Document v6pO2zEV0KYJRaxwQzQXV1j7Y

Jean B. Sweeney Vice President 3M Environmental, Health and Safety Operations 3M Center, Building 0 2 2 4-0 5 % -(l3 St. Paul, MN 55144-1000 651 737 3569 November 9, 2009 C E R T IF IE D M A IL NOCBI Document Processing Center EPA East - Room 6428 Attn: Section 8(e) Office of Pollution Prevention and Toxics, U.S. EPA 1200 Pennsylvania Avenue NW Washington, DC 20460-0001 :r: Re: TSCA 8(e) Substantial Risk Notice: Sulfonate-based and Carboxylic-based Fluorochemicals, Docket 8EHQ-0598-373 - Results from 2009 Analyses of Fish and Surface Water from the Mississippi River Dear Sir or Madam: 3M is submitting this notice to supplement previous submissions on sulfonyl and carboxylicbased fluorochemicals (FCs), and more specifically our June 20, 2006 submittal concerning fish data generated by the Minnesota Pollution Control Agency (MPCA). 3M is providing analytical summary sheets recently received from the MPCA and final analytical reports for a subset of sample analyses generated by the 3M Environmental Laboratory. These documents pertain to a fish and surface water sampling program conducted by the MPCA for Pool 2 of the Mississippi River in 2009. The following summarizes key aspects of the state-directed study: The study was designed to be representative of the entirety of Pool 2 from Lock and Dam No. 1 (RM 847.6) to Lock and Dam No. 2 (RM 815.2). For this study, Pool 2 was divided into four distinct reaches. These are generally identified as Reaches 1-4. Fish sampling was conducted by the Minnesota Department of Natural Resources. These samples were apparently collected in a late May - early June 2009 timeframe. Water sampling was coordinated by the MPCA. 3M provided a contractor (Pace Analytical) to assist in this effort. Surface water samples were collected on July 8, 2009. Three locations within each of the four reaches were sampled. These were numbered sequentially Location 1 through Location 12. Five fish species were evaluated: bluegill sunfish, smallmouth bass, common carp, white bass and freshwater drum. Nominally fifteen fish of each species were collected from each of the four reaches. The total number of fish collected was 297. For analytical validation purposes, approximately 10 percent of the fish samples and all twelve of the water samples were split with 3M. Analytes included: C4-C12 perfluorocarboxylates; C4, C6 and C8 perfluorosulfonates; and perfluorooctanesulfonamide. Study results are summarized in the following documents that have been copied to the enclosed CD: P-2 An Excel file, provided to 3M by the MPCA, entitled "Miss R POOL 2 JULY 2009 water sampling.xls". This file contains the surface water data generated by the contract laboratory hired by the MPCA for this work. An Excel file, provided to 3M by the MPCA, entitled "PFCs MissPool2 Fish all years.xls". This file contains fish data from the 2009 study that is the subject of this submittal, in addition to data previously obtained by the MPCA. In this spreadsheet, the aforementioned reaches are identified as "UM- 8-1" through UM- 8-4". 3M Environmental Laboratory Report No. E09-0365, Fluorochemical Characterization of Surface Water Samples, Mississippi River - Pool 2; July 2009. This report contains results for split samples corresponding to the MPCA surface water sampling Excel spreadsheet (noted above). 3M Environmental Laboratory Report No. E09-0372, Fluorochemical Analysis of Fish Fillet FJomogenates Collected from the Mississippi River by the Minnesota Pollution Control Agency May 2009 - Phase 1: PFOS. In this report, the aforementioned reaches are referred to as "Section 1" through "Section 4". This report contains results for split samples corresponding to a 10% subset of the data contained in the MPCA fish sampling Excel spreadsheet (noted above). Sample identification numbers in the two documents can be cross-referenced to compare split sample results. A 3MProject Summary report, prepared by Pace Analytical to document the field work associated with 3M Environmental Laboratory Report No. E09-0365. Of note, this report contains several maps, provided by the MPCA, intended to document the various study sampling locations. As this was a state-directed study, 3M is not in a position to provide specific information on sampling rationale(s), field sampling procedures pertaining to fish collection, specific fish sample locations, or on analytical techniques, data quality objectives*, or Quality Assurance/Quality Control outcomes, for the MPCA-generated data. While 3M does not believe that any of these data taken alone or cumulatively meet the "substantial risk" reporting threshold, and 3M was not responsible for the generation of this information (other than the 3M analytical data provided here), we nevertheless recognize the ongoing work by U.S. EPA to assess fluorochemical exposure pathways. Therefore, we are placing these results in the 8(e) docket as a supplement to previous submissions. If you have any questions, please do not hesitate to contact Deanna Luebker at 651-737-1374 or djluebker@mmm.com. Sincerely, Jean B. Sweeney Vice President Environmental, Health and Safety Operations Enclosure qualified samples (coded as "E" for estimated) sample PFC____________________ 090068 PFBA 090122 ALL 090139 PFOSA 090141 PFOSA 090142 PFOSA 090151 PFBA 090197 PFOSA 090203 PFOSA 090215 PFOSA 090219 PFOSA 090220 PFOSA 090222 PFOSA 090223 PFOSA 090227 PFOA 090229 PFOA 090231 PFOA 090233 PFOA 090234 PFOA 090236 PFOA, PFHxS, PFOSA 090237 PFOA, PFHxS 090247 PFOS, PFOSA 041315 041316 041317 051128 051129 051130 051131 051132 051133 051134 051135 051136 051137 051138 051139 051140 051141 051142 051143 051144 051145 051146 051147 051148 062158 062159 062160 062161 062162 062163 062164 062165 062166 062167 062168 062169 062171 062172 062173 062174 062175 062176 062177 062178 062180 062181 062183 062184 062185 062186 062187 MISSISSIPPI R. MISSISSIPPI R. MISSISSIPPI R. MISSISSIPPI R. MISSISSIPPI R. MISSISSIPPI R. MISSISSIPPI R. MISSISSIPPI R. MISSISSIPPI R. MISSISSIPPI R. MISSISSIPPI R. MISSISSIPPI R. MISSISSIPPI R. 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MISSISSIPPI R. allfish J o rm a t_ 2 0 0 9 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Page 7 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-3 UM- 8-3 UM- 8-3 UM- 8-3 UM- 8-3 UM- 8-3 UM- 8-3 UM- 8-3 UM- 8-3 UM- 8-3 UM- 8-3 UM- 8-3 UM- 8-3 UM- 8-3 UM- 8-3 UM- 8-3 UM- 8-3 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-4 UM- 8-1 UM- 8-1 p. 10 090291 090292 090293 090294 090295 090296 090297 MISSISSIPPI R. MISSISSIPPI R. MISSISSIPPI R. MISSISSIPPI R. MISSISSIPPI R. MISSISSIPPI R. MISSISSIPPI R. allfish Jormat_2009 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 Pool 2 p. 11 UM- 8-1 U M - 8-1 UM- 8-1 UM- 8-1 UM- 8-1 UM- 8-1 UM- 8-1 Page 8 allfish_format_2009 CTY AREA 20040831 SMB 20040831 SMB 20040831 WHB 20051003 WE 20051003 WE 20051003 WE 20051003 WE 20051003 C 20051003 C 20051003 C 20051003 C 20051003 C 20051003 SMB 20051003 SMB 20051003 SMB 20051003 SMB 20051003 SMB 20051003 SMB 20051003 WHB 20051003 WHB 20051003 WHB 20051003 WHB 20051003 WHB 20051003 SMB 200608xx CHC 200608xx CHC 200608xx CHC 200608xx CHC 200608xx CHC 200608xx SMB 200608xx SMB 200608xx SMB 200608xx SMB 200608xx SMB 200608xx BGS 200608xx BGS 200608xx CHC 200608xx CHC 200608xx CHC 200608xx CHC 200608xx CHC 200608xx SMB 200608xx SMB 200608xx SMB 200608xx BGS 200608xx BGS 200608xx CHC 200608xx CHC 200608xx CHC 200608xx CHC 200608xx CHC FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK Page 9 1 15.5 1 10.5 4 14.5 1 27.55906 1 21.25984 1 19.29134 1 27.55906 1 20.86614 1 21.65354 1 22.44094 1 24.01575 1 24.40945 1 10.23622 1 10.23622 1 8.661417 1 11.02362 1 8.661417 1 10.23622 1 12.20472 1 14.56693 1 12.59843 1 9.448819 1 14.96063 1 19.29134 1 29.52756 1 27.55906 1 21.25984 1 25.98425 1 22.12598 1 15.23622 1 12.59843 1 9.094488 1 8.976378 1 9.055118 1 7.086614 1 6.102362 1 24.6063 1 25.19685 1 27.55906 1 29.92126 1 25.19685 1 6.299213 1 8.937008 1 8.740157 1 5.708661 1 5.905512 1 22.04724 1 26.37795 1 26.77165 1 26.45669 1 24.40945 P - 12 allfsh_format_2009 200608XX SMB 200608XX SMB 200608XX SMB 200608XX BGS 200608XX BGS 20080609 BGS 20080609 BGS 20080609 BGS 20080609 BGS 20080609 BGS 20080609 BKS 20080609 SAG 20080609 SAG 20080609 SMB 20080609 SMB 20080609 SMB 20080609 SMB 20080609 SMB 20080609 WE 20080609 WE 20080609 WE 20080609 WE 62 RM 844-84 20090528 FWD 62 RM 844-84 20090528 FWD 62 RM 844-84 20090528 FWD 62 RM 844-84 20090528 FWD 62 RM 844-84 20090528 FWD 62 RM 844-84 20090528 FWD 62 RM 844-84 20090528 FWD 62 RM 844-84 20090528 FWD 62 RM 844-84 20090528 FWD 62 RM 844-84 20090528 FWD 62 RM 844-84 20090528 FWD 62 RM 844-84 20090528 FWD 62 RM 844-84 20090528 FWD 62 RM 844-84 20090528 FWD 62 RM 844-84 20090528 WHB 62 RM 844-84 20090528 WHB 62 RM 844-84 20090528 WHB 62 RM 844-84 20090528 WHB 62 RM 844-84 20090528 WHB 62 RM 844-84 20090528 WHB 62 RM 844-84 20090528 WHB 62 RM 844-84 20090528 WHB 62 RM 844-84 20090528 WHB 62 RM 844-84 20090528 WHB 62 RM 844-84 20090528 WHB 62 RM 844-84 20090528 WHB 62 RM 844-84 20090528 WHB 62 RM 844-84 20090528 WHB 62 RM 844-84 20090528 WHB 62 RM 844-84 20090528 SMB FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK Page 10 p. 13 1 8.661417 1 9.84252 1 9.448819 1 5.511811 1 5.472441 1 7.677165 1 7.480315 1 7.283465 1 7.480315 1 6.692913 1 11.02362 1 13.38583 1 18.11024 1 7.677165 1 8.661417 1 9.055118 1 8.858268 1 8.267717 1 20.47244 1 20.47244 1 9.448819 1 13.38583 1 13.0 1 13.8 1 13.4 1 14.2 1 14.2 1 15.0 1 18.1 1 14.6 1 13.0 1 12.6 1 13.0 1 11.0 1 13.4 1 14.4 1 12.6 1 11.0 1 13.4 1 12.6 1 13.8 1 14.2 1 14.6 1 12.2 1 12.6 1 12.2 1 12.6 1 13.8 1 13.4 1 14.6 1 14.6 1 15.0 62 RM 844-84 20090528 SMB 62 RM 844-84 20090528 SMB 62 RM 844-84 20090528 SMB 62 RM 844-84 20090528 SMB 62 RM 844-84 20090528 SMB 62 RM 844-84 20090528 SMB 62 RM 844-84 20090528 SMB 62 RM 844-84 20090528 SMB 62 RM 844-84 20090528 SMB 62 RM 844-84 20090528 SMB 62 RM 844-84 20090528 SMB 62 RM 844-84 20090528 SMB 62 RM 844-84 20090528 SMB 62 RM 844-84 20090528 SMB 62 RM 844-84 20090528 C 62 RM 844-84 20090528 C 62 RM 844-84 20090528 C 62 RM 844-84 20090528 C 62 RM 844-84 20090528 C 62 RM 844-84 20090528 C 62 RM 844-84 20090528 C 62 RM 844-84 20090528 C 62 RM 844-84 20090528 C 62 RM 844-84 20090528 C 62 RM 844-84 20090528 C 62 RM 844-84 20090528 C 62 RM 844-84 20090528 C 62 RM 844-84 20090528 C 62 RM 844-84 20090528 BGS 62 RM 844-84 20090528 BGS 62 RM 844-84 20090528 BGS 62 RM 836-84 20090529 WHB 62 RM 836-84 20090529 WHB 62 RM 836-84 20090529 WHB 62 RM 836-84 20090529 WHB 62 RM 836-84 20090529 WHB 62 RM 836-84 20090529 WHB 62 RM 836-84 20090529 WHB 62 RM 836-84 20090529 WHB 62 RM 836-84 20090529 WHB 62 RM 836-84 20090529 WHB 62 RM 836-84 20090529 WHB 62 RM 836-84 20090529 WHB 62 RM 836-84 20090529 WHB 62 RM 836-84 20090529 WHB 62 RM 836-84 20090529 WHB 62 RM 836-84 20090529 FWD 62 RM 836-84 20090529 FWD 62 RM 836-84 20090529 FWD 62 RM 836-84 20090529 FWD 62 RM 836-84 20090529 FWD 62 RM 836-84 20090529 FWD allfish_format__2009 FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK Page 11 p. 14 1 15.7 1 13.8 1 13.0 1 16.1 1 11.4 1 13.8 1 13.0 1 15.0 1 15.0 1 14.6 1 16.5 1 14.2 1 12.2 1 11.0 1 21.3 1 18.9 1 17.7 1 27.2 1 23.6 1 21.3 1 18.9 1 22.0 1 19.7 1 19.7 1 21.3 1 19.7 1 22.4 1 15.4 1 7.5 1 5.1 1 6.1 1 11.8 1 12.6 1 14.6 1 11.8 1 13.8 1 11.4 1 14.2 1 13.0 1 12.2 1 10.2 1 15.0 1 10.2 1 12.2 1 11.4 1 12.2 1 11.8 1 11.8 1 13.0 1 13.8 1 12.2 1 10.2 62 RM 836-84 20090529 FWD 62 RM 836-84 20090529 FWD 62 RM 836-84 20090529 FWD 62 RM 836-84 20090529 FWD 62 RM 836-84 20090529 FWD 62 RM 836-84 20090529 FWD 62 RM 836-84 20090529 FWD 62 RM 836-84 20090529 FWD 62 RM 836-84 20090529 FWD 62 RM 836-84 20090529 SMB 62 RM 836-84 20090529 SMB 62 RM 836-84 20090529 SMB 62 RM 836-84 20090529 SMB 62 RM 836-84 20090529 SMB 62 RM 836-84 20090529 SMB 62 RM 836-84 20090529 SMB 62 RM 836-84 20090529 SMB 62 RM 836-84 20090529 SMB 62 RM 836-84 20090529 SMB 62 RM 836-84 20090529 SMB 62 RM 836-84 20090529 SMB 62 RM 836-84 20090529 SMB 62 RM 836-84 20090529 SMB 62 RM 836-84 20090529 SMB 62 RM 836-84 20090529 BGS 62 RM 836-84 20090529 BGS 62 RM 836-84 20090529 BGS 62 RM 836-84 20090529 BGS 62 RM 836-84 20090529 BGS 62 RM 836-84 20090529 BGS 62 RM 836-84 20090529 BGS 62 RM 836-84 20090529 BGS 62 RM 836-84 20090529 BGS 62 RM 836-84 20090529 BGS 62 RM 836-84 20090529 BGS 62 RM 836-84 20090529 BGS 62 RM 836-84 20090529 BGS 62 RM 836-84 20090529 BGS 62 RM 836-84 20090529 BGS 62 RM 836-84 20090529 C 62 RM 836-84 20090529 C 62 RM 836-84 20090529 C 62 RM 836-84 20090529 C 62 RM 836-84 20090529 C 62 RM 836-84 20090529 C 62 RM 836-84 20090529 C 62 RM 836-84 20090529 C 62 RM 836-84 20090529 C 62 RM 836-84 20090529 C 62 RM 836-84 20090529 C 62 RM 836-84 20090529 C 62 RM 836-84 20090529 C allfish_format_2009 FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK Page 12 1 12.6 1 12.2 1 14.2 1 11.2 1 16.3 1 13.2 1 16.9 1 13.6 1 12.2 1 13.6 1 13.8 1 9.3 1 9.1 1 11.4 1 10.6 1 10.0 1 14.2 1 12.2 1 13.0 1 11.0 1 10.2 1 12.6 1 13.4 1 11.4 1 6.9 1 5.3 1 5.7 1 5.3 1 4.9 1 6.5 1 5.5 1 6.1 1 5.1 1 4.9 1 5.5 1 5.5 1 5.9 1 5.1 1 5.1 1 22.8 1 18.5 1 20.1 1 19.3 1 20.5 1 17.7 1 22.0 1 21.7 1 18.5 1 17.7 1 15.4 1 21.7 1 18.5 p. 15 62 RM 836-84 20090529 C 62 RM 836-84 20090529 C 62 RM 844-84 20090528 FWD 62 RM 833.5-i 20090529 WHB 62 RM 833.5-! 20090529 WHB 62 RM 833.5-! 20090529 WHB 62 RM 833.5-! 20090529 WHB 62 RM 833.5-! 20090529 WHB 62 RM 833.5-! 20090529 WHB 62 RM 833.5-! 20090529 WHB 62 RM 833.5-i 20090529 WHB 62 RM 833.5-i 20090529 WHB 62 RM 833.5-! 20090529 WHB 62 RM 833.5-! 20090529 WHB 62 RM 833.5-! 20090529 WHB 62 RM 833.5-i 20090529 WHB 62 RM 833.5-! 20090529 WHB 62 RM 833.5-i 20090529 WHB 19 RM 827-83 20090601 FWD 19 RM 827-83 20090601 FWD 19 RM 827-83 20090601 FWD 19 RM 827-83 20090601 FWD 19 RM 827-83 20090601 FWD 19 RM 827-83 20090601 FWD 19 RM 827-83 20090601 FWD 19 RM 827-83 20090601 FWD 19 RM 827-83 20090601 FWD 19 RM 827-83 20090601 FWD 19 RM 827-83 20090601 FWD 19 RM 827-83 20090601 FWD 19 RM 827-83 20090601 FWD 19 RM 827-83 20090601 FWD 19 RM 827-83 20090601 FWD 19 RM 827-83 20090601 SMB 19 RM 827-83 20090601 SMB 19 RM 827-83 20090601 SMB 19 RM 827-83 20090601 SMB 19 RM 827-83 20090601 SMB 19 RM 827-83 20090601 SMB 19 RM 827-83 20090601 SMB 19 RM 827-83 20090601 SMB 19 RM 827-83 20090601 SMB 19 RM 827-83 20090601 SMB 19 RM 827-83 20090601 SMB 19 RM 827-83 20090601 SMB 19 RM 827-83 20090601 SMB 19 RM 827-83 20090601 SMB 19 RM 827-83 20090601 SMB 62 RM 833.5-! 20090528 C 62 RM 833.5-! 20090528 C 62 RM 833.5-i 20090528 C 62 RM 833.5-I 20090528 C allfish_format_2009 FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK Page 13 1 20.5 1 21.7 1 13.0 1 13.8 1 13.0 1 14.2 1 13.0 1 14.2 1 12.6 1 13.4 1 13.8 1 14.2 1 13.8 1 11.8 1 14.6 1 13.0 1 11.8 1 12.2 1 13.0 1 11.8 1 16.1 1 13.4 1 14.2 1 14.2 1 12.6 1 12.2 1 13.4 1 13.2 1 12.8 1 13.0 1 13.0 1 10.6 1 14.0 1 9.4 1 12.2 1 14.2 1 11.0 1 11.0 1 9.8 1 10.2 1 15.0 1 9.8 1 12.6 1 12.6 1 9.8 1 10.2 1 13.4 1 10.2 1 18.5 1 21.3 1 22.0 1 15.0 p. 16 a llfish jo rm a t_ 2 0 0 9 62 RM 833.5-J 20090528 C 62 RM 833.5- 20090528 C 62 RM 833.5-! 20090528 C 62 RM 833.5-! 20090528 C 62 RM 833.5- 20090528 C 62 RM 833.5-! 20090528 C 62 RM 833.5-! 20090528 C 62 RM 833.5- 20090528 C 62 RM 833.5-! 20090528 C 62 RM 833.5-! 20090528 C 19 RM 815-82 20090601 BGS 19 RM 815-82 20090601 BGS 19 RM 815-82 20090601 BGS 19 RM 815-82 20090601 BGS 19 RM 815-82 20090601 BGS 19 RM 815-82 20090601 BGS 19 RM 815-82 20090601 BGS 19 RM 815-82 20090601 BGS 19 RM 815-82 20090601 BGS 19 RM 815-82 20090601 BGS 19 RM 815-82 20090601 BGS 19 RM 815-82 20090601 BGS 19 RM 815-82 20090601 BGS 19 RM 815-82 20090601 BGS 19 RM 815-82 20090601 BGS 19 RM 815-82 20090601 WHB 19 RM 815-82 20090601 WHB 19 RM 815-82 20090601 WHB 19 RM 815-82 20090601 WHB 19 RM 815-82 20090601 WHB 19 RM 815-82 20090601 WHB 19 RM 815-82 20090601 WHB 19 RM 815-82 20090601 WHB 19 RM 815-82 20090601 WHB 19 RM 815-82 20090601 WHB 19 RM 815-82 20090601 WHB 19 RM 815-82 20090601 WHB 19 RM 815-82 20090601 WHB 19 RM 815-82 20090601 WHB 19 RM 815-82 20090601 WHB 19 RM 815-82 20090601 FWD 19 RM 815-82 20090601 FWD 19 RM 815-82 20090601 FWD 19 RM 815-82 20090601 FWD 19 RM 815-82 20090601 FWD 19 RM 815-82 20090601 FWD 19 RM 815-82 20090601 FWD 19 RM 815-82 20090601 FWD 19 RM 815-82 20090601 FWD 19 RM 815-82 20090601 FWD 19 RM 815-82 20090601 FWD 19 RM 815-82 20090601 FWD FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK Page 14 1 23.6 1 18.5 1 15.0 1 23.2 1 19.3 1 18.1 1 22.0 1 19.3 1 15.7 1 15.7 1 6.1 1 3.9 1 4.9 1 6.9 1 6.9 1 5.9 1 6.7 1 5.5 1 4.3 1 5.9 1 6.7 1 3.9 1 5.1 1 5.3 1 6.7 1 13.8 1 13.4 1 12.6 1 12.2 1 14.6 1 13.8 1 11.8 1 12.6 1 12.2 1 14.2 1 14.6 1 11.0 1 13.4 1 13.4 1 14.2 1 11.0 1 13.6 1 14.2 1 10.6 1 13.2 1 15.4 1 13.0 1 12.2 1 12.0 1 15.4 1 14.6 1 14.6 p. 17 19 RM 815-82 20090601 FWD 19 RM 815-82 20090601 FWD 19 RM 815-82 20090601 FWD 19 RM 815-82 20090601 SMB 19 RM 815-82 20090601 SMB 19 RM 815-82 20090601 SMB 19 RM 815-82 20090601 SMB 19 RM 815-82 20090601 SMB 19 RM 815-82 20090601 SMB 19 RM 815-82 20090601 SMB 19 RM 815-82 20090601 SMB 19 RM 815-82 20090601 SMB 19 RM 815-82 20090601 SMB 19 RM 815-82 20090601 SMB 19 RM 815-82 20090601 SMB 19 RM 815-82 20090601 SMB 19 RM 815-82 20090601 SMB 19 RM 815-82 20090601 SMB 62 RM 833.5-! 20090528 BGS 62 RM 833.5-1 20090528 BGS 62 RM 833.5-1 20090528 BGS 62 RM 833.5-! 20090528 BGS 62 RM 833.5-! 20090528 BGS 62 RM 833.5-! 20090528 BGS 62 RM 833.5-! 20090528 BGS 62 RM 833.5-1 20090528 BGS 62 RM 833.5-! 20090528 BGS 62 RM 833.5-1 20090528 BGS 62 RM 833.5-1 20090528 BGS 62 RM 833.5-1 20090528 BGS 62 RM 833.5-! 20090528 BGS 62 RM 833.5-! 20090528 BGS 62 RM 833.5-i 20090528 BGS 62 RM 833.5-! 20090528 C 62 RM 833.5-! 20090528 C 19 RM 815-82 20090601 C 19 RM 815-82 20090601 C 19 RM 815-82 20090601 C 19 RM 815-82 20090601 C 19 RM 815-82 20090601 C 19 RM 815-82 20090601 C 19 RM 815-82 20090601 C 19 RM 815-82 20090601 C 19 RM 815-82 20090601 C 19 RM 815-82 20090601 C 19 RM 815-82 20090601 C 19 RM 815-82 20090601 C 19 RM 815-82 20090601 C 19 RM 815-82 20090601 C 19 RM 815-82 20090601 C 62 RM 844-84 20090528 BGS 62 RM 844-84 20090528 BGS allfish_format_2009 FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK FILSK Page 15 1 14.2 1 14.2 1 13.4 1 13.0 1 11.0 1 11.8 1 10.6 1 11.8 1 13.0 1 15.7 1 11.6 1 10.0 1 11.0 1 16.3 1 14.6 1 8.7 1 10.6 1 10.6 1 5.3 1 5.5 1 5.3 1 5.1 1 5.1 1 5.3 1 5.1 1 6.5 1 6.3 1 5.9 1 4.9 1 5.5 1 5.5 1 6.7 1 5.1 1 22.0 1 18.9 1 18.1 1 20.9 1 16.9 1 20.1 1 18.5 1 19.3 1 13.4 1 15.0 1 17.3 1 18.9 1 15.0 1 18.5 1 14.2 1 21.3 1 20.5 1 3.1 1 3.9 p. 18 62 RM 844-84 20090528 BGS 62 RM 844-84 20090528 BGS 62 RM 844-84 20090528 BGS 62 RM 844-84 20090528 BGS 62 RM 844-84 20090528 BGS 62 RM 844-84 20090528 BGS 62 RM 844-84 20090528 BGS allfish_format_2009 FILSK FILSK FILSK FILSK FILSK FILSK FILSK 1 3.9 1 3.9 1 3.7 1 3.7 1 3.1 1 3.7 1 3.1 p. 19 Page 16 WTKG LAT 3.275 1.079 1.23 3.125 1.771 2.532 2.416 4.675 5.175 0.285 0.252 0.165 0.303 0.135 0.215 0.416 0.78 0.441 0.219 0.665 2.633 4.5 2.8 1.75 2.5 1.75 0.692 0.454 0.178 0.162 0.166 0.155 0.092 2.25 2.5 3.25 3.5 3 0.063 0.175 0.175 0.065 0.075 2 2.5 3.25 3.25 2 allfish_format_2009 p. 20 LONG AGE SEX LIPPCJ PfOAPPBPFOACOD PFOSPPB 0.453 K 950 0.631 K 105 0.668 K 138 7M 0.581 K 13.1 3F 0.614 K 75.5 2F 0.591 K 180 7F 0.538 K 45.5 4M 1.24 347 5F 0.602 K 73.5 5M 0.59 K 175 6F 0.608 K 420 6F 0.605 K 66.4 5M 0.619 K 269 4M 0.596 K 336 4F 0.607 K 167 5M 0.615 K 158 4F 0.591 K 122 4F 0.578 K 156 2F 0.609 K 510 4F 0.6 K 102 2F 0.605 K 240 1F 1.17 1860 4F 0.602 K 83.6 F 0.605 K 374 0.5 K 2.97 0.5 K 2.34 0.5 K 4.02 0.5 K 9.08 0.5 K 11.7 0.948 178 0.972 89.8 0.856 19 0.796 53.2 0.904 45 NR 32.3 NR 30.3 0.5 K 8.54 0.5 K 95.2 0.5 K 5.6 0.5 K 6.18 0.5 K 10.7 NR 589 NR 110 NR 1320 NR 709 NR 59.7 0.622 69.2 0.5 K 11.7 1.16 2.86 1.71 42 1.34 7.74 Page 17 0.158 0.274 0.214 0.072 0.069 0.193 0.144 0.13 0.161 0.1003 0.292 0.346 0.876 0.103 0.149 0.187 0.162 0.137 1.264 1.599 0.03119 0.34 0.374 0.505 0.509 0.421 0.571 0.530 1.006 0.651 0.348 0.399 0.403 0.313 0.538 0.499 0.301 0.229 0.519 0.412 0.525 0.563 0.763 0.449 0.549 0.434 0.416 0.648 0.601 0.869 0.765 0.846 allfish_format_2009 3M 3F 3M 3F 3M 5M 5M 7F 3U 5F 5M 5F 4F 9M 9F 3U 5U 5J 5F 5J 6M 6M 7M 10 M 6F 5F 4F 5M 3F 5M 6M 3M 2M 4F 3M 4F 5M 6F 3F 3F 3M 3M 4F 4M 6F 6M 7M 0.34 0.4 0.4 0.59 0.51 0.32 2.42 3.28 0.52 0.47 0.5 0.37 0.61 1.87 2.6 0.73 0.75 1.1 1.89 2.78 0.71 0.37 0.76 1.87 0.55 0.96 2.25 0.61 1.08 0.81 4.24 0.81 0.86 1.78 3.15 2.4 3.49 3.83 3.55 3.24 1.01 1.08 2.03 3.59 4.77 0.95 1.21 NR NR NR NR NR 2.4 K 2.46 K 2.42 K 2.43 K 2.48 K 2.51 K 2.49 K 2.43 K 2.48 K 2.37 K 2.35 K 2.48 K 2.46 K 2.49 K 2.45 K 2.49 K 2.45 K 2.49 K 2.42 K 2.38 -, 2.48 K ' 2.46 K 2.5 2.46 K 2.44 K ' 2.48 K 2.45 K 2.5 K 2.48 K 2.45 K 2.4 2.48 K 2.48 K 2.36 K 2.5 K 2.44 K 2.45 K 2.43 K 2.39 K f 2.39 K 2.43 K 2.4 2.45 K 2.46 K ' 2.46 K 2.45 K,. 2.45 K . 290 5150 884 331 330 165 102 157 317 122 46 31 36.2 48.8 380 118 120 143 28.6 44.8 69.6 40.5 72.8 123 62.9 111 30.1 53.9 34 5.3 15.7 74 75.7 31 60 29.6 89.9 61.5 85.5 71.1 60.1 146 51.5 90.6 58.3 44.5 62.7 71 90.3 66.4 95.1 38.2 Page 18 0.968 0.667 0.527 1.072 0.406 0.727 0.568 0.873 1.023 0.805 1.189 0.712 0.548 0.352 2.074 1.781 1.176 4.268 2.393 1.980 1.447 2.467 1.760 1.883 2.106 1.690 2.186 0.719 0.160 0.049 0.075 0.440 0.486 0.760 0.362 0.819 0.342 0.744 0.633 0.430 0.290 0.779 0.239 0.482 0.310 0.393 0.368 0.376 0.402 0.496 0.329 0.201 allfish_format_2009 8M 7M 5M 9F 4F 6M 5M 7F 7M 7F 9M 7F 5F 3F 6M 5M 5M 9F 7M 6M 5M 6M 5M 5M 6M 5M 7M 4J 7F 3M 5M 3F 3F 5F 3F 4M 2F 5F 4F 3F 2F 6F 2F 3M 2F 3F 4F 4J 5F 5M 4M 2J 0.89 0.72 0.7 0.56 0.53 0.94 1 0.92 1.29 0.74 1.56 0.33 0.83 0.44 7.32 6.05 4.66 6.38 4.49 3.62 2.78 6 4.38 4.67 11.6 4.53 1.98 0.86 0.5 0.63 0.48 3.02 2.82 2.82 1.27 4.45 0.88 1.01 3.28 2.53 2.95 2.52 2.78 1.01 1.11 1.4 2.21 1.39 11.2 1.25 2.11 0.38 2.44 K 2.44 K 2.48 K 2.23 .. 2.48 K 2.49 K 2.39 K 2.34 K 2.34 K 2.42 K 2.48 K 2.48 K 2.36 K 2.46 K 2.39 K 2.37 K: 2.16 k 2.14 2.42 K V; 2.35 K 2.21 K , 2.26 K 2.37 K 2.16 K 2.15 K 2.5 K 2.46 K' 2.4 K 2.44 K 2.5 k:'- . 2.46 K 2.44 K 2.4 K 2.49 K 2.49 k 2.43 K 2.5 K 2.4 K 2.4 K 2.48 K , 2.43 K 2.5 K 2.44 K 2.42 K 2.42 K 2.45 K 2.46 k 2.44 K 2.39 K*':' -- 2.49 K 2.43 K 2.39 K 86.5 24.8 17.2 107 30.9 23.1 21.5 58.2 49.3 59.2 35.6 14.4 13.6 26.4 93.1 42.7 12.3 24.9 32.4 13.6 11.5 71.1 6.86 32 29.9 7.02 29.1 14.2 17.5 11.9 144 75.6 71.4 57.7 75.2 79.7 59.3 94.7 61.9 130 77.5 63.1 73.5 46.8 37.7 71.3 90.1 77.9 4.78 104 39.3 41.8 Page 19 0.400 0.316 0.550 0.335 0.755 0.484 1.302 0.561 0.405 0.689 0.750 0.164 0.196 0.374 0.292 0.222 0.642 0.468 0.573 0.438 0.256 0.513 0.662 0.358 0.118 0.052 0.066 0.043 0.042 0.099 0.061 0.059 0.051 0.048 0.061 0.084 0.076 0.046 0.056 2.365 1.502 1.704 1.439 1.922 1.073 2.455 2.427 1.693 1.023 0.883 2.488 1.538 allfish_format_2009 4F 4M 6M 3J 8M 5M 9F 5F 4M 6M 7F 2F 2M 4M 3M 3F 7M 5F 5M 3M 3F 5M 6M 4F 6F 3F 4F 3F 3J 6M 4M 5J 3M 3F 4F 4M 4M 3F 3F 7M 5F 5M 5M 6M 5M 6F 6M 5M 5F 4M 6M 5M 2.26 2.46 K 36.6 2.62 2.44 K 22.9 4.23 2.38 je 67.6 1.41 2.44 K 'i ' ' 52.3 2.78 2.48 K 71.8 2.77 2.43 K 38.8 0.61 2.39 , ' 4.78 1.6 2.46 K 64.4 1 2.34 19.1 1.04 2.46 K 39 1.13 2.44 K ' 30.2 0.28 2.36 K 12.6 0.54 2.36 K . ` 30.8 1.07 2.48 K - 22.5 0.7 2.49 K 13.3 0.36 2.42 K 14 0.8 ' 2.45 K 14.9 0.55 2.26 K - 19.2 0.81 2.49 K 59.6 0.93 2.29 K 30.6 WMII0.54 2.31 25 0.46 2.49 K 13.1 0.64 2.43 K 38.1 SpM0.47 2.25 25.1 I"0.41 2.51 K 0.6 2.37 -;; 46.5 25.9 0.34 2.38 K 24.6 0.37 2.51 K 45.4 1.31 2.39 K 55.9 0.42 2.38 K 30.3 0.57 2.49 K 44.1 0.61 2.46 K 44.1 0.53 2.48 K- 43.8 0.65 2.38 K 50.9 0.5 2.31 k : P - 37.8 0.49 2.5 K ' 47.9 0.62 2.26 K 36.4 0.61 2.34 K 18.6 0.59 2.42 K 55.4 2.73 2.4 K,E 41.8 4.09 2.44 K 19.2 2.95 2.36 K 32.3 3.66 2.49 K 26.1 2.48 2.5 K 12.4 3.25 2.45 K 15.1 2.63 2.3 K; 13.7 4.49 2.46 K , 11.1 4.59 2.19 K 16.6 1.15 2.35 K 4.69 2.2 2.49 K 5.57 8.04 2.49 K 10.8 1.2 2.38 K - 10.7 Page 20 1.705 2.872 0.340 0.615 0.587 0.639 0.435 0.617 0.516 0.541 0.611 0.809 0.597 0.418 0.748 0.552 0.369 0.430 0.459 0.297 0.925 0.495 0.461 0.537 0.383 0.353 0.478 0.457 0.335 0.448 0.400 0.273 0.530 0.191 0.432 0.673 0.299 0.358 0.235 0.251 0.833 0.269 0.445 0.511 0.229 0.255 0.560 0.327 1.560 2.208 2.178 0.652 allfish_format_2009 6F 6F 5J 4M 4F 5M 4F 5F 3M 4M 4F 5F 4F 3F 5M 4F 3M 3F 5F 4M 8F 5F 6F 6F 4F 4M 5F 5F 5F 5F 5F 3M F 2J 5M 7F 4F 4F 3M 3M 7F 3F 5M 5M 3F 3J 6F 3M 5M 6M 6M 4F 1.57 2.39 K 3.17 2.43 K 0.79 2.44 K 2.34 2.48 K 3.28 2.45 K 1.57 2.44 K 1.13 2.49 K 1.53 2.44 K 2.07 2.44 K 2.19 2.4 K 3.41 2.49 K 2.66 2.37 K 0.5 2.45 K 1.9 2.43 K 4.37 2.37 K 1.85 2.43 K 2.29 2.5 K 1.99 2.37 K 0.55 2.49 K 0.77 2.5 K 0.48 2.48 K 0.65 2.5 K 0.66 2.43 K 0.6 2.5 K 0.35 2.44 K 0.69 2.44 k 0.57 2.49 K 0.35 2.45 K 0.76 2.4 K 0.47 2.4 K 0.61 2.4 K 1.39 2.49 K 0.54 2.37 K 0.59 2.34 K 0.36 2.4 K 0.53 2.13 K 0.38 2.34 K 0.27 2.38 K 0.43 2.24 K 0.3 2.18 K 0.47 2.26 K 0.54 2.45 K 0.33 2.43 K 0.46 2.36 K 0.57 2.39 K 0.56 2.33 K 0.37 2.39 K 0.59 2.5 K 3.56 2.48 K 4.88 2.5 K 2.37 2.48 K 0.43 4.69 Page 21 4.78 12.9 46.3 105 61.6 71.2 69.6 73.9 114 90.2 57.6 111 63.1 68.9 106 60.6 85.9 101 106 137 63.3 38.8 57.9 31.8 27 45.7 103 99 57.5 104 11.4 92.4 98.3 44.9 52.6 30.8 32.6 27.9 46 37.6 60.3 70.3 60.9 111 37.1 49.3 25.9 48.6 52.3 25.7 10.2 27.1 2.734 1.379 0.824 2.452 1.822 1.684 2.199 1.659 1.032 0.968 0.095 0.021 0.039 0.134 0.148 0.077 0.114 0.060 0.031 0.079 0.131 0.020 0.047 0.063 0.089 0.514 0.539 0.389 0.394 0.684 0.614 0.363 0.364 0.423 0.620 0.704 0.233 0.535 0.645 0.621 0.391 0.519 0.608 0.375 0.510 0.791 0.430 0.365 0.344 0.788 0.669 0.714 a llfish jo rm a t_ 2 0 0 9 7M 5F 4F 7M 5M 5F 6M 5F 4M 4M 5M 2J 3J 6M 6M 4F 6M 4M 2F 4F 6F 2F 3J 3J 5M 4F 4F 2M 3F 5F 4F 3M 3F 3F 5M 5F 2F 4M 4F 6F 3M 5M 6F 3F 5M 8F 5F 4M 4F 8F 6F 6F 4.86 2.46 K 45.2 0.57 2.48 K 7.29 2.04 2.48 K 38.7 3.23 2.48 K 18.9 3.67 2.49 K 58.8 1.72 2.5 K 30.6 5.43 2.38 K 57.3 5.62 2.48 K 23.9 11.8 2.5 K 90.6 3.27 2.48 K 23.6 0.45 2.44 K 313 0.77 2.5 K 32.3 0.66 2.44 K 39.2 0.77 2.46 37.8 0.38 2.45 K 36.1 0.4 2.48 K - 451 0.38 2.49 K 399 0.76 2.24 K 53.1 2.2 K 84.8 0.98 2.19 K . 48.1 0.73 2.5 K 39.5 2.46 910 0.61 2.46 65.4 0.77 2.4 K 1350 0.81 2.5 K 42.3 1.17 2.46 IC 56.8 2.73 2.49 K 87.4 2.23 2.45 k 65.3 3.26 2.39 K 230 3.33 2.44 K 80.7 4.2 2.5 W m m 174 3.42 2.4 K 44 1.48 2.4 K 82 1.92 2.5 K 81.3 1.13 2.42 K 163 2.67 2.38 K . 128 2.57 2.46 K 764 1.05 2.48 K 171 2.98 2.5 K 88.1 3.06 2.44 k - 162 0.72 9.39 E 2850 1.55 2.48 K 49.8 1.8 12.6 E 997 0.91 9.19 441 0.88 6.88 E 1090 1.71 2.42 K 30.2 0.63 16.8 E 592 1.76 5.01 E 210 1.4 2.38 K 91.6 3.14 17.5 E 3580 1.24 27.6 E 632 0.41 2.46 K 29.8 Page 22 0.868 0.684 0.750 0.547 0.372 0.432 0.293 0.419 0.436 0.990 0.382 0.236 0.360 0.911 0.886 0.200 0.231 0.308 0.049 0.069 0.048 0.050 0.043 0.068 0.042 0.126 0.095 0.079 0.048 0.052 0.063 0.118 0.047 2.296 1.603 1.633 2.124 0.952 1.594 1.411 1.597 0.700 0.896 1.015 1.450 0.815 1.432 0.754 1.918 2.010 0.007 0.020 allfish_format_2009 6F 6J 5F 5F 3F 4F 3F 4M 5F 8F 4F 3F 4M 9F 7M 2M 3F 3J 3F 3M 3F 3F 3M 3F 3M 5M 5M 4F 2M 4J 4M 6M 3F 6M 5M 5F 6M 5M 6M 5F 5F 2M 2M 5F 5F 4M 6F 3J 6M 6F 1J 1J 0.76 1.62 1.79 0.44 0.49 0.38 0.48 0.4 0.4 0.46 0.34 0.28 0.39 0.54 0.3 0.67 0.22 1.01 0.34 0.44 0.47 0.86 0.47 0.86 0.72 1.16 0.36 0.98 0.85 0.52 0.26 0.72 1.01 4.99 3.77 4.29 3.97 3.24 3.21 0.79 2.66 2.67 2.09 0.77 3.26 2.54 6.92 1.28 0.95 11 N N 7.87 2.33 K ; 2.48 K 2.49 K 2.49 K 2.97 2.5 K 2.49 K 2.5 K 2.35 K 2.46 - 2.37 K 2.43 K 2.46 K 2.49 K 2.48 K 2.48 K 2.4 2.46 K 2.46 K 2.46 k `: 2.44 k 2.49 K ' 2.51 K 2.37 K 2.5 k 2.46 K 2.48 K 2.48 k 2.44 K. 2.37 K 2.39 K 2.43 K 2.48 K 2.49 K 2.37 K" 2.49 K 12.1 2.35 K- 4.2 2 .24#--' 2.34 K- 2.44 K 2.42 K 2.26 K 2.43 K . 2.33 K 2.12 # < `! V ; V 2.21 K : v - 2.45 K 2.5 K 2.49 K 401 67.6 24.2 436 76.5 561 495 259 42 612 52.1 92.8 219 71.7 521 98.6 210 153 155 34 55.9 71.3 80.7 143 74.6 204 84.4 37.6 63.6 201 94.6 82.3 105 65.5 53.3 8.68 130 1340 52.6 283 874 27.1 56.4 19.6 58.6 117 86.9 37.9 106 158 16.8 10.5 Page 23 0.018 0.021 0.013 0.016 0.007 0.013 0.009 ailfish_format_2009 1J 1J 1J 1J 1J 1J 1J N 2.5 K N 2.49 K N 2.46 K N 2.5 K N 2.58 K N 2.48 k N 2.49 K p. 27 9.14 9.21 8.31 11.5 11.3 13.9 18.1 Page 24 allfish_format_2009 MPCAMiss R Pool2-SMB #i fillet L7474-38 (A) MPCAMiss R Pool2 -SMB #2 fillet L7474-39 (A) MPCAMiss R Pool2-WB #2, #3, #4, #5- fillet composite L7474-40 (A) MPCA L8616-25WE-1 MPCA L8616-26WE-2 MPCA L8616-27WE-3 MPCA L8616-28WE-4 MPCA L8616-6Carp-1 MPCA L8616-7Carp-2 MPCA L8616-8Carp-3 MPCA L8616-9Carp-4 MPCA L8616-10Carp-5 MPCA L8616-29SMB-1 MPCA L8616-30SMB-2 MPCA L8616-31 SMB-3 MPCA L8616-32SMB-4 MPCA L8616-33SMB-5 MPCA L8616-34SMB-6 MPCA L8616-20WB-1 MPCA L8616-21WB-2 MPCA L8616-22WB-3 MPCA L8616-23WB-4 MPCA L8616-24WB-5 MPCA L8616-1 ISMBuffalo 3MChannel catfish 6 0.5 K K 3MChannel catfish 7 0.5 K K 3MChannel catfish 8 0.5 K K 3MChannel catfish 9 0.5 K K 3MChannel catfish 10 0.5 K K 3MSmallmouth bass 1 0.5 K K 3MSmallmouth bass 2 0.5 K K 3MSmallmouth bass 3 0.5 K K 3MSmallmouth bass 4 0.5 K K 3MSmallmouth bass 5 0.5 K K 3MBIuegill sunfish 6 0.5 K K 3MBIuegill sunfish 7 0.5 K K 3MChannel catfish 16 0.5 K K 3MChannel catfish 17 0.5 K K 3MChannel catfish 18 0.5 K K 3MChannel catfish 19 0.5 K K 3MChannel catfish 20 0.5 K K 3MSmallmouth bass 6 0.5 K K 3MSmallmouth bass 7 0.5 K K 3MSmallmouth bass 8 0.5 K K 3MBIuegill sunfish 13 0.5 K K 3MBIuegill sunfish 14 0.5 K K 3MChannel catfish 26 0.5 K K 3MChannel catfish 27 0.5 K K 3MChannel catfish 28 0.5 K K 3MChannel catfish 29 0.5 K K 3MChannel catfish 30 0.5 K K 33.1 5.04 4.54 Page 25 a llfish jo rm a t_2 0 09 3MSmallmouth bass 9 3MSmalimouth bass 10 3MSmallmouth bass 11 3MBIuegill sunfish 20 3MBIuegill sunfish 21 AxysL11311-13 R AxysL11311-14 R AxysH 1311-15 R AxysL11311-16 R AxysH 1311-17 R AxysL11311-12 R AxysL.11311-5 R AxysLI1311-6 R AxysLI1311-7 R AxysU 1311-8 R AxysL11311-9 R AxysL11311-10 R AxysLI1311-11 R AxysL11311-1 R AxysL11311-2 R (A) AxysLI1311-3 R AxysL11311-4 R AXYSJ.12945-22 AXYSJ-12945-23 AXYSJ.12945-24 AXYSJ-12945-25 AXYSJ.12945-26 AXYSJ_12945-27 AXYS_L12945-28 (A) AXYSJ-12945-29 AXYSJ.12945-30 AXYS_L12946-1 AXYS_L12946-2 AXYSJ.12945-5 AXYS_L12945-6 AXYS_L12945-7 AXYSJ.12934-16 AXYS_L12934-17 AXYS_L12934-18 AXYS_L12934-19 AXYS_L12934-20 AXYSJ-12934-21 A X Y S L I2934-22 (A) AXYS_L12934-23 AXYS_L12934-9 AXYS_L12934-10 AXYS_L12934-11 AXYS_L12934-12 AXYSJ.12934-13 AXYSJ.12934-14 XYSJ.12934-15 AXYSJ-12931-12 3.33 0.5 K 0.5 K 0.5 K 0.5 K 4.81 K 4.93 K 4.83 K 4.85 K 4.95 K 5.03 K 4.98 K 4.85 K 4.95 K 4.74 K 4.69 K 4.95 K 4.93 K 4.98 K 4.9 K 4.98 K 4.9 K 4.98 K 4.83 K 4.76 K 4.95 K 4.93 K 5K 4.93 K 4.88 K 4.95 K 4.9 K 5K 4.95 K 4.9 K 4.81 K 4.95 K 4.95 K 4.72 K 5K 4.88 K 4.9 K 4.85 K 4.78 K 4.78 K 4.85 K 4.81 K 4.9 K 4.93 K 4.93 K 4.9 K 4.9 K K K K K K Page 26 3.41 J 2.46 K 3.05 J 5.78 J 3.82 2.51 K 2.49 K 3.09 J 5.87 J 2.37 K 13.8 J 9.86 J 13.5 J 2.49 K 3.32 J 2.82 J 2.45 K 2.49 K 2.42 K 2.38 K 2.48 K 2.46 K 2.5 K 2.46 K 2.44 K 2.48 K 2.45 K 2.5 K 2.48 K 2.45 K 2.4 K 2.48 K 2.48 K 2.55 2.65 6.47 2.92 2.43 K 2.78 2.43 2.43 K 2.4 K 2.45 K 2.46 K 5.74 2.45 K 2.45 K allfish_format_2009 AXYSJ-12931-13 AXYS_L12931-14 (A) AXYS_L12931 -15 AXYS_L12931-16 AXYS_L12931-17 AXYSJJ2931-18 AXYS_L12931 -19 (A) AXYS_L12931 -20 AXYS_L12931-21 AXYS_L12931 -22 AXYS_L12932-8 AXYS_L12932-9 AXYS_L12932-10 AXYSJJ2932-11 AXYSL12916-17 AXYS_L12916-18 AXYSJJ 2916-19 AXYS_L12916-20 AXYS_L12916-21 AXYSJJ 2917-13 AXYS_L12917-14 AXYS_L12916-22 (A) AXYS_L12916-23 AXYS_L12916-24 AXYSJJ 2916-25 X YS JJ2916-26 AXYSJ -1 2917-15 AXYS_L12916-27 AXYS_L12948-15 (A) AXYSJJ 2948-16 AXYS_L12948-17 AXYSJJ 2933-16 AXYS_L12933-17 AXYS_L12933-18 (A) AXYSJJ2933-19 AXYSJJ 2933-20 AXYS_L12933-21 AXYS_L12933-22 AXYS_L12933-23 AXYS_L12933-24 AXYS_L12933-25 AXYS_L12933-26 AXYSJJ 2934-27 AXYSJJ 2934-28 AXYS_L12934-29 AXYS_L12934-30 AXYS_L12945-15 AXYS_L12945-16 AXYSJJ 2945-17 ^ X Y S J J 2945-18 AXYS_L12945-19 AXYS_L12945-20 4.88 K 4.88 K 4.95 K 4.46 K 4.95 K 4.98 K 4.78 K 4.67 K 4.67 K 4.83 K 4.95 K 4.95 K 4.72 K 4.93 K 4.78 K 4.74 K 4.33 K 4.27 K 4.83 K 4.69 K 4.42 K 4.52 K 4.74 K 4.31 K 4.29 K 5K 4.93 K 4.81 K 4.88 K 5K 4.93 K 4.88 K 4.81 K 4.98 K 4.98 K 4.85 K 5K 4.81 K 4.81 K 4.95 K 4.85 K 5K 4.88 K 4.83 K 4.83 K 4.9 K 4.93 K 4.88 K 4.78 K 4.98 K 4.85 K 4.78 K Page 27 2.44 K 2.44 K 2.48 K 2.23 K 2.48 K 2.49 K 2.39 K 2.34 K 2.34 K 2.42 K 2.48 K 2.48 K 7.19 2.46 K 2.39 K 2.37 K 2.16 K 2.14 K 2.42 K 2.35 K 2.21 K 2.26 K 2.37 K 2.16 K 2.15 K 2.5 K 2.46 K 2.4 K 2.44 K 2.5 K 2.46 K 2.44 K 3.39 22.3 2.49 K 2.43 K 5.96 6.85 2.4 K 2.71 2.43 K 11.8 3.02 3.08 2.42 K 3.84 2.46 K 2.44 K 2.39 K 2.49 K 2.43 K 2.39 K allfish format_2009 AXYSJ.12945-21 AXYS_L12946-25 AXYSJ-12946-26 AXYS_L12946-27 AXYSJ-12946-28 AXYS_L12946-29 A0(YS_,Li2945-8 AXYS_L12945-9 AXYSJ.12945-10 AXYSJ-12931-30 AXYS_L12932-1 AXYS_L12932-2 AXYS_L12932-3 AXYS_L12932-4 AXYS_L12932-5 AXYS_L12932-6 AXYS_L12932-7 AXYS_L12931 -23 AXYSJ.12931-24 AXYSJ-12931 -25 AXYSJ.12931-26 AXYSJ.12931-27 AXYSJ-12931 -28 AXYSJJ 2931 -29 AXYS_L12948-8 AXYS_L12948-9 AXYSJ -1 2948-10 AXYSJ-12948-11 AXYS_L12947-13 AXYS_L12947-14 AXYS_L12947-15 AXYS_L12947-16 AXYSJ.12947-17 AXYSJ-12947-18 AXYSJ.12947-19 AXYS_L12947-20 AXYSJ-12947-21 AXYS_L12947-22 AXYS_L12947-23 AXYS_L12917-16 AXYSJ-12917-17 AXYSJ-12917-18 AXYS-L12917-19 AXYS_L12917-20 AXYS_L12917-21 AXYS_L12917-22 AXYS_L12917-23 (A) AXYS_L12917-24 AXYSJ-12917-25 AXYSJ-12917-26 AXYSJ-12917-27 Ai(YS_L12917-28 4.93 4.88 4.76 4.88 4.95 4.85 4.78 4.93 4.67 4.93 4.88 4.72 4.72 4.95 4.98 4.83 4.9 4.52 4.98 4.59 4.63 4.98 4.85 4.5 5.03 4.74 4.76 5.03 4.78 4.76 4.98 4.93 4.95 4.76 4.63 5 4.52 4.67 4.83 4.81 4.88 4.72 4.98 5 4.9 4.61 4.93 4.39 4.69 4.98 4.98 4.76 K fc r" " K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K, E K K K K K K K K K K K K '' Page 28 2.46 2.44 2.38 2.44 2.48 2.43 2.39 2.46 2.34 2.46 2.44 2.36 2.36 2.48 2.49 2.42 2.45 2.26 2.49 2.29 2.31 2.49 2.43 2.25 2.51 2.37 2.38 2.51 2.39 2.38 2.49 2.46 2.48 2.38 2.31 2.5 2.26 3.68 2.42 2.4 2.44 2.36 2.49 2.5 2.45 2.3 2.46 2.19 2.35 2.49 2.49 2.38 K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K, K K K K K K K K K K K K a llfish jo rm a t_2 0 09 AXYSJ.12917-29 AXYS_L12917-30 AXYSJJ 2946-30 AXYS_L12933-10 AXYS_L12933-11 (A) AX YSJJ 2933-12 AXYSJJ 2933-13 AXYS_L12933-14 AXYSJJ 2933-15 AXYS_L12933-27 AXYS_L12933-28 AXYS_L12933-29 AXYSJJ 2933-30 AXYS_L12934-1 AXYS_L12934-2 AXYS_L12934-3 (A) AXYS_L12934-4 AXYS_L12934-5 AXYS_L12945-1 AXYS,,L12945-2 AXYSJJ 2946-14 AXYSJJ 2946-15 AXYSJJ 2946-16 AXYS_L12946-17 AXYSJJ 2946-18 AXYS_L12946-19 AXYSJJ 2946-20 AXYS_L12946-21 AXYS_L12946-22 A X Y S JJ2946-23 (A) AXYS_L12946-24 AXYSJJ 2945-3 AXYS_L12945-4 AXYSJJ 2931-1 AXYSJJ 2931-2 AXYSJJ 2931-3 A X YS JJ 2931-4 AXYSJJ 2931-5 AXYSJJ 2931-6 AXYSJJ 2931-7 AXYSJJ 2931-8 AXYSJJ 2931-9 AXYSJJ 2931-10 AX Y S JJ 2931-11 AXYS_L12932-27 AXYS_L12932-28 AXYSJJ 2932-29 AXYS_L12932-30 AXYSJJ 2916-6 AXYSJJ 2916-7 AXYSJJ 2916-8 AXYSJJ 2916-9 4.78 4.85 4.88 4.95 4.9 4.88 4.98 4.88 4.88 4.81 4.98 4.74 4.9 4.85 4.74 4.85 5 4.74 4.98 5 4.95 5 4.85 5 4.88 4.88 4.98 4.9 4.81 4.81 4.81 4.98 4.74 4.67 4.81 4.26 4.67 4.76 4.48 4.37 4.52 4.9 4.85 4.72 4.78 4.65 4.78 5 4.95 5 4.95 4.98 K .. , K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K Page 29 2.39 2.43 2.44 2.48 2.71 2.44 2.97 3.4 2.44 5.27 4.07 4.2 2.74 3.35 2.6 2.54 2.5 3.77 2.49 2.5 2.48 2.5 2.43 2.5 2.44 2.44 2.49 2.45 2.4 2.4 2.4 2.49 2.37 2.34 2.4 2.13 2.34 2.38 2.24 2.18 2.26 2.45 2.43 2.36 2.39 2.33 2.39 2.5 2.48 2.5 2.48 2.49 K K K K E K E E K K K K K K K K K K K K K K K K K K K K K K K K K K k K K K K K K K K K allfish_format_2009 AXYS_L12916-10 AXYS_L12916-11 AXYS_L12916-12 AXYS_L12916-13 AXYS_L12916-14 AXYSJ.12916-15 (A) AXYSJ.12916-16 AXYSJ.12916-1 AXYSJ.12916-2 AXYS_L12916-3 AXYS_L12948-1 AXYS_L12948-2 AXYS_L12948-3 AXYS_L12948-4 AXYS_L12948-5 AXYS_L12948-6 AXYS_L12948-7 AXYSJ.12947-24 AXYS_L12947-25 AXYS_L12947-26 AXYSJ.12947-27 AXYS_L12947-28 AXYS_L12947-29 AXYSJ.12947-30 AXYS_L12947-31 (A) AXYS_L12934-24 AXYS_L12934-25 AXYS_L12934-26 AXYS_L12933-1 AXYS_L12933-2 AXYSJ.12933-3 AXYS_L12933-4 AXYS_L12933-5 AXYSJ.12933-6 AXYS_L12933-7 AXYS_L12933-8 AXYS_L12933-9 AXYSJ.12934-6 AXYS_L12934-7 AXYSJ.12934-8 AXYS_L12946-3 AXYS_L12946-4 AXYSJ.12946-5 AXYS_L12946-6 AXYSJ.12946-7 AXYS_L12946-8 AXYS_L12946-9 AXYS_L12946-10 AXYS_L12946-11 AXYSJ.12946-12 (A) AXYS_L12946-13 AXYS_L12945-11 4.93 4.95 4.95 4.95 4.98 5 4.76 4.95 5 4.95 4.88 5 4.88 4.93 4.9 4.95 4.98 4.48 4.41 4.39 5 4.93 4.93 4.81 5 4.93 4.98 4.9 4.78 4.88 5 4.81 4.81 5 4.83 4.76 4.93 4.95 5 4.88 4.98 4.95 4.88 4.95 4.98 4.83 4.93 4.98 4.76 4.95 4.83 4.93 K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K Page 30 p. 33 2.46 K 2.48 K 2.48 K 2.48 K 2.49 K 2.5 K 2.38 K 2.48 K 3.49 2.48 K 5.33 E 2.5 K 2.44 K 2.46 K 2.45 K 2.48 K 2.96 E 2.24 K 2.57 2.19 K 2.5 K 13.3 2.46 K 13.3 2.5 K 2.46 K 2.58 2.62 7.2 E 2.44 K 2.5 K 2.4 K 3.79 2.75 E 2.42 K 5.46 E 32.2 E 2.97 3.18 6.82 23.2 2.48 K 17.3 4.28 40.3 2.42 K 2.46 K 2.49 K 2.38 K 48.3 E 6.35 2.46 allfishJorm a L 2 0 0 9 AXYS_L12945-12 (A) AXYS_L12945-13 AXYS_L12945-14 AXYS_L12932-20 AXYS_L12932-21 AXYS_L12932-22 AXYSJ.12932-23 AXYS_L12932-24 (A) AXYS_L12932-25 AXYS_L12932-26 AXYS_L12932-12 AXYS_L12932-13 AXYS_L12932-14 AXYS_L12932-15 (A) AXYS_L12932-16 AXYS_L12932-17 AXYS_L12932-18 AXYS_L12932-19 AXYSJ.12948-12 AXYS_L12948-13 AXYSJ.12948-14 AXYS_L12947-1 AXYS_L12947-2 AXYS_L12947-3 AXYS_L12947-4 AXYSJ-12947-5 (A) AXYSJ.12947-6 AXYS_L12947-7 AXYSJ.12947-8 AXYS_L12947-9 AXYS_L12947-10 AXYS_L12947-11 AXYSJ.12947-12 AXYS_H2916-4 AXYS_H2916-5 AXYS_H2917-2 AXYS_L12917-3 (A) AXYS_L129.17-4 AXYS_H2917-5 AXYS_L12917-6 AXYSJ.12917-7 AXYS_L12917-8 AXYS_L12917-9 AXYS_L12917-10 AXYS_L12917-11 AXYS_L12917-12 AXYS_L12916-28 AXYSJ.12916-29 AXYS_L12916-30 AXYSJ.12917-1 AXYS_L13148-1 AXYS_L13148-2 4.9 K 4.65 K 4.95 K 4.98 K 4.98 K 4.93 K 5K 4.98 K 5K 4.69 K 4.93 K 4.74 K 4.85 K 4.93 K 4.98 K 4.95 K 4.95 K 4.81 K 4.93 K 4.93 K 4.93 K 4.88 K 4.98 K 5.03 K 4.74 K 5K 4.93 K 4.95 K 4.95 K 4.88 K 4.74 K 4.78 K 4.85 K 4.95 K 4.98 K 4.74 K 4.98 K 4.46 K 4.69 K 4.81 K 4.48 K 4.67 K 4.88 K 4.83 K 4.52 K 4.85 K 4.65 K 4.24 K 4.42 K 4.9 K 5K 4.98 K Page 31 p. 34 6.61 2.45 2.48 K 38.5 2.85 18.9 17.6 5.12 2.52 E 37.5 2.46 K 6.95 8.03 4.76 4.07 3.09 2.72 9.83 2.46 K 2.46 K 2.46 K 2.44 K 2.49 K 2.51 K 2.37 K 2.63 2.46 K 2.48 K 2.48 K 6.06 2.37 K 2.39 K 2.43 K 2.48 K 2.49 K 2.37 K 2.49 K 4.66 2.35 K 2.4 K 33.5 2.34 K 2.44 K 2.42 K 2.26 K 2.43 K 2.33 K 2.12 K 2.21 K 2.45 K 2.5 K 2.49 K AXYSJ-13148-3 AXYSJ.13148-4 AXYS_L13148-5 AXYS_L13148-6 AXYS_L13148-7 AXYSJ-13148-8 AXYS_L13148-9 allfish_format_2009 5K 4.98 K 4.93 K 5K 5.15 K 4.95 K 4.98 K p. 35 2.5 K 2.49 K 2.46 K 2.5 K 2.58 K 2.48 K 2.49 K Page 32 allfish_format_2009 p. 36 PFPeAPPE PFPeACOI PFDAPPB PFDACOD PFUnAPPE PFUnACOI PFDoAPPE PFDoACOI PFHxAPPE 2.97 2.4 4.73 0.558 2.42 2.23 2.53 0.65 4.1 1.63 1.62 0.767 Page 33 allfish_format_2009 2.4 K 2.46 K 2.42 K 2.43 K 2.48 K 2.51 K 2.49 K 2.43 K 2.48 K 2.37 K 2.35 K 2.48 K 2.46 K 2.49 K 2.45 K 2.49 K 2.45 K 2.49 K 2.42 K 2.38 K 2.48 K 2.46 K 2.5 K 2.46 K 2.44 K 2.48 K 2.45 K 2.5 K 2.48 K 2.45 K 2.4 K 2.48 K 2.48 K 2.36 K 2.5 K 2.44 K 2.45 K 2.43 K 2.39 K 2.39 K 2.43 K 2.4 K 2.45 K 2.46 K 2.46 K 2.45 K 2.45 K 2.4 K 2.63 3.83 7.8 2.48 K 2.51 K 2.49 K 2.43 K 2.48 K 2.44 3.29 2.48 3.21 2.49 K 2.45 K 2.49 K 2.45 K 2.49 K 2.42 K 2.38 K 2.92 2.46 K 2.5 K 2.46 K 2.44 K 2.48 K 2.45 K 2.5 K 2.48 K 2.45 K 2.4 K 2.98 2.92 2.54 2.5 K 2.44 K 6.69 3.21 3.67 2.63 2.71 2.69 2.88 3.29 2.46 K 3.17 2.45 K 2.64 2.46 K 3 4.74 2.48 K 2.51 K 2.49 K 2.43 K 2.48 K 2.37 K 3.45 2.48 3.32 2.49 K 2.45 K 2.49 K 2.45 K 2.49 K 2.42 K 2.38 K 2.48 K 2.46 K 2.5 K 2.46 K 2.44 K 2.48 K 2.45 K 2.5 K 2.48 K 2.45 K 2.4 K 2.48 K 2.48 K 2.36 K 2.5 K 2.44 K 4.37 2.43 K 2.39 K 2.39 K 2.43 K 2.4 K 2.45 K 2.46 K 2.46 K 2.45 K 2.45 K Page 34 3.69 2.46 K 2.42 K 2.5 2.48 K 2.51 K 2.49 K 2.43 K 2.48 K 2.37 K 3.08 2.48 K 2.89 2.49 K 2.45 K 2.49 K 2.45 K 2.49 K 2.42 K 2.38 K 2.48 K 2.46 K 2.5 K 2.46 K 2.44 K 2.48 K 2.45 K 2.5 K 2.48 K 2.45 K 2.4 K 2.48 K 2.48 K 2.36 K 2.5 K 2.44 K 2.7 2.43 K 2.39 K 2.39 K 2.43 K 2.43 2.45 K 2.46 K 2.46 K 2.45 K 2.45 K 2.4 2.46 2.42 2.43 2.48 2.51 2.49 2.43 2.48 2.37 2.35 2.48 2.46 2.49 2.45 2.49 2.45 2.49 2.42 2.38 2.48 2.46 2.5 2.46 2.44 2.48 2.45 2.5 2.48 2.45 2.4 2.48 2.48 2.36 2.5 2.44 2.45 2.43 2.39 2.39 2.43 2.4 2.45 2.46 2.46 2.45 2.45 2.44 K 2.44 K 2.48 K 2.23 K 2.48 K 2.49 K 2.39 K 2.34 K 2.34 K 2.42 K 2.48 K 2.48 K 2.36 K 2.46 K 2.39 K 2.37 K 2.16 K 2.14 K 2.42 K 2.35 K 2.21 K 2.26 K 2.37 K 2.16 K 2.15 K 2.5 K 2.46 K 2.4 K 2.44 K 2.5 K 2.46 K 2.44 K 2.4 K 2.49 K 2.49 K 2.43 K 2.5 K 2.4 K 2.4 K 2.48 K 2.43 K 2.5 K 2.44 K 2.42 K 2.42 K 2.45 K 2.46 K 2.44 K 2.39 K 2.49 K 2.43 K 2.39 K 2.78 2.44 K 2.48 K 2.58 2.48 K 2.49 K 2.39 K 2.34 K 2.34 K 2.42 K 2.48 K 2.48 K 2.36 K 2.46 K 2.39 K 2.37 K 2.16 K 2.14 K 2.42 K 2.35 K 2.21 K 2.26 K 2.66 2.16 K 2.15 K 2.5 K 2.46 K 2.4 K 2.44 K 2.5 K 2.46 K 2.52 2.71 3.33 3.81 2.43 K 2.5 K 3.52 3.24 3.45 2.99 2.5 K 2.44 K 3.2 2.42 K 2.45 K 2.46 K 2.44 K 2.39 K 2.49 K 2.43 K 2.39 K allfish_ format_2009 3.84 2.44 K 2.48 K 2.23 K 2.48 K 2.49 K 2.39 K 2.34 K 2.34 K 2.42 K 2.48 K 2.48 K 2.36 K 2.46 K 2.39 K 2.37 K 2.16 K 2.14 K 2.42 K 2.35 K 2.21 K 2.26 K 2.37 K 2.16 K 2.15 K 2.5 K 2.46 K 2.4 K 2.44 K 2.5 K 2.46 K 2.44 K 2.4 K 6.7 2.49 K 2.43 K 2.5 K 2.4 K 2.41 2.48 K 2.43 K 4.16 2.44 K 4.38 2.42 K 2.45 K 2.46 K 2.44 K 2.39 K 2.49 K 2.43 K 2.39 K 2.44 K 2.44 K 2.48 K 2.23 K 2.48 K 2.49 K 2.39 K 2.34 K 2.34 K 2.42 K 2.48 K 2.48 K 2.36 K 2.46 K 2.39 K 2.37 K 2.16 K 2.14 K 2.42 K 2.35 K 2.21 K 2.26 K 2.37 K 2.16 K 2.15 K 2.5 K 2.46 K 2.4 K 2.44 K 2.5 K 2.46 K 2.44 K 2.4 K 29.8 2.49 K 2.43 K 2.5 K 2.4 K 2.4 K 2.48 K 2.43 K 11.8 2.44 K 9.44 2.42 K 2.45 K 2.46 K 2.44 K 2.39 K 2.49 K 2.43 K 2.39 K Page 35 2.44 2.44 2.48 2.23 2.48 2.49 2.39 2.34 2.34 2.42 2.48 2.48 2.36 2.46 2.39 2.37 2.16 2.14 2.42 2.35 2.21 2.26 2.37 2.16 2.15 2.5 2.46 2.4 2.44 2.5 2.46 2.44 2.4 2.49 2.49 2.43 2.5 2.4 2.4 2.48 2.43 2.5 2.44 2.42 2.42 2.45 2.46 2.44 2.39 2.49 2.43 2.39 2.46 K 2.44 K 2.38 K 2.44 K 2.48 K 2.43 K 2.39 K 2.46 K 2.34 K 2.46 K 2.44 K 2.36 K 2.36 K 2.48 K 2.49 K 2.42 K 2.45 K 2.26 K 2.49 K 2.29 K 2.31 K 2.49 K 2.43 K 2.25 K 2.51 K 2.37 K 2.38 K 2.51 K 2.39 K 2.38 K 2.49 K 2.46 K 2.48 K 2.38 K 2.31 K 2.5 K 2.26 K 2.34 K 2.42 K 2.4 K, E 2.44 K 2.36 K 2.49 K 2.5 K 2.45 K 2.3 K 2.46 K 2.19 K 2.35 K 2.49 K 2.49 K 2.38 K 2.46 K 2.44 K 2.38 K 2.44 K 2.48 K 2.43 K 2.39 K 2.46 K 2.34 K 2.46 K 2.44 K 2.36 K 2.36 K 2.48 K 2.49 K 2.42 K 2.45 K 2.26 K 2.49 K 2.29 K 2.31 K 2.49 K 2.43 K 2.25 K 2.51 K 2.37 K 2.38 K 2.51 K 2.39 K 2.38 K 2.49 K 2.46 K 2.48 K 2.38 2.31 K 2.5 K 2.33 3.95 3.31 2.4 K, E 2.44 K 2.36 K 2.49 K 2.5 K 2.45 K 2.3 K 2.46 K 2.19 K 2.35 K 2.49 K 2.49 K 2.38 K allfish J o rm a t_ 2 0 0 9 2.46 K 2.44 K 2.38 K 2.44 K 2.48 K 2.43 K 2.39 K 2.46 K 2.34 K 2.46 K 2.44 K 2.36 K 2.36 K 2.48 K 2.49 K 2.42 K 2.45 K 2.26 K 2.49 K 2.29 K 2.31 K 2.49 K 2.43 K 2.25 K 2.51 K 2.37 K 2.38 K 2.51 K 2.39 K 2.38 K 2.49 K 2.46 K 2.48 K 2.38 K 2.31 K 2.5 K 2.26 K 5.13 2.42 K 2.4 K,E 2.44 K 2.36 K 2.49 K 2.5 K 2.45 K 2.3 K 2.46 K 2.19 K 2.35 K 2.49 K 2.49 K 2.38 K 2.46 2.44 2.38 2.44 2.48 2.43 2.39 2.46 2.34 2.46 2.44 2.36 2.36 2.48 2.49 2.42 2.45 2.26 2.49 2.29 2.31 2.49 2.43 2.25 2.51 2.37 2.38 2.51 2.39 2.38 2.49 2.46 2.48 2.38 2.31 2.5 2.26 4 2.42 2.4 2.44 2.36 2.49 2.5 2.45 2.3 2.46 2.19 2.35 2.49 2.49 2.38 K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K, E K K K K K K K K K K K K Page 36 2.46 2.44 2.38 2.44 2.48 2.43 2.39 2.46 2.34 2.46 2.44 2.36 2.36 2.48 2.49 2.42 2.45 2.26 2.49 2.29 2.31 2.49 2.43 2.25 2.51 2.37 2.38 2.51 2.39 2.38 2.49 2.46 2.48 2.38 2.31 2.5 2.26 2.34 2.42 2.4 2.44 2.36 2.49 2.5 2.45 2.3 2.46 2.19 2.35 2.49 2,49 2.38 2.39 2.43 2.44 2.48 2.45 2.44 2.49 2.44 2.44 2.4 2.49 2.37 2.45 2.43 2.37 2.43 2.5 2.37 2.49 2.5 2.48 2.5 2.43 2.5 2.44 2.44 2.49 2.45 2.4 2.4 2.4 2.49 2.37 2.34 2.4 2.13 2.34 2.38 2.24 2.18 2.26 2.45 2.43 2.36 2.39 2.33 2.39 2.5 2.48 2.5 2.48 2.49 K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K 2.39 2.43 2.44 3.18 2.45 2.44 2.49 2.44 2.52 2.4 2.49 2.37 2.45 2.43 3.32 2.43 3.75 2.37 3.19 2.51 2.92 2.5 2.43 2.5 2.44 2.44 2.68 2.55 2.4 2.49 2.4 2.49 2.47 2.34 2.4 2.13 2.34 2.38 2.24 2.18 2.26 3.04 2.43 2.36 2.39 2.33 2.39 2.5 2.48 2.5 2.48 4.51 K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K K allfish_format_2009 2.39 2.43 2.44 2.48 2.45 2.44 2.49 2.44 2.44 2.4 2.49 2.37 2.45 2.43 2.37 2.43 2.5 2.37 2.49 2.5 2.48 2.5 2.43 2.5 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2.48 K K 2.48 K 2.48 K 4.95 K 2.48 k K 2.44 K 2.44 K 4.88 K 2.44 K K 2.37 K 2.37 K 4.74 K 2.37 K K 2.39 k 2.39 K 4.78 K 2.39 k k 2.43 K 2.43 K 4.85 K 2.43 K K 2.48 K 2.48 K 4.95 K 2.48 K K 2.49 K 2.49 K 4.98 K 2.49 K K 2.37 K 2.37 K 4.74 K 2.37 K K 2.49 K 2.49 K 4.98 K 2.49 K K 2.23 K 2.23 K 4.66 6.01 K 2.35 K 2.35 K 4.69 K 2.35 K k 2.4 K 2.4 K 4.81 K 2.4 K K 2.24 K 2.24 K 4.58 10.4 K 2.34 K 2.34 K 4.67 K 2.34 K K 2.44 K 2.44 K 4.88 K 2.44 K K 2.42 K 2.42 K 4.83 K 2.42 K k 2.26 K 2.26 K 4.52 K 2.26 K K 2.43 K 2.43 K 4.85 K 2.43 K k 2.33 K 2.33 K 4.65 K 2.33 K K 2.12 K 2.12 K 4.24 K 2.12 K k 2.21 k 2.21 K 4.42 K 2.21 K K 2.45 K 2.45 K 4.9 K 2.45 K K 2.5 K 2.5 K 5K 2.5 K K 2.49 K 2.49 K 4.98 K 2.49 K Page 47 Pv T v * * * A PC 2.5 K 2.49 K 2.46 K 2.5 K 2.58 K 2.48 K 2.49 K allfish_format_2009 2.5 K 2.49 K 2.46 K 2.5 K 2.58 K 2.48 K 2.49 K 5K 4.98 K 4.93 K 5K 5.15 K 4.95 K 4.98 K 2.5 K 2.49 K 2.46 K 2.5 K 2.58 K 2.48 K 2.49 K Page 48 DOWLKNl RNAME ALT_NAME allfishjorm at_2009 p. 52 Page 49 allfish_format_2009 p. 53 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 Page 50 allfish _format_2009 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 a llfish _ fo rm a t,,2 0 0 9 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM-8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM-8-2) RM 836-843 MISSISSIPPI R. PoolI 2 (UM-8-2) RM 836-843 MISSISSIPPI R. PoolI 2 (UM-8-2) RM 836-843 MISSISSIPPI R. Pool12 (UM-8-2) RM 836-843 allfishjorm at_2009 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-2) RM 836-843 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 827-830 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 Page 53 p. 56 allfish_format_2009 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 Page 54 p. 57 allfish_format_2009 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-3) RM 833.5-834 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-4) RM 815-820 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 MISSISSIPPI R. Pool 2 (UM- 8-1) RM 844-847.5 Page 55 p. 58 allfish_format_2009 MISSISSIPPI MISSISSIPPI MISSISSIPPI MISSISSIPPI MISSISSIPPI MISSISSIPPI MISSISSIPPI Pool 2 (UM- 8-1) RM 844-847.5 Pool 2 (UM- 8-1) RM 844-847.5 Pool 2 (UM- 8-1) RM 844-847.5 Pool 2 (UM- 8-1) RM 844-847.5 Pool 2 (UM- 8-1) RM 844-847.5 Pool 2 (UM- 8-1) RM 844-847.5 Pool 2 (UM- 8-1) RM 844-847.5 p. 59 Page 56 qualified samples (coded as "E" for estimated) sample PFC____________________ 090068 PFBA 090122 ALL 090139 PFOSA 090141 PFOSA 090142 PFOSA 090151 PFBA 090197 PFOSA 090203 PFOSA 090215 PFOSA 090219 PFOSA 090220 PFOSA 090222 PFOSA 090223 PFOSA 090227 PFOA 090229 PFOA 090231 PFOA 090233 PFOA 090234 PFOA 090236 PFOA, PFHxS, PFOSA 090237 PFOA, PFHxS 090247 PFOS, PFOSA p. 61 3M ENVIR O N M EN TA L LABORATORY R EP O R T NO. E09-0365 Final Report Fluorochemical Characterization of Surface Water Samples, Mississippi River - Pool 2; July 2009 Laboratory Request Number: E09-0365 Method Requirement: 3M Method ETS-8-154.3 ETS-8-154.3: "Determination of Perfluorinated Acids, Alcohols, Amides, and Sulfonates in Water by Solid Phase Extraction and High Performance Liquid Chromatography/Mass Spectrometry" Report D ate - August 12, 2009 Testing Laboratory 3M EHS Operations 3M Environmental Laboratory Building 260-5N-17 Maplewood, MN 55144-1000 Requester Gary Hohenstein 3M Building 224-5W-03 Saint Paul, MN 55144-1000 Phone: (651) 737-3570 ht ACCREDITED The testing reported herein meet the requirements of ISO/IEC 17025-2005 "General Requirements for the Competence of Testing and Calibration Laboratories", in accordance with the A2LA Certificate #2052-01. Testing that complies with this International Standard also operate in accordance with ISO 9001:2000. Certificate #2052-01 PAGE 1OF32 p. 62 3M ENVIR O N M EN TA L LABO RATO RY R E P O R T NO. 09-0365 3M Environmental Laboratory 3M Environmental Laboratory Manager: William K. Reagen, Ph.D. 3M Principal Analytical Investigator and Report Author: Susan Wolf Analytical Report E09-0365 Fluorochemical Characterization of Surface Water Samples, Mississippi River - Pool 2; July 2009 Report Date: August 12,2009 1 Introduction/Summary The 3M Environmental Laboratory prepared and analyzed surface water samples collected by PACE Analytical Services personnel from Pool 2 on the Mississippi River. Samples were collected on July 8, 2009. Samples were returned to the 3M Environmental Laboratory on July 8 at ambient conditions for the analysis for thirteen fluorochemical compounds under laboratory project number E09-0365. The 3M Environmental Laboratory prepared sample containers for twelve sampling locations. Each sample set consisted of a field sample, field sample duplicate, and a 25 ppt field spike. Each empty container was marked with a "fill to here" line that corresponded to a final volume of 200 mL. Containers reserved for field matrix spikes were fortified with an appropriate matrix spike solution containing all analytes prior to being sent to the field for sample collection. Samples were prepared and analyzed using method ETS-8-154.3 "Determination of Perfluorinated Acids, Alcohols, Amides, and Sulfonates in Water by Solid Phase Extraction and High Performance Liquid Chromatography/Mass Spectrometry". Table 1 summarizes the sample results using the analytical method identified above. All results for quality control samples prepared and analyzed with the samples will be reported and discussed elsewhere in this report. X CCREDITED The testing reported herein meet the requirements of ISO/IEC 17025-2005 "General Requirements far the Competence of Testing and Calibration Laboratories", in accordance with the A2LA Certificate #2052-01. Testing that complies with this International Standard also operate in accordance with ISO 9001:2000. Certificate #2052-01 PAGE 2OF32 3M ENVIRONM ENTA L LABORATORY R E P O R T NO. 09-0365 Table 1. Sam ple R esu lts S um m ary*1' 3M LIMS ID E09-0365-001 E09-0365-002 094)3654)04 E09-0365-005 E09-0365-007 E09-0365-008 E09-0365-010 E09-0365-011 Sample Concentration (ng/L) Sample Description Reach 1 Location 1 Sample Reach 1 Location 1 Sample Dup PFBA 4.84 4.76 PFPeA PFHxA PFHpA <2.53 <2 53 <2.53 <2.53 <2.53 <2.53 PFOA <3.00 <3.00 PFNA PFDA PFUnA PFDoA PFBS <2.50 <2.49 <2.50 <3.00 <3.06 <2.50 <2.49 <2.50 <3.00 <3.06 Averagi 4.80 <2.53 <2.53 <2.53 <3.00 <2.50 <2.49 <2.50 <3.00 <3.06 %RPD Sample/Sample Duplicate 1.7 Reach 1 Location 2 Sample 6.36 Reach 1 Location 2 Sample Dup 6.50 NA <2.53 <2.53 NA <2.53 <2.53 NA <2.53 <2.53 NA <3.00 <3.00 NA NA NA NA NA <2.50 <2.49 <2.50 <3.00 <3.06 <2.50 <2.49 <2.50 <3.00 <3.06 Average 6.43 <2.53 <2.53 <2.53 <3.00 <2.50 <2.49 <2.50 <3.00 <3.06 %RPD Sample/Sample Duplicate 2.2 Reach 1 Location 3 Sample 5.37 Reach 1 Location 3 Sample Dup 5.17 NA <2 53 <2.53 NA <2.53 <2.53 NA <2.53 <2.53 NA <3.00 <3.00 NA NA NA NA NA <2.50 <2.49 <2.50 <3.00 <3.06 <2.50 <2.49 <2.50 <3.00 <3.06 Average 5.27 <2.53 <2.53 <2.53 <3.00 <2.50 <2.49 <2.50 <3.00 <3.06 %RPD Sample/Sample Duplicate 3.8 Reach 2 Location 4 Sample 4.86 Reach 2 Location 4 Sample Dup 5.32 NA <2.53 <2.53 NA <2.53 <2.53 NA <2.53 <2.53 NA <3.00 <3.00 NA <2.50 <2.50 NA <2.49 <2.49 NA <2.50 <2.50 NA <3.00 <3.00 NA <3.06 <3.06 Average 5.09 <2.53 <2.53 <2.53 <3.00 <2.50 <2.49 <2.50 <3.00 <3.06 %RPD Sample/Sample Duplicate 9.0 NA NA NA NA NA NA NA NA NA PFHS <2.50 <2.50 <2.50 NA <2.50 <2.50 <2.50 NA <2.50 <2.50 <2.50 NA <2.50 <2.50 <2.50 NA PFOS PFOSA <2.50 <2.99 <2.50 <2.99 <2.50 <2.99 NA NA <2.50 <2.99 <2.50 <2.99 <2.50 <2.99 NA NA <2.50 <2.99 <2.50 <2.99 <2.50 NA <2.50 <2.99 NA <2.99 <2.50 <2 99 <2.50 <2.99 NA NA p. 63 PAGE 3OF32 3M ENVIRONM ENTA L LABORATORY R EPO R T NO. E09-0365 T ab le 1 continued. S am p le R es u lts S u m m ary*1* 3M UMS ID E09-0365-013 E09-0365-014 E09-0365-016 E09-0365-017 E09-0365-019 E09-0365-020 E09-0365-022 E09-0365-023 Sample Concentration (ng/L) Sample Description Reach 2 Location 5 Sample Reach 2 Location 5 Sample Dup PFBA 5.45 4.97 PFPeA PFHxA PFHpA PFOA <2.53 <2.53 <2.53 <3.00 <2.53 <2.53 <2.53 <3.00 PFNA PFDA PFUnA PFDoA PFBS <2.50 <2.49 <2.50 <3.00 <3.06 <2.50 <2.49 <2.50 <3.00 <3.06 Average 5.21 <2.53 <2.53 <2.53 <3.00 <2.50 c2.49w <2.50 <3.00 <3.06 %RPD Sample/Sample Duplicate 9.2 Reach 2 Location 6 Sample 7.05 Reach 2 Location 6 Sample Dup 7.46 NA <2.53 <2.53 NA <2.53 <2.53 NA <2.53 <2.53 NA 3.97 3.66 NA NA NA NA NA <2.50 <2.49 <2.50 <3.00 <3.06 <2.50 <2.49 <2.50 <3.00 <3.06 Average 7.26 <2.53 <2.53 <2.53 3.82 <2.50 <2.49 <2.50 <3.00 <3.06 %RPD Sample/Sample Duplicate 5.7 Reach 3 Location 7 Sample 9.34 Reach 3 Location 7 Sample Dup 10.2 NA <2.53 <2.53 NA <2.53 <2.53 NA : 8.1 <2.53 5.38 <2.53 6.10 NA NA NA NA NA <2.50 <2.49 <2.50 <3.00 4.77 <2.50 <2.49 <2.50 <3.00 5.76 Average 9.77^' %RPD Sample/Sample Duplicate 8.8 Reach 3 Location 8 Sample 8.13 Reach 3 Location 8 Sample Dup 8.25 <2.53 NA <2.53 2.55 <2.53 NA <2.53 <2.53 <2.53 NA <2.53 <2.53 5.74 13 5.79 4.30 <2.50 C2.491"' <2.50 <3.00 5.27 NA <2.50 NA <2.49 NA <2.50 NA <3.00 19 5.24 <2.50 <2.49 <2.50 <3.00 4.59 Average 8.19 2.55 <2.53 <2.53 5.05 <2.50 <2.49 <2.50 <3.00 4.92 %RPD Sample/Sample Duplicate 1.5 NC,J| NA NA 30P) NA NA NA NA 13 PFHS <2.50 <2.50 <2.50 NA <2.50 <2.50 <2.50 NA <2.50 <2.50 <2.50 NA <2.50 <2.50 <2.50 NA PFOS PFOSA <2.50 <2.99 <2.50 <2.99 <2.50 <2.99 NA NA 8.48 <2.99 8.59 <2.99 8.54 1.3 <2.99 NA 12.4 <2 99 13.1 <2.99 12.8" ' 5.5 11.2 <2.99 NA <2.99 9.76 <2.99 10.5 <2.99 14 NA p. 64 PAGE 4OF 32 3M ENVIRONM ENTAL LABO RATO RY R E P O R T NO. EQ9-0365 T able 1 continued. S a m p le R e s u lts S u m m a ry 01 3M LIMS ID E 0M 365- 25 E09-0365-026 E09-036&028 E09-0365-029 E09-0365-031 E09-0365O32 E09-0365-034 E09-0365-035 Sample Concentration (ng/L) Sample Description Reach 3 Location 9 Sample Reach 3 Location 9 Sample Dup PFBA PFPeA PFHxA PFHpA PFOA 103 2.86 <2.53 <2.53 5.43 10.5 <2.53 <2.53 <2.53 4.78 PFNA PFDA PFUnA PFDoA PFBS <2.50 <2.49 <2.50 <3.00 <3.06 <2.50 <2.49 <2.50 <3.00 <3.06 Average 10.4 2.86 <2.53 <2.53 5.11 <2.50 <2.49 <2.50 <3.00 <3.06 % R P D S am p le/S am p le D u plicate 1.9 Reach 4 Location 10 Sample 9.92 Reach 4 Location 10 Sample Dup 9.86 A verage 9.89 % R P D S a m p le /S a m p le D u p lic a te 0.61 Reach 4 Location 11 Sample 144 Reach 4 Location 11 Sample Dup 119 NC(J) 3.03 2.66 2.85 13 21.8 26.4 NA NA <2.53 <2.53 <2.53 <2.53 <2.53 <2.53 NA NA 17.1 8 18 19.8 10.0 13 4.45 3.77 4.11 17 113 125 NA NA NA NA NA <2.50 <2.49 <2.50 <3.00 <3.06 <2.50 <2.49 <2.50 <3.00 <3.06 <2.50 <2.49 <2.50 <3.00 <3.06 NA NA NA NA NA <2.50 <2.49 <2.50 <3.00 106 <2.50 <2.49 <2.50 <3.00 70.9 Average 132 % R P D S am p le/S am p le D u plicate 19 Reach 4 Location 12 Sample 35.9 Reach 4 Location 12 Sample Dup 45.1 24.1 19 743 8.23 18.5 15 5.91 5.88 9.09 20 2.55 <2.53 119 10 21.7 24.9 <2.50 <2.49 NA NA <2.50 <2.49 <2.50 <2.49 <2.50 NA <2.50 <2.50 <3.00 NA <3.00 <3.00 88.5 4013' 24.4 29.4 A v e ra g e 40.5 % R P D S a m p le /S a m p le D u p licate 23<3| 7.83 10 5.90 0.51 2.55 NC<2' 23.3 14 <2.50 <2.49 NA NA <2.50 <3.00 26.9 NA NA 19 PFHS <2.50 <2.50 <2.50 NA <2.50 <2.50 <2.50 NA 37.0 42.1 39.6 13 15.6 18.6 17.1 18 PFOS PFOSA 4.35 <2.99 3.90 <2.99 4.13 <2.99 11 NA 4.33 <2.99 4.11 <2.99 4.22 <2.99 5.2 NA 108 3.67 120 4.08 114 3.88 11 23.0 11 <2.99 26.5 <2.99 24.8W <2.99 14 NA p. 65 PAGE 5OF32 3M ENVIR O N M EN TA L LABORATORY R E P O R T NO. 09-0365 NA = Not Applicable (1) The analytical method uncertainties associated with the reported results are as follows: P F B A 100% 19%, PFPeA 100% 21%, PFHxA 100% 19%, PFHpA 100% 18%, PFOA 100% 21%, PFNA 100% 21%, PFDA 100% 17%, PFUnA 100% 18%, PFDoA, 100% 25%, PFBS 100% 20%, PFHS 100% 23%, PFOS 100% 27% and PFOSA 100% 22%. (2) Not Calculated; The sample and sample duplicate produced one result above the LOQ and one result below the LOQ. The reported average concentration represents only the result above the LOQ. A true average was not calculated. (3) The relative percent difference (RPD) between the sample and sample duplicate exceeded method acceptance criteria of 20% . (4) The analytical uncertainty has been expanded due to field matrix spike recovery. See section 4 of the report for additional information. 2 Methods - Analytical and Preparatory 2.1 Methods Analysis was completed following 3M Environmental Laboratory method ETS-8-154.3 "Determination of Perfluorinated Acids, Alcohols, Amides, and Sulfonates in Water by Solid Phase Extraction and High Performance Liquid Chromatography/Mass Spectrometry". TargetA n alytes Perfluorobutanesutfbnate (C4 Sulfonate) Perfluorohexanesulfonate (C6 Sulfonate) Perfluorooctanesulfonate (C8 Sulfonate) Perfluorobutanoic Acid (C4 Acid) Perfiuoropentanoic Acid (C5 Acid) Perftuorohexanoic Acid {C6 Add) Perfluoroheptanoic Acid (C7 Acid) Perfiuorooctanoic Add (C8 Acid) Perfluoronortanoic Acid (C9 Acid) Perfluorodecanoic Acid (C10 Acid) Perfluoroundecanoic Acid (C11 Add) Perfiuorododecanoic Acid (C12 Add) Perfluorooctanesulfonamide A c ro n y m PFBS PFHS PFOS PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFOSA R e fere n c e M aterial Structure Linear Linear Linear Linear Linear Linear Linear Linear Linear Linear Linear Linear Branched 2.2 Sample Collection Samples were collected on July 8, 2009 in NalgeneTM (high-density polyethylene) bottles prepared at the 3M Environmental Laboratory. Prior to sample collection, bottles designated for field matrix spikes were spiked in the laboratory with a known volume of an appropriate matrix spiking solution containing the analytes of interest. Collected sample bottles were returned to the laboratory at ambient conditions on July 8, 2009. 2.3 Sample Preparation All samples, calibration standards, and associated quality control samples were extracted following ETS-8-154.3. Briefly, 50 mL of sample were loaded onto a pre-conditioned Waters tC18 solid-phase extraction (SPE) cartridge (1.0 g, 6 cc) using a vacuum manifold. The loaded SPE cartridges were then eluted with 2.5 mL of methanol. This extraction procedure concentrates the samples by a factor of twenty-five. (Initial volume = 50 mL, final volume = 2.5 mL). PAGE6OF32 p. 67 3M EN VIR O N M EN TA L LABORATORY R E P O R T NO. 09-0365 2.4 Analysis All samples and quality control samples were analyzed for thirteen target analytes using high performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). Pertinent instrument parameters, the liquid chromatography gradient program, and the specific mass transitions analyzed are described in the tables below. Sample results for PFBA were analyzed on 7/31/09 Sample results for PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFBA, PFHS, PFOS, and PFOSA were analyzed 7/21/09. Sample results for PFDA, PFUnA, and PFDoA were analyzed 7/28/09. Sample results for sampling location Reach 4 Location 11, PFBA, PFOA, PFBS, and PFOS were analyzed 7/23/09. Table 2. Instrument Parameters. Instrument Name ETS Ginger/Jonas ETS Ollie Liquid Chromatograph Analytes Aqilent 1100 All analytes01 Agilent 11) PFBA Guard column Betasil C18 (2.1 mm X 100 mm), 5 p Prism RP (2.1 mm X 50 mm), 5 u Analytical column Betasil C18 (2.1 mm X 100 mm), 5 u Prism RP (2.1 mm X 50 mm), 5 u Injection Volume Mass Spectrometer 5 mL Applied Biosystems API 5000 20 nL Applied Biosystems API 4000 Ion Source Turbo Spray Turbo Spray Polarity Negative Negative Software Analyst 1.4.2 Analyst 1.4.2 (1) PFBA was analyzed using ETS Ollie for all samples with the exception of Reach 4 Location 11, which was reported from ETS Jonas. Table 3. Liquid Chromatography Gradient Program. Step Number 0 1 2 3 4 5 6 0 1 2 3 4 5 Total Time (m in ) 0.0 3.5 11.0 13.5 15.0 17.5 21.0 0.0 2.0 14.5 15.5 16.5 20.0 ETS Ginger and ETS Jonas Flow Rate (fiL/min) Percent A (2 m M am m onium acetate) 300 90.0 300 40.0 300 40.0 300 10.0 300 10.0 300 90.0 300 90.0 ETS Ginger (PFDA, PFUnA, and PFDA) 300 90.0 300 90.0 300 10.0 300 10.0 300 90.0 300 90.0 PercentB (M e th a n o l) 10.0 60.0 60.0 90.0 90.0 10.0 10.0 10.0 10.0 90.0 90.0 10.0 10.0 PAGE 7OF 32 3M EN VIR O N M EN TA L LABORATORY R EPO R T NO. E09-0365 Table 3 continued. Liquid Chrom atography Gradient Program. Step Number 0 1 2 3 4 5 Total Time (min) 0.0 3.0 12 13 14 17 ETS Olile (PFBA) Flow Rate (pL/min) Percent A (5 mM ammonium acetate with 0.01% Acetic Acid) 300 90.0 300 90.0 200 10.0 300 10.0 300 90.0 300 90.0 Table 4. Mass Transitions Percent B (Methanol) 10.0 10.0 900 90.0 10.0 10.0 Analyte PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA Mass Transition Q1/Q3 213/169 263/219 313/119 313/269 363/319 363/169 413/369 413/219 413/169 463/419 463/169 463/219 513/469 513/269 513/219 Analyte PFUnA PFDoA PFBS PFHS PFOS PFOSA Mass Transition Q1/Q3 563/519 563/269 563/219 613/569 613/319 613/169 299/80 299/99 399/80 399/99 499/99 499/80 499/130 498/78 Dwell time varied by run (nom 5 0 - 1 0 0 msec lor each transition analyzed. The acquisition method used for the initial analysis where all analytes were analyzed in a single run, was broken into two time periods to accommodate the number of transitions being monitored. 3 Data Analysis 3.1 Calibration Calibration standards were prepared by spiking known amounts of stock solutions containing the analytes of interest into 50 mL of reverse-osmosis purified water. Each spiked water standard was then extracted in the same manner as the collected samples. A total of thirteen spiked standards ranging from a nominal concentration of 0.0025 ng/mL (2.5 ng/L) to 5 ng/mL (5000 ng/L) were prepared. A quadratic, 1/x weighted, calibration curve was used to fit the data for each analyte. The data were not forced through zero during the fitting process. Calculating the standard concentration using the peak area counts and the resultant calibration curve confirmed accuracy of each curve point. PAGE 8OF 32 p. 69 3M ENVIR O N M EN TA L LABORATORY R E P O R T NO . E09-0365 Each curve point was quantitated using the overall calibration curve and reviewed for accuracy. Method calibration accuracy requirements of 10025% (10030% for the lowest curve point) were met for all analytes. The correlation coefficient (r) was greater than 0.995 for all analytes. 3.2 System Suitability A calibration standard was analyzed four times at the beginning of the analytical sequence to demonstrate overall system suitability. All analytes met the acceptance criteria of less than or equal to 5% relative standard deviation (RSD) for peak area and retention time criteria of less than or equal to 2% RSD with the exception of PFOSA which had an area count RSD of 11%. A method deviation is filed with the raw data. 3.3 Limit of Quantitation (LOQ) The LOQ as defined in method ETS-8-154.3 is the lowest non-zero calibration standard in the curve that meets linearity and accuracy requirements and for which the area counts are at least twice those of the appropriate blanks. The LOQs associated with the sample analysis are listed in the table below. Table 5. LOQ Analyte LOQ, ng/L P F B A (V 3.03 PFPeA 2.53 PFHxA 2.53 PFHpA 2.53 PFOAm 3.00 PFNA 2.50 PFDA 2.49 PFUnA 2.50 PFDoA 3.00 P FB S f'> 3.06 PFHS 2.50 P F O & 1' 2.50 PFOSA 2.99 (1) Sampling location Reach 4 Location 11 was re-extracted with a LMS. The reported results for this location has a LOQ for PFBA of 101 ng/L, PFOA at 25.0 ng/L, PFBS at, 25.5 ng/L, and PFO S at 25.0 ng/L. 3.4 Continuing Calibration During the course of the analytical sequence, several continuing calibration verification samples (CCVs) were analyzed to confirm that the instrument response and the initial calibration curve were still in control. The method acceptance criteria of 100% 25% was met for all analytes. 3.5 Blanks Three types of blanks were prepared and analyzed with the samples: method blanks, solvent blanks, and field/trip blanks. Each blank result was reviewed and used to evaluate method performance to determine the LOQ for each analyte. 3.6 Lab Control Spikes (LCSs) Low and high lab control spikes were prepared and analyzed in triplicate. LCSs were prepared by spiking known amounts of the analytes into 40 mL of reverse-osmosis matrix matched blank water to produce the desired concentration. The spiked water samples were then extracted and analyzed in the same manner as the samples. Analysis of triplicate LCSs at the two specified levels cross-validates the analytical method as used here for any modifications/deviations from ETS 8-154.3. The method acceptance criteria states that the average recovery of all LCS be between 80%-120% with a RSD PAGE 9OF 32 3M EN VIR O N M EN TA L LABORATORY R EPO R T NO. E09-0365 20% . All LCS samples met method acceptance criteria and were used in the determination of analytical uncertainty where applicable. As the reference materials used for quantitation of PFOA and PFOS are predominantly linear, and the analytes present in the water samples are comprised of branched isomers, LCS samples of branched PFOA and PFOS were prepared in triplicate, at two concentrations to evaluate the potential for analytical bias. The average recovery and RSD values for branched PFOA and PFOS met method acceptance criteria. The following calculations were used to generate data in Table 6. Calculated Concentration 100LCS Percent Recovery = % Spike Concentration LCS% RSD = standafd devia tion LCS replicates . 1Q0% average LCS recovery PAGE 10OF32 3M ENVIRO NM ENTA L LABORATORY R EPO R T NO. E09-0365 Table 6. Lab Control S pike Results. ETS-8-154.3 Lab ID PFBA S p ik e d C a lc u la te d Concentration Concentration (ng/L) (ng/L) LCS-090713-1 25.3 24.5 LCS-090713-2 LCS-090713-3 LCS-090713-4 LCS-090713-5 LCS-090713-6 25.3 25.3 1010 1010 1010 23.3 27.5 894 942 1040 Average %RSD 97.1% 7.9% `/R e c o v e r y 96.9 91.9 109 88.5 93.2 103 PFPeA S p ik e d C o n c e n tra tio n (ngA.) C a lc u la te d Concentration (ng/L) 25.3 26.5 25.3 23.8 25.3 25.3 1010 1030 1010 1120 1010 1150 104% 6.9% PFHxA % R eco very Spiked C a lc u la te d Concentration Concentration (ngA-) (n g /Q 105 25.3 24.6 94.0 100 102 25.3 25.3 1010 22.3 22.3 1030 110 1010 1110 114 1010 1130 99.4% 10% `/R e c o v e ry 97.1 88.1 88.1 102 109 112 ETS-8-154.3 PFHpA Lab ID S p ik e d C a lc u la te d Concentration Concentration (ngn.) (ng/L) LCS-090713-1 25.3 26.0 LCS-090713-2 LCS-090713-3 LCS-0907134 25.3 25.3 1010 23.9 24.1 1040 LCS-090713-5 LCS-090713-6 1010 1010 1120 1150 Average %RSD 103% 7.7% `/ R e c o v e ry 103 94.5 95.2 103 111 114 PFOA S p ik e d C a lc u la te d C oncentration Concentration (ngA.) (ngA.) 25.0 27.3 25.0 25.0 25.5 25.4 999 1040 999 1110 999 1140 107% 4.7% PFNA Spiked C a lc u la te d Concentration Concentration %Recovery (ngA.) (ngA.) 109 25.0 28.6 102 25.0 25.3 102 25.0 25.2 104 1000 1090 111 1000 1180 114 1000 1190 111% 7.4% `/R e c o v e r y 115 101 101 109 118 119 p. 71 PAGE 11OF32 3 M ENVIRO NM ENTA L LABORATORY R E P O R T NO . 09-0365 Table 6 continued. Lab Control Spike Results. ETS-8-154.3 Lab ID LCS-090713-1 LCS-090713-2 LCS-090713-3 LCS-090713-4 LCS-090713-5 LCS-09071S6 Average %RSD PEDA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 24.9 25.9 24.9 24.9 997 997 997 23.4 22.8 971 1060 1090 100% 7.3% %Recovery 104 93.9 91.4 97.4 106 110 PFUnA Spiked Calculated Concentration Concentration (ng/L) (ngA.) 25.0 26.3 25.0 25.0 999 999 999 24.2 23.8 1010 1110 1130 104% 7.1% PFDoA Spiked Calculated Concentration Concentration % R eco vetv (ngA.) (ng/L) 105 25.0 25.7 96.7 25.0 22.4 95.3 25.0 23.3 101 1000 939 111 1000 1080 113 1000 1080 99.3% 8.1% "/Recovery 103 89.8 93.3 93.9 108 108 ETS-8-154.3 PFBS Lab ID LCS-090713-1 LCS-090713-2 LCS-090713-3 LCS-090713-4 LCS-090713-5 LCS-090713-6 Spiked Calculated Concentration Concentration (ng/L) (ng/L) 25.5 26.8 25.5 24.8 25.5 24.7 1020 1020 1020 1080 1020 1120 Average %RSD 103% 5.2% %Recovery 105 97.2 96.8 100 106 110 PFHS Spiked Calculated Concentration Concentration (ng/L) (ng/L) 25.0 26.9 25.0 24.3 25.0 24.7 1000 998 1000 1090 1000 1100 104% 5.6% PFOS %Recovery Spiked Calculated Concentration Concentration (ng*-) (ng/L) 108 25.0 27.3 97.0 25.0 25.2 98.7 25.0 25.4 99.8 1000 1030 109 1000 1110 110 1000 1120 106% 4.6% % Recovery 109 101 102 103 111 112 p. 72 PAGE 12OF32 3M E N V IR O N M E N T A L L A B O R A T O R Y R E P O R T NO. E09-0365 Table 6 continued. Lab Control Spike Results. ETS-8-154.3 PFOSA L a b lO LCS-090713-1 LCS-090713-2 ICS-090713-3 LCS-090713-4 LCS-090713-5 LCS-090713-6 S p ik e d C a lc u la te d Concentration Concentration ("9*-) (ngd-) 24.9 29.3 24.9 26.1 24.9 1000 25.6 954 1000 1000 1070 987 % Recovery 118 105 103 95.8 107 99.1 Average %RSD 105% 7.3% ETS-8-154.3 PFBA Lab ID S p ik e d C a lc u la te d Concentration Concentration (ng/L) (ng/L) LCS-090722-1 LCS-090722-2 LCS-090722-3 LCS-090722-4 LCS-090722-5 LCS-090722-6 202 202 202 5050 5050 5050 192 185 183 4490 5810 5880 Average %RSD 100% 13% PFOA PFBS YoRecovery S p ik e d Calculated Concentration Concentration (ng/L) (ng/L) YoRecovery S p ik e d C a lc u la te d Concentration Concentration (ngA.) (ng/L) YoRecovery 95.2 91.5 90.4 89.0 115 117 200 200 200 5000 5000 5000 197 221 217 4110 5110 5290 98.6 110 108 82.2 102 106 204 204 204 5100 5100 5100 220 248 254 4420 5540 5410 108 122 125 66.7 109 106 101% 10% 109% 12% p. 73 PAGE 13OF32 p. 74 3M ENVIR O N M EN TA L LABORATORY R EP O R T NO, E09-0365 Table 6 continued. Lab Control Spike Results. ETS-a-154.3 Lab ID LCS-090722-1 LCS-090722-2 LCS-090722-3 LCS-090722-4 LCS-090722-5 LCS-090722-6 Average %RSD PFOS S p ik e d C o n c e n tra tio n ("90-) Calculated C o n c e n tra tio n (ng/L) 200 192 200 214 200 227 5000 4760 5000 5780 5000 5490 % R eco very 95.8 107 113 95.3 116 110 106% 8.3% ETS-8-154.3 L a b ID LCS-090722-7 ECF LCS-090722-8 ECF LCS-090722-9 ECF LCS-090722-10 ECF LCS-090722-11 ECF LCS-090722-12 ECF Average %RSD PFOA PFOS S p ik e d Calculated Concentration Concentration (n g /m L ) (n g /m L ) % R eco very S p ik e d C a lc u la te d Concentration Concentration (n g /m L ) (n g /m L ) %Recovery 200 200 200 5000 5000 5000 225 229 231 5950 5800 6210 113 199 207 115 199 205 116 199 213 119 4980 5500 116 4980 5580 124 4980 5510 104 103 107 110 112 111 117% 3.3% 108% 3.5% 3.7 Analytical Method Uncertainty Analytical uncertainty is based on historical QC data that is control charted and used to evaluate method accuracy and precision. The method uncertainty is calculated following ETS-12-012.2. The standard deviation is calculated for the set of accuracy results (in %) obtained for the QC samples. The expanded uncertainty is calculated by multiplying the standard deviation by a factor of 2, which corresponds to a confidence level of 95%. Fifty data points were used to determine method uncertainty by this method. PAGE 14OF 32 p. 75 3M EN VIR O N M EN TA L LABORATORY R EPO R T NO. E09-0365 Table 7. Analytical Method Uncertainty. Analyte PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHS PFOS PFOSA : Standard Deviation 9.51 10.3 9.41 8.73 10.3 10.3 8.27 8.91 12.4 9.86 11.5 13.6 11.2 Method Uncertainty 100%19% 100%21% 100%19% 100%18% 100%21% 100%21% 100%17% 100%18% 100%25% 100%20% 100%23% 100%27% 100%22% 3.8 Laboratory Matrix Spike (LMS) A laboratory matrix spike at a nominal concentration of 200 ppt was prepared for sample locations Reach 4 Location 11, as the field matrix spike level (25ppt) did not accurately reflect the concentration detected in the samples of PFBA, PFOA, PFBS, and PFOS. A laboratory matrix spike was prepared on an aliquot of sample E09-0365-031 prior to sample extraction by ETS-8-154.3. LMS recoveries on this sample are presented in Table 18. Laboratory matrix spike recoveries within method acceptance criteria of 10030% confirm that "unknown" components in the sample matrix do not significantly interfere with the extraction and analysis. (IM S Sample Concentration - Average Concentration : Sample & Sample D u p .), __0 LMS Recovery = -- ..... ............................... - .......... .......... ......... - -- * 1 U U / o LMS Spike Concentraton 3.9 Field Matrix Spikes (FMS) A 25ppt (nominal) field matrix spike was collected at each sampling point to verify that the analytical method is applicable to the collected matrix. The field matrix spike was generated by adding a measured volume of field sample to a container spiked by the laboratory with the target analytes prior to shipping sample containers for sample collection. Field matrix spike recoveries within method acceptance criteria of 10030% confirm that "unknown" components in the sample matrix do not significantly interfere with the extraction and analysis of the analytes of interest. Field matrix spikes are presented in the section 4 of this report. Five field matrix spike sample bottles were filled more than 10% over the 200mL fill line. The field matrix spike true value was adjusted accordingly. Sample bottles that were overfilled include: E090365-009 (225mL), E09-0365-012 (225 mL), E09-0365-018 (225 mL), E09-0365-024 (231 mL), and E09-0365-036 (225 mL). FMS Recovery - (Sample Concentration of FMS - Average Concentration .Field Sample & Field Sample D u p.). 10QO/ Spike Concentraton PAGE 15OF 32 p. 76 3M ENVIR O N M EN TA L LABORATORY R E P O R T NO. E09-0365 4 Data Summary and Discussion The tables below summarize the sample results and field matrix spike recovery for the twelve locations as well as the Trip Blank. Each table provides the average concentration and the relative percent difference (%RPD) of the sample and sample duplicate. Results and average values are rounded to three significant figures. Percent relative difference (%RPD) values are rounded to two significant figures. Because of rounding, values may vary slightly from those listed in the raw data. Field matrix spikes meeting the method acceptance criteria of 30%, demonstrate that the method is appropriate for the given matrix. Reach 2 Location 5 - The 25 ppt FMS recovery for PFDA did not meet method acceptance criteria of 100% 30% with a recovery of 68.2%. The analytical uncertainty has been adjusted accordingly for PFDA to 100% 32%. Reach 3 Location 7 - The 25 ppt FMS recovery for PFBA, PFDA, and PFOS did not meet method acceptance criteria of 100% 30% with recoveries of 67.4%, 63.0%, and 67.8%, respectively. The analytical uncertainty has been adjusted accordingly for PFBA to 100% 33%, for PFDA to 100% 37%, and for PFOS to 100% 32%. Reach 4 Location 12 - The 25 ppt FMS recovery for PFOS did not meet method acceptance criteria of 100% 30% with a recovery of 64.1%. The analytical uncertainty has been adjusted accordingly for PFOS to 100% 36%. PAGE 16OF32 3M E N VIRO NM ENTA L LABORATORY R E P O R T NO. E09-0365 Table 8. Reach 1 Location 1. 3M U M S ID Description E09-0365-001 Reach 1 Loc 1 Sample E09-0365-002 Reach 1 Loc 1 Sam ple Dup E09-0365-003 Reach 1 Loc 1 Spike Average Concentration (ng/mLj i %RPD PFBA PFPeA PFHxA PFHpA Concentration (ngn.) %Recovery 4.84 NA 4.76 NA 25.7 82.8 4.80 ng/L 1 1.7% Concentration (ngn.) %Recovery <2.53 NA <2.53 NA 27.8 110 <2.53 ng/L Concentration (ng/L) %Recovery <2.53 NA <2.53 24.6 NA 974 <2.53 ng/L Concentration (ng/L) XRecovery <2.53 NA <2.53 NA 26.4 105 <2.53 ng/L 3M U M S ID Description E09-0365-001 Reach 1 Loc 1 Sample E09-0365-002 Reach 1 Loc 1 Sample Dup E09-0365-003 Reach 1 Loc 1 Spike Average Concentration (ng/mL) %RPD PFOA PFNA PFOA PFUnA Concentration (ngn.) %Recovery <3.00 NA <3.00 26.6 NA 107 <3.00 ng/L Concentration (ng/L) XRecovery <2.50 NA <2.50 24.2 NA 96.6 <2.50 ng/L Concentration (ngn.) %Recovery <2.49 NA <2.49 NA 19.9 79.8 <2.49 ng/L Concentration (ng/L) %Recovery <2.50 NA <2.50 20.0 NA 80.1 <2.50 ng/L PFDoA PFBS PFHS PFOS PFOSA 3M U M S ID Description E09-0365-001 Reach 1 Loc 1 Sam ple E09-0365-002 Reach 1 Loc 1 Sam ple Dup E09-0365-003 Reach 1 Loc 1 Spike Average Concentration (ng/mL) %RPD Concentration Concentration Concentration Concentration Concentration (ng/L) XRecovery (ngn.) % Recovery (ngA.) %Recovery (ngn.) %Recovery (ngn.) %Recovery <3.00 NA <3.06 NA <2.50 NA <2.50 NA <2.99 NA <3.00 NA <3.06 NA <2.50 NA <2.50 NA <2.99 NA 24.9 100 27.7 109 25.1 100 21.9 87.6 30.1 121 <3.00 ng/L <3.06 ng/L <2.50 ng/L <2.50 ng/L <2.99 ngn. MA = Not Applicable p. 77 PAGE 17OF32 3M E N VIR O N M EN TA L LABORATORY R EP O R T NO. E09-0365 Table 9. Reach 1 Location 2. 3M U M S ID Description E09-0365-004 Reach 1 Loc 2 Sample E09-0365-005 Reach 1 Loc 2 Sam ple Dup E09-0365-006 Reach 1 Loc 2 Spike Average Concentration (ng/mL) t %RPO PFBA PFPeA PFHxA PFHpA Concentration (ngA.) %Reco very 6.36 NA 6.50 NA 24.6 71.8 6.43 ng/L 1 2.7% Concentration (ng/L) %Recoverv <2.53 NA <2.53 NA 27.2 108 <2.53 ng/L Concentration (ng/L) %Recovery <2.53 NA <253 NA 25.3 100 <2.53 ng/L Concentration (ngA.) "/R e c o v e ry <2.53 NA <2.53 25.8 NA 102 <2.53 ng/L 3M U M S ID Description E09-0365-004 Reach 1 Loc 2 Sample E09-0365-005 E09-0365-006 Reach 1 Loc 2 Sample Dup Reach 1 Loc 2 Spike Average Concentration (ng/mL) %RPD PFOA PFNA PFOA PFUnA Concentration (ng/L) %Recovery <3.00 NA <3.00 25.3 NA 101 <3.00 ng/L Concentration (ng/L) %Recovery <2.50 NA <2.50 NA 22.6 90.4 <2.50 ng/L Concentration (ng/L) %Recovery <2.49 NA <2.49 18.7 NA 75.0 <2.49 ng/L Concentration (ngri.) % Recovery <2.50 NA <2.50 18.1 NA 72.5 <2.50 ng/L PFDoA PFBS PFHS PFOS PFOSA 3M U M S ID Description E09-0365-004 Reach 1 Loc 2 Sample E09-0365-005 E09-0365-006 Reach 1 Loc 2 Sam ple Dup Reach 1 Loc 2 Spike Average Concentration (ng/mL) %RPD Concentration Concentration Concentration Concentration Concentration (ng/L) %Recovery (ng/L) %Recovery (ng/L) % Recovery (ng/L) % R ecovery (nWL) %Recovery <3.00 NA <3.06 NA <2.50 NA <2.50 NA <2.99 NA <3.00 NA <3.06 NA <2.50 NA <2.50 NA <2.99 NA 22.1 88.4 27.2 107 24.4 97.6 20.2 80.8 27.5 110 <3.00 ng/L <3.05 ng/L <2.50 ng/L <2.50 ng/L <2.99 ng/L NA = Not Applicable p. 78 PAGE 18OF32 3M E N V IR O N M E N T A L L A B O R A T O R Y R EPO R T NO. E09-0365 Table 10. Reach 1 Location 3. 3M U M S ID Description E09-0365-007 Reach 1 lo c 3 Sample E09-0365-008 Reach 1 Loc 3 Sample Dup 09-0365-0091 Reach 1 Loc 3 Spike Average Concentration (ng/mL) %RPD PFBA PFPeA PFHxA PFHpA Concentration ("9*1 5.37 %Recovery NA 5.17 NA 25.1 i 88.5 5.27 ng/mL 3.8% Concentration (ng/L) %Recovery <2.53 NA <2.53 NA 26.5 118 <2.53 ngA Concentration ( 9 U <2.53 %Recovery NA <2.53 NA 23.7 106 < 2 5 3 ng/L Concentration (n& Q %Recovery <2.53 NA <2.53 NA 25.9 115 <2.53 ng/L 3M U M S ID Description E09-0365-007 Reach 1 Loc 3 Sample E09-0365-008 Reach 1 Loc 3 Sample Dup E09-0365-0091" Reach 1 Loc 3 Spike Average Concentration (ng/mL) i %RPD PFOA PFNA PFDA PFUnA Concentration (ngA) %Recovery <3.00 NA <3.00 NA 23.8 107 <3.00 ng/L Concentration %Recovery <2.50 NA <2.50 NA 22.1 99.5 <2.50 ng/L Concentration (ngA.) %Recovery <2.49 NA <2.49 17.9 NA 80.6 <2.49 ng/L Concentration (ngA.) %FRecovery <2.50 NA <2.50 17.7 NA 79.7 <2.50 ng/L PFDoA PFBS PENS PFOS PFOSA 3M U M S ID Description E09-0365-007 Reach 1 Loc 3 Sample E09-0365-008 Reach 1 Loc 3 Sample Dup E09-0365-009"' Reach 1 Loc 3 Spike Average Concentration (ng/mL) %RPD Concentration Concentration Concentration Concentration Concentration (ngA.) %Recovery (ngA.) "/,, R e c o v e r y (ngA.) %Recovery (ngA) %Recovery (ngA) "/,, R e c o v e r y <3.00 NA <3.06 NA <2.50 NA <2.50 NA <2.99 NA <3.00 NA <3.06 NA <2.50 NA <2.50 NA <2.99 NA 22.0 99.1 26.9 119 24.7 111 20.1 90.5 26.8 121 <3.00 ng/L <3.06 ng/L <2.50 ngA <2.50 ngA <2.99 ngA NA=NotApplicable (1) TheFMS samplebottlewasoverfilledandthespikelevelwascorrectedaccordingly. p. 79 PAGE 19OF 32 3M ENVIRO NM ENTA L LABORATORY R E P O R T NO. 09-0365 Table 11. Reach 2 Location 4. 3M U M SIO Description E09-365-010 Reach 2 Loc 4 Sample E09-0365-011 Reach 2 Loc 4 Sample Dup E09-0365-012M) Reach 2 Loc 4 Spike Average Concentration (ng/mL) %RPD PFBA PFPeA PFHxA PFHpA Concentration (ng.) % R ecovery 4.86 NA 5.32 NA 26.2 94.2 5.09 n g /L 9.0% Concentration (ng/L) XRecovery <2.53 NA <2.53 NA 26.5 118 <2.53 ng/L Concentration ( " O '1-) <2.53 %Recovery NA <2.53 24.1 NA 107 <2.53 ng/L Concentration (ng/L) %Recovery <2.53 NA <2.53 NA 25.4 113 <2.53 ng/L 3M U M S ID Description E09-0365-010 Reach 2 Loc 4 Sample E09-0365-011 Reach 2 Loc 4 Sample Dup E09-0365-0121' 1 Reach 2 Loc 4 Spike Average Concentration (ng/mL) t %RPD PFOA PFNA PFDA PFUnA Concentration (ng/L) % R e c o v e /y <3.00 NA <3.00 NA 23.9 108 <3.00 ng/L Concentration (n&L) %Recovery <2.50 NA <2.50 NA 21.4 96.3 <2.50 ng/L Concentration (ng/L) XRecovery <2.49 <2.49 18.0 NA NA 81.1 <2.49 ng/L Concentration (ncf/L) XRecovery <2.50 NA <2.50 NA 19.6 88.3 <2.50 ng/L PFDoA PFBS PFHS PFOS PFOSA 3M U M S ID Description E09-0365-010 Reach 2 Loc 4 Sample E09-0365-011 Reach 2 Loc 4 Sample Dup E 09-0365-0121'1 Reach 2 Loc 4 Spike Average Concentration (ng/mL) t %RPD Concentration Concentration Concentration Concentration Concentration XRecovery (n{0-) XRecovery (n g V XRecovery (n # 1-) XRecovery (ngo.) XRecovery <3.00 NA <3.06 NA <2.50 NA <2.50 NA <2.99 NA <3.00 NA <3.06 NA <2.50 NA <2.50 NA <2.99 NA 24.6 111 25.8 114 23.9 108 19.7 88.7 25.4 114 <3.00 ng/L <3.06 ng/L <2.50 ng/L <2.50 ng/L <2.99 ng/L NA =NotApplicable (1) The FMSsamplebottlewasoverfilledandthespikelevel wascorrectedaccordingly. p. 80 PAGE 20OF32 3M ENVIRONM ENTAL LABORATORY R EP O R T NO. E09-0365 Table 12. Reach 2 Location 5. 3 M U M S ID Description E09-0365-013 Reach 2 Loc 5 Sample E09-0365-014 Reach 2 Loc 5 Sample Dup E09-0365-015 Reach 2 Loc 5 Spike Average C oncentration (ng/mL) i % R PD PFBA PFPeA PFHxA PFHpA C o n c e n tra tio n (ngA.) % Recovery 5.45 NA 4.97 NA 23.7 73.1 5.21 ng/L 9.2% C o n c e n tra tio n (ng/L) % R eco very <2.53 NA <2.53 NA 27.6 109 <2.53 ng/L C o n c e n tra tio n (n& L ) . <2.53 % R eco very NA <2.53 NA 25.5 101 <2.53 ng/L C o n c e n tra tio n (ng/L) % R eco verv <2.53 NA <2.53 NA 27.0 107 <2.53 ng/L 3M LIM S ID D e s c rip tio n E09-0365-013 Reach 2 Loc 5 Sample E09-0365-014 E09-0365-015 Reach 2 Loc 5 Sample Dup Reach 2 Loc 5 Spike Average Concentration (ng/mL) i % R PD PFOA PFNA PFDA PFUnA C o n c e n tra tio n (ngn.) % R eco very <3.00 NA <3.00 NA 24.0 96.1 <3.00 ng/L Concentration (ngn.) % R ecovery <2.50 NA <2.50 NA 21.0 84.0 <2.50 n g/L C o n c e n tra tio n (ng/L) % R eco very <2.49 NA <2.49 17.0 NA 6 8 . 2 ni < 2 .49 ng/LTM Concentration (ngn.) % R eco very <2.50 NA <2.50 17.7 NA 70.9 <2.50 ng/L PFDoA PFBS PFHS PFOS PFOSA 3M U M S ID Description E09-0365-013 Reach 2 Loc 5 Sample E09-0365-014 Reach 2 Loc 5 Sample Dup E09-365-015 Reach 2 Loc 5 Spike Average Concentration (ng/mL) i % R PD C o n c e n tra tio n C o n c e n tra tio n Concentration Concentration Concentration (ngn.) % R ecovcry (ngn.) % Recovery (ngn.) % R ecovery (ng/L) % R eco very (ngn.) % R eco very <3.00 NA <3.06 NA <2.50 NA <2.50 NA <2.99 NA <3.00 NA <3.06 NA <2.50 NA <2.50 NA <2.99 NA 22.6 90.4 27.9 109 25.1 100 19.0 76.0 28.1 113 <3.00 ng/L <3.06 ngn. <2.50 ngn. <2.50 ng/L <2.99 n g n NA = Not Applicable (1) Field matrix spike did not meet method acceptance criteria of 100% 30%. (2) The analytical uncertainty has been adjusted for the recovery of the FM S for PFDA to ` 00% 32%. p. 81 PAGE21OF 32 3M ENVIRO NM ENTA L LABORATORY R EP O R T NO. E09-0365 Table 13. Reach 2 Location 6. 3M LIM SID Description E09-0365-016 Reach 2 Loc 6 Sample E09-0365-017 Reach 2 Loc 6 Sample Dup E09-0365-0181" Reach 2 Loc 6 Spike Average Concentration (ng/mL) %RPD PFBA PFPeA PFHxA PFHpA Concentration (ngA.) %Recovery 7.05 NA 7.46 24.4 NA 76.5 7.26 ng/mL 5.7% Concentration (ngn.) `/,, R e c o v e r y <2.53 NA <2.53 NA 27.5 123 <2.53 ng/L Concentration (ng/L) "/,,Recovery <2.53 NA <2.53 25.9 NA 115 <2.53 ng/L Concentration (ng/L) %Recovery <2.53 NA <2.53 26.2 NA 117 <2.53 ng/L 3M U M S ID Description E09-0365-016 Reach 2 Loc 6 Sample E09-0365-017 Reach 2 Loc 6 Sample Dup Eog-oses-oie1" Reach 2 Loc 6 Spike Average Concentration (ng/mL) t %RPD PFOA PFNA PFDA PFUnA Concentration (ngn.) "/,,Recovery 3.97 NA 3.66 26.9 NA 104 3.82 n g/Lt 8.1% Concentration (ngn.) % Recovery <2.50 NA <2.50 22.7 NA 102 <2.50 ng/L Concentration (ngn.) "/,,Recovery <2.49 NA <2.49 18.7 NA 84.2 <2.49 ng/L Concentration (ngn.) % Recovery <2.50 NA <2.50 19.2 NA 86.5 <2.50 ngn. PFDoA PFBS PFHS PFOS PFOSA 3M U M S ID Description E09-0365-016 Reach 2 Loc 6 Sample E09-0365-017 Reach 2 Loc 6 Sample Dup E09-0365-018'1' Reach 2 Loc 6 Spike Average Concentration (ng/mL) %RPD Concentration Concentration Concentration Concentration Concentration (n g n .) "/,,Recovery (n g n .) %Recovery (ngn.) "/,,Recovery (ngn.) %Recovery (ngn.) '/,, R e c o v e ry <3.00 NA <3.06 NA <2.50 NA 8.48 NA <2.99 NA <3.00 NA <3.06 NA <2.50 NA 8.59 NA <2.99 NA 24.2 109 29.0 128 25.5 115 27.3 84.4 28.4 128 <3.00 ng/L <3.06 ng/L <2.50 non. 8.54 ng/Lt 1.3% <2.99 ngn. NA=NotApplicable (1) The FMS sample bottlewas overfilled and the spike level was corrected accordingly. p. 82 PAGE22OF 32 3M ENVIRONM ENTAL LABORATORY R E P O R T NO. E09-036S Table 14. Reach 3 Location 7. 3M U M S ID Description E09-0365-019 Reach 3 Loc 7 Sample E09-0365-020i,) Reach 3 Loc 7 Sample Dup E09-0365-021 Reach 3 Loc 7 Spike Average Concentration (ng/mL) %RPD PFBA PFPeA PFHxA PFHpA Concentration (ngn.) %Recovery 9.34 NA 26.8 67 .4 (2) 10.2 NA 9.77 ng/mL 8.8% m Concentration (ng.) %Recovery <2.53 NA 26.3 104 <2.53 NA <2.53 ng/L Concentration ("&) <2.53 %Recovery NA 25.2 100 <2.53 NA <2.53 ng/L Concentration (ngo.) `/oRecovery <2.53 NA 25.7 102 <2.53 NA <2.53 ng/L 3M U M S ID Description E09-0365-019 Reach 3 Loc 7 Sample E09-0365-020'" Reach 3 Loc 7 Sample Dup E09-0365-021 Reach 3 Loc 7 Spike Average Concentration (ng/mL) %RPD PFOA PFNA PFDA PFUnA Concentration (ng/L) %Recovery 5.38 NA 27.9 88.7 6.10 NA 5.74 ng/L 13% Concentration (ng/L) `/o R e c o v e r y <2.50 NA 20.8 <2.50 83.2 NA <2.50 ng/L Concentration (ng/L) `/o R e c o v e r y <2.49 NA 15.9 <2.49 6 3 .8 <2i NA <2.49 ng/Li3) Concentration (ngn.) '/oRecovery <2.50 NA 17.8 <2.50 71.3 NA <2.50 ng/L PFDoA PFBS PFHS PFOS PFOSA 3M U M S ID Description E09-0365-019 Reach 3 Loc 7 Sample E09-0365-020(,) Reach 3 Loc 7 Sample Dup E09-0365-021 Reach 3 Loc 7 Spike Average Concentration (ng/mL) %RPD Concentration Concentration Concentration Concentration Concentration (ng/L) `/o R e c o v e r y (ng/L) `/o R e c o v e r y (ng/L) `/o R e c o v e r y (ng/L) `/oRecovery (ng/L) %Recovery <3.00 NA 4.77 NA <2.50 NA 12.4 NA <2.99 NA 24.0 <3.00 96.0 NA 30.8 5.76 100 26.2 105 NA <2.50 NA 29.7 13.1 6 7 . 8 (2> NA 21.6 <2.99 86.7 NA <3.00 ng/L 5.27 ng/L 19% <2.50 ng/L 1 2 .8n g /L 5 .5% m <2.99 ng/L NA = Not Applicable (1 ) Sample duplicate bottle and FM S bottle were switched during either bottle or sample prep. The sample results are presented based on this assumption. (2) Field matrix spike did not meet method acceptance criteria of 100% 30%. (3) The analytical uncertainty has been adjusted for the recovery of the FM S for PFBA to 100% 33% , PFDA to 100% 36% and for PF O S to 100% 32%. PAGE 23OF 32 p. 83 3M E N VIR O N M EN TA L LABORATORY R EP O R T NO. E09-0365 Table 15. Reach 3 Location 8. 3M U M S ID Description E09-0365-022 Reach 3 Loc 8 Sample E09-0365-023 Reach 3 Loc 8 Sample Dup E09-0365-024"' Reach 3 Loc 8 Spike Average Concentration (ng/mL) % RPD PFBA PFPeA PFHxA PFHpA Concentration (ngri.) %Recovery 8.13 NA 8.25 NA 24.9 76.3 8.19 n g /L 1.5% Concentration (ngri.) % R ecovery <2.53 NA 2.55 27.5 NA 113 2.55 n g /L a Concentration (n<0.) <2.53 %Recovery NA <2.53 NA 25.7 118 <2.53 ngri. Concentration (ng/L) %Recovery <2.53 NA <2.53 NA 25.8 118 <2.53 ng/L 3M U M S ID Description E09-0365-022 Reach 3 Loc 8 Sample E09-0365-023 Reach 3 Loc 8 Sample Dup E09-0365-02401 Reach 3 Loc 8 Spike Average Concentration (ng/mL) %RPD PFOA PENA PFOA PFUnA Concentration (ngri.) XRecovery 5.79 NA 4.30 27.5 NA 104 5.05 ngri, 30%IJ> Concentration (ngri.) % R ecovery <2.50 NA <2.50 21.2 NA 97.9 <2.50 ng/L Concentration (ngri.) XRecovery <2.49 NA <2.49 NA 17.5 81.0 <2.49 ngri. Concentration (ngri.) %Recovery <2.50 NA <2.50 19.2 NA 88.9 <2.50 ng/L NA = Not Applicable (1 ) The FMS sample bottle was overfilled and the spike level was corrected accordingly. (2) The sample and sample duplicate produced one result above the LOQ and one result below the LOQ. The reported average concentration represents only the result above the LOQ. A true average was not calculated. (3) The relative percent difference (R P D ) between the sample and sample duplicate exceeded method acceptance criteria of <20%. p. 84 PAGE24OF 32 3M ENVIRONM ENTAL LABORATORY R E P O R T NO . 09-0365 Table 15 continued. R each 3 Location 8. PFDoA PFBS PFHS PFOS PFOSA 3M LIM SID Description E09-0365-022 Reach 3 Loc 8 Sam ple E09-0365-023 Reach 3 Loc 8 Sam ple Dup E09-0365-024(l) Reach 3 Loc 8 Spike Average Concentration (ng/mL) %RPD Concentration (ngA.) <3.00 %Recovery NA Concentration Concentration Concentration Concentration (ng/L) % Recovery ew %Recovery (ngA.) % Recovery .....f r g V XRecovery 5.24 NA <2.50 NA 11.2 NA <2.99 NA <3.00 NA 4.59 NA <2.50 NA 9.76 NA <2.99 NA 25.0 116 29.6 112 25.7 119 28.5 83.3 24.6 114 <3.00 ng/L 4.92 n g/Lt 13% <2.50 ng/L 10.5 n g/Lt 14% <2.99 ng/L MA = Not Applicable (1 ) The FM S sample bottle was overfilled and the spike level was corrected accordingly. (2) The sample and sample duplicate produced one result above the LOQ and one result below the LOQ. The reported average concentration represents only the result above the LOQ. A true average was not calculated. (3) The relative percent difference (RPD) between the sample and sample duplicate exceeded method acceptance criteria of 520%. p. 85 PAGE25OF 32 3 M ENVIR O N M EN TA L LABORA TORY R E P O R T NO. E 09-0365 Table 16. Reach 3 Location 9. 3M U M S ID Description E09-0365-025 Reach 3 lo c 9 Sample E09-0365-026 E09-0365-027 Reach 3 Loc 9 Sample Dup Reach 3 Loc 9 Spike Average Concentration (ng/mL) %RPD PFBA PFPeA PFHxA PFHpA Concentration (ng/L) %Recovery 10.3 NA 10.5 NA 30.9 81.0 10.4 ng/L 1.9% Concentration (n g n .) %Recovery 2.86 NA <2.53 NA 28.4 101 2.86 ng/LTM Concentration (ngA.) %Recovery <2.53 NA <2.53 NA 26.5 105 <2.53 ng/L Concentration (ng/L) %Recovery <2.53 NA <2.53 NA 26.5 105 < Z 53 ng/L 3M U M S ID Description E09-0365-025 Reach 3 Loc 9 Sample E09-0365-026 Reach 3 Loc 9 Sample Dup E09-0365-027 Reach 3 Loc 9 Spike Average Concentration (ng/mL) %RPD PFOA PFNA PFOA PRJnA Concentration (ngn.) %Recovery 5.43 NA 4.78 NA 29.8 98.9 5.11 ng/L 13% Concentration (ngn.) %Recovery <2.50 NA <2.50 NA 23.0 92.0 <2.50 ng/L Concentration (ng/L) %Recovery <2.49 NA <249 NA 18.7 75.0 <2.49 ng/L Concentration (ng/L) %Recovery <2.50 <2.50 20.4 NA NA 81.7 <2.50 ng/L PFDoA PFBS PFHS PFOS PFOSA 3M U M S ID Description E09-0365-025 Reach 3 Loc 9 Sample E09-0365-026 Reach 3 Loc 9 Sample Dup E09-0365-027 Reach 3 Loc 9 Spike Average Concentration (ng/mL) i %RPD Concentration Concentration Concentration Concentration Concentration (ngO.) %Recovery (ngn.) %Recovery (ngn.) %Recovery (ngn.) %Recovery (ngn.) %Recovery <3.00 NA <3.06 NA <2.50 NA 4.35 NA <2.99 NA <3.00 NA <3.06 NA <2.50 NA 3.90 NA <2.99 NA 24.4 97.6 28.6 112 28.0 112 24.8 82.7 27.9 112 <3.00 ng/L <3.06 ng/L <2.50 ngn. 4.13 ng/L 11% <2.99 ngn. NA = Not Applicable (1) The sample and sample duplicate produced one result above the LOQ and one resutt below the LOQ. The reported average concentration represents only the result above the IO Q . A true average was not calculated. p. 86 PAGE26OF 32 3M ENVIRO NM ENTA L LABORATORY R EPO R T NO. E09-0365 Table 17. Reach 4 Location 10. PFBA PFPeA PFHxA PFHpA 3M U M SID Description E09-0365-028 Reach 4 Loc 10 Sample E09-0365-029 Reach 4 Loc 10 Sample Dup E09-0365-030 Reach 4 Loc 10 Spike Average Concentration (ng/mL) %RPD Concentration (n g*-) %Recovery 9.92 NA 9.86 NA 31.2 84.2 9.89 n g /L 0.61% Concentration (ngn.) % R ecavery 3.03 NA 2.66 NA 30.1 108 Z 6 5 n g /L 13% Concentration (ngn.) %Recovery <2.53 NA <2.53 NA 27.5 109 <2.53 ng/L Concentration (ngiL) %Recovery <2.53 NA <2.53 NA 27.5 109 <2.53 ng/L PFOA PFNA PFOA PFUnA 3MLIM SID Description E09-0365-028 Reach 4 Loc 10 Sample E09-0365-029 Reach 4 Loc 10 Sample Dup E09-0365-030 Reach 4 Loc 10 Spike Average Concentration (ng/mL) %RPD Concentration (ngA.) %Recovery 4.45 NA 3.77 29.0 NA 99.7 4.11 n g /L 17% Concentration (ng/L) %Recovery <2.50 NA <2.50 NA 22.4 89.6 <2.50 ng/L Concentration (ngn.) %Recovery <2.49 NA <2.49 NA 17.6 70.6 <2.49 ng/L Concentration (ngn.) %Recovery <2.50 NA <2.50 18.5 NA 74.1 <2.50 ng/L PFDoA PFBS PFHS PFOS PFOSA 3MLIM SID Description Concentration Concentration Concentration Concentration Concentration (ngn.) %Recovery (ngn.) %Recovery (ng/L) %Recovery (ngn.) % Recovery (ngn.) %Recovery E09-0365-028 Reach 4 Loc 10 Sample <3.00 NA <3.06 NA <2.50 NA 4.33 NA <2.99 NA E09-0365-029 Reach 4 Loc 10 Sample Dup <3.00 NA <3.06 NA <2.50 NA 4.11 NA <2.99 NA E09-0365-030 Reach 4 Loc 10 Spike 23.6 94.4 28.5 112 27.9 112 23.2 75.9 26.3 106 Average Concentration (ng/mL) %RPD <3.00 ng/L <3.06 ng/L <2.50 ng/L 4.22 ngn. 5.2% <2.99 ng/L NA = Not Applicable p. 87 PAGE 27OF 32 3M E N V IR O N M E N T A L L A B O R A T O R Y R E P O R T N O . 09-0365 Table 18. R each 4 L ocation 11. PFBA PFPeA PFHxA PFHpA 3M U M SID Description E09-0365-031 Reach 4 Loc 11 Sample E09-0365-032 Reach 4 Loc 11 Sample Dup E09-0365-033 Reach 4 Loc 11 Spike E09-0365-031 Reach 4 Loc 11 Sam ple - 200ppt LMS 200ppt LMS Average Concentration (ng/mL) %RPD Concentration (ngA.) 144 119 NC 291 %Recovery NA NA NC 79.0 132 ngA. 19% Concentration (ng/L) 21.8 26.4 51.8 NA %Recovery NA NA 110 NA 24.1 ngn. 1 9 % Concentration (ngn.) 17.1 19.8 44.3 NA %Recovery NA NA 102 NA ia .5 n g /L 1 5 % Concentration (ngn.) 8.18 10.0 36.3 NA %Recovery NA NA 108 NA 9.09ngn.20% PFOA PFNA PFOA PFUnA 3M LIM SID Description E09-0365-031 Reach 4 Loc 11 Sample E09-0365-032 Reach 4 Loc 11 Sample Dup E09-0365-033 Reach 4 Loc 11 Spike E09-0365-031 Reach 4 Loc 11 Sample - 200ppt LMS 200ppt LMS Average Concentration (ng/mL) %RPD Concentration (ng/L) 113 125 NC 308 %Recovery NA NA NC 94.5 119 ngn. 1 10% Concentration (ngn.) <2.50 <2.50 22.7 NA %Recovery NA NA 90.8 NA <2.50 ng/L Concentration (ng/L) <2.49 <2.49 19.3 NA %Recovery NA NA 77.4 NA <2.49 ng/L Concentration (ngn.) <2.50 <2.50 18.4 NA %Recovery NA NA 73.7 NA <2.50 ngn. NA = Not Applicable NC= Not Calculated; Endogenous level greater than 2x spike level. (1) The relative percent difference (RPD) between the sample and sample duplicate exceeded method acceptance criteria of s20%. p. 88 PAGE 28OF 32 3 M ENVIRO NM ENTA L LABORATORY R EP O R T NO. E09-036S Table 18 continued. Reach 4 Location 11. PFDoA PFBS PFHS PFOS PFOSA 3M U M SID E09-0365-031 Description Reach 4 Loc 11 Sample Concentration (n 9^-) <3.00 %Recovery NA Concentration Concentration Concentration Concentration fns/LJ % Recovery (n&L) %Recovery (ngA.) %Recovery (" W %Recovery 106 NA 37.0 NA 108 NA 3.67 NA E09-0365-032 Reach 4 Loc 11 Sam ple Dup <3.00 NA 70.9 NA 42.1 NA 120 NA 4.08 NA E09-0365-033 Reach 4 Loc 11 Spike 22.7 90.8 NC NC 64.0 97.8 NC NC 30.2 106 E09-0365-031 Reach 4 Loc 11 Sam ple - 200ppt LMS 200ppt LMS NA NA 296 102 NA NA 289 87.5 NA NA Average Concentration (ng/mL) %RPD <3.00 ng/L 88.5 ng/L 40% (,> 3 9 .6 n g /L 1 3 % 114ng/L11% 3.88 ng/L 11% NA = Not Applicable (1) The relative percent difference (RPD) between the sample and sample duplicate exceeded method acceptance criteria of 20%. p. 89 PAGE 29OF 32 3M ENVIRO NM ENTA L LABORATORY R EP O R T NO. E09-0365 Table 19. Reach 4 Location 12. PFBA PFPeA PFHxA 3M U M S ID Description E09-0365-034 Reach 4 Loc 12 Sample E09-0365-035 Reach 4 Loc 12 Sample Dup E09-0365-036O) Reach 4 Loc 12 Spike Average Concentration (ng/mL) %RPD Concentration (ng/L) % R ecovery 35.9 NA 45.1 NA 60.4 88.8 40.5 ng/mL 23% Concentration (ng/L) "/Recovery 7.43 NA 8.23 32.3 NA 109 7.83ng/L10% Concentration (ng/L) 5.91 NA 5.88 NA 31.3 113 5.90 ng/L 0.51% oV'-i1 PFHpA Concentration (ngn.) %Recovery 2.55 NA <2.53 NA 28.3 115 2.55 ng/L PFOA PFNA PFDA PFUnA 3M U M S ID Description E09-0365-034 Reach 4 Loc 12 Sample E09-0365-035 Reach 4 Loc 12 Sam ple Dup E09-0365-036*" Reach 4 Loc 12 Spike Average Concentration (ng/mL) %RPD Concentration (ngO.) % R ecovery 21.7 NA 24.9 NA 44.1 93.7 23.3 ng/L 14% Concentration (ng/L) "/Recovery <2.50 NA <2.50 21.2 NA 95.4 <2.50 ng/L Concentration (n g n .) % Recovery <2.49 NA <2.49 NA 16.7 75.2 <2.49 ng/L Concentration (ngA.) %Recovery <2.50 NA <2.50 15.7 NA 70.7 <2.50 ng/L PFDoA PFBS PFHS PFOS PFOSA 3M U M S ID Description Concentration Concentration Concentration Concentration Concentration (ng/L) %Recovery (ng/L) "/Recovery (n g i) %Recovery _ (ngn.) "/Recovery (ngn.) "/Recovery E09-0365-034 Reach 4 Loc 12 Sample <3.00 NA 24.4 NA 15.6 NA 23.0 NA <2.99 NA E09-0365-035 Reach 4 Loc 12 Sample Dup <3.00 NA 29.4 NA 18.6 NA 26.5 NA <2.99 NA E09-0365-036'1' Reach 4 Loc 12 Spike 18.5 83.3 49.7 101 41.5 101 39.0 6 4 . 1 |4> 25.8 116 Average Concentration (ng/mL) %RPD <3.00 ng/L 26.9 ng/L 19% 17.1 ng/L 18% 24.8 ng/L 14% <2.99 ng/L NA = Not Applicable (1 ) The FMS sample bottle was overfilled and the spike level was corrected accordingly. (2) The relative percent difference (RPD) between the sample and sample duplicate exceeded method acceptance criteria of s20%. (3) The sample and sample dupScate produced o re result above the LOQ and one result below h e LOQ. The reported average concentration represents only the result above the LOQ. A true average was not calculated. (4) Field matrix spike did not meet method acceptance criteria of 100% 30% . (5) The analytical uncertainty has been adjusted for the recovery of the FM S for PFO S to 100% 36%. p. 90 PAGE 30OF 32 3M EN VIRO NM ENTA L LABORATORY R EPO R T NO. 09-0365 Table 20. Trip Blank. 3M U M SID E09-0365-037 E09-0365-038 Description Trip Blank Sample Trip Blank 25 ppt Spike PFBA PFPeA PFHxA PFHpA Concentration (ngA.) <3.03 26.3 %Recovery NA 104 Concentration (nSV <2.53 %Recovery NA 27.5 109 Concentration (n&L) <2.53 27.0 %Recovery NA 107 Concentration (ng/L) <2.53 27.7 %Recovery NA 110 3M U M S ID E09-0365-037 E09-0365-038 Description Trip Blank Sample Trip Blank 25 ppt Spike PFOA PFNA PFDA PFUnA Concentration (ngfi-) <3.00 26.6 Concentration Concentration /Recovery (ng/L) "/Recovery (ng/L) NA <2.50 NA <2.49 107 22.4 89.6 18.3 `/Recovery NA 73.4 Concentration (ng/L) <2.50 16.5 `/Recovery NA 6 6 .1 1' 1 3M U M S ID E09-0365-037 E09-0365-038 Description Trip Blank Sample Trip Blank 25 ppt Spike PFDoA PFBS PFHS PROS PFOSA Concentration Concentration Concentration Concentration Concentration (ng/Q %Recovery (ng/L) `/ R e c o v e ry (ng/L) %Recovery (ngri.) `/Recovery (ng/L) `/ R e c o v e r y <3.00 NA <3.06 NA <2.50 NA <2.50 NA <2.99 NA 12.1 4 8 .3 (,) 28.9 113 28.0 112 21.3 85.2 17.9 71.7 NA = Not Applicable (1) Field matrix spike did not meet method acceptance criteria of 100% 30%. p. 91 PAGE 31 OF 32 3M EN VIR O N M EN TA L LABORATORY R EP O R T NO. E09-0379 5 Conclusion Laboratory control spikes were used to determine the analytical method accuracy and precision for all analytes. The accuracy and precision were then used to estimate the method uncertainty for the results. Field or lab matrix spike recoveries demonstrated that the analytical method was appropriate for the given sample matrix. Analysis was completed following 3M Environmental Laboratory method ETS-8-154.3 "Determination of Perfluorinated Acids, Alcohols, Amides, and Sulfonates in Water by Solid Phase Extraction and High Performance Liquid Chromatography/Mass Spectrometry". Analytical results are reported in Table 1,8, through 20 of this report. q Data / Sample Retention All remaining sample and associated project data (hardcopy and electronic) will be archived according to 3M Environmental Laboratory standard operating procedures. 7 Signatures The 3M Environmental Laboratory's Quality Assurance Unit has audited the data and report for this project. H- Oihh1 Quality Assurance Representative Date PAGE 32OF 32 3M EN VIRO NM ENTA L LABO RATORY REPO RT NO. E09-0372 Final Analytical Report Perfluorochemical Analysis of Fish Fillet Homogenates Collected from the Mississippi River by the Minnesota Pollution Control Agency May 2009 - Phase I: PFOS Laboratory Request Number: E09-0372 Method Requirement: ETS 8-45.0 Testing Laboratory 3M EHS Operations 3M Environmental Laboratory 3M Center Building 260-5N-17 Maplewood, MN 55144 Requester Gary Hohenstein 3M EHS Operations 3M Center Building 224-5W-03 Maplewood, MN 55144 mm 1accredited! Certificate #2052-01 The testing reported herein meet the requirements of ISO/IEC 17025-2005 "General Requirements for the Competence of Testing and Calibration Laboratories", in accordance with the A2LA Certificate #2052-01. Testing that complies with this International Standard also operate in accordance with ISO 9001:2000. 3MENVIRONMENTALLABORATORY PAGE 1OF29 3M ENVIRO NM ENTA L LABO RATORY R E P O R T NO. Em-0372 3M Environmental Laboratory 3M Environmental Laboratory Manager William K. Reagen, Ph.D. 3M Principal Analytical Investigator and Report Author: Michelle D. Malinsky, Ph.D. Analytical Report E09-0372 Perfluorochemical Analysis of Fish Fillet Homogenates Collected from the Mississippi River by the Minnesota Pollution Control Agency May 2009 - Phase I: PFOS 1 Introduction Report Date: Upon Signing The Minnesota Pollution Control Agency (MPCA) submitted thirty fish fillet homogenates to the 3M Environmental Laboratory for perfluorochemical analysis under project number E09-0372. The thirty submitted samples represented an approximate ten percent split of the total samples collected during a May 2009 fish sampling campaign from Pool 2 of the Mississippi River. Five samples from six different species comprised the sample set. The fillet homogenates were extracted and analyzed using method ETS 8-45.0 "Determination of Fluorochemicals via Protein Precipitation of Fish Tissues (Fillet or Whole Body) and Analysis by High Performance Liquid Chromatography with Tandem Mass Spectrometry". The target analytes for this study included perfluoroalkane carboxylic acids ranging from C4 to C12, perfluoroalkane sulfonates (C4, C6, and C8), and perfluorooctanesulfbnamide. This Phase report summarizes the results for perfluorooctane sulfonate (PFOS) only. The results for the other target analytes will be issued in a subsequent Phase II report. The 3M Environmental Laboratory maintains A2LA accreditation to ISO/IEC 17025 for the specific tests/calibrations listed in A2LA Certificate #2052-01 and meets the relevant quality systems requirements of ISO 9001:2000. ETS 8-45.0 falls under the laboratory's current scope of accreditation. The data and final report were audited for compliance to laboratory's ISO/IEC17025 quality system. Table 1 below summarizes the PFOS results. All results for quality control samples prepared and analyzed with the samples will be reported and discussed elsewhere in this report. I\ [accredited! The testing reported herein meet the requirements of ISO/IEC 17025-2005 "General Requirements for the Competence of Testing and Calibration Laboratories", in accordance with the A2LA Certificate #2052-01. Testing that complies with this International Standard also operate in accordance with ISO 9001:2000. Certificate #2052-01 3MENVIRONMENTALLABORATORY PAGE2OF29 3 M ENVIRONM ENTAL LABORATORY R EPO R T NO. E09-0372 Tablei. Sample Results Summary: PFOS m U M S Number E09-0372-001 E09-0372-001 Dup Sem ple D escription Axys ID- L12916-14, Client ID- 090191 Axvs ID- L12916-14, Client ID- 090191 Dup E09-0372-002 E09-0372-002 Dup Axys ID- L12916-24, Client ID- 090054 Axys ID- L12916-24, Client ID- 090054 Dup E09-0372-003 E09-0372-003 Dup Axys ID- L12916-26, Client ID- 090056 Axvs ID- L12916-26, Client ID- 090056 Dup E09-0372-004 E09-0372-004 Dup Axys ID- L12917-3, Client ID- 090275 Axvs ID- L12917-3, Client ID- 090275 Dup E09-0372-005 E09-0372-005 Dup Axys ID- L12917-10, Client ID- 090282 Axys ID- L12917-10, Client ID- 090282 Dup E09-0372-006 E09-0372-006 Dup Axys ID- L12917-17, Client ID- 090123 Axys ID- L12917-17, Client ID- 090123 Dup E09-0372-007 E09-0372-007 Dup Axys ID- L12931-6, Client ID- 090173 Axys ID- L12931-6, Client ID- 090173 Dup E09-0372-008 E09-0372-008 Dup Axys ID- L12931-14, Client ID- 090032 Axys ID- L12931-14, Client ID- 090032 Dup E09-0372-009 E09-0372-009 Dup Axys ID- L12932-2, Client ID- 090094 Axys ID- L12932-2, Client ID- 090094 Dup E09-0372-010 E09-0372-010 Dup Axys ID- L12932-4, Client ID- 090096 Axys ID- L12932-4, Client ID- 090096 Dup S p e c ie s Carp Carp Carp Carp Carp Carp Smallmouth Bass Smallmouth Bass Smallmouth Bass Smallmouth Bass R iver L o c a tio n Section 3 A v e ra g e %RPD Section 1 A v e ra g e %RPD Section 1 A verag e %RPD Section 4 A verag e %RPD Section 4 A verag e %RPD Section 2 A verag e %RPD Section 3 A verag e %RPD Section 1 A verag e %RPD Section 2 A verag e %RPD Section 2 A verag e %RPD 111P F O S Cone, (n g /g ) 45.0 46.5 45.8 3.2 27.1 25.4 26 3 6.3 4.90 5.79 5.35 17 96.1 94.3 95.2 1.9 15.6 17.0 16.3 8.5 17.9 18.1 18.0 1.2 41.3 39.8 40.6 3.8 26.9 31.7 29.3 16 10.8 13.2 12.0 20 15.1 14.4 14.8 4.2 3MENVIRONMENTALLABORATORY PAGE3OF29 3M ENVIRO NM ENTA L LABO RATORY R E P O R T N O Em-0372 Table 1 Continued. 3M LIM S N um ber E09-0372-011 E 09-0372-011 Dup S a m p le Description Axys ID- L12932-9, Client ID- 090042 Axys ID- L12932-9, Client ID- 090042 Dup S p e c ie s Smallmouth Bass E09-0372-012 E09-0372-012 Dup Axys ID- L12932-26, Client ID- 090248 Axys ID- L12932-26, Client ID- 090248 Dup Smallmouth Bass E09-0372-013 E09-0372-013 Dup Axys ID- L12933-18, Client ID- 090064 Axys ID- L12933-18, Client ID- 090064 Dup White Bass E09-0372-014 E09-0372-014 Dup Axys ID- L12933-20, Client ID- 090066 Axys ID- L12933-20, Client ID- 090066 Dup White Bass E09-0372-015 E09-0372-015 Dup Axys ID- L12933-25, Client ID- 090071 Axys ID- L12933-25, Client ID- 090071 Dup White Bass E09-0372-016 E09-0372-016 Dup Axys ID- L12934-10, Client ID- 090024 Axys ID- L12934-10, Client ID- 090024 Dup White Bass E09-0372-017 E09-0372-017 Dup Axys ID- L12934-12, Client ID- 090026 Axys ID- L12934-12, Clienl ID- 090026 Dup White Bass E09-0372-018 E09-0372-018 Dup Axys ID- L12934-18, Client ID- 090017 Axys ID- L12934-18, Client ID- 090017 Dup White Bass E09-0372-019 E09-0372-019 Dup E09-0372-020 EQ9-0372-020 Dup Axys ID- L12945-1, Client ID- 090153 Axys ID- L12945-1, Client ID- 090153 Dup Fresh W ater Drum Axys ID- L12945-4, Client ID- 090167 Axys ID- L12945-4, Client ID- 090167 Dup Fresh W ater Drum R iver L o c a tio n Section 1 A v e ra g e %RPD Section 4 A verag e %RPD Section 2 A verag e %RPD Section 2 A verag e %RPD Section 2 A verag e %RPD Section 1 A verag e %RPD Section 1 A verag e %RPD Section 1 A verag e %RPD Section 3 A verag e %RPD Section 3 A v e ra g e %RPD '''P FO S Cone. (n g /g ) 13.7 15.3 14.5 11 12*581 <2)558 <2)570 4.0 52.0 56.4 54.2 8.1 71.5 71.0 71.3 0.82 65.0 62.2 63.6 4.5 477 50.9 49.3 6.6 71.7 65.8 68.7 8.5 86.4 82.4 84.4 4.7 113 103 108 9.1 82.1 82.3 82.2 0.24 3MENVIRONMENTALLABORATORY PAGE4OF29 3M EN VIRO NM ENTA L LABO RATORY REPORT NO. E m -0372 Table 1Continued. 3M L IM S N u m b er S am ple D escription S p e c ie s R iver L o c a tio n ,vPFO S Cone. (ng/g) E09-0372-021 E09-0372-021 Dup Axys ID- L12945-14, Client ID- 090241 Axys ID- L12945-14, Client ID- 090241 Dup Fresh W ater Drum Section 4 A verag e 246 225 23.6 %RPD 8.9 E09-0372-022 E09-0372-022 Dup Axys ID- L12945-16, Client ID- 090078 Axys ID- L12945-16, Client ID- 090078 Dup Fresh W ater Drum Section 2 A verag e 74.9 80.4 77.7 %RPD 7.2 E09-0372-023 E09-0372-023 Dup Axys ID- L12945-19, Client ID- 090081 Axys ID- L12945-19, Client ID- 090081 Dup Fresh W ater Drum Section 2 A v e ra g e 41 3 32.9 37.1 %RPD 23 E09-0372-024 E09-0372-024 Dup Axys ID- L12945-30, Client ID- 090009 Axys ID- L12945-30, Client ID- 090009 Dup Fresh W ater Drum Section 1 A v e ra g e 14.7 13.7 14.2 %RPD 7.0 E09-0372-025 E09-0372-025 Dup Axys ID- L12947-7, Client ID- 090266 Axys ID- L12947-7, Client ID- 090266 Dup Bluegill Sunfish Section 3 A verag e 34 5 32.1 33.3 %RPD 7.2 E09-0372-026 E09-0372-026 Dup Axys ID- L12947-8, Client ID- 090267 Axys ID- L12947-8, Client ID- 090267 Dup Bluegill Sunfish Section 3 A verag e 55.1 55.5 55.3 %RPD 0.75 E09-0372-027 E09-0372-027 Dup Axys ID- L12947-13, Client ID- 090111 Axys ID- L12947-13, Client ID- 090111 Dup Bluegill Sunfish Section 2 A verag e 40.6 40.0 40.3 %RPD 1.5 E09-0372-028 Axys ID- L12947-25, Client ID- 090205 Bluegill Sunfish Section 4 93.2 E09-0372-028 Dup Axys ID- L12947-25, Client ID- 090205 Dup A verag e 80.6 86.9 %RPD 14 E09-0372-029 Axys ID- L12947-26, Client ID- 090206 Bluegill Sunfish Section 4 31.4 E09-0372-029 Dup Axys ID- L12947-26, Client ID- 090206 Dup A verag e 28.2 29.8 E09-0372-030 Axys ID- L12948-17, Client ID- 090061 Bluegill Sunfish %RPD Section 1 11 0)129 E09-0372-030 Dup Axys ID- L12948-17, Client ID- 090061 Dup <3,141 A verag e <31135 %RPD 8.9 (1) Unless otherwise specified, the recovery of associated laboratory matrix spike (LMS) was within 100t30% which meets ETS 8-45 0 method acceptance criteria. Sample results are considered accurate to within the overall analytical method uncertainty 100+18% (PFOS) See Section 4.9 Determination o fAnalytical Method Uncertainty lor more information. Sample results are reported to three significant figures and %RPD to two significant figures. Additional significant 3MENVIRONMENTALLABORATORY PAGE 5OF 29 3 M ENVIRONMENTAL LABORATORY REPORT NO. Em-0372 figures were used to calculate the average, %RPD, and %recoveiy. Values in the raw data may vary slightly due to rounding. (2) Sample results were reported from a 1:100 post-extraction dilution. (3) LMS recovery was 67.4%, sample accuracy has been adjusted to 10050%. 2 Study and Sample Information 2.1 Target Analytes. Table 2 belowprovides pertinentinformationregardingthetargetanalytes, internal standards, and surrogate recoverystandardsinvestigatedinthisstudy. Surrogate recoverystandardswereseparate isotopicallycompoundsspiked intoeach sample aliquotpriortoextraction. The recoveryofthe surrogatewas used toevaluatetheoverall extraction process and anypotential matrixeffects. Table 2. Target Analyte Summary. Compound Name Perfkjorobutanoic acid Perttuoropentanoic add Perfluorohexanoic add Perfluoroheptanoic acid Synonym or Acronym PFBA (04 Acid) PFPeA (C5 Add) PFHxA (C6 Add) PFHpA (C7 Acid) Perfluorooctanoic add PFOA (C8 Add) Perfluorononanoic acid Perfluoradecanoic acid Perfluoroundecanoic add Perfluorododecandc add Perfluorabutane sulfonate Perfluorohexane sulfonate PFNA (C9 Add) P F D A (C IO A d d ) PFUnA (C11 Add) PFDoA (C12 Add) PFBS (0 4 Sulfonate) PFHS (C6 Sulfonate) Perfluorooctane sulfonate PFOS (C8 Sulfonate) Peffluorooctanestifonamide FOSA(C8 Sulfonamide) F o rm u la CsFtCOOH C ,F bC O O H C5F 11C O O H CsFnCOOH C 7F 15C O O H CiF^COONHT CgF^COOH OF^COOH C tQF21COOH Ci i Fj3COOH OFsSQX CnF^SQjNa" CbF 17SQ,1C C s F ^ S O jlC C a F ^ O jN H j A n a ly tic a l Purpose Reference Standard Source Taiget Target Target Taget Target Target Target Target Target Target Target Target Aldrich Alfa Aesar Oakwood Products Aldrich L-PFQA (linear) Wellington Labs ECF PFOA (branched) 3M Production Lot 332 Oakwood Products Oakwood Products Oakwood Products Oakwood Products 3M Production Lot 2 L-PFHS (linear) Wellington Labs L-PFOS (linear) Wellington Labs ECF PFOS (branched) 3M Production Lot 217 Target 3M (L-15709) 3MENVIRONMENTAL LABORATORY PAGE 6OF 29 3M ENVIRO NM ENTA L LABO RATORY REPO RT NO. E09-0372 Table 2 Continued. Compound Name ,3G,-PerfluorobutanoK; add Synonym or A cro n ym [1 ,2,3,4-13G i]PFBA " CrPerfluorobexanotc add [1,2 -13CJPFHxA '3G,-Perfluorooctanotc add [1,2,3,413C l]PFOA "Cs-PeifliJorononiBXJtc add [1^,3,4,5-13C5]PFNA ,3QrPerftuorodecanotc aad [1,2 -,3CJPFDA ,3C2-PertuonxrtdecancHC aad [1,2 -'3CyPFUnA ,3C2-Perfluofododecano(c add Ammonium Perfluorobutane sulfonate ,8Oi-Ammonium Perfluorohexane sulfonate " C-Sodium Perfluorooctane sulfonate '"QrPerftuorooctanesuttbnamide [1 ,2 -'3CJPFDqA [,8Oi]PFBS [18Q J P F H S [1,2,3,4-13C]PFOS ['"C y F O S A ,3C;rPerfiuorooctanotc add ,8QrAmmonium Perfluorooctane sulfonate [1,2-13C2]PFOA [,8Oj]PFOS Form ula 13CF3(13CF2)213COOH CF3<CF2)3(13CF2),3COOH C F 3(CF2)3( ,3CF2)313C O O H C F 3(CF2)3( ,3CF2),13C O O H C F 3(C F 2)7(13C F 2),3C O O H CF 3(C F 2)b(13C F 2)13C O O H A n aly tic al Purpose IS IS IS IS IS IS IS [C4F(lS 18Q 2O r N lV IS [C,F13S,80 20rN F L * CF3(CF2)3(13CF2)313CF2S Q j` Na" [CbFi7S180 2NH2] CF3(CF2)5(13CF2) 13COOH IS IS IS Surrogate [CsF17S'8Q 20r NFL* Surrogate Reference Standard Source Wellington Labs Wellington Labs Wellington Labs Wellington Labs Wellington Labs Wellington Labs Wellington Labs RTI International Wellington Labs Wellington Labs RTI International Perkin Elmer RTI International 2.2 Sample Collection and Receipt. OnAugust6,2009, the3MEnvironmental Laboratoryreceivedthe homogenizedfilletsamples in Nalgene bottlesondry ice. The sampleswere logged intothe 3M Environmental LaboratoryLIMS systemunderprojectE09-0372 and placed infrozenstorage. No informationwas provided regarding the sampling date. Itshould be notedthatthesefish samples have been previouslyhandled andanalyzed atanother laboratoryundercontract bythe MPCA. Itis unknown howthese samples have been handledand if theintegrityofthesesamples has been comprised priortoreceipt. 3MEnvironmental Laboratorypersonnel removed the homogenized fishtissuefromthesample container bycuttingthe bottleawayfromthefrozen sample mass usinga dean utilityknife. The frozen sample masswasthen rehomogenized before extraction. See Section 3.1 formore information. Based onthesampleconsistency inthe Nalgene bottles, itappeared thatthesample homogenates hadthawedatsome pointbeforethey arrivedatthe3M Environmental Laboratory. (Homogenized tissue had refrozen intoa solid mass thatcould notbe broken upwhilefrozen inthecontainer.) 3 Methods - Analytical and Preparatory 3.1 Tissue Preparation Each submittedsampleand biuegill filletcontrol tissue (TN08-0220-1/1) purchased fromOsage Catfisheries, Inc. (Osage Beach, MO)were rehomogenized frozen using dry ice. 3MENVIRONMENTALLABORATORY PAGE 7OF 29 p. 100 3M ENVIRO NM ENTA L LABO RATORY REPO RT NO. E09-0372 Frozen fishhomogenatewas added toa pre-chilledstainless steel bowl ofa RobotCoupe RSI 2Y-1 vertical batchprocessorand homogenizedwithdryice until a fine powderconsistencywas reached. Afterhomogenization, thegroundfishtissuewastransferredtoa polyethylenebagwhichwas placed in thefreezerat-20Cunsealedovernighttoallowthe residual carbondioxidetosublime. After sublimation, thebagwas sealed and homogenateswere keptfrozen. 3.2 Sample Extraction A 0.25gsub-sampleofthefishtissue homogenatewasaccuratelyweighed ina 50mL polyethylene centrifugetube. Tissue aliquotswerethen spikedwithinternal standards (ISs)and surrogatesto produceanapproximateconcentrationof 1ng/g. Samples designatedas labmatrixspikes or matrixmatched calibrationstandardswere additionallyspikedwiththetargetand surrogateanalytesat appropriate levelstoproducethedesiredtissue concentrations. Samples intendedforlaboratoryQC (laboratorycontrol matrixspikes)werespikedwithsurrogates at 1ng/gandtheothertargetanalytesat approximately0.5 ng/g, 1.5ng/g, and8 ng/g. Afterspiking, thetissue homogenateswereallowedtosit for30minutesbefore2.5 mLofacetonitrilewasadded. The sampleswerethenthoroughly homogenizedwiththeacetonitrile usingan Omni Prep multi-placehomogenizerwithdisposable plastic probes (15,000 rpmfor2 minutes). The acetonitrile/tissueextractswere thenplaced inafreezer at20Cforatleastone hour. Upon removal fromthefreezer, sampleextractswere centrifugedat a targetedtemperatureof-5C for20minutesat3000 rpm. Aftercentrifugation, 1mLofclarified supernatantwastransferredtoa2 mLautovial spikedwith 10pL of 10%formicacid. Autovialswerethencapped and vortexmixed. Sampleswereextracted inthreeseparate batches. Foreach submittedsample, a sample, sample duplicate, and laboratorymatrixspike(LMS)were prepared. Each extractionbatch includedthe followingqualitycontrol samples: athirteenpointextracted matrixcalibrationcurve usingthe purchased bluegill filletcontrol tissue triplicatelabcontrol spikesofthebluegill filletcontrol tissueatthree levelsofall targetanalytes (0.5ng/g, 1.5ng/g, and 8ng/g) triplicatelabcontrol spikesof3Melectrochemical fluorination (ECF) PFOA and PFOS at5 ng/g triplicatelabcontrol spikes of PFOS onlyat 100ng/g duplicatecontrol matrixblankswithandwithoutinternal standards and surrogates duplicate method(aqueous) blankswithandwithout internal standardsand surrogates Thetable belowsummarizesthe preparation datesand samples prepared ineach batch. Table 3. Sample Preparation Summary. Batch Num ber Batch 1 Batch 2 Batch 3 Preparation Dates 8/25/2009 - 8/26/2009 8/27/2009 - 8/28/2009 8/31/2009 - 9/1/2009 Sam ples E09-0372-001 to E09-0372-010 E09-0372-021 to E09-0372-030 EQ9-0372-011 to E09-0372-020 3.3 Analysis Analysisforthe PFCs listedinTable 2was performed usinghighperformanceliquidchromatographytandemmass spectrometry(HPLC/MS/MS). Forthisinvestigation, sampleswereanalyzed usingan Agilent 1100series (PaloAlto, CA) HPLC systeminterlacedtoeithera PE SCIEXAPI4000triple quadrupole orSCIEX API 4000Q-Trap mass spectrometer(FosterCity, CA). Both instrumentswere equippedwitha SCIEX TurboV ion-spray interfaceoperating inthenegative ionMS/MS mode using multiple reaction monitoring(MRM). AnalystTM 1.4.2softwarewas usedforall datacollection and 3MENVIRONMENTAL LABORATORY PAGE8OF29 p. 101 3M EN VIRO NM ENTA L LABO RATORY REPO RT NO. E09-0372 reduction. Table4 liststhe MRMtransitionsmonitoredforeach analyte. A Thermo Scientific PRISM RP guard column (2.1mm*50mm; 5pparticlesize)was placed in-lineafterthe purgevalveand before thesample injectionporttotrapany PFC contaminantscomingfromthe HPLC instrument and/orthemobilephases. This sufficientlyseparated theelutionofthe"system" PFC peaksfromthose present inthesample extracts. 3MENVIRONMENTALLABORATORY PAGE9OF29 p. 102 3M ENVIRO NM ENTA L LABO RATORY REPORT NO E m -0372 Table 4. MRM Transition Summary. Compound PFBA (C4 Acid) PFPeA (C5 Add) PFHxA (C6 Add) PFHpA (C7 Add) A nalyte Description Target Target Target Target PFOA (C8 Add) Target PFNA (C9 Add) Target P F D A (C ID A d d ) Target PFUnA(C11 Acid) Target PFDcA (C12 Acid) PFBS (C4 Sulfonate) PFHS (C6 Sulfonate) Target Target Target PFOS (C8 Sulfonate) FOSA (C8 Sulfonamide) [1 ,2 ,3 ,4 - 13C4]PFBA [ 1 , 2 - 13C2]PFHxA [1,2,3,4-'3GJPFOA [1,2 ,3 ,4 ,5 -'3C 5]PF NA [1,2 -13Q,]PFDA [1,2 -'"CdPFUnA [1,2 -13CyPFDoA [180 2]PFBS ['"O J P F H S [1,2,3,4- ,3C4]PFOS [180 2]F0SA [1,2- 13CJPFOA ['"OjJPFOS Target Target IS for PFBA and PFPeA IS for PFHxA IS for PFHpA and PFOA IS for PFNA IS for PFDA IS for PFUnA IS for PFDoA IS for PFBS IS for PFHS IS for PFOS IS for FOSA Surrogate (Adds) Sunggate(Sulfonates, FOSA) IVM RM Transitionfs) 213>169 263>219 313>269 3 1 3 > 1 19 363>319 363>169 413>369 413>219 413>169 463>419 463>219 463>169 513>469 513>269 513>219 563>519 563>269 563>219 613>569 613>319 613>169 299>80 299>99 399>80 399>99 499>80 499>99 499>130 498>78 217>172 315>270 417>372 468>423 515>470 565>520 615>570 303>84 403>84 503>80 502>82 415>370 503>84 D w ell Tim e (m s) 100 100 100 100 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 100 100 50 50 50 50 50 50 50 50 50 50 50 3MENVIRONMENTAL LABORATORY PAGE 10OF29 p. 103 3M ENVIRONM ENTAL LABORA TOR Y REPO RT NO. E09-0372 Analysis oftheshort-chain acids (C4 throughC6) was performed usinga Thermo Scientific PRISMRP column (2.1mmx50mm; 5p particlesize) heldat30Cwiththemobile phase systemconsistingof5 mMammoniumacetatewith0.01%acetic add inwater(A)and methanol <B). The gradientused to elutetheanalytesof interestis presented inTable 5. The flowratewas heldat300 pL/minthroughout therunand a20 pL injectionvolumewas used. Theoutletoftheanalytical columnwasdirectedtoa column switchingvalvewherethefirstthree minutesofthe runweredivertedtowaste. Afterthree minutes, thevalvewas switchedtodirecttheeffluenttothe mass spectrometerforanalysis. The large-chainadds (C7throughC12), thesulfonates, and FOSAwereanalyzed usingaThermo Sdentific BetasilTM C18 analytical column(2.1mm* 100mm; 5p particlesize) heldat30Cwiththe mobilephase systemconsistingof2 mMammoniumacetateinwater(A) and acetonitrile(B). The gradient used isalso provided inTable 5. The flowratewas heldat400pL/minthroughouttherunand a25 pL injectionvolumewas used. Sampleswereinjectedontoa Waters (Milford, MA) OasisHLB on-lineextractioncolumn (3.0 mm*20 mm, 25 ppartidesize)withtheoutletdirectedtoa column switchingvalvewherethefirstfive minutesweredivertedtowaste. Afterfive minutes, thevalvewas switchedandtheeffluentwas directedtotheanalytical columnforseparationofthetargetanalytesand analysis bythemass spectrometer. Table 5. LC Gradient Parameters. S m a ll A d d s : C4-C6 Large A d d s : C7-C12: Sulfonates, FOSA Step 0 1 2 3 4 5 6 Total Tim e (min) 0.0 3.0 3.5 9.0 15.0 15.1 19.0 %A 90 90 30 5.0 5.0 90 90 %B 10 10 70 95 95 10 10 A 5 mM ammonium acetate with 0.01% acetic add (aq) B Methanol Step 0 1 2 3 4 5 6 7 8 A B Total Time (m in ) 0.0 3.0 3.5 13.5 15.5 16.0 180 18.3 21.0 %A 97 97 70 40 40 10 10 97 97 2 mM ammonium acetate (aq) Acetonitrile %B 3.0 3.0 30 60 60 90 90 3.0 3.0 To manage thelarge numberoftransitionsrequiredforthelargeacids, sulfonates, and FOSA, a multiperiodmethodwas constructed. The `firstperiod (time=0minutesto 11 minutes)collected the transitionsfor PFBS, PFHpA, PFOA, [1,2- 13C2]PFOA, PFHS, PFNA andtheirrespective ISs. The second period (time=11minto21.0minutes) collectedthetransitionsfor PFDA, PFUnA, PFOS, [1802]PF0S, PFDoA, and FOSA and theirrespective ISs. Foranalyteswhere morethanonetransition was acquired, atotal ionchromatogram(TIC)whichsummed the respectivetransitionsforthatanalyte was usedanalyzethedata. ' Exact location of the period break may vary as individual analytical columns may perform differently or if instrument tubing is changed. 3MENVIRONMENTALLABORATORY PAGE 11OF29 p. 104 3M E N VIR O N M EN TA L LABORATORY REPO RT NO. E09-0372 4 Data Analysis 4.1 Calibration Extracted 'matrix-matchedcalibrationstandardsand QCs wereprepared byspikingknownamounts of targetanalytes, surrogates, and internal standards intoindividual 0.25g aliquotsofbluegill filletcontrol tissue (TN08-0202-1/1)fishtissue homogenate. Each spikedfishaliquotwasthen extractedusingthe proceduresoutlinedinSection 3.2. A total ofthirteenspikedstandards rangingfrom0.25ng/gto300 ng/g(nominal)were prepared. Additionally, an unextractedacetonitrilesolvent curve rangingfrom 0.0025ng/mLto50ng/mLwas also preparedwhichisequivalent to0.025 ng/gto500 ng/gtissue concentration. All sample results forPFOS and [^OJPFOS werequantitatedagainsttheextracted, matrix-matchedcalibrationcurve. To demonstrateequivalency, thelaboratorycontrol QC samples werequantitatedusingthesolvent curve. The recoveriesoftheQC samplesquantitatedagainstthe unextractedacetonitrilecalibrationcurveare provided intheSupplemental InformationSection 10.2. A quadratic, 1/xweightedcalibration curvewas usedtofitthedatafor PFOS and [^OJPFOS. Internal standardquantitationwas used. The datawasnotforcedthroughzeroduringthefittingprocess. The accuracyofeach curve pointwas verifiedby back-calculatingtheconcentration usingtheareacount ratioofthetargetanalytetothe internal standard. Each solventcalibrationstandard usedtogenerate thefinal calibrationcurve metthe methodcalibrationaccuracy requirementof 10025%, exceptthe LOQ standard(10030%). The coefficientsofdetermination (r2)weregreaterthan 0.990forall analytes. As required byETS 8-45, a minimumofsixcalibrationpointswere used togeneratethefinal calibration curve. For PFHS, PFOS, and PFOA, the reference standard usedforcalibrationand labcontrol spikeswas comprised predominantlyofthelinear isomer. A separate setofLCSs usinganelectrochemical fluorination(ECF) sourceofPFOS and PFOAwas also included. *As fish matrix can vary greatly from species to species, the control matrix used to generate the extracted calibration curve and laboratory control (X ) samples is considered to be matrix-matched for the bluegill samples only. The laboratory control matrix should be considered as a "surrogate" control matrix for the other species investigated in this study. 4.2 Limit of Quantitation (LOQ) The LOQ as defined inETS 8-45isthe lowest non-zerocalibrationstandard inthecurve inwhichthe areacountsofthetargetanalyteareatleasttwicethoseofthe matrixblank(s). Since PFOS was detected inthecontrol matrixata measurable level, the methodofstandard additionwas used to determinetheendogenousconcentration. The resultantendogenousconcentrationwasthen usedto correctthe PFOS concentration intheextractedcalibrationstandardsand QC samples. 4.3 System Suitability Three replicate injections ofa solventcalibration standardwereanalyzed atthebeginning ofthe analytical sequencetodemonstrate overall systemsuitability. Methodcriteriastatesthatsystem suitabilityinjectionsshall produce a RSD oflessthan7%forthe ratiooftargetanalytearea countsto internal standard area countsand an RSD oflessthan2%forthe retentiontime. Methodacceptance criteriawere metforboth PFOS and [^OJPFOS forthesamples analyzed inthefirstandthirdprep batches. The %RSDsofthe area count ratiointhesecond prepbatchanalysiswere 10%and 11%for PFOS and [1802]PFOS, respectively. A methoddeviationhas been issued and is included inthedatapackage. The overall impacttothe sample resultsisconsidered minimal. An increase invariabilityintheareacount precision isoften observedwithan increased numberof MRMtransitionscollectedwithinagiven periodofthedata acquisitionmethod. Witha large numberofMRMs, fewerscans acrossthechromatographicpeakare collected and overall peak shapecan vary morefrominjectiontoinjection. However, thecalibration 3MENVIRONMENTALLABORATORY PAGE 12OF29 3M ENVIRONM ENTAL LABORATORY REPO RT NO. E09-0372 curve, QCs, andsamples all experiencethe same conditions. Any increasedvariabilityobserved inthe systemsuitabilityinjectionswouldalso beobserved inthe LCS datawhich is usedtodetermineoverall methoduncertainty. Thus, thevariabilityisaccounted for intheassigned methoduncertaintyreported withthesample results. 4.4 Continuing Calibration Duringthecourseoftheanalytical sequence, several continuingcalibrationverificationsamples (CCVs) wereanalyzedtoconfirmthatthe instrument responsefrominitial calibrationcurvewasstill in control. CCV injections produced recoveriesof PFOS and [1802]PF0S within 100%25%, whichmet method criteria. 4.5 Blanks Fivetypesofblankswere prepared andanalyzedwiththesamples: matrixblanksofbluegill fillet control tissue (twowith ISandsurrogate, twowithout ISandsurrogate), aqueous methodblanks (two with ISand surrogate, twowithout ISand surrogate), acidified acetonitrilesolvent blanks, acetonitrile blankswithinternal standardsand surrogates, and acetonitrilesolvent blanks (unmodified). Each blank resultwas reviewedand used toevaluatemethod performancetodeterminethe LOQ foreach analyte. Surrogate recoveriesofspiked blanksare provided intheSupplemental InformationSection 10.3. 4.6 Lab Control Spikes (LCSs) Triplicate labcontrol spikesofthepurchased bluegill filletcontrol matrixatthreedifferentlevelsforall analyteswere prepared each extractiondaytodetermineanalytical method uncertainty(See Section 4.9). ForPFHS, PFOS, and PFOA, thestandard reference material usedforthe LCS spikeswas the linearisomer, whichwasthesame usedforthecalibrationcurves. Additional triplicate PFOS LCSs at 100ng/gwereprepared. Separate 3Melectrochemical fluorination (ECF) spikes ofbranched PFOS and PFOAwereprepared toevaluateany potential biasfromquantitationagainsta linearstandard. Lab control spikeswerepreparedtoevaluate methodaccuracyand precision andwereusedto determineanalytical method uncertainty(See Section 4.9). The [1802]PF0S surrogatewasspiked ata consistent 1ng/g(0.1 ng/mL)forall LCS samples. For PFOS, thespiked concentrationwas corrected fortheaverage PFOS concentrationdeterminedforthecontrol matrixinthesame extractionbatch. Lab control spike recoveries areprovided intheSupplemental Information(Section 10.1). For both PFOS and [1OJPFOS, all replicates(N=45) produced recoverieswithinmethodacceptance criteria 100%25%. 4.7 Sample Concentration Calculation The extractedcalibrationcurve usedforquantitationprovidedextract concentration inunitsofng/mL. Thefollowingequationwas used toconverttheextractconcentrationtosampletissue concentration in unitsof ng/g. Tissue Concentration (-- ) 9 Extraction Volume = 2.5 ml_ Extracted Mass -0.2 5 g Extract Concentration (-22.)* ExtractionVolume(mL) _____________________ m L ______________________ Extracted Mass (g) 4.8 Lab Matrix Spikes (LMSs) Foreach submittedsample, a separate laboratorymatrixspikewas prepared byextractinga separate aliquotofthefillettissuethatwasspikedwiththetargetanalytes. For each LMS, all targetanalytes werespiked ata nominal concentrationof 10ng/gexcept PFOS, whichwas spiked ata concentration of approximately 110ng/g. The recoveryofthe LMSwas calculated usingthefollowingequation. 3MENVIRONMENTALLABORATORY PAGE 13OF29 p. 106 3M ENVIRO NM ENTA L LABO RATORY REPO RT NO. E09-0372 ^Extract Cone. (-L1L)* ExtractionVolume(mL) j-^ A v e ra g e Sample C o n c |-- j * LMS Sample Mass (g )j LMS%Recovery = Spike Amount (ng) 100% Although ETS 8-45.0does notprovidespecificcriteriaforthelab matrixspikeconcentrations, the3M Environmental Laboratory uses a general guidelinethatlabmatrixspikeconcentrationshould be at least halftheendogenousconcentration beforethespike isconsidered "appropriate"forthegiven matrix. For PFOS, theLMSwas 27.6ng (-110 ng/gtissueconcentration)exceptforsamples E090372-012wherethe LMSwas 128ng (-510 ng/gtissueconcentration). The [1OJPFOS surrogate was spikedat0.261 ng(-1 ng/gtissueconcentration). 4.9 Analytical Uncertainty ETS 8-45.0statesthattheanalytical method uncertaintywill be determinedbystatistical evaluationof theindividual analyterecoveries inLCSs. Current projectQC results, aswell as historical values, are used intheevaluationuntil a maximumoffiftypoints (minimumoftwenty, ifpossible)are included. For ETS 8-45.0, the historical LCSs arecategorized bytissuetype: whole-bodyorfilletunlessthereis strongevidencesuggestingthata species-specific matrixeffect is present andthatresultsfromthese species should beconsidered separately. The standard deviationofthecollectiverecovery results(in %)iscalculated. The expanded uncertaintyisthencalculated bymultiplyingthestandarddeviation by a factoroftwo, whichcorrespondstothe95%confidence limit. Table 6belowprovidestheanalytical uncertaintyforPFOS andthe[1802]PF0S surrogate. Table 6. Analytical Method Uncertainty Average % Recovery Standard Deviation 2 'S tand ard Deviation N Analytical Uncertainty PFOS 101 9.17 18.3 50 (45 Bluegill fillets, 5 Walleye fillets) 18% t'O J P F O S Surrogate 106 8.73 17.46 50 (45 Bluegill fillets, 5 WaHeve filets) 17% 5 Data Summary and Discussion Table 7 belowprovidesthesampleand labmatrixspike resultsforPFOS andthe [1802]PFOS surrogatequantitatedusingtheextractedcalibrationcurve prepared inbluegill filletcontrol tissue. All samples produced PFOS LMS recoverieswithinmethodacceptance criteriaof 10030%exceptfor. E09-0372-030(67.4%). The analytical uncertaintyforthissample has been adjustedto 10050%. In general, mostsamples produced surrogate recoverieswithin 10030%. Exceptions havebeenflagged appropriatelyinthedatatable. ETS 8-45.0specifies noacceptance criteriaforsurrogate recoveries as theintentofthesurrogateis toevaluatesystematicbiases or interferencesthatmay be present. The recoveriesofthe3MEOF LCSs preparedwitheach extractionbatch (N=9forthestudy)ranged from98.9%to 114%witha calculated averageof 107%(4.7%RSD). SeeSection 10.1. Theresultsof the ECF QC spikes demonstratedthatthereisnodiscernible biaswhen PFOS ECF isomersare quantitated againstthepredominantly linearreferencestandard. Therefore, thereported PFOS values areconsidered accuratetowithinthe statedmethoduncertaintyregardless ofthedegreeofbranched PFOS isomerspresent inthesampleextracts. 3MENVIRONMENTALLABORATORY PAGE 14OF29 3M ENVIRONMENTAL LABORATORY REPORT NO. E 09-0372 Table 7. S am ple and L ab M atrix S p ike R esults: PFO S and [180 2]P F O S s u rro g a te . 3M UM S Num ber E09-0372-001 E09-0372-001 Dup E09-0372-001 LMS S am ple D escription Axys ID - L12916-14, Client ID- 090191 Axys ID- L12916-14, Client ID- 090191 Dup Axys ID- L12916-14, Client ID- 090191 LMS E09-0372-002 E09-0372-002 Dup E09-0372-002 LMS Axys ID - L 12916-24, Client ID- 090054 Axys ID- L12916-24, Client ID- 090054 Dup Axys ID- L 12916-24, Client ID- 090054 LMS E09-0372-003 E09-0372-003 Dup E09-0372-003 LMS Axys ID- L12916-26, Client ID- 090056 Axys ID- L12916-26, Client ID- 090056 Dup Axys ID- L12916-26, Client ID- 090056 LMS E09-0372-004 E09-0372-004 Dup E09-0372-004 LMS Axys ID- L12917-3, Client ID- 090275 Axys ID- L12917-3, Client ID- 090275 Dup Axys ID- L12917-3, Client ID- 090275 LMS E09-0372-005 E09-0372-005 Dup E09-0372-005 LMS Axys ID- L12917-10, Client ID- 090282 Axys ID- L12917-10, Client ID - 090282 Dup Axys ID- L12917-10, Client ID- 090282 LMS S p e c ie s Carp Carp Carp Carp Carp R iver Location Section 3 A verag e % R PD /% R SD Section 1 A verag e %RPCH%RSD Section 1 A verag e % R PD /% R SD Section 4 A verag e % R PD /% R SD Section 4 A v e ra g e % R PD /% R SD Mass E x tra c te d (a) 0.2403 0.2344 0.2584 0.2555 0.2613 0.2475 0.2468 0.2328 0.2508 0.2364 0.2512 0.2633 0.2690 0.2604 0.2632 mPFO S Cone. (ngfg) 45.0 46.5 168 45.8 3.2 27.1 25.4 152 26.3 6.3 4.90 5.79 124 5.35 17 96.1 94.3 221 95.2 1.9 15.6 17.0 124 16.3 8.5 PFOS LMS % R ecovery NA NA 115 NA NA 112 NA NA 108 NA NA 120 NA NA 103 % Recovery ["O JP FO S 95.8 89.8 98.7 94.8 4.8 104 86.8 98.7 96.6 9.3 95.6 106 103 101 5.4 96.8 95.8 103 98.4 3.7 95.4 94 2 95.8 95.1 0.90 p . 107 3MENVIRONMENTAL LABORATORY K'AUti&Uh 29 3M ENVIRONMENTAL LABORATORY REPORT NO. E09-0372 Table 7 Continued. 3M UM S Num ber E09-0372-006 E09-0372-006 Dup E09-0372-006 LMS Sam ple D escription Axys ID- L12917-17, Client ID- 090123 Axys ID- L12917-17, Client ID- 090123 Dup Axys ID- L12917-17, Client ID- 090123 LMS E09-0372-007 E09-0372-007 Dup E09-0372-007 LMS Axys ID- L 12931-6, Client ID- 090173 Axys ID- L 12931-6, Client ID- 090173 Dup Axys ID- L 12931-6, Client ID- 090173 LMS EQ9-0372-008 E09-0372-008 Dup E09-0372-008 LMS Axys ID- L12931-14, CSent ID- 090032 Axys ID- L12931-14, Client ID- 090032 Dup Axys ID- L12931-14, Client ID- 090032 LMS E09-0372-009 E09-0372-009 Dup E09-0372-009 LMS Axys ID- L 12932-2, Client ID- 090094 Axys ID- L 12932-2, Client ID- 0 9 0094 Dup Axys ID- L 12932-2, Client ID- 090094 LM S E09-0372-010 E09-0372-010 Dup E09-0372-010 LMS Axys ID- L 12932-4, Client ID- 090096 Axys ID- L 12932-4, Client ID- 090096 Dup Axys ID- L 12932-4, Client ID- 090096 LMS E09-0372-011 E09-0372-011 Dup E09-0372-011 LMS Axys ID- L 12932-9, Client ID- 090042 Axys ID- L 12932-9, Client ID- 090042 Dup Axys ID- L 12932-9, Client ID- 090042 LMS S p e c ie s Carp Smallmouth Bass Smallmouth Bass Smallmouth Bass Smallmouth Bass Smallmouth Bass R iver Location Section 2 A verag e % R PD /% R SD Section 3 A v e ra g e % R PO /% R SD Section 1 A verag e % R PD /% R SD Section 2 A v e ra g e % R PD /% R SD Section 2 A verag e % R PD /% R SD Section 1 A verag e % R PD /% R SD M ass E x tra c te d (a) 0.2638 0.2482 0.2594 0.2414 0.2563 0.2689 0.2607 0.2507 0.2601 0.2375 0.2699 0.2688 0.2622 0.2561 0.2434 0.2430 0.2548 0.2483 ^PFOS Cone. (n g /g ) 17.9 18.1 119 18.0 1.2 41.3 39.8 139 40.6 3.8 26.9 31.7 134 29.3 16 10.8 13.2 113 12.0 20 15.1 14.4 130 14.8 4.2 13.7 15.3 134 14.5 11 PFOS LMS % Recovery NA NA 94.5 NA NA 96.4 NA NA 98.3 NA NA 97.9 NA NA 102 NA NA 107 `/ R e c o v e ry f 1,O tlP F O S 95.8 82.9 89.9 89.5 7.2 88.6 88.1 91.4 89.4 2.0 97.7 118 101 105 10 90.5 101 98.7 96.6 5.5 103 105 106 105 1.4 101 116 111 109 7.2 p. 108 3MENVIRONMENTALLABORATORY PAGE 16OF 29 3M ENVIRONMENTAL LABORATORY REPORT NO. E09-0372 Table 7 Continued. 3M UMS Number E09-0372-012 E09-0372-012 Dup; E09-0372-012 LMS; Sam ple Description Axys ID- L12932-26, Client ID- 090248 Axys ID- L12932-26, Client ID- 090248 Dup Axys ID- L 12932-26, Client ID- 090248 LMS E09-0372-013 E09-0372-013 Dup E09-0372-013 LMS Axys ID- L12933-18, Client ID- 090064 Axys ID- L12933-18, Client ID- 090064 Dup Axys ID- L12933-18, Client ID- 090064 LMS E09-0372-014 E09-0372-014 Dup E09-0372-014 LMS Axys ID- L12933-20, Client ID- 090066 Axys ID- L12933-20, Client ID- 090066 Dup Axys ID- L 12933-20, Client ID- 090066 LMS E09-0372-015 E09-0372-015 Dup E09-0372-015 LMS Axys ID- L12933-25, Client ID- 090071 Axys ID- L12933-25, Client ID- 090071 Dup Axys ID- L12933-25, Client ID- 090071 LMS E09-0372-016 E09-0372-016 Dup E09-0372-016 LMS Axys ID- L12934-10, Client ID- 090024 Axys ID- L 12934-10, Client ID- 090024 Dup Axys ID- L12934-10, Client ID- 090024 LMS E09-0372-017 E09-0372-017 Dup E09-0372-017 LMS Axys ID- L12934-12, Client ID- 090026 Axys ID- L12934-12, Client ID- 090026 Dup Axys ID- L12934-12, Client ID- 090026 LMS S p e c ie s Smallmouth Bass White Bass White Bass White Bass White Bass White Bass R iver Location Section 4 A verag e % R PD/% R SD Section 2 A verag e % R PD /% R SD Section 2 A verag e % R PD /% R SD Section 2 A verag e % R PD /% R SD Section 1 A verag e % R PD /% R SD Section 1 A verag e %RPCV%RSD M ass Extracted (a) 0.2646 0.2602 0.2667 0.2433 0.2599 0.2547 0.2488 0.2424 0.2666 0.2518 0.2492 0.2461 0.2570 0.2436 0.2633 0.2442 0.2545 0.2528 wPFOS Cone. (n & g ) (J)581 <2)558 B14 <570 4.0 52.0 56.4 150 54.2 8.1 71.5 71.0 185 71.3 0.82 65.0 62.2 178 63.6 4.5 47.7 50.9 148 49.3 6.6 71.7 65.8 176 68.7 8.5 PFOS LMS % R eco very NA NA 72.0 NA NA 88.6 NA NA 110 NA NA 102 NA NA 94.3 NA NA 98.3 % Recovery i"0,1P F O S 8)112 103 B)104 w 106 4.4 117 118 110 115 3.6 103 106 113 107 5.0 111 108 106 109 2.2 96.8 117 113 109 9.8 114 111 124 116 5.6 p. 109 3MENVIRONMENTAL LABORATORY KUt i /Uh 29 3M ENVIRONMENTAL LABORATORY REPORT NO. E09-0372 Table 7 Continued. 3M LIMS Num ber E09-0372-018 E09-0372-018 Dup E09-0372-018 LMS Sam ple D escription Axys ID- L 12934-18, Client ID- 090017 Axys ID- L12934-18, Client ID- 090017 Dup Axys ID- L12934-18, Client ID- 090017 LMS E09-0372-019 E09-0372-019 Dup E09-0372-019 LMS Axys ID- L12945-1, Client ID- 090153 Axys ID- L12945-1, Client ID- 090153 Dup Axys ID- L12945-1, Client ID- 090153 LMS E09-0372-020 E09-0372-020 Dup E09-0372-020 LMS Axys ID- L12945-4, Client ID- 090167 Axys ID- L12945-4, Client ID- 090167 Dup Axys ID- L12945-4, Client ID- 090167 LMS E09-0372-021 E09-0372-021 Dup E09-0372-021 LMS Axys ID- L12945-14, Client ID- 090241 Axys ID- L12945-14, Client ID- 090241 Dup Axys ID- L12945-14, Client ID- 090241 LMS E09-0372-022 E09-0372-022 Dup E09-0372-022 LMS Axys ID- L12945-16, Client ID- 090078 Axys ID- L12945-16, Client ID- 090078 Dup Axys ID- L12945-16, Client ID- 090078 LMS E09-0372-023 E09-0372-023 Dup E09-0372-023 LMS Axys ID- L12945-19, Client ID- 090081 Axys ID- L12945-19, Client ID- 090081 Dup Axys ID- L 12945-19, Client ID- 090081 LMS S p e c ie s White Bass Fresh Water Drum Fresh Water Drum Fresh Water Drum Fresh Water Drum Fresh Water Drum R iver Location Section 1 A verag e % R PD /% R SD Section 3 A verag e % R PD /% R SD Section 3 A verag e % R PD /% R SD Section 4 A verag e % R PD /% R SD Section 2 A verag e % R PD /% R SD Section 2 A v e ra g e % R PD /% R SD Mass Extracted (a) 0.2640 0.2433 0.2549 0.2568 0.2473 0.2478 0.2372 0.2509 0.2618 0.2375 0.2574 0.2341 0.2468 0.2657 0.2533 0.2345 0.2537 0.2528 wPFOS Cone. (n g /g ) 86.4 82.4 191 84.4 4.7 113 103 224 108 9.1 82.1 82.3 176 82.2 0.24 24.6 22.5 155 23.6 8.9 74.9 80.4 154 77.7 7.2 41.3 32.9 132 37.1 23 PFOS LMS % Recovery NA NA 98.7 NA NA 104 NA NA 88.7 NA NA 111 NA NA 70.1 NA NA 86.5 `/(R e c o v e ry f'O ilP F O S 120 102 124 115 10 121 109 126 118 7.1 115 111 112 113 1.8 97.7 103 126 109 14 92.5 120 107 107 13 104 103 97.7 102 3.6 p. 110 3MENVIRONMENTALLABORATORY PAGE 18OF29 3M ENVIRONMENTAL LABORATORY REPORT NO. E09-0372 Table 7 Continued. 3M UMS Number E09-0372-024 E09-0372-024 Dup E09-0372-024 LMS S am ple D escription Axys ID- L12945-30, Client ID- 090009 Axys ID- L12945-30, Client ID- 090009 Dup Axys ID- L12945-30, Client ID- 090009 LMS E09-0372-025 E09-0372-025 Dup E09-0372-025 LMS Axys ID- L12947-7, Client ID- 090266 Axys ID- L12947-7, Client ID- 090266 Dup Axys ID- L 12947-7, Client ID- 090266 LMS E09-0372-026 E09-0372-026 Dup E09-0372-026 LMS Axys ID- L12947-8, Client ID- 090267 Axys ID- L 12947-8, Client ID- 090267 Dup Axys ID- L12947-8, Client ID- 090267 LMS E09-0372-027 E09-0372-027 Dup E09-0372-027 LMS Axys ID- L12947-13, Client ID- 090111 Axys ID-L12947-13, Client ID -090111 Dup Axys ID- L12947-13, Client ID- 090111 LMS E09-0372-028 E09-0372-028 Dup E09-0372-028 LMS Axys ID- L12947-25, Client ID- 090205 Axys ID- L12947-25, Client ID- 090205 Dup Axys ID- L12947-25, Client ID- 090205 LMS E09-0372-029 E09-0372-029 Dup E09-0372-029 LMS Axys ID- L12947-26, Client ID- 090206 Axys ID- L12947-26, Client ID- 090206 Dup Axys ID- L 12947-26, Client ID- 090206 LMS S p e c ie s Fresh Water Drum Bluegill Sunfish Bluegill Sunfish Bluegill Sunfish Bluegill Sunfish Bluegill Sunfish R iver Location Section 1 A v e ra g e '/R P D rtiR S D Section 3 A verag e % R PD /% R SD Section 3 A verag e % R PD /% R SD Section 2 A v e ra g e % R PD /% R SD Section 4 A verag e % R PD /% R SD Section 4 A verag e % R PD /% R SD M ass Extracted (a) 0.2385 0.2430 0.2470 0.2338 0.2583 0.2576 0.2355 0.2495 0.2502 0.2610 0.2581 0.2691 0.2455 0.2524 0.2488 0.2421 0.2479 0.2397 ,vP F O S Cone. (nolo) 14.7 13.7 116 14.2 7.0 34.5 32.1 171 33.3 7.2 55.1 55.5 153 55.3 0.75 40.6 40.0 147 40.3 1.5 93.2 80.6 167 86.9 14 31.4 28.2 136 29.8 11 PFOS LMS % Recovery NA NA 91.5 NA NA 128 NA NA 88.5 NA NA 104 NA NA 72.1 NA NA 91.9 % Recovery ["O tlP F O S 102 107 109 106 3.8 99.6 112 119 110 8.8 106 111 104 107 3.2 110 95.7 114 107 9.1 98.7 103 106 103 3.7 (4>135 w 137 129 (4)134 3.0 3MENVIRONMENTAL LABORATORY PAGfc 19UT29 p. 111 3M ENVIRONMENTAL LABORATORY REPORT NO. E09-0372 Table 7 Continued. 3M UM S Num ber E09-0372-030 E09-0372-030 Dup E09-0372-030 LMS Sam ple D escription Axys ID- L12948-17, Client ID- 090061 Axys ID- L 12948-17, Client ID -090061 Dup Axys ID- L 12948-17, Client ID- 090061 LMS S p e c ie s Bluegill Sunfish R iver Location Section 1 A verag e % R PD /% R SD Mass E x tra c te d (9) 0.2544 0.2577 0.2350 wPFOS Cone. (ng/g) 129 141 214 135 8.9 PFOS LMS % R ecovery NA NA `*67.4 % Recovery f'O J P F O S 116 (4)132 101 116 14 (1) Unless otherwise specified, the recovery of associated PFOS laboratory matrix spike (LMS) was within 100*30% which meets ETS 8-45.0 method acceptance criteria. Sample results are considered aocurate to within the overall analytical method uncertainty 100*18% for PFOS and 100*17% for [^OJPFOS See Section 4.9 Determination of Analytical Method Uncertainty for more information. Sample results are reported to three significant figures and %RPD to two significant figures Additional significant figures were used to calculate the average, %RPD, and %recovery. Values in the raw data may vary slightlydue to rounding. (2) Sample results were reported from a 1:100 post-extraction dilution. (3) LMS recovery was 67.4%, sample accuracy has been adjusted to 100*50%. (4) [" OdPFOS surrogate recovery exceeded 130%. p. 112 3MENVIRONMENTALLABORATORY PAGE 20 OF 29 p. 113 3M ENVIRONMENTAL LABORATORY REPORT NO. E09-0372 Conclusions The PFOS sampleresultspresented in and Table 7areconsideredaccuratewithintheoverall method uncertaintyof 10018%. The accuracy (%recovery)and precision (%RSD)of3MECF (branched) PFOS laboratorycontrol spikes quantitatedagainstthe predominantlylinearreferencestandard demonstratedthatthe isomersproduce nodiscemabiequantitativebias. Resultsfortheothertargetanalyteswill beforthcoming ina subsequent report. 7 Data/Sample Retention All remainingsample and associated projectdata (hardcopyandelectronic)will bearchived according to3M Environmental Laboratorystandard operating procedures. 8 Analytical Personnel 8.1 3M Environmental Laboratory Michelle D. Malinsky, Ph.D Research Specialist 8.2 Pace Lab Ops Jonathan Steege 3MENVIRONMENTALLABORATORY PAGE21OF29 p. 114 3M ENVIRONMENTAL LABORATORY REPORT NO. E09-0372 _______________________ lo k fs tm ;ialist, Principal Analytical Investigator Date /o /r /io o g William K. Reagen, Ph.D., Environmental LaboratoryManagement Date Date The 3MEnvironmental Laboratory's QualityAssurance Unithasaudited thedataand reportforthis project. QAI Representative 'O 9 Date 3MENVIRONMENTALLABORATORY PAGE 22OF 29 3M ENVIRONMENTAL LABORATORY REPORT NO. E09-0372 10 Supplemental Information 10.1 Lab Control Spike Recoveries by Extracted Matrix-Matched Calibration with IS Quantitation. Table 8. LCS Recoveries for Extraction Batch 1 Using Extracted Matrix-Matched Calibration. PFOS ['OJPFOS Sample ID Sample Description Extracted Mass (g) ' ' 'Corrected Spike Cone. (ng/mL) Calc. Cone. (ng/mL) % Recovery Spike Cone. (ng/mL) Calc. Cone. (ng/mL) % Recovery 090826 BGF LCS Low 1 LCS Low 1 0.2663 0.107 0.104 97.3 0.104 0.101 97.5 090826 BGF LCS Low 2 LCS Low 2 0.2594 0.106 0.106 100 0.104 0.109 104 090826 BGF LCS Low 3 LCS Low 3 0.2596 0.106 0.121 115 0.104 0.124 119 090826 BGF LCS Mid 1 LCS Mid 1 0.2676 0.210 0.205 97.8 0.104 0.117 113 090826 BGF LCS Mid 2 LCS Mid 2 0.2523 0.207 0.184 89.1 0.104 0.105 101 090826 BGF LCS Mid 3 LCS Mid 3 0.2557 0.207 0.194 93.6 0.104 0.100 96.2 090826 BGF LCS High 1 LCS High 1 0.2666 0.864 0.766 88.7 0.104 0.097 93.3 090826 BGF LCS High 2 LCS High 2 0.2586 0.862 0.705 81.8 0.104 0.0968 93.1 090826 BGF LCS High 3 LCS High 3 0.2687 0.864 0.709 82.0 0.104 0.106 101 090826 BGF ECF LCS 1 ECF L C S 1 0.2577 0.574 0.568 98.9 0.104 0.110 106 090826 BGF ECF LCS 2 ECF LCS 2 0.2585 0.574 0.612 107 0.104 0.112 107 090826 BGF ECF LCS 3 ECF LCS 3 0.2474 0.572 0.587 103 0.104 0.109 105 090826 BGF PFOS LCS 1 PFOS LCS 1 0.2615 10.6 10.6 100 0.104 0.0914 87.9 090826 BGF PFOS LCS 2 PFOS LCS 2 0.2639 10.6 10.5 99.4 0.104 0.104 99.6 090826 BGF PFOS LCS 3 PFOS LCS 3 0.2589 10.6 11.7 111 0.104 0.108 104 A verag e 97.6 102 %RSD 9.7 7.8 (1) Spikeconcentrationcorrectedfortheendogenous PFOS concentration inthebluegill fillet(BGF) control matrixas determined by methodof standard addition=0.525 ng/g. p. 115 3MENVIRONMENTALLABORATORY PAGE 23 OF 23 3M ENVIRONMENTAL LABORATORY REPORT NO. E09-0372 Table 9. LC S R eco veries fo r E xtractio n B atch 2 U sin g E xtracted M atrix-M atch ed C alib ratio n . PFOS [" O jlP F O S Sample ID Sample Description Extracted Mass(g) '"Corrected Spike Cone. (ng/mL) Calc. Cone. (ng/mL) % Recovery Spike Cone. (ng/mL) Calc. Cone. (ng/mL) % Recovery 090828 BGF LCS Low 1 LCS Low 1 0.2538 0.102 0.116 113 0.104 0.111 106 090828 BGF LCS Low 2 LCS Low 2 0.2641 0.105 0.114 109 0.104 0.113 109 090828 BGF LCS Low 3 LCS Low 3 0.2439 0.100 0.119 118 0.104 0.119 114 090828 BGF LCS Mid 1 LCS Mid 1 0.2609 0.206 0.185 89.6 0.104 0.106 102 090828 BGF LCS Mid 2 LCS Mid 2 0.2567 0.206 0.213 104 0.104 0.102 98.5 090828 BGF LCS Mid 3 LCS Mid 3 0.2637 0.207 0.207 100 0.104 0.0975 93.7 090828 BGF LCS High 1 LCS High 1 0.2526 0.859 0.785 91.4 0.104 0.106 102 090828 BGF LCS High 2 LCS High 2 0.2634 0.861 0.758 88.0 0.104 0.112 107 090828 BGF LCS High 3 LCS High 3 0.2576 0.860 0.796 92.5 0.104 0.111 107 090828 BGF ECF LCS 1 ECF L C S 1 0.2605 0.573 0.638 111 0.104 0.122 118 090828 BGF ECF LCS 2 ECF LCS 2 0.2531 0.571 0.605 106 0.104 0.115 110 090828 BGF ECF LCS 3 ECF LCS 3 0.2635 0.573 0.653 114 0.104 0.126 121 090828 BGF PFOS LCS 1 PFOS LCS 1 0.2569 10.6 11.2 106 0.104 0.119 114 090828 BGF PFOS LCS 2 PFOS LCS 2 0.2430 10.6 11.2 106 0.104 0.111 107 090828 BGF PFOS LCS 3 PFOS LCS 3 0.2596 10.6 12.2 116 0.104 0.122 117 Average 104 108 %RSD 9.5 7.0 (1) Spikeconcentrationcorrectedforthe endogenous PFOS concentration inthebluegill fillet(BGF) control matrixas determined bymethodof standardaddition=0.507 ng/g. p. 116 3MENVIRONMENTALLABORATORY PAGE 24OF 29 3M ENVIRONMENTAL LABORATORY REPORT NO. E 09-0372 Table 10. LCS Recoveries for Extraction Batch 3 Using Extracted Matrix-M atched Calibration. PFOS ["OJPFOS Sample ID Sample Description Extracted Mass (g) `''Corrected Spike Cone. (ng/mL) Calc. Cone. (ng/mL) % Recovery Spike Cone. (ng/mL) Calc. Cone. (ng/mL) % Recovery 090901 BGF LCS Low 1 LCS Low 1 0.2424 0.0992 0.0982 99.0 0.104 0.0946 91.0 090901 BGF LCS Low 2 LCS Low 2 0.2589 0.102 0.0983 95.9 0.104 0.116 112 090901 BGF LCS Low 3 LCS Low 3 0.2642 0.104 0.110 106 0.104 0.118 114 090901 BGF LCS Mid 1 LCS Mid 1 0.2641 0.206 0.229 111 0.104 0.126 121 090901 BGF LCS Mid 2 LCS Mid 2 0.2498 0.203 0.217 107 0.104 0.124 120 090901 BGF LCS Mid 3 LCS Mid 3 0.257 0.205 0.185 90.4 0.104 0.105 101 090901 BGF LCS High 1 LCS High 1 0.2676 0.861 0.861 100 0.104 0.115 110 090901 BGF LCS High 2 LCS High 2 0.262 0.860 0.889 103 0.104 0.106 102 090901 BGF LCS High 3 LCS High 3 0.2586 0.859 0.841 97.9 0.104 0.112 107 090901 BGF ECF LCS 1 ECF LCS 1 0.2482 0.569 0.616 108 0.104 0.102 98.0 090901 BGF ECF LCS 2 ECF LCS 2 0.258 0.571 0.649 114 0.104 0.123 118 090901 BGF ECF LCS 3 ECF LCS 3 0.25 0.570 0.593 104 0.104 0.104 99.8 090901 BGF PFOS LCS 1 PFOS LCS 1 0.2427 10.6 11.4 108 0.104 0.128 123 090901 BGF PFOS LCS 2 PFOS LCS 2 0.2495 10.6 11.7 111 0.104 0.116 111 090901 BGF PFOS LCS 3 PFOS LCS 3 0.241 10.6 10.5 100 0.104 0.113 108 A verag e 104 109 %RSD 6.2 8.6 (1) Spikeconcentrationcorrectedforthe endogenous PFOS concentration inthe bluegill fillet(BGF) control matrixas determined bymethodof standard addition=0.497 ng/g. p. 117 KUt 5 Uh 29 3M ENVIRONMENTAL LABORATORY REPORT NO. E09-0372 10.2 Lab Control Spike Recoveries by Unextracted Acetonitrile Calibration using IS Quantitation. Table 11. LCS Recoveries for Extraction Batch 1 Using Unextracted Acetonitrile Calibration. PFOS f1' 0 2]PFOS Sample ID Sample Description Extracted Mass (g) (1'Corrected Spike Cone. (ng/mL) Calc. Cone. (ng/mL) % Recovery Spike Cone. (ng/mL) Calc. Cone. (ng/mL) % Recovery 090826 BGF LCS Low 1 LCS Low 1 0.2663 0.109 0.0965 88.7 0.104 0.104 100 090826 BGF LCS Low 2 LCS Low 2 0.2594 0.107 0.0985 91.8 0.104 0.112 108 090826 BGF LCS Low 3 LCS Low 3 0.2596 0.107 0.113 105 0.104 0.128 123 090826 BGF LCS Mid 1 LCS Mid 1 0.2676 0.212 0.200 94.3 0.104 0.121 117 090826 BGF LCS Mid 2 LCS Mid 2 0.2523 0.209 0.178 85,3 0.104 0.108 104 090826 BGF LCS Mid 3 LCS Mid 3 0.2557 0.210 0.188 89.7 0.104 0.103 99.0 090826 BGF LCS High 1 LCS High 1 0.2666 0.868 0.773 89.1 0.104 0.0997 95.9 090826 BGF LCS High 2 LCS High 2 0.2586 0.866 0.710 82.0 0.104 0.0995 95.7 090826 BGF LCS High 3 LCS High 3 0.2687 0.868 0.714 82.2 0.104 0.109 105 090826 BGF ECF LCS 1 ECF LCS 1 0.2577 0.574 0.570 99.3 0.104 0.114 110 090826 BGF ECF LCS 2 ECF LCS 2 0.2585 0.574 0.615 107 0.104 0.115 111 090826 BGF ECF LCS 3 ECF LCS 3 0.2474 0.572 0.590 103 0.104 0.112 108 090826 BGF PFOS LCS 1 ECF LCS 4 0.2615 10.6 10.5 99.5 0.104 0.0938 90.2 090826 BGF PFOS LCS 2 ECF LCS 5 0.2639 10.6 10.4 98.5 0.104 0.107 103 090826 BGF PFOS LCS 3 ECF LCS 6 0.2589 10.6 11.5 109 0.104 0.112 107 A v e ra g e 95.0 105 %RSD 9.4 8.1 (D Spikeconcentrationcorrectedfor theendogenous PFOS concentration inthebluegill fillet(BGF) contra matrixas determinedby quantitation ofthe matrixblanks=0.543ng/g. p. 118 3MENVIRONMENTALLABORATORY PAGE 26OF 29 3M ENVIRONMENTAL LABORATORY REPORT NO. E09-0372 Table 12. LCS Recoveries for Extraction Batch 2 Using Unextracted A cetonitrile Calibration. PFOS ["O iIPFOS Sam ple ID Sam ple Description Extracted Mass (g) "'C o rre c te d Spike Cone. (n g /m L ) Calc. Cone. (n g /m L ) % Recovery Spike Cone. (n g /m L ) Calc. Cone. (n g /m L ) % Recovery 090828 BGF LCS Low 1 LCS Low 1 0.2538 0.109 0.114 105 0.104 0.0984 94.6 090828 BGF LCS Low 2 LCS Low 2 0.2641 0.111 0.112 101 0.104 0.101 96.9 090828 BGF LCS Low 3 LCS Low 3 0.2439 0.106 0.117 110 0.104 0.106 102 090828 BGF LCS Mid 1 LCS Mid 1 0.2609 0.213 0.189 88.6 0.104 0.0944 90.7 090828 BGF LCS Mid 2 LCS Mid 2 0.2567 0.212 0.219 103 0.104 0.0907 87.2 090828 BGF LCS Mid 3 LCS Mid 3 0.2637 0.214 0.213 99.6 0.104 0.0860 82.7 090828 BGF LCS High 1 LCS High 1 0.2526 0.867 0.836 96.4 0.104 0.0940 90.4 090828 BGF LCS High 2 LCS High 2 0.2634 0.870 0.807 92.8 0.104 0.0992 95.4 090828 BGF LCS High 3 LCS High 3 0.2576 0.869 0.848 97.6 0.104 0.0990 95.2 090828 BGF ECF LCS 1 ECF LCS 1 0.2605 0.577 0.677 117 0.104 0.109 105 090828 BGF ECF LCS 2 ECF LCS 2 0.2531 0.575 0.642 112 0.104 0.102 98 2 090828 BGF ECF LCS 3 ECF LCS 3 0.2635 0.578 0.694 120 0.104 0.113 109 090828 BGF PFOS LCS 1 ECF LCS 4 0.2569 10.6 11.9 113 0.104 0.106 102 090828 BGF PFOS LCS 2 ECF LCS 5 0.2430 10.6 11.9 113 0.104 0.0987 94.9 090828 BGF PFOS LCS 3 ECF LCS 6 0.2596 10.6 13.0 123 0.104 0.109 105 Average 106 96.6 %RSD 9.7 7 A (1) Spike concentration corrected tor the endogenous PFOS concentration in the bluegill fillet (BGF) control matrix as determined by quantitation of the matrix blanks = 0.568 ng/g. p. 119 3MENVIRONMENTAL LABORATORY PAGE 27 OF 29 3M ENVIRONMENTAL LABORATORY REPORT NO. E09-0372 Table 13. LCS Recoveries for Extraction Batch 3 Using Unextracted A cetonitrile Calibration. PFOS r1'O j]P F O S Sam ple ID Sam ple Description Extracted Mass (g) `"Corrected Spike Cone. (n g /m L ) Calc. Cone. (n g /m L ) % Recovery Spike Cone. (n g /m L ) Calc. Cone. (n g /m L ) % Recovery 090901 BGF LCS Low 1 LCS Low 1 0.2424 0.0916 0.0754 82.3 0.104 0.0906 87.1 090901 BGF LCS Low 2 LCS Low 2 0.2589 0.0944 0.0755 80.0 0.104 0.111 107 090901 BGF LCS Low 3 LCS Low 3 0.2642 0.0953 0.0870 91.3 0.104 0.114 109 090901 BGF LCS Mid 1 LCS Mid 1 0.2641 0.198 0.199 100 0.104 0.121 116 090901 BGF LCS Mid 2 LCS Mid 2 0.2498 0.196 0.188 96.0 0.104 0.120 115 090901 BGF LCS Mid 3 LCS Mid 3 0.2570 0.197 0.158 80.2 0.104 0.100 97.0 090901 BGF LCS High 1 LCS High 1 0.2676 0.855 0.802 93.8 0.104 0.110 106 090901 BGF LCS High 2 LCS High 2 0.2620 0,854 0.829 97.1 0.104 0.102 97.9 090901 BGF LCS High 3 LCS High 3 0.2586 0.853 0.783 91.8 0.104 0.107 103 090901 BGF ECF LCS 1 ECF LCS 1 0.2482 0.560 0.568 102 0.104 0.0977 94.0 090901 BGF ECF LCS 2 ECF LCS 2 0.2580 0.561 0.600 107 0.104 0.118 113 090901 BGF ECF LCS 3 ECF LCS 3 0.2500 0.560 0.546 97.5 0.104 0.0995 95.7 090901 BGF PFOS LCS 1 ECF LCS 4 0.2427 10.5 11.3 107 0.104 0.123 N/A 090901 BGF PFOS LCS 2 ECF LCS 5 0.2495 10.5 11.5 109 0.104 0.111 N/A 090901 BGF PFOS LCS 3 ECF LCS 6 0.2410 10.5 10.4 98.7 0.104 0.108 N/A Average 95.6 103 %RSD 9.7 8.9 (1) Spike concentration corrected for the endogenous PFOS concentration in the bluegill fillet (BGF) control matrix as determined by quantitation of the matrix blanks = 0.419 ng/g. p. 120 3MENVIRONMENTALLABORATORY PAGE28OF 29 10.3 Surrogate Recoveries in Spiked Blanks. B atch 1 Sam ple ID 090826 BGF Matrix Blank-1 090826 BGF Matrix Blank-2 090826 Aqueous Blank-1 090826 Aqueous Blank-2 Acetonitrile Blank with IS & S uit Acetonitrile Blank with IS & S uit B atch 2 090828 BGF Matrix Blank-1 090828 BGF Matrix Blank-2 090828 Aqueous Blank-1 090828 Aqueous Blank-2 Acetonitrile Blank with IS & Surr. Acetonitrile Blank with IS & Surr. B atch 3 090901 BGF Matrix Blank-1 090901 BGF Matrix Blank-2 090901 Aqueous Blank-1 090901 Aqueous Blank-2 Acetonitrile Blank with IS & Surr. Acetonitrile Blank with IS & Surr. Sample Description (with IS/surr) (with IS/surr) (with IS/surr) (with IS/surr) 08 007-145 08 007-145 (with IS/surr) (with IS/surr) (with IS/surr) (with IS/surr) 08 007-145 08 007-145 (with IS/surr) (with IS/surr) (with IS/surr) (with IS/surr) 08 007-145 08 007-145 3M ENVIRONMENTAL LABORATORY REPORT NO. E 09-0372 ["O JP F O S S p ike Cone. (ng /m L ) 0.104 0.104 0.104 0.104 0.0956 0.0956 0.104 0.104 0.104 0.104 0.0956 0.0956 0.104 0.104 0.104 0.104 0.0956 0.0956 C alc. Cone. (ng /m L ) 0.112 0.121 0.0810 0.110 0.0995 0.0948 0.101 0.107 0.0998 0.118 0.109 0.125 0.109 0.112 0.112 0.109 0.105 0.110 % R ec 108 116 77.9 106 104 99.2 97.1 103 96.0 113 114 131 105 108 108 105 110 115 p. 121 3MENVIRONMENTALLABORATORY KAut 29uF 29 p. 123 A li P tz il 53 <*IA1*2*fJ FsH p. 124 secs MNP I *fl 5 2 *i S Fish mH H 26 r i w p. 127 Mississippi River Pool 2 Surface Water Maps (received onsite from Bruce Monson) V- Water Sample Points M ****,. m Reach 4 Approximately 4.7 river miles to Lock & Dam #2 in Hastings. '*'C '? J p iv 1 ?*!< -' " ' bi?- *-'* I .v ' . b i a s 's T .\ (1 i f TM 508556? *'. .-?v; v'C^iwCMV *, (12) UTI fe w r ||ftSKiW.': K, 495B963 P A * V ^ , ' I ~l>m/ , '. r j t or 0.00 Miles 5/13/2009 Scale = 1:32.892 rooo 5/13/2009 2:19 PM Scale = 1:102.981 p. 129  'i * *<!Z'i- ise toZoom In 5/13/2009 2:12 PM Scale = 1:37.962 wo >. / t .-ris h fO 5 /1 3 /2 0 0 3 River mile estimates described on following slides are based on the navigation channel. 5 /1 3 /2 0 0 9 1:52 PM p. 133 11M' I f f Q |1"1 ,J i0 .1 C p. 134 Mississippi River Pool 2 - July 2009 Surface Water Event Reach 4-Location 11 (moving away from the site) Reach 4-Location 12 Mississippi River Pool 2 --Jul\ 2009 Surface Water Lvent Reach 3-Location 9 p. 135 Reach 4-Location 10 p. 136 Mississippi River Pool 2 - July 2009 Surface Water Event Reach 3-Location 7 Missed Photo Reach 3-Location 8 Mississippi River Pool 2 - July 2009 Surface Water Lvent Reach 2-Location 5 p. 137 Reach 2-Location 6 [Mississippi River Pool 2 - July 2009 Surface Water Event Reach 1-Location 3 p. 138 Reach 2-Location 4 Mississippi River Pool 2 - July 2009 Surlace Waler Lvcnt Reach 1-Location 1 p. 139 Reach 1-Location 2 p. 1 4 0 Mississippi River Pool 2 Surface Water Site Photographs Environmental Laboratory ShippingAOdntt: 3M Cantor Bldg 2B0-SN-17 S t Paul. MN 55144 7efepAone; Sample Receiving: (851 ) 736-6559 Alternato: (651)733-9873 FAX: (651)733-5982 Contact Name Gary Hohenstein Company 3M Com pany Mailing Address City, State, Zip Special Instructions and/or Specific Regulatory Requirements: (method, limitofdetection, rep Chain of Custody / Request for Laboratory Analytical Services Project ID/Proiect Name Mississippi River Pool 2 Surface Water Sampling July 2009 Tem plate# Final Report Due Date Project Lead Sue W olf Internai Due Date Dept, # (main) 452090 Class/Job/Project 9 0040152373 Data Available Date Due Contract Lab Preservatives: For M om * Use Only . E09-0365 3MEnvironmental Lab Analysis Requested: Complete below. Attach any associated information. Total Number of Containers Item Client Sample Identification 1. R each 4 - L o c 11 Sam ple 2. Reach 4 - L o c 11 Sam ple Dup 3. Reach 4 - L oc 11 Spike 4. Reach 4 - Loc 12 Sam ple 5. Reach 4 - Loc 12 Sam ple Dup 6. Reach 4 - L o c 12 Spike 7. Trip Blank Sam ple 8. Trip Blank 25 ppt Spike 9. - 10. A)A \\J Collected by print): B V -acL . J -a c 'JsflsW V I ii i 1 See AttachedLabRequest 3M UMS# 031 032 033 034 035 036 037 038 Date Sampled 1 0 *5 " Tim e Sampled ' V/ to ro j M atrix/ media W W W W Enter the number of container of each ( 1 1 r 1 1 (Enter an X in the box below to indicate requeat) \ / Si ** ** W W W W *~T---u 11 i( ii i1 -- 97 q /S r --- - > . om Collector's signature: .StdneatfJK i / r J ---- -------------------- , - \ * e -- ,-iif w, afnfietfrMi Time Bate (L W X 5_ Sample Condition Upon Receipt: Temperature: Other Associated CoCs: ^O&cceptable O Other: O Received on Ice (Ice not required for this project (RAS-Pace)) Copies to: Comments: *=Blanks are pm -filled by P ace U fa Sciences and accom pany the study bottles for the duration o f d ie field sam pling. mm Page Of Original - Accompanying Samples Last Page - Originator See Reverse Side for Instructions Environmental Laboratory 3M Cantor BU 28M N-17 8L Paul, MN 86144 Stonato Raotovmg: (SSI) 736-666 Altamato: (51) 7334873 FAX: (61)7334882 Contact Nam Gary Hohenstein Company 3M Com pany Mailing Address City, State. Zip Chain of Custody / Request for Laboratory Analytical Services Project ID/Project Name MssssddIRiver Pool 2Surface w ater Santolina July 2009 Tem plate# Final Report Due Date Project Lead Sue W olf Dept.# (main) 452090 Internal Due Date Ctass/Job/Proiect#0040152373 Data Available Data Due Contract Lab E09-0365 3MEnvironmental Lab Special Instructions and/or Specific Regulatory Requirements: (method, limaofdetection, rep Preservatilires: 11 Item # Client Sample Identification 1. R each 3 - Loc 7 Spike 2. R each 3 - Lo c 8 Sam ple 3. R each 3 - L o c 8 Sam ple Dup 4. R each 3 - L o c 8 Spike 5. R each 3 - Lo c 9 Sam ple 6. R each 3 - L o c 9 Sam ple Dup 7, R each 3 - Loc 9 Spike 8. R each 4 - Loc 10 Sam ple 9. R each 4 - L o c 10 Sam ple Dup 10. R each 4 - L o c 10 Spike 3M UM 8# 021 022 023 024 025 026 027 028 029 030 T .W Sampled 0^10 Oci --I V/ Jf _s Collected by (print): tat# -/vi*!5?. 1s t ' --C O t i i i JTflj latoiieae<*iitomMBM eA f ^-- *7 \j /A ^ - IfSMI ___ f // CVn.L*Time Sampled L_____ Sample Condition upon Receipt: Temperature: Other Associated CoCs: * Acceptable O Other: O Received on Ice (Ice not requited for this project (RAS-Pace)) Copies to: i i1 M atrix/ m edia W W W W W W W W W W Enter the number orcontornare oteech 1 1 i { i l ( ( i JJL .StlXMdVlftT -, ------ r~ i-- J iM /, Comments: 'S ?i i i 1 ( { / ( i / / Analysis Requested: 1 tolete below. Attach anv associated Information. 1 SeeAttachedLabRequest (Enteren 'X Inthe bo* below to indicato request) 1 -iiIiT i. ... " lise-- :Qmr\ 7/v/oJ p . 142 P a g e '*? Of ^ Original - Accompanying Samples Last Page Originator See Reverse Side for Instructions Environmental Laboratory ShippingAddrm: Tmlmphon*: 3M Conter Bldg 26M N -17 Sample Receiving: <661) 736-65S9 Alternate <651)733-9873 SI. Paul. MN 55144 FAX: (651) 733-5662 Contact Name G a/y Hohenstein Company 3M Company j | ' Mailina Address City, State. Zip Speedit Instructions and/or Specific Regulatory Requirements: (method Omitof detection, rap Chain of Custody / Request for Laboratory Analytical Services Protect ID/Proiect Name Mississippi River Pool 2 Surface Water Santolina July 2009 Tem plate# final Report Due Date Project Lead S u e W olf Internal Due Date Dept. # (main) 452090 Class/Job/Project # 0040152373 Date Available Date Due Contract Lab PreservatW'es: 'S iX ni* 1 1 1 rOTfnWnilrUmmffUy E09-0365 3MEnvironmental Lab Analysis Requested: Com plate below. Attach any associated information. See AttachedLabRequest Item # Client Sample Identification 1 . R each 2 - Loc 4 Sam ple Dup 2. R each 2 - Lo c 4 Spike 3. R each 2 - Lo c 5 Sam ple 4. R each 2 - L o c 5 Sam ple Dup 5. R each 2 - L o c 5 Spike 6. R each 2 - L o c 6 Sam ple 7. R each 2 - Lo c 6 Sam ple Dup 8. R each 2 - Loc 6 Spike 9. R each 3 - L o c 7 Sam ple 10. R each 3 - Lo c 7 Sam ple Dup 3M UMS# 011 012 013 014 015 016 017 018 019 020 Date Sampled Time Sampled /*/* v/ IT S O V (23? __ \/ CRSO L- >i __ M atrix/ media W W W IN W W W W W W i !Enter tee number of containera ofeach 1) 1 i lI 11 !( i1 11 -1 (Enter an 'X mthe box batow to indicate request) -to i,:.. -:' ' A /M M M rf'SM M Htetim i ^ __ -H m i /6 ^ DaAft / a M H M d v ia r. : ' ' ) l H in n ? * ///r -7 ' Beta'' ^Q Lj 7 )7 /0 9 * Sample Condition Upon Receipt: Temperature: 'C Other Associated CoCs: ^Acceptable O Other: O Received on Ice (Ice not required for this project (RAS-Pace)) Copies to: p. 143 Page '2- Of j Original -Accompanying Samples Last Page -Originator See Reverse Side for Instructions Environmental Laboratory S flfe p fa yA d ifre cs.' 3M Cantar Stag. 280-6M-17 S t Paul. MN 55144 TatapSona: Sampta R aoaM * (651) 738-6668 Atam ete (651)73W 673 FAX: (651)733-5982 Contact Name Gary Hohenstein Company 3 M Com pany Mailino Address City, State. Zip Spedai Instructions and/or SpecMc Regulatory Requirements: (method, limit ofdetacBon, reporting unit*, ate.) Chain of Custody / Request for Laboratory Analytical Services Proiect ID/Proiect Name Misslssipol River Pool 2 Surface Water Semolino Jutv 2008 Tam elata# Final Reoort Due Date Proiect Lead Sue W olf Internal Due Data Dept. # (main) 452090 Class/Job/Proiect# 0040192373 Date Available Date Due Contract Lab Prservativwe: Nam # Client Sample Identification 1. Reach 1 - Loc 1 Sam ple 2 . Reach 1 - L o c 1 Sam ple Dup 3. R each 1 - L o c 1 Spike 4. Reach 1 - L o c 2 Sam ple 9. Reach 1 - L oc 2 Sam ple Dup 6 . Reach 1 - L o c 2 Spike 7. Reach 1 - L o c 3 Sam ple 8. Reach 1 - L o c 3 Sam ple Dup 9. Reach 1 - L o c 3 Spike . 10. Reach 2 - L o c 4 Sam ple Wf * 1 I-I \J V 3M UNSI 001 002 003 004 005 006 007 008 009 010 Date Sampled W <* / Tim e Sam pled im o \/ >/ /S ir V______ n it Matrix/ media W W W W W W W W W W ii il 1 Entar the rumbar of container of aach i \ i 1 1 1 r i if 1 i 1 1 1 i j"--''a-fbPmi ma i:'` iLVi- & j'--fL w ( Sample Condition Uoon Receipt: Temperature: Q jf'C Other Associated CoCs:' dCteceptable O Other O Received on Ice (Ice not required for this proiect (RAS-Pace)) Copies to: Comments: Total Number of Containers E09-0365 3MEnvironmentalLab Analysia Requested: Corntolete below. Attach any associated information. SeeAttachedLabRequest (Entar an X in tha box M ow to indicate raquaal) -& ' ik jo lr p. 144 Page_J__ Of Original Accompanying Samples Last Page - Originator See Reverse Side for Instructions p. 145 Mississippi River Pool 2 Surface Water Chain of Custody Forms  2 vceAnalytical Field Services Division p. 146 Mississippi River Pool 2 Surface Water. Sampling Lab Request Number: Site Identification: GPS Coordinates: Proposed UTM Actual UTM Field Sampling Notes I - L.&C- 2______ Date Collected: f Time Collected: _ 1 3 l/ Collected By: 5 ^ 0 <i cj f U Ln Signature _______ ,________ Observations - Subsurface {~4-6"): f r -y * -/ ___ 3 ^ ^ y#e ^ p.f ^ z-__ 3 rn ftvp ,, S h f C A f V / 1 ____......................... t F .T r ; p y X Field Measurements t'V w _ Wind Direction: ^ f - ______ -RiverDepth: lo L f r lk (ft.) - Ambient Temp.: -WaterTemp.: (C ) F/e/d Sampling Notes Site Identification: f<-<a 1- (______ Date Collected: ''h / % / Q 7 GPS Coordinates: Time Collected: ( / Q Proposed UTM V % H f C 1 s * /tT 2 '? 4 d Z Collected By: _ & T - Actuil UTM <,</gWVT V? ??<<> Signature: ,, J. Observations Subsurface (~4-6"): D rp_g_f_t_-M__k__4__Z_______t _o_______ f P i p kn terni fi*o- *-- e ____ V / * X AOIVu|,Hg y., n r t *n/Js SI, J . -'sA - &Ktf/(tu. J.1 -- rAv ,--y ?~Ar\?i c -4If. .. U sTM ___________________________________________ - < * l ) / d 2. A jc fy d- 1 \1 Wind Direction: - River Depth: Field Measurements `Sd _ _____ t *S (ft.) - Ambient Temp.: CC) - Water Temp.: 7J^~- ?- ( C) Form revised: 07/09-BGJ Page /ZaceAnalytical Field Services Division p. 147 Mississippi River Pool 2 Surface Water Sampling Lab Request Number: <M Field Sampling Notes Site Identification: GPS Coordinates: Proposed UTM Actual UTM y_ - (_^c V < /S 7 ? -T f 7?- Date Collected: ") Time Collected: / 3 i Collected By: 0 6 -1 " Signature:"^, * r * J r Observations - Subsurface (~4-6"): p .y b U f X s lJ ( 7 Df> 2 - i> u p t < *P c a tP c * ,v.r-'/- fiV /1f t v .v 7^.y>rt c 'P & 6 r~ ,, Field Measurements Wind Direction: ` fr /g _______ - River Depth: *2 .2 . fft) ~ = f- / Y / c r j - " ^T - Ambient Temp.: " pc) - Water Temp.: 'Z,*f.S* ( C) Field Sampling Notes Site Identification: l - lo c 3______ GPS Coordinates: Proposed UTM ^ Actual UTM e > < /f+ C z t- i ; < /T ? -/5 % 0 Date Collected: Time Collected: Collected By: a z : Signature:V/ Observations F - Subsurface (--4-6"): `^^ f t / f A f/c . / 3 ^ P/p g,tr<*- & z___ t> :p \V i^ T - A* /.w . n / w __________ ^ 3 //A . et ip G rl P ^ p _______________________________________ cr Field Measurements Wind Direction: $ c ? _______ - River Depth: / (ft.) - Ambient Temp.xSf 7-T ( C) - Water Temp.: C) Form revised: 07/09-BG J Page uceAnalytical F itto S ervlets Division p. 148 Mississippi River Pool 2 Surface Water. Sampling Lab Request Number: Field Sampling Notes Site Identification: d * u 2~ - U o c . Co Date Collected: T y 'g /o ? GPS Coordinates: Time Collected: f 2 ,3 3 Proposed UTM______ ___________________ Actual UTM O V - J ^ M O O ' m M ' J Z - Collected By: B gtT ' Slgnlurar~i<, / Observations - Subsurface (~4-6"): fa p Ht-H-Cv M i F^h * .. iff r> fc J/^ ci -2 tn y - I K DvV> , ***feri _________________ ^ ,y> ~ : y 9 _______________ .. S t r- . y / ' t / c . j Wind Direction: - River Depth: Field Measurements _______ t j (ft.) #= - Ambient Temp.: ^9-* (6 } - Water Temp.: z S , O ( C) Site Identification: GPS Coordinates: Proposed UTM Actual UTM Field Sampling Notes c<?d y " " e > Y ? 6 e ? - i - ??7*5 Date Collected: Time Collected: Collected By: 2 J /e s J2ZL o Y ^ o f - r V??S2C>, S lg n a tu re r^ ^ Z Observations - Subsurface (~4-6"): b .p + * -e ynrrx ? ** r ^ ,/ .v+Zd~ itp t v 1pYa-. & H Field Measurements Wind Direction: $ _______ - River Depth: f (ft) . revised: 07/09-B G J t - Ambient Temp.: ^ ^ o ( c) - Water Temp.: 7-C S'" ( C) Page  2 aceAnalytical Field Services Division p. 149 Mississippi River Pool 2 Surface Water Sampling Lab Request Number: F & " o 3 < .< Site Identification: GPS Coordinates: Proposed UTM Actual UTM Field Sampling Notes s ,, .U V - ( V\ Date Collected: *?_____________ Time Collected: IO'Z- S'"*__________ 7 7 -7 Collected By: ._________ r) Y 7 7 5 ^ 7 ^ ? Slanaturel^ ^ j L ^ L a - z . -- , ___ Observations - Subsurface (~4-6"): Co Y JS/y> StfPGt, * (__ 3 / n S ^ K T-****- * * ArYA . # ^ v?rvi r $/>*- --------- - - -- -------( ^ 6 L ~ ^ _________________________________ **/*<-'* ^ v-w . ^ -------------------------- ------------------------------------------------------ i r__ r hSf. ------------------------- Wind Direction: - River Depth: Field Measurements - U "s u /<-/" l> (ft.)- cio**' ^ >i^'U A Ambient Temp.: ^ Cr~ ( C) - Water Temp.:g fc ff ( c 5> fit. Site Identification: GPS Coordinates: Proposed UTM T __ : 57 *0 ? 7 ./ ? to IS , Field Sampling Notes Date Collected: ~ ffy 'o T Time Collected: f p S~<^ i Collected By: tS fi * i Signature: n~L~^ Observations p.f, h m * A i nP " *- W e* V <i;p 7^,y/Ar*-U_ <,'ft r~*~ -t r* rc. *f r f * "fi V x. ___ . _______________ \ .............................. ..: _______\ Field Measurements Wind Direction: _> & ________ - River Pepth^ljM *7 (ft.) -x f - Ambient Temp.: (C) -Water Temp.: P f . z r o Form revised: 07/09-BGJ P a g e __ J l of weeAnalytical F ie li Services Division p. 150 Mississippi River Pool 2 Surface W atet Sampling Lab Request Number: Vy? - o ' U s ' Site Identification: GPS Coordinates: ProposedUTM Actual UTM 3 vfO ltrVZ, Field Sampling Notes *?_________ Date Collected: ~)~/%y <? *j 2 V 9r6? ? -ff Time Collected: *7 Collected By: 8 ^ 3 ^ Signature: ^3^ . Subsurface(~4-6"): Y **h > Z ^ Observations t - 3** S -t M .1 r i t i f a U . _ _ P-^, _________________ ? 5 X v T -y y Field Measurements Wind Direction: r*l>AU^r ^ Sg - River Depth: ^ (ft.) Ambient Temp.: ^ 6 C ' J 1 C) -WaterTemp.: 2 Y . Y (C) Field Sampling Notes Site Identification: 6 > , ( A </ - C d c ( & GPSCoordinates: Date Collected: > / ^ o T Time Collected: Q*7S~*i Proposed UTM u/ Col l ect ed By: 8 & S ~ Actual UTM d^f^5~?7 / y * i F iF4-Y 6o-J~ Vsj, Signature:_________ C & y i W , YlSUtZ-'l^ ** 7" Observations -Subsurface(~4-6"): fiy ^4- j - ^ T^-yy>/^ 13s Field Measurements Wind Direction: *? _______ - River Depth: {?,, ^ (ft) - Ambient Temp.: ** ( C) - Water Temp.: Z ^ ? (qC) Form revised: 07/09-B G J Page aceAnalytical Field Services Division p. 151 Mississippi River Pool 2 Surface Water Sampling Lab Request Number: rz>Y~o'5(e x ' Site Identification: GPS Coordinates: Proposed UTM Actual UTM --- /<> T Field Sampling Notes - Loc ________ Date Collected: " 7 " / % / 0 * 7 Time Collected: Q% S~& Collected By: P<S 5~~ ? 7 gS~7 5 ' Signature:! ^ ^ j ( ___ Observations y - Subsurface (--4-6"): t l7-/< o s * -I i< - />r|pp'w>| D ',f> 1 f r P r 'M $ -? r r \ $ pu. t v f - r \ P < * >.)> * c-i~ -f* S Z r .V l**p + fe - /*9 K V S~ uQ / R ( * ~ t r < ! * . P t * F r TEo-.-^ Fo/'wu-ti __ r# (C * lvi *>,V\ F s f '} & - i f^Vp )Field Measurements Wind Direction: ^A~f ? - River Depth:--- i j (ft.) - Ambient Temp.: (cJ i) - Water Temp.: 2-V, T (c ? Site Identification: GPS Coordinates: Proposed UTM Actual UTM Field Sampling Notes q - .>c ^ 76331-% Date Collected: Time Collected: o ^ f / O Collected By: y~ JSignature:- * ^ ~ ^ Observations JtSubsurface (~4-6"): i P p & M ( . 3 ^ S * - v ^ p U PMo ( P A fH * - >//> * * P c 4 - f t* * ffefaS * * ______________ ft g y *?P ' ^ ^ T T ,'^i7 ------- Field Measurements Wind Direction: I.^lv *7 `i - River Depth: i ^ (ft.) Ambient Temp.: r^GT~ (C) - Water Temp.: z . X (C) Form revised. 07/09-BGJ Page. _______o f ____ p. 152 Mississippi River Pool 2 Surface W ater Field Data Log Sheet(s) Mississippi River Pool 2 Surface Water Sampling Sampling Matrix Report Summary July 8, 2009 3M Lab Request E09-0365 S am ple ID Description Main Channel Reach 1 - Loc 1 Depth to Bottom: 13 feet / W ater Temp.: 25.7 C Old MN River Channel Reach 1 - Loc 2 Depth to Bottom: 10 feet / W ater Temp.: 25.2 C Main channel before confluence w / MN River Reach 1 - Loc 3 Depth to Bottom: 12 feet / W ater Temp.: 24.9 C GPS Coordinates Proposed UTM 484163, 4973008 Actual UTM 484143, 4973007 Proposed UTM 485961, 4970846 Actual UTM 486067, 4971149 Proposed UTM 487626, 4971558 Actual UTM 487624, 4971560 3M Samples - 0.25 L S am p le Sample Dup Spike Primary 111 1 1 11 1 11 1 1 MPCA Samples - 1.0 L Duplicate Triplicate MS-1 MS-2 MS-3 1 1 111 11 11 Main channel out from boat launch Proposed UTM 489751, 4973897 Reach 2 - Loc 4 Depth to Bottom: 22 feet / W ater Temp.: 24.8 C Actual UTM 489727, 4973910 1 1 1 1 1 1 Main channel adjacent to Holman Field Proposed UTM 496076, 4975338 Reach 2 - Loc 5 Depth to Bottom: 13 feet / W ater Temp.: 25.5 C Actual UTM 496075, 4975266 1 1 1 1 1 1 Bay downstream of Pigs Eye Lake Proposed UTM -- -- 1Reach 2 - Loc 6 Depth to Bottom: 4 feet / W ater Temp.: 25.0 C Actual UTM 497900, 4971442 1 11 1 1 Just south of boat landing - south of Newport Proposed UTM -- -- Reach 3 - Loc 7 Depth to Bottom: 11 feet / W ater Temp.: 24.7 C Actual UTM 499081, 4965125 1 1 1 1 1 1 Above the small Island No. 112 Proposed UTM -- -- Reach 3 - Loc 8 Depth to Bottom: 12 feet / W ater Temp.: 24.7 C Actual UTM 499272, 4963328 1 1 1 1 1 1 Middle of Spring Lake Proposed UTM 503307, 4956202 Reach 3 - Loc 9 Depth to Bottom: 9 feet / W ater Temp.: 24.4 C Actual UTM 503642, 4956878 1 1 1 1 1 1 Main Nav. Channel dwnstrm of Grey Cloud Slough Proposed UTM 505382, 4958615 1 1Reach 4 - Loc 10 Depth to Bottom: 12 fe e t/W a te r Temp.: 23.9 C Actual UTM 505348, 4958622 11 1 1 In vicinity just downstream of 3M CG discharge Proposed UTM 508556, 4958779 Reach 4 - Loc 11 Depth to Bottom: 6 feet / W ater Temp.: 23.9 C Actual UTM 508545, 4958789 1 1 1 1 1 1 111 Main Nav. channel just upstream of Lock & Dam #2 1 1Reach 4 - Loc 12 Depth to Bottom: 14 feet / W ater Temp.: 24.3 C Proposed UTM 510032, 4956963 Actual UTM 510018, 4956960 1 1 1 1 ____ _ __ __ _ p. 153 'aceAnalyticai Field Services Division p. 154 3M PROJECT SUMMARY P ro je ct N am e: Mississippi River Pool 2 Surface Water Lab R equest: E09-0365______________________ M onitoring D ate: 7/8/2009_______________________ P re pa re d By: Brad Jacobson (BGJ)_____________ D ate: 7/22/2009 3 M R equester: Gary Hohenstein 3 M P ro je ct Lead: Sue Wolf_____ ITEM Laboratory Results Sampling Matrix Report Summary Table Field Data Log Sheet(s) Chain of Custody Form(s) Site Photographs Maps (from Bruce Monson 07-01-09 email) Maps (received onsite from Bruce Monson) INCLUDED N/A COMMENTS G e n e ra l F ie ld S a m p lin g S u m m ary 1. Sample bottles were prepared by the 3M Environmental Lab. The pre-filled trip blank and trip blank spike accompanied________ the sample bottles for the project duration.________________________________________________________________________ 2. Project was mobilized from the public landing located at the intersection of 7th Ave and Forest St in St. Paul Park, MN._________ 3. Onsite Personnel: Brad Jacobson (Pace) and State representatives Bruce Monson, Harold Wiegner and Marvin Hora._________ 4. Collection Method: Samples were collected by submerging a 2-liter plastic transfer (dipping) container in the river, uncapping the container and allowing it to fill while the boat was slowly idled forward into fresh water. A second 2-liter container was filled in the same fashion. The 3M "Sample", 3M "Spike" and MPCA "Primary" samples were filled from the first dipping container.__________ The 3M "Duplicate" and MPCA "Duplicate" were filled from the second dipping container. MPCA direct dipped the sample container for the MPCA "Triplicate" sample. A new pair of nitrile gloves were worn during the collection procedure at each site.____________ 5. MPCA collected additional volume for three matrix spike samples at Reach 1-Location 1 and Reach 4-Location 11.____________ 6. Due to expected windy, rough conditions on the "big water" areas, the plan to sample from the point of lowest expected________ concentration to highest was not adhered to.______________________________________________________________________ 7. The sample containers, and samples remained in the custody of the Pace field technician until delivery to the 3M Environmental laboratory._________________________________________________________________________________________________ 1700 Elm Street, Suite 200 Minneapolis, MN 55414 TEL: 612-607-1700 FAX: 612-607-6444 Offices Serving: Asheville, NC Charlotte, NC Green 8ay, Wl Indianapolis, IN Kansas City, KS Minneapolis, MN New Orleans, LA Pittsburgh, PA Puerto Rico Seattle, WA SE Kansas Waltz Mill, PA Mississippi River Pool 2 | II Surface Water Sampling - MPCA WATER SAMPLES FOR PFCs DATE 7/8/09 SAMPLEID 1-01-1 1-01-2 1-01-3 1-01-1S 1-01-2S 1-01-3S REACH Reach1 LOCATION Location 1 REPLICATE Primary Duplicate Triplicate MS-1 MS-2 MS-3 Voi (L) 1 1 1 1 1 1 TIME (HH:MM) Water Depth (ft) 14:08 13 Temp 25.74 p. 155 Quanta Sonde SpC DO 378 9.24 pH UTM Coordinates 6.89 0484143 4973007 *pH probe not calibrated* 1-02-1 1-02-2 1-02-3 Location 2 Primary Duplicate Triplicate 1 1 1 13:51 10 25.21 380 9.28 6.84 0486067 4971149 1-03-1 1-03-2 1-03-3 Location 3 Primary Duplicate Triplicate 1 1 1 13:30 12 24.93 382 8.93 6.81 0487624 4971560 2-04-1 2-04-2 2-04-3 Reach 2 Location 4 Primary Duplicate Triplicate 1 1 1 13:17 22 24.21 536 8.67 6.1 0489737 4973910 2-05-1 2-05-2 2-05-3 Location 5 Primary Duplicate Triplicate 1 1 1 12:47 13 . 25.52 525 9.46 6.78 0496075 4975366 2-06-1 2-06-2 2-06-3 Location 6 Primary Duplicate Triplicate 1 1 1 12:30 4 25.03 580 8.72 6.74 0497900 4971442 3-07-1 3-07-2 3-07-3 Reach3 Location 7 Primary Duplicate Triplicate 1 1 1 8:43 11 24.71 587 7.96 6.45 0499081 4965125 3-08-1 3-08-2 3-08-3 Location 8 Primary Duplicate Triplicate 1 1 1 9:06 12 24.73 576 7.82 6.3 0499272 4963280 3-09-1 3-09-2 3-09-3 Location 9 Primary Duplicate Triplicate 1 1 1 9:40 9 24.38 579 7.85 6.4 0503642 4956878 4-10-1 4-10-2 4-10-3 Reach 4 Location 10 Primary Duplicate Triplicate 1 1 1 9:58 12 23.87 579 7.41 6.54 0505348 4958622 4-11-1 4-11-2 4-11-3 4-11-1S 4-11-2S 4-11-3S Location 11 Primary Duplicate Triplicate MS-1 MS-2 MS-3 1 1 1 1 1 1 10:24 4 23.86 566 7.92 6.72 0508545 4958789 4-12-1 4-12-2 4-12-3 Location 12 Primary Duplicate Triplicate 1 1 1 10:47 17 24.28 574 7.26 6.56 0510018 4956960 Random MS/MSD Site Selection LOCATION Rand # 1 0.051 X 11 0.194 X 9 0.225 10 0.266 5 0.276 7 0.380 3 0.426 8 0.538 2 0.554 6 0.856 12 0.869 4 0.965 C:\DOCUME-1\us335208\LOCALS-nTemp\nofesBAAA25\Miss R POOL 2 JULY 2009 water sampling.xls, MPCA SamplelD & Field Sheet, 10/29/09 2 of 3 p. 156 Mississippi River Pool 2 Surface Water Sampling July 2009 Reach-Location-Replicate example: *1-01-1 Reach1 Location 1 MPCA Sample Bottles Vol (L) Vol (L) 3M Sample Bottles Vol (L) Vol (L) Primary Duplicate Triplicate 1 Spike for primary 1 Spike for duplicate 1 Spike for triplicate 1 Primary 0.25 Spike 1 Duplicate 0.25 1 0.25 Voi (L) 2 2 2 Sample Collection CdlDDina") Containers Comments on Use Container will be dipped twice to fill all four bottles, then discarded. Container will be dipped twice to fill all three bottles, then discarded. Container will be dipped once to fill both bottles, then discarded. Location 2 Primary Duplicate Triplicate 1 1 1 Primary 0.25 Spike Duplicate 0.25 0.25 2 2 Use triplicate bottle Container will be dipped once to fill all three bottles, then discarded. Container will be dipped once to fill both bottles, then discarded. Sample bottle itself can serve as "dipping" container. Location 3 Primary Duplicate Triplicate 1 1 1 Primary 0.25 Spike Duplicate 0.25 0.25 2 2 Use triplicate bottle Container will be dipped once to fill ad three bottles, then discarded. Container will be dipped once to fill both bottles, then discarded. Sample bottle itself can serve as "dipping" container. Reach 2 Location 4 Primary Duplicate Triplicate 1 1 1 Primary 0.25 Spike Duplicate 0.25 0.25 2 2 Use triplicate bottle Container will be dipped once to fill all three bottles, then discarded. Container will be dipped once to fill both bottles, then discarded. Sample bottle itself can serve as "dipping" container. Location 5 Primary Duplicate Triplicate 1 1 1 Primary 0.25 Spike Duplicate 0.25 2 2 Use triplicate bottle Container will be dipped once to fill alt three bottles, then discarded. Container will be dipped once to fill both bottles, then discarded. Sample bottle itself can serve as "dipping" container. Location 6 Primary Duplicate Triplicate 1 1 1 Primary 0.25 Spike Duplicate 0.25 2 2 Use triplicate bottle Container will be dipped once to fill all three bottles, then discarded. Container will be dipped once to fill both bottles, then discarded. Sample bottle itself can serve as "dipping" container. Reach3 Location 7 Primary Duplicate Triplicate 1 Spike for primary 1 Spike for duplicate 1 Spike for triplicate 1 Primary 0.25 Spike 1 Duplicate 0.25 1 0.25 2 Container will be dipped twice to fill all four bottles, then discarded. 2 Container will be dipped twice to fill all three bottles, then discarded. 2 Container will be dipped once to fill both bottles, then discarded. Location 8 Primary Duplicate Triplicate 1 1 1 Primary 0.25 Spike Duplicate 0.25 0.25 2 2 Use triplicate bottie Container will be dipped once to fill all three bottles, then discarded. Container will be dipped once to fill both bottles, then discarded. Sample bottie itself can serve as "dipping" container. Location 9 Primary Duplicate Triplicate 1 1 1 Primary 0.25 Spike Duplicate 0.25 0.25 2 2 Use triplicate bottle Container will be dipped once to fill all three bottles, then d iscard ed . Container will be dipped once to fill both bottles, then discarded. Sample bottle itself can serve as "dipping" container. Reach 4 Location 10 Primary Duplicate Triplicate 1 1 1 Primary 0.25 Spike Duplicate 0.25 0.25 2 2 Use triplicate bottle Container will be dipped once to fill all three bottles, then discarded. Container will be dipped once to fill both bottles, then discarded. Sample bottle itself can serve as "dipping" container. Location 11 Primary Duplicate Triplicate 1 1 1 Primary 0.25 Spike Duplicate 0.25 2 2 Use triplicate bottle Container will be dipped once to fill all three bottles, then discarded. Container will be dipped once to fill both bottles, then discarded. Sample bottle itself can serve as "dipping" container. Location 12 Primary Duplicate Triplicate 1 1 1 Primary 0.25 Spike Duplicate 0.25 2 2 Use triplicate bottle Container will be dipped once to fill all three bottles, then discarded. Container will be dipped once to fill both bottles, then discarded. Sample bottle itself can serve as "dipping" container. Number of 1 L bottles required = Number of 0.25 L bottles required = Number of 2 L bottles required = 42 36 26 Note; locations for additional spike bottles for MPCA samples have been arbitrarily assumed - key is that 2 of 12 locations will be sampled in this manner. C:\OOCUME-1\us335208\LOCALS-1\Temp\notesBAAA25\Miss R POOL 2 JULY 2009 water sampting.xls, Gary's Table. 10/29/09 1 of3 p. 157 DI \ CA /O> 'rV(J UQ//tO- T/I//WA Q* ; C L IE N T ID UNITS 1-01-1 ng/L 1-01-2 ng/L 1-01-3 ng/L 1-02-1 ng/L 1-02-2 ng/L 1-02-3 ng/L 1-03-1 ng/L 1-03-2 ng/L 1-03-3 ng/L 2-04-1 ng/L 2-04-2 ng/L 2-04-3 ng/L 2-05-1 ng/L 2-05-2 ng/L 2-05-3 ng/L 2-06-1 ng/L 2-06-2 ng/L 2-06-3 ng/L 3-07-1 ng/L 3-07-2 ng/L 3-07-3 ng/L 3-08-1 ng/L 3-08-2 ng/L 3-08-3 ng/L 3-09-1 ng/L 3-09-2 ng/L 3-09-3 ng/L 4-10-1 ng/L 4-10-2 ng/L 4-10-3 ng/L 4-11-1 ng/L 4-11-2 ng/L 4-11-3 ng/L 4-12-1 ng/L 4-12-2 ng/L 4-12-3 ng/L Lab Blank ng/L PFBA PFPeA 3.76 4.33 5.16 4.4 4.16 5.38 6.79 < 2.56 < 2 .5 7 < 2 .5 4 < 2 .5 4 < 2 .5 5 <2.51 < 2 .5 8 5.01 < 2 .5 2 5.08 < 2 .4 9 3.96 4.81 4.45 4.87 5.25 <2.51 <2.55 <2.52 < 2 .5 4 < 2 .5 6 5.23 < 2 .4 6 8.95 < 2 .5 0 8.61 < 2 .5 2 5.79 < 2 .5 5 10.6 < 2.53 10.7 < 2 .4 9 9.82 < 2 .5 3 11 9.63 9.44 13.2 < 2 .5 5 < 2 .5 5 < 2 .5 6 < 2 .5 2 13.3 < 2 .5 2 11.9 < 2 .5 9 14.8 < 2 .5 4 12.9 < 2 .5 3 9.81 < 2 .4 8 161 14.7 155 15.3 189 16.9 48.6 5.78 51.6 6.15 31.4 3.18 < 2.50 < 2,50 PFHxA < 2 .5 6 < 2 ,5 7 < 2 .5 4 < 2 .5 4 < 2 .5 5 <2.51 < 2 .5 8 < 2 .5 2 < 2 .4 9 <2.51 <2.55 <2.52 < 2 .5 4 < 2 .5 6 < 2 .4 6 < 2 .5 0 2.63 < 2 .5 5 3 3.58 2.57 3.14 < 2.55 2.77 3.06 2.76 3.12 2.91 2.93 < 2.48 16.7 17.9 18 5.23 6.85 4.6 < 2.50 PFHpA < 2 .5 6 < 2 .5 7 < 2 .5 4 < 2 .5 4 < 2 .5 5 <2.51 < 2 .5 8 < 2 .5 2 < 2 .4 9 <2.51 <2.55 <2.52 < 2 .5 4 < 2 .5 6 < 2 .4 6 < 2 .5 0 < 2 .5 2 < 2 .5 5 < 2 .5 3 < 2 .4 9 < 2 .5 3 < 2 .5 5 < 2 .5 5 < 2 .5 6 < 2 .5 2 <2.52 < 2 .5 9 < 2 .5 4 < 2 .5 3 < 2 .4 8 5.77 5.83 6.05 < 2.54 2.91 <2.53 < 2.50 PFOA < 2 .5 6 < 2,57 < 2 .5 4 < 2 .5 4 < 2 .5 5 <2.51 < 2 .5 8 < 2 .5 2 < 2 .4 9 <2.51 <2.55 < 2 .5 2 < 2 .5 4 < 2 .5 6 2.51 3.74 3.94 3.2 4.48 5.01 4.75 5.42 3.91 4.5 4.22 4.63 5.03 3.91 4.21 4.07 88.1 95.8 98.4 17.5 21.3 11.3 < 2.50 PFNA PFDA PFUnA < 2.56 < 2 .56 < 2 .56 < 2.57 < 2 .5 7 < 2 .5 7 <2.54 <2.54 <2.54 <2.54 <2.54 <2.54 <2.55 <2.55 <2.55 <2.51 <2.51 <2.51 <2.58 <2.58 < 2.58 <2.52 <2.52 <2.52 <2.49 <2.49 <2.49 <2.51 <2.51 <2.51 <2.55 <2.55 <2.55 <2.52 <2.52 <2.52 <2.54 <2.54 <2.54 <2,56 <2.56 <2.56 <2.46 <2.46 <2.46 <2.50 <2.50 <2.50 <2.52 <2.52 <2.52 <2.55 <2.55 < 2.55 <2.53 <2.53 <2.53 <2.49 <2.49 <2.49 <2.53 <2.53 <2.53 <2.55 <2.55 <2.55 <2.55 <2.55 <2.55 <2.56 <2.56 <2.56 <2.52 <2.52 <2.52 <2.52 < 2.52 < 2.52 <2.59 <2.59 < 2.59 <2.54 <2.54 <2.54 <2.53 <2.53 <2.53 <2.48 <2.48 < 2.48 <2.54 <2.54 <2.54 <2.59 <2.59 <2.59 <2.48 <2.48 <2.48 <2.54 <2.54 <2.54 <2.55 <2.55 <2.55 <2.53 <2.53 <2.53 < 2.50 < 2.50 < 2.50 PFDoA < 2 .5 6 < 2 .5 7 < 2 .5 4 < 2.54 < 2 .5 5 <2.51 < 2 .5 8 < 2 .5 2 < 2 .4 9 <2.51 <2.55 <2.52 < 2 .5 4 < 2 .5 6 < 2 .4 6 < 2 .5 0 < 2 .5 2 < 2 .5 5 < 2 .5 3 < 2 .4 9 < 2 .5 3 < 2 .5 5 < 2 .5 5 < 2 .5 6 < 2 .5 2 < 2 .5 2 < 2 .5 9 < 2 .5 4 < 2 .5 3 < 2 .4 8 < 2 .5 4 < 2 .5 9 < 2 .4 8 < 2 .5 4 < 2 .5 5 < 2 .5 3 < 2.50 PFBS PFHxS <5.12 <5.12 < 5.14 < 5 ,1 4 < 5.08 < 5 .08 <5.08 <5.08 < 5.10 < 5 .1 0 <5.02 <5.02 <5.15 <5.15 <5.03 <5.03 <4.97 <4.97 <5.03 <5.03 < 5 .0 9 < 5.09 <5.04 <5.04 <5.07 <5.07 <5.11 <5.11 <4.93 <4.93 <5.01 <5.01 <5.05 <5.05 <5.09 <5.09 <5.06 <5.06 <4.98 <4.98 <5.07 <5.07 <5.10 <5.10 <5.09 <5.09 <5.11 <5.11 <5.05 <5.05 <5.04 <5.04 <5.17 <5.17 <5.07 <5.07 <5.05 <5.05 <4.97 <4.97 40.2 28.8 41.7 27.7 41.9 27.9 12.9 16.1 7.69 1 1 .8 13.1 5.64 < 5.00 < 5.00 PFOSA PFOS P F O S PFOS-avg PFOS-avg <2.56 <5.12 2 .5 6 2.56 2.54 < 2.57 <5.14 2 .5 7 <2.54 <5,08 2 .5 4 <2.54 <5.08 2 .5 4 2.53 <2.55 <5.10 2 .5 5 <2.51 < 5.02 2 51 <2.58 <5.15 2 58 2.53 <2.52 <5.03 2 52 <2.49 <4.97 2 49 <2.51 <5.03 8 55 2.53 4.25 <2.55 <5.09 ;5v> <2.52 < 5.04 2 52 <2.54 <5.07 5 54 2.52 <2.56 <5.11 2 56 <2.46 <4.93 2 47 < 2 .5 0 7.1 7 10 7.71 < 2 .5 2 7.8 7 80 < 2 .5 5 8.24 8 24 < 2 .5 3 10.5 in 50 10.30 7.12 < 2 .4 9 10.5 10 50 < 2 .5 3 9.91 Q <-1 < 2 .5 5 8.74 H !A 8.51 < 2 .5 5 8.4 3 40 < 2 .5 6 8.4 3 40 <2.52 <5.05 2 53 2.54 <2.52 <5.04 2 53 <2.59 <5.17 2 59 <2.54 <5.07 2 54 2.52 35.92 <2.53 <5.05 2 45 <2.48 <4.97 2 49 < 2 .5 4 84.4 84 4 0 90.07 < 2 .5 9 91.3 91 80 < 2 .4 8 94.5 94 50 < 2 .5 4 15.1 15 10 15.17 < 2 .5 5 19.2 19 20 <2.53 11.2 i 1 20 < 2.50 | < 5.00 section 1 1 1 2 2 2 3 3 3 4 4 4 using 1/2 DL station PFOS-avg 1 2.56 2 2.53 3 2.53 4 2.53 5 2.52 6 7.71 7 10.30 8 8.51 9 2.54 10 2.52 11 90.07 12 15.17 section PFOS-avg 1 2.54 2 4.25 3 7.12 4 35.92 section 4 median 15.10 C:\DOCUME-1\us335208\LOCALS~1\Temp\notesBAAA25\Miss R POOL 2 JULY 2009 water sampling.xls, Lab Results, 10/29/09 3 of 3