3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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# Final Report
Analysis of PFOA, PFBS, PFHS, and PFOS in Ground Water Samples Collected at the Former Sludge Incorporation Area (FSIA) from Decatur, AL 2 nd 

## Quarter 201 3 Laboratory Request Number: ISO13
- 05
- 02 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 the A2LA Testing Certificate # 2052.01. Additionally, the laboratory’s qual ity 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
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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 -**  **02** Analysis of PFOA, PFBS, PFHS, and PFOS in Ground Water Samples Collected at the Former Sludge Incorporation Area (FSIA) from Decatur, AL 2 nd 

### 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 June 21, June 26 , June 27, June 28, July 1, July 2, and July 3, 2013 and returned to the 3M Environmental Laboratory on July 11 , 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
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. 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 spi ke 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
- 138R, and DAL
- GW
- 140R were not collected due to the well being dry or it could not be accessed. 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 re port.

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. 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
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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
- 02
- 001 DAL
- GW
- 130R
- 0
- 130626 881 15.0 122 524 ISO13
- 05
- 02
- 002 DAL
- GW
- 130R
- DB
- 130626 1000 17.6 141 600 Average 941 (2 ) 16.3 132 562 %RPD Sample/Sample Dup 13 16 14 14 ISO13
- 05
- 02
- 004 DAL
- GW
- 130S
- 0
- 130626 190 3.55 31.3 142 ISO13
- 05
- 02
- 005 DAL
- GW
- 130S
- DB
- 130626 186 3.37 30.6 143 Average 188 3.46 31.0 143 %RPD Sample/Sample Dup 2.1 5.2 2.3 0.70 ISO13
- 05
- 02
- 007 DAL
- GW
- 130L
- 0
- 130626 63.0 1.43 11.6 70.9 ISO13
- 05
- 02
- 008 DAL
- GW
- 130L
- DB
- 130626 61.9 1.37 11.7 69.8 Average 62.5 1.40 11.7 70.4 %RPD Sample/Sample Dup 1.8 4.3 0.86 1.6 ISO13
- 05
- 02
- 009 DAL
- GW
- 131R
- 0
- 130703 2460 57.1 330 1440 ISO13
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- 010 DAL
- GW
- 131R
- DB
- 130703 2290 53.4 317 1360 Average 23 80 55.3 324 1400 %RPD Sample/Sample Dup 7.2 6.7 4.0 5.7 ISO13
- 05
- 02
- 011 DAL
- GW
- 131S
- 0
- 130703 27.0 0.957 5.70 5.88 ISO13
- 05
- 02
- 012 DAL
- GW
- 131S
- DB
- 130703 24.2 0.765 4.75 5.39 Average 25.6 (3 ) 0.861 (3 ) 5.23 (3 ) 5.64 (3 ) %RPD Sample/Sample Dup 11 22 (4 ) 18 8.7 ISO13
- 05
- 02
- 013 DAL
- GW
- 131L
- 0
- 130703 105 3.22 22.4 42.3 ISO13
- 05
- 02
- 014 DAL
- GW
- 131L
- DB
- 130703 106 3.37 22.2 44.6 Average 106 3.30 22.3 43.5 %RPD Sample/Sample Dup 0.95 4.6 0.90 5.3 ISO13
- 05
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- 015 DAL
- GW
- 133R
- 0
- 130703 52.6 2.63 15.5 29.0 ISO13
- 05
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- 016 DAL
- GW
- 133R
- DB
- 130703 53.2 2.61 15.6 29.0 Average 52.9 2.62 15.6 29.0 %RPD Sample/Sample Dup 1.1 0.76 0.64 0.0 ISO13
- 05
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- 017 DAL
- GW
- 133S
- 0
- 130703 379 9.11 70.8 307 ISO13
- 05
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- 018 DAL
- GW
- 133S
- DB
- 130703 379 9.40 72.6 306 Average 379 9.26 71.7 307 %RPD Sample/Sample Dup 0.0 3.1 2.5 0.33 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
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- 044.1 by dire ct injection are as follows: PFOA ± 21%, PFBS ± 13 %, PFHS ± 1 4 %, and PFOS ± 16 %. (2) The analytical method uncertainty has been expanded to ±32% for PFOA. See section 4 for further discussion. (3) 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 ± 1 1 %, PFBS ± 1 2%, PFHS ± 12%, and PFOS ± 1 2%. (4) The RPD value did not meet method acc eptance criteria of ≤ 20%. (5) The analytical method uncertainty has been expanded to ±3 9 % for PFOA. See section 4 for further discussion. (6) The analytical method uncertainty has been expanded to ±3 1 % for PFHS . See section 4 for further discussion.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 4 OF 21 

### 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
- 02
- 019 DAL
- GW
- 133L
- 0
- 130703 694 13.2 110 746 ISO13
- 05
- 02
- 020 DAL
- GW
- 133L
- DB
- 130703 658 12.9 108 730 Average 676 13.1 109 738 %RPD Sample/Sample Dup 5.3 2.3 1.8 2.2 ISO13
- 05
- 02
- 021 DAL
- GW
- 134R
- 0
- 130626 1920 49.7 480 1280 ISO13
- 05
- 02
- 022 DAL
- GW
- 134R
- DB
- 130626 1920 49.7 483 1270 Average 1920 49.7 482 1280 %RPD Sample/Sample Dup 0.0 0.0 0.62 0.78 ISO13
- 05
- 02
- 024 DAL
- GW
- 134S
- 0
- 130626 15.8 0.384 4.41 17.5 ISO13
- 05
- 02
- 025 DAL
- GW
- 134S
- DB
- 130626 15.3 0.395 4.56 17.5 Average 15.6 (3 ,5 ) 0.390 (3 ) 4.49 (3 ) 17.5 (3 ) %RPD Sample/Sample Dup 3.2 2.8 3.3 0.0 ISO13
- 05
- 02
- 027 DAL
- GW
- 134L
- 0
- 130626 507 9.86 97.0 521 ISO13
- 05
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- 028 DAL
- GW
- 134L
- DB
- 130626 502 9.84 97.3 522 Average 505 9.85 97.2 522 %RPD Sample/Sample Dup 0.99 0.20 0.31 0.19 ISO13
- 05
- 02
- 029 DAL
- GW
- 135R
- 0
- 130703 3510 62.1 746 1180 ISO13
- 05
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- 030 DAL
- GW
- 135R
- DB
- 130703 3420 59.5 727 1120 Average 34 70 60.8 737 1150 %RPD Sample/Sample Dup 2.6 4.3 2.6 5.2 ISO13
- 05
- 02
- 031 DAL
- GW
- 135S
- 0
- 130703 40.5 1.79 16.0 12.8 ISO13
- 05
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- 032 DAL
- GW
- 135S
- DB
- 130703 40.2 1.65 14.3 10.7 Average 40.4 1.72 (3 ) 15.2 (3 ,6 ) 11.8 (3 ) %RPD Sample/Sample Dup 0.74 8.1 11 18 ISO13
- 05
- 02
- 034 DAL
- GW
- 135L
- 0
- 130703 5 74 15.1 130 147 ISO13
- 05
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- 035 DAL
- GW
- 135L
- DB
- 130703 592 14.9 128 156 Average 5 83 15.0 129 152 %RPD Sample/Sample Dup 3.1 1.3 1.6 5.9 ISO13
- 05
- 02
- 039 DAL
- GW
- 136S
- 0
- 130628 103 2.59 19.0 118 ISO13
- 05
- 02
- 040 DAL
- GW
- 136S
- DB
- 130628 105 2.78 19.4 122 Average 104 2.69 19.2 120 %RPD Sample/Sample Dup 1.9 7.1 2.1 3.3 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 dire ct injection are as follows: PFOA ± 21%, PFBS ± 13%, PFHS ± 14%, and PFOS ± 16%. (2) The analytical method uncertainty has been expanded to ±32% for PFOA. See section 4 for further discussion. (3) 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 ± 11%, PFBS ± 12%, PFHS ± 12%, and PFOS ± 12%. (4) The RPD value did not meet method acc eptance criteria of ≤ 20%. (5) The analytical method uncertainty has been expanded to ±3 9 % for PFOA. See section 4 for further discussion. (6) The analytical method uncertainty has been expanded to ±3 1 % for PFHS . See section 4 for further discussion.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 5 OF 21 

### 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
- 02
- 041 DAL
- GW
- 136L
- 0
- 130628 90.0 2.27 15.6 95.4 ISO13
- 05
- 02
- 042 DAL
- GW
- 136L
- DB
- 130628 90.4 2.27 16.2 92.3 Average 90.2 2.27 15.9 93.9 %RPD Sample/Sample Dup 0.44 0.0 3.8 3.3 ISO13
- 05
- 02
- 045 DAL
- GW
- 137S
- 0
- 130627 0.346 0.115 0.0865 0.523 ISO13
- 05
- 02
- 046 DAL
- GW
- 137S
- DB
- 130627 0.346 0.107 0.0983 0.530 Average 0.346 (3 ) 0.111 (3 ) 0.0924 (3 ) 0.527 (3 ) %RPD Sample/Sample Dup 0.0 7.2 13 1.3 ISO13
- 05
- 02
- 047 DAL
- GW
- 137L
- 0
- 130626 0.355 0.0775 0.0906 1.17 ISO13
- 05
- 02
- 048 DAL
- GW
- 137L
- DB
- 130626 0.384 0.0725 0.0871 1.21 Average 0.370 (3 ) 0.0750 (3 ) 0.0889 (3 ) 1.19 (3 ) %RPD Sample/Sample Dup 7.8 6.7 3.9 3.4 ISO13
- 05
- 02
- 052 DAL
- GW
- 138S
- 0
- 130628 174 4.86 23.6 236 ISO13
- 05
- 02
- 053 DAL
- GW
- 138S
- DB
- 130628 175 4.90 23.7 237 Average 175 4.88 23.7 237 %RPD Sample/Sample Dup 0.57 0.82 0.42 0.42 ISO13
- 05
- 02
- 054 DAL
- GW
- 138L
- 0
- 130628 1.21 0.0529 0.139 0.638 ISO13
- 05
- 02
- 055 DAL
- GW
- 138L
- DB
- 130628 1.10 0.0433 0.159 0.687 Average 1.16 (3 ) 0.0481 (3 ) 0.149 (3 ) 0.663 (3 ) %RPD Sample/Sample Dup 9.5 20 13 7.4 ISO13
- 05
- 02
- 057 DAL
- GW
- CW26C
- 0
- 130628 411 7.39 59.9 408 ISO13
- 05
- 02
- 058 DAL
- GW
- CW26C
- DB
- 130628 407 7.60 61.5 428 Average 409 7.50 60.7 418 %RPD Sample/Sample Dup 0.98 2.8 2.6 4.8 ISO13
- 05
- 02
- 059 DAL
- GW
- CW26L
- 0
- 130628 665 13.0 99.3 969 ISO13
- 05
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- 060 DAL
- GW
- CW26L
- DB
- 130628 642 12.1 97.0 924 Average 654 12.6 98.2 947 %RPD Sample/Sample Dup 3.5 7.2 2.3 4.8 ISO13
- 05
- 02
- 064 DAL
- GW
- 141R
- 0
- 130702 1.88 0.0519 0.334 5.42 ISO13
- 05
- 02
- 065 DAL
- GW
- 141R
- DB
- 130702 2.16 0.0499 0.321 5.11 Average 2.02 (3 ) 0.0509 (3 ) 0.328 (3 ) 5.27 (3 ) %RPD Sample/Sample Dup 14 3.9 4.0 5.9 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 ± 21%, PFBS ± 13%, PFHS ± 14%, and PFOS ± 16%. (2) The analytical method uncertainty has been expanded to ±32% for PFOA. See section 4 for further discussion. (3) 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 ± 11%, PFBS ± 12%, PFHS ± 12%, and PFOS ± 12%. (4) The RPD value did not meet method acceptance criteria of ≤ 20%. (5) The analytical method uncertainty has been expanded to ±3 9 % for PFOA. See section 4 for further discussion. (6) The analytical method uncertainty has been expanded to ±3 1 % for PFHS . See section 4 for further discussion.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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### 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
- 02
- 066 DAL
- GW
- 142R
- 0
- 130628 68.3 2.27 13.6 162 ISO13
- 05
- 02
- 067 DAL
- GW
- 142R
- DB
- 130628 67.0 2.29 12.9 170 Average 67.7 2.28 13.3 166 %RPD Sample/Sample Dup 1.9 0.88 5.3 4.8 ISO13
- 05
- 02
- 068 DAL
- GW
- 143R
- 0
- 130621 35.3 1.73 6.93 24.3 ISO13
- 05
- 02
- 069 DAL
- GW
- 143R
- DB
- 130621 36.0 1.61 6.53 26.0 Average 35.7 1.67 6.73 25.2 %RPD Sample/Sample Dup 2.0 7.2 5.9 6.8 ISO13
- 05
- 02
- 070 DAL
- GW
- 145R
- 0
- 130701 74.3 1.98 9.45 135 ISO13
- 05
- 02
- 071 DAL
- GW
- 145R
- DB
- 130701 75.3 1.98 9.65 141 Average 74.8 1.98 9.55 138 %RPD Sample/Sample Dup 1.3 0.0 2.1 4.3 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 ± 21%, PFBS ± 13%, PFHS ± 14%, and P FOS ± 16%. (2) The analytical method uncertainty has been expanded to ±32% for PFOA. See section 4 for further discussion. (3) 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 ± 11%, PFBS ± 12%, PFHS ± 12%, and PFOS ± 12%. (4) The RPD value did not meet method acceptance criteria of ≤ 20%. (5) The analytical method uncertainty has be en expanded to ±3 9 % for PFOA. See section 4 for further discussion. (6) The analytical method uncertainty has been expanded to ±3 1 % for PFHS . See section 4 for further discussion. 

## 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 June 21, June 26, June 27, June 28, July 1, July 2, and July 3, 2013 and returned to the 3M Environme ntal Laboratory on July 11, 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 PF OS

.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 7 OF 21 

### Table 3
. Sample Description Key Code.

String Number String Descriptor Example : DAL - GW - 130R - DB - 130626 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 130626

– June 26 , 2013 

## 2.3 Sample Preparation 7/15/ 13 and 8/20/13 : 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. Sam ples 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. 7/19/ 13 : All samples were prepared by removing a 0.75 mL aliquot of the well mixed sample and diluting it with 0.75 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 bo ttles 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 specific mass transitions analyzed are described in the tables below. The following analytical runs were processed and reported herein:

• 7/16 /13 : Solvent dilution / external standard analysis for PFOA, PFBS, PFHS, PFOS (samples extracted 7/15/13) ; locations 130R, 130S, 130L, 131R, 131L, 133R, 133S, 133L, 134R, 134L, 135R, 135L, 136S, 136L, 138S, CW26C, CW26L, 142R, 143R, 145R, Trip Blank mid and h igh FMS

.

• 7/19/13 : Direct injection / in ternal standard analysis for PFOA, PFBS, PFHS, PFOS (samples ext racted 7/19/13) ; location s 131S, 134S, 135S, 137S, 137L, 138L, 141R, rinseate blanks, trip blank and trip blank low FMS.

• 7/20/13: Solvent dilution / external standard analysis for PFHS (samples prepared on 7/15/13) ; Trip Blank h igh FMS.

• 8/21/13: Solvent dilution/external standard analysis for PFOA (samples prepared on 8/20/13); locations 135S and 135L.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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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 isom ers 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 integration s by the QAU, and where necessary the review of manual integrations by laboratory management. Table 4 . Instrument Parameters

Instrument Name ETS Buster Analysis Dates 7/16/13, 7/19/13, 7/20/13 , 8/21/13 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 2, 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 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 21 

### 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 7 /19/13. 

## 3 Data Analysis 3.1 Calibration 7/16/13, 7/20/13 , and 8/21/13 : 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 (nominal) 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 t he peak area counts 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. 7/19/13 : 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 contained an internal standard mix at a nominal concentration of 0.5 ng/mL. A total of thirteen curve points were analyzed with the sample s ranging from 0.0 1 25 ng/mL to 5 0 ng/mL. A quadratic, 1/x weighted, calibration curve o f 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 usi ng 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 Syst em 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 peak 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

.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 10 OF 21 

## 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 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 associ ated 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

7/16/13 External standard 2 0.192 0.200 0.500 0.464 5 0.479 0.500 1.25 1.16 10 0.958 1.00 2.50 2.32 20 1.92 2.00 5.00 4.64 50 4.79 5.00 12.5 11.6 7/19/13 Internal standard 2 0.0240 0.0250 0.0250 0.0232 7/20/13 External standard 25 NA NA 2.50 NA 8/21/13 External standard 10 0.958 NA NA NA 50 4.79 NA NA NA NA=Not Applicable 

## 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 a nalysis . 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: 7/16 /13 analysis: The acceptance criteria for accuracy were met with the exception of the mid set of LCS for PF O A ( 12 1 %). 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 generate data in Table 8

.
100% * ion Concentrat Spike ion Concentrat Calculated Recovery Percent LCS =3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 11 OF 21 100% * recovery LCS average replicates LCS deviation standard RSD LCS% =



### Table 8 . Lab Control Spike Results
ETS
- 8
- 044.1 Analyzed 7/16/ 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
- 130715
- 1 0.958 1.05 109 1.00 1.06 106 LCS
- 130715
- 2 0.958 1.04 109 1.00 1.07 107 LCS
- 130715
- 3 0.958 1.00 104 1.00 1.03 103 Average ± %RSD 10 7 % ± 2.7 % 105 % ± 2.0 % LCS
- 130715
- 4 9.58 11.4 119 10.0 11.2 112 LCS
- 130715
- 5 9.58 11.7 122 10.0 11.6 116 LCS
- 130715
- 6 9.58 11.8 123 10.0 11.3 113 Average ± %RSD 121 % ± 1.7 % (1) 11 4 % ± 1.8 % LCS
- 130715
- 7 38.2 37.2 97.5 39.8 37.3 93.7 LCS
- 130715
- 8 38.2 41.4 108 39.8 41.0 103 LCS
- 130715
- 9 38.2 41.0 107 39.8 41.3 104 Average ± %RSD 104 % ± 5.6 % 100 % ± 5.7 %
ETS
- 8
- 044.1 Analyzed 7/16 /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
- 130715
- 1 1.00 1.03 103 0.927 0.932 101 LCS
- 130715
- 2 1.00 1.00 100 0.927 0.980 106 LCS
- 130715
- 3 1.00 1.04 104 0.927 0.929 100 Average ± %RSD 10 2 % ± 2.0 % 10 2 % ± 3.1 % LCS
- 130715
- 4 10.0 11.6 116 9.27 10.7 115 LCS
- 130715
- 5 10.0 11.9 119 9.27 11.0 118 LCS
- 130715
- 6 10.0 11.8 118 9.27 10.6 115 Average ± %RSD 11 8 % ± 1.3 % 11 6 % ± 1.5 % LCS
- 130715
- 7 39.8 38.2 95.9 36.9 35.2 95.3 LCS
- 130715
- 8 39.8 40.8 103 36.9 39.2 106 LCS
- 130715
- 9 39.8 42.2 106 36.9 40.2 109 Average ± %RSD 102 % ± 5.1 % 103 % ± 7.0 % (1) Average LCS recovery did not meet method acceptance criteria of 100 ± 20%

.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 12 OF 21 

### Table 8 continued. Lab Control Spike Results
ETS
- 8
- 044.1 Analyzed 7/19 /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
- 130719
- 1 0.190 0.172 90.3 0.199 0.178 89.2 LCS
- 130719
- 2 0.190 0.168 88.4 0.199 0.168 84.5 LCS
- 130719
- 3 0.190 0.162 85.5 0.199 0.184 92.2 Average ± %RSD 88.1 % ± 2.7 % 88.6 % ± 4.4 % LCS
- 130719
- 4 1.90 1.84 97.0 1.99 1.93 97.0 LCS
- 130719
- 5 1.90 1.72 90.5 1.99 2.02 101 LCS
- 130719
- 6 1.90 1.64 86.5 1.99 1.80 90.6 Average ± %RSD 91.3 % ± 5.8 % 96.2 % ± 5.5 % LCS
- 130719
- 7 19.0 15.4 81.1 19.9 16.1 80.9 LCS
- 130719
- 8 19.0 15.9 83.9 19.9 16.5 82.9 LCS
- 130719
- 9 19.0 16.1 84.5 19.9 16.4 82.6 Average ± %RSD 83.2 % ± 2.2 % 82.1 % ± 1.3 %
ETS
- 8
- 044.1 Analyzed 7/19/13 Internal Standard 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
- 130719
- 1 0.199 0.188 94.3 0.184 0.176 95.7 LCS
- 130719
- 2 0.199 0.184 92.6 0.184 0.171 93.1 LCS
- 130719
- 3 0.199 0.166 83.3 0.184 0.180 97.6 Average ± %RSD 90.1 % ± 6.6 % 95.5 % ± 2.4 % LCS
- 130719
- 4 1.99 1.95 98.0 1.84 1.76 95.9 LCS
- 130719
- 5 1.99 2.10 105 1.84 1.82 98.8 LCS
- 130719
- 6 1.99 1.90 95.5 1.84 1.78 96.8 Average ± %RSD 99.5 % ± 4.9 % 97.2 % ± 1.5 % LCS
- 130719
- 7 19.9 16.1 81.0 18.4 15.4 83.6 LCS
- 130719
- 8 19.9 16.4 82.3 18.4 16.3 88.4 LCS
- 130719
- 9 19.9 17.1 86.1 18.4 15.7 85.1 Average ± %RSD 83.1 % ± 3.2 % 85.7 % ± 2.7 %3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 13 OF 21 

### Table 8 continued. Lab Control Spike Results
ETS
- 8
- 044.1 Analyzed 8/21/13 External Standard C alibration PFOA (Linear and Branched)

Lab ID Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery LCS
- 130820
- 1 0.958 0.830 86.6 LCS
- 130820
- 2 0.958 0.917 95.7 LCS
- 130820
- 3 0.958 0.900 94.0 Average ± %RSD 92.1 % ± 5.3 % LCS
- 130820
- 4 9.58 10.0 104 LCS
- 130820
- 5 9.58 10.1 105 LCS
- 130820
- 6 9.58 10.3 107 Average ± %RSD 105 % ± 1.5 % LCS
- 130820
- 7 38.2 39.3 103 LCS
- 130820
- 8 38.2 39.8 104 LCS
- 130820
- 9 38.2 40.9 107 Average ± %RSD 105 % ± 2.0 %



## 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 O A by ex te rnal standard calibration was ± 15 %. However, t he recovery of the mid set of LCS analyzed on 7/16 /13 was 12 1 % for PF O A by external standard calibration for the samples analyzed on this date. The refore, the analytical method uncertainty was expanded for sa mples analyzed by external standard calibration for PFOA to ± 2 1 %. Table 9
. Analytical Method Uncertainty Analyte Calibration Standard Deviation (%) Method Uncertainty PFOA External NA ±21 % PFBS External 6.42 ±13 % PFH S External 7.13 ±14 % PFOS External 8.24 ±16 % PFOA Internal 5.28 ±11% PFBS Internal 6.08 ±12% PFHS Internal 5.98 ± 12 % PFOS Internal 6.16 ± 12 % NA = Not Applicable3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 14 OF 21 

## 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 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. The locations for which FMS sample containers were prepared are listed in Table 10

. An appropriate field matrix spike was not available for PFOA for sampling locati ons 135S and 135L; therefore, a laborator y matrix spike was prepared on the primary sample to verify that the method was appropriate for these two locations. 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 − =


### Table 10 . Field Matrix Spike (FMS) and Lab Matrix Spike (LMS) Concentrations

Sampling location Spike Level PFO A ng/mL PFBS ng/mL PF HS ng/mL PF OS ng/mL 137L and 138L FMS 1.00 1.00 0.999 1.00 134S and 135S FMS 20.0 20.1 20.0 19.9 130S, 135L, and 140R FMS 100 100 99.8 99.4 130R FMS 501 502 499 497 134R FMS 1002 1004 998 994 Trip Blank FMS Low 1.00 1.00 0.999 1.00 FMS Mid 100 100 99.8 99.4 FMS High 1002 1004 998 994 ISO13
- 05
- 02
- 031 (135S) LMS 99.0 NA NA NA ISO13
- 05
- 02
- 034 (135L) LMS 1000 NA NA NA 

## 4 Data Summary and Discussion
Tables 11 - 20 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 duplicate. Results and average values are rounded to three significant figures. Percent relative difference (%RPD) values are rounded to two significant figures. Because of rounding, values may vary slightly from those listed in the raw data. Field matrix spikes meeting the method acceptance criteria of ± 30%, demonstrate that the method is appropriate for the given matrix.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 15 OF 21 

### All target analyte field matrix spike s met method acceptance criteria with the following exceptions:

• DAL
- GW
- 130R ; The FMS recovery for PFOA was 67.8%. The analytical uncertainty for this location was expanded to ± 32%.

• DAL
- GW
- 134S ; The FMS recovery for PFOA was 60.6%. The analytical uncertainty for this location was expanded to ± 39%.

• DAL
- GW
- 135S ; The FMS recovery for PF HS was 69.4 %. The analytical uncertainty for this location was expanded to ± 31 %. An appropriate field matrix spike was not available for PFOA for sampling locations DAL GW 135S and DAL GW 135L; therefore, a laboratory matrix spike was prepared on the primary sample to verify that the method was appropriate for these two locations. The laboratory matrix spike recoveries met method acceptance criteria.

Table 11
. DAL - GW - 130R

PFO A PF BS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 001 DAL
- GW
- 130R
- 0
- 130626 881 NA 15.0 NA ISO13
- 05
- 02
- 002 DAL
- GW
- 130R
- DB
- 130626 1000 NA 17.6 NA ISO13
- 05
- 02
- 003 DAL
- GW
- 130R
- FMS
- 130626 1280 67.8 (1) 527 102 Average Concentration (ng/mL) ± %RPD 941 ng/mL ± 13 % (1) 16.3 ng/mL ± 16 %
PFH S PFOS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 001 DAL
- GW
- 130R
- 0
- 130626 122 NA 524 NA ISO13
- 05
- 02
- 002 DAL
- GW
- 130R
- DB
- 130626 141 NA 600 NA ISO13
- 05
- 02
- 003 DAL
- GW
- 130R
- FMS
- 130626 661 106 1090 106 Average Concentration (ng/mL) ± %RPD 132 ng/mL ± 14 % 562 ng/mL ± 14 % NA = Not Applicable Samples were diluted 1:20 and analyzed using external standard quantitation. (1) FMS did not meet method acceptance criteria of ± 30. The analytical uncertainty was expanded to ± 32 %.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 16 OF 21 

### Table 12
. DAL - GW - 130S

PFO A PF BS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 004 DAL
- GW
- 130S
- 0
- 130626 190 NA 3.55 NA ISO13
- 05
- 02
- 005 DAL
- GW
- 130S
- DB
- 130626 186 NA 3.37 NA ISO13
- 05
- 02
- 006 DAL
- GW
- 130S
- FMS
- 130626 273 84.8 103 99.1 Average Concentration (ng/mL) ± %RPD 188 ng/mL ± 2.1 % 3.46 ng/mL ± 5.2 %
PFH S PFOS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 004 DAL
- GW
- 130S
- 0
- 130626 31.3 NA 142 NA ISO13
- 05
- 02
- 005 DAL
- GW
- 130S
- DB
- 130626 30.6 NA 143 NA ISO13
- 05
- 02
- 006 DAL
- GW
- 130S
- FMS
- 130626 136 105 248 106 Average Concentration (ng/mL) ± %RPD 31.0 ng/mL ± 2.3 % 143 ng/mL ± 0.70 % NA = Not Applicable Samples were diluted 1:10 and analyzed using external standard quantitation. 

### Table 13
. DA L - GW - 134R

PFO A PF BS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 021 DAL
- GW
- 134R
- 0
- 130626 1920 NA 49.7 NA ISO13
- 05
- 02
- 022 DAL
- GW
- 134R
- DB
- 130626 1920 NA 49.7 NA ISO13
- 05
- 02
- 023 DAL
- GW
- 134R
- FMS
- 130626 2620 69.9 825 77.2 Average Concentration (ng/mL) ± %RPD 1920 ng/mL ± 0.0 % 49.7 ng/mL ± 0.0 %
PFH S PFOS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 021 DAL
- GW
- 134R
- 0
- 130626 480 NA 1280 NA ISO13
- 05
- 02
- 022 DAL
- GW
- 134R
- DB
- 130626 483 NA 1270 NA ISO13
- 05
- 02
- 023 DAL
- GW
- 134R
- FMS
- 130626 1320 84.0 2210 94.1 Average Concentration (ng/mL) ± %RPD 482 ng/mL ± 0.62 % 1280 ng/mL ± 0.78 % NA = Not Applicable Samples were diluted 1:2 0 and analyzed using external standard quantitation.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 17 OF 21 

### Table 14

. DAL - GW - 134S

PFO A PF BS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 024 DAL
- GW
- 134S
- 0
- 130626 15.8 NA 0.384 NA ISO13
- 05
- 02
- 025 DAL
- GW
- 134S
- DB
- 130626 15.3 NA 0.395 NA ISO13
- 05
- 02
- 026 DAL
- GW
- 134S
- FMS
- 130626 27.7 60.6 (1) 15.4 74.8 Average Concentration (ng/mL) ± %RPD 15.6 ng/mL ± 3.2 % (1) 0.390 ng/mL ± 2.8 %
PFH S PFOS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 024 DAL
- GW
- 134S
- 0
- 130626 4.41 NA 17.5 NA ISO13
- 05
- 02
- 025 DAL
- GW
- 134S
- DB
- 130626 4.56 NA 17.5 NA ISO13
- 05
- 02
- 026 DAL
- GW
- 134S
- FMS
- 130626 19.5 75.2 33.2 79.0 Average Concentration (ng/mL) ± %RPD 4.49 ng/mL ± 3.3 % 17.5 ng/mL ± 0.0 % NA = Not Applicable Samples were diluted 1: 2 and analyzed using in ternal standard quantitation. (1) FMS did not meet method acceptance criteria of ± 30. The analytical uncertainty was expanded to ± 39 %. 

### Table 15
. DAL - GW - 135S

PFO A (1 ) PF BS (2)

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 031 DAL
- GW
- 135S
- 0
- 130703 40.5 NA 1.79 NA ISO13
- 05
- 02
- 032 DAL
- GW
- 135S
- DB
- 130703 40.2 NA 1.65 NA ISO13
- 05
- 02
- 033 DAL
- GW
- 135S
- FMS
- 130703 NA NA 16.5 73.6 ISO13
- 05
- 02
- 031 LMS DAL
- GW
- 135S
- 0
- 130703 LMS 137 97. 6 NA NA Average Concentration (ng/mL) ± %RPD 40.4 ng/mL ± 0.74 % 1.72 ng/mL ± 8.1 %
PFH S (2) PFOS (2)

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 031 DAL
- GW
- 135S
- 0
- 130703 16.0 NA 12.8 NA ISO13
- 05
- 02
- 032 DAL
- GW
- 135S
- DB
- 130703 14.3 NA 10.7 NA ISO13
- 05
- 02
- 033 DAL
- GW
- 135S
- FMS
- 130703 29.0 69.4 (3 ) 26.5 74.2 ISO13
- 05
- 02
- 031 LMS DAL
- GW
- 135S
- 0
- 130703 LMS NA NA NA NA Average Concentration (ng/mL) ± %RPD 15.2 ng/mL ± 11 % (3 ) 11.8 ng/mL ± 18 % NA = Not Applicable (1) Samples were diluted 1:10 and analyzed using external standard quantitation. (2) Samples were diluted 1:2 and analyzed using internal standard quantitation. (3) FMS did not meet method acceptance criteria of ± 30. The analytical uncertainty was expanded to ± 31%.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
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PAGE 18 OF 21 

### Table 16
. DAL - GW - 135L

PFO A (1 ) PF BS (2 )

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 034 DAL
- GW
- 135L
- 0
- 130703 574 NA 15.1 NA ISO13
- 05
- 02
- 035 DAL
- GW
- 135L
- DB
- 130703 592 NA 14.9 NA ISO13
- 05
- 02
- 036 DAL
- GW
- 135L
- FMS
- 130703 NA NA 114 98.6 ISO13
- 05
- 02
- 034 LMS DAL
- GW
- 135L
- 0
- 130703 LMS 1510 9 2.7 NA NA Average Concentration (ng/mL) ± %RPD 583 ng/mL ± 3.1 % 15.0 ng/mL ± 1.3 %
PFH S ( 2 ) PFOS (2 )

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 034 DAL
- GW
- 135L
- 0
- 130703 130 NA 147 NA ISO13
- 05
- 02
- 035 DAL
- GW
- 135L
- DB
- 130703 128 NA 156 NA ISO13
- 05
- 02
- 036 DAL
- GW
- 135L
- FMS
- 130703 229 100 250 99.1 ISO13
- 05
- 02
- 034 LMS DAL
- GW
- 135L
- 0
- 130703 LMS NA NA NA NA Average Concentration (ng/mL) ± %RPD 129 ng/mL ± 1.6 % 152 ng/mL ± 5.9 % NA = Not Applicable NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concentration. (1) Samples were diluted 1:50 and analyzed using external standard quantitation. (2) Samples were diluted 1:10 and analyzed using external standard quantitation. 

### Table 17
. DAL - GW - 137L

PFO A PF BS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 047 DAL
- GW
- 137L
- 0
- 130626 0.355 NA 0.0775 NA ISO13
- 05
- 02
- 048 DAL
- GW
- 137L
- DB
- 130626 0.384 NA 0.0725 NA ISO13
- 05
- 02
- 049 DAL
- GW
- 137L
- FMS
- 130626 1.13 76.1 0.897 82.2 Average Concentration (ng/mL) ± %RPD 0.370 ng/mL ± 7.8 % 0.0750 ng/mL ± 6.7 %
PFH S PFOS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 047 DAL
- GW
- 137L
- 0
- 130626 0.0906 NA 1.17 NA ISO13
- 05
- 02
- 048 DAL
- GW
- 137L
- DB
- 130626 0.0871 NA 1.21 NA ISO13
- 05
- 02
- 049 DAL
- GW
- 137L
- FMS
- 130626 0.982 89.4 2.06 87.0 Average Concentration (ng/mL) ± %RPD 0.0889 ng/mL ± 3.9 % 1.19 ng/mL ± 3.4 % NA = Not Applicable Samples were diluted 1:2 and analyzed using internal standard quantitation.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
- 05
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PAGE 19 OF 21 

### Table 18
. DAL - GW - 138L

PFO A PF BS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 054 DAL
- GW
- 138L
- 0
- 130628 1.21 NA 0.0529 NA ISO13
- 05
- 02
- 055 DAL
- GW
- 138L
- DB
- 130628 1.10 NA 0.0433 NA ISO13
- 05
- 02
- 056 DAL
- GW
- 138L
- FMS
- 130628 1.89 73.5 0.872 82.4 Average Concentration (ng/mL) ± %RPD 1.16 ng/mL ± 9.5 % 0.0481 ng/mL ± 20 %

PFH S PFOS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 054 DAL
- GW
- 138L
- 0
- 130628 0.139 NA 0.638 NA ISO13
- 05
- 02
- 055 DAL
- GW
- 138L
- DB
- 130628 0.159 NA 0.687 NA ISO13
- 05
- 02
- 056 DAL
- GW
- 138L
- FMS
- 130628 1.01 86.2 1.51 84.8 Average Concentration (ng/mL) ± %RPD 0.149 ng/mL ± 13 % 0.663 ng/mL ± 7.4 % NA = Not Applicable Samples were diluted 1:2 and analyzed using internal standard quantitation.



### Table 19
. Trip Blank

PFO A PF BS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 074 DAL
- GW
- TRIP
- 0
- <0.0240 (1 ) NA <0.0250 (1 ) NA ISO13
- 05
- 02
- 075 DAL
- GW
- TRIP
- LS
- 0.757 (1 ) 75.7 0.819 (1 ) 81.9 ISO13
- 05
- 02
- 076 DAL
- GW
- TRIP
- MS
- 92.4 (2 ) 92.2 109 (2 ) 109 ISO13
- 05
- 02
- 077 DAL
- GW
- TRIP
- HS
- 774 (2) 77.2 931 (2 ) 92.7
PFH S PFOS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery ISO13
- 05
- 02
- 074 DAL
- GW
- TRIP
- 0
- <0.0250 (1 ) NA <0.0232 ( 1 ) NA ISO13
- 05
- 02
- 075 DAL
- GW
- TRIP
- LS
- 0.877 (1 ) 87.8 0.745 (1 ) 74.5 ISO13
- 05
- 02
- 076 DAL
- GW
- TRIP
- MS
- 105 (2 ) 105 101 (2 ) 102 ISO13
- 05
- 02
- 077 DAL
- GW
- TRIP
- HS
- 976 (2 ) 97.8 1000 (2) 101 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.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13
- 05
- 02

PAGE 20 OF 21 

### Table 20
. 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
- 02
- 072 DAL
- GW
- 141R
- RB
- 130702 <0.0240 <0.0250 <0.0250 <0.0232 ISO13
- 05
- 02
- 073 DAL
- GW
- 130S
- RB
- 130626 <0.0240 <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 recoveries 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 1 1
- 20 of this report. 

## 6 Data / Sample Retention All remaining sample and associated project data (hardcopy and electronic) will be archived according to 3M Environmental Laboratory standard operating procedures.3M ENVIRONMENTAL LABORATORY REPORT

NO. ISO13-05-02



## 7 Signature s

Susa n T

. Wolf , 3 M Pripqipa 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 Quality Assuranc e Uni t ha s audite d th e dat a an d repor t fo r thi s project

.

Qualit y Assurat^p 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 1 O F 2 1