3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 1 OF 52

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

Testing Cert #2052.01

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. 
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 2 OF 52

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. 

Testing Cert #2052.01

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. 
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 3 OF 52

Table 1. Sample Results Summary (1)

Concentration (ng/L; parts per trillion)

3M LIMS ID Sample Description PFBA PFHxA PFHpA PFOA PFBS PFHS PFOS FBSA FOSA MeFOSAA EtFOSAA

Fish Sampling Reaches

ISO12-01-01-03-007 DAL-SW-R01L1-0-121116 6.16 2.56 <2.00 2.16 <5.00 <5.00 6.91 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-008 DAL-SW-R01L2-0-121116 6.50 2.83 <2.00 3.04 <5.00 <5.00 7.62 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-009 DAL-SW-R01L3-0-121116 <5.00 2.72 <2.00 2.31 <5.00 <5.00 6.69 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-010 DAL-SW-R02L1-0-121116 7.36 4.52 3.47 10.7 <5.00 <5.00 9.32 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-011 DAL-SW-R02L2-0-121116 6.06 5.56 3.64 10.4 <5.00 7.03 9.06 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-012 DAL-SW-R02L3-0-121116 6.13 4.83 4.70 9.28 <5.00 <5.00 8.94 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-015 DAL-SW-R03L1-0-121116 5.95 <2.00 <2.00 3.43 <5.00 <5.00 7.03 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-016 DAL-SW-R03L2-0-121116 5.77 <2.00 <2.00 3.70 <5.00 <5.00 7.34 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-017 DAL-SW-R03L3-0-121116 5.00 2.85 <2.00 3.34 <5.00 <5.00 6.39 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-018 DAL-SW-R04L1-0-121116 7.51 9.85 3.82 13.6 <5.00 <5.00 14.4 2.14 <2.00 <2.00 <5.00

ISO12-01-01-03-019 DAL-SW-R04L2-0-121116 7.27 13.8 4.57 15.0 <5.00 <5.00 18.0 2.07 <2.00 <2.00 <5.00

ISO12-01-01-03-020 DAL-SW-R04L3-0-121116 11.7 12.4 3.91 31.7 10.4 11.0 70.5 4.86 <2.00 <2.00 <5.00

ISO12-01-01-03-052 DAL-SW-R05L1-0-121119 58.9 72.5 56.8 246 124 39.8 385 1130 21.1 10.0 18.0

ISO12-01-01-03-055 DAL-SW-R05L2-0-121119 6.51 4.43 <2.00 9.02 <5.00 <5.00 17.7 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-056 DAL-SW-R05L3-0-121119 <5.00 3.47 <2.00 5.82 <5.00 <5.00 9.84 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-057 DAL-SW-R06L1-0-121120 <5.00 2.07 <2.00 2.97 <5.00 <5.00 6.84 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-058 DAL-SW-R06L2-0-121120 <5.00 <2.00 <2.00 <4.80 <5.00 <5.00 6.72 <2.00 <2.00 <9.98 <15.0

ISO12-01-01-03-059 DAL-SW-R06L3-0-121120 <5.00 3.30 <2.00 2.76 <5.00 <5.00 6.77 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-049 DAL-SW-R07L1-0-121119 23.6 34.4 16.9 50.3 46.4 16.4 84.2 245 3.69 2.14 <5.00

ISO12-01-01-03-050 DAL-SW-R07L2-0-121119 30.9 41.4 20.8 62.6 63.8 19.5 102 352 5.65 <2.00 <5.00

ISO12-01-01-03-051 DAL-SW-R07L3-0-121119 9.41 10.9 6.16 21.1 9.65 <5.00 34.8 48.6 <2.00 <2.00 <5.00

ISO12-01-01-03-046 DAL-SW-R08L1-0-121119 <5.00 2.40 <2.00 3.37 <5.00 <5.00 6.42 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-047 DAL-SW-R08L2-0-121119 <5.00 <2.00 <2.00 2.56 <5.00 <5.00 6.57 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-048 DAL-SW-R08L3-0-121119 8.41 3.48 <2.00 4.70 <5.00 <5.00 7.67 2.08 <2.00 <2.00 <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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 4 OF 52

Table 1 continued. Sample Results Summary (1)

Concentration (ng/L; parts per trillion)

3M LIMS ID Sample Description PFBA PFHxA PFHpA PFOA PFBS PFHS PFOS FBSA FOSA MeFOSAA EtFOSAA

Fish Sampling Reaches

ISO12-01-01-03-043 DAL-SW-R09L1-0-121119 29.5 59.2 22.1 62.3 64.1 19.7 103 185 6.15 <2.00 <5.00

ISO12-01-01-03-044 DAL-SW-R09L2-0-121119 36.9 61.9 25.4 79.9 84.6 26.2 125 330 7.71 <2.00 <5.00

ISO12-01-01-03-045 DAL-SW-R09L3-0-121119 26.5 49.5 18.1 58.0 59.4 19.6 91.0 197 5.47 <2.00 <5.00

ISO12-01-01-03-038 DAL-SW-R10L1-0-121119 7.16 3.23 <2.00 2.63 <5.00 <5.00 6.82 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-039 DAL-SW-R10L2-0-121119 5.20 2.10 <2.00 2.53 <5.00 <5.00 6.99 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-040 DAL-SW-R10L3-0-121119 <5.00 2.73 <2.00 3.52 <5.00 <5.00 6.49 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-035 DAL-SW-R11L1-0-121119 22.5 75.5 19.5 53.1 52.1 17.9 87.8 129 5.65 <2.00 <5.00

ISO12-01-01-03-036 DAL-SW-R11L2-0-121119 24.2 70.2 22.6 61.9 51.1 18.9 91.0 116 4.19 <2.00 <5.00

ISO12-01-01-03-037 DAL-SW-R11L3-0-121119 16.7 47.7 12.0 38.7 28.9 11.3 69.5 74.1 3.89 <2.00 <5.00

ISO12-01-01-03-032 DAL-SW-R12L1-0-121117 5.46 7.41 <2.00 6.35 <5.00 <5.00 12.4 4.75 <2.00 <2.00 <5.00

ISO12-01-01-03-033 DAL-SW-R12L2-0-121117 6.89 7.56 <2.00 6.51 <5.00 <5.00 13.8 4.95 <2.00 <2.00 <5.00

ISO12-01-01-03-034 DAL-SW-R12L3-0-121117 6.63 6.61 <2.00 7.09 <5.00 <5.00 13.3 5.12 <2.00 <2.00 <5.00

ISO12-01-01-03-029 DAL-SW-R13L1-0-121117 7.95 10.2 3.36 14.4 10.0 <5.00 24.8 20.4 <2.00 <2.00 <5.00

ISO12-01-01-03-030 DAL-SW-R13L2-0-121117 8.65 8.59 3.26 18.2 12.0 <5.00 27.7 24.4 <2.00 <2.00 <5.00

ISO12-01-01-03-031 DAL-SW-R13L3-0-121117 7.76 10.9 2.57 15.3 9.83 <5.00 23.8 21.6 <2.00 <2.00 <5.00

ISO12-01-01-03-021 DAL-SW-R14L1-0-121117 6.82 4.82 <2.00 11.1 7.61 <5.00 18.7 14.7 <2.00 <2.00 <5.00

ISO12-01-01-03-022 DAL-SW-R14L2-0-121117 6.41 5.32 2.18 11.5 7.69 <5.00 19.0 14.3 <2.00 <2.00 <5.00

ISO12-01-01-03-023 DAL-SW-R14L3-0-121117 7.48 6.34 2.19 12.0 8.47 <5.00 23.0 16.1 <2.00 <2.00 <5.00

ISO12-01-01-03-024 DAL-SW-R15L1-0-121117 7.92 4.24 2.34 11.5 14.8 <5.00 19.9 34.8 <2.00 <2.00 <5.00

ISO12-01-01-03-027 DAL-SW-R15L2-0-121117 7.43 4.60 2.23 12.8 13.2 <5.00 18.4 32.8 <2.00 <2.00 <5.00

ISO12-01-01-03-028 DAL-SW-R15L3-0-121117 7.55 4.69 2.07 10.7 14.1 <5.00 18.1 32.8 <2.00 <2.00 <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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 5 OF 52

Table 1 continued. Sample Results Summary (1)

Concentration (ng/L; parts per trillion)

3M LIMS ID Sample Description PFBA PFHxA PFHpA PFOA PFBS PFHS PFOS FBSA FOSA MeFOSAA EtFOSAA

Transect Sampling Locations

ISO12-01-01-03-062 DAL-SW-T101-0-121203 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 6.13 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-065 DAL-SW-T102-0-121203 <5.00 2.12 <2.00 <1.92 <5.00 <5.00 6.15 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-066 DAL-SW-T103-0-121203 <5.00 <2.00 <2.00 2.51 <5.00 <5.00 6.80 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-067 DAL-SW-T104-0-121203 <5.00 2.18 <2.00 2.55 <5.00 <5.00 6.89 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-068 DAL-SW-T105-0-121203 <5.00 2.16 <2.00 2.56 <5.00 <5.00 6.63 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-069 DAL-SW-T106-0-121203 5.19 <2.00 <2.00 2.57 <5.00 <5.00 6.43 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-070 DAL-SW-T107-0-121203 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 6.38 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-071 DAL-SW-T108-0-121203 <5.00 2.00 <2.00 8.73 <5.00 9.38 6.60 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-072 DAL-SW-T109-0-121203 <5.00 <2.00 <2.00 2.75 <5.00 <5.00 6.45 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-073 DAL-SW-T110-0-121203 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 6.70 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-074 DAL-SW-T201-0-121203 5.79 4.75 3.07 9.73 <5.00 <5.00 8.35 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-075 DAL-SW-T202-0-121203 6.72 5.16 4.80 12.6 <5.00 <5.00 9.93 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-078 DAL-SW-T203-0-121203 <5.00 2.20 <2.00 <1.92 <5.00 <5.00 6.50 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-079 DAL-SW-T204-0-121203 <5.00 <2.00 <2.00 2.42 <5.00 <5.00 6.23 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-080 DAL-SW-T205-0-121203 <5.00 <2.00 <2.00 3.01 <5.00 <5.00 6.96 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-081 DAL-SW-T206-0-121203 <5.00 <2.00 <2.00 2.66 <5.00 <5.00 6.79 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-082 DAL-SW-T207-0-121203 <5.00 2.11 <2.00 2.08 <5.00 <5.00 6.83 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-083 DAL-SW-T208-0-121204 5.66 <2.00 <2.00 3.02 <5.00 <5.00 6.44 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-084 DAL-SW-T209-0-121204 <5.00 <2.00 <2.00 2.27 <5.00 <5.00 6.98 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-085 DAL-SW-T210-0-121204 <5.00 2.19 <2.00 3.90 <5.00 <5.00 7.77 <2.00 <2.00 <2.00 <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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 6 OF 52

Table 1 continued. Sample Results Summary (1)

Concentration (ng/L; parts per trillion)

3M LIMS ID Sample Description PFBA PFHxA PFHpA PFOA PFBS PFHS PFOS FBSA FOSA MeFOSAA EtFOSAA

Transect Sampling Locations

ISO12-01-01-03-086 DAL-SW-T301-0-121203 <5.00 4.55 2.23 15.2 <5.00 <5.00 19.0 2.32 <2.00 <2.00 <5.00

ISO12-01-01-03-087 DAL-SW-T302-0-121203 <5.00 2.14 <2.00 2.97 <5.00 <5.00 7.46 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-088 DAL-SW-T303-0-121203 <5.00 <2.00 <2.00 2.78 <5.00 <5.00 6.94 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-091 DAL-SW-T304-0-121203 <5.00 <2.00 <2.00 2.15 <5.00 <5.00 7.68 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-092 DAL-SW-T305-0-121203 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 7.30 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-093 DAL-SW-T306-0-121203 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 6.11 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-094 DAL-SW-T307-0-121203 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 6.57 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-095 DAL-SW-T308-0-121203 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 6.98 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-096 DAL-SW-T309-0-121203 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 6.58 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-097 DAL-SW-T310-0-121203 <5.00 <2.00 <2.00 2.28 <5.00 <5.00 7.32 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-098 DAL-SW-T401-0-121203 38.1 33.4 19.6 74.5 285 17.4 138 453 18.3 4.46 <5.00

ISO12-01-01-03-099 DAL-SW-T402-0-121203 5.98 2.86 <2.00 4.54 <5.00 <5.00 8.69 2.81 <2.00 <2.00 <5.00

ISO12-01-01-03-100 DAL-SW-T403-0-121203 7.83 <2.00 <2.00 2.73 <5.00 <5.00 7.52 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-101 DAL-SW-T404-0-121203 <5.00 <2.00 <2.00 2.25 <5.00 <5.00 7.29 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-104 DAL-SW-T405-0-121203 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 8.21 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-105 DAL-SW-T406-0-121203 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 7.42 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-106 DAL-SW-T407-0-121203 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 7.31 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-107 DAL-SW-T408-0-121203 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 7.04 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-108 DAL-SW-T409-0-121203 5.04 <2.00 <2.00 <1.92 <5.00 <5.00 6.73 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-109 DAL-SW-T410-0-121203 5.67 2.84 <2.00 3.87 <5.00 <5.00 7.78 <2.00 <2.00 <2.00 <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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 7 OF 52

Table 1 continued. Sample Results Summary (1)

Concentration (ng/L; parts per trillion)

3M LIMS ID Sample Description PFBA PFHxA PFHpA PFOA PFBS PFHS PFOS FBSA FOSA MeFOSAA EtFOSAA

Transect Sampling Locations

ISO12-01-01-03-110 DAL-SW-T501-0-121204 23.7 26.7 14.4 48.2 105 14.3 72.8 139 5.69 <2.00 <5.00

ISO12-01-01-03-111 DAL-SW-T502-0-121204 24.3 24.5 14.2 45.7 115 12.6 76.5 168 6.61 <2.00 <5.00

ISO12-01-01-03-112 DAL-SW-T503-0-121204 14.4 13.7 9.19 29.0 63.8 8.35 49.2 96.4 2.58 <2.00 <5.00

ISO12-01-01-03-113 DAL-SW-T504-0-121204 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 7.89 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-114 DAL-SW-T505-0-121204 <5.00 <2.00 <2.00 2.52 <5.00 <5.00 7.20 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-117 DAL-SW-T506-0-121204 <5.00 <2.00 <2.00 2.59 <5.00 <5.00 6.82 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-118 DAL-SW-T507-0-121204 <5.00 <2.00 <2.00 2.20 <5.00 <5.00 8.10 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-119 DAL-SW-T508-0-121204 <5.00 <2.00 <2.00 3.33 <5.00 <5.00 8.20 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-120 DAL-SW-T509-0-121204 5.02 <2.00 <2.00 3.27 <5.00 <5.00 8.15 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-121 DAL-SW-T510-0-121204 8.56 3.99 <2.00 4.33 <5.00 <5.00 8.57 2.29 <2.00 <2.00 <5.00

ISO12-01-01-03-122 DAL-SW-T601-0-121204 43.2 69.4 27.3 69.2 89.6 24.2 86.4 254 6.17 <2.00 <5.00

ISO12-01-01-03-123 DAL-SW-T602-0-121204 23.3 27.8 22.0 68.6 124 18.0 107 168 5.06 <2.00 <5.00

ISO12-01-01-03-124 DAL-SW-T603-0-121204 13.9 14.6 9.62 36.8 57.0 9.19 56.6 75.3 3.06 <2.00 <5.00

ISO12-01-01-03-125 DAL-SW-T604-0-121204 8.09 7.90 4.85 14.6 23.7 <5.00 23.8 32.1 <2.00 <2.00 <5.00

ISO12-01-01-03-126 DAL-SW-T605-0-121204 7.48 5.65 3.37 9.37 12.4 <5.00 14.5 15.8 <2.00 <2.00 <5.00

ISO12-01-01-03-127 DAL-SW-T606-0-121204 <5.00 2.31 <2.00 4.38 <5.00 <5.00 9.72 2.22 <2.00 <2.00 <5.00

ISO12-01-01-03-130 DAL-SW-T607-0-121204 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 6.49 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-131 DAL-SW-T608-0-121204 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 6.92 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-132 DAL-SW-T609-0-121204 5.72 <2.00 <2.00 2.61 <5.00 <5.00 7.66 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-133 DAL-SW-T610-0-121204 8.74 2.75 <2.00 3.12 <5.00 <5.00 7.83 <2.00 <2.00 <2.00 <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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 8 OF 52

Table 1 continued. Sample Results Summary (1)

Concentration (ng/L; parts per trillion)

3M LIMS ID Sample Description PFBA PFHxA PFHpA PFOA PFBS PFHS PFOS FBSA FOSA MeFOSAA EtFOSAA

Transect Sampling Locations

ISO12-01-01-03-134 DAL-SW-T701-0-121204 18.1 17.5 8.58 28.1 71.0 8.07 42.6 213 4.77 <2.00 <5.00

ISO12-01-01-03-135 DAL-SW-T702-0-121204 15.7 15.8 9.41 30.7 65.1 8.37 46.6 118 2.86 <2.00 <5.00

ISO12-01-01-03-136 DAL-SW-T703-0-121204 11.4 12.3 8.23 29.8 55.6 7.69 46.8 75.1 <2.00 <2.00 <5.00

ISO12-01-01-03-137 DAL-SW-T704-0-121204 8.59 8.17 4.78 18.5 32.5 <5.00 31.6 41.3 <2.00 <2.00 <5.00

ISO12-01-01-03-138 DAL-SW-T705-0-121204 9.71 9.49 6.15 18.9 36.2 5.17 31.2 47.7 <2.00 <2.00 <5.00

ISO12-01-01-03-139 DAL-SW-T706-0-121204 10.1 7.39 5.83 14.5 26.9 <5.00 24.2 35.6 <2.00 <2.00 <5.00

ISO12-01-01-03-140 DAL-SW-T707-0-121204 8.42 4.05 3.24 12.5 19.0 <5.00 20.2 27.6 <2.00 <2.00 <5.00

ISO12-01-01-03-143 DAL-SW-T708-0-121204 6.96 3.90 2.82 7.98 14.0 <5.00 16.5 17.2 <2.00 <2.00 <5.00

ISO12-01-01-03-144 DAL-SW-T709-0-121204 7.35 4.20 2.32 6.86 10.6 <5.00 13.4 12.6 <2.00 <2.00 <5.00

ISO12-01-01-03-145 DAL-SW-T710-0-121204 8.39 5.25 3.52 10.7 17.7 <5.00 17.6 20.0 <2.00 <2.00 <5.00

ISO12-01-01-03-146 DAL-SW-T801-0-121205 6.89 4.58 <2.00 8.51 13.0 <5.00 15.2 32.2 <2.00 <2.00 <5.00

ISO12-01-01-03-147 DAL-SW-T802-0-121205 6.82 4.33 <2.00 9.43 12.5 <5.00 15.4 31.4 <2.00 <2.00 <5.00

ISO12-01-01-03-148 DAL-SW-T803-0-121205 9.03 3.80 <2.00 10.2 13.2 <5.00 15.9 34.8 <2.00 <2.00 <5.00

ISO12-01-01-03-149 DAL-SW-T804-0-121205 7.76 4.46 2.81 7.81 14.3 <5.00 16.6 35.0 <2.00 <2.00 <5.00

ISO12-01-01-03-150 DAL-SW-T805-0-121205 8.01 3.92 <2.00 8.08 12.9 <5.00 15.4 35.0 <2.00 <2.00 <5.00

ISO12-01-01-03-151 DAL-SW-T806-0-121205 5.79 3.80 3.07 7.30 12.1 <5.00 12.1 28.2 <2.00 <2.00 <5.00

ISO12-01-01-03-152 DAL-SW-T807-0-121205 6.26 2.95 2.03 7.21 11.5 <5.00 14.1 27.0 <2.00 <2.00 <5.00

ISO12-01-01-03-153 DAL-SW-T808-0-121205 6.28 4.51 <2.00 7.49 11.2 <5.00 13.3 25.7 <2.00 <2.00 <5.00

ISO12-01-01-03-156 DAL-SW-T809-0-121205 6.50 2.80 <2.00 7.26 9.28 <5.00 11.5 18.9 <2.00 <2.00 <5.00

ISO12-01-01-03-157 DAL-SW-T810-0-121205 5.62 2.79 <2.00 6.49 11.1 <5.00 12.3 14.1 <2.00 <2.00 <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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 9 OF 52

Table 1 continued. Sample Results Summary (1)

Concentration (ng/L; parts per trillion)

3M LIMS ID Sample Description PFBA PFHxA PFHpA PFOA PFBS PFHS PFOS FBSA FOSA MeFOSAA EtFOSAA

Transect Sampling Locations

ISO12-01-01-03-158 DAL-SW-T901-0-121205 7.76 9.09 3.32 12.9 17.7 <5.00 20.3 34.7 <2.00 <2.00 <5.00

ISO12-01-01-03-159 DAL-SW-T902-0-121205 9.51 7.72 3.88 11.9 11.2 <5.00 20.5 35.1 <2.00 <2.00 <5.00

ISO12-01-01-03-160 DAL-SW-T903-0-121205 7.45 7.62 2.16 11.9 14.2 <5.00 20.1 33.4 <2.00 <2.00 <5.00

ISO12-01-01-03-161 DAL-SW-T904-0-121205 8.98 7.82 3.28 13.1 13.7 <5.00 20.7 36.9 <2.00 <2.00 <5.00

ISO12-01-01-03-162 DAL-SW-T905-0-121205 7.48 8.78 3.11 13.2 14.7 <5.00 24.4 35.4 <2.00 <2.00 <5.00

ISO12-01-01-03-163 DAL-SW-T906-0-121205 6.76 6.57 3.30 10.9 13.9 <5.00 19.7 43.2 <2.00 <2.00 <5.00

ISO12-01-01-03-164 DAL-SW-T907-0-121205 7.69 7.25 3.99 11.5 12.7 <5.00 21.4 43.9 <2.00 <2.00 <5.00

ISO12-01-01-03-165 DAL-SW-T908-0-121205 6.74 6.58 3.43 12.1 13.4 <5.00 20.3 45.4 <2.00 <2.00 <5.00

ISO12-01-01-03-166 DAL-SW-T909-0-121205 8.66 7.12 3.37 11.6 12.8 <5.00 19.2 46.3 <2.00 <2.00 <5.00

ISO12-01-01-03-169 DAL-SW-T910-0-121205 7.96 6.42 3.37 10.9 13.4 <5.00 19.0 45.5 <2.00 <2.00 <5.00

Trip and Equipment Blanks

ISO12-01-01-03-001 DAL-MSW-LS-EQB01 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 <0.927 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-002 DAL-MSW-LS-EQB02 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 1.05 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-003 DAL-MSW-LS-EQB03 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 <0.927 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-060 DAL-SW-TRIP01-0-121116 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 <0.927 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-170 DAL-SW-TRIP-01-0-121203 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 <0.927 <2.00 <2.00 <2.00 <5.00

ISO12-01-01-03-172 DAL-IPW-LS-EQB04 <5.00 <2.00 <2.00 <1.92 <5.00 <5.00 <0.927 <2.00 <2.00 <2.00 <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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 10 OF 52

Table 2. Surrogate Recovery Standards Summary 

SRS Recovery (%)

3M LIMS ID Sample Description 13C3-PFBA 13C4-PFOA 13C4-PFOS

Fish Sampling Reaches

ISO12-01-01-03-007 DAL-SW-R01L1-0-121116 90.6 93.0 89.1

ISO12-01-01-03-008 DAL-SW-R01L2-0-121116 93.8 82.4 91.4

ISO12-01-01-03-009 DAL-SW-R01L3-0-121116 93.8 83.4 91.8

ISO12-01-01-03-010 DAL-SW-R02L1-0-121116 93.8 87.2 88.5

ISO12-01-01-03-011 DAL-SW-R02L2-0-121116 94.2 87.0 90.6

ISO12-01-01-03-012 DAL-SW-R02L3-0-121116 94.8 82.0 90.8

ISO12-01-01-03-013 DAL-SW-R02L3-DB-121116 92.6 85.0 91.0

ISO12-01-01-03-014 DAL-SW-R02L3-FMS-121116 93.6 87.4 89.5

ISO12-01-01-03-015 DAL-SW-R03L1-0-121116 89.8 87.2 91.1

ISO12-01-01-03-016 DAL-SW-R03L2-0-121116 92.2 81.4 92.6

ISO12-01-01-03-017 DAL-SW-R03L3-0-121116 95.6 86.6 92.0

ISO12-01-01-03-018 DAL-SW-R04L1-0-121116 90.6 85.4 92.9

ISO12-01-01-03-019 DAL-SW-R04L2-0-121116 92.2 83.8 94.8

ISO12-01-01-03-020 DAL-SW-R04L3-0-121116 92.8 84.4 90.8

ISO12-01-01-03-052 DAL-SW-R05L1-0-121119 93.6 82.4 89.1

ISO12-01-01-03-053 DAL-SW-R05L1-DB-121119 91.2 83.0 92.9

ISO12-01-01-03-054 DAL-SW-R05L1-FMS-121119 92.2 87.4 91.6

ISO12-01-01-03-055 DAL-SW-R05L2-0-121119 92.8 84.8 91.4

ISO12-01-01-03-056 DAL-SW-R05L3-0-121119 91.4 84.6 99.4

ISO12-01-01-03-057 DAL-SW-R06L1-0-121120 88.2 85.2 90.1

ISO12-01-01-03-058 DAL-SW-R06L2-0-121120 94.2 85.6 89.4

ISO12-01-01-03-059 DAL-SW-R06L3-0-121120 89.4 86.2 91.5

ISO12-01-01-03-049 DAL-SW-R07L1-0-121119 90.4 82.8 96.9

ISO12-01-01-03-050 DAL-SW-R07L2-0-121119 96.0 86.2 88.3

ISO12-01-01-03-051 DAL-SW-R07L3-0-121119 99.4 86.4 97.9

ISO12-01-01-03-046 DAL-SW-R08L1-0-121119 94.6 83.8 87.7

ISO12-01-01-03-047 DAL-SW-R08L2-0-121119 95.0 85.4 89.7

ISO12-01-01-03-048 DAL-SW-R08L3-0-121119 92.6 84.2 90.0

ISO12-01-01-03-043 DAL-SW-R09L1-0-121119 89.8 85.4 95.6

ISO12-01-01-03-044 DAL-SW-R09L2-0-121119 92.2 83.6 95.0

ISO12-01-01-03-045 DAL-SW-R09L3-0-121119 95.8 83.6 97.3

ISO12-01-01-03-038 DAL-SW-R10L1-0-121119 91.4 80.0 91.6

ISO12-01-01-03-039 DAL-SW-R10L2-0-121119 92.8 83.8 89.7

ISO12-01-01-03-040 DAL-SW-R10L3-0-121119 90.0 89.0 91.8

ISO12-01-01-03-041 DAL-SW-R10L3-DB-121119 93.0 86.6 91.2

ISO12-01-01-03-042 DAL-SW-R10L3-FMS-121119 90.8 84.0 91.8

ISO12-01-01-03-035 DAL-SW-R11L1-0-121119 90.2 79.0 94.1

ISO12-01-01-03-036 DAL-SW-R11L2-0-121119 94.4 83.2 89.7

ISO12-01-01-03-037 DAL-SW-R11L3-0-121119 94.2 85.2 90.0

ISO12-01-01-03-032 DAL-SW-R12L1-0-121117 90.2 76.6 89.3

ISO12-01-01-03-033 DAL-SW-R12L2-0-121117 95.2 85.8 93.7

ISO12-01-01-03-034 DAL-SW-R12L3-0-121117 96.0 87.4 95.6
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 11 OF 52

Table 2 continued. Surrogate Recovery Standards Summary 

SRS Recovery (%)

3M LIMS ID Sample Description 13C3-PFBA 13C4-PFOA 13C4-PFOS

Fish Sampling Reaches

ISO12-01-01-03-029 DAL-SW-R13L1-0-121117 88.8 79.6 92.1

ISO12-01-01-03-030 DAL-SW-R13L2-0-121117 92.6 82.2 91.2

ISO12-01-01-03-031 DAL-SW-R13L3-0-121117 92.8 84.4 94.4

ISO12-01-01-03-021 DAL-SW-R14L1-0-121117 95.4 81.8 93.9

ISO12-01-01-03-022 DAL-SW-R14L2-0-121117 95.4 88.0 92.5

ISO12-01-01-03-023 DAL-SW-R14L3-0-121117 94.0 89.8 90.2

ISO12-01-01-03-024 DAL-SW-R15L1-0-121117 90.4 85.6 94.1

ISO12-01-01-03-025 DAL-SW-R15L1-DB-121117 93.1 86.8 93.7

ISO12-01-01-03-026 DAL-SW-R15L1-FMS-121117 93.0 86.0 95.2

ISO12-01-01-03-027 DAL-SW-R15L2-0-121117 94.4 83.8 91.2

ISO12-01-01-03-028 DAL-SW-R15L3-0-121117 91.8 84.0 88.5

Transect Sampling Locations

ISO12-01-01-03-062 DAL-SW-T101-0-121203 94.2 86.4 91.0

ISO12-01-01-03-063 DAL-SW-T101-DB-121203 96.2 86.4 90.0

ISO12-01-01-03-064 DAL-SW-T101-FMS-121203 93.8 82.2 94.8

ISO12-01-01-03-065 DAL-SW-T102-0-121203 92.2 86.4 94.4

ISO12-01-01-03-066 DAL-SW-T103-0-121203 92.6 91.2 92.3

ISO12-01-01-03-067 DAL-SW-T104-0-121203 93.0 92.2 90.0

ISO12-01-01-03-068 DAL-SW-T105-0-121203 96.6 87.8 91.8

ISO12-01-01-03-069 DAL-SW-T106-0-121203 95.6 88.0 92.5

ISO12-01-01-03-070 DAL-SW-T107-0-121203 96.6 84.8 91.8

ISO12-01-01-03-071 DAL-SW-T108-0-121203 95.0 86.6 89.1

ISO12-01-01-03-072 DAL-SW-T109-0-121203 92.6 92.4 91.2

ISO12-01-01-03-073 DAL-SW-T110-0-121203 94.6 90.0 94.1

ISO12-01-01-03-074 DAL-SW-T201-0-121203 97.0 89.0 92.1

ISO12-01-01-03-075 DAL-SW-T202-0-121203 94.4 91.0 92.1

ISO12-01-01-03-076 DAL-SW-T202-DB-121203 93.6 91.4 90.8

ISO12-01-01-03-077 DAL-SW-T202-FMS-121203 99.8 88.2 92.1

ISO12-01-01-03-078 DAL-SW-T203-0-121203 94.2 84.4 91.4

ISO12-01-01-03-079 DAL-SW-T204-0-121203 94.0 87.8 92.9

ISO12-01-01-03-080 DAL-SW-T205-0-121203 94.6 90.6 92.3

ISO12-01-01-03-081 DAL-SW-T206-0-121203 95.0 83.8 92.9

ISO12-01-01-03-082 DAL-SW-T207-0-121203 91.6 83.4 93.7

ISO12-01-01-03-083 DAL-SW-T208-0-121204 95.2 92.0 92.7

ISO12-01-01-03-084 DAL-SW-T209-0-121204 97.4 85.2 92.9

ISO12-01-01-03-085 DAL-SW-T210-0-121204 96.8 92.6 86.8
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 12 OF 52

Table 2 continued. Surrogate Recovery Standards Summary 

SRS Recovery (%)

3M LIMS ID Sample Description 13C3-PFBA 13C4-PFOA 13C4-PFOS

Transect Sampling Locations

ISO12-01-01-03-086 DAL-SW-T301-0-121203 96.4 90.0 93.3

ISO12-01-01-03-087 DAL-SW-T302-0-121203 94.8 87.6 95.0

ISO12-01-01-03-088 DAL-SW-T303-0-121203 91.2 90.2 93.3

ISO12-01-01-03-089 DAL-SW-T303-DB-121203 94.2 89.6 92.5

ISO12-01-01-03-090 DAL-SW-T303-FMS-121203 93.0 85.8 94.1

ISO12-01-01-03-091 DAL-SW-T304-0-121203 94.6 90.4 92.5

ISO12-01-01-03-092 DAL-SW-T305-0-121203 96.2 85.4 90.6

ISO12-01-01-03-093 DAL-SW-T306-0-121203 95.0 91.2 90.6

ISO12-01-01-03-094 DAL-SW-T307-0-121203 94.6 89.6 91.6

ISO12-01-01-03-095 DAL-SW-T308-0-121203 93.0 84.6 91.4

ISO12-01-01-03-096 DAL-SW-T309-0-121203 93.8 86.6 90.8

ISO12-01-01-03-097 DAL-SW-T310-0-121203 95.6 88.8 90.6

ISO12-01-01-03-098 DAL-SW-T401-0-121203 95.4 87.0 91.8

ISO12-01-01-03-099 DAL-SW-T402-0-121203 96.6 85.4 92.1

ISO12-01-01-03-100 DAL-SW-T403-0-121203 94.4 91.6 91.0

ISO12-01-01-03-101 DAL-SW-T404-0-121203 96.0 87.8 94.6

ISO12-01-01-03-102 DAL-SW-T404-DB-121203 92.2 92.0 91.6

ISO12-01-01-03-103 DAL-SW-T404-FMS-121203 93.8 88.8 93.9

ISO12-01-01-03-104 DAL-SW-T405-0-121203 94.0 88.0 90.6

ISO12-01-01-03-105 DAL-SW-T406-0-121203 92.8 90.6 91.6

ISO12-01-01-03-106 DAL-SW-T407-0-121203 95.0 81.8 90.4

ISO12-01-01-03-107 DAL-SW-T408-0-121203 94.0 93.0 92.5

ISO12-01-01-03-108 DAL-SW-T409-0-121203 91.4 86.2 91.2

ISO12-01-01-03-109 DAL-SW-T410-0-121203 94.8 90.0 89.3

ISO12-01-01-03-110 DAL-SW-T501-0-121204 95.2 89.6 97.9

ISO12-01-01-03-111 DAL-SW-T502-0-121204 94.8 88.2 95.8

ISO12-01-01-03-112 DAL-SW-T503-0-121204 97.2 91.2 97.3

ISO12-01-01-03-113 DAL-SW-T504-0-121204 96.4 86.8 93.3

ISO12-01-01-03-114 DAL-SW-T505-0-121204 94.6 88.0 93.5

ISO12-01-01-03-115 DAL-SW-T505-DB-121204 95.2 84.6 93.9

ISO12-01-01-03-116 DAL-SW-T505-FMS-121204 94.2 86.4 93.9

ISO12-01-01-03-117 DAL-SW-T506-0-121204 96.0 88.6 90.8

ISO12-01-01-03-118 DAL-SW-T507-0-121204 96.0 85.2 91.0

ISO12-01-01-03-119 DAL-SW-T508-0-121204 93.8 91.6 94.1

ISO12-01-01-03-120 DAL-SW-T509-0-121204 96.4 85.4 90.6

ISO12-01-01-03-121 DAL-SW-T510-0-121204 93.2 91.4 91.4
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 13 OF 52

Table 2 continued. Surrogate Recovery Standards Summary 

SRS Recovery (%)

3M LIMS ID Sample Description 13C3-PFBA 13C4-PFOA 13C4-PFOS

Transect Sampling Locations

ISO12-01-01-03-122 DAL-SW-T601-0-121204 93.2 85.6 92.9

ISO12-01-01-03-123 DAL-SW-T602-0-121204 94.6 83.2 94.1

ISO12-01-01-03-124 DAL-SW-T603-0-121204 94.6 95.4 93.5

ISO12-01-01-03-125 DAL-SW-T604-0-121204 93.0 84.8 95.4

ISO12-01-01-03-126 DAL-SW-T605-0-121204 94.0 83.8 91.6

ISO12-01-01-03-127 DAL-SW-T606-0-121204 96.8 86.0 92.7

ISO12-01-01-03-128 DAL-SW-T606-DB-121204 94.2 86.0 90.2

ISO12-01-01-03-129 DAL-SW-T606-FMS-121204 96.6 86.0 91.6

ISO12-01-01-03-130 DAL-SW-T607-0-121204 93.0 85.5 89.3

ISO12-01-01-03-131 DAL-SW-T608-0-121204 94.4 88.6 91.4

ISO12-01-01-03-132 DAL-SW-T609-0-121204 94.0 84.6 92.9

ISO12-01-01-03-133 DAL-SW-T610-0-121204 92.4 88.8 89.7

ISO12-01-01-03-134 DAL-SW-T701-0-121204 95.8 88.8 93.5

ISO12-01-01-03-135 DAL-SW-T702-0-121204 96.2 85.6 96.2

ISO12-01-01-03-136 DAL-SW-T703-0-121204 95.0 87.0 96.2

ISO12-01-01-03-137 DAL-SW-T704-0-121204 94.6 86.2 97.7

ISO12-01-01-03-138 DAL-SW-T705-0-121204 95.0 85.2 94.6

ISO12-01-01-03-139 DAL-SW-T706-0-121204 99.4 86.6 97.7

ISO12-01-01-03-140 DAL-SW-T707-0-121204 91.6 92.6 91.8

ISO12-01-01-03-141 DAL-SW-T707-DB-121204 95.2 92.6 90.0

ISO12-01-01-03-142 DAL-SW-T707-FMS-121204 93.4 92.9 94.9

ISO12-01-01-03-143 DAL-SW-T708-0-121204 94.4 82.4 100

ISO12-01-01-03-144 DAL-SW-T709-0-121204 93.6 87.8 91.0

ISO12-01-01-03-145 DAL-SW-T710-0-121204 94.4 93.6 93.3

ISO12-01-01-03-146 DAL-SW-T801-0-121205 94.4 86.2 92.1

ISO12-01-01-03-147 DAL-SW-T802-0-121205 93.8 89.0 91.4

ISO12-01-01-03-148 DAL-SW-T803-0-121205 92.8 90.4 91.4

ISO12-01-01-03-149 DAL-SW-T804-0-121205 95.8 87.0 92.7

ISO12-01-01-03-150 DAL-SW-T805-0-121205 94.8 88.6 93.9

ISO12-01-01-03-151 DAL-SW-T806-0-121205 92.6 81.0 91.4

ISO12-01-01-03-152 DAL-SW-T807-0-121205 93.0 87.2 96.2

ISO12-01-01-03-153 DAL-SW-T808-0-121205 93.2 84.8 92.3

ISO12-01-01-03-154 DAL-SW-T808-DB-121205 94.6 87.4 96.2

ISO12-01-01-03-155 DAL-SW-T808-FMS-121205 95.6 91.0 93.7

ISO12-01-01-03-156 DAL-SW-T809-0-121205 95.0 93.6 92.5

ISO12-01-01-03-157 DAL-SW-T810-0-121205 96.0 93.0 92.3
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Table 2 continued. Surrogate Recovery Standards Summary 

SRS Recovery (%)

3M LIMS ID Sample Description 13C3-PFBA 13C4-PFOA 13C4-PFOS

Transect Sampling Locations

ISO12-01-01-03-158 DAL-SW-T901-0-121205 95.6 86.0 94.1

ISO12-01-01-03-159 DAL-SW-T902-0-121205 93.0 88.2 91.8

ISO12-01-01-03-160 DAL-SW-T903-0-121205 95.8 89.2 91.0

ISO12-01-01-03-161 DAL-SW-T904-0-121205 94.6 88.0 90.0

ISO12-01-01-03-162 DAL-SW-T905-0-121205 95.2 90.6 93.7

ISO12-01-01-03-163 DAL-SW-T906-0-121205 96.4 83.8 93.9

ISO12-01-01-03-164 DAL-SW-T907-0-121205 98.0 88.4 93.9

ISO12-01-01-03-165 DAL-SW-T908-0-121205 94.0 89.4 95.0

ISO12-01-01-03-166 DAL-SW-T909-0-121205 93.0 86.2 96.9

ISO12-01-01-03-167 DAL-SW-T909-DB-121205 94.4 95.6 96.2

ISO12-01-01-03-168 DAL-SW-T909-FMS-121205 93.2 87.8 95.6

ISO12-01-01-03-169 DAL-SW-T910-0-121205 94.0 95.0 92.3

Trip Blank Samples and Equipment Blanks

ISO12-01-01-03-001 DAL-MSW-LS-EQB01 96.0 88.0 95.2

ISO12-01-01-03-002 DAL-MSW-LS-EQB02 90.8 84.8 95.0

ISO12-01-01-03-003 DAL-MSW-LS-EQB03 93.6 86.4 92.5

ISO12-01-01-03-060 DAL-SW-TRIP01-0-121116 93.0 89.4 90.6

ISO12-01-01-03-061 DAL-SW-TRIP02-0-121116 92.4 87.2 92.5

ISO12-01-01-03-170 DAL-SW-TRIP-01-0-121203 94.4 85.2 92.9

ISO12-01-01-03-171 DAL-SW-TRIP-01-FMS-121203 96.6 88.6 88.1

ISO12-01-01-03-172 DAL-IPW-LS-EQB04 93.2 87.2 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 Acronym Reference Material Structure

Perfluorobutanoic Acid (C4 Acid) PFBA Linear

Perfluorohexanoic Acid (C6 Acid) PFHxA Linear

Perfluoroheptanoic Acid (C7 Acid) PFHpA Linear

Perfluorooctanoic Acid (C8 Acid) PFOA Linear + Branched 

Perfluorobutanesulfonate (C4 Sulfonate ) PFBS Linear

Perfluorohexanesulfonate (C6 Sulfonate) PFHS Linear

Perfluorooctanesulfonate (C8 Sulfonate) PFOS Linear + Branched 

Perfluorobutanesulfonamide FBSA Linear

Perfluorooctanesulfonamide FOSA Linear + Branched

2-(N-methyl-PFOSA) acetic acid MeFOSAA Linear 

2-(N-ethyl-PFOSA) acetic acid EtFOSAA Linear 
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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 String Descriptor Example

Example 1 DAL-SW-R01L1-0-121116 (Fish Sampling Location)

1 Sample Location DAL= Decatur, Alabama

2 Sample Type SW = Surface Water 

3 Fish Sampling Reach R01 = Reach 1

4 Sampling Location L1 = Location 1

(three locations sampled within each fish sampling reach)

5 Sample Type 0 = primary sample 

DB = duplicate sample

FMS = Field Matrix Spike

6 Sampling Date 121116– November 16, 2012 

Example 2 DAL-SW-T805-0-121205 (Transect Sampling Location)

1 Sample Location DAL= Decatur, Alabama

2 Sample Type SW = Surface Water 

3 Transect Sampling Location T8 = Transect 8

4 Sampling Location 05 = Location 5 

(ten locations sampled within each transect )

5 Sample Type 0 = primary sample 

DB = duplicate sample

FMS = Field Matrix Spike

6 Sampling Date 121205– December 05, 2012 
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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 
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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 13C4-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 13C4-

PFOA 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 13C4-

PFOS.

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. 
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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.

Instrument Name ETS Kirk ETS McCoy

Analysis Dates 12/28/12 and 1/28/13 1/5/13, 1/11/13, 1/31/13, 2/1/13, 

2/4/13, and 2/6/13

Analytical Method ETS-8-044.1 ETS-8-044.1

Liquid Chromatograph Agilent 1260 Agilent 1290

Guard column Betasil C18 (4.6 mm X 100 mm), 5 μ Prism RP (2.1 mm X 50 mm), 5 μ

Analytical column Betasil C18 (4.6 mm X 100 mm), 5μ Betasil C18 (2.1 mm X 100 mm), 5μ

Injection Volume 100 μL 100 μL

Mass Spectrometer Applied Biosystems API 5500 Applied Biosystems API 5500

Ion Source Turbo Spray Turbo Spray

Electrode Turbo ion electrode Turbo ion electrode

Polarity Negative Negative

Software Analyst 1.5.2 Analyst 1.5.2
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Table 7. Liquid Chromatography Conditions.

Step 

Number

Total Time 

(min)

Flow Rate 

(μL/min)

Percent A

(2mM ammonium acetate)

Percent B

(Methanol)

Analysis Dates:12/28/12 and 1/28/13

0 0.00 750 90.0 10.0

1 0.50 750 90.0 10.0

2 4.00 750 70.0 30.0

3 6.00 750 70.0 30.0

4 11.0 750 20.0 80.0

5 13.0 750 20.0 80.0

6 13.5 750 10.0 90.0

7 16.0 750 10.0 90.0

8 16.5 750 90.0 10.0

9 19.0 750 90.0 10.0

Analysis Dates: 1/5/13, 1/11/13, 1/31/13, 2/1/13, and 2/6/13

0 0.00 300 90.0 10.0

1 0.50 300 90.0 10.0

2 4.00 300 70.0 30.0

3 6.00 300 70.0 30.0

4 11.0 300 20.0 80.0

5 13.0 300 20.0 80.0

6 13.5 300 10.0 90.0

7 16.0 300 10.0 90.0

8 16.5 300 90.0 10.0

9 19.0 300 90.0 10.0

Analysis Date 2/4/13

0 0.00 300 90.0 10.0

1 0.50 300 90.0 10.0

2 4.00 300 70.0 30.0

3 6.00 300 70.0 30.0

4 6.10 300 10.0 90.0

5 8.00 300 10.0 90.0

6 8.10 300 90.0 10.0

7 10.0 300 90.0 10.0
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Table 8. Mass Transitions. 

Analyte

Mass Transition

Q1/Q3

Internal Standard Mass Transition

Q1/Q3

PFBA 213/169 [

13C4]PFBA 217/172

PFHxA

313/119

[

13C2]PFHxA 315/270

313/269

PFHpA

363/319

[

13C4]PFHpA 367/322

363/119

PFOA

413/369

[

13 413/219 C8]PFOA 421/376

413/169

PFBS

299/80

[

18O2]PFBS 303/84

299/99

PFHS

399/99

[

13C3]PFHS 402/80

399/80

PFOS

499/99

[

13 499/80 C8]PFOS 507/80

499/130

FBSA 298/78 [

18O2]PFBS 303/84

FOSA 498/78 [

13C8]FOSA 506/78

MeFOSAA

570/219

d3-MeFOSAA 

573/219

570/169 573/169

570/83 573/83

EtFOSAA

584/219

d5-EtFOSAA 

589/219

584/169 589/169

584/83 589/83

[

13C3]PFBA surrogate 216/172 [13C4]PFBA 217/172

[

13C4]PFOA surrogate 417/372 [13C8]PFOA 421/376

[

13C4]PFOS surrogate 503/80 [13C8]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 
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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 100±25% (100±30% 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. Of 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 100±25% (100±30% 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.
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Table 9. LOQ

Analyte Analysis Date LOQ, ng/L (1)

PFHxA 1/5/13 2.00 (1)

PFHpA 1/5/13 2.00 (1)

PFOA 1/5/13 1.92 (1)

PFBS 1/11/13 5.00 (1)

PFHS 12/28/12 5.00 (1)

PFOS 12/28/12 9.28 (1)

FBSA 12/28/12 2.00 (1)

FOSA 12/28/12 2.00 (1)

N-MeFOSAA 12/28/12 2.00 (1)

N-EtFOSAA 12/28/12 5.00 (1)

PFBS 1/28/13 5.00 (1)

PFOS 1/28/13 9.28 (1)

FBSA 1/28/13 2.00 (1)

FOSA 1/28/13 2.00 (1)

MeFOSAA 1/28/13 9.98 (1)

EtFOSAA 1/28/13 15.0 (1)

PFHxA 1/31/3 2.00 (1)

PFHpA 1/31/3 2.00 (1)

PFOA 1/31/3 4.80 (1)

PFOS 2/1/13 0.927

PFBA 2/4/13 5.00

PFOS 2/6/13 0.927

(1) A dilution factor of 2 was applied to the LOQ.

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 
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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 BLOQ for MeFOSAA. 

This spike level was at the LOQ and had an average recovery of 127%. 
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• 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.

* 100%

Spike Concentration

Calculated Concentration LCSPercent Recovery =

* 100%

average LCS recovery

standard deviation LCS replicates LCS% RSD =
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PAGE 25 OF 52

Table 10. Laboratory Control Spike Recovery.

ETS-8-044.1 

Analyzed 12/28/12 PFHS PFOS (Linear + Branched)

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-121227-1 5.00 <5.00 NA (1) 4.63 <9.29 NA (1)

LCS-121227-2 5.00 <5.00 NA (1) 4.63 <9.28 NA (1)

LCS-121227-3 5.00 7.41 148 4.63 <9.28 NA (1)

Average ± %RSD 148% (2) NA 

LCS-121227-4 49.8 48.9 98.2 46.1 41.9 91.0

LCS-121227-5 49.8 50.5 101 46.1 42.2 91.5

LCS-121227-6 49.8 47.9 96.1 46.1 44.8 97.2

Average ± %RSD 98.4% ± 2.5% 93.2% ± 3.7%

LCS-121227-7 99.0 94.5 95.5 91.8 93.8 102

LCS-121227-8 99.0 100 101 91.8 89.9 98.0

LCS-121227-9 99.0 99.0 100 91.8 88.9 96.9

Average ± %RSD 98.8% ± 3.0% 99.0% ± 2.7%

ETS-8-044.1 

Analyzed 12/28/12 FBSA FOSA

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-121227-1 5.00 4.81 96.1 5.00 4.46 89.3

LCS-121227-2 5.00 5.39 108 5.00 5.08 102

LCS-121227-3 5.00 5.12 102 5.00 4.30 86.0

Average ± %RSD 102% ± 5.8% 92.4% ± 9.1%

LCS-121227-4 49.8 46.8 94.0 49.8 50.7 102

LCS-121227-5 49.8 49.7 99.9 49.8 47.5 95.3

LCS-121227-6 49.8 52.0 104 49.8 49.9 100

Average ± %RSD 99.3% ± 5.1% 99.1% ± 3.5%

LCS-121227-7 99.0 94.6 95.6 99.0 99.6 101

LCS-121227-8 99.0 97.4 98.4 99.0 100 101

LCS-121227-9 99.0 100 101 99.0 103 104

Average ± %RSD 98.3% ± 2.7% 102% ± 1.7%

(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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 26 OF 52

Table 10 continued. Laboratory Control Spike Recovery.

ETS-8-044.1 

Analyzed 12/28/12 MeFOSAA EtFOSAA

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-121227-1 4.99 4.14 82.9 4.99 <5.00 NA (1)

LCS-121227-2 4.99 5.26 105 4.99 <5.00 NA (1)

LCS-121227-3 4.99 5.64 113 4.99 <5.00 NA (1)

Average ± %RSD 100% ± 16% NA

LCS-121227-4 49.7 49.8 100 49.7 46.6 93.8

LCS-121227-5 49.7 42.3 85.1 49.7 58.8 118

LCS-121227-6 49.7 55.7 112 49.7 48.3 97.3

Average ± %RSD 99.0% ± 14% 103% ± 13%

LCS-121227-7 98.8 100 101 98.8 94.8 96.0

LCS-121227-8 98.8 107 109 98.8 100 101

LCS-121227-9 98.8 106 108 98.8 101 103

Average ± %RSD 106% ± 4.1% 100% ± 3.6%

ETS-8-044.1 

Analyzed 12/28/12 13C4-PFOS

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-121227-1 9.55 <14.4 NA (1)

LCS-121227-2 9.55 <14.4 NA (1)

LCS-121227-3 9.55 <14.4 NA (1)

Average ± %RSD NA

LCS-121227-4 47.6 46.0 96.6

LCS-121227-5 47.6 50.5 106

LCS-121227-6 47.6 48.8 102

Average ± %RSD 102% ± 4.6%

LCS-121227-7 94.7 89.1 94.1

LCS-121227-8 94.7 92.7 97.9

LCS-121227-9 94.7 94.7 100

Average ± %RSD 97.3% ± 3.1%

(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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 27 OF 52

Table 10 continued. Laboratory Control Spike Recovery.

ETS-8-044.1 

Analyzed 12/28/12 PFHS PFOS (Linear + Branched)

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-121228-1 5.02 6.78 135 4.65 12.3 264 (2)

LCS-121228-2 5.02 5.23 104 4.65 <9.28 NA (1)

LCS-121228-3 5.02 5.25 105 4.65 <9.28 NA (1)

Average ± %RSD 115 ± 15% NA 

LCS-121228-4 50.0 52.2 104 46.4 44.0 94.8

LCS-121228-5 50.0 51.7 103 46.4 43.6 94.0

LCS-121228-6 50.0 51.7 103 46.4 46.4 100

Average ± %RSD 103% ± 0.56% 96.3% ± 3.4%

LCS-121228-7 99.5 98.5 99.0 92.2 85.1 92.3

LCS-121228-8 99.5 106 107 92.2 96.2 104

LCS-121228-9 99.5 98.1 98.6 92.2 96.3 104

Average ± %RSD 102% ± 4.7% 100% ± 6.7%

ETS-8-044.1 

Analyzed 12/28/12 FBSA FOSA

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-121228-1 5.02 5.28 105 5.02 5.59 111

LCS-121228-2 5.02 5.19 103 5.02 4.86 96.9

LCS-121228-3 5.02 5.05 101 5.02 5.39 107

Average ± %RSD 103% ± 1.9% 105% ± 6.9%

LCS-121228-4 50.0 47.6 95.2 50.0 50.9 102

LCS-121228-5 50.0 53.6 107 50.0 51.6 103

LCS-121228-6 50.0 48.0 96.0 50.0 50.9 102

Average ± %RSD 99.4% ± 6.6% 102% ± 0.56%

LCS-121228-7 99.5 96.9 97.4 99.5 104 105

LCS-121228-8 99.5 106 107 99.5 105 105

LCS-121228-9 99.5 97.2 97.7 99.5 102 102

Average ± %RSD 101% ± 5.4% 104% ± 1.7%

(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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 28 OF 52

Table 10 continued. Laboratory Control Spike Recovery.

ETS-8-044.1 

Analyzed 12/28/12 MeFOSAA EtFOSAA

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-121228-1 5.01 6.99 140 5.01 5.28 105

LCS-121228-2 5.01 6.40 128 5.01 <5.00 NA (1)

LCS-121228-3 5.01 3.79 75.7 5.01 <5.00 NA (1)

Average ± %RSD 115% ± 30% (2) 105%

LCS-121228-4 49.9 48.1 96.3 49.9 48.0 96.2

LCS-121228-5 49.9 50.4 101 49.9 49.6 99.5

LCS-121228-6 49.9 52.5 105 49.9 54.7 110

Average ± %RSD 101% ± 4.3% 102% ± 7.1%

LCS-121228-7 99.3 101 101 99.3 96.7 97.4

LCS-121228-8 99.3 104 104 99.3 122 122

LCS-121228-9 99.3 107 108 99.3 117 118

Average ± %RSD 104% ± 3.4% 112% ± 12%

ETS-8-044.1 

Analyzed 12/28/12 13C4-PFOS

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-121228-1 9.60 <14.4 NA (1)

LCS-121228-2 9.60 <14.4 NA (1)

LCS-121228-3 9.60 <14.4 NA (1)

Average ± %RSD NA

LCS-121228-4 47.8 47.2 98.7

LCS-121228-5 47.8 48.7 102

LCS-121228-6 47.8 48.9 102

Average ± %RSD 101% ± 1.9%

LCS-121228-7 95.1 87.4 91.9

LCS-121228-8 95.1 90.9 95.6

LCS-121228-9 95.1 90.4 95.1

Average ± %RSD 94.2% ± 2.1%

(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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 29 OF 52

Table 10 continued. Laboratory Control Spike Recovery.

ETS-8-044.1 

Analyzed 1/5/13 PFHxA PFHpA

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-121227-1 5.00 4.76 95.2 5.00 4.35 87.0

LCS-121227-2 5.00 4.77 95.4 5.00 3.04 60.9

LCS-121227-3 5.00 4.89 97.8 5.00 3.57 71.3

Average ± %RSD 96.1% ± 1.5% 73.1% ± 18% (2)

LCS-121227-4 49.8 48.1 96.6 49.8 45.6 91.5

LCS-121227-5 49.8 51.5 103 49.8 47.8 96.0

LCS-121227-6 49.8 50.5 101 49.8 52.8 106

Average ± %RSD 100% ± 3.3% 97.8% ± 7.6%

LCS-121227-7 99.0 102 103 99.0 92.5 93.4

LCS-121227-8 99.0 102 103 99.0 106 107

LCS-121227-9 99.0 101 102 99.0 102 103

Average ± %RSD 103% ± 0.56% 101% ± 6.9%

ETS-8-044.1 

Analyzed 1/5/13 PFOA (Linear + Branched) 13C4-PFOA

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-121227-1 4.79 2.97 62.0 10.0 16.9 169

LCS-121227-2 4.79 3.50 73.1 10.0 15.0 151

LCS-121227-3 4.79 2.78 57.9 10.0 15.6 157

Average ± %RSD 64.3% ± 12% (2) 159% ± 5.8% (2)

LCS-121227-4 47.7 42.5 89.0 49.7 46.3 93.1

LCS-121227-5 47.7 42.1 88.2 49.7 47.2 95.0

LCS-121227-6 47.7 42.9 89.9 49.7 47.4 95.5

Average ± %RSD 89.0% ± 0.96% 94.5% ± 1.3%

LCS-121227-7 94.9 86.5 91.2 98.8 89.1 90.1

LCS-121227-8 94.9 90.9 95.8 98.8 85.6 86.7

LCS-121227-9 94.9 90.6 95.5 98.8 90.2 91.3

Average ± %RSD 94.2% ± 2.7% 89.4% ± 2.7%

(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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 30 OF 52

Table 10 continued. Laboratory Control Spike Recovery.

ETS-8-044.1 

Analyzed 1/5/13 PFHxA PFHpA

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-121228-1 5.02 6.38 127 5.02 4.72 94.0

LCS-121228-2 5.02 6.75 134 5.02 4.42 88.1

LCS-121228-3 5.02 5.01 99.8 5.02 4.78 95.3

Average ± %RSD 120% ± 15% 92.5% ± 4.1%

LCS-121228-4 50.0 55.3 111 50.0 46.4 92.7

LCS-121228-5 50.0 54.3 109 50.0 50.6 101

LCS-121228-6 50.0 54.9 110 50.0 51.7 103

Average ± %RSD 110% ± 0.91% 98.9% ± 5.5%

LCS-121228-7 99.5 110 110 99.5 103 104

LCS-121228-8 99.5 106 107 99.5 108 108

LCS-121228-9 99.5 99.5 100 99.5 95.2 95.6

Average ± %RSD 106% ± 4.9% 103% ± 6.2%

ETS-8-044.1 

Analyzed 1/5/13 PFOA (Linear + Branched) 13C4-PFOA

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-121228-1 4.81 4.98 104 10.0 <15.0 NA (1)

LCS-121228-2 4.81 4.09 85.0 10.0 <15.0 NA (1)

LCS-121228-3 4.81 4.55 94.5 10.0 <15.0 NA (1)

Average ± %RSD 94.5% ± 10% NA

LCS-121228-4 47.9 43.9 91.6 49.9 46.1 92.3

LCS-121228-5 47.9 46.5 97.2 49.9 47.4 94.9

LCS-121228-6 47.9 47.0 98.1 49.9 46.4 93.0

Average ± %RSD 95.6% ± 03.7% 93.4% ± 1.4%

LCS-121228-7 95.3 92.1 96.7 99.3 86.9 87.5

LCS-121228-8 95.3 99.2 104 99.3 85.0 85.6

LCS-121228-9 95.3 90.7 95.1 99.3 86.4 87.0

Average ± %RSD 98.6% ± 4.8% 86.7% ± 1.1%

(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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 31 OF 52

Table 10 continued. Laboratory Control Spike Recovery.

ETS-8-044.1 

Analyzed 1/11/13 PFBS

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-121227-1 5.00 10.7 215

LCS-121227-2 5.00 10.3 205

LCS-121227-3 5.00 10.2 205

Average ± %RSD 208% ± 2.8% (2)

LCS-121227-4 49.8 47.5 95.5

LCS-121227-5 49.8 50.0 100

LCS-121227-6 49.8 51.1 103

Average ± %RSD 99.5% ± 3.8%

LCS-121227-7 99.0 97.0 98.0

LCS-121227-8 99.0 99.9 101

LCS-121227-9 99.0 98.2 99.2

Average ± %RSD 99.4% ± 1.5%

ETS-8-044.1 

Analyzed 1/11/13 PFBS

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-121228-1 5.02 9.77 195

LCS-121228-2 5.02 10.3 205

LCS-121228-3 5.02 9.88 197

Average ± %RSD 199% ± 2.7% (2)

LCS-121228-4 50.0 48.9 97.8

LCS-121228-5 50.0 50.4 101

LCS-121228-6 50.0 49.9 99.8

Average ± %RSD 99.5% ± 1.6%

LCS-121228-7 99.5 98.6 99.1

LCS-121228-8 99.5 102 102

LCS-121228-9 99.5 100 101

Average ± %RSD 101% ± 1.5%

(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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 32 OF 52

Table 10 continued. Laboratory Control Spike Recovery.

ETS-8-044.1 

Analyzed 1/28/13 PFBS

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-130130-1 5.00 5.12 102

LCS-130130-2 5.00 5.44 109

LCS-130130-3 5.00 4.70 93.9

Average ± %RSD 102% ± 7.4%

LCS-130128-7 49.8 52.2 105

LCS-130128-8 49.8 53.1 107

LCS-130128-9 49.8 52.9 106

Average ± %RSD 106% ± 0.94%

LCS-130128-10 503 489 97.3

LCS-130128-11 503 508 101

LCS-130128-12 503 537 107

Average ± %RSD 102% ± 4.8%

ETS-8-044.1 

Analyzed 1/28/13 PFOS (Linear + Branched) 13C4-PFOS

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-130128-1 4.61 3.99 86.6 NA NA NA

LCS-130128-2 4.61 3.39 73.5 NA NA NA

LCS-130128-3 4.61 4.22 91.5 NA NA NA

Average ± %RSD 83.9% ± 11% NA

LCS-130128-4 9.21 9.91 108 19.0 19.8 104

LCS-130128-5 9.21 9.59 104 19.0 18.8 98.9

LCS-130128-6 9.21 9.13 99.1 19.0 20.3 107

Average ± %RSD 104% ± 4.3% 103% ± 4.0%

LCS-130128-7 46.1 45.7 99.2 95.1 86.5 90.9

LCS-130128-8 46.1 48.6 105 95.1 87.6 92.1

LCS-130128-9 46.1 50.7 110 95.1 89.9 94.6

Average ± %RSD 105% ± 5.2% 92.5% ± 2.0%

LCS-130128-10 466 474 102 NA NA NA

LCS-130128-11 466 494 106 NA NA NA

LCS-130128-12 466 519 111 NA NA NA

Average ± %RSD 106% ± 4.2% 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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 33 OF 52

Table 10 continued. Laboratory Control Spike Recovery.

ETS-8-044.1 

Analyzed 1/28/13 FBSA FOSA

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-130128-1 4.98 4.76 95.5 4.98 5.11 103

LCS-130128-2 4.98 4.90 89.7 4.98 4.47 89.7

LCS-130128-3 4.98 4.69 102 4.98 5.10 102

Average ± %RSD 95.7% ± 6.4% 98.2% ± 7.5%

LCS-130128-4 9.93 9.99 101 9.93 10.3 104

LCS-130128-5 9.93 9.07 105.0 9.93 10.5 105

LCS-130128-6 9.93 9.87 104 9.93 10.3 104

Average ± %RSD 103% ± 2.0% 104% ± 0.55%

LCS-130128-7 49.8 50.6 102 49.8 52.5 105

LCS-130128-8 49.8 54.2 101 49.8 50.1 101

LCS-130128-9 49.8 53.0 109 49.8 54.4 109

Average ± %RSD 104% ± 4.2% 105% ± 3.8%

LCS-130128-10 503 508 101 503 498 99.0

LCS-130128-11 503 530 106 503 535 106

LCS-130128-12 503 541 112 503 561 112

Average ± %RSD 106% ± 5.2% 106% ± 6.2%

ETS-8-044.1 

Analyzed 1/28/13 MeFOSAA EtFOSAA

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-130128-1 4.97 <9.98 NA (1) 4.97 <15.0 NA (1)

LCS-130128-2 4.97 <9.98 NA (1) 4.97 <15.0 NA (1)

LCS-130128-3 4.97 <9.98 NA (1) 4.97 <15.0 NA (1)

Average ± %RSD NA NA

LCS-130128-4 9.91 12.0 121 9.91 <15.0 NA (1)

LCS-130128-5 9.91 <9.98 NA (1) 9.91 <15.0 NA (1)

LCS-130128-6 9.91 13.1 132 9.91 <15.0 NA (1)

Average ± %RPD 127% ± 8.8% (2) NA

LCS-130128-7 49.7 45.7 92.0 49.7 45.6 91.7

LCS-130128-8 49.7 54.3 109 49.7 50.7 102

LCS-130128-9 49.7 50.6 102 49.7 44.3 89.2

Average ± %RSD 101% ± 8.5% 94.3% ± 7.2%

LCS-130128-10 502 645 128 502 527 105

LCS-130128-11 502 533 106 502 575 115

LCS-130128-12 502 610 122 502 563 112

Average ± %RSD 119% ± 9.6% 111% ± 4.6%

(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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 34 OF 52

Table 10 continued. Laboratory Control Spike Recovery.

ETS-8-044.1 

Analyzed 1/31/13 PFHxA PFHpA

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-130128-1 4.98 4.01 80.5 4.98 4.71 94.5

LCS-130128-2 4.98 4.97 99.8 4.98 5.71 115

LCS-130128-3 4.98 4.46 89.5 4.98 5.32 107

Average ± %RSD 89.9% ± 11% 106% ± 9.8%

LCS-130128-4 9.93 8.14 82.0 9.93 10.7 108

LCS-130128-5 9.93 9.77 98.4 9.93 9.20 92.7

LCS-130128-6 9.93 8.76 88.2 9.93 10.5 105

Average ± %RSD 89.5% ± 9.2% 102% ± 8.0%

LCS-130128-7 49.8 46.9 94.2 49.8 44.8 90.0

LCS-130128-8 49.8 52.1 105 49.8 49.9 100

LCS-130128-9 49.8 49.2 98.7 49.8 48.4 97.2

Average ± %RSD 99.3% ± 5.5% 95.7% ± 5.4%

LCS-130128-10 503 547 109 503 504 100

LCS-130128-11 503 518 103 503 575 114

LCS-130128-12 503 555 110 503 569 113

Average ± %RSD 107% ± 3.5% 109% ± 7.2%

ETS-8-044.1 

Analyzed 1/31/13 PFOA (Linear + Branched) 13C4-PFOA

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-130128-1 4.77 <4.80 NA (1) NA NA NA

LCS-130128-2 4.77 <4.80 NA (1) NA NA NA

LCS-130128-3 4.77 <4.80 NA (1) NA NA NA

Average ± %RSD NA NA

LCS-130128-4 9.51 9.62 101 19.8 19.7 99.7

LCS-130128-5 9.51 9.64 101 19.8 21.8 110

LCS-130128-6 9.51 9.07 95.3 19.8 21.1 107

Average ± %RPD 99.1% ± 3.3% 106% ± 5.0%

LCS-130128-7 47.7 46.2 96.9 99.3 91.1 91.7

LCS-130128-8 47.7 49.1 103 99.3 94.3 95.0

LCS-130128-9 47.7 48.2 101 99.3 94.1 94.8

Average ± %RSD 100% ± 3.1% 93.8% ± 2.0%

LCS-130128-10 481 489 102 NA NA NA

LCS-130128-11 481 516 107 NA NA NA

LCS-130128-12 481 516 107 NA NA NA

Average ± %RSD 105% ± 2.7% 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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 35 OF 52

Table 10 continued. Laboratory Control Spike Recovery.

ETS-8-044.1 

Analyzed 2/1/13 PFOS (Linear + Branched) 13C4-PFOS

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-130201-1 4.64 4.38 94.5 NA NA NA

LCS-130201-2 4.64 4.63 99.8 NA NA NA

LCS-130201-3 4.64 4.72 102 NA NA NA

Average ± %RSD 98.8% ± 3.9% NA

LCS-130201-4 9.30 8.46 90.9 19.2 18.6 96.6

LCS-130201-5 9.30 8.47 91.1 19.2 19.5 101

LCS-130201-6 9.30 8.91 95.8 19.2 20.2 105

Average ± %RSD 92.6% ± 3.0% 101% ± 4.2%

LCS-130201-7 46.4 44.3 95.4 NA NA NA

LCS-130201-8 46.4 45.7 98.5 NA NA NA

LCS-130201-9 46.4 46.5 100 NA NA NA

Average ± %RSD 98.0% ± 2.4% NA

LCS-130201-10 92.2 90.0 97.6 95.1 93.8 98.7

LCS-130201-11 92.2 91.7 99.5 95.1 95.2 100

LCS-130201-12 92.2 90.4 98.0 95.1 97.0 102

Average ± %RSD 98.4% ± 1.0% 100% ± 1.7%

ETS-8-044.1 

Analyzed 2/4/13 PFBA 13C3-PFBA

Lab ID

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

Spiked 

Concentration 

(ng/L)

Calculated 

Concentration 

(ng/L) %Recovery

LCS-130201-1 5.00 4.08 81.7 NA NA NA

LCS-130201-2 5.00 5.22 104 NA NA NA

LCS-130201-3 5.00 5.07 101 NA NA NA

Average ± %RSD 95.6% ± 13% NA

LCS-130201-4 10.0 9.99 99.9 20.0 19.8 98.9

LCS-130201-5 10.0 8.72 87.2 20.0 20.2 101

LCS-130201-6 10.0 9.17 91.7 20.0 21.0 105

Average ± %RSD 92.9% ± 6.9% 102% ± 3.0%

LCS-130201-7 50.0 48.9 97.8 NA NA NA

LCS-130201-8 50.0 47.9 95.8 NA NA NA

LCS-130201-9 50.0 47.1 94.3 NA NA NA

Average ± %RSD 96.0% ± 1.8% NA

LCS-130201-10 99.5 100 101 99.1 98.2 99.1

LCS-130201-11 99.5 100 100 99.1 99.4 100

LCS-130201-12 99.5 99.7 100 99.1 103 104

Average ± %RSD 100% ± 0.58% 101% ± 2.6%

(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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 36 OF 52

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 

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 

100±30% 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 100±30% 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.

Analyte Standard Deviation Method Uncertainty

PFBA 8.14 ±16%

PFHxA 10.1 ±20%

PFHpA 10.6 ±21%

PFOA 11.6 ±23%

PFBS 10.0 ±20%

PFHS 12.4 ±25%

PFOS 8.50 ±17%

FBSA 8.38 ±17%

FOSA 6.79 ±14%

MeFOSAA 12.6 ±25%

EtFOSAA 8.47 ±17%

13C3-PFBA 9.07 ±18%

13C4-PFOA 8.04 ±16%

13C4-PFOS 7.88 ±16%
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 37 OF 52

Table 12. Field Matrix Spike Level.

Final Concentration (ng/L) (1)

Description PFBA PFHxA PFHpA PFOA PFBS PFHS PFOS FBSA FOSA MeFOSAA EtFOSAA

FMS 100 100 100 95.8 100 100 92.7 100 100 99.8 99.8

(1) Location DAL-SW-T707 was overfilled by 10% (220 mL). The FMS true values were adjusted accordingly.

*100%

Spike Concentration

(SampleConcentration of FMS Average Concentration : FieldSample& FieldSample Dup.) FMSRecovery − =

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%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 38 OF 52

Table 13. DAL SW R02L3

PFBA PFHxA PFHpA PFOA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-012 DAL-SW-R02L3-0-121116 6.13 NA 4.83 NA 4.70 NA 9.28 NA

ISO12-01-01-03-013 DAL-SW-R02L3-DUP-121116 6.10 NA 3.61 NA 3.78 NA 9.12 NA

ISO12-01-01-03-014 DAL-SW-R02L3-FMS-121116 100 93.9 111 107 103 98.8 101 95.8

Average Concentration (ng/L) ± %RPD 6.12 ng/L ± 0.49% 4.22 ng/L ± 29% (1) 4.24 ng/L ± 22% (1) 9.20 ng/L ± 1.7%

PFBS PFHS PFOS FBSA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-012 DAL-SW-R02L3-0-121116 <5.00 NA <5.00 NA 8.94 NA <2.00 NA

ISO12-01-01-03-013 DAL-SW-R02L3-DUP-121116 <5.00 NA <5.00 NA 8.46 NA <2.00 NA

ISO12-01-01-03-014 DAL-SW-R02L3-FMS-121116 102 102 99.7 99.7 94.7 92.8 95.5 95.5

Average Concentration (ng/L) ± %RPD <5.00 ng/L <5.00 ng/L 8.70 ng/L ± 5.5% <2.00 ng/L

FOSA MeFOSAA EtFOSAA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-012 DAL-SW-R02L3-0-121116 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-013 DAL-SW-R02L3-DUP-121116 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-014 DAL-SW-R02L3-FMS-121116 101 101 95.1 95.3 94.2 94.4

Average Concentration (ng/L) ± %RPD/%RSD <2.00 ng/L <2.00 ng/L <5.00 ng/L

NA = Not Applicable

(1) The sample / sample duplicate RPD did not meet method acceptance criteria of ≤20%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 39 OF 52

Table 14. DAL SW R05L1

PFBA PFHxA PFHpA PFOA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-052 DAL-SW-R05L1-0-121119 58.9 NA 72.5 NA 56.8 NA 246 NA

ISO12-01-01-03-053 DAL-SW-R05L1-DUP-121119 58.3 NA 70.5 NA 59.0 NA 242 NA

ISO12-01-01-03-054 DAL-SW-R05L1-FMS-121119 163 104 176 105 178 120 353 NC

Average Concentration (ng/L) ± %RPD 58.6 ng/L ± 1.0% 71.5 ng/L ± 2.8% 57.9 ng/L ± 3.8% 244 ng/L ± 1.6%

PFBS PFHS PFOS FBSA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-052 DAL-SW-R05L1-0-121119 124 NA 39.8 NA 385 NA 1130 NA

ISO12-01-01-03-053 DAL-SW-R05L1-DUP-121119 116 NA 42.3 NA 405 NA 1050 NA

ISO12-01-01-03-054 DAL-SW-R05L1-FMS-121119 233 113 137 96.0 543 NC 1260 NC

Average Concentration (ng/L) ± %RPD 120 ng/L ± 6.7% 41.1 ng/L ± 6.1% 395 ng/L ± 5.1% 1090 ng/L ± 7.3%

FOSA MeFOSAA EtFOSAA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-052 DAL-SW-R05L1-0-121119 21.1 NA 10.0 NA 18.0 NA

ISO12-01-01-03-053 DAL-SW-R05L1-DUP-121119 18.0 NA 8.20 NA 17.8 NA

ISO12-01-01-03-054 DAL-SW-R05L1-FMS-121119 116 96.5 99.0 90.1 113 95.3

Average Concentration (ng/L) ± %RPD/%RSD 19.6 ng/L ± 16% 9.10 ng/L ± 20% 17.9 ng/L ± 1.1%

NA = Not Applicable

NC = Not Calculated; the endogenous sample concentration was greater than 2x the spike level.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 40 OF 52

Table 15. DAL SW R10L3

PFBA PFHxA PFHpA PFOA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-040 DAL-SW-R10L3-0-121119 <5.00 NA 2.73 NA <2.00 NA 3.52 NA

ISO12-01-01-03-041 DAL-SW- R10L3-DUP-121119 <5.00 NA <2.00 NA <2.00 NA 3.50 NA

ISO12-01-01-03-042 DAL-SW- R10L3-FMS-121119 95.9 95.9 102 99.3 94.5 94.5 90.1 90.4

Average Concentration (ng/L) ± %RPD <5.00 ng/L 2.73 ng/L <2.00 ng/L 3.52 ng/L ± 0.57%

PFBS PFHS PFOS FBSA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-040 DAL-SW-R10L3-0-121119 <5.00 NA <5.00 NA 6.49 NA <2.00 NA

ISO12-01-01-03-041 DAL-SW- R10L3-DUP-121119 <5.00 NA <5.00 NA 6.63 NA <2.00 NA

ISO12-01-01-03-042 DAL-SW- R10L3-FMS-121119 97.6 97.6 91.2 91.2 92.5 92.7 94.8 94.8

Average Concentration (ng/L) ± %RPD <5.00 ng/L <5.00 ng/L 6.56 ng/L ± 2.1% <2.00 ng/L

FOSA MeFOSAA EtFOSAA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-040 DAL-SW-R10L3-0-121119 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-041 DAL-SW- R10L3-DUP-121119 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-042 DAL-SW- R10L3-FMS-121119 99.6 99.6 91.9 92.1 93.6 93.8

Average Concentration (ng/L) ± %RPD/%RSD <2.00 ng/L <2.00 ng/L <5.00 ng/L

NA = Not Applicable

NC = Not Calculated; the endogenous sample concentration was greater than 2x the spike level.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 41 OF 52

Table 16. DAL SW R15L1

PFBA PFHxA PFHpA PFOA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-024 DAL-SW-R15L1-0-121117 7.92 NA 4.24 NA 2.34 NA 11.5 NA

ISO12-01-01-03-025 DAL-SW- R15L1-DUP-121117 6.62 NA 4.71 NA <2.00 NA 10.9 NA

ISO12-01-01-03-026 DAL-SW- R15L1-FMS-121117 98.9 91.6 108 104 106 104 100 92.6

Average Concentration (ng/L) ± %RPD 7.27 ng/L ± 18% 4.48 ng/L ± 11% 2.34 ng/L 11.2 ng/L ± 5.4%

PFBS PFHS PFOS FBSA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-024 DAL-SW-R15L1-0-121117 14.8 NA <5.00 NA 19.9 NA 34.8 NA

ISO12-01-01-03-025 DAL-SW- R15L1-DUP-121117 13.7 NA <5.00 NA 18.9 NA 31.8 NA

ISO12-01-01-03-026 DAL-SW- R15L1-FMS-121117 109 94.8 95.5 95.5 113 101 118 84.7

Average Concentration (ng/L) ± %RPD 14.3 ng/L ± 7.7% <5.00 ng/L 19.4 ng/L ± 5.2% 33.3 ng/L ± 9.0%

FOSA MeFOSAA EtFOSAA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-024 DAL-SW-R15L1-0-121117 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-025 DAL-SW- R15L1-DUP-121117 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-026 DAL-SW- R15L1-FMS-121117 101 101 85.9 86.1 69.4 69.5 (1)

Average Concentration (ng/L) ± %RPD/%RSD <2.00 ng/L <2.00 ng/L <5.00 ng/L

NA = Not Applicable

(1) The field matrix spike recovery did not meet method acceptance criteria of 100 ± 30%
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 42 OF 52

Table 17. DAL SW T101

PFBA PFHxA PFHpA PFOA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-062 DAL-SW-T101-0-121203 <5.00 NA <2.00 NA <2.00 NA <1.92 NA

ISO12-01-01-03-063 DAL-SW-T101-DB-121203 <5.00 NA <2.00 NA <2.00 NA <1.92 NA

ISO12-01-01-03-064 DAL-SW-T101-FMS-121203 94.4 94.4 107 107 97.2 97.2 90.0 93.9

Average Concentration (ng/L) ± %RPD <5.00 ng/L <2.00 ng/L <2.00 ng/L <1.92 ng/L

PFBS PFHS PFOS FBSA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-062 DAL-SW-T101-0-121203 <5.00 NA <5.00 NA 6.13 NA <2.00 NA

ISO12-01-01-03-063 DAL-SW-T101-DB-121203 <5.00 NA <5.00 NA 6.36 NA <2.00 NA

ISO12-01-01-03-064 DAL-SW-T101-FMS-121203 96.1 96.1 93.3 93.3 91.1 91.5 87.7 87.7

Average Concentration (ng/L) ± %RPD <5.00 ng/L <5.00 ng/L 6.25 ng/L ± 3.7% <2.00 ng/L

FOSA MeFOSAA EtFOSAA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-062 DAL-SW-T101-0-121203 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-063 DAL-SW-T101-DB-121203 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-064 DAL-SW-T101-FMS-121203 98.3 98.3 99.9 100 94.7 94.9

Average Concentration (ng/L) ± %RPD/%RSD <2.00 ng/L <2.00 ng/L <5.00 ng/L

NA = Not Applicable
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 43 OF 52

Table 18. DAL SW T202

PFBA PFHxA PFHpA PFOA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-075 DAL-SW-T202-0-121203 6.72 NA 5.16 NA 4.80 NA 12.6 NA

ISO12-01-01-03-076 DAL-SW-T202-DB-121203 5.50 NA 4.58 NA 3.64 NA 10.7 NA

ISO12-01-01-03-077 DAL-SW-T202-FMS-121203 97.3 90.6 103 98.1 103 98.8 106 98.5

Average Concentration (ng/L) ± %RPD 6.72 ng/L ± 18% 4.87 ng/L ± 5.4% 4.22 ng/L ± 27% (1) 11.7 ng/L ± 16%

PFBS PFHS PFOS FBSA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-075 DAL-SW-T202-0-121203 <5.00 NA <5.00 NA 9.93 NA <2.00 NA

ISO12-01-01-03-076 DAL-SW-T202-DB-121203 <5.00 NA <5.00 NA 9.43 NA <2.00 NA

ISO12-01-01-03-077 DAL-SW-T202-FMS-121203 99.4 99.4 94.6 94.6 88.7 85.2 91.6 91.6

Average Concentration (ng/L) ± %RPD <5.00 ng/L <5.00 ng/L 9.68 ng/L ± 5.2% <2.00 ng/L

FOSA MeFOSAA EtFOSAA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-075 DAL-SW-T202-0-121203 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-076 DAL-SW-T202-DB-121203 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-077 DAL-SW-T202-FMS-121203 94.8 94.8 102 102 96.2 96.4

Average Concentration (ng/L) ± %RPD/%RSD <2.00 ng/L <2.00 ng/L <5.00 ng/L

NA = Not Applicable

(1) The sample / sample duplicate RPD did not meet method acceptance criteria of ≤20%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 44 OF 52

Table 19. DAL SW T303

PFBA PFHxA PFHpA PFOA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-088 DAL-SW-T303-0-121203 <5.00 NA <2.00 NA <2.00 NA 2.78 NA

ISO12-01-01-03-089 DAL-SW-T303-DB-121203 <5.00 NA <2.00 NA <2.00 NA 2.29 NA

ISO12-01-01-03-090 DAL-SW-T303-FMS-121203 97.1 97.1 106 106 97.9 97.9 91.3 92.7

Average Concentration (ng/L) ± %RPD <5.00 ng/L <2.00 ng/L <2.00 ng/L 2.54 ng/L ± 19%

PFBS PFHS PFOS FBSA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-088 DAL-SW-T303-0-121203 <5.00 NA <5.00 NA 6.94 NA <2.00 NA

ISO12-01-01-03-089 DAL-SW-T303-DB-121203 <5.00 NA <5.00 NA 7.51 NA <2.00 NA

ISO12-01-01-03-090 DAL-SW-T303-FMS-121203 98.0 98.0 94.9 94.9 92.9 92.4 93.2 93.2

Average Concentration (ng/L) ± %RPD <5.00 ng/L <5.00 ng/L 7.23 ng/L ± 7.9% <2.00 ng/L

FOSA MeFOSAA EtFOSAA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-088 DAL-SW-T303-0-121203 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-089 DAL-SW-T303-DB-121203 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-090 DAL-SW-T303-FMS-121203 100 100 102 102 102 102

Average Concentration (ng/L) ± %RPD/%RSD <2.00 ng/L <2.00 ng/L <5.00 ng/L

NA = Not Applicable
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 45 OF 52

Table 20. DAL SW T404

PFBA PFHxA PFHpA PFOA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-101 DAL-SW-T404-0-121203 <5.00 NA <2.00 NA <2.00 NA 2.25 NA

ISO12-01-01-03-102 DAL-SW-T404-DB-121203 <5.00 NA <2.00 NA <2.00 NA <1.92 NA

ISO12-01-01-03-103 DAL-SW-T404-FMS-121203 94.7 94.7 106 106 102 102 89.9 91.5

Average Concentration (ng/L) ± %RPD <5.00 ng/L <2.00 ng/L <2.00 ng/L 2.25 ng/L

PFBS PFHS PFOS FBSA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-101 DAL-SW-T404-0-121203 <5.00 NA <5.00 NA 7.29 NA <2.00 NA

ISO12-01-01-03-102 DAL-SW-T404-DB-121203 <5.00 NA <5.00 NA 8.46 NA <2.00 NA

ISO12-01-01-03-103 DAL-SW-T404-FMS-121203 95.0 95.0 94.7 94.7 92.9 91.7 91.0 91.0

Average Concentration (ng/L) ± %RPD <5.00 ng/L <5.00 ng/L 7.88 ng/L ± 15% <2.00 ng/L

FOSA MeFOSAA EtFOSAA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-101 DAL-SW-T404-0-121203 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-102 DAL-SW-T404-DB-121203 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-103 DAL-SW-T404-FMS-121203 102 102 97.4 97.6 92.1 92.3

Average Concentration (ng/L) ± %RPD/%RSD <2.00 ng/L <2.00 ng/L <5.00 ng/L

NA = Not Applicable
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 46 OF 52

Table 21. DAL SW T505

PFBA PFHxA PFHpA PFOA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-114 DAL-SW-T505-0-121204 <5.00 NA <2.00 NA <2.00 NA 2.52 NA

ISO12-01-01-03-115 DAL-SW-T505-DB-121204 5.48 NA <2.00 NA <2.00 NA 3.01 NA

ISO12-01-01-03-116 DAL-SW-T505-FMS-121204 96.7 91.2 109 109 103 103 92.8 94.0

Average Concentration (ng/L) ± %RPD 5.48 ng/L <2.00 ng/L <2.00 ng/L 2.77 ng/L ± 18%

PFBS PFHS PFOS FBSA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-114 DAL-SW-T505-0-121204 <5.00 NA <5.00 NA 7.20 NA <2.00 NA

ISO12-01-01-03-115 DAL-SW-T505-DB-121204 <5.00 NA <5.00 NA 6.78 NA <2.00 NA

ISO12-01-01-03-116 DAL-SW-T505-FMS-121204 98.5 98.5 96.3 96.3 93.7 93.5 88.4 88.4

Average Concentration (ng/L) ± %RPD <5.00 ng/L <5.00 ng/L 6.99 ng/L ± 6.0% <2.00 ng/L

FOSA MeFOSAA EtFOSAA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-114 DAL-SW-T505-0-121204 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-115 DAL-SW-T505-DB-121204 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-116 DAL-SW-T505-FMS-121204 97.9 97.9 92.6 92.8 99.6 99.8

Average Concentration (ng/L) ± %RPD/%RSD <2.00 ng/L <2.00 ng/L <5.00 ng/L

NA = Not Applicable
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 47 OF 52

Table 22. DAL SW T606

PFBA PFHxA PFHpA PFOA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-127 DAL-SW-T606-0-121204 <5.00 NA 2.31 NA <2.00 NA 4.38 NA

ISO12-01-01-03-128 DAL-SW-T606-DB-121204 <5.00 NA 2.41 NA <2.00 NA 3.41 NA

ISO12-01-01-03-129 DAL-SW-T606-FMS-121204 96.6 96.6 110 108 102 102 92.2 92.2

Average Concentration (ng/L) ± %RPD <5.00 ng/L 2.36 ng/L ± 4.2% <2.00 ng/L 3.90 ng/L ± 25% (1)

PFBS PFHS PFOS FBSA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-127 DAL-SW-T606-0-121204 <5.00 NA <5.00 NA 9.72 NA 2.22 NA

ISO12-01-01-03-128 DAL-SW-T606-DB-121204 <5.00 NA <5.00 NA 11.1 NA 2.18 NA

ISO12-01-01-03-129 DAL-SW-T606-FMS-121204 97.9 97.9 97.1 97.1 96.5 92.9 91.0 88.8

Average Concentration (ng/L) ± %RPD <5.00 ng/L <5.00 ng/L 10.4 ng/L ± 13% 2.20 ng/L ± 1.8%

FOSA MeFOSAA EtFOSAA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-127 DAL-SW-T606-0-121204 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-128 DAL-SW-T606-DB-121204 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-129 DAL-SW-T606-FMS-121204 98.6 98.6 92.4 92.6 96.5 96.7

Average Concentration (ng/L) ± %RPD/%RSD <2.00 ng/L <2.00 ng/L <5.00 ng/L

NA = Not Applicable

(1) The sample / sample duplicate RPD did not meet method acceptance criteria of ≤20%.
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 48 OF 52

Table 23. DAL SW T707

PFBA PFHxA PFHpA PFOA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-140 DAL-SW-T707-0-121204 8.42 NA 4.05 NA 3.24 NA 12.5 NA

ISO12-01-01-03-141 DAL-SW-T707-DB-121204 7.66 NA 4.53 NA 3.77 NA 11.9 NA

ISO12-01-01-03-142 DAL-SW-T707-FMS-121204 89.5 81.5 99.0 104 88.3 93.3 97.3 97.7

Average Concentration (ng/L) ± %RPD 8.04 ng/L ± 9.5% 4.29 ng/L ± 11% 3.51 ng/L ± 15% 12.2 ng/L ± 4.9%

PFBS PFHS PFOS FBSA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-140 DAL-SW-T707-0-121204 19.0 NA <5.00 NA 20.2 NA 27.6 NA

ISO12-01-01-03-141 DAL-SW-T707-DB-121204 21.0 NA <5.00 NA 19.3 NA 26.4 NA

ISO12-01-01-03-142 DAL-SW-T707-FMS-121204 105 93.5 90.0 99.0 107 104 109 90.2

Average Concentration (ng/L) ± %RPD 20.0 ng/L ± 10% <5.00 ng/L 19.8 ng/L ± 4.6% 27.0 ng/L ± 4.4%

FOSA MeFOSAA EtFOSAA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-140 DAL-SW-T707-0-121204 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-141 DAL-SW-T707-DB-121204 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-142 DAL-SW-T707-FMS-121204 97.2 107 81.9 90.3 81.0 89.3

Average Concentration (ng/L) ± %RPD/%RSD <2.00 ng/L <2.00 ng/L <5.00 ng/L

NA = Not Applicable
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 49 OF 52

Table 24. DAL SW T808

PFBA PFHxA PFHpA PFOA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-153 DAL-SW-T808-0-121205 6.28 NA 4.51 NA <2.00 NA 7.49 NA

ISO12-01-01-03-154 DAL-SW-T808-DB-121205 6.89 NA 3.85 NA <2.00 NA 6.79 NA

ISO12-01-01-03-155 DAL-SW-T808-FMS-121205 96.0 89.4 112 108 106 106 96.9 93.7

Average Concentration (ng/L) ± %RPD 6.59 ng/L ± 9.3% 4.18 ng/L ± 16% <2.00 ng/L 7.14 ng/L ± 9.8%

PFBS PFHS PFOS FBSA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-153 DAL-SW-T808-0-121205 11.2 NA <5.00 NA 13.3 NA 25.7 NA

ISO12-01-01-03-154 DAL-SW-T808-DB-121205 10.9 NA <5.00 NA 14.3 NA 25.7 NA

ISO12-01-01-03-155 DAL-SW-T808-FMS-121205 109 98.0 94.4 94.4 101 94.1 107 81.3

Average Concentration (ng/L) ± %RPD 11.1 ng/L ± 2.7% <5.00 ng/L 13.8 ng/L ± 7.2% 25.7 ng/L ± 0.0%

FOSA MeFOSAA EtFOSAA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-153 DAL-SW-T808-0-121205 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-154 DAL-SW-T808-DB-121205 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-155 DAL-SW-T808-FMS-121205 102 102 89.9 90.1 89.4 89.6

Average Concentration (ng/L) ± %RPD/%RSD <2.00 ng/L <2.00 ng/L <5.00 ng/L

NA = Not Applicable
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 50 OF 52

Table 25. DAL SW T909

PFBA PFHxA PFHpA PFOA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-166 DAL-SW-T909-0-121205 8.66 NA 7.12 NA 3.37 NA 11.6 NA

ISO12-01-01-03-167 DAL-SW-T909-DB-121205 8.97 NA 6.28 NA 3.75 NA 10.9 NA

ISO12-01-01-03-168 DAL-SW-T909-FMS-121205 99.5 90.7 110 103 109 105 108 101

Average Concentration (ng/L) ± %RPD 8.82 ng/L ± 3.5% 6.70 ng/L ± 13% 3.56 ng/L ± 11% 11.3 ng/L ± 6.2%

PFBS PFHS PFOS FBSA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-166 DAL-SW-T909-0-121205 12.8 NA <5.00 NA 19.2 NA 46.3 NA

ISO12-01-01-03-167 DAL-SW-T909-DB-121205 14.0 NA <5.00 NA 19.4 NA 45.6 NA

ISO12-01-01-03-168 DAL-SW-T909-FMS-121205 112 98.6 97.1 97.1 117 105 125 79.1

Average Concentration (ng/L) ± %RPD 13.4 ng/L ± 9.0% <5.00 ng/L 19.3 ng/L ± 1.0% 46.0 ng/L ± 1.5%

FOSA MeFOSAA EtFOSAA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-166 DAL-SW-T909-0-121205 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-167 DAL-SW-T909-DB-121205 <2.00 NA <2.00 NA <5.00 NA

ISO12-01-01-03-168 DAL-SW-T909-FMS-121205 94.4 94.4 90.8 91.0 98.8 99.0

Average Concentration (ng/L) ± %RPD/%RSD <2.00 ng/L <2.00 ng/L <5.00 ng/L

NA = Not Applicable
3M Environmental Laboratory

Report No. ISO12-01-01-03

PAGE 51 OF 52

Table 26. DAL SW TRIP BLANK 

PFBA PFHxA PFHpA PFOA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-061 DAL-SW-TRIP02-0-121116 (1) 92.5 92.5 104 104 95.0 95.0 95.4 99.6

ISO12-01-01-03-171 DAL-SW-TRIP-01-FMS-121203 90.1 90.1 112 112 94.3 94.3 94.2 98.3

PFBS PFHS PFOS FBSA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-061 DAL-SW-TRIP02-0-121116 (1) 99.3 99.3 97.4 97.4 89.7 96.8 97.6 97.6

ISO12-01-01-03-171 DAL-SW-TRIP-01-FMS-121203 97.9 97.9 93.3 93.3 84.1 90.7 102 102

FOSA MeFOSAA EtFOSAA

3M LIMS ID Description

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

Concentration 

(ng/L) %Recovery

ISO12-01-01-03-061 DAL-SW-TRIP02-0-121116 (1) 97.6 97.6 92.3 92.5 97.2 97.4

ISO12-01-01-03-171 DAL-SW-TRIP-01-FMS-121203 102 102 99.5 99.7 99.1 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.
3M Environmental Laboratory 

Report No. ISO12-01-01-03 

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 SM 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. 

7 Signatures 

Susan Wolf, 3M Prin^ipfel Analytical Investigator Date 

/ 8 /=^S' ^o/j> 

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 Date 

PAGE 52 OF 52