <LOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOD cLOD cLOD cLOD CLOD cLOQ cLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD LO D --limit o f detection (0.0003 pjnol/kg) LO Q = lim it o f quantitation (0.0044 fimol/kg) F ortified R ecoveries A erobic A naerobic 0.020 0.020 0.018 0.019 0.020 0.021 0.020 0.020 0.019 0.019 0.022 0.020 0.022 0.018 0.017 0.020 0.013 0.014 92% 90% 81% 85% 91% 95% 90% 91% 88% 87% 100% 94% 102% 82% 78% 90% 59% 63% 0.016 0.019 ,0.017 0.019 0.017 0.021 0.018 0.018 0.021 0.017 0.022 0.023 0.022 0.019 73% 88% 77% 87% 77% 98% 80% 80% 97% 78% $9% 107% 100% 85% ,Friday O ctober 12, 2007 Page2 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -270- p. 271 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 1 1 2 E-K)8 , 1 0 9 ,1 1 0 Measured Concentrations of 8-2 FTUA (jimol/kg) in Untreated and Fortified Soils Sam ple Untreated C ontrols S o il Type__________ In terval________ A ero b ic A naerobic F ortified R ecoveries A erobic A naerobic A lfiso l DayO Week 1 Week 2 Week 4 M onth2 Month 4 Month 6 Month 9 M onth 12 M onth IS Month 18 Month 24 <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD LOD = lim it o f detection (0.0003 nmol/kg) LOQ = lim it o f quantitation (0.0044 pmol/kg) <LOD <LOD <LOD <LOD <LOD <LOD cLOD <LOD CLOD <LOD cLOD CLOD cLOD CLOD 0.018 0.017 0.019 0.021 0.023 0.017 0.016 0.020 0.021 0.020 0.014 0.020 0.018 0.020 0.018 0.024 0.014 0.015 84% 77% 86% 98% 105% 76% 75% 92% 96% 91% 66% 90% 84% 90% 80% 111% 62% 67% 0.020 0.016 0.020 0.021 0.020 0.019 0.019 0.020 0.024 0.024 0.018 0.018 0.023 0.018 89% 75% 93% 95% 92% 89% 86% 94% 309% 308% 81% 83% 103% 83% Friday, O ctober 12, 2007 Page 2 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -271 - p. 272 projectNo.: 112E-108 Wildlife International, Ltd. Project Numbers 112E-108,109,110 Measured Concentrations of 8-2 FTUA (ftmol/kg) in Untreated and Fortified Soils Soil Type Sample Interval Untreated Controls Aerobic Anaerobic Inceutisol Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month IS Month 18 Month 24 CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD cLOD CLOD CLOD CLOD cLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOD cLOD cLOD CLOD LOD = limit of detection (0.0003 pmol/kg) LOQ = limit of quantitation (0.0044 pmol/kg) Fortified Recoveries Aerobic Anaerobic 0.024 0.021 0.024 0.018 0.019 0.021 0.020 0.017 0.018 0.020 0.022 0.018 0.015 0.015 0.016 0.014 0.012 0.011 110% 96% 108% 83% 88% 97% 94% 79% 80% 89% 101% 81% 70% 68% 74% 64% 53% 52% 0.017 0.018 0.018 0.016 0.019 0.017 0.017 0.018 0.017 0.019 0.014 0.015 0.013 0.016 79% 81% 83% 75% 85% 78% 77% 82% 76% 88% 66% 70% 61% 71% Friday, O ctober 12, 2007 P a g e4 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -272- p. 273 Project No.: 112E-108 Wildlife International, Ltd. ProjectNumbersll2E-108,109,110 Measured Concentrations of 8-2 FTA (jtunol/kg) in Untreated and Fortified Soils Sample Untreated Controls Fortified Recoveries Soil Type________ Interval______ Aerobic Anaerobic_____ Aerobic______ Anaerobic Ultisol Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOD <LOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD <LOD CLOD cLOD CLOD CLOD cLOD cLOQ CLOQ cLOD cLOD CLOD LOD = limit ofdetection (0.0011 pxnol/kg) LOQ - limit of quantitation (0.0042 jimol/kg) CLOD CLOD CLOD cLOD CLOD CLOD CLOD <LOD CLOD CLOD CLOD CLOD cLOD CLOD 0.013 0.012 0.013 0.014 0.011 0.011 0.011 0.011 0.007 0.005 0.007 0.008 cLOQ CLOQ 0.009 cLOQ 1% 58% 62% 69% 54% 55% 54% 53% 33% 24% 34% 37% 41% 0.014 0.014 0.015 0.015 0.013 0.014 0.011 0.013 0.015 0.011 0 .0 1 0 0 .0 1 0 0.007 0.007 67% 66% 70% 69% 61% 65% 53% 63% 72% 51% 48% 46% 35% 32% Friday, October 12, 2007 Page 1 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -273 - p. 274 project no : 112E-ios Wildlife International, L td._________________ P ro je c t N u m b e rs 11 2 E -1 0 8 ,1 0 9 ,1 1 0 Measured Concentrations of 8-2 FTA (fimol/kg) in Untreated and Fortified Soils S oil Type M ollisol Sam ple In terval DayO Week 1 Week 2 Week 4 Month 2 M onth 4- Month 6 Month 9 M onth 12 M onth 15 M onth 18 M onth 24 U ntreated C ontrols A erobic A naerobic <LOD CLOD 0.006 CLOD CLOD CLOD cLOQ CLOD cLOD CLOD cLOD CLOD cLOD CLOD cLOD CLOD cLOD cLOQ cLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOD cLOD CLOD CLOD cLOD CLOD cLOD CLOD L O D *lim it o f detection (0.0011 fimol/kg) LO Q = lim it o f quantitation (0.0042 pmol/kg) F ortified R ecoveries A erobic A naerobic 0.018 0.019 0.018 0.019 0.019 0.018 0.017 0.017 0.016 0.017 0.017 0.014 0.013 0.013 0.010 0.013 0.005 CLOQ 87% 90% 84% 90% 90% 88% 83% 81% 78% 79% 84% $9% $4% 62% 50% 63% 23% 0.015 0.018 0.015 0.016 0.013 0.017 0.013 0.015 0.017 0.015 0.012 0.014 0.012 0.011 70% 87% 71% 76% 64% 83% 63% 70% 80% 71% 58% 6S% 57% 52% Friday, O ctober 12, 2007 Page 2 o f4 Company Sanitized. Does not contain TSCA CBI W ildlife International, Ltd. -274- p. 275 Project No.: 112E-108 Wildlife International, Ltd. ProjectN um bersiiZE-108, 109,110 Measured Concentrations of 8-2 FTA (jimol/kg) in Untreated and Fortified Soils S o il Type Sam ple U ntreated C ontrols F ortified R ecoveries In terval_________A erobic A naerobic______ A erobic A naerobic A liiso l Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month IS Month 24 <LOD <LOD <LOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOQ CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOQ cLOQ 0.016 0.017 0.016 0.018 0.022 0.018 0.014 0.017 0.016 0.015 0.009 0.014 0.013 0.014 0.011 0.016 0.008 0.008 78% 79% 78% 84% 106% 87% 68% 84% 75% 70% 42% 67% 60% 66% 51% 77% 40% 37% 0.018 0.014 0.018 0.018 0.018 0.017 0.016 0.017 0.018 0.017 0.014 0.014 0.015 0.015 88% 67% 85% 84% 84% 81% 77% 83% 88% 83% 67% 66% 73% 70% LOD = limit o f detection (0.0011 pmol/kg) LOQ = limit o f quantitation (0.0042 pm ol/kg) Friday, O ctober 12, 2007 Page 3 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -275 - p. 276 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 112E-108,109,110 Measured Concentrations of 8-2 FTA (junol/kg) in Untreated and Fortified Soils Sample Untreated Controls Fortified Recoveries Soil Type________ Interval______ Aerobic Anaerobic_____ A erobic_____ Anaerobic Inceotisol DayO Week 1 Week 2 Week 4 Month 2 Mbnth4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOD <LOD CLOD <LOD CLOD CLOD cLOQ CLOD CLOD CLOD cLOD CLOD cLOD <LOD cLOQ cLOQ cLOQ CLOD cLOD CLOD cLOQ LOD = limit of detection (0.0011 pmol/kg) LOQ = limit of quantitation (0.0042 pmol/kg) CLOD CLOD CLOD CLOD CLOD CLOD CLOD <LOD cLOD cLOD cLOD CLOD cLOD CLOD 0.022 0.020 0.020 0.016 0.015 0.018 0.015 0.013 0.011 0.012 0.011 0.009 0.009 0.008 0.007 0.007 0.004 CLOQ 10794 96S 98% 76% 70% 84% 71% 63% 55% 58% 53% 45% 43% 37% 34% 34% 21% 0.016 0.015 0.015 0.014 0.015 0.016 0.012 0.014 0.010 0.013 0.008 0.007 0.005 0.007 78% 72% 70% 67% 72% 76% 59% 66% 48% 63% 36% 34% 26% 35% Friday, O ctober 12, 2007 Page 4 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -276- p. 277 Project No.: 112E-108 Wildlife International, Ltd. P roject N um bers 1 12E-108,109,110 Measured Concentrations of PFNA (umol/kg) in Untreated and Fortified Soils Soil Type Sample Interval Untreated Controls Aerobic Anaerobic Ultisol DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month IS Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOD = limit of detection (0.0003 jamol/kg) LOQ = limit of quantitation (0.0043 pmol/kg) Fortified Recoveries Aerobic Anaerobic 0.020 0.017 0.021 0.021 0.021 0.021 0.022 0.022 0.024 0.024 0.022 0.023 0.015 0.022 0.017 0.014 94% 78% 97% 98% 95% 98% 104% 101% 114% 114% 103% 106% 70% 103% 79% 67% 0.022 0.021 0.021 0.023 0.021 0.022 0.022 0.021 0.024 0.024 0.025 0.025 0.023 0.025 100% 99% 99% 107% 97% 103% 103% 96% 112% 110% 116% 117% 108% 116% Friday, O ctober 12, 2007 Page 1 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -277- p. 278 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 112E-108,109,110 Measured Concentrations of PFNA (junol/kg) in Untreated and Fortified Soils Soil Type Sample Interval Untreated Controls Aerobic Anaerobic MoDisol DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOD <LOD <LOD <LOD <LOD <LOD <LOQ <LOQ <LOD <LOD <LOD <LOD <LOD LOD = limit of detection (0.0003 pmol/kg) LOQ = limit of quantitation. (0.0043 pmol/kg) <LOD <LOD <LOQ <LOD <LOD <LOD <LOD <LOD CLOD CLOD cLOD CLOD CLOD CLOD Fortified Recoveries Aerobic Anaerobic 0.020 0.021 0.021 0.021 0.021 0.021 0.022 0.018 0.023 0.023 0.026 0.026 0.026 0.025 0.022 0.024 0.017 0.018 94% 96% 97% 97% 95% 99% 102% 86% 107% 106% 122% 119% 120% 117% 100% 112% 81% 83% 0.021 0.022 0.019 0.021 0.021 0.021 0.020 0.021 0.023 0.022 0.025 0.028 0.026 0.026 96% 101% 89% 98% 96% 99% 93% 98% 107% 101% 116% 128% 122% 119% Friday, O ctober 12, 2007 F a g e 2 o f4 Company Sanitized. Does not contain TSCA CBI. ,W ildlife International Ltd. -278 - p. 279 Project No.: 112E-108 Wildlife International, Ltd. P ro ject N u m b ers 1 1 2 E -1 0 8 ,109,110 Measured Concentrations of PFNA (pmoi/kg) in Untreated and Fortified Soils Sample Untreated Controls Fortified Recoveries Soil Type________ Interval______ Aerobic Anaerobic_____ Aerobic______ Anaerobic Aliisol Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 13 Month 18 Month 24 <LOD <LOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD <LOD CLOD <L0Q cLOQ cLOQ CLOQ cLOQ cLOQ CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOQ CLOQ 0.021 0.020 0.020 0.024 0.022 0.020 0.022 0.023 0.024 0.024 0.022 0.025 0.023 0.025 0.024 0.026 0.019 0.018 98% 93% 94% 112% 103% 91% 103% 107% * 113% 110% 100% 114% 108% 114% 113% 123% 87% 86% 0.021 0,017 0.020 0.022 0.021 0.022 0.022 0.022 0.024 0.024 0.023 0.023 0.025 0.022 97% 81% 94% 101% 98% 101% 103% 100% 110% 110% 107% 107% 115% 102% LOD - limit of detection (0.0003 pmol/kg) LOQ = limit of quantitation (0.0043 pmol/kg) ,Friday October 12, 2007 Page 3 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -219- p. 280 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 112E-108,109,110 Measured Concentrations of PFNA (junol/kg) in Untreated and Fortified Soils Soil Type Sample Interval Untreated Controls Aerobic Anaerobic Inceotisol DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOD <LOD CLOQ <LOQ <LOQ <LOD CLOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ CLOQ <LOQ <LOD <LOQ <LOD LOD *=limit of detection (0.0003 jjmol/kg) LOQ = limit of quantitation (0.0043 umol/kg) <LOD <LOD CLOD CLOD CLOQ CLOQ CLOQ cLOQ CLOQ CLOD cLOQ CLOQ cLOQ cLOQ Fortified Recoveries Aerobic Anaerobic 0.027 0.025 0.028 0.023 0.023 0.023 0.027 0.023 0.024 0.026 0.030 0.023 0.022 0.021 0.028 0.023 0.019 0.019 124% 116% 130% 106% 107% 107% 125% 107% 112% 119% 140% 105% 104% 100% 130% 109% 89% 88% 0.022 0.022 0.023 0.021 0.022 0.022 0.022 0.023 0.024 0.024 0.024 0.023 0.022 0.023 102% 100% 108% 98% 103% 102% 101% 107% 111% 111% 110% 108% 101% 108% Friday, O ctober 12, 2007 Page 4 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -280- p. 281 Project No.: 112E-108 Wildiife International, Ltd. P ro je ct N u m b ers 1 12E -108,109,110 Measured Concentrations of PFDA (pmol/kg) in Untreated and Fortified Soils Sample Untreated Controls Fortified Recoveries Soil Type________ Interval______ Aerobic Anaerobic_____ Aerobic______ Anaerobic Ultisol DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 2+ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOQ <LOQ <LOQ <L0Q <LOQ <L0D <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 0.018 0.014 0.017 0.017 0.017 0.017 0.018 0.018 0.021 0.021 0.019 0.019 0.010 0.018 0.016 0.014 93% 74% 89% 86% 88% 89% 94% 93% 109% 109% 96% 100% 52% 95% 84% 70% 0.018 0.018 0.018 0019 0.018 0.018 0.018 0.016 0.020 0.020 0.021 0.021 0.019 0.020 92% 91% 90% 97% 94% 92% 93% 80% 104% 102% 110% 109% 96% 104% LOD = lim it o f detection (0.0002 pmol/kg) LOQ = lim it o f quantitation (0.0039 pmol/kg) Friday, October 12,2007 Page l e f t Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -281 - p. 282 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 112E-108,109,110 Measured Concentrations of PFDA (junoL/kg) in Untreated and Fortified Soils Soil Type Sample Interval Untreated Controls Aerobic Anaerobic Mollisol DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month? Month 12 Month IS Month 18 Month 24 <LOQ <LOQ <LOD <LOD CLOD CLOD cLOQ cLOQ CLOD CLOD cLOD CLOD <LOD cLOD cLOQ cLOQ CLOD CLOD cLOD CLOD cLOQ CLOQ CLOQ cLOQ CLOD CLOD CLOD cLOD CLOD CLOD CLOD cLOD CLOD cLOD CLOD LGD = limit of detection (0.0002 pmol/kg) LOQ = limit of quantitation (0.0039 unol/kg) Fortified Recoveries Aerobic Anaerobic 0.019 0.019 0.019 0.020 0.019 0.020 0.019 0.016 0.019 0.019 0.023 0.021 0.024 0.022 0.018 0.020 0.015 0.016 100% 100% 98% 104% 97% 101% 98% 81% 99% 97% 117% 109% 121% 112% 92% 102% 76% 80% 0.018 0.019 0.016 0.018 0.018 0.018 0.017 0.018 0.020 0.018 0.022 0.024 0.022 0.021 92% 99% 82% 95% 92% 93% 90% 90% 104% 92% 114% 121% 112% 109% Friday, O ctober 12, 2007 Page 2 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -282- p. 283 Project No.: 112E-108 Wildlife International, Ltd. P roject N um bers 1 12E -108,109,110 Measured Concentrations of PFDA (jnnol/kg) in Untreated and Fortified Soils Soil Type Sample Interval Untreated Controls Aerobic Anaerobic Alfisol Day 0 Week 1 Week 2 Wed; 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOQ CLOD CLOD CLOD CLOD LOD = limit of detection (0.0002 ^imol/kg) LOQ = limit of quantitation (0.0039 jimol/kg) cLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD cLOD CLOD CLOD CLOQ Fortified Recoveries Aerobic Anaerobic 0.018 0.018 0.018 0.021 0.020 0.017 0.018 0.020 0.023 0.022 0.018 0.021 0.021 0.022 0.021 0.026 0.018 0.018 93% 93% 94% 110% 101% 86% 90% 105% 119% 112% 93% 109% 107% 112% 109% 133% 92% 93% 0.018 0.014 0.017 0.018 0.018 0.019 0.019 0.019 0.022 0.022 0.018 0.019 0.023 0.017 92% 74% 87% 93% 90% 95% 97% 96% 113% 114% 90% 96% 116% 86% Friday, O ctober 12, 2007 Page 3 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -283 - p. 284 Project No.: 112E-108 Wildlife InternationalLtd. P ro ject N um bers 112E -108,109,110 Measured Concentrations of PFDA (funol/kg) in Untreated and Fortified Soils Soil Type Sample Interval Untreated Controls Aerobic Anaerobic Incentisol Day 6 Weekl Week 2 Week 4 Month. 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOQ <LOQ LOD = limit of detection (0.0002 pmol/kg) LOQ = limit of quantitation (0.0039 pmol/kg) <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ Fortified Recoveries Aerobic Anaerobic 0.027 0.024 0.028 0.023 0.022 0.022 0.024 0.022 0.023 0.026 0.027 0.021 0.021 0.018 0.025 0.021 0.018 0.018 139% 124% 146% 116% 113% 116% 121% 115% 120% 133% 141% 108% 107% 92% 128% 109% 95% 92% 0.019 0.019 0.021 0.019 0.021 0.020 0.020 0.021 0.023 0.024 0.021 0.023 0.019 0.021 99% 97% 107% 96% 108% 105% 101% 107% 118% 122% 108% 116% 96% 106% Friday, O ctober 12, 2007 Page 4 o f 4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -284- p. 285 Project No.: 112E-108 Wildlife International, Ltd. P roject N um bers 112E -108,109,110 Measured Concentrations of PFUA (punol/kg) in Untreated and Fortified Soils Sample Untreated Controls Fortified Recoveries Soil Type________ Interval______ Aerobic Anaerobic_____ Aerobic______ Anaerobic UWsoI Day 0 Week 1 Week 2 Week 4 Mouth. 2 Month. 4 Month6 Month 9 Month 12 Month 15 Month IS Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <L0Q <LOQ <LOQ <LOQ <LOQ <L0Q <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOD <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <L0Q <L0Q <LOQ 0.015 0.012 0.015 0.014 0.013 0.014 0.015 0.013 0.018 0.018 0.016 0.017 0.007 0.015 0.013 0.011 85% 69% 82% 82% 76% 78% 86% 74% 102% 101% 92% 93% 41% 84% 72% 62% 0.015 0.016 0.015 0.015 0.016 0.015 0.016 0.012 0.017 0.017 0.017 0.017 0.016 0.018 85% 88% 85% 84% 88% 86% 91% 70% 98% 95% 94% 95% 88% 99% LOD = limit of detection (0.0002 j^mol/kg) LOO = limit of quantitation (0.0036 fimol/kg) Triday, O ctober 22, 2007 Page 1 o f4 Company Sanitized. Does not contain TSCA CBI. .W ildlife International, L td -285 - p. 286 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 1 1 2 E -1 0 8 , 109,110 Measured Concentrations of PFUA (punol/kg) in Untreated and Fortified Soils Soil Type Sample Interval Untreated Controls Aerobic Anaerobic Mollisol DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOD CLOD <LOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD <LOQ <LOQ <LOQ cLOQ CLOD <LOD <LOD <LOD CLOD cLOQ CLOQ cLOQ cLOD CLOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD LOD = limit of detection (0.0002 funol/kg) LOQ = limit of quantitation (0.0036 pmol/kg) Fortified Recoveries Aerobic Anaerobic 0.017 0.017 0.015 0.017 0.016 0.016 0.015 0.012 0.015 0.015 0.018 0.018 0.017 0.015 0.013 0.016 0.011 0.011 95% 96% 87% 93% 90% 92% 87% 69% 84% 84% 101% 101% 95% 87% 74% 88% 61% 63% 0.015 0.015 0.012 0.014 0.011 0.013 0.011 0.014 0.015 0.013 0.017 0.017 0.017 0.014 82% 86% 67% 76% 63% 71% 63% 80% 85% 75% 96% 94% 98% 79% ,Friday O ctober 12, 2007 Page 2 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. - 286- p. 287 Project No.: 112E-108 Wildlife International, Ltd. Project N um bers 1123-108,109,110 Measured Concentrations of PFUA (pmol/kg) in Untreated and Fortified Soils Sample Soil Type________ Interval Untreated Controls Fortified Recoveries Aerobic Anaerobic_____ Aerobic______ Anaerobic Alfisol DayO Week 1 Week 2 Week 4 Month. 2 Month4 Month 6 Month 9 Month 12 Month IS Month 18 Month 24 <LOD <LOD <L0D CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOQ CLOQ CLOD <LOD CLOD CLOD CLOD CLOD cLOD cLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOQ CLOQ 0.016 0.016 0.016 0.019 0.017 0.014 0.014 0.017 0.018 0.017 0.013 0.016 0.016 0.016 0.015 0.022 0.016 0.016 92% 87% 92% 109% 94% 80% 77% 94% 103% 97% 73% 89% 89% 93% 86% 122% 87% 88% 0.015 0.011 0.015 0.015 0.014 0.014 0.012 0.013 0.016 0.017 0.013 0.013 0.017 0.012 83% 61% 83% 86% 79% 79% 70% 76% 88% 99% 74% 72% 95% 67% LOD --limit of detection (0.0002 umol/kg) LOQ = limit of quantitation (0.0036 pmol/kg) Friday, O ctober 12, 2007 Page 3 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -287- p. 288 Project No.: 112E-108 Wildlife International, ltd . P ro ject N u m b ers 112E -108,109,110 Measured Concentrations of PFUA (p.mol/kg) in Untreated and Fortified Soils Soil Type Sample Interval Untreated Controls Aerobic Anaerobic InceDtisol Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOQ <LOQ <LOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD <LOD CLOD cLOQ <LOQ cLOQ <LOQ CLOQ CLOQ CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOQ cLO Q LOD limit of detection (0.0002 pmol/kg) LOQ = limit of quantitation (0.0036 pmol/kg) Fortified Recoveries Aerobic Anaerobic 0.021 0.020 0.022 0.018 0.016 0.018 0.017 0.016 0.018 0.021 0.022 0.016 0.014 0.015 0.018 0.015 0.013 0.012 120% 112% 125% 101% 92% 103% 98% 89% 104% 117% 122% 88% 82% 83% 99% 82% 74% 69% 0.014 0.013 0.014 0.013 0.013 0.015 0.014 0.015 0.015 0.018 0.012 0.013 0.012 0.015 79% 74% 79% 74% 74% 87% 80% 85% 87% 103% 69% 73% 70% 85% >Friday O ctober 12, 2007 Page 4 o f4 Company Sanitized. Does not contain TSCA CBi. W ildlife International, Ltd. -288 - p. 289 Project No.: 112E-108 Wildlife InternationalLtd. Project Numbers 112B-108,109,110 Measured Concentrations of 8-2 FTOH (jtmol/kg) in Untreated and Fortified Soils Sample Untreated Controls Fortified Recoveries Soil Type________ Interval______ Aerobic Anaerobic_____ Aerobic______ Anaerobic Uhisol Dayo Week 1 Week 2 Week 4 Montk 2 Month 4 Month 6 Month 9 Month 12 Month IS Month 18 Month 24 <LOD <LOD <LOD <LOD <LOD CLOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD 0.622 0.609 0.525 0.531 0.452 0.448 0.356 0.317 0.220 CLOQ cLOQ CLOQ CLOQ CLOQ CLOQ CLOQ cLOQ CLOQ 115% 113% 97% 99% 84% 83% 66% 59% 41% 39% 18% 21% 16% 9% 9% 0% 0% 0% 0.627 0.621 0.475 0.555 116% 115% 88% 103% 0.536 0.390 0.385 0.334 0.356 0.253 CLOQ CLOQ cLOQ 99% 72% 71% 62% 66% 47% 35% 22% 27% LOD = limit o f detection (0.048 pmol/kg) LOQ = limit ofquantitation (0.216 pmol/kg) M onday, O ctober 25, 2007 Page 1 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -289 - p. 290 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 112E-108,109,110 Measured Concentrations of 8-2 FTOH (pmol/kg) in Untreated and Fortified Soils Sample Untreated Controls Fortified Recoveries Soil Type________ Interval_______Aerobic Anaerobic_____ Aerobic______ Anaerobic MoDisol Da? 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month IS Month IS Month 24 <LOD <LOD <LOD <LOD CLOD CLOD CLOD CLOD CLOD <LOD CLOD CLOD CLOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD CLOD CLOD 0.645 0.562 0.459 0.469 0.419 0.241 0.256 cLOQ cLOQ cLOQ CLOQ cLOQ cLOQ CLOQ cLOQ cLOQ CLOQ 120% 104% 85% 87% 78% 45% 48% 21% 25% 7% 13% 3% 4% 0% 3% 0% 0% 0.574 0.602 0.526 0.589 0.554 0.524 0.412 0.413 CLOQ 0.349 cLOQ cLOQ cLOQ CLOQ 106% 112% 98% 109% 103% 97% 77% 77% 40% 65% 28% 18% 14% 6% LOD = limit of detection (0.048 pmol/kg) L O Q = lim it o f quantitation (0.216 pm ol/kg) M onday, O ctober IS , 2007 Page 2 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -290- p. 291 Project No.: 112E-108 Wildlife International, Ltd. ProjectNumbersll2E-108,109,110 Measured Concentrations of 8-2 FTOH (junol/kg) in Untreated and Fortified Soils Sam ple Untreated Controls F ortified R ecoveries S o il Type__________ In terval________ A erobic A naerobic______ A erobic_______ A naerobic Alfisol DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOD <LOD CLOD <LOD CLOD <LOD CLOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD cLOD CLOD CLOD CLOD cLOD CLOD cLOD CLOD CLOD CLOD CLOD cLOD CLOD <LOD CLOD CLOD CLOD CLOD CLOD CLOD CLOD 0.662 0.527 0.453 0.309 0.336 0.307 0.252 0.241 cLOQ <LOQ cLOQ CLOQ cLOQ CLOQ cLOQ CLOQ cLOQ CLOQ 123% 98% 84% 57% 62% 57% 47% 45% 30% 32% 22% 21% 5% 12% 4% 7% 0% 0% 0.574 0.548 0.462 0.437 0.441 0.347 0.274 0.308 CLOQ cLOQ cLOQ CLOQ cLOQ CLOQ 107% 102% 86% 81% 82% 64% 51% 57% 33% 25% 20% 15% 4% 7% LOD = limit of detection (0.048 pmol/kg) LOQ = limit ofquantitation (0.216 pmol/kg) M onday, October IS , 2007 Page 3 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -291 - p. 292 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 1123-108,109,110 Measured Concentrations of 8-2 FTOH (junol/kg) in Untreated and Fortified Soils Sample Untreated Controls Fortified Recoveries Soil Type________ Interval______ Aerobic Anaerobic_____ Aerobic______ Anaerobic Incentisol Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 <LOD <LOD <LOD CLOD CLOD CLOD CLOD CLOD <LOD CLOD cLOD <LOD cLOD cLOD cLOD CLOD CLOD CLOD CLOD cLOD CLOD LOD = limit of detection (0.048 pmol/kg) LOQ = limit of quantitation (0.216 pmol/kg) CLOD CLOD CLOD CLOD CLOD CLOD cLOD <LOD CLOD CLOD CLOD CLOD cLOD CLOD 0.613 0.565 0.575 0.613 0.529 0.505 0.470 0.612 0.434 0.430 0.338 0.401 cLOQ cLOQ <LOQ 0.248 cLOQ cLOQ 114% 105% 107% 114% 98% 94% 87% 114% 81% 80% 63% 74% 34% 34% 22% 46% 0% 0% 0.619 0.613 0.555 0.560 0.511 0.507 0.495 0.471 0.289 0.356 0.228 0.228 cLOQ CLOQ 115% 114% 103% 104% 95% 94% 92% 87% 54% 66% 42% 42% 17% 15% M onday, O ctober 15, 2007 Page 4 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -292 - p. 293 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers m E - ,1 0 8 1 0 9 ,1 1 0 Measured Concentrations of 8-2 FTOH (jimoI/L) in Headspace Gases from Untreated and Fortified Soils Sam ple Untreated C ontrols F ortified S oils S o il Type__________ In terva l______ A erobic A naerobic_______A ero b ic A naerobic Ultisol DayO Week 1 Week 2 Week4 Month.2 Month4 Month 6 Month 9 Month 12 Month 15 Month IS Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOQ = limit of quantitation (0.027 jimol/L ofheadspace) M onday, O ctober IS , 2007 P agel o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -293 - p. 294 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 112E-108,109,110 Measured Concentrations of 8-2 FTOH (pmol/L) in Headspace Gases from Untreated and Fortified Soils S oil Type Sam ple In terval U ntreated C ontrols A erobic A naerobic Mollisol DayO Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month IS Month IS Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOQ = limit of quantitation (0.027 pmoVL ofheadspace) F ortified S oils A erobic A naerobic <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ M onday, O ctober 15, 2007 Page2 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -294- p. 295 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 11 2 E-108,109,110 Measured Concentrations of 8-2 FTOH (junol/L) in Headspace Gases from Untreated and Fortified Soils S oil Type Sam ple In terval U ntreated C ontrols A erobic A naerobic Alfisol Day 0 Week 1 . Week2 Week4 Month2 Month 4 Month 6 Month 9 Month 12 Month 15 Month IS Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ , <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ ` LOQ = limit of quantitation (0.027 pmol/L ofheadspace) F ortified S oils A erobic A naerobic <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ . <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ - M onday, October IS , 2007 Page 3 o f4 Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. -295- p. 296 Project No.: 112E-108 Wildlife International, Ltd. Project Numbers 112E-108,109,110 Measured Concentrations of 8-2 FTOH (pmol/L) in Headspace Gases from Untreated and Fortified Soils S oil Type Sam ple In terval U ntreated C ontrols A erobic A naerobic Incentisol Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month IS Month 24 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ LOQ = limit of quantitation (0.027 pmol/L of headspace) F ortified S o ils A erobic A naerobic <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ M onday, O ctober 15, 2007 Pap: 4 o f4 p. 297 Company Sanitized. Does not contain TSCA CB1. .W ildlife International, Ltd Project No.: 112E-108 -296- Appendix III Example Calculations Standard Curves by Linear Regression Standard curves were prepared by plotting the ratio of analyte concentration (pg/L ng/mL) o f 8-2 FTOH, 8-2 FTA, 8-2 FTUA, PFOA, PFNA, PFDA, PFUA, 7-2 sFTOH and 7-3 Acid to the internal standard concentration (0.75 ng/mL 2-13C PFOA for 8-2 FTA, 8-2 FTUA, PFOA, PFNA, PFDA, PFUA and 7-3 Acid and 100 ng/mL HDFD for 8-2 FTOH and 7-2 sFTOH) in solutions with known concentrations on the abscissa and the respective peak area responses on the ordinate. Weighted regression (1/x) was applied to analysis of the data to determine the equation with respect to the abscissa as shown below: A = [ m x ( C / Q ) + b] x A; where A = Ai = m C= Ci = b= analyte area internal standard area slope analyte concentration (ng/mL) internal standard concentration (ng/mL) intercept Concentrations o f analytes in the final solutions of processed samples, just prior to injection, were calculated using a rearrangement o f the above equation: c _ C, x (AJAj) - b m Residue Concentrations of 8-2 FTOH. 8-2 FTA. 8-2 FTUA. PFOA. PFNA. PFDA. PFUA, 7-2 sFTOH and 7-3 Acid in Soil Extracts Residue concentrations (pg/kg) of 8-2 FTOH, 8-2 FTA, 8-2 FTUA, PFOA, PFNA, PFDA, PFUA, 7-2 sFTOH and 7-3 Acid in soil extracts were determined using the following equation: Sample Concentration in pg/kg = (V ^ where C = Concentration (ng/mL) as determined above Ve = Extraction volume (125 mL) V;i = First initial volume (mL) Vi2 = Second initial volume (if required) Vf, = First final volume (mL) Vf2 = Second final volume (mL) W = Weight of sample (25 g dry weight). Company Sanitized. Does not contain TSCA CBI. W ildlife International, Ltd. p. 298 project n o : 112E-108 -297 - Residue concentrations (pmol/kg) of 8-2 FTOH, 8-2 FTA, 8-2 FTUA, PFOA, PFNA, PFDA, PFUA, 7-2 sFTOH and 7-3 Acid in soil extracts were determined using the following equation: Sample Concentration in pmol/kg = C x molecular weight (pmol/pg) where C = Sample concentration (pg/kg) as determined above C. Procedural Recoveries in Fortified Controls Procedural recoveries were calculated for fortified control samples prepared in each test condition at known concentrations in 8-2 FTOH (250 pg/kg), 8-2 FTA (10.00 pg/kg), 8-2 FTUA (10.00 pg/kg), PFOA (10.00 pg/kg), PFNA (10.00 pg/kg), PFDA (10.00 pg/kg) and PFUA (10.00 pg/kg). Percent recoveries of the each analyte were determined to provide confirmation that the method was performing adequately. Percent recoveries were determined by dividing the concentration of the analyte recovered in the fortified sample by the nominal concentration added as shown below: Percent Recovery = gg/kgFoun^ x i 00% pg/kg Added be* oO Company Sanitized. Does not contain TSCA CBI. .W ildlife International, Ltd Sampling Interval Day 0 Week 1 Week 2 Week 4 Month 2 Month 4 Month 6 Month 9 Month 12 Month 15 Month 18 Month 24 -2 9 8 - Appendix IV Duration of Incubation Actual Days of Incubation Alfisol 0 7 14 28 63 119 182 273 365 462 546 728 Inceptisol 0 7 14 28 63 119 182 . 273 365 462 546 728 Ultisol 0 7 14 28 56 119 182 273 364 462 553 728 p. 299 Project No.: 112E-108 Mollisol 0 7 14 28 56 119 182 273 364 462 553 728 C o m p a n y Sanitized