3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-02

PAGE 1 OF 21

Final Report

Analysis of PFOA, PFBS, PFHS, and PFOS in Ground Water Samples Collected at 

the Former Sludge Incorporation Area (FSIA) from Decatur, AL

2nd Quarter 2013

Laboratory Request Number: ISO13-05-02

Method Requirement: 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 

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 LABORATORY

REPORT NO. ISO13-05-02

PAGE 2 OF 21

3M Environmental Laboratory

3M Environmental Laboratory Technical 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

2nd 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. Samples 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, 2013

at ambient conditions. All samples were analyzed for perfluorooctanoic acid (PFOA), perfluorobutane 

sulfonate (PFBS), perfluorohexane sulfonate (PFHS) and perfluorooctane sulfonate (PFOS) under 

laboratory project number ISO13-05-02.

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-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, PFBS, PFHS, 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 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 LABORATORY

REPORT NO. ISO13-05-02

PAGE 3 OF 21

Table 1. Sample Results Summary (1)

3M LIMS ID Sample Description 

PFOA 

Concentration 

(ng/mL)

PFBS 

Concentration 

(ng/mL)

PFHS 

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

ISO13-05-02-010 DAL-GW-131R-DB-130703 2290 53.4 317 1360

Average 2380 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

ISO13-05-02-015 DAL-GW-133R-0-130703 52.6 2.63 15.5 29.0

ISO13-05-02-016 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

ISO13-05-02-017 DAL-GW-133S-0-130703 379 9.11 70.8 307

ISO13-05-02-018 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 external 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 ±39% for PFOA. See section 4 for further discussion. 

(6) The analytical method uncertainty has been expanded to ±31% for PFHS. See section 4 for further discussion. 
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-02

PAGE 4 OF 21

Table 1 continued. Sample Results Summary (1)

3M LIMS ID Sample Description 

PFOA 

Concentration 

(ng/mL)

PFBS 

Concentration 

(ng/mL)

PFHS 

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

ISO13-05-02-028 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

ISO13-05-02-030 DAL-GW-135R-DB-130703 3420 59.5 727 1120

Average 3470 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

ISO13-05-02-032 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 574 15.1 130 147

ISO13-05-02-035 DAL-GW-135L-DB-130703 592 14.9 128 156

Average 583 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 external 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 ±39% for PFOA. See section 4 for further discussion. 

(6) The analytical method uncertainty has been expanded to ±31% for PFHS. See section 4 for further discussion. 
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-02

PAGE 5 OF 21

Table 1 continued. Sample Results Summary (1)

3M LIMS ID Sample Description 

PFOA 

Concentration 

(ng/mL)

PFBS 

Concentration 

(ng/mL)

PFHS 

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

ISO13-05-02-060 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 external 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 ±39% for PFOA. See section 4 for further discussion. 

(6) The analytical method uncertainty has been expanded to ±31% for PFHS. See section 4 for further discussion. 
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-02

PAGE 6 OF 21

Table 1 continued. Sample Results Summary (1)

3M LIMS ID Sample Description 

PFOA 

Concentration 

(ng/mL)

PFBS 

Concentration 

(ng/mL)

PFHS 

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 external 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 ±39% for PFOA. See section 4 for further discussion. 

(6) The analytical method uncertainty has been expanded to ±31% 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) PFOA Linear and Branched

Perfluorooctanoic Acid (C8 Acid) PFBS Linear

Perfluorobutanesulfonate (C4 Sulfonate ) PFHS Linear

Perfluorooctanesulfonate (C8 Sulfonate) PFOS Linear and Branched

2.2 Sample Collection

All samples were collected in 250 mL NalgeneTM (high-density polyethylene) bottles prepared at the 3M 

Environmental Laboratory. Samples 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, 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 PFOA, PFBS, 

PFHS, and PFOS. 
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-02

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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. 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. 

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 bottles 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 

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:

• 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 high FMS.

• 7/19/13: Direct injection / internal standard analysis for PFOA, PFBS, PFHS, PFOS (samples 

extracted 7/19/13); locations 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 high FMS.

• 8/21/13: Solvent dilution/external standard analysis for PFOA (samples prepared on 8/20/13); 

locations 135S and 135L. 
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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 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 1100

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 

(μL/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 10.0
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REPORT NO. ISO13-05-02

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Table 6. Mass Transitions

Analyte

Mass Transition

Q1/Q3

Internal Standard Mass Transition

Q1/Q3

Reference Material 

Structure

PFOA

413/369

[

13C8]PFOA (1) 413/219 421/376 Linear and Branched

413/169

PFBS

299/80

[

18O2]PFBS (1) 303/84 Linear

299/99

PFHS

399/99

[

13C3]PFHS (1) 402/99 Linear

399/80

PFOS

499/99

[

13C8]-PFOS (1) 499/80 507/80 Linear and Branched

499/130

Dwell time was 50 msec for each transition. The individual transitions were summed to produce a “total ion chromatogram” 

(TIC), which was used 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 / external standard calibration.

Diluted samples were analyzed against an external 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 calibration 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 were not 

forced through zero during the fitting process. Calculating the standard concentration using the peak 

area counts and the resultant calibration curve confirmed accuracy of each curve point. 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 / internal 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 laboratoryprepared 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 samples ranging 

from 0.0125 ng/mL to 50 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, 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.

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 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 criteria were met for all analytes.
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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 

associated with the sample analysis are listed in the table below.

Table 7. LOQ

Analysis 

Date Calibration Dilution Factor

PFOA

LOQ, ng/mL

PFBS

LOQ, ng/mL

PFHS

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 with the samples: method/procedural blanks, a 

field/trip blank, and a single equipment rinseate blank. Method blank results 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 groundwater 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 analysis. The 

method acceptance criteria, average of each level of LCS should be within 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 PFOA (121%).

A method deviation is filed in the raw data. All batch LCS recovery results were used in the evaluation 

of the analytical method uncertainty in section 3.7 of the report. 

The following calculations were used to generate data in Table 8.

* 100%

Spike Concentration

Calculated Concentration LCSPercent Recovery =
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-02

PAGE 11 OF 21

* 100%

average LCS recovery

standard deviation LCS replicates LCS% RSD =

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 107% ± 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) 114% ± 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 102% ± 2.0% 102% ± 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 118% ± 1.3% 116% ± 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%.
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Table 8 continued. Lab Control Spike Results 

ETS-8-044.1

Analyzed 7/19/13

Internal 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-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 

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-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%
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Table 8 continued. Lab Control Spike Results 

ETS-8-044.1

Analyzed 8/21/13

External Standard 

Calibration 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 PFOA by external 

standard calibration was ±15%. However, the recovery of the mid set of LCS analyzed on 

7/16/13 was 121% for PFOA by external standard calibration for the samples analyzed 

on this date. Therefore, the analytical method uncertainty was expanded for samples 

analyzed by external standard calibration for PFOA to ±21%.

Table 9. Analytical Method Uncertainty

Analyte Calibration Standard Deviation (%) Method Uncertainty

PFOA External NA ±21%

PFBS External 6.42 ±13%

PFHS 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 Applicable
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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 target 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 locations 135S and 135L; 

therefore, a laboratory 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%

Spike Concentraton

(Sample Concentration of FMS Average Concentration:FieldSample & FieldSample Dup.) FMS Recovery − =

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

Sampling location

Spike 

Level

PFOA

ng/mL

PFBS

ng/mL

PFHS

ng/mL

PFOS

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 Trip Blank. Each table provides the average concentration and 

the relative percent difference (%RPD) of the sample and sample duplicate. Results and average 

values are rounded to three significant figures. Percent relative difference (%RPD) values are rounded 

to two significant figures. Because of rounding, values may vary slightly from those listed in the raw 

data. Field matrix spikes meeting the method acceptance criteria of ± 30%, demonstrate that the 

method is appropriate for the given matrix. 
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All target analyte field matrix spikes 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 PFHS 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

PFOA PFBS

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%

PFHS 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%.
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REPORT NO. ISO13-05-02

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Table 12. DAL-GW-130S

PFOA PFBS

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%

PFHS 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. DAL-GW-134R

PFOA PFBS

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%

PFHS 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 1:20 and analyzed using external standard quantitation. 
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Table 14. DAL-GW-134S

PFOA PFBS

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%

PFHS 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 internal standard quantitation. 

(1) FMS did not meet method acceptance criteria of ±30. The analytical uncertainty was expanded to ±39%.

Table 15. DAL-GW-135S

PFOA (1) PFBS (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%

PFHS (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%.
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REPORT NO. ISO13-05-02

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Table 16. DAL-GW-135L

PFOA (1) PFBS (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 92.7 NA NA

Average Concentration (ng/mL) ± %RPD 583 ng/mL ± 3.1% 15.0 ng/mL ± 1.3%

PFHS (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

PFOA PFBS

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%

PFHS 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. 
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REPORT NO. ISO13-05-02

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Table 18. DAL-GW-138L

PFOA PFBS

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%

PFHS 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

PFOA PFBS

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

PFHS 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.
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REPORT NO. ISO13-05-02

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Table 20. Rinseate Blank

PFOA PFBS PFHS 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 11-20 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 Signatures 

Susan T. Wolf, 3M Pripqipal Analytical Investigator Date 

William K. Reagen, Ph.D., 3M Environmental Technical Director Date 

The 3M Environmental Laboratory's Quality Assurance Unit has audited the data and report for this 

project. 

Quality Assurat^pe Representative Date 

This test report shall not be reproduced except in full, without written approval of the 3M 

Environmental Laboratory. 

PAGE 21 OF 21