3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-03

PAGE 1 OF 17

Final Report

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

Collected at the Browns Ferry Road Site Located in Decatur, AL

3rd Quarter 2013

Laboratory Request Number: ISO13-05-03

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. ISO13-05-03

PAGE 2 OF 17

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 ISO13-05-03

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

Collected at the Browns Ferry Road Site Located in Decatur, AL

3rd 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 August 27 and 28, 2013 and

returned to the 3M Environmental Laboratory on September 4, 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 ISO13-05-03.

The 3M Environmental Laboratory prepared sample containers for fourteen groundwater well and three 

surface water locations. Also included was a sample container for the collection of a soil/sediment 

rinseate blank. The results for the rinseate blank are included herein. The results for the soil/sediment 

samples are reported under project E13-0618. 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 sampling location 

included a field sample and field sample duplicate. Select locations also included a target analyte field 

matrix spike. Containers designated for field matrix spikes were fortified with an appropriate matrix

spike solution containing PFOA, PFBS, PFHS, and PFOS prior to being sent to the field for sample 

collection. All sample containers were fortified with internal standards and surrogate recovery 

standards prior to being sent to the field for sample collection.

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. ISO13-05-03

PAGE 3 OF 17

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)

ISO13-05-03-001 BFRS-GW-MW1R-0-130827 1.79 0.108 0.874 1.69

ISO13-05-03-002 BFRS-GW-MW1R-DB-130827 1.70 0.110 0.869 1.69

Average 1.75 0.109 0.872 1.69

%RPD Sample/Sample Dup 5.2 1.8 0.57 0.0

ISO13-05-03-004 BFRS-GW-MW3R-0-130827 22.0 4.34 21.8 26.0

ISO13-05-03-005 BFRS-GW-MW3R-DB-130827 16.8 3.47 17.4 20.4

Average 19.4 3.91 19.6 23.2

%RPD Sample/Sample Dup 27 (2) 22 (2) 22 (2) 24 (2)

ISO13-05-03-006 BFRS-GW-MW4R-0-130827 9.87 0.728 18.5 25.8

ISO13-05-03-007 BFRS-GW-MW4R-DB-130827 7.59 0.567 14.5 20.9

Average 8.73 0.648 16.5 23.4

%RPD Sample/Sample Dup 26 (2) 25 (2) 24 (2) 21 (2)

ISO13-05-03-008 BFRS-GW-MW4L-0-130827 0.269 0.0964 0.263 0.524

ISO13-05-03-009 BFRS-GW-MW4L-DB-130827 0.264 0.0906 0.245 0.556

Average 0.267 0.0935 0.254 0.540

%RPD Sample/Sample Dup 1.9 6.2 7.1 5.9

ISO13-05-03-011 BFRS-GW-MW5R-0-130828 0.212 0.0535 0.131 0.0874

ISO13-05-03-012 BFRS-GW-MW5R-DB-130828 0.206 0.0675 0.144 0.0905

Average 0.209 0.0605 0.138 0.0890

%RPD Sample/Sample Dup 2.9 23(2) 9.5 3.5

ISO13-05-03-013 BFRS-GW-MW5L-0-130828 0.635 0.165 0.262 1.24

ISO13-05-03-014 BFRS-GW-MW5L-DB-130828 0.591 0.170 0.284 1.29

Average 0.613 0.168 0.273 1.27

%RPD Sample/Sample Dup 7.2 3.0 8.1 4.0

ISO13-05-03-016 BFRS-GW-MW6R-0-130828 2.57 0.249 0.665 7.64

ISO13-05-03-017 BFRS-GW-MW6R-DB-130828 2.65 0.250 0.688 7.71

Average 2.61 0.250 0.677 7.68

%RPD Sample/Sample Dup 3.1 0.40 3.4 0.91

ISO13-05-03-018 BFRS-GW-MW6L-0-130828 0.195 0.0536 0.0853 0.324

ISO13-05-03-019 BFRS-GW-MW6L-DB-130828 0.238 0.0565 0.0857 0.360

Average 0.217 0.0551 0.0855 0.342

%RPD Sample/Sample Dup 20 5.3 0.47 11

ISO13-05-03-020 BFRS-GW-MW7R-0-130827 8.79 0.533 1.80 24.4

ISO13-05-03-021 BFRS-GW-MW7R-DB-130827 8.24 0.497 1.74 25.7

Average 8.52 0.515 1.77 25.1

%RPD Sample/Sample Dup 6.5 7.0 3.4 5.2

NA = Not Applicable

(1) 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 ± 13%, 

PFBS ± 13%, PFHS ± 12%, and PFOS ± 16%.

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

REPORT NO. ISO13-05-03

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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)

ISO13-05-03-022 BFRS-GW-MW8R-0-130828 0.220 0.0590 0.121 0.268

ISO13-05-03-023 BFRS-GW-MW8R-DB-130828 0.216 0.0575 0.117 0.250

Average 0.218 0.0583 0.119 0.259

%RPD Sample/Sample Dup 1.8 2.6 3.4 6.9

ISO13-05-03-025 BFRS-GW-MW9R-0-130827 0.112 <0.0250 0.0579 <0.0232

ISO13-05-03-026 BFRS-GW-MW9R-DB-130827 0.109 <0.0250 0.0510 <0.0232

Average 0.111 <0.0250 0.0545 <0.0232

%RPD Sample/Sample Dup 2.7 NA 13 NA

ISO13-05-03-027 BFRS-GW-MW9L-0-130827 0.0301 <0.0250 <0.0250 0.0446

ISO13-05-03-028 BFRS-GW-MW9L-DB-130827 0.0344 <0.0250 <0.0250 0.0443

Average 0.0323 <0.0250 <0.0250 0.0445

%RPD Sample/Sample Dup 13 NA NA 0.67

ISO13-05-03-029 BFRS-GW-MW10R-0-130827 0.644 0.0692 0.293 0.536

ISO13-05-03-030 BFRS-GW-MW10R-DB-130827 0.669 0.0658 0.306 0.594

Average 0.657 0.0675 0.300 0.565

%RPD Sample/Sample Dup 3.8 5.0 4.3 10

ISO13-05-03-032 BFRS-GW-MW11L-0-130828 0.286 <0.0250 0.0823 0.387

ISO13-05-03-033 BFRS-GW-MW11L-DB-130828 0.275 <0.0250 0.0730 0.378

Average 0.281 <0.0250 0.0777 0.383

%RPD Sample/Sample Dup 3.9 NA 12 2.4

ISO13-05-03-034 BFRS-SW-ET02-0-130828 0.0314 0.0350 <0.0250 0.0547

ISO13-05-03-035 BFRS-SW-ET02-DB-130828 0.0313 0.0350 <0.0250 0.0544

Average 0.0314 0.0350 <0.0250 0.0546

%RPD Sample/Sample Dup 0.32 0.0 NA 0.55

ISO13-05-03-036 BFRS-SW-ET03-0-130828 0.147 0.0565 0.0820 0.295

ISO13-05-03-037 BFRS-SW-ET03-DB-130828 0.178 0.0560 0.0792 0.260

Average 0.163 0.0563 0.0806 0.278

%RPD Sample/Sample Dup 19 0.89 3.5 13

ISO13-05-03-039 BFRS-SW-ET04-0-130828 0.0507 0.0371 <0.0250 0.113

ISO13-05-03-040 BFRS-SW-ET04-DB-130828 0.0465 0.0352 <0.0250 0.105

Average 0.0486 0.0362 <0.0250 0.109

%RPD Sample/Sample Dup 8.6 5.3 NA 7.3

ISO13-05-03-041 BFRS-SS08-RB-0-130828 <0.0240 <0.0250 <0.0250 <0.0232

ISO13-05-03-042 BFRS-GW-TRIP01-0 <0.0240 <0.0250 <0.0250 <0.0232

NA = Not Applicable

(1) 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 ± 13%, 

PFBS ± 13%, PFHS ± 12%, and PFOS ± 16%. 

(2) The RPD value did not meet method acceptance criteria of ≤20%.
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REPORT NO. ISO13-05-03

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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 August 27 and 28, 2013 and returned to the 3M 

Environmental Laboratory on September 4, 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. 

Table 3. Sample Description Key Code.

String Number String Descriptor Example: BFRS-GW-MW4L-0-130827

1 Sample Location BFRS= Browns Ferry Road Site

2 Sample Type GW= Ground Water

SW=Surface Water

3 Well Identifier Example: MW4

4 Well Level R = Residuum shallow water-bearing zone 

L = Bedrock water-bearing zone

5 Sample Type 0 =primary sample 

DB =duplicate sample

FMS = Field Matrix Spike

6 Sampling Date 130827 – August 27, 2013

2.3 Sample Preparation

9/10/13: Samples were prepared by removing an aliquot of the well mixed sample and placing it in an 

autovial for analysis.

9/13/13: Samples requiring dilution prior to analysis were prepared by removing a 0.4 mL aliquot of the 

well mixed sample and diluting it with 0.4 mL of methanol (dilution factor of 2).

All samples were analyzed by internal standard calibration. 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.

 
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-03

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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:

• 9/10/13: Direct Injection/internal standard analysis PFOA, PFBS, PFHS, PFOS, 

13C4-PFOA, 

and 13C4-PFOS; all locations.

• 9/13/13: Solvent dilution / internal standard analysis PFOS and 13C4-PFOS; locations BFRSGW-MW3R, BFRS-GW-MW4R, and BFRS-GW-MW7R. 

Due to the nature of the samples, the wide range of concentrations found in the samples, 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 9/10/13 and 9/13/13

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 20 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. ISO13-05-03

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Table 6. Mass Transitions

Analyte

Mass Transition

Q1/Q3

Internal Standard Mass Transition

Q1/Q3

PFOA

413/369

[

13 413/219 C8]PFOA 421/376

413/169

PFBS

299/80

[

18O2]PFBS 303/84

299/99

PFHS

399/99

[

13C3]PFHS 402/99

399/80

PFOS

499/99

[

13 499/80 C8]-PFOS 507/80

499/130

[

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

[

13C4]-PFOS surrogate 503/80 [13C8]-PFOS 507/80

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.

3 Data Analysis

3.1 Calibration

9/10/13: 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 1.0 ng/mL. Ten curve points ranging from 0.025 ng/mL to 25 ng/mL (nominal) were 

analyzed with the samples. Of these ten calibration standards, nine contained the surrogates at 

concentrations ranging from 0.0250 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. The data were not forced through zero during the 

fitting process. 

9/13/13: Solvent Dilution / internal standard calibration.

Samples were analyzed against an internal standard matrix-matched calibration curve. Calibration 

standards were prepared by spiking known amounts of the stock solution into a 50:50 Methanol: 

Laboratory Reagent Water. The calibration standards contained an internal standard mix at a nominal 

concentration of 0.5 ng/mL. Twelve standards ranging from 0.0125 ng/mL to 25 ng/mL (nominal) were 

analyzed with the samples. Of these twelve 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. The data were not forced through zero during the 

fitting process.

For both 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. ISO13-05-03

PAGE 8 OF 17

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

9/10/13 Internal standard NA <0.0240 <0.0250 <0.0250 <0.0232

9/13/13 Internal standard 2 NA NA NA <0.0232

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 for the target analytes and analyzed in triplicate, 

while only low and high lab control samples were prepared for the surrogates. LCSs were prepared by 

spiking known amounts of the analytes into laboratory reagent 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. 

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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Table 8. Lab Control Spike Results

ETS-8-044.1

Analyzed 9/10/13

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-130910-1 0.190 0.179 94.2 0.198 0.192 97.1

LCS-130910-2 0.190 0.187 98.6 0.198 0.200 101

LCS-130910-3 0.190 0.177 93.3 0.198 0.195 98.3

Average ± %RSD 95.4% ± 3.0% 98.8% ± 2.0%

LCS-130910-4 1.90 1.97 103 1.98 2.19 110

LCS-130910-5 1.90 1.98 104 1.98 2.05 103

LCS-130910-6 1.90 1.99 105 1.98 2.07 104

Average ± %RSD 104% ± 0.96% 106% ± 3.6%

LCS-130910-7 16.2 14.4 89.0 16.9 15.7 92.9

LCS-130910-8 16.2 14.5 89.7 16.9 15.6 92.3

LCS-130910-9 16.2 14.4 89.0 16.9 15.5 91.8

Average ± %RSD 89.2% ± 0.45% 92.3% ± 0.60%

ETS-8-044.1

Analyzed 9/10/13

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-130910-1 0.198 0.197 99.7 0.184 0.180 97.7

LCS-130910-2 0.198 0.211 107 0.184 0.180 97.9

LCS-130910-3 0.198 0.193 97.3 0.184 0.202 110

Average ± %RSD 101% ± 5.0% 102% ± 6.9%

LCS-130910-4 1.98 2.21 112 1.84 1.98 107

LCS-130910-5 1.98 2.42 122 1.84 1.89 103

LCS-130910-6 1.98 2.21 112 1.84 1.81 98.6

Average ± %RSD 115% ± 5.0% 103% ± 4.1%

LCS-130910-7 16.9 16.8 99.6 15.7 13.7 87.0

LCS-130910-8 16.9 16.1 95.1 15.7 13.6 86.6

LCS-130910-9 16.9 16.2 95.6 15.7 13.6 86.9

Average ± %RSD 96.8% ± 2.5% 86.8% ± 0.24%
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Table 8 continued. Lab Control Spike Results 

ETS-8-044.1

Analyzed 9/10/13

Internal Standard 

Calibration 13C4-PFOA 13C4-PFOS

Lab ID

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

LCS-130910-1 0.198 0.203 103 0.189 0.208 110

LCS-130910-2 0.198 0.209 106 0.189 0.195 103

LCS-130910-3 0.198 0.209 106 0.189 0.219 116

Average ± %RSD 105% ± 1.6% 110% ± 5.9%

LCS-130910-4 1.98 2.15 109 1.89 2.11 112

LCS-130910-5 1.98 2.01 102 1.89 1.93 102

LCS-130910-6 1.98 2.08 105 1.89 1.88 99.4

Average ± %RSD 105% ± 3.3% 104% ± 6.4%

ETS-8-044.1

Analyzed 9/13/13

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-130913-1 0.184 0.166 90.2 0.189 0.181 95.5

LCS-130913-2 0.184 0.158 86.1 0.189 0.184 97.2

LCS-130913-3 0.184 0.170 92.5 0.189 0.181 95.6

Average ± %RSD 89.6% ± 3.6% 96.1% ± 0.99%

LCS-130913-4 1.84 1.80 98.0 1.89 1.76 93.1

LCS-130913-5 1.84 1.70 92.6 1.89 1.85 98.0

LCS-130913-6 1.84 1.77 96.2 1.89 1.88 99.4

Average ± %RSD 95.6% ± 2.9% 96.8% ± 3.4%

LCS-130913-7 32.2 31.1 96.6

LCS-130913-8 32.2 31.7 98.4

LCS-130913-9 32.2 31.4 97.6

Average ± %RSD 97.5% ± 0.92%
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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 Internal 6.42 ±13%

PFBS Internal 6.72 ±13%

PFHS Internal 6.12 ±12%

PFOS Internal 8.22 ±16%

3.8 Field Matrix Spikes (FMS)

Field matrix spike sample containers were prepared for select sampling locations to verify that the 

analytical method is applicable to the collected matrix. Field matrix spikes are generated by adding a 

measured volume of field sample to a container spiked by the laboratory with the target analytes prior 

to shipping sample containers 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

PFOA

ng/mL

PFBS

ng/mL

PFHS

ng/mL

PFOS

ng/mL

GW-MW1R, GW-MW4L, GW-MW5L, GWMW8R, GW-MW10R, SW-ET03, and Trip Blank 0.958 1.00 1.00 0.927

4 Data Summary and Discussion

Tables 11-18 below summarize the sample results and target analyte field matrix spike recoveries for 

the sampling locations as well as the Trip Blank. The surrogate recovery standard recoveries are 

presented in Table 19. 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. Field matrix spikes meeting the method acceptance criteria of ± 30%, demonstrate that the 

method is appropriate for the given matrix. 
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-03

PAGE 12 OF 17

All target analyte field matrix spikes met method acceptance criteria with the following exception:

• BFRS-SW-ET03; The 13C4-PFOS results for this location are not reportable due to the analyte 

area counts were below the LLOQ area counts and less than two times the average area 

counts for the method blanks. This location had acceptable FMS recoveries for each analyte. 

Table 11. BFRS-GW-MW1R

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-03-001 BFRS-GW-MW1R-0-130827 1.79 NA 0.108 NA

ISO13-05-03-002 BFRS-GW-MW1R-DB-130827 1.70 NA 0.110 NA

ISO13-05-03-003 BFRS-GW-MW1R-FMS-130827 2.55 84.0 1.02 91.1

Average Concentration (ng/mL) ± %RPD 1.75 ng/mL ± 5.2% 0.109 ng/mL ± 1.8%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-03-001 BFRS-GW-MW1R-0-130827 0.874 NA 1.69 NA

ISO13-05-03-002 BFRS-GW-MW1R-DB-130827 0.869 NA 1.69 NA

ISO13-05-03-003 BFRS-GW-MW1R-FMS-130827 1.92 105 2.62 100

Average Concentration (ng/mL) ± %RPD 0.872 ng/mL ± 0.57% 1.69 ng/mL ± 0.0%

NA = Not Applicable

Table 12. BFRS-GW-MW4L

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-03-008 BFRS-GW-MW4L-0-130827 0.269 NA 0.0964 NA

ISO13-05-03-009 BFRS-GW-MW4L-DB-130827 0.264 NA 0.0906 NA

ISO13-05-03-010 BFRS-GW-MW4L-FMS-130827 1.22 99.5 1.10 101

Average Concentration (ng/mL) ± %RPD 0.267 ng/mL ± 1.9% 0.0935 ng/mL ± 6.2%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-03-008 BFRS-GW-MW4L-0-130827 0.263 NA 0.524 NA

ISO13-05-03-009 BFRS-GW-MW4L-DB-130827 0.245 NA 0.556 NA

ISO13-05-03-010 BFRS-GW-MW4L-FMS-130827 1.32 107 1.55 109

Average Concentration (ng/mL) ± %RPD 0.254 ng/mL ± 7.1% 0.540 ng/mL ± 5.9%

NA = Not Applicable
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-03

PAGE 13 OF 17

Table 13. BFRS-GW-MW5L

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-03-013 BFRS-GW-MW5L-0-130828 0.635 NA 0.165 NA

ISO13-05-03-014 BFRS-GW-MW5L-DB-130828 0.591 NA 0.170 NA

ISO13-05-03-015 BFRS-GW-MW5L-FMS-130828 1.59 102 1.11 94.3

Average Concentration (ng/mL) ± %RPD 0.613 ng/mL ± 7.2% 0.168 ng/mL ± 3.0%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-03-013 BFRS-GW-MW5L-0-130828 0.262 NA 1.24 NA

ISO13-05-03-014 BFRS-GW-MW5L-DB-130828 0.284 NA 1.29 NA

ISO13-05-03-015 BFRS-GW-MW5L-FMS-130828 1.35 108 2.26 107

Average Concentration (ng/mL) ± %RPD 0.273 ng/mL ± 8.1% 1.27 ng/mL ± 4.0%

NA = Not Applicable

Table 14. BFRS-GW-MW8R

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-03-022 BFRS-GW-MW8R-0-130828 0.220 NA 0.0590 NA

ISO13-05-03-023 BFRS-GW-MW8R-DB-130828 0.216 NA 0.0575 NA

ISO13-05-03-024 BFRS-GW-MW8R-FMS-130828 1.23 106 1.01 95.2

Average Concentration (ng/mL) ± %RPD 0.218 ng/mL ± 1.8% 0.0583 ng/mL ± 2.6%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-03-022 BFRS-GW-MW8R-0-130828 0.121 NA 0.268 NA

ISO13-05-03-023 BFRS-GW-MW8R-DB-130828 0.117 NA 0.250 NA

ISO13-05-03-024 BFRS-GW-MW8R-FMS-130828 1.15 103 1.17 98.3

Average Concentration (ng/mL) ± %RPD 0.119 ng/mL ± 3.4% 0.259 ng/mL ± 6.9%

NA = Not Applicable
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-03

PAGE 14 OF 17

Table 15. BFRS-GW-MW10R

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-03-029 BFRS-GW-MW10R-0-130827 0.644 NA 0.0692 NA

ISO13-05-03-030 BFRS-GW-MW10R-DB-130827 0.669 NA 0.0658 NA

ISO13-05-03-031 BFRS-GW-MW10R-FMS-130827 1.50 88.0 1.15 108

Average Concentration (ng/mL) ± %RPD 0.657 ng/mL ± 3.8% 0.0675 ng/mL ± 5.0%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-03-029 BFRS-GW-MW10R-0-130827 0.293 NA 0.536 NA

ISO13-05-03-030 BFRS-GW-MW10R-DB-130827 0.306 NA 0.594 NA

ISO13-05-03-031 BFRS-GW-MW10R-FMS-130827 1.26 96.1 1.42 92.2

Average Concentration (ng/mL) ± %RPD 0.300 ng/mL ± 4.3% 0.565 ng/mL ± 10%

NA = Not Applicable

Table 16. BFRS-SW-ET03

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-03-036 BFRS-SW-ET03-0-130828 0.147 NA 0.0565 NA

ISO13-05-03-037 BFRS-SW-ET03-DB-130828 0.178 NA 0.0560 NA

ISO13-05-03-038 BFRS-SW-ET03-FMS-130828 1.16 104 1.04 98.4

Average Concentration (ng/mL) ± %RPD 0.163 ng/mL ± 19% 0.0563 ng/mL ± 0.89%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-03-036 BFRS-SW-ET03-0-130828 0.0820 NA 0.295 NA

ISO13-05-03-037 BFRS-SW-ET03-DB-130828 0.0792 NA 0.260 NA

ISO13-05-03-038 BFRS-SW-ET03-FMS-130828 1.06 97.9 1.36 117

Average Concentration (ng/mL) ± %RPD 0.0806 ng/mL ± 3.5% 0.278 ng/mL ± 13%

NA = Not Applicable
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-03

PAGE 15 OF 17

Table 17. Trip Blank

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-03-042 BFRS-GW-TRIP01-0 <0.0240 NA <0.0250 NA

ISO13-05-03-043 BFRS-GW-TRIP01-FMS 0.874 91.2 0.974 97.4

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-03-042 BFRS-GW-TRIP01-0 <0.0250 NA <0.0232 NA

ISO13-05-03-043 BFRS-GW-TRIP01-FMS 1.03 103 0.856 92.3

NA = Not Applicable

Table 18. Soil/Sediment Rinseate Blank

PFOA PFBS PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL)

Concentration 

(ng/mL)

Concentration 

(ng/mL)

Concentration 

(ng/mL)

ISO13-05-03-041 BFRS-SS08-RB-0-130828 <0.0240 <0.0250 <0.0250 <0.0232

. 

Table 19. Surrogate Recovery

3M LIMS ID Description

13C4-PFOA 13C4-PFOS

%Recovery %Recovery

ISO13-05-03-001 BFRS-GW-MW1R-0-130827 100 91.9

ISO13-05-03-002 BFRS-GW-MW1R-DB-130827 89.9 95.8

ISO13-05-03-003 BFRS-GW-MW1R-FMS-130827 84.7 106

ISO13-05-03-004 BFRS-GW-MW3R-0-130827 91.2 97.8, 94.7 (2)

ISO13-05-03-005 BFRS-GW-MW3R-DB-130827 90.6 100, 85.7 (2)

ISO13-05-03-006 BFRS-GW-MW4R-0-130827 97.6 99.7, 93.3 (2)

ISO13-05-03-007 BFRS-GW-MW4R-DB-130827 90.8 101, 90.3 (2)

ISO13-05-03-008 BFRS-GW-MW4L-0-130827 84.3 99.5

ISO13-05-03-009 BFRS-GW-MW4L-DB-130827 90.1 99.1

ISO13-05-03-010 BFRS-GW-MW4L-FMS-130827 89.9 94.5

ISO13-05-03-011 BFRS-GW-MW5R-0-130828 95.4 88.7

ISO13-05-03-012 BFRS-GW-MW5R-DB-130828 91.3 91.9

ISO13-05-03-013 BFRS-GW-MW5L-0-130828 96.6 98.6

ISO13-05-03-014 BFRS-GW-MW5L-DB-130828 92.0 95.0

ISO13-05-03-015 BFRS-GW-MW5L-FMS-130828 94.9 106

(1) NR=Not Reportable; Area counts were below the LLOQ and were not two times the method blank area counts. 

(2) Result from analysis on 9/13/13 for PFOS and 13C4-PFOS surrogate. 
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-03

PAGE 16 OF 17

Table 19 continued. Surrogate Recovery

3M LIMS ID Description

13C4-PFOA 13C4-PFOS

%Recovery %Recovery

ISO13-05-03-016 BFRS-GW-MW6R-0-130828 103 102

ISO13-05-03-017 BFRS-GW-MW6R-DB-130828 98.4 95.8

ISO13-05-03-018 BFRS-GW-MW6L-0-130828 94.5 94.7

ISO13-05-03-019 BFRS-GW-MW6L-DB-130828 109 91.8

ISO13-05-03-020 BFRS-GW-MW7R-0-130827 101 98.8, 95.4 (2)

ISO13-05-03-021 BFRS-GW-MW7R-DB-130827 94.2 90.1, 92.2 (2)

ISO13-05-03-022 BFRS-GW-MW8R-0-130828 96.0 105

ISO13-05-03-023 BFRS-GW-MW8R-DB-130828 94.3 90.3

ISO13-05-03-024 BFRS-GW-MW8R-FMS-130828 94.1 97.4

ISO13-05-03-025 BFRS-GW-MW9R-0-130827 91.5 99.2

ISO13-05-03-026 BFRS-GW-MW9R-DB-130827 86.5 85.3

ISO13-05-03-027 BFRS-GW-MW9L-0-130827 91.9 92.9

ISO13-05-03-028 BFRS-GW-MW9L-DB-130827 101 93.0

ISO13-05-03-029 BFRS-GW-MW10R-0-130827 88.4 90.4

ISO13-05-03-030 BFRS-GW-MW10R-DB-130827 92.6 105

ISO13-05-03-031 BFRS-GW-MW10R-FMS-130827 91.3 103

ISO13-05-03-032 BFRS-GW-MW11L-0-130828 89.7 104

ISO13-05-03-033 BFRS-GW-MW11L-DB-130828 76.0 107

ISO13-05-03-034 BFRS-SW-ET02-0-130828 85.1 97.0

ISO13-05-03-035 BFRS-SW-ET02-DB-130828 93.7 110

ISO13-05-03-036 BFRS-SW-ET03-0-130828 91.3 NR (1)

ISO13-05-03-037 BFRS-SW-ET03-DB-130828 87.2 NR (1)

ISO13-05-03-038 BFRS-SW-ET03-FMS-130828 94.5 NR (1)

ISO13-05-03-039 BFRS-SW-ET04-0-130828 98.2 99.8

ISO13-05-03-040 BFRS-SW-ET04-DB-130828 92.4 94.6

ISO13-05-03-041 BFRS-SS08-RB-0-130828 90.8 95.7

ISO13-05-03-042 BFRS-GW-TRIP01-0 98.9 109

ISO13-05-03-043 BFRS-GW-TRIP01-FMS 93.6 93.3

(1) NR=Not Reportable; Area counts were below the LLOQ and were not two times the method blank area counts. 

(2) Result from analysis on 9/13/13 for PFOS and 13C4-PFOS surrogate. 
3M ENVIRONMENTAL LABORATORY 

REPORT NO. IS013-05-03 

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 -19 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 Pmnjcipal Analytical Investigator Date 

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

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

project. 

Quality Assurance Redresentative / Date 

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

Environmental Laboratory. 

PAGE 17 OF 17