3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO14-05-02

PAGE 1 OF 24

Final Report

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

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

1st Quarter 2014

Laboratory Request Number: ISO14-05-02

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 A2LA Certificate # 2052.01. 

Additionally, the laboratory’s quality system has been audited and was 

determined to be in conformance with the EPA GLPs (40 CFR 792) by an 

independent assessment. 
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO14-05-02

PAGE 2 OF 24

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 ISO14-05-02

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

Former Sludge Incorporation Area (FSIA) from Decatur, AL

1st Quarter 2014

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 March 11, March 12 and March 13, 

2014 and returned to the 3M Environmental Laboratory on March 14, 2014 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 ISO14-05-02.

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 a target analyte field matrix 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 and DAL-GW-137R were not collected due to the wells being dry.

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 A2LA Certificate # 2052.01. 

Additionally, the laboratory’s quality system has been audited and was 

determined to be in conformance with the EPA GLPs (40 CFR 792) by an 

independent assessment.
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO14-05-02

PAGE 3 OF 24

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)

ISO14-05-02-001 DAL-GW-130R-0-140312 875 17.0 115 522

ISO14-05-02-002 DAL-GW-130R-DB-140312 851 16.5 124 506

Average 863 16.8 120 514

%RPD Sample/Sample Dup 2.8 3.0 7.5 3.1

ISO14-05-02-003 DAL-GW-130S-0-140313 186 4.58 33.6 148

ISO14-05-02-004 DAL-GW-130S-DB-140313 197 4.06 36.2 148

Average 192 4.32 34.9 148

%RPD Sample/Sample Dup 5.7 12 7.4 0.0

ISO14-05-02-005 DAL-GW-130L-0-140312 57.5 1.59 10.7 66.8

ISO14-05-02-006 DAL-GW-130L-DB-140312 58.6 1.56 10.6 68.9

Average 58.1 1.58 10.7 67.9

%RPD Sample/Sample Dup 1.9 1.9 0.94 3.1

ISO14-05-02-008 DAL-GW-131R-0-140311 2510 64.7 384 1120

ISO14-05-02-009 DAL-GW-131R-DB-140311 2490 71.7 355 1170

Average 2500 68.2 370 1150

%RPD Sample/Sample Dup 0.80 10 7.8 4.4

ISO14-05-02-010 DAL-GW-131S-0-140312 38.7 1.03 6.28 7.03

ISO14-05-02-011 DAL-GW-131S-DB-140312 35.6 0.962 5.88 6.62

Average 37.22) 0.996 (2) 6.08 (2) 6.83 (2)

%RPD Sample/Sample Dup 8.3 6.8 6.6 6.0

ISO14-05-02-013 DAL-GW-131L-0-140312 119 2.94 22.2 45.3

ISO14-05-02-014 DAL-GW-131L-DB-140312 110 3.02 20.9 46.1

Average 115 (2) 2.98 (2) 21.6 (2) 45.7 (2)

%RPD Sample/Sample Dup 7.9 2.7 6.0 1.8

ISO14-05-02-016 DAL-GW-133R-0-140311 60.6 2.37 15.4 25.3

ISO14-05-02-017 DAL-GW-133R-DB-140311 58.9 2.19 15.5 25.5

Average 59.8 (2) 2.28 (2) 15.5 (2) 25.4 (2)

%RPD Sample/Sample Dup 2.8 7.9 0.65 0.79

ISO14-05-02-018 DAL-GW-133S-0-140311 439 10.8 76.2 336

ISO14-05-02-019 DAL-GW-133S-DB-140311 378 9.82 70.5 301

Average 409 10.3 73.4 319

%RPD Sample/Sample Dup 15 9.5 7.8 11

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 ± 17%, PFBS ± 12%, PFHS ± 14%, and PFOS ± 14%.

(2) All samples associated with the reported sampling location were analyzed by internal standard calibration. The analytical 

method uncertainties for the reported results using method ETS-8-044.1 by direct injection are as follows: PFOA ± 18%, 

PFBS ± 22%, PFHS ± 24%, and PFOS ± 20%.

(3) The analytical uncertainty for location 140R was expanded to ±37% for PFOA. See section 4 of the report for additional 

information.

(4) The analytical uncertainty for location 142R was expanded to ±48% for PFOA. See section 4 of the report for additional 

information.

(5) The RPD value did not meet method acceptance criteria of ≤20%.
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO14-05-02

PAGE 4 OF 24

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)

ISO14-05-02-020 DAL-GW-133L-0-140311 457 9.43 74.0 525

ISO14-05-02-021 DAL-GW-133L-DB-140311 420 9.62 71.3 503

Average 439 9.53 72.7 514

%RPD Sample/Sample Dup 8.4 2.0 3.7 4.3

ISO14-05-02-023 DAL-GW-134R-0-140313 2130 53.2 512 1420

ISO14-05-02-024 DAL-GW-134R-DB-140313 2210 50.9 527 1470

Average 2170 52.1 520 1450

%RPD Sample/Sample Dup 3.7 4.4 2.9 3.5

ISO14-05-02-025 DAL-GW-134S-0-140313 23.8 0.502 6.04 23.9

ISO14-05-02-026 DAL-GW-134S-DB-140313 23.4 0.490 6.15 23.9

Average 23.6 (2) 0.496 (2) 6.10 (2) 23.9 (2)

%RPD Sample/Sample Dup 1.7 2.4 1.8 0.0

ISO14-05-02-027 DAL-GW-134L-0-140313 521 10.3 92.7 494

ISO14-05-02-028 DAL-GW-134L-DB-140313 518 9.48 92.7 508

Average 520 9.89 92.7 501

%RPD Sample/Sample Dup 0.58 8.3 0.0 2.8

ISO14-05-02-029 DAL-GW-135R-0-140313 4000 65.2 721 1450

ISO14-05-02-030 DAL-GW-135R-DB-140313 4240 65.0 746 1490

Average 4120 65.1 734 1470

%RPD Sample/Sample Dup 5.8 0.31 3.4 2.7

ISO14-05-02-031 DAL-GW-135S-0-140313 94.4 2.26 25.9 23.8

ISO14-05-02-032 DAL-GW-135S-DB-140313 89.2 2.25 26.3 24.3

Average 91.8 (2) 2.26 (2) 26.1 (2) 24.1 (2)

%RPD Sample/Sample Dup 5.7 0.44 1.5 2.1

ISO14-05-02-033 DAL-GW-135L-0-140313 371 11.6 81.1 91.4

ISO14-05-02-034 DAL-GW-135L-DB-140313 381 12.1 75.8 93.7

Average 376 11.9 78.5 92.6

%RPD Sample/Sample Dup 2.7 4.2 6.8 2.5

ISO14-05-02-037 DAL-GW-136S-0-140311 114 3.19 20.2 130

ISO14-05-02-038 DAL-GW-136S-DB-140311 117 3.43 20.1 124

Average 116 3.31 20.2 127

%RPD Sample/Sample Dup 2.6 7.3 0.50 4.7

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 ± 17%, PFBS ± 12%, PFHS ± 14%, and PFOS ± 14%.

(2) All samples associated with the reported sampling location were analyzed by internal standard calibration. The analytical 

method uncertainties for the reported results using method ETS-8-044.1 by direct injection are as follows: PFOA ± 18%, 

PFBS ± 22%, PFHS ± 24%, and PFOS ± 20%.

(3) The analytical uncertainty for location 140R was expanded to ±37% for PFOA. See section 4 of the report for additional 

information.

(4) The analytical uncertainty for location 142R was expanded to ±48% for PFOA. See section 4 of the report for additional 

information.

(5) The RPD value did not meet method acceptance criteria of ≤20%.
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO14-05-02

PAGE 5 OF 24

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)

ISO14-05-02-039 DAL-GW-136L-0-140311 92.9 2.48 15.7 93.8

ISO14-05-02-040 DAL-GW-136L-DB-140311 93.5 2.40 17.2 95.5

Average 93.2 2.44 16.5 94.7

%RPD Sample/Sample Dup 0.64 3.3 9.1 1.8

ISO14-05-02-043 DAL-GW-137S-0-140312 1.38 0.201 0.255 0.697

ISO14-05-02-044 DAL-GW-137S-DB-140312 1.38 0.175 0.275 0.708

Average 1.38 (2) 0.188 (2) 0.265 (2) 0.703 (2)

%RPD Sample/Sample Dup 0.0 14 7.5 1.6

ISO14-05-02-045 DAL-GW-137L-0-140312 0.460 0.101 0.109 1.68

ISO14-05-02-046 DAL-GW-137L-DB-140312 0.474 0.108 0.119 1.70

Average 0.467 (2) 0.1052) 0.114 (2) 1.69 (2)

%RPD Sample/Sample Dup 3.0 6.7 8.8 1.2

ISO14-05-02-047 DAL-GW-138R-0-140313 306 9.67 37.4 368

ISO14-05-02-048 DAL-GW-138R-DB-140313 307 7.68 37.9 370

Average 307 8.68 37.7 369

%RPD Sample/Sample Dup 0.33 23(3) 1.3 0.54

ISO14-05-02-049 DAL-GW-138S-0-140313 208 6.02 26.2 316

ISO14-05-02-050 DAL-GW-138S-DB-140313 203 5.63 26.4 294

Average 206 5.83 26.3 305

%RPD Sample/Sample Dup 2.4 6.7 0.76 7.2

ISO14-05-02-052 DAL-GW-138L-0-140313 0.523 <0.0250 0.0691 0.362

ISO14-05-02-053 DAL-GW-138L-DB-140313 0.552 0.0324 0.0688 0.362

Average 0.538 (2) 0.0324 (2) 0.0690 (2) 0.362 (2)

%RPD Sample/Sample Dup 5.4 NA 0.44 0.0

ISO14-05-02-054 DAL-GW-CW26C-0-140311 417 7.76 57.6 430

ISO14-05-02-055 DAL-GW-CW26C-DB-140311 420 7.51 58.1 442

Average 419 7.64 57.9 436

%RPD Sample/Sample Dup 0.72 3.3 0.86 2.8

ISO14-05-02-056 DAL-GW-CW26L-0-140311 973 15.9 122 1570

ISO14-05-02-057 DAL-GW-CW26L-DB-140311 948 15.6 122 1530

Average 961 15.8 122 1550

%RPD Sample/Sample Dup 2.6 1.9 0.0 2.6

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 ± 17%, PFBS ± 12%, PFHS ± 14%, and PFOS ± 14%.

(2) All samples associated with the reported sampling location were analyzed by internal standard calibration. The analytical 

method uncertainties for the reported results using method ETS-8-044.1 by direct injection are as follows: PFOA ± 18%, 

PFBS ± 22%, PFHS ± 24%, and PFOS ± 20%.

(3) The analytical uncertainty for location 140R was expanded to ±37% for PFOA. See section 4 of the report for additional 

information.

(4) The analytical uncertainty for location 142R was expanded to ±48% for PFOA. See section 4 of the report for additional 

information.

(5) The RPD value did not meet method acceptance criteria of ≤20%.
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO14-05-02

PAGE 6 OF 24

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)

ISO14-05-02-058 DAL-GW-140R-0-140312 113 1.45 14.4 127

ISO14-05-02-059 DAL-GW-140R-DB-140312 116 1.49 15.5 131

Average 115 (3) 1.47 15.0 129

%RPD Sample/Sample Dup 2.6 2.7 7.4 3.1

ISO14-05-02-061 DAL-GW-141R-0-140313 2.45 0.0769 0.383 6.74

ISO14-05-02-062 DAL-GW-141R-DB-140313 2.60 0.0670 0.404 6.83

Average 2.53 (2) 0.0720 (2) 0.394 (2) 6.79 (2)

%RPD Sample/Sample Dup 5.9 14 5.3 1.3

ISO14-05-02-064 DAL-GW-142R-0-140312 76.8 2.59 13.7 204

ISO14-05-02-065 DAL-GW-142R-DB-140312 75.1 2.67 15.0 208

Average 76.0 (4) 2.63 14.4 206

%RPD Sample/Sample Dup 2.2 3.0 9.1 1.9

ISO14-05-02-067 DAL-GW-143R-0-140313 27.0 1.33 5.22 24.5

ISO14-05-02-068 DAL-GW-143R-DB-140313 25.3 1.45 4.80 25.0

Average 26.2 (2) 1.39 (2) 5.01 (2) 24.8 (2)

%RPD Sample/Sample Dup 6.5 8.6 8.4 2.0

ISO14-05-02-069 DAL-GW-145R-0-140311 33.1 0.723 4.07 92.1

ISO14-05-02-070 DAL-GW-145R-DB-140311 32.2 0.899 3.90 89.9

Average 32.7 0.811 3.99 91.0

%RPD Sample/Sample Dup 2.8 22 (5) 4.3 2.4

ISO14-05-02-072 DAL-GW-TRIP-0-140313 <0.0240 <0.0250 <0.0250 <0.0232

ISO14-05-02-071 DAL-GW-141R-RB-140313 <0.0240 <0.0250 <0.0250 <0.0232

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 ± 17%, PFBS ± 12%, PFHS ± 14%, and PFOS ± 14%.

(2) All samples associated with the reported sampling location were analyzed by internal standard calibration. The analytical 

method uncertainties for the reported results using method ETS-8-044.1 by direct injection are as follows: PFOA ± 18%, 

PFBS ± 22%, PFHS ± 24%, and PFOS ± 20%.

(3) The analytical uncertainty for location 140R was expanded to ±37% for PFOA. See section 4 of the report for additional 

information.

(4) The analytical uncertainty for location 142R was expanded to ±48% for PFOA. See section 4 of the report for additional 

information.

(5) The RPD value did not meet method acceptance criteria of ≤20%.

2 Methods - Analytical and Preparatory

2.1 Methods

Analysis was completed using 3M Environmental Laboratory Method ETS-8-044.1 “Method of Analysis 

for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis”.
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO14-05-02

PAGE 7 OF 24

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 March 11, March 12 and March 13, 2014 and 

returned to the 3M Environmental Laboratory on March 14, 2014 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. 

Table 3. Sample Description Key Code.

String Number String Descriptor Example: DAL-GW-130R-DB-140312

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 140312 – March 12, 2014

2.3 Sample Preparation

3/26/14, 4/14/14: 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 spiking it with 0.1 mL of surrogate 

solution and diluting it with 8.9 mL of methanol. Samples requiring a 1:20 dilution were prepared by 

removing a 0.5 mL aliquot of the well mixed sample and spiking it with 0.1 mL of surrogate solution and 

diluting it with 9.4 mL of methanol. Samples requiring a 1:50 dilution were prepared by removing a 0.2 

mL aliquot of the well mixed sample and spiking it with 0.1 mL of surrogate solution and diluting it with 

9.7 mL of methanol. Samples requiring a 1:100 dilution were prepared by removing a 0.1 mL aliquot of 

the well mixed sample and spiking it with 0.1 mL of surrogate solution and diluting it with 9.8 mL of 

methanol.

4/10/14: All samples were prepared by adding 0.01 mL of a surrogate solution to 10.0 mL of sample 

and then removing a 0.4 mL aliquot of the well mixed sample and diluting it with 0.4 mL of methanol 

(dilution factor of 2). During the preparation of the laboratory control samples, an aliquot of a separate 

internal standard spiking solution was added to the laboratory control samples (nominal concentration 

of 1 ng/mL). The sample 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. 
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO14-05-02

PAGE 8 OF 24

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:

• 3/26/14: Solvent dilution / external standard analysis for PFOA, PFBS, PFHS, PFOS, and 

surrogates (samples extracted 3/26/14); locations 130R, 130S, 130L, 131R, 133S, 133L, 

134R, 134L, 135R, 135L, 136S, 136L, 138R, CW26C, CW26L, 145R, Trip Blank high FMS.

PFOA, PFBS, PFHS, and 13C4-PFOA; location 138S. PFBS, PFHS, PFOS, and 13

C4-PFOS; 

locations 140R and 142R. 

• 4/10/14: Solvent dilution / internal standard analysis for PFOA, PFBS, PFHS, PFOS and 

surrogates (samples extracted 4/10/13); locations 131S, 131L, 133R, 134S, 135S, 137S, 

137L, 138L, 141R, 143R, rinseate blanks, trip blank and trip blank low FMS. 

• 4/17/14: Solvent dilution / external standard analysis for PFOA and 13C4-PFOA (samples 

prepared 4/14/14); locations 140R and 142R. PFOS and 13C4-PFOS; location 138S. 

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 ETS McCoy

Analysis Dates 3/26/14 4/10/14

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

Liquid Chromatograph Agilent 1100 Agilent 1290

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

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

Injection Volume 5, 10, 25, μL(1) 10 μL

Mass Spectrometer Applied Biosystems API 4000 Applied Biosystems API 5500

Ion Source Turbo Spray Turbo Spray

Polarity Negative Negative

Software Analyst 1.6.1 Analyst 1.6.1
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO14-05-02

PAGE 9 OF 24

Table 4 continued. Instrument Parameters

Instrument Name ETS DaVinci

Analysis Dates 4/17/14

Analytical Method ETS-8-044.1 

Liquid Chromatograph Agilent 1290

Guard column Prism RP (2.1 mm X 50 mm), 5 μ

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

Injection Volume 5 μL

Mass Spectrometer Applied Biosystems API 6500

Ion Source Turbo Spray

Polarity Negative

Software Analyst 1.6.1

(1) Larger injection volumes were used for select samples to achieve a lower dilution factor.

Table 5. Liquid Chromatography Gradient Program

Step

Total Time 

(min)

Flow Rate 

(μL/min) 2 mM Ammonium Acetate Methanol

3/26/14, 4/10/14

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

Step

Total Time 

(min)

Flow Rate 

(μL/min) 2 mM Ammonium Acetate Methanol

4/17/14

0 0 300 90.0 10.0

1 0.5 300 90.0 10.0

2 4.0 300 70.0 30.0

3 6.0 300 70.0 30.0

4 11.0 300 20.0 80.0

5 13.0 300 20.0 80.0

6 13.5 300 10.0 90.0

7 16.0 300 10.0 90.0

8 16.5 300 90.0 10.0

9 19.0 300 90.0 10.0
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO14-05-02

PAGE 10 OF 24

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) 402/80 Linear

399/80

PFOS

499/99

[

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

499/130

[

13C4]PFOA surrogate 417/372 [13C8]PFOA (1) 421/376 Linear

[

13C4]PFOS surrogate 503/80 [13C8]PFOS (1) 507/80 Linear

Dwell time was 20 or 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 4/10/14. 

3 Data Analysis

3.1 Calibration

3/26/14, 4/17/14: Solvent dilution / external standard calibration.

Diluted samples were analyzed against an external standard calibration curve. 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.

4/10/14: 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 stock solutions into 50 mL of 50:50 

methanol: laboratory reagent water. The calibration standards contained an internal standard mix at a 

nominal concentration of 0.5 ng/mL. A total of fourteen spiked standards ranging from 0.0125 ng/mL to 

100 ng/mL (nominal) were analyzed with the prepared samples. Of these fourteen calibration 

standards, ten contained the surrogates at concentrations ranging from 0.0125 ng/mL to 10 ng/mL 

(nominal). A quadratic, 1/x weighted, calibration curve of the ratio of the standard peak area counts 

over the internal standard peak area counts was used to fit the data for each analyte.

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 
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO14-05-02

PAGE 11 OF 24

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, 

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

3/26/14 External standard

2 0.192 0.200 0.200 0.185

5 0.479 0.500 0.500 0.464

10 0.958 1.00 1.00 0.927

20 1.92 2.00 2.00 1.85

50 4.79 5.00 5.00 4.64

100 9.58 10.0 10.0 9.27

4/10/14 Internal standard 2 0.0240 0.0250 0.0250 0.0232

4/17/14 External standard 10 0.958 NA NA 0.927

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%, were met for all LCSs. 

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 =

* 100%

average LCS recovery

standard deviation LCS replicates LCS% RSD =
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REPORT NO. ISO14-05-02

PAGE 12 OF 24

Table 8. Lab Control Spike Results

ETS-8-044.1

Analyzed 3/26/14

External Standard 

Calibration PFOA (Linear and Branched) 13C4-PFOA

Lab ID

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

LCS-140326-1 0.479 0.430 89.7 0.499 0.473 94.7

LCS-140326-2 0.479 0.494 103 0.499 0.472 94.5

LCS-140326-3 0.479 0.427 89.1 0.499 0.553 111

Average ± %RSD 93.9% ± 8.4% 100% ± 9.5%

LCS-140326-4 4.79 4.66 97.3 4.99 5.39 108

LCS-140326-5 4.79 4.53 94.6 4.99 5.71 114

LCS-140326-6 4.79 4.59 95.9 4.99 5.34 107

Average ± %RSD 95.9% ± 1.4% 110% ± 3.5%

LCS-140326-7 38.2 35.9 94.0

LCS-140326-8 38.2 37.9 99.2

LCS-140326-9 38.2 36.8 96.4

Average ± %RSD 96.5% ± 2.7%

ETS-8-044.1

Analyzed 3/26/14

External Standard 

Calibration PFBS PFHS

Lab ID

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

LCS-140326-1 0.500 0.531 106 0.500 0.476 95.2

LCS-140326-2 0.500 0.543 109 0.500 0.506 101

LCS-140326-3 0.500 0.443 88.7 0.500 0.482 96.4

Average ± %RSD 101% ± 11% 97.5% ± 3.1%

LCS-140326-4 5.00 6.01 120 5.00 5.02 100

LCS-140326-5 5.00 5.44 109 5.00 5.19 104

LCS-140326-6 5.00 4.60 91.9 5.00 4.54 90.9

Average ± %RSD 107% ± 13% 98.3% ± 6.8%

LCS-140326-7 39.8 39.9 100 39.8 38.6 96.9

LCS-140326-8 39.8 41.0 103 39.8 38.3 96.0

LCS-140326-9 39.8 39.5 99.1 39.8 39.6 99.4

Average ± %RSD 101% ± 2.0% 97.4% ± 1.8%
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO14-05-02

PAGE 13 OF 24

Table 8 continued. Lab Control Spike Results 

ETS-8-044.1

Analyzed 3/26/14

External Standard 

Calibration PFOS (Linear and Branched) 13C4-PFOS

Lab ID

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

LCS-140326-1 0.464 0.416 89.8 0.478 0.413 86.3

LCS-140326-2 0.464 0.404 87.2 0.478 0.498 104

LCS-140326-3 0.464 0.402 86.8 0.478 0.514 108

Average ± %RSD 87.9% ± 1.9% 99.4% ± 12%

LCS-140326-4 4.63 4.77 103 4.78 5.11 107

LCS-140326-5 4.63 4.49 96.8 4.78 4.86 102

LCS-140326-6 4.63 4.32 93.3 4.78 4.61 96.4

Average ± %RSD 97.7% ± 5.0% 102% ± 5.2%

LCS-140326-7 36.9 35.7 96.6

LCS-140326-8 36.9 35.5 96.1

LCS-140326-9 36.9 36.3 98.2

Average ± %RSD 97.0% ± 1.1%

ETS-8-044.1

Analyzed 4/10/14

Internal Standard 

Calibration PFOA (Linear and Branched) 13C4-PFOA

Lab ID

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

LCS-140410-1 0.190 0.181 95.1 0.198 0.194 97.9

LCS-140410-2 0.190 0.173 91.1 0.198 0.196 98.8

LCS-140410-3 0.190 0.182 95.8 0.198 0.200 101

Average ± %RSD 94.0% ± 2.7% 99.2% ± 1.6%

LCS-140410-4 9.50 8.68 91.4 1.98 1.91 96.5

LCS-140410-5 9.50 9.35 98.4 1.98 1.86 94.1

LCS-140410-6 9.50 9.38 98.7 1.98 1.89 95.4

Average ± %RSD 96.2% ± 4.3% 95.3% ± 1.3%

LCS-140410-7 38.0 36.0 94.7

LCS-140410-8 38.0 36.8 96.9

LCS-140410-9 38.0 38.7 102

Average ± %RSD 97.9% ± 3.8%
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO14-05-02

PAGE 14 OF 24

Table 8 continued. Lab Control Spike Results 

ETS-8-044.1

Analyzed 4/10/14

Internal Standard 

Calibration PFBS PFHS

Lab ID

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

LCS-140410-1 0.198 0.170 86.0 0.198 0.184 93.1

LCS-140410-2 0.198 0.173 87.4 0.198 0.180 90.8

LCS-140410-3 0.198 0.170 85.7 0.198 0.183 92.3

Average ± %RSD 86.4% ± 1.1% 92.1% ± 1.3%

LCS-140410-4 9.92 7.69 77.6 9.92 8.75 88.2

LCS-140410-5 9.92 7.78 78.4 9.92 9.16 92.3

LCS-140410-6 9.92 8.32 83.9 9.92 9.56 96.4

Average ± %RSD 80.0% ± 4.3% 92.3% ± 4.4%

LCS-140410-7 39.6 30.6 77.3 39.6 37.4 94.3

LCS-140410-8 39.6 32.0 80.9 39.6 37.8 95.4

LCS-140410-9 39.6 32.3 81.6 39.6 40.8 103

Average ± %RSD 79.9% ± 2.9% 97.6% ± 4.9%

ETS-8-044.1

Analyzed 4/10/14

Internal Standard 

Calibration PFOS (Linear and Branched) 13C4-PFOS

Lab ID

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

LCS-140410-1 0.184 0.173 93.8 0.189 0.178 94.0

LCS-140410-2 0.184 0.174 94.7 0.189 0.184 97.4

LCS-140410-3 0.184 0.171 93.0 0.189 0.178 94.0

Average ± %RSD 93.8% ± 0.91% 95.1% ± 2.1%

LCS-140410-4 9.20 8.66 94.2 1.90 1.93 101

LCS-140410-5 9.20 8.86 96.3 1.90 1.84 97.1

LCS-140410-6 9.20 8.80 95.7 1.90 1.88 99.2

Average ± %RSD 95.4% ± 1.1% 99.1% ± 2.0%

LCS-140410-7 36.7 33.4 91.0

LCS-140410-8 36.7 34.3 93.6

LCS-140410-9 36.7 36.7 99.9

Average ± %RSD 94.8% ± 4.8%
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REPORT NO. ISO14-05-02

PAGE 15 OF 24

Table 8 continued. Lab Control Spike Results 

ETS-8-044.1

Analyzed 4/17/14

External Standard 

Calibration PFOA (Linear and Branched) 13C4-PFOA

Lab ID

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

LCS-140414-1 0.479 0.570 119 0.499 0.492 98.6

LCS-140414-2 0.479 0.568 119 0.499 0.509 102

LCS-140414-3 0.479 0.499 104 0.499 0.498 99.7

Average ± %RSD 114% ± 7.6% 100% ± 1.7%

LCS-140414-4 4.79 4.78 99.7 4.99 4.76 95.5

LCS-140414-5 4.79 4.91 102 4.99 4.95 99.1

LCS-140414-6 4.79 4.62 96.4 4.99 4.82 96.6

Average ± %RSD 99.4% ± 2.8% 97.1% ± 1.9%

LCS-140414-7 38.2 37.3 97.5

LCS-140414-8 38.2 37.1 97.2

LCS-140414-9 38.2 38.1 99.8

Average ± %RSD 98.2% ± 1.4%

ETS-8-044.1

Analyzed 4/17/14

External Standard 

Calibration PFOS (Linear and Branched) 13C4-PFOS

Lab ID

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

LCS-140414-1 0.464 0.509 110 0.478 0.509 106

LCS-140414-2 0.464 0.508 110 0.478 0.517 108

LCS-140414-3 0.464 0.489 105 0.478 0.497 104

Average ± %RSD 108% ± 2.7% 106% ± 1.9%

LCS-140414-4 4.64 4.77 103 4.78 4.79 100

LCS-140414-5 4.64 4.92 106 4.78 4.91 103

LCS-140414-6 4.64 4.78 103 4.78 4.82 101

Average ± %RSD 104% ± 1.7% 101% ± 1.5%

LCS-140414-7 36.9 38.3 104

LCS-140414-8 36.9 36.6 99.2

LCS-140414-9 36.9 38.7 105

Average ± %RSD 103% ± 3.0%
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PAGE 16 OF 24

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%. 

Table 9. Analytical Method Uncertainty

Analyte Calibration Standard Deviation (%) Method Uncertainty

PFOA External 8.29 ±17%

PFBS External 5.88 ±12%

PFHS External 7.14 ±14%

PFOS External 7.16 ±14%

PFOA Internal 9.07 ±18%

PFBS Internal 11.2 ±22%

PFHS Internal 11.8 ±24%

PFOS Internal 10.0 ±20%

3.8 Field Matrix Spikes (FMS) and Laboratory Matrix Spikes (LMS)

Field matrix spike sample containers were prepared for select 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.

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) Concentrations

Sampling location

Spike 

Level

PFOA

ng/mL

PFBS

ng/mL

PFHS

ng/mL

PFOS

ng/mL

141R FMS 4.96 5.00 5.00 4.99

131S FMS 24.8 25.0 25.0 25.0

130L and 131L FMS 49.6 50.0 50.0 49.9

140R and 142R FMS 99.2 100 100 99.8

133L and 138S FMS 198 200 200 200

Trip Blank FMS Low 4.96 5.00 5.00 4.99

FMS High 198 200 200 200
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PAGE 17 OF 24

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. All target analyte field matrix spikes met method 

acceptance criteria with the following exceptions: 

• An appropriate field matrix spike was not available for PFOA for sampling locations DAL GW 

131L and DAL GW 133L and for PFOS for sampling location DAL-GW-133L; all samples were 

spiked with surrogate recovery standards prior to extraction. The surrogate recovery standard

recoveries met method acceptance criteria.

• DAL-GW-140R; The FMS recovery for PFOA was 63.0%. The analytical uncertainty for this 

location was expanded to ± 37%.

• DAL-GW-142R; The FMS recovery for PFOA was 52.5%. The analytical uncertainty for this 

location was expanded to ± 48%.

Table 11. DAL-GW-130L

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-005 DAL-GW-130L-0-140312 57.5 NA 1.59 NA

ISO14-05-02-006 DAL-GW-130L-DB-140312 58.6 NA 1.56 NA

ISO14-05-02-007 DAL-GW-130L-FMS-140312 109 103 56.7 110

Average Concentration (ng/mL) ± %RPD 58.1 ng/mL ± 1.9% 1.58 ng/mL ± 1.9%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-005 DAL-GW-130L-0-140312 10.7 NA 66.8 NA

ISO14-05-02-006 DAL-GW-130L-DB-140312 10.6 NA 68.9 NA

ISO14-05-02-007 DAL-GW-130L-FMS-140312 63.8 106 124 113

Average Concentration (ng/mL) ± %RPD 10.7 ng/mL ± 0.94% 67.9 ng/mL ± 3.1%

NA = Not Applicable

Samples were diluted 1:10 and analyzed using external standard quantitation.
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REPORT NO. ISO14-05-02

PAGE 18 OF 24

Table 12. DAL-GW-131S

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-010 DAL-GW-131S-0-140312 38.7 NA 1.03 NA

ISO14-05-02-011 DAL-GW-131S-DB-140312 35.6 NA 0.962 NA

ISO14-05-02-012 DAL-GW-131S-FMS-140312 62.6 103 21.9 83.6

Average Concentration (ng/mL) ± %RPD 37.2 ng/mL ± 8.3% 0.996 ng/mL ± 6.8%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-010 DAL-GW-131S-0-140312 6.28 NA 7.03 NA

ISO14-05-02-011 DAL-GW-131S-DB-140312 5.88 NA 6.62 NA

ISO14-05-02-012 DAL-GW-131S-FMS-140312 30.6 98.1 32.8 104

Average Concentration (ng/mL) ± %RPD 6.08 ng/mL ± 6.6% 6.83 ng/mL ± 6.0%

NA = Not Applicable

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

Table 13. DAL-GW-131L

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-013 DAL-GW-131L-0-140312 119 NA 2.94 NA

ISO14-05-02-014 DAL-GW-131L-DB-140312 110 NA 3.02 NA

ISO14-05-02-015 DAL-GW-131L-FMS-140312 160 NC 49.6 93.2

Average Concentration (ng/mL) ± %RPD 115 ng/mL ± 7.9% 2.98 ng/mL ± 2.7%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-013 DAL-GW-131L-0-140312 22.2 NA 45.3 NA

ISO14-05-02-014 DAL-GW-131L-DB-140312 20.9 NA 46.1 NA

ISO14-05-02-015 DAL-GW-131L-FMS-140312 74.9 107 97.7 104

Average Concentration (ng/mL) ± %RPD 21.6 ng/mL ± 6.0% 45.7 ng/mL ± 1.8%

NA = Not Applicable

NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concentration.

Samples were diluted 1:2 and analyzed using internal standard quantitation.
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PAGE 19 OF 24

Table 14. DAL-GW-133L

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-020 DAL-GW-133L-0-140311 457 NA 9.43 NA

ISO14-05-02-021 DAL-GW-133L-DB-140311 420 NA 9.62 NA

ISO14-05-02-022 DAL-GW-133L-FMS-140311 639 NC 193 91.7

Average Concentration (ng/mL) ± %RPD 439 ng/mL ± 8.4% 9.53 ng/mL ± 2.0%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-020 DAL-GW-133L-0-140311 74.0 NA 525 NA

ISO14-05-02-021 DAL-GW-133L-DB-140311 71.3 NA 503 NA

ISO14-05-02-022 DAL-GW-133L-FMS-140311 263 95.0 776 NC

Average Concentration (ng/mL) ± %RPD 72.7 ng/mL ± 3.7% 514 ng/mL ± 4.3%

NA = Not Applicable

NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concentration.

Samples were diluted 1:10 and analyzed using external standard quantitation.

Table 15. DAL-GW-138S

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-049 DAL-GW-138S-0-140313 208 NA 6.02 NA

ISO14-05-02-050 DAL-GW-138S-DB-140313 203 NA 5.63 NA

ISO14-05-02-051 DAL-GW-138S-FMS-140313 366 80.9 224 109

Average Concentration (ng/mL) ± %RPD 206 ng/mL ± 2.4% 5.83 ng/mL ± 6.7%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-049 DAL-GW-138S-0-140313 26.2 NA 316 NA

ISO14-05-02-050 DAL-GW-138S-DB-140313 26.4 NA 294 NA

ISO14-05-02-051 DAL-GW-138S-FMS-140313 240 107 534 115

Average Concentration (ng/mL) ± %RPD 26.3 ng/mL ± 0.76% 305 ng/mL ± 7.2%

NA = Not Applicable

Samples were diluted 1:10 and analyzed using external standard quantitation.
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO14-05-02

PAGE 20 OF 24

Table 16. DAL-GW-140R

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-058 DAL-GW-140R-0-140312 113 NA 1.45 NA

ISO14-05-02-059 DAL-GW-140R-DB-140312 116 NA 1.49 NA

ISO14-05-02-060 DAL-GW-140R-FMS-140312 177 63.0 (1) 110 109

Average Concentration (ng/mL) ± %RPD 115 ng/mL ± 2.6% (2) 1.47 ng/mL ± 2.7%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-058 DAL-GW-140R-0-140312 14.4 NA 127 NA

ISO14-05-02-059 DAL-GW-140R-DB-140312 15.5 NA 131 NA

ISO14-05-02-060 DAL-GW-140R-FMS-140312 121 106 212 83.2

Average Concentration (ng/mL) ± %RPD 15.0 ng/mL ± 7.4% 129 ng/mL ± 3.1%

NA = Not Applicable

Samples were diluted 1:10 and analyzed using external standard quantitation.

(1) FMS did not meet method acceptance criteria of ±30. 

(2) The analytical uncertainty was expanded to ±37%.

Table 17. DAL-GW-141R

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-061 DAL-GW-141R-0-140313 2.45 NA 0.0769 NA

ISO14-05-02-062 DAL-GW-141R-DB-140313 2.60 NA 0.0670 NA

ISO14-05-02-063 DAL-GW-141R-FMS-140313 7.43 98.9 4.47 88.0

Average Concentration (ng/mL) ± %RPD 2.53 ng/mL ± 5.9% 0.0720 ng/mL ± 14%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-061 DAL-GW-141R-0-140313 0.383 NA 6.74 NA

ISO14-05-02-062 DAL-GW-141R-DB-140313 0.404 NA 6.83 NA

ISO14-05-02-063 DAL-GW-141R-FMS-140313 4.98 91.7 11.5 94.5

Average Concentration (ng/mL) ± %RPD 0.394 ng/mL ± 5.3% 6.79 ng/mL ± 1.3%

NA = Not Applicable

Samples were diluted 1:2 and analyzed using internal standard quantitation.
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Table 18. DAL-GW-142R

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-064 DAL-GW-142R-0-140312 76.8 NA 2.59 NA

ISO14-05-02-065 DAL-GW-142R-DB-140312 75.1 NA 2.67 NA

ISO14-05-02-066 DAL-GW-142R-FMS-140312 128 52.5 (1) 99.2 96.6

Average Concentration (ng/mL) ± %RPD 76.0 ng/mL ± 2.2% (2) 2.63 ng/mL ± 3.0%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-064 DAL-GW-142R-0-140312 13.7 NA 204 NA

ISO14-05-02-065 DAL-GW-142R-DB-140312 15.0 NA 208 NA

ISO14-05-02-066 DAL-GW-142R-FMS-140312 112 97.5 277 71.1

Average Concentration (ng/mL) ± %RPD 14.4 ng/mL ± 9.1% 206 ng/mL ± 1.9%

NA = Not Applicable

Samples were diluted 1:10 and analyzed using external standard quantitation.

(1) FMS did not meet method acceptance criteria of ±30. 

(2) The analytical uncertainty was expanded to ±48%.

Table 19. Trip Blank

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-072 DAL-GW-TRIP-0-140313 <0.0240 (1) NA <0.0250 (1) NA

ISO14-05-02-073 DAL-GW-TRIP-LS-140313 5.14 (1) 104 4.49 (1) 89.8

ISO14-05-02-074 DAL-GW-TRIP-HS-140313 195 (2) 98.3 200 (2) 100

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO14-05-02-072 DAL-GW-TRIP-0-140313 <0.0250 (1) NA <0.0232 (1) NA

ISO14-05-02-073 DAL-GW-TRIP-LS-140313 4.76 (1) 95.2 4.70 (1) 94.2

ISO14-05-02-074 DAL-GW-TRIP-HS-140313 199 (2) 99.3 201 (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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Table 20. Surrogate Recovery Standards (1)

3M LIMS ID Description

13C4-PFOA 13C4-PFOS

%Recovery %Recovery

ISO14-05-02-001 DAL-GW-130R-0-140312 83.4 83.1

ISO14-05-02-002 DAL-GW-130R-DB-140312 79.3 85.3

ISO14-05-02-003 DAL-GW-130S-0-140313 91.2 82.6

ISO14-05-02-004 DAL-GW-130S-DB-140313 90.7 86.3

ISO14-05-02-005 DAL-GW-130L-0-140312 90.2 83.7

ISO14-05-02-006 DAL-GW-130L-DB-140312 95.6 90.6

ISO14-05-02-007 DAL-GW-130L-FMS-140312 95.0 99.8

ISO14-05-02-008 DAL-GW-131R-0-140311 96.2 106

ISO14-05-02-009 DAL-GW-131R-DB-140311 104 92.3

ISO14-05-02-010 DAL-GW-131S-0-140312 104 99.1

ISO14-05-02-011 DAL-GW-131S-DB-140312 84.0 95.4

ISO14-05-02-012 DAL-GW-131S-FMS-140312 89.5 102

ISO14-05-02-013 DAL-GW-131L-0-140312 95.9 94.6

ISO14-05-02-014 DAL-GW-131L-DB-140312 81.3 88.6

ISO14-05-02-015 DAL-GW-131L-FMS-140312 87.7 87.4

ISO14-05-02-016 DAL-GW-133R-0-140311 95.6 92.6

ISO14-05-02-017 DAL-GW-133R-DB-140311 101 100

ISO14-05-02-018 DAL-GW-133S-0-140311 91.3 97.1

ISO14-05-02-019 DAL-GW-133S-DB-140311 79.5 73.5

ISO14-05-02-020 DAL-GW-133L-0-140311 80.1 77.0

ISO14-05-02-021 DAL-GW-133L-DB-140311 74.2 77.0

ISO14-05-02-022 DAL-GW-133L-FMS-140311 87.9 87.3

ISO14-05-02-023 DAL-GW-134R-0-140313 90.0 93.1

ISO14-05-02-024 DAL-GW-134R-DB-140313 91.4 101

ISO14-05-02-025 DAL-GW-134S-0-140313 94.3 109

ISO14-05-02-026 DAL-GW-134S-DB-140313 95.2 95.7

ISO14-05-02-027 DAL-GW-134L-0-140313 98.1 87.1

ISO14-05-02-028 DAL-GW-134L-DB-140313 87.9 91.3

ISO14-05-02-029 DAL-GW-135R-0-140313 99.2 85.7

ISO14-05-02-030 DAL-GW-135R-DB-140313 92.1 90.2

ISO14-05-02-031 DAL-GW-135S-0-140313 100 96.2

ISO14-05-02-032 DAL-GW-135S-DB-140313 86.7 98.2

ISO14-05-02-033 DAL-GW-135L-0-140313 88.1 94.4

ISO14-05-02-034 DAL-GW-135L-DB-140313 96.9 82.3

(1) All surrogate recovery standards were added during sample preparation.
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Table 20 continued. Surrogate Recovery Standards (1)

3M LIMS ID Description

13C4-PFOA 13C4-PFOS

%Recovery %Recovery

ISO14-05-02-037 DAL-GW-136S-0-140311 95.2 92.9

ISO14-05-02-038 DAL-GW-136S-DB-140311 94.2 92.9

ISO14-05-02-039 DAL-GW-136L-0-140311 96.0 87.7

ISO14-05-02-040 DAL-GW-136L-DB-140311 94.8 88.5

ISO14-05-02-043 DAL-GW-137S-0-140312 94.3 98.1

ISO14-05-02-044 DAL-GW-137S-DB-140312 93.0 98.0

ISO14-05-02-045 DAL-GW-137L-0-140312 82.1 99.6

ISO14-05-02-046 DAL-GW-137L-DB-140312 87.6 101

ISO14-05-02-047 DAL-GW-138R-0-140313 90.3 91.2

ISO14-05-02-048 DAL-GW-138R-DB-140313 99.0 91.9

ISO14-05-02-049 DAL-GW-138S-0-140313 92.2 92.1, 84.0

ISO14-05-02-050 DAL-GW-138S-DB-140313 95.7 93.6, 81.1

ISO14-05-02-051 DAL-GW-138S-FMS-140313 94.7 86.3, 77.8

ISO14-05-02-052 DAL-GW-138L-0-140313 89.9 118

ISO14-05-02-053 DAL-GW-138L-DB-140313 96.0 118

ISO14-05-02-054 DAL-GW-CW26C-0-140311 90.8 92.8

ISO14-05-02-055 DAL-GW-CW26C-DB-140311 95.9 86.5

ISO14-05-02-056 DAL-GW-CW26L-0-140311 94.7 85.9

ISO14-05-02-057 DAL-GW-CW26L-DB-140311 97.3 94.5

ISO14-05-02-058 DAL-GW-140R-0-140312 79.9 86.3

ISO14-05-02-059 DAL-GW-140R-DB-140312 80.5 92.1

ISO14-05-02-060 DAL-GW-140R-FMS-140312 78.9 86.8

ISO14-05-02-061 DAL-GW-141R-0-140313 93.9 104

ISO14-05-02-062 DAL-GW-141R-DB-140313 89.2 104

ISO14-05-02-063 DAL-GW-141R-FMS-140313 91.0 99.7

ISO14-05-02-064 DAL-GW-142R-0-140312 85.7 95.7

ISO14-05-02-065 DAL-GW-142R-DB-140312 83.1 94.7

ISO14-05-02-066 DAL-GW-142R-FMS-140312 81.3 84.7

ISO14-05-02-067 DAL-GW-143R-0-140313 95.2 106

ISO14-05-02-068 DAL-GW-143R-DB-140313 88.9 104

ISO14-05-02-069 DAL-GW-145R-0-140311 98.7 86.3

ISO14-05-02-070 DAL-GW-145R-DB-140311 98.2 85.3

ISO14-05-02-071 DAL-GW-141R-RB-140313 102 106

ISO14-05-02-072 DAL-GW-TRIP-0-140313 94.8 94.1

ISO14-05-02-073 DAL-GW-TRIP-LS-140313 93.8 93.0

ISO14-05-02-074 DAL-GW-TRIP-HS-140313 94.0 85.5

(1) All surrogate recovery standards were added during sample preparation. 
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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 Tables 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.

7 Signatures

Susan T. Wolf, 3M Principal Analytical Investigator

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

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

project.

Quality Assurance Representative 

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

Environmental Laboratory.