Document jmkxQQzY3o568jm9N5JGDM9rp

3M Environmental Laboratory Report No. ISO12-01-01-03 Final Report Analysis of Water Samples from the Tennessee River - Fall 2012 Laboratory Request Number: ISO12-01 -01 -03 Method Requirement: 3M Method ETS-8-044.1 Report Date - Date of Final Signature Testing Laboratory 3M Environmental, Health, Safety, and Sustainability Operations Environmental Laboratory 3M Center, Bldg 260-05-N-17 St. Paul, MN 55144 Requester Gary Hohenstein 3M Environmental, Health, Safety, and Sustainability Operations 3M Building 224-5W-03 Saint Paul, MN 55144-1000 Phone: (651) 737-3570 The testing reported herein meet the requirements of ANSI/ ISO/IEC 17025:2005 "General Requirements for the Competence of Testing and Calibration Laboratories", in accordance with the A2LA Testing Certificate # 2052.01. Testing that complies with this International Standard also meets principles of ISO 9001:2000. Testing Cert #2052.01 PAGE 1 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 3M Environmental Laboratory 3M Environmental Laboratory Manager: William K. Reagen, Ph.D. 3M Principal Analytical Investigator and Report Author: Susan Wolf Analytical Report ISO12-01-01-03 Analysis of Water Samples from the Tennessee River - Fall 2012 Report Date: Data of Last Signature 1 Summary/Introduction The 3M Environmental Laboratory prepared samples collected by Weston personnel from the Tennessee River, conducted per the study work plan dated October 2012 and titled "Revised Work Plan for Fall 2012 Fish and Surface Water Sampling in the Tennessee " in Decatur, Alabama. Samples were collected from the fish sampling reaches from November 16 - 20, 2012. Samples were collected from the transect locations from December 3-5, 2012. Equipment blank samples were collected November 3 and 29, 2012. Samples were returned to the 3M Environmental Laboratory on November 6, 30 and December 11, 2012, at ambient conditions and under 3M Environmental Laboratory project number ISO12-01-01-03. All samples were analyzed for PFBA, PFHxA, PFHpA, PFOA, PFBS, PFHS, PFOS, FBSA, FOSA, MeFOSAA and EtFOSAA. The 3M Environmental Laboratory prepared sample containers for forty-five (45) surface water locations associated with the fish sampling reaches, and ninety (90) surface water locations associated with the nine transect locations. Each empty container was marked with a "fill to here" line that corresponded to a final volume of 200 mL. Single sample replicates were collected at each of the locations. Field sample duplicates were collected at 10% of the sampling locations (four (4) field duplicates collected at the fish sampling reaches and nine (9) field duplicates collected at the transect locations). In addition to each of the field duplicate samples, at those same locations, a target analyte field matrix spike sample was also collected (four (4) target analyte field matrix spikes collected at the fish sampling reaches and nine (9) target analyte field matrix spikes collected at the transect locations). All samples bottles included the addition of internal standards (ISs) and surrogate recovery standards (SRSs) 13C3-PFBA, 13C4-PFOA, and 13C4-PFOS, which were added to the sample containers prior to being sent to the field for sample collection. Sample bottles reserved for field matrix spikes were fortified with solutions containing the target analytes, prior to being sent to the field for sample collection. Samples were prepared and analyzed using direct injection with and without solvent dilution according to 3M Environmental Laboratory method ETS-8-044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis". Internal standards were used to aid in the data quality objectives. 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. The testing reported herein meet the requirements of ANSI/ISO/IEC 17025:2005 "General Requirements for the Competence of Testing and Calibration Laboratories", in accordance with the A2LA Testing Certificate # 2052.01. Testing that complies with this International Standard also meets principles of ISO 9001:2000. Testing Cert #2052.01 PAGE 2 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 1. Sample Results Summary (1) 3M LIMS ID Sample Description Fish Sampling Reaches ISO12-01 -01 -03-007 DAL-SW-R01L1-0-121116 ISO12-01 -01 -03-008 DAL-SW-R01L2-0-121116 ISO12-01 -01 -03-009 DAL-SW-R01L3-0-121116 ISO12-01 -01 -03-010 DAL-SW-R02L1 -0-121116 ISO12-01 -01 -03-011 DAL-SW-R02L2-0-121116 ISO12-01 -01 -03-012 DAL-SW-R02L3-0-121116 ISO12-01 -01 -03-015 DAL-SW-R03L1 -0-121116 ISO12-01 -01 -03-016 DAL-SW-R03L2-0-121116 ISO12-01 -01 -03-017 DAL-SW-R03L3-0-121116 ISO12-01 -01 -03-018 DAL-SW-R04L1 -0-121116 ISO12-01 -01 -03-019 DAL-SW-R04L2-0-121116 ISO12-01 -01 -03-020 DAL-SW-R04L3-0-121116 ISO12-01 -01 -03-052 DAL-SW-R05L1 -0-121119 ISO12-01 -01 -03-055 DAL-SW-R05L2-0-121119 ISO12-01 -01 -03-056 DAL-SW-R05L3-0-121119 ISO12-01 -01 -03-057 DAL-SW-R06L1 -0-121120 ISO12-01 -01 -03-058 DAL-SW-R06L2-0-121120 ISO12-01 -01 -03-059 DAL-SW-R06L3-0-121120 ISO12-01 -01 -03-049 DAL-SW-R07L1 -0-121119 ISO12-01 -01 -03-050 DAL-SW-R07L2-0-121119 ISO12-01 -01 -03-051 DAL-SW-R07L3-0-121119 ISO12-01 -01 -03-046 DAL-SW-R08L1 -0-121119 ISO12-01 -01 -03-047 DAL-SW-R08L2-0-121119 ISO12-01 -01 -03-048 DAL-SW-R08L3-0-121119 PFBA PFHxA PFHpA Concentration (ng/L; parts per trillion) PFOA PFBS PFHS PFOS FBSA FOSA MeFOSAA EtFOSAA 6.16 6.50 <5.00 7.36 6.06 6.13 5.95 5.77 5.00 7.51 7.27 11.7 58.9 6.51 <5.00 <5.00 <5.00 <5.00 23.6 30.9 9.41 <5.00 <5.00 8.41 2.56 2.83 2.72 4.52 5.56 4.83 <2.00 <2.00 2.85 9.85 13.8 12.4 72.5 4.43 3.47 2.07 <2.00 3.30 34.4 41.4 10.9 2.40 <2.00 3.48 <2.00 <2.00 <2.00 3.47 3.64 4.70 <2.00 <2.00 <2.00 3.82 4.57 3.91 56.8 <2.00 <2.00 <2.00 <2.00 <2.00 16.9 20.8 6.16 <2.00 <2.00 <2.00 2.16 3.04 2.31 10.7 10.4 9.28 3.43 3.70 3.34 13.6 15.0 31.7 246 9.02 5.82 2.97 <4.80 2.76 50.3 62.6 21.1 3.37 2.56 4.70 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 10.4 124 <5.00 <5.00 <5.00 <5.00 <5.00 46.4 63.8 9.65 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 7.03 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 11.0 39.8 <5.00 <5.00 <5.00 <5.00 <5.00 16.4 19.5 <5.00 <5.00 <5.00 <5.00 6.91 7.62 6.69 9.32 9.06 8.94 7.03 7.34 6.39 14.4 18.0 70.5 385 17.7 9.84 6.84 6.72 6.77 84.2 102 34.8 6.42 6.57 7.67 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 2.14 2.07 4.86 1130 <2.00 <2.00 <2.00 <2.00 <2.00 245 352 48.6 <2.00 <2.00 2.08 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 21.1 <2.00 <2.00 <2.00 <2.00 <2.00 3.69 5.65 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 10.0 <2.00 <2.00 <2.00 <9.98 <2.00 2.14 <2.00 <2.00 <2.00 <2.00 <2.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 18.0 <5.00 <5.00 <5.00 <15.0 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 (1) All samples associated with the reported sampling location were analyzed using internal calibration. The analytical method uncertainties for the reported results are as follows: PFBA 16%, PFHxA 20%, PFHpA 21 %, PFOA 23%, PFBS 20%, PFHS 25% , PFOS 17%, FBSA 17%, FOSA 14%, MeFOSAA 25%, and EtFOSAA 17%. PAGE 3 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 1 continued. Sample Results Summary (1) 3M LIMS ID Sample Description Fish Sampling Reaches ISO12-01 -01 -03-043 DAL-SW-R09L1 -0-121119 ISO12-01 -01 -03-044 DAL-SW-R09L2-0-121119 ISO12-01 -01 -03-045 DAL-SW-R09L3-0-121119 ISO12-01 -01 -03-038 DAL-SW-R10L1-0-121119 ISO12-01 -01 -03-039 DAL-SW-R10L2-0-121119 ISO12-01 -01 -03-040 DAL-SW-R10L3-0-121119 ISO12-01 -01 -03-035 DAL-SW-R11L1 -0-121119 ISO12-01 -01 -03-036 DAL-SW-R11L2-0-121119 ISO12-01 -01 -03-037 DAL-SW-R11L3-0-121119 ISO12-01 -01 -03-032 DAL-SW-R12L1-0-121117 ISO12-01 -01 -03-033 DAL-SW-R12L2-0-121117 ISO12-01 -01 -03-034 DAL-SW-R12L3-0-121117 ISO12-01 -01 -03-029 DAL-SW-R13L1-0-121117 ISO12-01 -01 -03-030 DAL-SW-R13L2-0-121117 ISO12-01 -01 -03-031 DAL-SW-R13L3-0-121117 ISO12-01 -01 -03-021 DAL-SW-R14L1-0-121117 ISO12-01 -01 -03-022 DAL-SW-R14L2-0-121117 ISO12-01 -01 -03-023 DAL-SW-R14L3-0-121117 ISO12-01 -01 -03-024 DAL-SW-R15L1-0-121117 ISO12-01 -01 -03-027 DAL-SW-R15L2-0-121117 ISO12-01 -01 -03-028 DAL-SW-R15L3-0-121117 PFBA PFHxA PFHpA Concentration (ng/L; parts per trillion) PFOA PFBS PFHS PFOS FBSA FOSA MeFOSAA EtFOSAA 29.5 36.9 26.5 7.16 5.20 <5.00 22.5 24.2 16.7 5.46 6.89 6.63 7.95 8.65 7.76 6.82 6.41 7.48 7.92 7.43 7.55 59.2 61.9 49.5 3.23 2.10 2.73 75.5 70.2 47.7 7.41 7.56 6.61 10.2 8.59 10.9 4.82 5.32 6.34 4.24 4.60 4.69 22.1 25.4 18.1 <2.00 <2.00 <2.00 19.5 22.6 12.0 <2.00 <2.00 <2.00 3.36 3.26 2.57 <2.00 2.18 2.19 2.34 2.23 2.07 62.3 79.9 58.0 2.63 2.53 3.52 53.1 61.9 38.7 6.35 6.51 7.09 14.4 18.2 15.3 11.1 11.5 12.0 11.5 12.8 10.7 64.1 84.6 59.4 <5.00 <5.00 <5.00 52.1 51.1 28.9 <5.00 <5.00 <5.00 10.0 12.0 9.83 7.61 7.69 8.47 14.8 13.2 14.1 19.7 26.2 19.6 <5.00 <5.00 <5.00 17.9 18.9 11.3 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 103 125 91.0 6.82 6.99 6.49 87.8 91.0 69.5 12.4 13.8 13.3 24.8 27.7 23.8 18.7 19.0 23.0 19.9 18.4 18.1 185 330 197 <2.00 <2.00 <2.00 129 116 74.1 4.75 4.95 5.12 20.4 24.4 21.6 14.7 14.3 16.1 34.8 32.8 32.8 6.15 7.71 5.47 <2.00 <2.00 <2.00 5.65 4.19 3.89 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 (1) All samples associated with the reported sampling location were analyzed using internal calibration. The analytical method uncertainties for the reported results are as follows: PFBA 16%, PFHxA 20%, PFHpA 21 %, PFOA 23%, PFBS 20%, PFHS 25%, PFOS 17%, FBSA 17%, FOSA 14%, MeFOSAA 25%, and EtFOSAA 17%. PAGE 4 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 1 continued. Sample Results Summary (1) 3M LIMS ID Sample Description Transect Sampling Locations ISO12-01 -01 -03-062 DAL-SW-T101 -0-121203 ISO12-01 -01 -03-065 DAL-SW-T102-0-121203 ISO12-01 -01 -03-066 DAL-SW-T103-0-121203 ISO12-01 -01 -03-067 DAL-SW-T104-0-121203 ISO12-01 -01 -03-068 DAL-SW-T105-0-121203 ISO12-01 -01 -03-069 DAL-SW-T106-0-121203 ISO12-01 -01 -03-070 DAL-SW-T107-0-121203 ISO12-01 -01 -03-071 DAL-SW-T108-0-121203 ISO12-01 -01 -03-072 DAL-SW-T109-0-121203 ISO12-01 -01 -03-073 DAL-SW-T 110-0-121203 ISO12-01 -01 -03-074 DAL-SW-T201 -0-121203 ISO12-01 -01 -03-075 DAL-SW-T202-0-121203 ISO12-01 -01 -03-078 DAL-SW-T203-0-121203 ISO12-01 -01 -03-079 DAL-SW-T204-0-121203 ISO12-01 -01 -03-080 DAL-SW-T205-0-121203 ISO12-01 -01 -03-081 DAL-SW-T206-0-121203 ISO12-01 -01 -03-082 DAL-SW-T207-0-121203 ISO12-01 -01 -03-083 DAL-SW-T208-0-121204 ISO12-01 -01 -03-084 DAL-SW-T209-0-121204 ISO12-01 -01 -03-085 DAL-SW-T210-0-121204 PFBA PFHxA PFHpA Concentration (ng/L; parts per trillion) PFOA PFBS PFHS PFOS FBSA FOSA MeFOSAA EtFOSAA <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 6.13 <2.00 <2.00 <2.00 <5.00 2.12 <2.00 <1.92 <5.00 <5.00 6.15 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 2.51 <5.00 <5.00 6.80 <2.00 <2.00 <2.00 <5.00 2.18 <2.00 2.55 <5.00 <5.00 6.89 <2.00 <2.00 <2.00 <5.00 2.16 <2.00 2.56 <5.00 <5.00 6.63 <2.00 <2.00 <2.00 5.19 <2.00 <2.00 2.57 <5.00 <5.00 6.43 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 6.38 <2.00 <2.00 <2.00 <5.00 2.00 <2.00 8.73 <5.00 9.38 6.60 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 2.75 <5.00 <5.00 6.45 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 6.70 <2.00 <2.00 <2.00 5.79 4.75 3.07 9.73 <5.00 <5.00 8.35 <2.00 <2.00 <2.00 6.72 5.16 4.80 12.6 <5.00 <5.00 9.93 <2.00 <2.00 <2.00 <5.00 2.20 <2.00 <1.92 <5.00 <5.00 6.50 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 2.42 <5.00 <5.00 6.23 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 3.01 <5.00 <5.00 6.96 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 2.66 <5.00 <5.00 6.79 <2.00 <2.00 <2.00 <5.00 2.11 <2.00 2.08 <5.00 <5.00 6.83 <2.00 <2.00 <2.00 5.66 <2.00 <2.00 3.02 <5.00 <5.00 6.44 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 2.27 <5.00 <5.00 6.98 <2.00 <2.00 <2.00 <5.00 2.19 <2.00 3.90 <5.00 <5.00 7.77 <2.00 <2.00 <2.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 (1) All samples associated with the reported sampling location were analyzed using internal calibration. The analytical method uncertainties for the reported results are as follows: PFBA 16%, PFHxA 20%, PFHpA 21 %, PFOA 23%, PFBS 20%, PFHS 25%, PFOS 17%, FBSA 17%, FOSA 14%, MeFOSAA 25%, and EtFOSAA 17%. PAGE 5 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 1 continued. Sample Results Summary (1) 3M LIMS ID Sample Description Transect Sampling Locations ISO12-01 -01 -03-086 DAL-SW-T301 -0-121203 ISO12-01 -01 -03-087 DAL-SW-T302-0-121203 ISO12-01 -01 -03-088 DAL-SW-T303-0-121203 ISO12-01 -01 -03-091 DAL-SW-T304-0-121203 ISO12-01 -01 -03-092 DAL-SW-T305-0-121203 ISO12-01 -01 -03-093 DAL-SW-T306-0-121203 ISO12-01 -01 -03-094 DAL-SW-T307-0-121203 ISO12-01 -01 -03-095 DAL-SW-T308-0-121203 ISO12-01 -01 -03-096 DAL-SW-T309-0-121203 ISO12-01 -01 -03-097 DAL-SW-T310-0-121203 ISO12-01 -01 -03-098 DAL-SW-T401 -0-121203 ISO12-01 -01 -03-099 DAL-SW-T402-0-121203 ISO12-01 -01 -03-100 DAL-SW-T403-0-121203 ISO12-01 -01 -03-101 DAL-SW-T404-0-121203 ISO12-01 -01 -03-104 DAL-SW-T405-0-121203 ISO12-01 -01 -03-105 DAL-SW-T406-0-121203 ISO12-01 -01 -03-106 DAL-SW-T407-0-121203 ISO12-01 -01 -03-107 DAL-SW-T408-0-121203 ISO12-01 -01 -03-108 DAL-SW-T409-0-121203 ISO12-01 -01 -03-109 DAL-SW-T410-0-121203 PFBA PFHxA PFHpA Concentration (ng/L; parts per trillion) PFOA PFBS PFHS PFOS FBSA FOSA MeFOSAA EtFOSAA <5.00 4.55 2.23 15.2 <5.00 <5.00 19.0 2.32 <2.00 <2.00 <5.00 2.14 <2.00 2.97 <5.00 <5.00 7.46 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 2.78 <5.00 <5.00 6.94 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 2.15 <5.00 <5.00 7.68 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 7.30 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 6.11 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 6.57 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 6.98 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 6.58 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 2.28 <5.00 <5.00 7.32 <2.00 <2.00 <2.00 38.1 33.4 19.6 74.5 285 17.4 138 453 18.3 4.46 5.98 2.86 <2.00 4.54 <5.00 <5.00 8.69 2.81 <2.00 <2.00 7.83 <2.00 <2.00 2.73 <5.00 <5.00 7.52 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 2.25 <5.00 <5.00 7.29 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 8.21 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 7.42 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 7.31 <2.00 <2.00 <2.00 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 7.04 <2.00 <2.00 <2.00 5.04 <2.00 <2.00 <1.92 <5.00 <5.00 6.73 <2.00 <2.00 <2.00 5.67 2.84 <2.00 3.87 <5.00 <5.00 7.78 <2.00 <2.00 <2.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 (1) All samples associated with the reported sampling location were analyzed using internal calibration. The analytical method uncertainties for the reported results are as follows: PFBA 16%, PFHxA 20%, PFHpA 21 %, PFOA 23%, PFBS 20%, PFHS 25%, PFOS 17%, FBSA 17%, FOSA 14%, MeFOSAA 25%, and EtFOSAA 17%. PAGE 6 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 1 continued. Sample Results Summary (1) 3M LIMS ID Sample Description Transect Sampling Locations ISO12-01 -01 -03-110 DAL-SW-T501 -0-121204 ISO12-01 -01 -03-111 DAL-SW-T502-0-121204 ISO12-01 -01 -03-112 DAL-SW-T503-0-121204 ISO12-01 -01 -03-113 DAL-SW-T504-0-121204 ISO12-01 -01 -03-114 DAL-SW-T505-0-121204 ISO12-01 -01 -03-117 DAL-SW-T506-0-121204 ISO12-01 -01 -03-118 DAL-SW-T507-0-121204 ISO12-01 -01 -03-119 DAL-SW-T508-0-121204 ISO12-01 -01 -03-120 DAL-SW-T509-0-121204 ISO12-01 -01 -03-121 DAL-SW-T510-0-121204 ISO12-01 -01 -03-122 DAL-SW-T601 -0-121204 ISO12-01 -01 -03-123 DAL-SW-T602-0-121204 ISO12-01 -01 -03-124 DAL-SW-T603-0-121204 ISO12-01 -01 -03-125 DAL-SW-T604-0-121204 ISO12-01 -01 -03-126 DAL-SW-T605-0-121204 ISO12-01 -01 -03-127 DAL-SW-T606-0-121204 ISO12-01 -01 -03-130 DAL-SW-T607-0-121204 ISO12-01 -01 -03-131 DAL-SW-T608-0-121204 ISO12-01 -01 -03-132 DAL-SW-T609-0-121204 ISO12-01 -01 -03-133 DAL-SW-T610-0-121204 PFBA PFHxA PFHpA Concentration (ng/L; parts per trillion) PFOA PFBS PFHS PFOS FBSA FOSA MeFOSAA EtFOSAA 23.7 24.3 14.4 <5.00 <5.00 <5.00 <5.00 <5.00 5.02 8.56 43.2 23.3 13.9 8.09 7.48 <5.00 <5.00 <5.00 5.72 8.74 26.7 24.5 13.7 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 3.99 69.4 27.8 14.6 7.90 5.65 2.31 <2.00 <2.00 <2.00 2.75 14.4 14.2 9.19 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 27.3 22.0 9.62 4.85 3.37 <2.00 <2.00 <2.00 <2.00 <2.00 48.2 45.7 29.0 <1.92 2.52 2.59 2.20 3.33 3.27 4.33 69.2 68.6 36.8 14.6 9.37 4.38 <1.92 <1.92 2.61 3.12 105 115 63.8 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 89.6 124 57.0 23.7 12.4 <5.00 <5.00 <5.00 <5.00 <5.00 14.3 12.6 8.35 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 24.2 18.0 9.19 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 72.8 76.5 49.2 7.89 7.20 6.82 8.10 8.20 8.15 8.57 86.4 107 56.6 23.8 14.5 9.72 6.49 6.92 7.66 7.83 139 168 96.4 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 2.29 254 168 75.3 32.1 15.8 2.22 <2.00 <2.00 <2.00 <2.00 5.69 6.61 2.58 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 6.17 5.06 3.06 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 (1) All samples associated with the reported sampling location were analyzed using internal calibration. The analytical method uncertainties for the reported results are as follows: PFBA 16%, PFHxA 20%, PFHpA 21 %, PFOA 23%, PFBS 20%, PFHS 25%, PFOS 17%, FBSA 17%, FOSA 14%, MeFOSAA 25%, and EtFOSAA 17%. PAGE 7 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 1 continued. Sample Results Summary (1) 3M LIMS ID Sample Description Transect Sampling Locations ISO12-01 -01 -03-134 DAL-SW-T701 -0-121204 ISO12-01 -01 -03-135 DAL-SW-T702-0-121204 ISO12-01 -01 -03-136 DAL-SW-T703-0-121204 ISO12-01 -01 -03-137 DAL-SW-T704-0-121204 ISO12-01 -01 -03-138 DAL-SW-T705-0-121204 ISO12-01 -01 -03-139 DAL-SW-T706-0-121204 ISO12-01 -01 -03-140 DAL-SW-T707-0-121204 ISO12-01 -01 -03-143 DAL-SW-T708-0-121204 ISO12-01 -01 -03-144 DAL-SW-T709-0-121204 ISO12-01 -01 -03-145 DAL-SW-T710-0-121204 ISO12-01 -01 -03-146 DAL-SW-T801 -0-121205 ISO12-01 -01 -03-147 DAL-SW-T802-0-121205 ISO12-01 -01 -03-148 DAL-SW-T803-0-121205 ISO12-01 -01 -03-149 DAL-SW-T804-0-121205 ISO12-01 -01 -03-150 DAL-SW-T805-0-121205 ISO12-01 -01 -03-151 DAL-SW-T806-0-121205 ISO12-01 -01 -03-152 DAL-SW-T807-0-121205 ISO12-01 -01 -03-153 DAL-SW-T808-0-121205 ISO12-01 -01 -03-156 DAL-SW-T809-0-121205 ISO12-01 -01 -03-157 DAL-SW-T810-0-121205 PFBA PFHxA PFHpA Concentration (ng/L; parts per trillion) PFOA PFBS PFHS PFOS FBSA FOSA MeFOSAA EtFOSAA 18.1 15.7 11.4 8.59 9.71 10.1 8.42 6.96 7.35 8.39 6.89 6.82 9.03 7.76 8.01 5.79 6.26 6.28 6.50 5.62 17.5 15.8 12.3 8.17 9.49 7.39 4.05 3.90 4.20 5.25 4.58 4.33 3.80 4.46 3.92 3.80 2.95 4.51 2.80 2.79 8.58 9.41 8.23 4.78 6.15 5.83 3.24 2.82 2.32 3.52 <2.00 <2.00 <2.00 2.81 <2.00 3.07 2.03 <2.00 <2.00 <2.00 28.1 30.7 29.8 18.5 18.9 14.5 12.5 7.98 6.86 10.7 8.51 9.43 10.2 7.81 8.08 7.30 7.21 7.49 7.26 6.49 71.0 65.1 55.6 32.5 36.2 26.9 19.0 14.0 10.6 17.7 13.0 12.5 13.2 14.3 12.9 12.1 11.5 11.2 9.28 11.1 8.07 8.37 7.69 <5.00 5.17 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 42.6 46.6 46.8 31.6 31.2 24.2 20.2 16.5 13.4 17.6 15.2 15.4 15.9 16.6 15.4 12.1 14.1 13.3 11.5 12.3 213 118 75.1 41.3 47.7 35.6 27.6 17.2 12.6 20.0 32.2 31.4 34.8 35.0 35.0 28.2 27.0 25.7 18.9 14.1 4.77 2.86 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 (1) All samples associated with the reported sampling location were analyzed using internal calibration. The analytical method uncertainties for the reported results are as follows: PFBA 16%, PFHxA 20%, PFHpA 21 %, PFOA 23%, PFBS 20%, PFHS 25%, PFOS 17%, FBSA 17%, FOSA 14%, MeFOSAA 25%, and EtFOSAA 17%. PAGE 8 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 1 continued. Sample Results Summary (1) 3M LIMS ID Sample Description Transect Sampling Locations ISO12-01 -01 -03-158 DAL-SW-T901 -0-121205 ISO12-01 -01 -03-159 DAL-SW-T902-0-121205 ISO12-01 -01 -03-160 DAL-SW-T903-0-121205 ISO12-01 -01 -03-161 DAL-SW-T904-0-121205 ISO12-01 -01 -03-162 DAL-SW-T905-0-121205 ISO12-01 -01 -03-163 DAL-SW-T906-0-121205 ISO12-01 -01 -03-164 DAL-SW-T907-0-121205 ISO12-01 -01 -03-165 DAL-SW-T908-0-121205 ISO12-01 -01 -03-166 DAL-SW-T909-0-121205 ISO12-01 -01 -03-169 DAL-SW-T910-0-121205 Trip and Equipment Blanks ISO12-01 -01 -03-001 DAL-MSW-LS-EQB01 ISO12-01 -01 -03-002 DAL-MSW-LS-EQB02 ISO12-01 -01 -03-003 DAL-MSW-LS-EQB03 ISO12-01 -01 -03-060 DAL-SW-TRIP01-0-121116 ISO12-01 -01 -03-170 DAL-SW-TRIP-01 -0-121203 ISO12-01 -01 -03-172 DAL-IPW-LS- EQB04 PFBA PFHxA PFHpA Concentration (ng/L; parts per trillion) PFOA PFBS PFHS PFOS FBSA FOSA MeFOSAA EtFOSAA 7.76 9.09 3.32 12.9 17.7 <5.00 20.3 34.7 <2.00 <2.00 9.51 7.72 3.88 11.9 11.2 <5.00 20.5 35.1 <2.00 <2.00 7.45 7.62 2.16 11.9 14.2 <5.00 20.1 33.4 <2.00 <2.00 8.98 7.82 3.28 13.1 13.7 <5.00 20.7 36.9 <2.00 <2.00 7.48 8.78 3.11 13.2 14.7 <5.00 24.4 35.4 <2.00 <2.00 6.76 6.57 3.30 10.9 13.9 <5.00 19.7 43.2 <2.00 <2.00 7.69 7.25 3.99 11.5 12.7 <5.00 21.4 43.9 <2.00 <2.00 6.74 6.58 3.43 12.1 13.4 <5.00 20.3 45.4 <2.00 <2.00 8.66 7.12 3.37 11.6 12.8 <5.00 19.2 46.3 <2.00 <2.00 7.96 6.42 3.37 10.9 13.4 <5.00 19.0 45.5 <2.00 <2.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <1.92 <1.92 <1.92 <1.92 <1.92 <1.92 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 <0.927 1.05 <0.927 <0.927 <0.927 <0.927 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <2.00 <5.00 <5.00 <5.00 <5.00 <5.00 <5.00 (1) All samples associated with the reported sampling location were analyzed using internal calibration. The analytical method uncertainties for the reported results are as follows: PFBA 16%, PFHxA 20%, PFHpA 21 %, PFOA 23%, PFBS 20%, PFHS 25%, PFOS 17%, FBSA 17%, FOSA 14%, MeFOSAA 25%, and EtFOSAA 17%. PAGE 9 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 2. Surrogate Recovery Standards Summary SRS R e c o v e ry (%) 3M LIMS ID Sample Description Fish Sampling Reaches ISO12-01-01-03-007 DAL-SW-R01L1 -0-121116 ISO12-01-01-03-008 DAL-SW-R01L2-0-121116 ISO12-01-01-03-009 DAL-SW-R01L3-0-121116 ISO12-01 -01 -03-010 DAL-SW-R02L1 -0-121116 ISO12-01-01-03-011 DAL-SW-R02L2-0-121116 ISO12-01 -01 -03-012 DAL-SW-R02L3-0-121116 ISO12-01 -01 -03-013 DAL-SW-R02L3-DB-121116 ISO12-01 -01 -03-014 DAL-SW-R02L3-FMS-121116 ISO12-01 -01 -03-015 DAL-SW-R03L1 -0-121116 ISO12-01 -01 -03-016 DAL-SW-R03L2-0-121116 ISO12-01 -01 -03-017 DAL-SW-R03L3-0-121116 ISO12-01 -01 -03-018 DAL-SW-R04L1 -0-121116 ISO12-01 -01 -03-019 DAL-SW-R04L2-0-121116 ISO12-01-01-03-020 DAL-SW-R04L3-0-121116 ISO12-01-01-03-052 DAL-SW-R05L1 -0-121119 ISO12-01-01-03-053 DAL-SW-R05L1 -DB-121119 ISO12-01-01-03-054 DAL-SW-R05L1 -FMS-121119 ISO12-01-01-03-055 DAL-SW-R05L2-0-121119 ISO12-01-01-03-056 DAL-SW-R05L3-0-121119 ISO12-01-01-03-057 DAL-SW-R06L1 -0-121120 ISO12-01-01-03-058 DAL-SW-R06L2-0-121120 ISO12-01-01-03-059 DAL-SW-R06L3-0-121120 ISO12-01-01-03-049 DAL-SW-R07L1 -0-121119 ISO12-01-01-03-050 DAL-SW-R07L2-0-121119 ISO12-01 -01 -03-051 DAL-SW-R07L3-0-121119 ISO12-01-01-03-046 DAL-SW-R08L1 -0-121119 ISO12-01-01-03-047 DAL-SW-R08L2-0-121119 ISO12-01-01-03-048 DAL-SW-R08L3-0-121119 ISO12-01-01-03-043 DAL-SW-R09L1 -0-121119 ISO12-01-01-03-044 DAL-SW-R09L2-0-121119 ISO12-01-01-03-045 DAL-SW-R09L3-0-121119 ISO12-01-01-03-038 DAL-SW-R10L1-0-121119 ISO12-01-01-03-039 DAL-SW-R10L2-0-121119 ISO12-01-01-03-040 DAL-SW-R10L3-0-121119 ISO12-01 -01 -03-041 DAL-SW-R10L3-DB-121119 ISO12-01-01-03-042 DAL-SW-R10L3-FMS-121119 ISO12-01-01-03-035 DAL-SW-R11L1-0-121119 ISO12-01-01-03-036 DAL-SW-R11L2-0-121119 ISO12-01-01-03-037 DAL-SW-R11L3-0-121119 ISO12-01-01-03-032 DAL-SW-R12L1-0-121117 ISO12-01-01-03-033 DAL-SW-R12L2-0-121117 ISO12-01-01-03-034 DAL-SW-R12L3-0-121117 13C3-PFBA 90.6 93.8 93.8 93.8 94.2 94.8 92.6 93.6 89.8 92.2 95.6 90.6 92.2 92.8 93.6 91.2 92.2 92.8 91.4 88.2 94.2 89.4 90.4 96.0 99.4 94.6 95.0 92.6 89.8 92.2 95.8 91.4 92.8 90.0 93.0 90.8 90.2 94.4 94.2 90.2 95.2 96.0 13C4-PFOA 93.0 82.4 83.4 87.2 87.0 82.0 85.0 87.4 87.2 81.4 86.6 85.4 83.8 84.4 82.4 83.0 87.4 84.8 84.6 85.2 85.6 86.2 82.8 86.2 86.4 83.8 85.4 84.2 85.4 83.6 83.6 80.0 83.8 89.0 86.6 84.0 79.0 83.2 85.2 76.6 85.8 87.4 13C4-PFOS 89.1 91.4 91.8 88.5 90.6 90.8 91.0 89.5 91.1 92.6 92.0 92.9 94.8 90.8 89.1 92.9 91.6 91.4 99.4 90.1 89.4 91.5 96.9 88.3 97.9 87.7 89.7 90.0 95.6 95.0 97.3 91.6 89.7 91.8 91.2 91.8 94.1 89.7 90.0 89.3 93.7 95.6 PAGE 10 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 2 continued. Surrogate Recovery Standards Summary 3M LIMS ID Sample Description Fish Sampling Reaches ISO12-01-01-03-029 DAL-SW-R13L1-0-121117 ISO12-01-01-03-030 DAL-SW-R13L2-0-121117 ISO12-01 -01 -03-031 DAL-SW-R13L3-0-121117 ISO12-01 -01 -03-021 DAL-SW-R14L1-0-121117 ISO12-01-01-03-022 DAL-SW-R14L2-0-121117 ISO12-01-01-03-023 DAL-SW-R14L3-0-121117 ISO12-01-01-03-024 DAL-SW-R15L1-0-121117 ISO12-01-01-03-025 DAL-SW-R15L1-DB-121117 ISO12-01-01-03-026 DAL-SW-R15L1-FMS-121117 ISO12-01-01-03-027 DAL-SW-R15L2-0-121117 ISO12-01-01-03-028 DAL-SW-R15L3-0-121117 Transect Sampling Locations ISO12-01-01-03-062 DAL-SW-T101-0-121203 ISO12-01-01-03-063 DAL-SW-T101-DB-121203 ISO12-01-01-03-064 DAL-SW-T 101-FMS-121203 ISO12-01-01-03-065 DAL-SW-T102-0-121203 ISO12-01-01-03-066 DAL-SW-T103-0-121203 ISO12-01-01-03-067 DAL-SW-T104-0-121203 ISO12-01-01-03-068 DAL-SW-T105-0-121203 ISO12-01-01-03-069 DAL-SW-T106-0-121203 ISO12-01 -01 -03-070 DAL-SW-T107-0-121203 ISO12-01 -01 -03-071 DAL-SW-T108-0-121203 ISO12-01-01-03-072 DAL-SW-T109-0-121203 ISO12-01-01-03-073 DAL-SW-T 110-0-121203 ISO12-01 -01 -03-074 DAL-SW-T201 -0-121203 ISO12-01-01-03-075 DAL-SW-T202-0-121203 ISO12-01 -01 -03-076 DAL-SW-T202-DB-121203 ISO12-01-01-03-077 DAL-SW-T202-FMS-121203 ISO12-01 -01 -03-078 DAL-SW-T203-0-121203 ISO12-01-01-03-079 DAL-SW-T204-0-121203 IS012-01-01-03-080 DAL-SW-T205-0-121203 ISO12-01 -01 -03-081 DAL-SW-T206-0-121203 ISO12-01-01-03-082 DAL-SW-T207-0-121203 ISO12-01-01-03-083 DAL-SW-T208-0-121204 ISO12-01-01-03-084 DAL-SW-T209-0-121204 ISO12-01-01-03-085 DAL-SW-T210-0-121204 SRS R e c o v e ry (%) 13C3-PFBA 13C4-PFOA 13C4-PFOS 88.8 92.6 92.8 95.4 95.4 94.0 90.4 93.1 93.0 94.4 91.8 79.6 82.2 84.4 81.8 88.0 89.8 85.6 86.8 86.0 83.8 84.0 92.1 91.2 94.4 93.9 92.5 90.2 94.1 93.7 95.2 91.2 88.5 94.2 96.2 93.8 92.2 92.6 93.0 96.6 95.6 96.6 95.0 92.6 94.6 97.0 94.4 93.6 99.8 94.2 94.0 94.6 95.0 91.6 95.2 97.4 96.8 86.4 86.4 82.2 86.4 91.2 92.2 87.8 88.0 84.8 86.6 92.4 90.0 89.0 91.0 91.4 88.2 84.4 87.8 90.6 83.8 83.4 92.0 85.2 92.6 91.0 90.0 94.8 94.4 92.3 90.0 91.8 92.5 91.8 89.1 91.2 94.1 92.1 92.1 90.8 92.1 91.4 92.9 92.3 92.9 93.7 92.7 92.9 86.8 PAGE 11 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 2 continued. Surrogate Recovery Standards Summary 3M LIMS ID Sample Description Transect Sampling Locations ISO12-01-01-03-086 DAL-SW-T301 -0-121203 ISO12-01-01-03-087 DAL-SW-T302-0-121203 ISO12-01-01-03-088 DAL-SW-T303-0-121203 ISO12-01-01-03-089 DAL-SW-T303-DB-121203 IS012-01-01-03-090 DAL-SW-T303-FMS-121203 ISO12-01 -01 -03-091 DAL-SW-T304-0-121203 ISO12-01-01-03-092 DAL-SW-T305-0-121203 ISO12-01-01-03-093 DAL-SW-T306-0-121203 ISO12-01-01-03-094 DAL-SW-T307-0-121203 ISO12-01-01-03-095 DAL-SW-T308-0-121203 ISO12-01-01-03-096 DAL-SW-T309-0-121203 ISO12-01-01-03-097 DAL-SW-T310-0-121203 ISO12-01-01-03-098 ISO12-01-01-03-099 ISO12-01 -01 -03-100 ISO12-01 -01 -03-101 ISO12-01 -01 -03-102 ISO12-01 -01 -03-103 ISO12-01 -01 -03-104 ISO12-01 -01 -03-105 ISO12-01 -01 -03-106 ISO12-01 -01 -03-107 ISO12-01 -01 -03-108 ISO12-01 -01 -03-109 ISO12-01-01-03-110 ISO12-01-01-03-111 ISO12-01-01-03-112 ISO12-01-01-03-113 ISO12-01-01-03-114 ISO12-01-01-03-115 ISO12-01-01-03-116 ISO12-01-01-03-117 ISO12-01-01-03-118 ISO12-01-01-03-119 ISO12-01 -01 -03-120 ISO12-01 -01 -03-121 DAL-SW-T401-0-121203 DAL-SW-T402-0-121203 DAL-SW-T403-0-121203 DAL-SW-T404-0-121203 DAL-SW-T404-DB-121203 DAL-SW-T404-FMS-121203 DAL-SW-T405-0-121203 DAL-SW-T406-0-121203 DAL-SW-T407-0-121203 DAL-SW-T408-0-121203 DAL-SW-T409-0-121203 DAL-SW-T410-0-121203 DAL-SW-T501 -0-121204 DAL-SW-T502-0-121204 DAL-SW-T503-0-121204 DAL-SW-T504-0-121204 DAL-SW-T505-0-121204 DAL-SW-T505-DB-121204 DAL-SW-T505-FMS-121204 DAL-SW-T506-0-121204 DAL-SW-T507-0-121204 DAL-SW-T508-0-121204 DAL-SW-T509-0-121204 DAL-SW-T510-0-121204 SRS R e c o v e ry (%) 13C3-PFBA 13C4-PFOA 13C4-PFOS 96.4 94.8 91.2 94.2 93.0 94.6 96.2 95.0 94.6 93.0 93.8 95.6 95.4 96.6 94.4 96.0 92.2 93.8 94.0 92.8 95.0 94.0 91.4 94.8 95.2 94.8 97.2 96.4 94.6 95.2 94.2 96.0 96.0 93.8 96.4 93.2 90.0 87.6 90.2 89.6 85.8 90.4 85.4 91.2 89.6 84.6 86.6 88.8 87.0 85.4 91.6 87.8 92.0 88.8 88.0 90.6 81.8 93.0 86.2 90.0 89.6 88.2 91.2 86.8 88.0 84.6 86.4 88.6 85.2 91.6 85.4 91.4 93.3 95.0 93.3 92.5 94.1 92.5 90.6 90.6 91.6 91.4 90.8 90.6 91.8 92.1 91.0 94.6 91.6 93.9 90.6 91.6 90.4 92.5 91.2 89.3 97.9 95.8 97.3 93.3 93.5 93.9 93.9 90.8 91.0 94.1 90.6 91.4 PAGE 12 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 2 continued. Surrogate Recovery Standards Summary 3M LIMS ID Sample Description Transect Sampling Locations ISO12-01 -01 -03-122 ISO12-01 -01 -03-123 ISO12-01 -01 -03-124 ISO12-01 -01 -03-125 ISO12-01 -01 -03-126 ISO12-01 -01 -03-127 ISO12-01 -01 -03-128 ISO12-01 -01 -03-129 ISO12-01 -01 -03-130 ISO12-01 -01 -03-131 ISO12-01 -01 -03-132 ISO12-01 -01 -03-133 DAL-SW-T601 -0-121204 DAL-SW-T602-0-121204 DAL-SW-T603-0-121204 DAL-SW-T604-0-121204 DAL-SW-T605-0-121204 DAL-SW-T606-0-121204 DAL-SW-T606-DB-121204 DAL-SW-T606-FMS-121204 DAL-SW-T607-0-121204 DAL-SW-T608-0-121204 DAL-SW-T609-0-121204 DAL-SW-T610-0-121204 ISO12-01 -01 -03-134 ISO12-01 -01 -03-135 ISO12-01 -01 -03-136 ISO12-01 -01 -03-137 ISO12-01 -01 -03-138 ISO12-01 -01 -03-139 ISO12-01 -01 -03-140 ISO12-01 -01 -03-141 ISO12-01 -01 -03-142 ISO12-01 -01 -03-143 ISO12-01 -01 -03-144 ISO12-01 -01 -03-145 DAL-SW-T701 -0-121204 DAL-SW-T702-0-121204 DAL-SW-T703-0-121204 DAL-SW-T704-0-121204 DAL-SW-T705-0-121204 DAL-SW-T706-0-121204 DAL-SW-T707-0-121204 DAL-SW-T707-DB-121204 DAL-SW-T707-FMS-121204 DAL-SW-T708-0-121204 DAL-SW-T709-0-121204 DAL-SW-T710-0-121204 ISO12-01 -01 -03-146 ISO12-01 -01 -03-147 ISO12-01 -01 -03-148 ISO12-01 -01 -03-149 ISO12-01 -01 -03-150 ISO12-01 -01 -03-151 ISO12-01 -01 -03-152 ISO12-01 -01 -03-153 ISO12-01 -01 -03-154 ISO12-01 -01 -03-155 ISO12-01 -01 -03-156 ISO12-01 -01 -03-157 DAL-SW-T801 -0-121205 DAL-SW-T802-0-121205 DAL-SW-T803-0-121205 DAL-SW-T804-0-121205 DAL-SW-T805-0-121205 DAL-SW-T806-0-121205 DAL-SW-T807-0-121205 DAL-SW-T808-0-121205 DAL-SW-T808-DB-121205 DAL-SW-T808-FMS-121205 DAL-SW-T809-0-121205 DAL-SW-T810-0-121205 SRS R e c o v e ry (%) 13C3-PFBA 13C4-PFOA 13C4-PFOS 93.2 94.6 94.6 93.0 94.0 96.8 94.2 96.6 93.0 94.4 94.0 92.4 95.8 96.2 95.0 94.6 95.0 99.4 91.6 95.2 93.4 94.4 93.6 94.4 94.4 93.8 92.8 95.8 94.8 92.6 93.0 93.2 94.6 95.6 95.0 96.0 85.6 83.2 95.4 84.8 83.8 86.0 86.0 86.0 85.5 88.6 84.6 88.8 88.8 85.6 87.0 86.2 85.2 86.6 92.6 92.6 92.9 82.4 87.8 93.6 86.2 89.0 90.4 87.0 88.6 81.0 87.2 84.8 87.4 91.0 93.6 93.0 92.9 94.1 93.5 95.4 91.6 92.7 90.2 91.6 89.3 91.4 92.9 89.7 93.5 96.2 96.2 97.7 94.6 97.7 91.8 90.0 94.9 100 91.0 93.3 92.1 91.4 91.4 92.7 93.9 91.4 96.2 92.3 96.2 93.7 92.5 92.3 PAGE 13 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 2 continued. Surrogate Recovery Standards Summary SRS R e c o v e ry (%) 3M LIMS ID Sample Description Transect Sampling Locations 13C3-PFBA ISO12-01 -01 -03-158 DAL-SW-T901 -0-121205 ISO12-01 -01 -03-159 DAL-SW-T902-0-121205 ISO12-01 -01 -03-160 DAL-SW-T903-0-121205 ISO12-01 -01 -03-161 DAL-SW-T904-0-121205 ISO12-01 -01 -03-162 DAL-SW-T905-0-121205 ISO12-01 -01 -03-163 DAL-SW-T906-0-121205 ISO12-01 -01 -03-164 DAL-SW-T907-0-121205 ISO12-01 -01 -03-165 DAL-SW-T908-0-121205 ISO12-01 -01 -03-166 DAL-SW-T909-0-121205 ISO12-01 -01 -03-167 DAL-SW-T909-DB-121205 ISO12-01 -01 -03-168 DAL-SW-T909-FMS-121205 ISO12-01 -01 -03-169 DAL-SW-T910-0-121205 Trip Blank Samples and Equipment Blanks ISO12-01 -01 -03-001 DAL-MSW-LS-EQB01 IS012-01-01-03-002 DAL-MSW-LS-EQB02 IS012-01-01-03-003 DAL-MSW-LS-EQB03 IS012-01-01-03-060 DAL-SW-TRIP01-0-121116 ISO12-01 -01 -03-061 DAL-SW-TRIP02-0-121116 ISO12-01 -01 -03-170 DAL-SW-TRIP-01 -0-121203 ISO12-01-01-03-171 DAL-SW-TRIP-01 -FMS-121203 ISO12-01 -01 -03-172 DAL-IPW-LS-EQB04 95.6 93.0 95.8 94.6 95.2 96.4 98.0 94.0 93.0 94.4 93.2 94.0 96.0 90.8 93.6 93.0 92.4 94.4 96.6 93.2 13C4-PFOA 86.0 88.2 89.2 88.0 90.6 83.8 88.4 89.4 86.2 95.6 87.8 95.0 88.0 84.8 86.4 89.4 87.2 85.2 88.6 87.2 13C4-PFOS 94.1 91.8 91.0 90.0 93.7 93.9 93.9 95.0 96.9 96.2 95.6 92.3 95.2 95.0 92.5 90.6 92.5 92.9 88.1 93.3 2 Method Summary 2.1 Methods Analysis of the surface water samples was completed following 3M Environmental Laboratory method ETS-8-044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS". Table 2 lists the target analytes for this sampling event. Table 3. Target Analytes. Target Analytes Perfluorobutanoic Acid (C4 Acid) Perfluorohexanoic Acid (C6 Acid) Perfluoroheptanoic Acid (C7 Acid) Perfluorooctanoic Acid (C8 Acid) Perfluorobutanesulfonate (C4 Sulfonate ) Perfluorohexanesulfonate (C6 Sulfonate) Perfluorooctanesulfonate (C8 Sulfonate) Perfluorobutanesulfonamide Perfluorooctanesulfonamide 2-(N-methyl-PFOSA) acetic acid 2-(N-ethyl-PFOSA) acetic acid Acronym PFBA PFHxA PFHpA PFOA PFBS PFHS PFOS FBSA FOSA MeFOSAA EtFOSAA Reference Material Structure Linear Linear Linear Linear + Branched Linear Linear Linear + Branched Linear Linear + Branched Linear Linear PAGE 14 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 2.2 Sample Collection Water samples were collected in 250 mL NalgeneTM (high-density polyethylene) bottles prepared at the 3M Environmental Laboratory. Laboratory prepared Trip Blanks and Trip Blank field matrix spikes were sent with the set of collection bottles. Samples were returned to the 3M Environmental Laboratory on November 6, 30 and December 11,2012, at ambient conditions. Samples were stored refrigerated at the laboratory after receipt. Table 3 defines how the samples were identified. Table 4. Sample Description Key Code. String Number Example 1 1 2 3 4 5 6 Example 2 1 2 3 4 5 6 String Descriptor Example DAL-SW-R01L1-0-121116 (Fish Sampling Location) Sample Location DAL= Decatur, Alabama Sample Type SW = Surface Water Fish Sampling Reach R01 = Reach 1 Sampling Location L1 = Location 1 (three locations sampled within each fish sampling reach) Sample Type 0 = primary sample DB = duplicate sample FMS = Field Matrix Spike Sampling Date 121116- November 16, 2012 DAL-SW-T805-0-121205 (Transect Sampling Location) Sample Location DAL= Decatur, Alabama Sample Type SW = Surface Water Transect Sampling Location T8 = Transect 8 Sampling Location Sample Type 05 = Location 5 (ten locations sampled within each transect ) 0 = primary sample DB = duplicate sample FMS = Field Matrix Spike Sampling Date 121205- December 05, 2012 PAGE 15 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 5 summarizes the general location of the fifteen fish sampling reaches and nine transect locations. Table 5. Sampling Locations. Fish Sampling reaches R01 Tennessee River RM 320 below Triana R02 Point Mallard RM 307.5 R03 Tennessee River RM 307.5 R04 Betty Rye Branch and Dry Branch RM 303 R05 Bakers Creek Mouth RM 301 R06 Swan Creek Mouth RM 301 R)7 Tennessee River RM 298 R08 Round Island Creek Mouth RM 298 R09 Fox Creek Mouth RM 296 R10 Browns Ferry - RM 294 R11 Mallard Creek Mouth RM 293.5 R12 Elk River Mouth RM 285 R13 Tennessee River RM 281 R14 Tennessee River RM 273 R15 Tennessee River RM 264 Transect Sampling Locations T1 Below Triana coincides with fish reach RM 320 T2 Coincides with fish sampling at RM 307.5 T3 Coincides with fish sampling reach at RM 303 T4 Coincides with fish sampling reach at RM 301 T5 Coincides with fish sampling reach at RM 298 T6 Coincides with fish sampling reach at RM 296 T7 Coincides with fish sampling reach at RM 293.5 T8 Coincides with fish sampling reach at RM 281 T9 Coincides with fish sampling reach at RM 264 2.3 Sample Preparation All samples were initially prepared by removing a 0.4 mL aliquot of the well mixed sample and diluting it with 0.4 mL of methanol (dilution factor of 2). During the preparation of the laboratory control samples, an aliquot of a separate internal standard spiking solution was added to the laboratory control samples (nominal concentration of 200 or 100 ng/L). The sample bottles were spiked with an internal standard mix at a nominal concentration of 100 ng/L prior to being sent to the field for sample collection. The laboratory control samples were then diluted with methanol in the same manner as the samples. All samples were prepared for PFBA analysis by removing an aliquot of the well mixed sample and placing it in an autovial for analysis. Several of the prepared samples were re-analyzed for PFOS to achieve a lower limit of quantitation than was obtainable by the analysis of the samples diluted with methanol. During the preparation of the laboratory control samples, an aliquot of a separate internal standard spiking solution was added to the laboratory control samples (nominal concentration of 100 ng/L). The PAGE 16 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 sample bottles were spiked with an internal standard mix at a nominal concentration of 100 ng/L prior to being sent to the field for sample collection. 2.4 Analysis All samples and quality control samples were analyzed for eleven 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. The following analytical runs were processed and reported herein. 12/28/12 Analysis: Samples were analyzed for all analytes by direct injection solvent dilution, however the QC criterias was not met for several analytes and the LOQ was higher than anticipated for PFHS and PFOS. Since no improvement was seen in the LOQ for PFHS and PFOS from the re-analysis, sample results from this run were reported for PFHS, PFOS, FBSA, FOSA, MeFOSAA, EtFOSAA, and PFOS-Surrogate. 1/5/13 Analysis: Samples were re-analyzed by direct injection solvent dilution for PFHxA, PFHpA, PFOA, PFBS, PFHS, and PFOS. Since no improvement was seen in the LOQ for PFHS and PFOS, sample results were reported for PFHS and PFOS from the initial analysis. Due to high background, PFBS was not reported from this run. Sample results from this run were reported for PFHxA PFHpA PFOA and PFOA-Surrogate. 1/11/13 Analysis: Samples were re-analyzed by direct injection solvent dilution and reported for PFBS. 1/28/12 Analysis: This run was a re-analysis by direct injection solvent dilution of locations DAL SW R05L1, DAL SW R06L2, DAL SW T401, and DAL SW T707, to verify results from initial analysis. FBSA results were reported for DAL SW R05L1, PFBS, FBSA, FOSA, MeFOSAA, and EtFOSAA were reported for DAL SW R06L2, and PFBS, PFOS, FBSA, FOSA, and C4-PFOS were reported for DAL SW T707. 1/31/13 Analysis: This run was a re-analysis by direct injection solvent dilution of locations DAL SW R06L2 and DAL SW T707 to verify results from initial analysis. PFHxA, PFHpA, PFOA, and 13C4PFOA were reported for DAL SW R06L2 and DAL SW T707. 2/1/13 Analysis: This run was a re-analysis of all sampling locations that had a PFOS below the limit of quantitation for the initial sample analysis. This was a direct injection (no solvent dilution) analysis. Sampling locations DAL SW R06L1, DAL SW R06L2, and DAL SW R06L3 were inadvertently missed during the re-analysis and were later analyzed on 2/7/13. Samples were reported for PFOS and 13C4PFOS. 2/4/13 Analysis: This was a direct injection (no solvent dilution) analysis of all samples for PFBA and 13C3-PFBA. 2/6/13 Analysis: This run was a re-analysis by direct injection (no solvent dilution) of sampling locations, DAL SW R03L1 - L3 and DAL SW R06L1-L3 for PFOS and 13C4-PFOS. PAGE 17 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Due to the nature of the sample, the wide range of concentrations found in the sample, and the environmental occurrence of multiple isomers of the laboratory's analytes of interest, the software used for processing the analytical results is not able to consistently integrate the analytical peak, manual integration of the analytical peak is necessary. All manual integrations are performed following the procedures outlined in method ETS-12-010. The consistency of the laboratory's integration is ensured through the training of laboratory personnel, the peer review process required for all manual integrations, the review of manual integrations by the QAU, and where necessary the review of manual integrations by laboratory management. Table 6. Instrument Parameters. Instrum ent Nam e Analysis Dates A nalytical Method Liquid Chrom atograph G uard colum n Analytical colum n Injection V olum e Mass Spectrom eter Ion S ource E le c tro d e P o la rity S o ftw a re ETS Kirk 12/28/12 and 1/28/13 ETS-8-044.1 Agilent 1260 Betasil C18 (4.6 mm X 100 mm), 5 g Betasil C18 (4.6 mm X 100 mm), 5g 100 gL Applied Biosystems API 5500 Turbo Spray Turbo ion electrode Negative Analyst 1.5.2 ETS McCoy 1/5/13, 1/11/13, 1/31/13, 2/1/13, 2/4/13, and 2/6/13 ETS-8-044.1 Agilent 1290 Prism RP (2.1 mm X 50 mm), 5 g Betasil C18 (2.1 mm X 100 mm), 5g 100 gL Applied Biosystems API 5500 Turbo Spray Turbo ion electrode Negative Analyst 1.5.2 PAGE 18 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 7. Liquid Chromatography Conditions. Step Number 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 8 9 0 1 2 3 4 5 6 7 Total Time (min) Flow Rate (uL/min) Percent A (2m M am m onium acetate) Analysis Dates:12/28/12 and 1/28/13 0.00 750 90.0 0.50 750 4.00 750 90.0 70.0 6.00 750 70.0 11.0 750 20.0 13.0 750 20.0 13.5 750 16.0 750 10.0 10.0 16.5 750 90.0 19.0 750 90.0 Analysis Dates: 1/5/13, 1/11/13, 1/31/13, 2/1/13, and 2/6/13 0.00 300 90.0 0.50 300 90.0 4.00 300 70.0 6.00 300 70.0 11.0 300 20.0 13.0 300 20.0 13.5 300 10.0 16.0 300 10.0 16.5 300 19.0 300 90.0 90.0 Analysis Date 2/4/13 0.00 300 90.0 0.50 300 90.0 4.00 300 70.0 6.00 300 70.0 6.10 300 8.00 300 10.0 10.0 8.10 300 90.0 10.0 300 90.0 Percent B (M e th a n o l) 10.0 10.0 30.0 30.0 80.0 80.0 90.0 90.0 10.0 10.0 10.0 10.0 30.0 30.0 80.0 80.0 90.0 90.0 10.0 10.0 10.0 10.0 30.0 30.0 90.0 90.0 10.0 10.0 PAGE 19 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 8. Mass Transitions. Analyte Mass Transition Q1/Q3 Internal Standard Mass Transition Q1/Q3 PFBA 213/169 ( 3C4]PFBA 217/172 PFHxA 313/119 313/269 fCJPFHxA 315/270 PFHpA 363/319 363/119 fC ]P F H p A 367/322 413/369 PFOA 413/219 tC jP FO A 421/376 413/169 PFBS 299/80 299/99 t 82]PFBS 303/84 PFHS 399/99 399/80 f 3C3]PFHS 402/80 499/99 PFOS 499/80 t 3C8]PFOS 507/80 499/130 FBSA 298/78 fO lP F B S 303/84 FOSA 498/78 f 3Cs 1FOSA 506/78 570/219 573/219 MeFOSAA 570/169 d3-MeFOSAA 573/169 570/83 573/83 584/219 589/219 EtFOSAA 584/169 d5-EtFOSAA 589/169 584/83 589/83 f 3C3PFBA surrogate 216/172 f 3C41PFBA 217/172 f 3C4PFOA surrogate 417/372 fC lP FO A 421/376 f 3C4lPFOS surrogate 503/80 f 3Cs !PFOS 507/80 Dwell time was 20 msec for each transition. The individual transitions were summed to produce a "total ion chromatogram" (TIC), which was used for quantitation. 3 Analytical Results 3.1 Calibration Samples were analyzed against a matrix-matched stable isotope internal standard calibration curve. Calibration standards were prepared by spiking known amounts of stock solutions into 25 mL of 50:50 laboratory reagent water:methanol. The calibration standards contained an internal standard mix at a nominal concentration of 50 ng/L. A total of nine calibration standards ranging from 1 ng/L to 250 ng/L (nominal) were prepared. Of these nine calibration standards, six contained the surrogates at concentrations ranging from 7.5 ng/L to 250 ng/L nominal. A quadratic, 1/x weighted, calibration curve of the ratio of the standard peak area counts over the internal standard peak area counts was used to fit the data for each analyte. The data were not forced through zero during the fitting process. Calculating the standard concentrations using the peak area ratios and the resultant calibration curve confirmed accuracy of each curve point. The reference standards of PFOA and PFOS used to prepare the calibration standards consisted of both linear and branched isomers. For samples that exceeded the PAGE 20 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 above calibration range, an additional set of standards were prepared which extended the calibration range to 2000 ng/L. 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. Samples for PFBA and PFOS were analyzed against a matrix-matched stable isotope internal standard calibration curve. Calibration standards were prepared by spiking known amounts of stock solutions into 25 mL of laboratory reagent water. The calibration standards contained an internal standard mix at a nominal concentration of 100 ng/L. A total of nine calibration standards ranging from 1 ng/L to 250 ng/L (nominal) were prepared. O f these nine calibration standards, six contained the surrogates at concentrations ranging from 10 ng/L to 250 ng/L nominal. A quadratic, 1/x weighted, calibration curve of the ratio of the standard peak area counts over the internal standard peak area counts was used to fit the data for each analyte. The data were not forced through zero during the fitting process. Calculating the standard concentrations using the peak area ratios and the resultant calibration curve confirmed accuracy of each curve point. The reference standard of PFOS used to prepare the calibration standards consisted of both linear and branched isomers. 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 PFBA, PFOS, 13C3-PFBA, and 13C4-PFOS. 3.2 System Suitability A calibration standard was analyzed four times at the beginning of the analytical sequence to demonstrate overall system suitability. The acceptance criteria of less than or equal to 5% relative standard deviation (RSD) for peak area ratio and retention time criteria of less than or equal to 2% RSD were met for all analytes. 3.3 Limit of Quantitation (LOQ) The LOQ as defined in method ETS-8-044.1 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 8 below. PAGE 21 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 9. LOQ Analyte Analysis Date PFHxA PFHpA 1/5/13 1/5/13 PFOA 1/5/13 PFBS 1/11/13 PFHS 12/28/12 PFOS 12/28/12 FBSA 12/28/12 FOSA N-MeFOSAA 12/28/12 12/28/12 N-EtFOSAA 12/28/12 PFBS 1/28/13 PFOS 1/28/13 FBSA FOSA 1/28/13 1/28/13 MeFOSAA 1/28/13 EtFOSAA 1/28/13 PFHxA 1/31/3 PFHpA 1/31/3 PFOA 1/31/3 PFOS 2/1/13 PFBA 2/4/13 PFOS 2/6/13 (1) A dilution factor of 2 was applied to the LOQ. LOQ, ng/L (1) 2.00 (1) 2.00 (1) 1.92 (1) 5.00 (1) 5.00 (1) 9.28 (1) 2.00 (1) 2.00 (1) 2.00 (1) 5.00 (1) 5.00 (1) 9.28 (1) 2.00 (1) 2.00 (1) 9.98 (1) 15.0 (1) 2.00 (1) 2.00 (1) 4.80 (1) 0.927 5.00 0.927 3.4 Continuing Calibration During the course of each analytical sequence, continuing calibration verification samples (CCVs) were analyzed to confirm that the instrument response and the initial calibration curve were still in control. All reported sample results were bracketed by CCVs that met method criteria of 100% 25% with the following exceptions: 12/28/12 Analysis: Twenty-one (21) CCV samples were anlyzed over the course of the analysis. One CCV for MeFOSAA did not meet method acceptance criteria with a recovery of 126%. Two CCVs for EtFOSAA did not meet method acceptance criteria with recoveries of 126% and 127%. One of the CCV samples was a standard that did not contain the surrogate 13C4-PFOS. 1/5/13 Analysis: Twenty (20) CCV samples were anlyzed over the course of the analysis. One of the CCV samples was a standard that did not contain the surrogate 13C4-PFOA. 2/1/13 Analysis: Thirteen (13) CCV samples were analyzed. Two of the CCV samples was a standard that did not contain the surrogate 13C4-PFOS. Two CCVs of the same concentration did not meet method acceptance criteria for PFOS with recoveries of 128% and 152%, however; the internal standard area counts suggest that the autiovial may have been low on sample. A new vial of the standard was analyzed at the end of the run and met method acceptance criteria. 3.5 Blanks Three types of blanks were prepared and analyzed with the samples: solvent blanks (procedural blanks), field/trip blanks, and equipment rinseate blanks for the surface water samples. Each blank result was reviewed and used to evaluate method performance. Procedural blank results were reviewed PAGE 22 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 according to the method and used to evaluate method performance to determine the LOQ for each analyte. 3.6 Lab Control Spikes (LCSs) Low, mid, and high lab control spikes were prepared and analyzed in triplicate for the target analytes, while only low and high lab control spikes were prepared for the surrogates. LCSs were prepared by spiking known amounts of the analytes into 10 mL of laboratory reagent water. Where applicable, the LCSs were then diluted 1:1 with methanol in the same manner as the samples. The method acceptance criteria states that the average recovery of LCSs be 100% 20% with a RSD <20%, when evaluated independently at each concentration level. All LCSs met these criteria with the following exceptions. 12/28/12 Analysis: Two sets of LCS samples were prepared and analyzed with the samples. One set was prepared on 12/27/12 and the second set was prepared on 12/28/12. The low set of LCSs prepared on 12/27/12 were below the limit of quantitation (BLOQ) for PFOS, 13C4-PFOS, and EtFOSAA. A recovery could not be calculated. Two of the three low LCSs prepared on 12/27/12 for PFHS were BLOQ. For the one replicate that was reportable, the recovery was 148%. The low set of LCSs prepared on 12/28/12 were BLOQ for 13C4-PFOS. Two of the three low LCSs for PFOS and EtFOSAA were BLOQ. For the one replicate that was reportable for PFOS, the recovery was 264%. This LCS was shown to be contaminated for PFOS during a re-anlysis of the samples on 1/5/13, however, no PFOS results are being reported from the 1/5/13 analysis. This replicate was not used in the determination of the method uncertainty in Secion 3.7. The low set of LCSs for MeFOSAA had a RPD value of 30%. 1/5/13 Analysis: Two sets of LCS samples were prepared and anlyzed with the samples. One set was prepared on 12/27/12 and the second set was prepared on 12/28/12. The low set of LCSs prepared on 12/27/12 had an average recoveries of 73.1% for PFHpA. 64.3% for PFOA, and 159% for 13C4-PFOA. The high recovery for the surrogate13C4-PFOA is possibly due to the trace level of 13C4-PFOA present in the 13C8-PFOA internal standard. The low set of LCSs prepared on 12/28/12 were BLOQ for 13C4-PFOA. 1/11/13 Analysis: Two sets of LCS samples were preapred and anlyzed with the samples. One set was prepared on 12/27/12 and the second set was preapred on 12/28/12. Both sets of low level LCSs had recoveries near 200%. Further investigation into the high recoveries concluded that the spiking solution that was used to prepare the low level LCSs was contaminated with PFBS. The mid and high sets of LCSs met method acceptance criteria. The low level LCSs are reported herein, but were not in the determination of the method uncertainty in Secion 3.7. 1/28/13 Analysis: Four spike levels were prepared for the target analytes, with only two of the spike levels contained the surrogates. The low set of LCSs (5 ppt) prepared on 1/28/13 were BLOQ for MeFOSAA and EtFOSAA. The low-mid set of LCSs (10 ppt) prepared on 1/28/13 were BLOQ for EtFOSAA. One of the three low-mid set of LCSs was BLo Q for MeFOSAA. This spike level was at the LOQ and had an average recovery of 127%. PAGE 23 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 1/31/13 Analysis: Four spike level were prepared for the target analytes, with ony two of the spike levels contained the surrogates. The low set of LCSs (5 ppt) prepared on 1/28/13 were BLOQ for PFOA. A method deviation is included with the raw data. The LCS results were used to determine overall method uncertainty in Section 3.7. The following calculations were used to generate data in Table 10 for laboratory control spikes. Calculated Concentration * ____ _ LCS Percent Recovery -------------------------------------* 100% Spike Concentration LCS% RSD = standard deviation LCS replicates * 1 0 0 % average LCS recovery PAGE 24 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 10. Laboratory Control Spike Recovery. ETS-8-044.1 Analyzed 12/28/12 Lab ID LCS-121227-1 LCS-121227-2 LCS-121227-3 Average %RSD LCS-121227-4 LCS-121227-5 LCS-121227-6 Average %RSD LCS-121227-7 LCS-121227-8 LCS-121227-9 Average %RSD PFHS Spiked Calculated Concentration Concentration (ng/L) (ng/L) 5.00 <5.00 5.00 5.00 <5.00 7.41 148% (2) 49.8 49.8 49.8 48.9 50.5 47.9 99.0 99.0 99.0 98.4% 2.5% 94.5 100 99.0 98.8% 3.0% %Recovery NA (1) NA (1) 148 98.2 101 96.1 95.5 101 100 PFOS (Linear + Branched) Spiked Calculated Concentration Concentration (ng/L) (ng/L) %Recovery 4.63 <9.29 NA (1) 4.63 4.63 <9.28 <9.28 NA NA (1) NA (1) 46.1 46.1 46.1 91.8 91.8 91.8 41.9 42.2 44.8 93.2% 3.7% 93.8 89.9 88.9 99.0% 2.7% 91.0 91.5 97.2 102 98.0 96.9 ETS-8-044.1 Analyzed 12/28/12 Lab ID LCS-121227-1 LCS-121227-2 LCS-121227-3 Average %RSD LCS-121227-4 LCS-121227-5 LCS-121227-6 Average %RSD LCS-121227-7 LCS-121227-8 LCS-121227-9 Average %RSD FBSA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 5.00 5.00 5.00 4.81 5.39 5.12 49.8 49.8 49.8 102% 5.8% 46.8 49.7 52.0 99.0 99.0 99.0 99.3% 5.1% 94.6 97.4 100 98.3% 2.7% %Recovery 96.1 108 102 94.0 99.9 104 95.6 98.4 101 FOSA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 5.00 5.00 5.00 4.46 5.08 4.30 92.4% 9.1% 49.8 49.8 49.8 50.7 47.5 49.9 99.0 99.0 99.0 99.1% 3.5% 99.6 100 103 102% 1.7% %Recovery 89.3 102 86.0 102 95.3 100 101 101 104 (1) NA = Not Applicable; the sample result was below the limit of quantitation and a recovery could not be calculated. (2) The average recovery did not meet method acceptance criteria of 100 20% or a RSD of <20%. PAGE 25 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 10 continued. Laboratory Control Spike Recovery. ETS-8-044.1 Analyzed 12/28/12 Lab ID LCS-121227-1 LCS-121227-2 LCS-121227-3 Average %RSD LCS-121227-4 LCS-121227-5 LCS-121227-6 Average %RSD LCS-121227-7 LCS-121227-8 LCS-121227-9 Average %RSD MeFOSAA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 4.99 4.14 4.99 4.99 5.26 5.64 49.7 49.7 49.7 98.8 98.8 98.8 100% 16% 49.8 42.3 55.7 99.0% 14% 100 107 106 106% 4.1% %Recovery 82.9 105 113 100 85.1 112 101 109 108 EtFOSAA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 4.99 <5.00 4.99 4.99 49.7 49.7 49.7 98.8 98.8 98.8 <5.00 <5.00 NA 46.6 58.8 48.3 103% 13% 94.8 100 101 100% 3.6% %Recovery NA (1) NA (1) NA (1) 93.8 118 97.3 96.0 101 103 ETS-8-044.1 Analyzed 12/28/12 Lab ID LCS-121227-1 LCS-121227-2 LCS-121227-3 Average %RSD LCS-121227-4 LCS-121227-5 LCS-121227-6 Average %RSD LCS-121227-7 LCS-121227-8 LCS-121227-9 Average %RSD 13C4-PFOS Spiked Calculated Concentration Concentration (ng/L) (ng/L) 9.55 <14.4 9.55 9.55 47.6 47.6 47.6 <14.4 <14.4 NA 46.0 50.5 48.8 94.7 94.7 94.7 102% 4.6% 89.1 92.7 94.7 97.3% 3.1% %Recovery NA (1) NA (1) NA (1) 96.6 106 102 94.1 97.9 100 (1) NA = Not Applicable; the sample result was below the limit of quantitation and a recovery could not be calculated. (2) The average recovery did not meet method acceptance criteria of 100 20% or a RSD of <20%. PAGE 26 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 10 continued. Laboratory Control Spike Recovery. ETS-8-044.1 Analyzed 12/28/12 Lab ID LCS-121228-1 LCS-121228-2 LCS-121228-3 Average %RSD LCS-121228-4 LCS-121228-5 LCS-121228-6 Average %RSD LCS-121228-7 LCS-121228-8 LCS-121228-9 Average %RSD PFHS Spiked Calculated Concentration Concentration (ng/L) (ng/L) 5.02 6.78 5.02 5.02 5.23 5.25 50.0 50.0 50.0 99.5 99.5 99.5 1 1 5 15% 52.2 51.7 51.7 103% 0.56% 98.5 106 98.1 102% 4.7% %Recovery 135 104 105 104 103 103 99.0 107 98.6 PFOS (Linear + Branched) Spiked Calculated Concentration Concentration (ng/L) (ng/L) %Recovery 4.65 12.3 264 (2) 4.65 4.65 46.4 46.4 46.4 92.2 92.2 92.2 <9.28 <9.28 NA 44.0 43.6 46.4 96.3% 3.4% 85.1 96.2 96.3 100% 6.7% NA (1)2 NA (1) 94.8 94.0 100 92.3 104 104 ETS-8-044.1 Analyzed 12/28/12 Lab ID LCS-121228-1 LCS-121228-2 LCS-121228-3 Average %RSD LCS-121228-4 LCS-121228-5 LCS-121228-6 Average %RSD LCS-121228-7 LCS-121228-8 LCS-121228-9 Average %RSD FBSA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 5.02 5.28 5.02 5.02 50.0 50.0 50.0 5.19 5.05 103% 1.9% 47.6 53.6 48.0 99.5 99.5 99.5 99.4% 6.6% 96.9 106 97.2 101% 5.4% %Recovery 105 103 101 95.2 107 96.0 97.4 107 97.7 FOSA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 5.02 5.59 5.02 5.02 50.0 50.0 50.0 99.5 99.5 99.5 4.86 5.39 105% 6.9% 50.9 51.6 50.9 102% 0.56% 104 105 102 104% 1.7% %Recovery 111 96.9 107 102 103 102 105 105 102 (1) NA = Not Applicable; the sample result was below the limit of quantitation and a recovery could not be calculated. (2) The average recovery did not meet method acceptance criteria of 100 20% or a RSD of <20%. PAGE 27 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 10 continued. Laboratory Control Spike Recovery. ETS-8-044.1 Analyzed 12/28/12 Lab ID LCS-121228-1 LCS-121228-2 LCS-121228-3 Average %RSD LCS-121228-4 LCS-121228-5 LCS-121228-6 Average %RSD LCS-121228-7 LCS-121228-8 LCS-121228-9 Average %RSD MeFOSAA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 5.01 6.99 5.01 6.40 5.01 3.79 49.9 49.9 49.9 99.3 99.3 99.3 115% 30% (2) 48.1 50.4 52.5 101% 4.3% 101 104 107 104% 3.4% %Recovery 140 128 75.7 96.3 101 105 101 104 108 EtFOSAA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 5.01 5.28 5.01 5.01 49.9 49.9 49.9 99.3 99.3 99.3 <5.00 <5.00 105% 48.0 49.6 54.7 102% 7.1% 96.7 122 117 112% 12% %Recovery 105 NA (1) NA (1) 96.2 99.5 110 97.4 122 118 ETS-8-044.1 Analyzed 12/28/12 Lab ID LCS-121228-1 LCS-121228-2 LCS-121228-3 Average %RSD LCS-121228-4 LCS-121228-5 LCS-121228-6 Average %RSD LCS-121228-7 LCS-121228-8 LCS-121228-9 Average %RSD 13C4-PFOS Spiked Calculated Concentration Concentration (ng/L) (ng/L) 9.60 <14.4 9.60 9.60 47.8 47.8 47.8 <14.4 <14.4 NA 47.2 48.7 48.9 101% 1.9% 95.1 87.4 95.1 90.9 95.1 90.4 94.2% 2.1% %Recovery NA (1)2 NA (1) NA (1) 98.7 102 102 91.9 95.6 95.1 (1) NA = Not Applicable; the sample result was below the limit of quantitation and a recovery could not be calculated. (2) The average recovery did not meet method acceptance criteria of 100 20% or a RSD of <20%. PAGE 28 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 10 continued. Laboratory Control Spike Recovery. ETS-8-044.1 Analyzed 1/5/13 Lab ID LCS-121227-1 LCS-121227-2 LCS-121227-3 Average %RSD LCS-121227-4 LCS-121227-5 LCS-121227-6 Average %RSD LCS-121227-7 LCS-121227-8 LCS-121227-9 Average %RSD PFHxA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 5.00 4.76 5.00 5.00 4.77 4.89 49.8 49.8 49.8 99.0 99.0 99.0 96.1% 1.5% 48.1 51.5 50.5 100% 3.3% 102 102 101 103% 0.56% %Recovery 95.2 95.4 97.8 96.6 103 101 103 103 102 PFHpA Spiked Concentration (ng/L) Calculated Concentration (ng/L) 5.00 4.35 5.00 5.00 49.8 49.8 49.8 99.0 99.0 99.0 3.04 3.57 73.1% 18% (2) 45.6 47.8 52.8 97.8% 7.6% 92.5 106 102 101% 6.9% %Recovery 87.0 60.9 71.3 91.5 96.0 106 93.4 107 103 ETS-8-044.1 Analyzed 1/5/13 Lab ID LCS-121227-1 LCS-121227-2 LCS-121227-3 Average %RSD LCS-121227-4 LCS-121227-5 LCS-121227-6 Average %RSD LCS-121227-7 LCS-121227-8 LCS-121227-9 Average %RSD PFOA (Linear + Branched) Spiked Calculated Concentration Concentration (ng/L) (ng/L) %Recovery 4.79 2.97 62.0 4.79 4.79 3.50 2.78 73.1 57.9 47.7 47.7 47.7 64.3% 12% (2) 42.5 42.1 42.9 89.0 88.2 89.9 94.9 94.9 94.9 89.0% 0.96% 86.5 90.9 90.6 91.2 95.8 95.5 94.2% 2.7% 13C4-PFOA Spiked Concentration (ng/L) Calculated Concentration (ng/L) 10.0 16.9 10.0 10.0 15.0 15.6 159% 5.8% (2) 49.7 49.7 49.7 46.3 47.2 47.4 98.8 98.8 98.8 94.5% 1.3% 89.1 85.6 90.2 89.4% 2.7% %Recovery 169 151 157 93.1 95.0 95.5 90.1 86.7 91.3 (1) NA = Not Applicable; the sample result was below the limit of quantitation and a recovery could not be calculated. (2) The average recovery did not meet method acceptance criteria of 100 20% or a RSD of <20%. PAGE 29 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 10 continued. Laboratory Control Spike Recovery. ETS-8-044.1 Analyzed 1/5/13 Lab ID LCS-121228-1 LCS-121228-2 LCS-121228-3 Average %RSD LCS-121228-4 LCS-121228-5 LCS-121228-6 Average %RSD LCS-121228-7 LCS-121228-8 LCS-121228-9 Average %RSD ETS-8-044.1 Analyzed 1/5/13 Lab ID LCS-121228-1 LCS-121228-2 LCS-121228-3 Average %RSD LCS-121228-4 LCS-121228-5 LCS-121228-6 Average %RSD LCS-121228-7 LCS-121228-8 LCS-121228-9 Average %RSD PFHxA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 5.02 6.38 5.02 5.02 6.75 5.01 50.0 50.0 50.0 99.5 99.5 99.5 120% 15% 55.3 54.3 54.9 110% 0.91% 110 106 99.5 106% 4.9% %Recovery 127 134 99.8 111 109 110 110 107 100 PFHpA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 5.02 4.72 5.02 5.02 50.0 50.0 50.0 99.5 99.5 99.5 4.42 4.78 92.5% 4.1% 46.4 50.6 51.7 98.9% 5.5% 103 108 95.2 103% 6.2% %Recovery 94.0 88.1 95.3 92.7 101 103 104 108 95.6 PFOA (Linear + Branched) Spiked Calculated Concentration Concentration (ng/L) (ng/L) %Recovery 4.81 4.98 104 4.81 4.09 85.0 4.81 4.55 94.5 47.9 47.9 47.9 94.5% 10% 43.9 46.5 47.0 91.6 97.2 98.1 95.3 95.3 95.3 95.6% 03.7% 92.1 99.2 90.7 96.7 104 95.1 98.6% 4.8% 13C4-PFOA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 10.0 <15.0 10.0 10.0 <15.0 <15.0 NA 49.9 49.9 49.9 46.1 47.4 46.4 99.3 99.3 99.3 93.4% 1.4% 86.9 85.0 86.4 86.7% 1.1% %Recovery NA (1)2 NA (1) NA (1) 92.3 94.9 93.0 87.5 85.6 87.0 (1) NA = Not Applicable; the sample result was below the limit of quantitation and a recovery could not be calculated. (2) The average recovery did not meet method acceptance criteria of 100 20% or a RSD of <20%. PAGE 30 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 10 continued. Laboratory Control Spike Recovery. ETS-8-044.1 Analyzed 1/11/13 Lab ID LCS-121227-1 LCS-121227-2 LCS-121227-3 Average %RSD LCS-121227-4 LCS-121227-5 LCS-121227-6 Average %RSD LCS-121227-7 LCS-121227-8 LCS-121227-9 Average %RSD PFBS Spiked Calculated Concentration Concentration (ng/L) (ng/L) 5.00 10.7 5.00 5.00 10.3 10.2 49.8 49.8 49.8 99.0 99.0 99.0 208% 2.8% (2) 47.5 50.0 51.1 99.5% 3.8% 97.0 99.9 98.2 99.4% 1.5% %Recovery 215 205 205 95.5 100 103 98.0 101 99.2 ETS-8-044.1 Analyzed 1/11/13 Lab ID LCS-121228-1 LCS-121228-2 LCS-121228-3 Average %RSD LCS-121228-4 LCS-121228-5 LCS-121228-6 Average %RSD LCS-121228-7 LCS-121228-8 LCS-121228-9 Average %RSD PFBS Spiked Calculated Concentration Concentration (ng/L) (ng/L) 5.02 9.77 5.02 5.02 50.0 50.0 50.0 10.3 9.88 199% 2.7% (2) 48.9 50.4 49.9 99.5 99.5 99.5 99.5% 1.6% 98.6 102 100 101% 1.5% %Recovery 195 205 197 97.8 101 99.8 99.1 102 101 (1) NA = Not Applicable; the sample result was below the limit of quantitation and a recovery could not be calculated. (2) The average recovery did not meet method acceptance criteria of 100 20% or a RSD of <20%. PAGE 31 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 10 continued. Laboratory Control Spike Recovery. ETS-8-044.1 Analyzed 1/28/13 Lab ID LCS-130130-1 LCS-130130-2 LCS-130130-3 Average %RSD LCS-130128-7 LCS-130128-8 LCS-130128-9 Average %RSD LCS-130128-10 LCS-130128-11 LCS-130128-12 Average %RSD PFBS Spiked Calculated Concentration Concentration (ng/L) (ng/L) 5.00 5.12 5.00 5.00 5.44 4.70 49.8 49.8 49.8 503 503 503 102% 7.4% 52.2 53.1 52.9 106% 0.94% 489 508 537 102% 4.8% %Recovery 102 109 93.9 105 107 106 97.3 101 107 ETS-8-044.1 Analyzed 1/28/13 Lab ID LCS-130128-1 LCS-130128-2 LCS-130128-3 Average %RSD LCS-130128-4 LCS-130128-5 LCS-130128-6 Average %RSD LCS-130128-7 LCS-130128-8 LCS-130128-9 Average %RSD LCS-130128-10 LCS-130128-11 LCS-130128-12 Average %RSD PFOS (Linear + Branched) Spiked Calculated Concentration Concentration (ng/L) (ng/L) %Recovery 4.61 3.99 86.6 4.61 3.39 73.5 4.61 4.22 91.5 83.9% 11% 9.21 9.91 108 9.21 9.59 104 9.21 9.13 99.1 104% 4.3% 46.1 45.7 99.2 46.1 48.6 105 46.1 50.7 110 105% 5.2% 466 474 102 466 494 106 466 519 111 106% 4.2% 13C4-PFOS Spiked Calculated Concentration Concentration (ng/L) (ng/L) NA NA NA NA 19.0 19.0 19.0 95.1 95.1 95.1 NA NA NA 19.8 18.8 20.3 103% 4.0% 86.5 87.6 89.9 92.5% 2.0% NA NA NA NA NA NA NA %Recovery NA NA NA 104 98.9 107 90.9 92.1 94.6 NA NA NA (1) NA = Not Applicable; the sample result was below the limit of quantitation and a recovery could not be calculated. (2) The average recovery did not meet method acceptance criteria of 100 20% or a RSD of <20%. PAGE 32 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 10 continued. Laboratory Control Spike Recovery. ETS-8-044.1 Analyzed 1/28/13 Lab ID LCS-130128-1 LCS-130128-2 LCS-130128-3 Average %RSD LCS-130128-4 LCS-130128-5 LCS-130128-6 Average %RSD LCS-130128-7 LCS-130128-8 LCS-130128-9 Average %RSD LCS-130128-10 LCS-130128-11 LCS-130128-12 Average %RSD FBSA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 4.98 4.76 4.98 4.98 4.90 4.69 9.93 9.93 9.93 49.8 49.8 49.8 95.7% 6.4% 9.99 9.07 9.87 103% 2.0% 50.6 54.2 53.0 104% 4.2% 503 508 503 530 503 541 106% 5.2% %Recovery 95.5 89.7 102 101 105.0 104 102 101 109 101 106 112 FOSA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 4.98 5.11 4.98 4.98 9.93 9.93 9.93 49.8 49.8 49.8 4.47 5.10 98.2% 7.5% 10.3 10.5 10.3 104% 0.55% 52.5 50.1 54.4 105% 3.8% 503 498 503 535 503 561 106% 6.2% %Recovery 103 89.7 102 104 105 104 105 101 109 99.0 106 112 ETS-8-044.1 Analyzed 1/28/13 Lab ID LCS-130128-1 LCS-130128-2 LCS-130128-3 Average %RSD LCS-130128-4 LCS-130128-5 LCS-130128-6 Average %RPD LCS-130128-7 LCS-130128-8 LCS-130128-9 Average %RSD LCS-130128-10 LCS-130128-11 LCS-130128-12 Average %RSD MeFOSAA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 4.97 4.97 4.97 <9.98 <9.98 <9.98 NA 9.91 12.0 9.91 <9.98 9.91 13.1 49.7 49.7 49.7 127% 8.8% (2) 45.7 54.3 50.6 101% 8.5% 502 645 502 533 502 610 119% 9.6% %Recovery NA (1) NA (1) NA (1) 121 NA (1) 132 92.0 109 102 128 106 122 EtFOSAA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 4.97 4.97 4.97 <15.0 <15.0 <15.0 NA 9.91 9.91 9.91 49.7 49.7 49.7 <15.0 <15.0 <15.0 NA 45.6 50.7 44.3 94.3% 7.2% 502 527 502 575 502 563 111% 4.6% %Recovery NA (1) NA (1) NA (1) NA (1) NA (1) NA (1) 91.7 102 89.2 105 115 112 (1) NA = Not Applicable; the sample result was below the limit of quantitation and a recovery could not be calculated. (2) The average recovery did not meet method acceptance criteria of 100 20% or a RSD of <20%. PAGE 33 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 10 continued. Laboratory Control Spike Recovery. ETS-8-044.1 Analyzed 1/31/13 Lab ID LCS-130128-1 LCS-130128-2 LCS-130128-3 Average %RSD LCS-130128-4 LCS-130128-5 LCS-130128-6 Average %RSD LCS-130128-7 LCS-130128-8 LCS-130128-9 Average %RSD LCS-130128-10 LCS-130128-11 LCS-130128-12 Average %RSD PFHxA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 4.98 4.01 4.98 4.98 4.97 4.46 9.93 9.93 9.93 49.8 49.8 49.8 89.9% 11% 8.14 9.77 8.76 89.5% 9.2% 46.9 52.1 49.2 99.3% 5.5% 503 547 503 518 503 555 107% 3.5% %Recovery 80.5 99.8 89.5 82.0 98.4 88.2 94.2 105 98.7 109 103 110 PFHpA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 4.98 4.71 4.98 4.98 9.93 9.93 9.93 49.8 49.8 49.8 5.71 5.32 106% 9.8% 10.7 9.20 10.5 102% 8.0% 44.8 49.9 48.4 95.7% 5.4% 503 504 503 575 503 569 109% 7.2% %Recovery 94.5 115 107 108 92.7 105 90.0 100 97.2 100 114 113 ETS-8-044.1 Analyzed 1/31/13 Lab ID LCS-130128-1 LCS-130128-2 LCS-130128-3 Average %RSD LCS-130128-4 LCS-130128-5 LCS-130128-6 Average %RPD LCS-130128-7 LCS-130128-8 LCS-130128-9 Average %RSD LCS-130128-10 LCS-130128-11 LCS-130128-12 Average %RSD PFOA (Linear + Branched) Spiked Calculated Concentration Concentration (ng/L) (ng/L) %Recovery 4.77 4.77 4.77 <4.80 <4.80 <4.80 NA (1) NA (1) NA (1) NA 9.51 9.62 101 9.51 9.64 101 9.51 9.07 95.3 47.7 47.7 47.7 99.1% 3.3% 46.2 49.1 48.2 100% 3.1% 96.9 103 101 481 489 102 481 516 107 481 516 107 105% 2.7% 13C4-PFOA Spiked Calculated Concentration Concentration (ng/L) (ng/L) NA NA NA NA NA NA NA 19.8 19.8 19.8 99.3 99.3 99.3 19.7 21.8 21.1 106% 5.0% 91.1 94.3 94.1 93.8% 2.0% NA NA NA NA NA NA NA %Recovery NA NA NA 99.7 110 107 91.7 95.0 94.8 NA NA NA (1) NA = Not Applicable; the sample result was below the limit of quantitation and a recovery could not be calculated. (2) The average recovery did not meet method acceptance criteria of 100 20% or a RSD of <20%. PAGE 34 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 10 continued. Laboratory Control Spike Recovery. ETS-8-044.1 Analyzed 2/1/13 Lab ID LCS-130201-1 LCS-130201-2 LCS-130201-3 Average %RSD LCS-130201-4 LCS-130201-5 LCS-130201-6 Average %RSD LCS-130201-7 LCS-130201-8 LCS-130201-9 Average %RSD LCS-130201-10 LCS-130201-11 LCS-130201-12 Average %RSD ETS-8-044.1 Analyzed 2/4/13 Lab ID LCS-130201-1 LCS-130201-2 LCS-130201-3 Average %RSD LCS-130201-4 LCS-130201-5 LCS-130201-6 Average %RSD LCS-130201-7 LCS-130201-8 LCS-130201-9 Average %RSD LCS-130201-10 LCS-130201-11 LCS-130201-12 Average %RSD PFOS (Linear + Branched) Spiked Calculated Concentration Concentration (ng/L) (ng/L) %Recovery 4.64 4.38 94.5 4.64 4.64 4.63 4.72 99.8 102 9.30 9.30 9.30 46.4 46.4 46.4 98.8% 3.9% 8.46 8.47 8.91 92.6% 3.0% 44.3 45.7 46.5 90.9 91.1 95.8 95.4 98.5 100 92.2 92.2 92.2 98.0% 2.4% 90.0 91.7 90.4 98.4% 1.0% 97.6 99.5 98.0 13C4-PFOS Spiked Calculated Concentration Concentration (ng/L) (ng/L) NA NA NA NA 19.2 19.2 19.2 NA NA NA NA NA NA 18.6 19.5 20.2 101% 4.2% NA NA NA NA 95.1 93.8 95.1 95.2 95.1 97.0 100% 1.7% %Recovery NA NA NA 96.6 101 105 NA NA NA 98.7 100 102 PFBA Spiked Calculated Concentration Concentration (ng/L) (ng/L) 5.00 4.08 5.00 5.00 5.22 5.07 10.0 10.0 10.0 95.6% 13% 9.99 8.72 9.17 50.0 50.0 50.0 92.9% 6.9% 48.9 47.9 47.1 99.5 99.5 99.5 96.0% 1.8% 100 100 99.7 100% 0.58% %Recovery 81.7 104 101 99.9 87.2 91.7 97.8 95.8 94.3 101 100 100 13C3-PFBA Spiked Calculated Concentration Concentration (ng/L) (ng/L) NA NA NA NA NA NA NA 20.0 20.0 20.0 19.8 20.2 21.0 102% 3.0% NA NA NA NA NA NA NA 99.1 98.2 99.1 99.4 99.1 103 101% 2.6% %Recovery NA NA NA 98.9 101 105 NA NA NA 99.1 100 104 (1) NA = Not Applicable; the sample result was below the limit of quantitation and a recovery could not be calculated. (2) The average recovery did not meet method acceptance criteria of 100 20% or a RSD of <20%. PAGE 35 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 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. For method ETS-8-044.1, the most recent fifty QC samples were used (where applicable). The analytical method uncertainty is calculated by multiplying the standard deviation by a factor of 2, which corresponds to a confidence level of 95%. Table 11. Analytical Method Uncertainty Analyte PFBA PFHxA PFHpA PFOA PFBS PFHS PFOS FBSA FOSA MeFOSAA EtFOSAA 13C3-PFBA 13C4-PFOA 13C4-PFOS Standard Deviation 8.14 10.1 10.6 11.6 10.0 12.4 8.50 8.38 6.79 12.6 8.47 9.07 8.04 7.88 Method Uncertainty 16% 20% 21% 23% 20% 25% 17% 17% 14% 25% 17% 18% 16% 16% 3.8 Field Matrix Spikes (FMS) A field matrix spike was collected at 10% of the sampling locations to verify that the analytical method is applicable to the collected matrix. Field matrix spikes are 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. The reference standards for PFOA and PFOS in the field matrix spiking solution consisted of linear and branched isomers. In addition, field matrix spikes for this project also included the use of stable isotope surrogate recovery standards (SRSs) 13C3-PFBA, 13C4-PFOA, and 13C4-PFOS, which was added at a nominal concentration of 50 ng/L to all sample bottles prior to sample collection. Surrogate matrix spike recoveries within method acceptance criteria of 10030% confirm that "unknown" components in the sample matrix do not significantly interfere with the preparation and analysis of the analytes of interest. Surrogate recovery standard results are presented in Table 2 of the report. PAGE 36 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 12. Field Matrix Spike Level. Description FMS PFBA PFHxA PFHpA 100 100 100 PFOA 95.8 Final Concentration (ng/L) (1) PFBS PFHS PFOS FBSA 100 100 92.7 100 FOSA MeFOSAA EtFOSAA 100 99.8 99.8 (1) Location DAL-SW-T707 was overfilled by 10% (220 mL). The FMS true values were adjusted accordingly. FMS Recovery = -(-S-a--m- ple Concentration ofsFMS - Average Spike CCoonncceennttrraattiioonn :Field Sample & Field Samp-l-e-D---u--p.) *100% 4 Data Summary and Discussion The tables below summarize the sample results and field matrix spike (FMS) recoveries for the sampling locations where a FMS sample was collected, along with the Trip Blank FMS results. Results and average values are rounded to three significant figures according to EPA rounding rules. Because of rounding, values may vary slightly from those listed in the raw data. Field matrix spike and surrogate recoveries meeting the method acceptance criteria of 30%, demonstrate that the method(s) were appropriate for the given matrix and their respective quantitative ranges. All FMS samples met method acceptance criteria with the following exception: DAL SW R05L1; the FMS level was not appropriate for PFOA, PFOS, and FBSA however, the surrogate recovery standards met method acceptance criteria. DAL SW R15L1; the FMS recovery for EtFOSAA was 69.5%. When rounded to two significant figures (70%), the recovery meets method acceptance criteria of 100% 30%. The following sampling locations had a sample/sample duplciate relative percent difference (RPD) outside method acceptance criteria of <20%: DAL SW R02L3; the RPD for PFHxA was 29% and 22% for PFHpA. DAL SW T202; the RPD for PFHpA was 27%. DAL SW T606; the RPD for PFOA was 25%. PAGE 37 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 13. DAL SW R02L3 3M U M S ID D e sc rip tio n ISO12-01 -01 -03-012 DAL-SW-R02L3-0-121116 ISO12-01 -01 -03-013 DAL-SW-R02L3-DUP-121116 ISO12-01 -01 -03-014 DAL-SW-R02L3-FMS-121116 A verage Concentration (ng/L) % RPD PFBA C o n c e n tra tio n (ng/L) % Recovery 6.13 NA 6.10 NA 100 93.9 6.12 ng/L 049% PFHxA PFHpA C o n cen tra tio n (ng/L) % Recovery 4.83 NA 3.61 NA 111 107 4.22 ng/L 29% (1) C o n c e n tra tio n (ng/L) % Recovery 4.70 NA 3.78 103 NA 98.8 4.2 4 ng/L 22% (1) PFOA C o n cen tra tio n (ng/L) % Recovery 9.28 NA 9.12 101 NA 95.8 9.20 ng/L 1.7% 3M U M S ID D e sc rip tio n ISO12-01 -01 -03-012 DAL-SW-R02L3-0-121116 ISO12-01 -01 -03-013 DAL-SW-R02L3-DUP-121116 ISO12-01 -01 -03-014 DAL-SW-R02L3-FMS-121116 A verage Concentration (ng/L) % RPD PFBS C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 102 102 <5.00 ng/L PFHS PFOS C o n cen tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 99.7 99.7 <5.00 ng/L C o n c e n tra tio n (ng/L) % Recovery 8.94 NA 8.46 NA 94.7 92.8 8.70 ng/L 5.5% FBSA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 95.5 95.5 <2.00 ng/L 3M U M S ID D e sc rip tio n ISO12-01 -01 -03-012 ISO12-01 -01 -03-013 ISO12-01 -01 -03-014 DAL-SW-R02L3-0-121116 DAL-SW-R02L3-DUP-121116 DAL-SW-R02L3-FMS-121116 Average Concentration (ng/L) %RPD/% RSD FOSA C o n c e n tra tio n (ng/L) <2.00 <2.00 101 % Recovery NA NA 101 <2.00 ng/L MeFOSAA C o n cen tra tio n (ng/L) <2.00 <2.00 95.1 % Recovery NA NA 95.3 <2.00 ng/L EtFOSAA C o n c e n tra tio n (ng/L) <5.00 <5.00 94.2 % Recovery NA NA 94.4 <5.00 ng/L NA = Not Applicable (1) The sample / sample duplicate RPD did not meet method acceptance criteria of <20%. PAGE 38 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 14. DAL SW R05L1 3M U M S ID D e sc rip tio n ISO12-01-01-03-052 DAL-SW-R05L1 -0-121119 ISO12-01-01-03-053 DAL-SW-R05L1 -DUP-121119 ISO12-01-01-03-054 DAL-SW-R05L1 -FMS-121119 A verage Concentration (ng/L) % RPD PFBA C o n c e n tra tio n (ng/L) % Recovery 58.9 NA 58.3 NA 163 104 58.6 ng/L 10% PFHxA PFHpA C o n cen tra tio n (ng/L) % Recovery 72.5 NA 70.5 NA 176 105 71.5 ng/L 2.8% C o n c e n tra tio n (ng/L) % Recovery 56.8 NA 59.0 NA 178 120 57.9 ng/L 3.8% PFOA C o n cen tra tio n (ng/L) % Recovery 246 NA 242 NA 353 NC 244 ng/L 1.6% 3M U M S ID D e sc rip tio n ISO12-01-01-03-052 ISO12-01-01-03-053 ISO12-01-01-03-054 DAL-SW-R05L1 -0-121119 DAL-SW-R05L1 -DUP-121119 DAL-SW-R05L1 -FMS-121119 A verage Concentration (ng/L) % RPD PFBS C o n c e n tra tio n (ng/L) % Recovery 124 NA 116 NA 233 113 120 ng/L 6.7% PFHS PFOS C o n cen tra tio n (ng/L) C o n c e n tra tio n % Recovery (ng/L) % Recovery 39.8 NA 42.3 NA 137 96.0 41.1 ng/L 6.1% 385 NA 405 NA 543 NC 395 ng/L 5.1% FBSA C o n cen tra tio n (ng/L) % Recovery 1130 NA 1050 NA 1260 NC 1090 ng/L 7.3% 3M U M S ID D e sc rip tio n ISO12-01-01-03-052 DAL-SW-R05L1 -0-121119 ISO12-01-01-03-053 DAL-SW-R05L1 -DUP-121119 ISO12-01-01-03-054 DAL-SW-R05L1 -FMS-121119 Average Concentration (ng/L) %RPD/% RSD FOSA C o n c e n tra tio n (ng/L) % Recovery 21.1 NA 18.0 NA 116 96.5 19.6 ng/L 16% MeFOSAA C o n cen tra tio n (ng/L) % Recovery 10.0 NA 8.20 NA 99.0 90.1 9.10 ng/L 20% EtFOSAA C o n c e n tra tio n (ng/L) % Recovery 18.0 NA 17.8 NA 113 95.3 17.9 ng/L 1.1% NA = Not Applicable NC = Not Calculated; the endogenous sample concentration was greater than 2x the spike level. PAGE 39 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 15. DAL SW R10L3 3M U M S ID D e sc rip tio n ISO12-01-01-03-040 DAL-SW-R10L3-0-121119 ISO12-01 -01 -03-041 DAL-SW- R10L3-DUP-121119 ISO12-01-01-03-042 DAL-SW- R10L3-FMS-121119 A verage Concentration (ng/L) % RPD PFBA C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 95.9 95.9 <5.00 ng/L PFHxA PFHpA C o n cen tra tio n (ng/L) % Recovery 2.73 NA <2.00 NA 102 99.3 2.73 ng/L C o n c e n tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 94.5 94.5 <2.00 ng/L PFOA C o n cen tra tio n (ng/L) % Recovery 3.52 NA 3.50 NA 90.1 90.4 3.52 ng/L 0.57% 3M U M S ID D e sc rip tio n IS012-01-01-03-040 ISO12-01 -01 -03-041 ISO12-01-01-03-042 DAL-SW-R10L3-0-121119 DAL-SW- R10L3-DUP-121119 DAL-SW- R10L3-FMS-121119 A verage Concentration (ng/L) % RPD PFBS C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 97.6 97.6 <5.00 ng/L PFHS PFOS C o n cen tra tio n (ng/L) C o n c e n tra tio n % Recovery (ng/L) % R ecoveiy <5.00 NA <5.00 NA 91.2 91.2 <5.00 ng/L 6.49 NA 6.63 NA 92.5 92.7 6.56 ng/L 2.1% FBSA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 94.8 94.8 <2.00 ng/L 3M U M S ID D e sc rip tio n IS012-01-01-03-040 DAL-SW-R10L3-0-121119 ISO12-01 -01 -03-041 DAL-SW- R10L3-DUP-121119 ISO12-01-01-03-042 DAL-SW- R10L3-FMS-121119 Average Concentration (ng/L) %RPD/% RSD FOSA C o n c e n tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 99.6 99.6 <2.00 ng/L MeFOSAA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 91.9 92.1 <2.00 ng/L EtFOSAA C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 93.6 93.8 <5.00 ng/L NA = Not Applicable NC = Not Calculated; the endogenous sample concentration was greater than 2x the spike level. PAGE 40 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 16. DAL SW R15L1 3M U M S ID D e sc rip tio n ISO12-01-01-03-024 DAL-SW-R15L1-0-121117 ISO12-01-01-03-025 DAL-SW- R15L1-DUP-121117 ISO12-01-01-03-026 DAL-SW- R15L1-FMS-121117 A verage Concentration (ng/L) % RPD PFBA C o n c e n tra tio n (ng/L) % Recovery 7.92 NA 6.62 NA 98.9 91.6 7.27 ng/L 18% PFHxA PFHpA C o n cen tra tio n (ng/L) % Recovery 4.24 NA 4.71 NA 108 104 4 4 8 ng/L 11% C o n c e n tra tio n (ng/L) % Recovery 2.34 NA <2.00 NA 106 104 2.34 ng/L PFOA C o n cen tra tio n (ng/L) % Recovery 11.5 NA 10.9 NA 100 92.6 11.2 ng/L 5.4% 3M U M S ID D e sc rip tio n ISO12-01-01-03-024 ISO12-01-01-03-025 ISO12-01-01-03-026 DAL-SW-R15L1-0-121117 DAL-SW- R15L1-DUP-121117 DAL-SW- R15L1-FMS-121117 A verage Concentration (ng/L) % RPD PFBS C o n c e n tra tio n (ng/L) % Recovery 14.8 NA 13.7 NA 109 94.8 14.3 ng/L 7.7% PFHS PFOS C o n cen tra tio n (ng/L) C o n c e n tra tio n % Recovery (ng/L) % R ecoveiy <5.00 NA <5.00 NA 95.5 95.5 <5.00 ng/L 19.9 NA 18.9 NA 113 101 1 9 4 ng/L 5.2% FBSA C o n cen tra tio n (ng/L) % Recovery 34.8 NA 31.8 NA 118 84.7 33.3 ng/L 9.0% 3M U M S ID D e sc rip tio n ISO12-01-01-03-024 DAL-SW-R15L1-0-121117 ISO12-01-01-03-025 DAL-SW- R15L1-DUP-121117 ISO12-01-01-03-026 DAL-SW- R15L1-FMS-121117 Average Concentration (ng/L) %RPD/% RSD FOSA C o n c e n tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 101 101 <2.00 ng/L MeFOSAA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 85.9 86.1 <2.00 ng/L EtFOSAA C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 69.4 69.5 (1) <5.00 ng/L NA = Not Applicable (1) The field matrix spike recovery did not meet method acceptance criteria of 100 30% PAGE 41 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 17. DAL SW T101 3M U M S ID D e sc rip tio n ISO12-01-01-03-062 DAL-SW-T101 -0-121203 ISO12-01-01-03-063 DAL-SW-T101-DB-121203 ISO12-01-01-03-064 DAL-SW-T 101 -FMS-121203 A verage Concentration (ng/L) % RPD 3M U M S ID D e sc rip tio n ISO12-01-01-03-062 DAL-SW-T 101 -0-121203 ISO12-01-01-03-063 DAL-SW-T 101-DB-121203 ISO12-01-01-03-064 DAL-SW-T 101 -FMS-121203 A verage Concentration (ng/L) % RPD PFBA C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 94.4 NA 94.4 <5.00 ng/L PFHxA PFHpA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 107 NA 107 <2.00 ng/L C o n c e n tra tio n (ng/L) % Recovery <2.00 NA <2.00 97.2 NA 97.2 <2.00 ng/L PFOA C o n cen tra tio n (ng/L) % Recovery <1.92 NA <1.92 90.0 NA 93.9 <1.92 ng/L PFBS C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 96.1 96.1 <5.00 ng/L PFHS PFOS C o n cen tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 93.3 93.3 <5.00 ng/L C o n c e n tra tio n (ng/L) % Recovery 6.13 NA 6.36 NA 91.1 91.5 6.25 ng/L 3.7% FBSA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 87.7 87.7 <2.00 ng/L 3M U M S ID D e sc rip tio n ISO12-01-01-03-062 ISO12-01-01-03-063 ISO12-01-01-03-064 DAL-SW-T 101 -0-121203 DAL-SW-T 101-DB-121203 DAL-SW-T 101 -FMS-121203 Average Concentration (ng/L) %RPD/% RSD NA = Not Applicable FOSA C o n c e n tra tio n (ng/L) <2.00 <2.00 98.3 % Recovery NA NA 98.3 <2.00 ng/L MeFOSAA C o n cen tra tio n (ng/L) <2.00 <2.00 99.9 % Recovery NA NA 100 <2.00 ng/L EtFOSAA C o n c e n tra tio n (ng/L) <5.00 <5.00 94.7 % Recovery NA NA 94.9 <5.00 ng/L PAGE 42 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 18. DAL SW T202 3M U M S ID D e sc rip tio n ISO12-01-01-03-075 DAL-SW-T202-0-121203 ISO12-01 -01 -03-076 DAL-SW-T202-DB-121203 ISO12-01-01-03-077 DAL-SW-T202-FMS-121203 A verage Concentration (ng/L) % RPD 3M U M S ID D e sc rip tio n ISO12-01-01-03-075 ISO12-01 -01 -03-076 ISO12-01-01-03-077 DAL-SW-T202-0-121203 DAL-SW-T202-DB-121203 DAL-SW-T202-FMS-121203 A verage Concentration (ng/L) % RPD PFBA C o n c e n tra tio n (ng/L) % Recovery 6.72 NA 5.50 NA 97.3 90.6 6.72 ng/L 18% PFHxA PFHpA C o n cen tra tio n (ng/L) % Recovery 5.16 NA 4.58 NA 103 98.1 4.8 7 ng/L 54% C o n c e n tra tio n (ng/L) % Recovery 4.80 NA 3.64 NA 103 98.8 4.22 ng/L 27% (1) PFOA C o n cen tra tio n (ng/L) % Recovery 12.6 NA 10.7 NA 106 98.5 11.7 ng/L 16% PFBS C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 99.4 99.4 <5.00 ng/L PFHS PFOS C o n cen tra tio n (ng/L) C o n c e n tra tio n % Recovery (ng/L) % Recovery <5.00 NA <5.00 NA 94.6 94.6 <5.00 ng/L 9.93 NA 9.43 NA 88.7 85.2 9.68 ng/L 5.2% FBSA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 91.6 91.6 <2.00 ng/L 3M U M S ID D e sc rip tio n ISO12-01-01-03-075 DAL-SW-T202-0-121203 ISO12-01 -01 -03-076 DAL-SW-T202-DB-121203 ISO12-01-01-03-077 DAL-SW-T202-FMS-121203 Average Concentration (ng/L) %RPD/% RSD FOSA C o n c e n tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 94.8 94.8 <2.00 ng/L MeFOSAA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 102 102 <2.00 ng/L EtFOSAA C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 96.2 96.4 <5.00 ng/L NA = Not Applicable (1) The sample / sample duplicate RPD did not meet method acceptance criteria of <20%. PAGE 43 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 19. DAL SW T303 3M U M S ID D e sc rip tio n ISO12-01-01-03-088 DAL-SW-T303-0-121203 ISO12-01-01-03-089 DAL-SW-T303-DB-121203 IS012-01-01-03-090 DAL-SW-T303-FMS-121203 A verage Concentration (ng/L) % RPD 3M U M S ID D e sc rip tio n ISO12-01-01-03-088 ISO12-01-01-03-089 IS012-01-01-03-090 DAL-SW-T303-0-121203 DAL-SW-T303-DB-121203 DAL-SW-T303-FMS-121203 A verage Concentration (ng/L) % RPD PFBA C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 97.1 97.1 <5.00 ng/L PFHxA PFHpA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 106 106 <2.00 ng/L C o n c e n tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 97.9 97.9 <2.00 ng/L PFOA C o n cen tra tio n (ng/L) % Recovery 2.78 NA 2.29 NA 91.3 92.7 2.54 ng/L 19% PFBS C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 98.0 98.0 <5.00 ng/L PFHS PFOS C o n cen tra tio n (ng/L) C o n c e n tra tio n % Recovery (ng/L) % R ecoveiy <5.00 NA <5.00 NA 94.9 94.9 <5.00 ng/L 6.94 NA 7.51 NA 92.9 92.4 7.23 ng/L 7.9% FBSA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 93.2 93.2 <2.00 ng/L 3M U M S ID D e sc rip tio n ISO12-01-01-03-088 DAL-SW-T303-0-121203 ISO12-01-01-03-089 DAL-SW-T303-DB-121203 IS012-01-01-03-090 DAL-SW-T303-FMS-121203 Average Concentration (ng/L) %RPD/% RSD NA = Not Applicable FOSA C o n c e n tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 100 100 <2.00 ng/L MeFOSAA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 102 102 <2.00 ng/L EtFOSAA C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 102 102 <5.00 ng/L PAGE 44 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 20. DAL SW T404 3M U M S ID D e sc rip tio n ISO12-01 -01 -03-101 DAL-SW-T404-0-121203 ISO12-01 -01 -03-102 DAL-SW-T404-DB-121203 ISO12-01 -01 -03-103 DAL-SW-T404-FMS-121203 A verage Concentration (ng/L) % RPD 3M U M S ID D e sc rip tio n ISO12-01 -01 -03-101 ISO12-01 -01 -03-102 ISO12-01 -01 -03-103 DAL-SW-T404-0-121203 DAL-SW-T404-DB-121203 DAL-SW-T404-FMS-121203 A verage Concentration (ng/L) % RPD PFBA C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 94.7 94.7 <5.00 ng/L PFHxA PFHpA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 106 106 <2.00 ng/L C o n c e n tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 102 102 <2.00 ng/L PFOA C o n cen tra tio n (ng/L) % Recovery 2.25 NA <1.92 NA 89.9 91.5 2.25 ng/L PFBS C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 95.0 95.0 <5.00 ng/L PFHS PFOS C o n cen tra tio n (ng/L) C o n c e n tra tio n % Recovery (ng/L) % Recovery <5.00 NA <5.00 NA 94.7 94.7 <5.00 ng/L 7.29 NA 8.46 NA 92.9 91.7 7.88 ng/L 15% FBSA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 91.0 91.0 <2.00 ng/L 3M U M S ID D e sc rip tio n ISO12-01 -01 -03-101 DAL-SW-T404-0-121203 ISO12-01 -01 -03-102 DAL-SW-T404-DB-121203 ISO12-01 -01 -03-103 DAL-SW-T404-FMS-121203 Average Concentration (ng/L) %RPD/% RSD NA = Not Applicable FOSA C o n c e n tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 102 102 <2.00 ng/L MeFOSAA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 97.4 97.6 <2.00 ng/L EtFOSAA C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 92.1 92.3 <5.00 ng/L PAGE 45 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 21. DAL SW T505 3M U M S ID D e sc rip tio n ISO12-01-01-03-114 DAL-SW-T505-0-121204 ISO12-01-01-03-115 DAL-SW-T505-DB-121204 ISO12-01-01-03-116 DAL-SW-T505-FMS-121204 A verage Concentration (ng/L) % RPD 3M U M S ID D e sc rip tio n ISO12-01-01-03-114 ISO12-01-01-03-115 ISO12-01-01-03-116 DAL-SW-T505-0-121204 DAL-SW-T505-DB-121204 DAL-SW-T505-FMS-121204 A verage Concentration (ng/L) % RPD PFBA C o n c e n tra tio n (ng/L) % Recovery <5.00 NA 5.48 NA 96.7 91.2 5 4 8 ng/L PFHxA PFHpA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 109 109 <2.00 ng/L C o n c e n tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 103 103 <2.00 ng/L PFOA C o n cen tra tio n (ng/L) % Recovery 2.52 NA 3.01 NA 92.8 94.0 2.77 ng/L 18% PFBS C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 98.5 98.5 <5.00 ng/L PFHS PFOS C o n cen tra tio n (ng/L) C o n c e n tra tio n % Recovery (ng/L) % Recovery <5.00 NA <5.00 NA 96.3 96.3 <5.00 ng/L 7.20 NA 6.78 NA 93.7 93.5 6.99 ng/L 6.0% FBSA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 88.4 88.4 <2.00 ng/L 3M U M S ID D e sc rip tio n ISO12-01-01-03-114 DAL-SW-T505-0-121204 ISO12-01-01-03-115 DAL-SW-T505-DB-121204 ISO12-01-01-03-116 DAL-SW-T505-FMS-121204 Average Concentration (ng/L) %RPD/% RSD NA = Not Applicable FOSA C o n c e n tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 97.9 97.9 <2.00 ng/L MeFOSAA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 92.6 92.8 <2.00 ng/L EtFOSAA C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 99.6 99.8 <5.00 ng/L PAGE 46 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 22. DAL SW T606 3M U M S ID D e sc rip tio n ISO12-01 -01 -03-127 DAL-SW-T606-0-121204 ISO12-01 -01 -03-128 DAL-SW-T606-DB-121204 ISO12-01 -01 -03-129 DAL-SW-T606-FMS-121204 A verage Concentration (ng/L) % RPD 3M U M S ID D e sc rip tio n ISO12-01 -01 -03-127 ISO12-01 -01 -03-128 ISO12-01 -01 -03-129 DAL-SW-T606-0-121204 DAL-SW-T606-DB-121204 DAL-SW-T606-FMS-121204 A verage Concentration (ng/L) % RPD PFBA C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 96.6 96.6 <5.00 ng/L PFHxA PFHpA C o n cen tra tio n (ng/L) % Recovery 2.31 NA 2.41 NA 110 108 2.36 ng/L 4.2% C o n c e n tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 102 102 <2.00 ng/L PFOA C o n cen tra tio n (ng/L) % Recovery 4.38 NA 3.41 NA 92.2 92.2 3.90 ng/L 25% (1) PFBS C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 97.9 97.9 <5.00 ng/L PFHS PFOS C o n cen tra tio n (ng/L) C o n c e n tra tio n % Recovery (ng/L) % R ecoveiy <5.00 NA <5.00 NA 97.1 97.1 <5.00 ng/L 9.72 NA 11.1 NA 96.5 92.9 1 0 4 ng/L 13% FBSA C o n cen tra tio n (ng/L) % Recovery 2.22 NA 2.18 NA 91.0 88.8 2.20 ng/L 1.8% 3M U M S ID D e sc rip tio n ISO12-01 -01 -03-127 DAL-SW-T606-0-121204 ISO12-01 -01 -03-128 DAL-SW-T606-DB-121204 ISO12-01 -01 -03-129 DAL-SW-T606-FMS-121204 Average Concentration (ng/L) %RPD/% RSD FOSA C o n c e n tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 98.6 98.6 <2.00 ng/L MeFOSAA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 92.4 92.6 <2.00 ng/L EtFOSAA C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 96.5 96.7 <5.00 ng/L NA = Not Applicable (1) The sample / sample duplicate RPD did not meet method acceptance criteria of <20%. PAGE 47 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 23. DAL SW T707 3M LIM S ID D e sc rip tio n ISO12-01 -01 -03-140 DAL-SW-T707-0-121204 ISO12-01 -01 -03-141 DAL-SW-T707-DB-121204 ISO12-01 -01 -03-142 DAL-SW-T707-FMS-121204 A verage Concentration (ng/L) % RPD 3M LIM S ID D e sc rip tio n ISO12-01 -01 -03-140 ISO12-01 -01 -03-141 ISO12-01 -01 -03-142 DAL-SW-T707-0-121204 DAL-SW-T707-DB-121204 DAL-SW-T707-FMS-121204 A verage Concentration (ng/L) % RPD PFBA C o n c e n tra tio n (ng/L) % Recovery 8.42 NA 7.66 NA 89.5 81.5 8.04 ng/L 9.5% PFHxA PFHpA C o n cen tra tio n (ng/L) % Recovery 4.05 NA 4.53 NA 99.0 104 4.29 ng/L 11% C o n c e n tra tio n (ng/L) % Recovery 3.24 NA 3.77 NA 88.3 93.3 3.51 ng/L 15% PFOA C o n cen tra tio n (ng/L) % Recovery 12.5 NA 11.9 NA 97.3 97.7 12.2 ng/L 4.9% PFBS C o n c e n tra tio n (ng/L) % Recovery 19.0 NA 21.0 NA 105 93.5 20.0 ng/L 10% PFHS PFOS C o n cen tra tio n (ng/L) C o n c e n tra tio n % Recovery (ng/L) % R ecoveiy <5.00 NA <5.00 NA 90.0 99.0 <5.00 ng/L 20.2 NA 19.3 NA 107 104 19.8 ng/L 4.6% FBSA C o n cen tra tio n (ng/L) % Recovery 27.6 NA 26.4 NA 109 90.2 27.0 ng/L 44% 3M LIM S ID D e sc rip tio n ISO12-01 -01 -03-140 DAL-SW-T707-0-121204 ISO12-01 -01 -03-141 DAL-SW-T707-DB-121204 ISO12-01 -01 -03-142 DAL-SW-T707-FMS-121204 Average Concentration (ng/L) %RPD/% RSD NA = Not Applicable FOSA C o n c e n tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 97.2 107 <2.00 ng/L MeFOSAA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 81.9 90.3 <2.00 ng/L EtFOSAA C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 81.0 89.3 <5.00 ng/L PAGE 48 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 24. DAL SW T808 3M U M S ID D e sc rip tio n ISO12-01 -01 -03-153 DAL-SW-T808-0-121205 ISO12-01 -01 -03-154 DAL-SW-T808-DB-121205 ISO12-01 -01 -03-155 DAL-SW-T808-FMS-121205 A verage Concentration (ng/L) % RPD 3M U M S ID D e sc rip tio n ISO12-01 -01 -03-153 ISO12-01 -01 -03-154 ISO12-01 -01 -03-155 DAL-SW-T808-0-121205 DAL-SW-T808-DB-121205 DAL-SW-T808-FMS-121205 A verage Concentration (ng/L) % RPD PFBA C o n c e n tra tio n (ng/L) % Recovery 6.28 NA 6.89 NA 96.0 89.4 6.59 ng/L 9.3% PFHxA PFHpA C o n cen tra tio n (ng/L) % Recovery 4.51 NA 3.85 NA 112 108 4.18 ng/L 16% C o n c e n tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 106 106 <2.00 ng/L PFOA C o n cen tra tio n (ng/L) % Recovery 7.49 NA 6.79 NA 96.9 93.7 7.14 ng/L 9.8% PFBS C o n c e n tra tio n (ng/L) % Recovery 11.2 NA 10.9 NA 109 98.0 11.1 ng/L 2.7% PFHS PFOS C o n cen tra tio n (ng/L) C o n c e n tra tio n % Recovery (ng/L) % Recovery <5.00 NA <5.00 NA 94.4 94.4 <5.00 ng/L 13.3 NA 14.3 NA 101 94.1 13.8 ng/L 7.2% FBSA C o n cen tra tio n (ng/L) % Recovery 25.7 NA 25.7 NA 107 81.3 2 5 .7 ng/L 0.0% 3M U M S ID D e sc rip tio n ISO12-01 -01 -03-153 DAL-SW-T808-0-121205 ISO12-01 -01 -03-154 DAL-SW-T808-DB-121205 ISO12-01 -01 -03-155 DAL-SW-T808-FMS-121205 Average Concentration (ng/L) %RPD/% RSD NA = Not Applicable FOSA C o n c e n tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 102 102 <2.00 ng/L MeFOSAA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 89.9 90.1 <2.00 ng/L EtFOSAA C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 89.4 89.6 <5.00 ng/L PAGE 49 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 25. DAL SW T909 3M U M S ID D e sc rip tio n ISO12-01 -01 -03-166 DAL-SW-T909-0-121205 ISO12-01 -01 -03-167 DAL-SW-T909-DB-121205 ISO12-01 -01 -03-168 DAL-SW-T909-FMS-121205 A verage Concentration (ng/L) % RPD 3M U M S ID D e sc rip tio n ISO12-01 -01 -03-166 ISO12-01 -01 -03-167 ISO12-01 -01 -03-168 DAL-SW-T909-0-121205 DAL-SW-T909-DB-121205 DAL-SW-T909-FMS-121205 A verage Concentration (ng/L) % RPD PFBA C o n c e n tra tio n (ng/L) % Recovery 8.66 NA 8.97 NA 99.5 90.7 8.82 ng/L 3.5% PFHxA PFHpA C o n cen tra tio n (ng/L) % Recovery 7.12 NA 6.28 NA 110 103 6.70 ng/L 13% C o n c e n tra tio n (ng/L) % Recovery 3.37 NA 3.75 NA 109 105 3.56 ng/L 11% PFOA C o n cen tra tio n (ng/L) % Recovery 11.6 NA 10.9 NA 108 101 11.3 ng/L 6.2% PFBS C o n c e n tra tio n (ng/L) % Recovery 12.8 NA 14.0 NA 112 98.6 1 3 4 ng/L 9.0% PFHS PFOS C o n cen tra tio n (ng/L) C o n c e n tra tio n % Recovery (ng/L) % Recovery <5.00 NA <5.00 NA 97.1 97.1 <5.00 ng/L 19.2 NA 19.4 NA 117 105 19.3 ng/L 1.0% FBSA C o n cen tra tio n (ng/L) % Recovery 46.3 NA 45.6 NA 125 79.1 46.0 ng/L 1.5% 3M U M S ID D e sc rip tio n ISO12-01 -01 -03-166 DAL-SW-T909-0-121205 ISO12-01 -01 -03-167 DAL-SW-T909-DB-121205 ISO12-01 -01 -03-168 DAL-SW-T909-FMS-121205 Average Concentration (ng/L) %RPD/% RSD NA = Not Applicable FOSA C o n c e n tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 94.4 94.4 <2.00 ng/L MeFOSAA C o n cen tra tio n (ng/L) % Recovery <2.00 NA <2.00 NA 90.8 91.0 <2.00 ng/L EtFOSAA C o n c e n tra tio n (ng/L) % Recovery <5.00 NA <5.00 NA 98.8 99.0 <5.00 ng/L PAGE 50 OF 52 3M Environmental Laboratory Report No. ISO12-01-01-03 Table 26. DAL SW TRIP BLANK PFBA 3M LIM S ID ISO12-01 -01 -03-061 ISO12-01-01-03-171 D e sc rip tio n DAL-SW-TRIP02-0-121116 (1) DAL-SW-TRIP-01 -FMS-121203 C o n c e n tra tio n (ng/L) 92.5 90.1 % Recovery 92.5 90.1 PFHxA PFHpA C o n cen tra tio n (ng/L) 104 112 % Recovery 104 112 C o n c e n tra tio n (ng/L) 95.0 94.3 % Recovery 95.0 94.3 PFOA C o n cen tra tio n (ng/L) 95.4 94.2 % Recovery 99.6 98.3 PFBS 3M LIM S ID D e sc rip tio n C o n c e n tra tio n (ng/L) % Recovery ISO12-01 -01 -03-061 DAL-SW-TRIP02-0-121116 (1) ISO12-01-01-03-171 DAL-SW-TRIP-01 -FMS-121203 99.3 97.9 99.3 97.9 PFHS PFOS C o n cen tra tio n (ng/L) C o n c e n tra tio n % Recovery (ng/L) % Recovery 97.4 93.3 97.4 93.3 89.7 84.1 96.8 90.7 FBSA C o n cen tra tio n (ng/L) % Recovery 97.6 102 97.6 102 FOSA 3M LIM S ID ISO12-01 -01 -03-061 ISO12-01-01-03-171 D e sc rip tio n DAL-SW-TRIP02-0-121116 (1) DAL-SW-TRIP-01 -FMS-121203 C o n c e n tra tio n (ng/L) 97.6 102 % Recovery 97.6 102 MeFOSAA C o n cen tra tio n (ng/L) 92.3 99.5 % Recovery 92.5 99.7 EtFOSAA C o n c e n tra tio n (ng/L) 97.2 99.1 % Recovery 97.4 99.3 (1) Sample ISO12-01-01-03-061 identified as DAL-SW-TRIP02-0-121116 is a trip blank FMS sample. The naming of the sample was not consistent with the set of Trip Blank samples collected on December 3, 2012. PAGE 51 OF 52 3M Environmental Laboratory Report No. IS012-01-01-03 5 Conclusion Laboratory control spikes were used to determine the analytical method accuracy and precision for PFOS. The accuracy and precision were then used to estimate the method uncertainty for the results. Field matrix spike recoveries demonstrated that the analytical method was appropriate for the given sample matrix. Analysis was completed using 3M Environmental Laboratory method ETS-8-044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis". Analytical results are reported in Tables 1 and 13-26 of this report. 6 Data/Sample Retention All remaining samples and associated project data (hardcopy and electronic) will be archived according to 3M Environmental Laboratory standard operating procedures. William K. Reagen, Ph.D., 3M Environmental Laboratory Manager Date The 3M Environmental Laboratory's Quality Assurance Unit has audited the data and report for this project. Quality Assurance Representative 2- Date PAGE 52 OF 52