3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
- 05 - 05

PAGE 1 OF 20 

# Final Report
Analysis of PFOA, PFBS, PFHS, and PFOS in Ground Water Samples Collected at the Former Sludge Incorporation Area (FSIA) from Decatur, AL 4 th 

## Quarter 201 3 Laboratory Request Number: ISO13
- 05 - 05 Method Re quirement: 3M Method ETS
- 8 - 044.1 Report Date

– Date of Final Signature 

## Testing Laboratory 3M Environmental Health and Safety Operations Environmental Laboratory 3M Center, Bldg 260
- 05 - N
- 17 St. Paul, MN 55144 Requester Gary Hohenstein 3M Building 224 - 5W
- 03 Saint Paul, MN 55144
- 1000 Phone: (651) 737
- 3570

The testing reported herein meet the requirements of ANSI/ISO/IEC 17025:2005 “General Requirements for the Competence of Testing and Calibration Laboratories”, in accordance with A2LA Certificate # 2052.01. Additionally, the laboratory’s quality system h as been audited and was determined to be in conformance with the EPA GLPs (40 CFR 792) by an independent assessment.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
- 05 - 05

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### 3M Environmental Laboratory 3M Environmental Laboratory T echnical Director : William K. Reagen, Ph.D. 3M Principal Analytical Investigator : Susan Wolf Report Author: Kevin Eich 

## Analytical Report **ISO13 -**  **05 -**  **05** Analysis of PFOA, PFBS, PFHS, and PFOS in Ground Water Samples Collected at the Former Sludge Incorporation Area (FSIA) from Decatur, AL 4 th 

### Quarter 2013 Report Date: Date of Final Signature 

## 1 Introduction/Summary The 3M Environmental Laboratory prepared and analyzed water samples collected by Weston Solutions personnel from Decatur, AL

. S ample s were collected on November 19, November 20, and November 21 and returned to the 3M Environmental Laboratory on November 25 , 201 3 at ambient conditions

. All samples were analyzed for perfluorooctanoic acid (PFOA), per fluorobutane sulfonate (PFBS), perfluorohexane sulfonate (PFHS) and perfluorooctane sulfonate (PFOS) under laboratory project number ISO13
- 05 - 05

. The 3M Environmental Laboratory prepared sample containers for thirty
- one groundwater well locations

. Each empty container was marked with a “fill to here” line that corresponded to a final volume of 200 mL. Sample bottle sets for each groundwater sampling location included a field sample and field sample duplicate . Select locations also included one field spike sample. Containers designated for field matrix samples were fortified with an appropriate matrix spike solution containing PFOA, PFBS, PFHS, and PFOS prior to being sent to the field for sample collection. Sampling locations DAL
- GW
- 136R, DAL
- GW
- 137R, DAL
- GW
- 137S, DAL
- GW
- 138R, and DAL
- GW
- 14 3 R were not collected due to the well being dry. Samples were analyzed for PFOA, PF B S, PF H S, and PFOS by ETS
- 8 - 044.1 “ Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis”. Table 1 summarizes the sample results using the analytical method identified above. All results for quality control samples prepared and analyzed with the samples will be reported and discussed elsewhere in this report.

The testing reported herein meet the requirements of ANSI/ISO/IEC 17025:2005 “General Requirements for the Competence of Testing and Calibration Laboratories”, in accordance with A2LA Certificate # 2052.01. Additionally, the laboratory’s quality system has been audited and was determined to be in conformance with the EPA GLPs (40 CFR 792) by an independent assessment.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
- 05 - 05

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### Table 1 . Sample Results Summary (1)

3M LIMS ID Sample Description PFOA Concentration (ng/mL) PFBS Concentration (ng/mL) PF HS Concentration (ng/mL) PFOS Concentration (ng/mL) ISO13
- 05 - 05 - 001 DAL
- GW
- 130R
- 0 - 131121 955 17.6 132 571 ISO13
- 05 - 05 - 002 DAL
- GW
- 130R
- DB
- 131121 962 17.9 132 585 Average 959 17.8 132 578 %RPD Sample/Sample Dup 0.73 1.7 0.0 2.4 ISO13
- 05 - 05 - 003 DAL
- GW
- 130S
- 0 - 131121 195 3.84 33.4 147 ISO13
- 05 - 05 - 004 DAL
- GW
- 130S
- DB
- 131121 187 3.71 32.8 140 Average 191 3.78 33.1 144 %RPD Sample/Sample Dup 4.2 3.4 1.8 4.9 ISO13
- 05 - 05 - 005 DAL
- GW
- 130L
- 0 - 131121 62.7 1.47 11.6 72.7 ISO13
- 05 - 05 - 006 DAL
- GW
- 130L
- DB
- 131121 59.5 1.39 10.8 68.5 Average 61.1 1.43 11.2 70.6 %RPD Sample/Sample Dup 5.2 5.6 7.1 5.9 ISO13
- 05 - 05 - 007 DAL
- GW
- 131R
- 0 - 131121 2300 54.8 303 1210 ISO13
- 05 - 05 - 008 DAL
- GW
- 131R
- DB
- 131121 2530 58.9 326 1300 Average 2420 56.9 315 1260 %RPD Sample/Sample Dup 9.5 7.2 7.3 7.2 ISO13
- 05 - 05 - 010 DAL
- GW
- 131S
- 0 - 131121 33.1 1.08 5.81 7.08 ISO13
- 05 - 05 - 011 DAL
- GW
- 131S
- DB
- 131121 33.2 1.05 6.08 6.58 Average 33.2 (2) 1.07 (2) 5.95 (2) 6.83 (2) %RPD Sample/Sample Dup 0.30 2.8 4.5 7.3 ISO13
- 05 - 05 - 012 DAL
- GW
- 131L
- 0 - 131121 104 3.73 22.6 45.6 ISO13
- 05 - 05 - 013 DAL
- GW
- 131L
- DB
- 131121 108 3.96 27.1 47.2 Average 106 (2) 3.85 (2) 24.9 (2) 46.4 (2) %RPD Sample/Sample Dup 3.8 6.0 18 3.4 ISO13
- 05 - 05 - 014 DAL
- GW
- 133R
- 0 - 131120 51.7 2.80 17.9 35.9 ISO13
- 05 - 05 - 015 DAL
- GW
- 133R
- DB
- 131120 52.1 2.90 16.1 31.7 Average 51.9 (2) 2.85 (2) 17.0 (2) 33.8 (2) %RPD Sample/Sample Dup 0.77 3.5 11 12 ISO13
- 05 - 05 - 017 DAL
- GW
- 133S
- 0 - 131120 393 9.68 70.5 251 ISO13
- 05 - 05 - 018 DAL
- GW
- 133S
- DB
- 131120 399 10.2 70.8 256 Average 396 9.94 70.7 254 %RPD Sample/Sample Dup 1.5 5.2 0.42 2.0 NA = Not Applicable (1) All samples associated with the reported sampling location were diluted and analyzed by ex ternal standard calibration unless noted otherwise. The analytical method uncertainties for the reported results using method ETS
- 8 - 044.1 by direct injection are as follows: PFOA ± 17 %, PFBS ± 17 %, PFHS ± 1 6 %, and PFOS ± 19 %. (2) All samples associated with t he reported sampling location were analyzed by internal standard calibration

. The analytical method uncertainties for the reported results using method ETS
- 8 - 044.1 by direct injection are as follows: PFOA ± 1 2% , PFBS ± 1 4 %, PFHS ± 22 %, and PFOS ± 1 4 %. (3) Th e RPD value did not meet method acceptance criteria of ≤ 20%.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 4 OF 20 

### Table 1 continued . Sample Results Summary (1)

3M LIMS ID Sample Description PFOA Concentration (ng/mL) PFBS Concentration (ng/mL) PF HS Concentration (ng/mL) PFOS Concentration (ng/mL) ISO13
- 05 - 05 - 020 DAL
- GW
- 133L
- 0 - 131120 367 8.29 59.2 310 ISO13
- 05 - 05 - 021 DAL
- GW
- 133L
- DB
- 131120 369 8.67 59.4 325 Average 368 8.48 59.3 318 %RPD Sample/Sample Dup 0.54 4.5 0.34 4.7 ISO13
- 05 - 05 - 022 DAL
- GW
- 134R
- 0 - 131120 1720 43.9 390 1240 ISO13
- 05 - 05 - 023 DAL
- GW
- 134R
- DB
- 131120 1820 45.6 405 1280 Average 1770 44.8 398 1260 %RPD Sample/Sample Dup 5.6 3.8 3.8 3.2 ISO13
- 05 - 05 - 024 DAL
- GW
- 134S
- 0 - 131120 25.8 0.688 7.49 27.8 ISO13
- 05 - 05 - 025 DAL
- GW
- 134S
- DB
- 131120 25.9 0.628 7.53 29.1 Average 25.9 (2) 0.658 (2) 7.51 (2) 28.5 (2) %RPD Sample/Sample Dup 0.39 9.1 0.53 4.6 ISO13
- 05 - 05 - 027 DAL
- GW
- 134L
- 0 - 131120 536 9.93 100 515 ISO13
- 05 - 05 - 028 DAL
- GW
- 134L
- DB
- 131120 535 10.6 97.4 498 Average 536 10.3 98.7 507 %RPD Sample/Sample Dup 0.19 6.5 2.6 3.4 ISO13
- 05 - 05 - 030 DAL
- GW
- 135R
- 0 - 131119 4060 71.8 812 1180 ISO13
- 05 - 05 - 031 DAL
- GW
- 135R
- DB
- 131119 4020 72.3 787 1210 Average 4040 72.1 800 1200 %RPD Sample/Sample Dup 0.99 0.69 3.1 2.5 ISO13
- 05 - 05 - 033 DAL
- GW
- 135S
- 0 - 131119 59.0 2.33 20.2 16.0 ISO13
- 05 - 05 - 034 DAL
- GW
- 135S
- DB
- 131119 60.0 2.32 21.6 15.8 Average 59.5 (2) 2.33 (2) 20.9 (2) 15.9 (2) %RPD Sample/Sample Dup 1.7 0.43 6.7 1.3 ISO13
- 05 - 05 - 035 DAL
- GW
- 135L
- 0 - 131119 595 15.7 124 183 ISO13
- 05 - 05 - 036 DAL
- GW
- 135L
- DB
- 131119 605 16.8 124 186 Average 600 16.3 124 185 %RPD Sample/Sample Dup 1.7 6.8 0.0 1.6 ISO13
- 05 - 05 - 039 DAL
- GW
- 136S
- 0 - 131120 120 2.98 20.6 126 ISO13
- 05 - 05 - 040 DAL
- GW
- 136S
- DB
- 131120 119 2.96 20.3 125 Average 120 2.97 20.5 126 %RPD Sample/Sample Dup 0.84 0.67 1.5 0.80 NA = Not Applicable (1) All samples associated with the reported sampling location were diluted and analyzed by ex ternal standard calibration unless noted otherwise. The analytical method uncertainties for the reported results using method ETS
- 8 - 044.1 by direct injection are as follows: PFOA ± 17%, PFBS ± 17%, PFHS ± 16%, and PFOS ± 19%. (2) All samples associated with the reported sampling location were analyzed by internal standard calibration

. The analy tical method uncertainties for the reported results using method ETS
- 8 - 044.1 by direct injection are as follows: PFOA ± 12%, PFBS ± 14%, PFHS ± 22%, and PFOS ± 14%. (3) The RPD value did not meet method acceptance criteria of ≤ 20%.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 5 OF 20 

### Table 1 con tinued . Sample Results Summary (1)

3M LIMS ID Sample Description PFOA Concentration (ng/mL) PFBS Concentration (ng/mL) PF HS Concentration (ng/mL) PFOS Concentration (ng/mL) ISO13
- 05 - 05 - 041 DAL
- GW
- 136L
- 0 - 131120 96.5 2.51 16.1 97.1 ISO13
- 05 - 05 - 042 DAL
- GW
- 136L
- DB
- 131120 96.7 2.52 16.0 97.2 Average 96.6 2.52 16.1 97.2 %RPD Sample/Sample Dup 0.21 0.40 0.62 0.10 ISO13
- 05 - 05 - 049 DAL
- GW
- 137L
- 0 - 131119 0.477 0.0920 0.115 1.84 ISO13
- 05 - 05 - 050 DAL
- GW
- 137L
- DB
- 131119 0.450 0.0903 0.0956 1.64 Average 0.464 (2) 0.0912 (2) 0.105 (2) 1.74 (2) %RPD Sample/Sample Dup 5.8 1.9 18 11 ISO13
- 05 - 05 - 053 DAL
- GW
- 138S
- 0 - 131119 178 5.64 24.3 247 ISO13
- 05 - 05 - 054 DAL
- GW
- 138S
- DB
- 131119 184 5.45 25.4 254 Average 181 5.55 24.9 251 %RPD Sample/Sample Dup 3.3 3.4 4.4 2.8 ISO13
- 05 - 05 - 055 DAL
- GW
- 138L
- 0 - 131119 0.613 <0.0250 0.0568 0.486 ISO13
- 05 - 05 - 056 DAL
- GW
- 138L
- DB
- 131119 0.664 <0.0250 0.0618 0.404 Average 0.639 (2) <0.0250 (2) 0.0593 (2) 0.445 (2) %RPD Sample/Sample Dup 8.0 NA 8.4 18 ISO13
- 05 - 05 - 057 DAL
- GW
- CW26C
- 0 - 131121 443 8.14 63.3 448 ISO13
- 05 - 05 - 058 DAL
- GW
- CW26C
- DB
- 131121 460 8.73 64.6 462 Average 452 8.44 64.0 455 %RPD Sample/Sample Dup 3.8 7.0 2.0 3.1 ISO13
- 05 - 05 - 060 DAL
- GW
- CW26L
- 0 - 131121 897 14.1 118 1400 ISO13
- 05 - 05 - 061 DAL
- GW
- CW26L
- DB
- 131121 871 14.6 113 1350 Average 884 14.4 116 1380 %RPD Sample/Sample Dup 2.9 3.5 4.3 3.6 ISO13
- 05 - 05 - 063 DAL
- GW
- 140R
- 0 - 131120 110 1.10 13.8 118 ISO13
- 05 - 05 - 064 DAL
- GW
- 140R
- DB
- 131120 113 1.06 13.3 119 Average 112 1.08 13.6 119 %RPD Sample/Sample Dup 2.7 3.7 3.7 0.84 ISO13
- 05 - 05 - 065 DAL
- GW
- 141R
- 0 - 131119 2.56 0.0731 0.418 7.41 ISO13
- 05 - 05 - 066 DAL
- GW
- 141R
- DB
- 131119 2.59 0.0491 0.459 6.93 Average 2.58 (2) 0.0611 (2) 0.439 (2) 7.17 (2) %RPD Sample/Sample Dup 1.2 39 (3) 9.4 6.7 NA = Not Applicable (1) All samples associated with the reported sampling location were diluted and analyzed by ex ternal standard calibration unless noted otherwise. The analytical method uncertainties for the reported results using method ETS
- 8 - 044.1 by direct injection are as follows: PFOA ± 17%, PFBS ± 17%, PFHS ± 16%, and PFOS ± 19%. (2) All samples associated with the reported sampling location were analyzed by internal standard calibration

. The analytical method uncertainties for the reported results using method ETS
- 8 - 044.1 by direct injection are as follows: PFOA ± 12%, PFBS ± 14%, PFHS ± 22%, and PFOS ± 14%. (3) The RPD value did not meet method acceptance criteria of ≤ 20%.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 6 OF 20 

### Table 1 continued . Sample Results Summary (1)

3M LIMS ID Sample Description PFOA Concentration (ng/mL) PFBS Concentration (ng/mL) PF HS Concentration (ng/mL) PFOS Concentration (ng/mL) ISO13
- 05 - 05 - 067 DAL
- GW
- 142R
- 0 - 131121 65.4 2.32 12.6 163 ISO13
- 05 - 05 - 068 DAL
- GW
- 142R
- DB
- 131121 68.1 2.30 13.3 166 Average 66.8 2.31 13.0 165 %RPD Sample/Sample Dup 4.0 0.87 5.4 1.8 ISO13
- 05 - 05 - 071 DAL
- GW
- 145R
- 0 - 131122 83.0 2.24 9.57 177 ISO13
- 05 - 05 - 072 DAL
- GW
- 145R
- DB
- 131122 85.3 2.32 10.0 181 Average 84.2 2.28 9.79 179 %RPD Sample/Sample Dup 2.7 3.5 4.4 2.2 NA = Not Applicable (1) All samples associated with the reported sampling location were diluted and analyzed by ex ternal standard calibration unless noted otherwise. The analytical method uncertainties for the reported results using method ETS
- 8 - 044.1 by direct injection are as follows: PFOA ± 17%, PFBS ± 17%, PFHS ± 16%, and PFOS ± 19%. (2) All samples associated with the reported sampling location were analyzed by internal standard calibratio n . The analytical method uncertainties for the reported results using method ETS
- 8 - 044.1 by direct injection are as follows: PFOA ± 12%, PFBS ± 14%, PFHS ± 22%, and PFOS ± 14%. (3) The RPD value did not meet method acceptance criteria of ≤ 20%. 

## 2 Methods - Analytical and Preparatory 2.1 Methods Analysis was completed using 3M Environmental Laboratory Method ETS
- 8 - 044.1 “ Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis”

. Table 2 . Target Analytes

Target Analytes Acronym Reference Material Structure Perfluorobutanoic Acid (C4 Acid) PF O A Linear and Branched Perfluorooctanoic Acid (C8 Acid) PF BS Linear Perfluorobutanesulfonate (C4 Sulfonate ) PF H S Linear Perfluorooctanesulfonate (C8 Sulfonate) PFOS Linear and Branched 

## 2.2 Sample Collection All samples were collected in 250 mL Nalgene TM 

### (high
- density polyethylene) bottles prepared at the 3M Environmental Laboratory. S amples were collected on November 19, November 20, and November 21 and returned to the 3M Environmental Laboratory on November 25, 2013 at ambient conditions

. Prior to sample collection, bottles designated for field matrix spikes were spiked in the laboratory with a known volume of an appropriate matrix spiking solution containing PF OA , PF BS , PF H S , and PFOS

.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 7 OF 20 

### Table 3 . Sample Description Key Code.

String Number String Descriptor Example : DAL - GW - 130R - DB - 13 1121 1 Sample Location DAL= Decatur, Alabama 2 Sample Type GW= Ground Water 3 Well Identifier Example: 130 4 Well Level R = Residuum shallow water
- bearing zone L = Bedrock water
- bearing zone S = Epikarst middle water
- bearing zone 5 Sample Type 0 =primary sample DB =duplicate sample FMS = Field Matrix Spike LS = Low field matrix spike HS = High field matrix spike 6 Sampling Date 131121
– November 21 , 2013 

## 2.3 Sample Preparation 12/5/13 : Solvent dilution / external standard analysis

. All samples and laboratory control spikes were diluted with methanol prior to sample analysis. Samples requiring a 1:10 dilution were prepared by removing a 1.0 mL aliquot of the well mixed sample and diluting it with 9.0 mL of methanol

. Samples requiring a 1:20 dilution were prepared by removing a 0.5 mL aliquot of the well mixed sample and diluting it with 9.5 mL of methanol. Samples requiring a 1:50 dilution were prepared by removing a 0.2 mL aliquot of the well mixed sample and diluting it with 9.8 mL of methanol. Sa mples requiring a 1:100 dilution were prepared by removing a 0.1 mL aliquot of the well mixed sample and diluting it with 9.9 mL of methanol. 12/10/13 : All samples were 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 1 ng/mL). The sample bott les were spiked with an internal standard mix at a nominal concentration of 1 ng/mL 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. 

## 2.4 Analysis All samples and quality control samples were analyzed for the four target analytes using high per formance liquid chromatography/ tandem mass spectrometry (HPLC/MS/MS). Pertinent instrument parameters, the liquid chromatography gradient program, and the spe cific mass transitions analyzed are described in the tables below. The following analytical runs were processed and reported herein:

• 12/5/13 : Solvent dilution / external standard analysis for PFOA, PFBS, PFHS, PFOS (samples extracted 12/5/13) ; locations 130R, 130S, 130L, 131R, 133S, 133L, 134R, 134L, 135R, 135L, 136S, 136L, 138S, CW26C, CW26L, 140R, 142R, 145R, Trip Blank mid and h igh FMS

.

• 12/10 /13 : Solvent dilution / in ternal standard analysis for PFOA, PFBS, PFHS, PFOS (samples extracted 12/10 /13) ; loc ation s 131S, 131L, 133R, 134S, 135S, 137L, 138L, 141R, rinseate blanks, trip blank and trip blank low FMS. 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 t he procedures outlined in method ETS
- 12 - 010. The consistency of the laboratory’s integration is ensured3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
- 05 - 05

PAGE 8 OF 20 

### through the training of laboratory personnel, the peer review process required for all manual integrations, the review of manual integrations by the QA U, and where necessary the review of manual integrations by laboratory management. Table 4 . Instrument Parameters

Instrument Name ETS Buster Analysis Dates 12/5/13 , 12/10/13 Analytical Method ETS
- 8 - 044.1 Liquid Chromatograph Agilent 1 100 Guard column Betasil C18 (4.6 mm X 100 mm), 5 μ Analytical column Betasil C18 (4.6 mm X 100 mm), 5 μ Injection Volume 5, 10, 20, 25 , μL Mass Spectrometer Applied Biosystems API 4000 Ion Source Turbo Spray Polarity Negative Software Analyst 1.6.1 

### Table 5 . Liquid Chromatography Gradient Program
Step Total Time (min) Flow Rate ( μ L/min) 2 mM Ammonium Acetate Methanol ETS Buster 12/5/13 and 12/10/13 0 0 750 90.0 10.0 1 0.5 750 90.0 10.0 2 4.0 750 70.0 30.0 3 6.0 750 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 10.03M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 9 OF 20 

### T able 6 . Mass Transitions
Analyte Mass Transition Q1/Q3 Internal Standard Mass Transition Q1/Q3 Reference Material Structure
PFOA 413/369 [ 13 C 8 ]PFOA (1) 421/376 Linear and Branched 413/219 413/169 PFBS 299/80 [ 18 O 2 ]PFBS (1) 303/84 Linear 299/99 PFHS 399/99 [ 13 C 3 ]PFHS (1) 402/99 Linear 399/80 PFOS 499/99 [ 13 C 8 ]
- PFOS (1) 507/80 Linear and Branched 499/80 499/130 Dwell time was 50 msec for each transition. The individual transitions were summed to produce a “total ion chromatogram” (TIC) , which was u sed for quantitation. (1) Internal standard was used for the analysis on 12/10/13. 

## 3 Data Analysis 3.1 Calibration 12/ 5/13 : Solvent dilution / externa l standard calibratio n. Diluted samples were analyzed against an ext ernal standard calibration curve for PFOA, PFBS, PFHS, and PFOS

. Calibration standards were prepared by spiking known amounts of stock solutions containing the analytes of interest into 50 mL of 90:10 methanol: laboratory Milli
- QTM water . A total of eleven calibra tion standards ranging from 0.1 ng/mL to 150 ng/mL (nom inal) were analyzed. A quadratic, 1/x weighted, calibration curve was used to fit the data for each analyte. The data w ere not forced through zer o during the fitting process. Calculating the standard concentration using the peak area counts and the resu ltant 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. 12/10 /13 : Direct Injection / in ternal standard calibration. Samples were analyzed against a matrix
- matched stable isotope internal standard calibration curve. Calibration standards were prepared by spiking known amounts of the stock solution into laboratory
prepared reagent water . The calibration standards conta ined an internal standard mix at a nominal concentration of 0.5 ng/mL. A total of four teen curve points were analyzed with the sample s ranging from 0.0 1 25 ng/mL to 100 ng/mL. 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. For all analyses, e ach 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. 

## 3.2 System Suitability A calibration standard was analyzed four times at the beginning of the analytical sequence to demonstrate overall system suitability. T he acceptance criteria for system suitability samples is less than or equal to 5% relative standard deviation (RSD) for pe ak area or peak area ratio and retention time criteria of less than or equal to 2% RSD

. These cri teria were met for all analytes with the following exceptions:3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 10 OF 20 

### • 12/10/13 Analysis: The system suitability for area counts was greater than five percent for PFHS (8.9%). A method deviation is included in the raw data. 

## 3.3 Limit of Quantitation (LOQ) The LOQ as defined in method ETS
- 8 - 044.1 is the lowest non
- zero calibr ation standard in the curve that meets linearity and accuracy requirements and for which the peak area ratio (or peak area) is at least two times the average peak area ratio (or peak area) of the method blanks. The LOQs associated with the sample analysis are listed in the table below. T able 7 . LOQ Analysis

Date Calibration Dilution Factor PF O A LOQ, ng/mL PF BS LOQ, ng/mL PF H S LOQ, ng/mL PFOS LOQ, ng/mL

12/5/13 External standard 2 0.192 0.200 0.200 0.185 5 0.479 0.500 0.500 0.464 10 0.958 1.00 1.00 0.927 20 1.92 2.00 2.00 1.85 50 4.79 5.00 5.00 4.64 100 9.58 10.0 10.0 9.27 12/10/13 Internal standard 2 0.0480 0.0250 0.0250 0.0232 

## 3.4 Continuing Calibration During the course of the analytical sequence, several continuing calibration verification samples (CCVs) were analyzed to confirm that the instrument response and the initial calibration curve were still in control. The method acceptance criteria of 100% ± 25% was met for all analytes for all analyses

. 

## 3.5 Blanks Three types of blanks were prepared and analyzed w ith the samples: method/procedural blanks , a field/trip blank, and a single equipment rinseate blank

. Method blank result s were reviewed 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 with each sample preparation batch for the target analytes and analyzed in triplicate

. LCSs were prepared by spiking known amounts of the analytes into synthetic ground water or laboratory Milli Q water to produce the desired concentration. The LCS samples were then diluted in a similar manner as the samples (if diluted) prior to sample anal ysis . The method acceptance criteria, average of each level of LCS should be with in 100% ± 20 % with an RSD ≤20% , was met for all LCSs with the following exceptions: 12/10/13 analysis: The acceptance criteria for accuracy were met with the exception of t he high set of LCS for PF HS ( 12 2 %). A method deviation is filed in the raw data. All batch LCS recovery results were used in the evaluat ion of the analytical method uncertainty in section 3.7 of the report. T he following calculations were used to gener ate data in Table 8

. 100% * ion Concentrat Spike ion Concentrat Calculated Recovery Percent LCS =3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
- 05 - 05

PAGE 11 OF 20 100% * recovery LCS average replicates LCS deviation standard RSD LCS% =



### Table 8 . Lab Control Spike Results
ETS
- 8 - 044.1 Analyzed 12/5 / 13 External Standard Calibration PFOA (Linear and Branched) PFBS
Lab ID Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery LCS
- 131204 - 1 0.477 0.496 104 0.498 0.490 98.5 LCS
- 131204 - 2 0.477 0.370 77.6 0.498 0.402 80.8 LCS
- 131204 - 3 0.477 0.457 95.7 0.498 0.473 95.0 Average ± %RSD 92.4 % ± 15 % 91.4 % ± 10 % LCS
- 131204 - 4 4.77 5.58 117 4.98 6.02 121 LCS
- 131204 - 5 4.77 5.20 109 4.98 5.53 111 LCS
- 131204 - 6 4.77 4.45 93.2 4.98 4.62 92.8 Average ± %RSD 106 % ± 11 % 108 % ± 13 % LCS
- 131204 - 7 38.2 38.3 100 39.8 41.1 103 LCS
- 131204 - 8 38.2 38.3 100 39.8 40.5 102 LCS
- 131204 - 9 38.2 41.0 107 39.8 42.8 107 Average ± %RSD 10 2 % ± 3.9 % 10 4 % ± 2.5 % ETS
- 8 - 044.1 Analyzed 12/5/13 External Standard Calibration PFHS PFOS (Linear and Branched)
Lab ID Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery LCS
- 131204 - 1 0.498 0.482 96.8 0.461 0.481 104 LCS
- 131204 - 2 0.498 0.377 75.7 0.461 0.346 75.1 LCS
- 131204 - 3 0.498 0.511 103 0.461 0.437 94.7 Average ± %RSD 91.8 % ± 16 % 91.3 % ± 16 % LCS
- 131204 - 4 4.98 5.96 120 4.61 5.46 118 LCS
- 131204 - 5 4.98 5.53 111 4.61 4.85 105 LCS
- 131204 - 6 4.98 4.62 92.8 4.61 4.33 93.9 Average ± %RSD 108 % ± 13 % 106 % ± 11 % LCS
- 131204 - 7 39.8 39.8 100 36.9 37.4 101 LCS
- 131204 - 8 39.8 40.2 101 36.9 36.7 99.4 LCS
- 131204 - 9 39.8 42.9 108 36.9 40.3 109 Average ± %RSD 103 % ± 4.2 % 103 % ± 5.0 %3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 12 OF 20 

### Table 8 continued. Lab Control Spike Results
ETS
- 8 - 044.1 Analyzed 12/10 /13 Internal S tandard C alibration PFOA (Linear and Branched) PFBS
Lab ID Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery LCS
- 131210 - 1 0.190 0.197 104 0.199 0.203 102 LCS
- 131210 - 2 0.190 0.194 102 0.199 0.251 126 LCS
- 131210 - 3 0.190 0.203 107 0.199 0.232 116 Average ± %RSD 104 % ± 2. 4 % 115 % ± 11 % LCS
- 131210 - 4 9.52 10.8 114 9.94 11.6 117 LCS
- 131210 - 5 9.52 10.2 107 9.94 10.3 104 LCS
- 131210 - 6 9.52 10.6 111 9.94 10.8 109 Average ± %RSD 111 % ± 3.2 % 110 % ± 6.0 % LCS
- 131210 - 7 38.0 41.7 110 39.6 42.8 108 LCS
- 131210 - 8 38.0 44.4 117 39.6 44.9 113 LCS
- 131210 - 9 38.0 42.3 111 39.6 44.9 113 Average ± %RSD 113 % ± 3.4 % 111 % ± 2.6 % ETS
- 8 - 044.1 Analyzed 12/10/13 Internal S tandard C alibration PFHS PFOS (Linear and Branched)
Lab ID Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery LCS
- 131210 - 1 0.199 0.196 98.7 0.184 0.204 111 LCS
- 131210 - 2 0.199 0.218 109 0.184 0.188 102 LCS
- 131210 - 3 0.199 0.221 111 0.184 0.205 112 Average ± %RSD 106 % ± 6.2 % 108 % ± 5.1 % LCS
- 131210 - 4 9.94 10.7 108 9.21 10.4 113 LCS
- 131210 - 5 9.94 10.7 108 9.21 10.3 112 LCS
- 131210 - 6 9.94 11.5 116 9.21 9.91 108 Average ± %RSD 111 % ± 4. 2 % 111 % ± 2.4 % LCS
- 131210 - 7 39.6 51.7 130 36.7 39.4 107 LCS
- 131210 - 8 39.6 44.9 113 36.7 42.2 115 LCS
- 131210 - 9 39.6 49.0 124 36.7 41.2 112 Average ± %RSD 122 % ± 7.0 % (1) 111 % ± 3.6 % (1) The a verage LCS recovery did not meet method acceptance criteria of 100% ± 20%.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 13 OF 20 

## 3.7 Analytical Method Uncertainty Analytical method uncertainty is based on historical QC data that is control charted and used to evaluate method accuracy and precision. The method uncertainty is calculated following ETS
- 12 - 012.2. The standard deviation is calculated for the set of accuracy results (in %) obtained for the QC samples. The expanded uncertainty is calculated by multiplying the standard deviation by a factor of 2, which corresponds to a confidence level of 95%.
• The analytical method uncertainty as calculated by ETS
- 12 - 012.2 for PF HS by in te rnal standard calibration was ±15 %. However, t he recovery of the high set of LCS analyzed on 12/10 /13 was 12 2 % for PF HS by in ternal standard calibration for the samples analyzed on this date. The refore, the analytical method uncertainty was expanded for samples analyzed by in ternal standard calibration for PF HS to ± 2 2 %. Table 9 . Analytical Method Uncertainty Analyte Calibration Standard Deviation (%) Method Uncertainty PFOA External 8.26 ±17 % PFBS External 8.67 ±17 % PFH S External 7.81 ±1 6 % PFOS External 9.34 ±19 % PFOA Internal 5.98 ±1 2 % PFBS Internal 7.07 ±14 % PFHS Internal NA ± 22 % PFOS Internal 7.19 ±14 % NA = Not Applicable 

## 3.8 Field Matrix Spikes (FMS) and Laboratory Matrix Spikes (LMS) Field matrix spike sample containers were prepared for all 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 t arget analytes prior to shipping sample containers to the field for sample collection. Field matrix spikes must be at least 0.5 times the analyte concentration to be considered an appropriate spike level. Field matrix spike recoveries within method accep tance 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 co nsisted of linear and branched isomers. The locations for which FMS sample containers were prepared are listed in Table 10

. Field matrix spikes are presented in section 4 of this report.
100% * on Concentrat Spike Dup.) Sample Field & Sample Field : ion Concentrat Average FMS of ion Concentrat (Sample Recovery FMS − =3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 14 OF 20 

### Table 10 . Field Matrix Spike (FMS) Concentrations

Sampling location Spike Level PFO A ng/mL PFBS ng/mL PF HS ng/mL PF OS ng/mL 137S FMS 0.992 1.00 1.00 0.998 134S FMS 9.92 10.0 10.0 9.98 133R, 136L FMS 49.6 50.0 50.0 49.9 133S, CW26C FMS 198 200 200 200 134L, CW26L FMS 496 500 501 499 131R, 135R FMS 1980 2000 2000 2000 Trip Blank FMS Low 9.92 10.0 10.0 9.98 FMS Mid 49.6 50.0 50.0 49.9 FMS High 1980 2000 2000 2000 

## 4 Data Summary and Discussion
Tables 11 - 2 1 below summarize the sample results and target analyte field matrix spike recoveries for the sampling locations as well as the T rip Blank

. Each table provides the average concentration and the relative percent difference (%RPD) of the sample and sample d uplicate. Results and average values are rounded to three significant figures. Percent relative difference (%RPD) values are rounded to two significant figures. Because of rounding, values may vary slightly from those listed in the raw data. Field matr ix spikes meeting the method acceptance criteria of ± 30%, demonstrate that the method is appropriate for the given matrix. All target analyte field matrix spikes met method acceptance criteria. Table 11 . DAL - GW - 131 R
PFO A PF BS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 007 DAL
- GW
- 131R
- 0 - 131121 2300 NA 54.8 NA ISO13
- 05 - 05 - 008 DAL
- GW
- 131R
- DB
- 131121 2530 NA 58.9 NA ISO13
- 05 - 05 - 009 DAL
- GW
- 131R
- FMS
- 131121 4510 106 2070 101 Average Concentration (ng/mL) ± %RPD 2420 ng/mL ± 9.5 % 56.9 ng/mL ± 7.2 %
PFH S PFOS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 007 DAL
- GW
- 131R
- 0 - 131121 303 NA 1210 NA ISO13
- 05 - 05 - 008 DAL
- GW
- 131R
- DB
- 131121 326 NA 1300 NA ISO13
- 05 - 05 - 009 DAL
- GW
- 131R
- FMS
- 131121 2380 103 3250 99.8 Average Concentration (ng/mL) ± %RPD 315 ng/mL ± 7.3 % 1260 ng/mL ± 7.2 % NA = Not Applicable Samples were diluted 1:10 0 and analyzed using external standard quantitation.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
- 05 - 05

PAGE 15 OF 20 

### Table 12 . DAL - GW - 133R
PFO A PF BS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 014 DAL
- GW
- 133R
- 0 - 131120 51.7 NA 2.80 NA ISO13
- 05 - 05 - 015 DAL
- GW
- 133R
- DB
- 131120 52.1 NA 2.90 NA ISO13
- 05 - 05 - 016 DAL
- GW
- 133R
- FMS
- 131120 100 97.0 61.9 118 Average Concentration (ng/mL) ± %RPD 51.9 ng/mL ± 0.77 % 2.85 ng/mL ± 3.5 %
PFH S PFOS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 014 DAL
- GW
- 133R
- 0 - 131120 17.9 NA 35.9 NA ISO13
- 05 - 05 - 015 DAL
- GW
- 133R
- DB
- 131120 16.1 NA 31.7 NA ISO13
- 05 - 05 - 016 DAL
- GW
- 133R
- FMS
- 131120 66.2 98.4 85.9 104 Average Concentration (ng/mL) ± %RPD 17.0 ng/mL ± 11 % 33.8 ng/mL ± 12 % NA = Not Applicable Samples were diluted 1:2 and analyzed using in ternal standard quantitation. 

### Table 13 . DA L - GW - 133S
PFO A PF BS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 017 DAL
- GW
- 133S
- 0 - 131120 393 NA 9.68 NA ISO13
- 05 - 05 - 018 DAL
- GW
- 133S
- DB
- 131120 399 NA 10.2 NA ISO13
- 05 - 05 - 019 DAL
- GW
- 133S
- FMS
- 131120 570 87.7 234 112 Average Concentration (ng/mL) ± %RPD 39 6 ng/mL ± 1.5 % 9.94 ng/mL ± 5.2 %
PFH S PFOS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 017 DAL
- GW
- 133S
- 0 - 131120 70.5 NA 251 NA ISO13
- 05 - 05 - 018 DAL
- GW
- 133S
- DB
- 131120 70.8 NA 256 NA ISO13
- 05 - 05 - 019 DAL
- GW
- 133S
- FMS
- 131120 288 108 471 109 Average Concentration (ng/mL) ± %RPD 70.7 ng/mL ± 0.42 % 254 ng/mL ± 2.0 % NA = Not Applicable Samples were diluted 1:1 0 and analyzed using external standard quantitation.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
- 05 - 05

PAGE 16 OF 20 

### Table 14

. DAL - GW - 134S
PFO A PF BS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 024 DAL
- GW
- 134S
- 0 - 131120 25.8 NA 0.688 NA ISO13
- 05 - 05 - 025 DAL
- GW
- 134S
- DB
- 131120 25.9 NA 0.628 NA ISO13
- 05 - 05 - 026 DAL
- GW
- 134S
- FMS
- 131120 35.7 NC 11.5 108 Average Concentration (ng/mL) ± %RPD 25.9 ng/mL ± 0.39 % 0.658 ng/mL ± 9.1 %
PFH S PFOS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 024 DAL
- GW
- 134S
- 0 - 131120 7.49 NA 27.8 NA ISO13
- 05 - 05 - 025 DAL
- GW
- 134S
- DB
- 131120 7.53 NA 29.1 NA ISO13
- 05 - 05 - 026 DAL
- GW
- 134S
- FMS
- 131120 18.3 108 38.0 NC Average Concentration (ng/mL) ± %RPD 7.41 ng/mL ± 0.53 % 28.5 ng/mL ± 4.6 % NA = Not Applicable NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concentration. Samples were diluted 1: 2 and analyzed using in ternal standard quantitation. 

### Table 15 . DAL - GW - 134L
PFO A PF BS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 027 DAL
- GW
- 134L
- 0 - 131120 536 NA 9.93 NA ISO13
- 05 - 05 - 028 DAL
- GW
- 134L
- DB
- 131120 535 NA 10.6 NA ISO13
- 05 - 05 - 029 DAL
- GW
- 134L
- FMS
- 131120 1000 93.6 536 105 Average Concentration (ng/mL) ± %RPD 536 ng/mL ± 0.19 % 10.3 ng/mL ± 6.5 %
PFH S PFOS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 027 DAL
- GW
- 134L
- 0 - 131120 100 NA 515 NA ISO13
- 05 - 05 - 028 DAL
- GW
- 134L
- DB
- 131120 97.4 NA 498 NA ISO13
- 05 - 05 - 029 DAL
- GW
- 134L
- FMS
- 131120 644 109 1080 115 Average Concentration (ng/mL) ± %RPD 98.7 ng/mL ± 2.6 % 507 ng/mL ± 3.4 % NA = Not Applicable Samples were diluted 1:10 and analyzed using external standard quantitation.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
- 05 - 05

PAGE 17 OF 20 

### Table 16 . DAL - GW - 135R
PFO A PF BS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 030 DAL
- GW
- 135R
- 0 - 131119 4060 NA 71.8 NA ISO13
- 05 - 05 - 031 DAL
- GW
- 135R
- DB
- 131119 4020 NA 72.3 NA ISO13
- 05 - 05 - 032 DAL
- GW
- 135R
- FMS
- 131119 5530 NC 2080 100 Average Concentration (ng/mL) ± %RPD 4040 ng/mL ± 0.99 % 72.1 ng/mL ± 0.69 %
PFH S PFOS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 030 DAL
- GW
- 135R
- 0 - 131119 812 NA 1180 NA ISO13
- 05 - 05 - 031 DAL
- GW
- 135R
- DB
- 131119 787 NA 1210 NA ISO13
- 05 - 05 - 032 DAL
- GW
- 135R
- FMS
- 131119 2750 97.5 3040 92.3 Average Concentration (ng/mL) ± %RPD 800 ng/mL ± 3.1 % 1200 ng/mL ± 2.5 % NA = Not Applicable NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concentration. Samples were diluted 1:50 and analyzed using external standard quantitation. 

### Table 17 . DAL - GW - 136 L
PFO A PF BS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 041 DAL
- GW
- 136L
- 0 - 131120 96.5 NA 2.51 NA ISO13
- 05 - 05 - 042 DAL
- GW
- 136L
- DB
- 131120 96.7 NA 2.52 NA ISO13
- 05 - 05 - 043 DAL
- GW
- 136L
- FMS
- 131120 153 114 60.5 116 Average Concentration (ng/mL) ± %RPD 96.6 ng/mL ± 0.21 % 2.52 ng/mL ± 0.40 %
PFH S PFOS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 041 DAL
- GW
- 136L
- 0 - 131120 16.1 NA 97.1 NA ISO13
- 05 - 05 - 042 DAL
- GW
- 136L
- DB
- 131120 16.0 NA 97.2 NA ISO13
- 05 - 05 - 043 DAL
- GW
- 136L
- FMS
- 131120 74.7 117 153 112 Average Concentration (ng/mL) ± %RPD 16.1 ng/mL ± 0.62 % 97.2 ng/mL ± 0.10 % NA = Not Applicable Samples were diluted 1: 10 with a larger injection volume to achieve a dilution factor of 2 and analyzed using external standard quantitation.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 18 OF 20 

### Table 18 . DAL - GW - CW26C
PFO A PF BS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 057 DAL
- GW
- CW26C
- 0 - 131121 443 NA 8.14 NA ISO13
- 05 - 05 - 058 DAL
- GW
- CW26C
- DB
- 131121 460 NA 8.73 NA ISO13
- 05 - 05 - 059 DAL
- GW
- CW26C
- FMS
- 131121 617 NC 236 114 Average Concentration (ng/mL) ± %RPD 452 ng/mL ± 3.8 % 8.44 ng/mL ± 7.0 %
PFH S PFOS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 057 DAL
- GW
- CW26C
- 0 - 131121 63.3 NA 448 NA ISO13
- 05 - 05 - 058 DAL
- GW
- CW26C
- DB
- 131121 64.6 NA 462 NA ISO13
- 05 - 05 - 059 DAL
- GW
- CW26C
- FMS
- 131121 284 110 680 NC Average Concentration (ng/mL) ± %RPD 64.0 ng/mL ± 2.0 % 455 ng/mL ± 3.1 % NA = Not Applicable NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concentration. Samples were diluted 1: 10 and analyzed using external standard quantitation. 

### Table 19 . DAL - GW - CW26L
PFO A PF BS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 060 DAL
- GW
- CW26L
- 0 - 131121 897 NA 14.1 NA ISO13
- 05 - 05 - 061 DAL
- GW
- CW26L
- DB
- 131121 871 NA 14.6 NA ISO13
- 05 - 05 - 062 DAL
- GW
- CW26L
- FMS
- 131121 1330 89.9 524 102 Average Concentration (ng/mL) ± %RPD 884 ng/mL ± 2.9 % 14.4 ng/mL ± 3.5 %
PFH S PFOS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 060 DAL
- GW
- CW26L
- 0 - 131121 118 NA 1400 NA ISO13
- 05 - 05 - 061 DAL
- GW
- CW26L
- DB
- 131121 113 NA 1350 NA ISO13
- 05 - 05 - 062 DAL
- GW
- CW26L
- FMS
- 131121 622 101 2030 NC Average Concentration (ng/mL) ± %RPD 116 ng/mL ± 4. 3 % 1380 ng/mL ± 3.6 % NA = Not Applicable NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concentration. Samples were diluted 1:2 0 and analyzed using internal standard quantitation.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 19 OF 20 

### Table 20 . Trip Blank
PFO A PF BS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 075 DAL
- GW
- TRIP
- 0 - 131121 <0.0480 (1) NA <0.0250 (1) NA ISO13
- 05 - 05 - 076 DAL
- GW
- TRIP
- LS
- 131121 11.1 (1) 112 11.7 (1) 117 ISO13
- 05 - 05 - 077 DAL
- GW
- TRIP
- MS
- 131121 55.0 (2) 111 57.1 (2) 114 ISO13
- 05 - 05 - 078 DAL
- GW
- TRIP
- HS
- 131121 2010 (3) 102 2200 (3) 110
PFH S PFOS
3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05 - 05 - 075 DAL
- GW
- TRIP
- 0 - 131121 <0.0250 (1) NA <0.0232 (1) NA ISO13
- 05 - 05 - 076 DAL
- GW
- TRIP
- LS
- 131121 10.9 (1) 109 10.7 (1) 107 ISO13
- 05 - 05 - 077 DAL
- GW
- TRIP
- MS
- 131121 56.4 (2) 113 56.5 (2) 113 ISO13
- 05 - 05 - 078 DAL
- GW
- TRIP
- HS
- 131121 2140 (3) 107 2100 (3) 105 NA = Not Applicable (1) Samples were diluted 1:2 and analyzed using internal standard quantitation. (2) Samples were diluted 1:10 and analyzed using external standard quantitation. (3) Samples were diluted 1:50 and analyzed using external standard quantitation.


### Table 21 . Rinseate Blank
PFO A PF BS PF HS PFOS
3M LIMS ID Description Concentration (ng/mL) Concentration (ng/mL) Concentration (ng/mL) Concentration (ng/mL) ISO13
- 05 - 05 - 073 DAL
- GW
- 145R
- RB01
- 131122 <0.0480 <0.0250 <0.0250 <0.0232 ISO13
- 05 - 05 - 074 DAL
- GW
- 135R
- RB02131119 <0.0480 <0.0250 <0.0250 <0.0232

. Samples were diluted 1:2 and analyzed using internal standard quantitation

. 

## 5 Conclusion Laboratory control spikes were used to determine the analytical method accuracy and precision for all analytes. The accuracy and precision were then used to estimate the method uncertainty for the results. Field and laboratory matrix spike rec overies demonstrated that the analytical method was appropriate for the given sample matrix . Method ETS
- 8 - 044.1 “ Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis ” was used for analysis. Analytical results are reported in Table 1 and 11 - 2 1 of this report.3M ENVIRONMENTAL LABORATORY REPORT

NO. IS013-05-05



## 6 Dat a /

Sampl e Retentio n Al l remainin g sampl e an d associate d projec t dat a (hardcop y an d electronic ) wil l b e archive d accordin g t o 3 M Environmenta l Laborator y standar d operatin g procedures

. 

## 7 Signature s 

# i/^^7 Susa n T

. Wolf , 3 M Pcincipa l Analytica l Investigato r Dat e

Willia m K

. Reagen , Ph.D. , 3 M Environmenta l Technica l Directo r ' Dat e

Th e 3 M Environmenta l Laboratory' s Qualit y Assuranc e Uni t ha s audite d th e dat a an d repor t fo r thi s project

.

Qualit y Assuranc e Representativ e ' Dat e

This test report shall not be reproduced

except in full, without

written approval

of the 3M Environmental

Laboratory.

PAG E 2 0 O F 2 0