3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-04

PAGE 1 OF 28

Final Report

Analysis of PFOA, PFBS, PFHS, and PFOS in Groundwater Samples 

Collected from Decatur, Alabama

3rd Quarter 2013

Laboratory Request Number: ISO13-05-04

Method Requirement: 3M Method ETS-8-044.1

Report Date – Date of Final Signature

Testing Laboratory

3M EHS&S Operations

3M Environmental Laboratory

Building 260-5N-17

Maplewood, MN 55144-1000

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 A2LA 

assessment.
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-04

PAGE 2 OF 28

3M Environmental Laboratory

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

3M Principal Analytical Investigator: Susan Wolf

Report Author: Chelsie Grochow

Analytical Report ISO13-05-04

Analysis of PFOA, PFBS, PFHS, and PFOS in Groundwater Samples 

Collected from 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 from September 27 – October 11,

2013 and returned to the 3M Environmental Laboratory on October 16, 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 ISO13-05-04.

The 3M Environmental Laboratory prepared sample containers for eighteen 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, 

field sample duplicate, and at least 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. 

Samples were prepared and analyzed by method ETS-8-044.1 “Method of Analysis for the 

Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis”. Select 

internal standards were used to aid in the data quality objectives.

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 A2LA assessment.
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-04

PAGE 3 OF 28

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)

ISO13-05-04-001 DAL-GW-203L-0-131001 153 23.3 147 787

ISO13-05-04-002 DAL-GW-203L-DB-131001 152 24.0 147 794

Average 153 23.7 147 791

%RPD Sample/Sample Dup 0.65 3.0 0.0 0.88

ISO13-05-04-005 DAL-GW-220R-0-131003 51.5 8.38 41.6 80.9

ISO13-05-04-006 DAL-GW-220R-DB-131003 47.0 7.85 39.0 76.8

Average 49.3 8.12 40.3 78.9

%RPD Sample/Sample Dup 9.1 6.5 6.5 5.2

ISO13-05-04-008 DAL-GW-220L-0-131003 26.3 4.88 17.0 49.5

ISO13-05-04-009 DAL-GW-220L-DB-131003 26.4 5.04 17.5 49.5

Average 26.4 4.96 17.3 49.5

%RPD Sample/Sample Dup 0.38 3.2 2.9 0.0

ISO13-05-04-011 DAL-GW-222R-0-131001 317 44.3 298 444

ISO13-05-04-012 DAL-GW-222R-DB-131001 323 46.6 317 474

Average 320 (2, 3) 45.5 308 459

%RPD Sample/Sample Dup 1.9 5.1 6.2 6.5

ISO13-05-04-015 DAL-GW-227R-0-131001 241 15.3 58.3 660

ISO13-05-04-016 DAL-GW-227R-DB-131001 235 14.9 55.8 653

Average 238 (2) 15.1 57.1 657

%RPD Sample/Sample Dup 2.5 2.6 4.4 1.1

ISO13-05-04-019 DAL-GW-227L-0-131001 178 264 83.0 826

ISO13-05-04-020 DAL-GW-227L-DB-131001 172 254 81.9 838

Average 175 259 82.5 832

%RPD Sample/Sample Dup 3.4 3.9 1.3 1.4

ISO13-05-04-023 DAL-GW-310R-0-131002 953 1310 310 778

ISO13-05-04-024 DAL-GW-310R-DB-131002 928 1300 304 755

Average 941 1310 307 767

%RPD Sample/Sample Dup 2.7 0.76 2.0 3.0

ISO13-05-04-026 DAL-GW-312R-0-131011 6740 7220 1320 2850

ISO13-05-04-027 DAL-GW-312R-DB-131011 6860 7300 1280 2860

Average 6800 7260 1300 2860

%RPD Sample/Sample Dup 1.8 1.1 3.1 0.35

ISO13-05-04-029 DAL-GW-317L-0-131002 0.290 <0.0250 0.0932 0.241 

ISO13-05-04-030 DAL-GW-317L-DB-131002 0.308 <0.0250 0.104 0.245 

Average 0.299 (2) <0.0250 (2) 0.0986 (2) 0.243 (2)

%RPD Sample/Sample Dup 6.0 NA 11 1.6

NA = Not Applicable

(1) All samples associated with the reported sampling location were 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 using 

solvent dilution are as follows: PFOA ± 14%, PFBS ± 14%, PFHS ± 12%, and PFOS ± 15%.

(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 ± 17%, 

PFBS ± 17%, PFHS ± 16%, and PFOS ± 18%.

(3) The analytical method uncertainty has been expanded to ± 34% for PFOA. See section 4 for further discussion. 
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-04

PAGE 4 OF 28

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)

ISO13-05-04-032 DAL-GW-324L-0-130927 219 74.6 55.3 78.0

ISO13-05-04-033 DAL-GW-324L-DB-130927 203 69.7 53.3 77.7

Average 211 72.2 54.3 77.9

%RPD Sample/Sample Dup 7.6 6.8 3.7 0.39

ISO13-05-04-035 DAL-GW-RW327R-0-131011 1180 59.9 159 617

ISO13-05-04-036 DAL-GW-RW327R-DB-131011 1190 63.8 169 708

Average 1190 (2) 61.9 164 663

%RPD Sample/Sample Dup 0.84 6.3 6.1 14

ISO13-05-04-039 DAL-GW-328R-0-130927 409 33.8 52.4 274

ISO13-05-04-040 DAL-GW-328R-DB-130927 397 32.5 51.0 265

Average 403 (2) 33.2 51.7 270

%RPD Sample/Sample Dup 3.0 3.9 2.7 3.3

ISO13-05-04-043 DAL-GW-328L-0-130927 108 45.7 17.6 1.29

ISO13-05-04-044 DAL-GW-328L-DB-130927 109 44.9 16.1 1.18

Average 109 (2) 45.3 (2) 16.9 1.24

%RPD Sample/Sample Dup 0.92 1.8 8.9 8.9

ISO13-05-04-047 DAL-GW-330R-0-130927 278 1430 163 676

ISO13-05-04-048 DAL-GW-330R-DB-130927 281 1440 163 688

Average 280 1440 163 682

%RPD Sample/Sample Dup 1.1 0.69 0.0 1.8

ISO13-05-04-051 DAL-GW-330L-0-130927 83.9 1360 462 181

ISO13-05-04-052 DAL-GW-330L-DB-130927 82.5 1310 455 177

Average 83.2 1340 459 179

%RPD Sample/Sample Dup 1.7 3.7 1.5 2.2

ISO13-05-04-054 DAL-GW-RW331S-0-131011 422 432 160 465

ISO13-05-04-055 DAL-GW-RW331S-DB-131011 428 427 161 457

Average 425 430 161 461

%RPD Sample/Sample Dup 1.4 1.2 0.62 1.7

ISO13-05-04-057 DAL-GW-335R-0-131002 4680 1230 1650 6440

ISO13-05-04-058 DAL-GW-335R-DB-131002 4650 1250 1660 6510

Average 4670 1240 1660 6480

%RPD Sample/Sample Dup 0.64 1.6 0.60 1.1

ISO13-05-04-060 DAL-GW-GRS04-0-131011 5530 2830 9540 2690

ISO13-05-04-061 DAL-GW-GRS04-DB-131011 5410 2730 9140 2940

Average 5470 2780 9340 2820

%RPD Sample/Sample Dup 2.2 3.6 4.3 8.9

NA = Not Applicable

(1) All samples associated with the reported sampling location were 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 using 

solvent dilution are as follows: PFOA ± 14%, PFBS ± 14%, PFHS ± 12%, and PFOS ± 15%.

(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 ± 17%, 

PFBS ± 17%, PFHS ± 16%, and PFOS ± 18%.

(3) The analytical method uncertainty has been expanded to ± 34% for PFOA. See section 4 for further discussion.
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-04

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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 + Branched

Perfluorooctanoic Acid (C8 Acid) PFBS Linear

Perfluorobutanesulfonate (C4 Sulfonate ) PFHS Linear

Perfluorooctanesulfonate (C8 Sulfonate) PFOS Linear + 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 from September 27 – October 11, 2013 and 

returned to the 3M Environmental Laboratory on October 16, 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

Example DAL-GW-317L-0-131002

1 Sample Location DAL= Decatur, Alabama

2 Sample Type GW= Ground Water

3 Well Identifier Example: 317

4 Well Level R = Residuum shallow water-bearing zone 

L = Bedrock water-bearing zone

S = Epikarst middle water-bearing zone

5 Sampling Date 131002 – October 2, 2013

6 Sample Type 0 =primary sample 

DB =duplicate sample

FMS = Field Matrix Spike

LS = Low field matrix spike

HS = High field matrix spike
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-04

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2.3 Sample Preparation

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 1:100 dilution were prepared by removing a 0.1 

mL aliquot of the well mixed sample and diluting it with 9.9 mL of methanol. Sample injection values 

were decreased for some samples if a larger dilution factor was desired.

Samples that did not have appropriate field matrix spike (FMS) levels based on the initial analysis, a 

laboratory matrix spike (LMS) sample was prepared by spiking the target analytes in a diluted aliquot of 

the primary sample (nominal concentration of 1000 ng/mL or 5000 ng/mL). 

Samples with low FMS recoveries based on the initial analysis, were analyzed with internal standard. 

Samples requiring dilution were diluted with synthetic groundwater and fortified with internal standard 

(nominal concentration of 1 ng/mL). Sample set 317L, trip blank sample, and rinseate blank were also

analyzed using internal standard and prepared by removing an aliquot of well mixed sample and 

fortifying with internal standard prior to sample analysis. During the preparation of the laboratory control 

samples, an aliquot of an internal standard spiking solution was added to the laboratory control 

samples (nominal concentration of 1 ng/mL). 

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.

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.
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-04

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Table 4. Instrument Parameters

Instrument Name ETS Kirk

Analysis Dates 10/18/13, 10/21/13, 10/22/13

Analytical Method ETS-8-044.1 

Liquid Chromatograph Agilent 1260

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

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

Injection Volume 5 or 20 μL

Mass Spectrometer Applied Biosystems TripleQuad 5500

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

Table 6. Mass Transitions

Analyte

Mass Transition

Q1/Q3

Internal Standard (1) Mass Transition

Q1/Q3

Reference Material 

Structure

PFOA

413/369

[

13 413/219 C8]PFOA 421/376 Linear + Branched

413/169

PFBS

299/80

[

18

O2]PFBS 303/84 Linear

299/99

PFHS

399/99

[

13C3]PFHS 402/80 Linear

399/80

PFOS

499/99

[

13 499/80 C8]-PFOS 507/80 Linear + Branched

499/130

Dwell time was 20 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 10/22/13.
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-04

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3 Data Analysis

3.1 Calibration

External Standard Calibration Analysis: Samples were analyzed against an external standard 

calibration curve. Calibration standards were prepared by spiking known amounts of the stock solution 

containing the target analytes into 90:10 methanol:laboratory Milli-QTM water. A total of eleven spiked 

standards ranging from 0.02 ng/mL to 50 ng/mL (nominal) were analyzed. A quadratic, 1/x weighted, 

calibration curve of the standard peak area counts was used to fit the data for each analyte. The data 

were not forced through zero during the fitting process. Calculating the standard concentrations using 

the peak area counts and the resultant calibration curve confirmed accuracy of each curve point. 

Internal Standard Calibration Analysis: 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 laboratory prepared reagent water. The calibration standards contained 

an internal standard mix at a nominal concentration of 1 ng/mL. A total of fourteen calibration 

standards ranging from 0.025 ng/mL to 50 ng/mL (nominal) were analyzed with the prepared samples. 

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. Calculating the standard concentrations using the peak area 

ratios and the resultant calibration curve confirmed accuracy of each curve point.

For each calibration curve, the reference standards of PFOA and PFOS used to prepare the calibration 

standards consisted of both linear and branched isomers. 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.

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

PFBA

LOQ, ng/mL

PFOA

LOQ, ng/mL

PFBS

LOQ, ng/mL

PFOS

LOQ, ng/mL

10/18/13 External Standard

10 0.192 0.200 0.200 0.185

100 1.92 2.00 2.00 1.85

400 7.68 8.00 8.00 7.40

10/21/13 External standard

100 1.92 2.00 2.00 1.85

400 7.68 8.00 8.00 7.40

10/22/13 Internal standard

1 0.0240 0.0250 0.0400 0.0232

10 0.240 0.250 0.400 0.232

100 2.40 2.50 4.00 2.32
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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 LCS samples.

Note: Lab matrix spike samples (LMS) for locations RW312R and 333L were prepared on 10/21/13 

without additional LCSs. This is a deviation from the method that states that LCSs should be prepared 

each day that samples are aliquoted. While this is a deviation from the method, the LMS samples were 

analyzed in an analytical batch with samples for which LCS samples were prepared. Both the LMS 

and LCS samples analyzed on 10/21/13 met method acceptance criteria.

All LCSs were used in the determination of the analytical method uncertainty in section 3.7.

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. ISO13-05-04

PAGE 10 OF 28

Table 8. Lab Control Spike Results

ETS-8-044.1

Analyzed 10/18/13

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-131018-1 0.191 0.193 101 0.200 0.212 106

LCS-131018-2 0.191 0.206 108 0.200 0.221 111

LCS-131018-3 0.191 0.193 101 0.200 0.210 105

Average ± %RSD 103% ± 3.9% 107% ± 3.0%

LCS-131018-4 4.77 5.15 108 4.98 5.20 104

LCS-131018-5 4.77 5.14 108 4.98 5.38 108

LCS-131018-6 4.77 5.22 109 4.98 5.33 107

Average ± %RSD 108% ± 0.53% 106% ± 2.0%

LCS-131018-7 38.2 37.8 98.9 39.8 40.0 101

LCS-131018-8 38.2 35.9 94.0 39.8 37.8 94.9

LCS-131018-9 38.2 36.6 95.9 39.8 38.5 96.7

Average ± %RSD 96.3% ± 2.6% 97.5% ± 3.2%

ETS-8-044.1

Analyzed 10/18/13

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-131018-1 0.200 0.202 101 0.185 0.201 109

LCS-131018-2 0.200 0.209 104 0.185 0.211 114

LCS-131018-3 0.200 0.207 103 0.185 0.202 109

Average ± %RSD 103% ± 1.5% 111% ± 2.6%

LCS-131018-4 4.98 5.29 106 4.61 5.21 113

LCS-131018-5 4.98 5.34 107 4.61 5.34 116

LCS-131018-6 4.98 5.40 109 4.61 5.30 115

Average ± %RSD 107% ± 1.4% 115% ± 1.3%

LCS-131018-7 39.8 40.2 101 36.9 38.3 104

LCS-131018-8 39.8 36.6 91.9 36.9 35.7 96.8

LCS-131018-9 39.8 38.0 95.4 36.9 36.8 99.9

Average ± %RSD 96.1% ± 4.8% 100% ± 3.6%
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Table 8 continued. Lab Control Spike Results 

ETS-8-044.1

Analyzed 10/21/13

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-131018-1 0.191 0.202 106 0.200 0.220 110

LCS-131018-2 0.191 0.207 108 0.200 0.221 111

LCS-131018-3 0.191 0.212 111 0.200 0.221 111

Average ± %RSD 108% ± 2.3% 111% ± 0.52%

LCS-131018-4 4.77 5.31 111 4.98 5.35 107

LCS-131018-5 4.77 5.35 112 4.98 5.62 113

LCS-131018-6 4.77 5.35 112 4.98 5.61 113

Average ± %RSD 112% ± 0.52% 111% ± 3.1%

LCS-131018-7 38.2 41.5 109 39.8 43.1 108

LCS-131018-8 38.2 38.6 101 39.8 39.6 99.6

LCS-131018-9 38.2 40.5 106 39.8 42.1 106

Average ± %RSD 105% ± 3.8% 105% ± 4.2%

ETS-8-044.1

Analyzed 10/21/13

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-131018-1 0.200 0.215 108 0.185 0.212 115

LCS-131018-2 0.200 0.219 109 0.185 0.215 116

LCS-131018-3 0.200 0.210 105 0.185 0.215 116

Average ± %RSD 107% ± 1.9% 116% ± 0.50%

LCS-131018-4 4.98 5.32 107 4.61 5.45 118

LCS-131018-5 4.98 5.53 111 4.61 5.58 121

LCS-131018-6 4.98 5.42 109 4.61 5.59 121

Average ± %RSD 109% ± 1.8% 120% ± 1.4%

LCS-131018-7 39.8 41.7 105 36.9 40.9 111

LCS-131018-8 39.8 38.2 96.0 36.9 37.4 101

LCS-131018-9 39.8 41.3 104 36.9 40.3 109

Average ± %RSD 102% ± 4.8% 107% ± 4.9%
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Table 8 continued. Lab Control Spike Results 

ETS-8-044.1

Analyzed 10/22/13

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-131022-1 0.190 0.178 93.9 0.199 0.196 98.4

LCS-131022-2 0.190 0.195 103 0.199 0.203 102

LCS-131022-3 0.190 0.197 104 0.199 0.196 98.4

Average ± %RSD 100% ± 5.6% 99.6% ± 2.1%

LCS-131022-4 4.74 5.04 106 4.95 5.20 105

LCS-131022-5 4.74 4.82 102 4.95 5.13 104

LCS-131022-6 4.74 5.00 106 4.95 5.29 107

Average ± %RSD 105% ± 2.2% 105% ± 1.5%

LCS-131022-7 38.0 37.5 98.8 39.6 42.2 107

LCS-131022-8 38.0 36.7 96.5 39.6 39.3 99.3

LCS-131022-9 38.0 36.0 94.7 39.6 39.2 98.9

Average ± %RSD 96.7% ± 2.1% 102% ± 4.5%

ETS-8-044.1

Analyzed 10/22/13

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-131022-1 0.199 0.199 99.8 0.184 0.194 105

LCS-131022-2 0.199 0.204 103 0.184 0.203 110

LCS-131022-3 0.199 0.208 105 0.184 0.191 104

Average ± %RSD 103% ± 2.5% 106% ± 3.0%

LCS-131022-4 4.95 5.22 105 4.59 4.89 107

LCS-131022-5 4.95 5.29 107 4.59 4.93 107

LCS-131022-6 4.95 5.21 105 4.59 4.93 107

Average ± %RSD 106% ± 1.1% 107% ± 0.0%

LCS-131022-7 39.6 39.9 101 36.7 38.9 106

LCS-131022-8 39.6 38.3 96.7 36.7 37.2 101

LCS-131022-9 39.6 37.9 95.6 36.7 36.7 99.9

Average ± %RSD 97.8% ± 2.9% 102% ± 3.2%
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REPORT NO. ISO13-05-04

PAGE 13 OF 28

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 6.91 ±14%

PFBS External 6.88 ±14%

PFHS External 6.04 ±12%

PFOS External 7.65 ±15%

PFOA Internal 8.54 ±17%

PFBS Internal 8.32 ±17%

PFHS Internal 7.79 ±16%

PFOS Internal 8.80 ±18%

3.8 Field Matrix Spikes (FMS)

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 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 9. Field matrix spikes are 

presented in section 4 of this report. 

*100%

Spike Concentration

(SampleConcentration of FMS Average Concentration : FieldSample& FieldSample Dup.) FMSRecovery − =
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REPORT NO. ISO13-05-04

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Table 10. Field Matrix Spike Concentrations

Sampling location

Spike 

Level

PFOA

ng/mL

PFBS

ng/mL

PFHS

ng/mL

PFOS

ng/mL

203L Low 100 100 99.8 99.4

High 501 502 499 497

220R and 220L FMS 50.0 50.0 49.9 49.7

222R and 227L Low 100 100 99.8 99.4

High 501 502 499 497

227R and 328R Low 50.0 50.0 49.9 49.7

High 501 502 499 497

330R Low 501 502 499 497

High 1000 1000 998 994

310R, RW312R, and RW331S FMS 1000 1000 998 994

317L FMS 1.00 1.00 0.999 1.00

324L FMS 200 200 200 199

RW327R Low 100 100 99.8 99.4

High 1000 1000 998 994

328L Low 1.00 1.00 0.999 1.00

High 100 100 99.8 99.4

330L FMS 501 502 499 497

335R and GRS04 FMS 5010 5020 4990 4970

Trip Blank

Low 1.00 1.00 0.999 1.00

Mid 100 100 99.8 99.4

High 1000 1000 998 994

3.9 Lab Matrix Spikes (LMS)

Due to inappropriate field matrix spike levels, lab matrix spike samples were prepared for locations

RW312R and 330L to verify that the analytical method is applicable to the collected matrix. Lab matrix 

spikes are generated by adding a measured volume of spiking solution to an aliquot of the primary 

sample post-dilution from each sample set. The LMS sample was spiked at a nominal concentration of 

5000 ng/mL for sampling location RW312R and 1000 ng/mL for sampling location 330L. 

Lab 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. Lab matrix spikes are presented in section 4 of this report. 

*100%

Spike Concentration

(SampleConcentration of LMS Concentration : FieldSample ) LMSRecovery − =
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REPORT NO. ISO13-05-04

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4 Data Summary and Discussion

The tables below summarize the sample results and target analyte field matrix spike recoveries for the 

sampling locations as well as the Trip Blank. Where applicable, the data tables also include the 

recovery results for a lab matrix spike. 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 and laboratory matrix spikes met method acceptance criteria with 

the following exceptions:

Location 222R; The FMS recovery for PFOA was 66.1%. The analytical uncertainty for this location 

was expanded to ± 34%.
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REPORT NO. ISO13-05-04

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Table 11. DAL GW 203L 131001

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-001 DAL-GW-203L-0-131001 153 NA 23.3 NA

ISO13-05-04-002 DAL-GW-203L-DB-131001 152 NA 24.0 NA

ISO13-05-04-003 DAL-GW-203L-LS-131001 236 83.0 113 89.3

ISO13-05-04-004 DAL-GW-203L-HS-131001 517 72.7 459 86.7

Average Concentration (ng/mL) ± %RPD 153 ng/mL ± 0.65% 23.7 ng/mL ± 3.0%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-001 DAL-GW-203L-0-131001 147 NA 787 NA

ISO13-05-04-002 DAL-GW-203L-DB-131001 147 NA 794 NA

ISO13-05-04-003 DAL-GW-203L-LS-131001 234 87.2 858 NC

ISO13-05-04-004 DAL-GW-203L-HS-131001 596 90.0 1410 125

Average Concentration (ng/mL) ± %RPD 147 ng/mL ± 0.0% 791 ng/mL ± 0.88%

NA = Not Applicable

NC= Not Calculated; Spike levels were less than 0.5x the endogenous sample concentration.

Samples were diluted 1:100 and analyzed by external standard quantitation.

Table 12. DAL GW 220R 131003

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-005 DAL-GW-220R-0-131003 51.5 NA 8.38 NA

ISO13-05-04-006 DAL-GW-220R-DB-131003 47.0 NA 7.85 NA

ISO13-05-04-007 DAL-GW-220R-FMS-131003 88.8 79.0 51.2 86.2

Average Concentration (ng/mL) ± %RPD 49.3 ng/mL ± 9.1% 8.12 ng/mL ± 6.5% 

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-005 DAL-GW-220R-0-131003 41.6 NA 80.9 NA

ISO13-05-04-006 DAL-GW-220R-DB-131003 39.0 NA 76.8 NA

ISO13-05-04-007 DAL-GW-220R-FMS-131003 85.0 89.6 128 98.8

Average Concentration (ng/mL) ± %RPD 40.3 ng/mL ± 6.5% 78.9 ng/mL ± 5.2%

NA = Not Applicable

Samples were diluted 1:10 and analyzed using external standard quantitation.
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REPORT NO. ISO13-05-04

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Table 13. DAL GW 220L 131003

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-008 DAL-GW-220L-0-131003 26.3 NA 4.88 NA

ISO13-05-04-009 DAL-GW-220L-DB-131003 26.4 NA 5.04 NA

ISO13-05-04-010 DAL-GW-220L-FMS-131003 68.2 83.6 49.5 89.1

Average Concentration (ng/mL) ± %RPD 26.4 ng/mL ± 0.38% 4.96 ng/mL ± 3.2%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-008 DAL-GW-220L-0-131003 17.0 NA 49.5 NA

ISO13-05-04-009 DAL-GW-220L-DB-131003 17.5 NA 49.5 NA

ISO13-05-04-010 DAL-GW-220L-FMS-131003 63.2 92.0 98.5 98.6

Average Concentration (ng/mL) ± %RPD 17.3 ng/mL ± 2.9% 49.5 ng/mL ± 0.0%

NA = Not Applicable

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

Table 14. DAL GW 222R 131001

PFOA (1) PFBS (2)

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-011 DAL-GW-222R-0-131001 317 NA 44.3 NA

ISO13-05-04-012 DAL-GW-222R-DB-131001 323 NA 46.6 NA

ISO13-05-04-013 DAL-GW-222R-LS-131001 NR (3) NR (3) 135 89.5

ISO13-05-04-014 DAL-GW-222R-HS-131001 651 66.1 (4) 420 74.6

Average Concentration (ng/mL) ± %RPD 320 ng/mL ± 1.9% (5) 45.5 ng/mL ± 5.1%

PFHS (2) PFOS (2)

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-011 DAL-GW-222R-0-131001 298 NA 444 NA

ISO13-05-04-012 DAL-GW-222R-DB-131001 317 NA 474 NA

ISO13-05-04-013 DAL-GW-222R-LS-131001 401 NC 548 NC

ISO13-05-04-014 DAL-GW-222R-HS-131001 707 80.0 861 80.9

Average Concentration (ng/mL) ± %RPD 308 ng/mL ± 6.2% 459 ng/mL ± 6.5%

NA = Not Applicable

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

(1) Samples were diluted 1:100 and analyzed using internal standard quantitation. Internal standard was added to the samples 

during sample preparation.

(2) Samples were diluted 1:100 and analyzed using external standard quantitation.

(3) NR = Not reportable; sample was not repeated since the spike level was less than 0.5x the sample concentration.

(4) FMS did not meet acceptance criteria of 100 ± 30%.

(5) The analytical uncertainty was expanded to ± 34% for PFOA.
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REPORT NO. ISO13-05-04

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Table 15. DAL GW 227R 131001

PFOA (1) PFBS (2)

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-015 DAL-GW-227R-0-131001 241 NA 15.3 NA

ISO13-05-04-016 DAL-GW-227R-DB-131001 235 NA 14.9 NA

ISO13-05-04-017 DAL-GW-227R-LS-131001 NR (3) NR (3) 59.7 89.2

ISO13-05-04-018 DAL-GW-227R-HS-131001 609 74.1 443 85.2

Average Concentration (ng/mL) ± %RPD 238 ng/mL ± 2.5% 15.1 ng/mL ± 2.6%

PFHS (2) PFOS (2)

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-015 DAL-GW-227R-0-131001 58.3 NA 660 NA

ISO13-05-04-016 DAL-GW-227R-DB-131001 55.8 NA 653 NA

ISO13-05-04-017 DAL-GW-227R-LS-131001 102 90.0 811 NC

ISO13-05-04-018 DAL-GW-227R-HS-131001 505 89.8 1140 97.2

Average Concentration (ng/mL) ± %RPD 57.1 ng/mL ± 4.4% 657 ng/mL ± 1.1%

NA = Not Applicable

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

(1) Samples were diluted 1:100 and analyzed using internal standard quantitation. Internal standard was added to the samples 

during sample preparation.

(2) Samples were diluted 1:100 and analyzed using external standard quantitation.

(3) NR = Not reportable; sample was not repeated since the spike level was less than 0.5x the sample concentration.
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REPORT NO. ISO13-05-04

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Table 16. DAL GW 227L 131001

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-019 DAL-GW-227L-0-131001 178 NA 264 NA

ISO13-05-04-020 DAL-GW-227L-DB-131001 172 NA 254 NA

ISO13-05-04-021 DAL-GW-227L-LS-131001 254 79.0 338 NC

ISO13-05-04-022 DAL-GW-227L-HS-131001 540 72.9 706 89.0

Average Concentration (ng/mL) ± %RPD 175 ng/mL ± 3.4% 259 ng/mL ± 3.9%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-019 DAL-GW-227L-0-131001 83.0 NA 826 NA

ISO13-05-04-020 DAL-GW-227L-DB-131001 81.9 NA 838 NA

ISO13-05-04-021 DAL-GW-227L-LS-131001 167 84.7 905 NC

ISO13-05-04-022 DAL-GW-227L-HS-131001 538 91.3 1310 96.2

Average Concentration (ng/mL) ± %RPD 82.5 ng/mL ± 1.3% 832 ng/mL ± 1.4%

NA = Not Applicable

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

Samples were diluted 1:100 and analyzed using external standard quantitation.

Table 17. DAL GW 310R 131002

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-023 DAL-GW-310R-0-131002 953 NA 1310 NA

ISO13-05-04-024 DAL-GW-310R-DB-131002 928 NA 1300 NA

ISO13-05-04-025 DAL-GW-310R-FMS-131002 1750 80.9 2200 89.0

Average Concentration (ng/mL) ± %RPD 941 ng/mL ± 2.7% 1310 ng/mL ± 0.76%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-023 DAL-GW-310R-0-131002 310 NA 778 NA

ISO13-05-04-024 DAL-GW-310R-DB-131002 304 NA 755 NA

ISO13-05-04-025 DAL-GW-310R-FMS-131002 1230 92.5 1720 95.9

Average Concentration (ng/mL) ± %RPD 307 ng/mL ± 2.0% 767 ng/mL ± 3.0%

NA = Not Applicable

Samples were diluted 1:100 and analyzed using external standard quantitation.
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REPORT NO. ISO13-05-04

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Table 18. DAL GW RW312R 131011

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-026 DAL-GW-RW312R-0-131011 6740 NA 7220 NA

ISO13-05-04-027 DAL-GW-RW312R-DB-131011 6860 NA 7300 NA

ISO13-05-04-028 DAL-GW-RW312R-FMS-131011 NR (1) NR (1) NR (1) NR (1)

ISO13-05-04-026; LMS DAL-GW-RW312R-0-LMS 12400 119 12600 108

Average Concentration (ng/mL) ± %RPD 6800 ng/mL ± 1.8% 7260 ng/mL ± 1.1%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-026 DAL-GW-RW312R-0-131011 1320 NA 2850 NA

ISO13-05-04-027 DAL-GW-RW312R-DB-131011 1280 NA 2860 NA

ISO13-05-04-028 DAL-GW-RW312R-FMS-131011 2260 96.2 NR (1) NR (1)

ISO13-05-04-026; LMS DAL-GW-RW312R-0-LMS NA NA 8550 124

Average Concentration (ng/mL) ± %RPD 1300 ng/mL ± 3.1% 2860 ng/mL ± 0.35%

NA = Not Applicable

Samples were diluted 1:100 and analyzed using external standard quantitation. The injection volume was decreased to produce a 

dilution factor of 400.

(1) NR = Not reportable; sample was not repeated since the spike level was less than 0.5x the sample concentration.

Table 19. DAL GW 317L 131002

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-029 DAL-GW-317L-0-131002 0.290 NA <0.0250 NA

ISO13-05-04-030 DAL-GW-317L-DB-131002 0.308 NA <0.0250 NA

ISO13-05-04-031 DAL-GW-317L-FMS-131002 1.18 88.1 0.989 98.9

Average Concentration (ng/mL) ± %RPD 0.299 ng/mL ± 6.0% <0.0250 ng/mL

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-029 DAL-GW-317L-0-131002 0.0932 NA 0.241 NA

ISO13-05-04-030 DAL-GW-317L-DB-131002 0.104 NA 0.245 NA

ISO13-05-04-031 DAL-GW-317L-FMS-131002 1.10 100 1.23 98.7

Average Concentration (ng/mL) ± %RPD 0.0986 ng/mL ± 11% 0.243 ng/mL ± 1.6%

NA = Not Applicable

Samples were analyzed using internal standard quantitation. Internal standard was added to the samples during sample 

preparation. 
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REPORT NO. ISO13-05-04

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Table 20. DAL GW 324L 130927

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-032 DAL-GW-324L-0-130927 219 NA 74.6 NA

ISO13-05-04-033 DAL-GW-324L-DB-130927 203 NA 69.7 NA

ISO13-05-04-034 DAL-GW-324L-FMS-130927 363 76.0 236 81.9

Average Concentration (ng/mL) ± %RPD 211 ng/mL ± 7.6% 72.2 ng/mL ± 6.8%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-032 DAL-GW-324L-0-130927 55.3 NA 78.0 NA

ISO13-05-04-033 DAL-GW-324L-DB-130927 53.3 NA 77.7 NA

ISO13-05-04-034 DAL-GW-324L-FMS-130927 228 86.9 264 93.5

Average Concentration (ng/mL) ± %RPD 54.3 ng/mL ± 3.7% 77.9 ng/mL ± 0.39%

NA = Not Applicable

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

Table 21. DAL GW RW327R 131011

PFOA (1) PFBS (2)

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-035 DAL-GW-RW327R-0-131011 1180 NA 59.9 NA

ISO13-05-04-036 DAL-GW-RW327R-DB-131011 1190 NA 63.8 NA

ISO13-05-04-037 DAL-GW-RW327R-LS-131011 NR (3) NR (3) 150 88.1

ISO13-05-04-038 DAL-GW-RW327R-HS-131011 1910 72.0 943 88.1

Average Concentration (ng/mL) ± %RPD 1190 ng/mL ± 0.84% 61.9 ng/mL ± 6.3%

PFHS (2) PFOS (2)

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-035 DAL-GW-RW327R-0-131011 159 NA 617 NA

ISO13-05-04-036 DAL-GW-RW327R-DB-131011 169 NA 708 NA

ISO13-05-04-037 DAL-GW-RW327R-LS-131011 257 93.2 747 NC

ISO13-05-04-038 DAL-GW-RW327R-HS-131011 1050 88.8 1530 87.2

Average Concentration (ng/mL) ± %RPD 164 ng/mL ± 6.1% 663 ng/mL ± 14%

NA = Not Applicable

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

(1) Samples were diluted 1:100 and analyzed using internal standard quantitation. Internal standard was added to the samples 

during sample preparation. 

(2) Samples were diluted 1:100 and analyzed using external standard quantitation.

(3) NR = Not reportable; sample was not repeated since the spike level was less than 0.5x the sample concentration.
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Table 22. DAL GW 328R 130927

PFOA (1) PFBS (2)

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-039 DAL-GW-328R-0-130927 409 NA 33.8 NA

ISO13-05-04-040 DAL-GW-328R-DB-130927 397 NA 32.5 NA

ISO13-05-04-041 DAL-GW-328R-LS-130927 NR (3) NR (3) 74.1 81.8

ISO13-05-04-042 DAL-GW-328R-HS-130927 787 76.6 428 78.6

Average Concentration (ng/mL) ± %RPD 403 ng/mL ± 3.0% 33.2 ng/mL ± 3.9%

PFHS (2) PFOS (2)

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-039 DAL-GW-328R-0-130927 52.4 NA 274 NA

ISO13-05-04-040 DAL-GW-328R-DB-130927 51.0 NA 265 NA

ISO13-05-04-041 DAL-GW-328R-LS-130927 94.8 86.4 311 NC

ISO13-05-04-042 DAL-GW-328R-HS-130927 461 82.0 693 85.1

Average Concentration (ng/mL) ± %RPD 51.7 ng/mL ± 2.7% 270 ng/mL ± 3.3%

NA = Not Applicable

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

(1) Samples were diluted 1:10 (0, DB, LS) or 1:100 (HS) and analyzed using internal standard quantitation. Internal standard 

was added to the samples during sample preparation. 

(2) Samples were diluted 1:10 (0, DB, LS) or 1:100 (HS) and analyzed using external standard quantitation.

(3) NR = Not reportable; sample was not repeated since the spike level was less than 0.5x the sample concentration.
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Table 23. DAL GW 328L 130927

PFOA (1) PFBS (1)

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-043 DAL-GW-328L-0-130927 108 NA 45.7 NA

ISO13-05-04-044 DAL-GW-328L-DB-130927 109 NA 44.9 NA

ISO13-05-04-045 DAL-GW-328L-LS-130927 NR (3) NR (3) NR (3) NR (3)

ISO13-05-04-046 DAL-GW-328L-HS-130927 207 98.0 143 97.7

Average Concentration (ng/mL) ± %RPD 109 ng/mL ± 0.92% 45.3 ng/mL ± 1.8%

PFHS (2) PFOS (2)

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-043 DAL-GW-328L-0-130927 17.6 NA 1.29 NA

ISO13-05-04-044 DAL-GW-328L-DB-130927 16.1 NA 1.18 NA

ISO13-05-04-045 DAL-GW-328L-LS-130927 17.0 NC 1.97 73.0

ISO13-05-04-046 DAL-GW-328L-HS-130927 92.6 75.9 87.0 86.3

Average Concentration (ng/mL) ± %RPD 16.9 ng/mL ± 8.9% 1.24 ng/mL ± 8.9%

NA = Not Applicable

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

(1) Samples were diluted 1:10 and analyzed using internal standard quantitation. Internal standard was added to the samples 

during sample preparation. 

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

(3) NR = Not reportable; sample was not repeated since the spike level was less than 0.5x the sample concentration.
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-04

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Table 24. DAL GW 330R 130927

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-047 DAL-GW-330R-0-130927 278 NA 1430 NA

ISO13-05-04-048 DAL-GW-330R-DB-130927 281 NA 1440 NA

ISO13-05-04-049 DAL-GW-330R-LS-130927 669 77.6 1860 NC

ISO13-05-04-050 DAL-GW-330R-HS-130927 1130 85.0 2320 88.0

Average Concentration (ng/mL) ± %RPD 280 ng/mL ± 1.1% 1440 ng/mL ± 0.69%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-047 DAL-GW-330R-0-130927 163 NA 676 NA

ISO13-05-04-048 DAL-GW-330R-DB-130927 163 NA 688 NA

ISO13-05-04-049 DAL-GW-330R-LS-130927 613 90.2 1160 96.2

ISO13-05-04-050 DAL-GW-330R-HS-130927 1080 91.9 1730 105

Average Concentration (ng/mL) ± %RPD 163 ng/mL ± 0.0% 682 ng/mL ± 1.8%

NA = Not Applicable

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

Samples were diluted 1:100 and analyzed using external standard quantitation. 

Table 25. DAL GW 330L 130927

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-051 DAL-GW-330L-0-130927 83.9 NA 1360 NA

ISO13-05-04-052 DAL-GW-330L-DB-130927 82.5 NA 1310 NA

ISO13-05-04-053 DAL-GW-330L-FMS-130927 481 79.4 NR (1) NR (1)

ISO13-05-04-051; LMS DAL-GW-330L-0-LMS NA NA 2350 99.1

Average Concentration (ng/mL) ± %RPD 83.2 ng/mL ± 1.7% 1340 ng/mL ± 3.7%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-051 DAL-GW-330L-0-130927 462 NA 181 NA

ISO13-05-04-052 DAL-GW-330L-DB-130927 455 NA 177 NA

ISO13-05-04-053 DAL-GW-330L-FMS-130927 925 93.4 681 101

Average Concentration (ng/mL) ± %RPD 459 ng/mL ± 1.5% 179 ng/mL ± 2.2%

NA = Not Applicable

Samples were diluted 1:00 and analyzed using external standard quantitation. 

(1) NR = Not reportable; sample was not repeated since the spike level was less than 0.5x the sample concentration.
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-04

PAGE 25 OF 28

Table 26. DAL GW RW331S 131011

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-054 DAL-GW-RW331S-0-131011 422 NA 432 NA

ISO13-05-04-055 DAL-GW-RW331S-DB-131011 428 NA 427 NA

ISO13-05-04-056 DAL-GW-RW331S-FMS-131011 1200 77.5 1270 84.0

Average Concentration (ng/mL) ± %RPD 425 ng/mL ± 1.4% 430 ng/mL ± 1.2%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-054 DAL-GW-RW331S-0-131011 160 NA 465 NA

ISO13-05-04-055 DAL-GW-RW331S-DB-131011 161 NA 457 NA

ISO13-05-04-056 DAL-GW-RW331S-FMS-131011 1040 88.1 1410 95.5

Average Concentration (ng/mL) ± %RPD 161 ng/mL ± 0.62% 461 ng/mL ± 1.7%

NA = Not Applicable

Samples were diluted 1:00 and analyzed using external standard quantitation. 

Table 27. DAL GW 335R 131002

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-057 DAL-GW-335R-0-131002 4680 NA 1230 NA

ISO13-05-04-058 DAL-GW-335R-DB-131002 4650 NA 1250 NA

ISO13-05-04-059 DAL-GW-335R-FMS-131002 9820 103 6110 97.0

Average Concentration (ng/mL) ± %RPD 4670 ng/mL ± 0.64% 1240 ng/mL ± 1.6%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-057 DAL-GW-335R-0-131002 1650 NA 6440 NA

ISO13-05-04-058 DAL-GW-335R-DB-131002 1660 NA 6510 NA

ISO13-05-04-059 DAL-GW-335R-FMS-131002 6540 97.8 11900 109

Average Concentration (ng/mL) ± %RPD 1660 ng/mL ± 0.60% 6480 ng/mL ± 1.1%

NA = Not Applicable

Samples were diluted 1:100 and analyzed using external standard quantitation. 
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-04

PAGE 26 OF 28

Table 28. DAL GW GRS04 131011

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-060 DAL-GW-GRS04-0-131011 5530 NA 2830 NA

ISO13-05-04-061 DAL-GW-GRS04-DB-131011 5410 NA 2730 NA

ISO13-05-04-062 DAL-GW-GRS04-FMS-131011 10800 106 7940 103

Average Concentration (ng/mL) ± %RPD 5470 ng/mL ± 2.2% 2780 ng/mL ± 3.6%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-060 DAL-GW-GRS04-0-131011 9540 NA 2690 NA

ISO13-05-04-061 DAL-GW-GRS04-DB-131011 9140 NA 2940 NA

ISO13-05-04-062 DAL-GW-GRS04-FMS-131011 15400 121 7720 98.6

Average Concentration (ng/mL) ± %RPD 9340 ng/mL ± 4.3% 2820 ng/mL ± 8.9%

NA = Not Applicable

Samples were diluted 1:100 and analyzed using external standard quantitation. 

Table 29. Trip Blank

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-063 DAL-GW-TRIP01-0 (1) <0.0240 NA <0.0250 NA

ISO13-05-04-064 DAL-GW-TRIP01-LS (2) 0.856 85.6 0.974 97.4

ISO13-05-04-065 DAL-GW-TRIP01-MS (2) 98.2 98.2 95.3 95.3

ISO13-05-04-066 DAL-GW-TRIP01-HS (2) 964 96.4 932 93.2

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-04-063 DAL-GW-TRIP01-0 (1) <0.0400 NA <0.0232 NA

ISO13-05-04-064 DAL-GW-TRIP01-LS (2) 0.915 91.6 0.894 89.4

ISO13-05-04-065 DAL-GW-TRIP01-MS (2) 98.2 98.4 106 107

ISO13-05-04-066 DAL-GW-TRIP01-HS (2) 968 97.0 1130 114

NA = Not Applicable

(1) Samples were analyzed using internal standard quantitation. Internal standard was added to the sample during sample 

preparation.

(2) Samples were diluted 1:10 (LS, MS) or 1:100 (HS) and analyzed using external standard quantitation. 
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-04

PAGE 27 OF 28

Table 30. Rinseate Blank

PFOA PFBS PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL)

Concentration 

(ng/mL)

Concentration 

(ng/mL)

Concentration 

(ng/mL)

ISO13-05-04-067 DAL-GW-324L-RB-130927 <0.0240 <0.0250 <0.0400 <0.0232

Samples were analyzed using internal standard quantitation. Internal standard was added to the sample during sample 

preparation.

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 10-29 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. ISO13-05-04 

7 Signatures 

J /// ^//3 

Susan T. Wolf, 3M Ecmcipa! Analytical Investigator Date 

William K. Reagen, Ph.D., SM EnvironmentalTechnical Director Date 

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

project. 

i / vl|lWj(3 

Quality Assurance Representative Date 

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

Environmental Laboratory. 

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