3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-01

PAGE 1 OF 28

Final Report

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

Collected from Decatur, AL

1st Quarter 2013

Laboratory Request Number: ISO13-05-01

Method Requirement: 3M Method ETS-8-044.1

Report Date – Date of Final Signature

Testing Laboratory

3M Environmental Health and Safety Operations

Environmental Laboratory

3M Center, Bldg 260-05-N-17

St. Paul, MN 55144

Requester 

Gary Hohenstein

3M Building 224-5W-03

Saint Paul, MN 55144-1000

Phone: (651) 737-3570

The testing reported herein meet the requirements of ANSI/ISO/IEC 17025:2005 “General 

Requirements for the Competence of Testing and Calibration Laboratories”, in 

accordance with the A2LA Testing Certificate # 2052.01. 
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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 ISO13-05-01

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

Collected from Decatur, AL

1st 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 March 21, March 22, March 27, and

March 28, 2013 and returned to the 3M Environmental Laboratory on March 29, 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 ISO13-05-01.

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 analyzed for PFOA, PFBS, PFHS, and PFOS by ETS-8-044.1 “Method of Analysis for 

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

Table 1 summarizes the sample results using the analytical method identified above. All results for 

quality control samples prepared and analyzed with the samples will be reported and discussed 

elsewhere in this report.

The testing reported herein meet the requirements of ANSI/ISO/IEC 17025:2005 

“General Requirements for the Competence of Testing and Calibration 

Laboratories”, in accordance with the A2LA Testing Certificate # 2052.01. 
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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)

ISO13-05-01-001 DAL-GW-203L-0-130328 220 35.3 233 796

ISO13-05-01-002 DAL-GW-203L-DB-130328 219 35.9 241 760

Average 220 35.6 237 778

%RPD Sample/Sample Dup 0.46 1.7 3.4 4.6

ISO13-05-01-005 DAL-GW-220R-0-130327 40.8 7.01 30.2 62.0

ISO13-05-01-006 DAL-GW-220R-DB-130327 41.3 7.00 31.9 59.8

Average 41.1 7.01 31.3 60.9

%RPD Sample/Sample Dup 1.2 0.14 5.5 3.6

ISO13-05-01-008 DAL-GW-220L-0-130327 45.0 7.89 37.4 63.8

ISO13-05-01-009 DAL-GW-220L-DB-130327 44.8 7.99 36.4 66.5

Average 44.9 7.94 36.9 65.2

%RPD Sample/Sample Dup 0.45 1.3 2.7 4.1

ISO13-05-01-011 DAL-GW-222R-0-130328 219 41.8 246 406

ISO13-05-01-012 DAL-GW-222R-DB-130328 232 42.8 258 422

Average 226 42.3 252 414

%RPD Sample/Sample Dup 5.8 2.4 4.8 3.9

ISO13-05-01-015 DAL-GW-227R-0-130321 273 16.5 69.4 574

ISO13-05-01-016 DAL-GW-227R-DB-130321 273 17.1 72.5 577

Average 273 16.8 71.0 576

%RPD Sample/Sample Dup 0.0 3.6 4.4 0.52

ISO13-05-01-019 DAL-GW-227L-0-130321 76.7 198 37.4 238

ISO13-05-01-020 DAL-GW-227L-DB-130321 81.7 204 37.0 244

Average 79.2 201 37.2 241

%RPD Sample/Sample Dup 6.3 3.0 1.1 2.5

ISO13-05-01-023 DAL-GW-310R-0-130322 925 1190 289 647

ISO13-05-01-024 DAL-GW-310R-DB-130322 917 1190 278 641

Average 921 1190 284 644

%RPD Sample/Sample Dup 0.87 0.0 3.9 0.93

ISO13-05-01-026 DAL-GW-312R-0-130328 1160 1160 501 809

ISO13-05-01-027 DAL-GW-312R-DB-130328 1080 1070 475 738

Average 1120 1120 488 774

%RPD Sample/Sample Dup 7.1 8.1 5.3 9.2

ISO13-05-01-029 DAL-GW-317L-0-130322 0.244 <0.0400 0.0809 0.155

ISO13-05-01-030 DAL-GW-317L-DB-130322 0.240 <0.0400 0.0918 0.207

Average 0.242 <0.0400 0.0864 0.181 (2)

%RPD Sample/Sample Dup 1.7 NA 13 29 (3)

NA = Not Applicable

(1) All samples associated with the reported sampling location were diluted and analyzed by external standard calibration unless 

noted otherwise. The analytical method uncertainties for the reported results using method ETS-8-044.1 by direct injection 

are as follows: PFOA ± 13%, PFBS ± 14%, PFHS ± 15%, and PFOS ± 22%.

(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: PFOS ± 25%. 

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

(4) The analytical method uncertainty has been expanded to ±32% for PFOA. See section 4 for further discussion. 

(5) The analytical method uncertainty has been expanded to ±31% for PFOA. See section 4 for further discussion.

(6) The analytical uncertainty has been expanded to ±34% for PFOA. See section 4 for further discussion.
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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)

ISO13-05-01-032 DAL-GW-324L-0-130321 254 67.0 71.0 203

ISO13-05-01-033 DAL-GW-324L-DB-130321 260 76.4 73.6 212

Average 257 (4) 71.7 72.3 208

%RPD Sample/Sample Dup 2.3 13 3.6 4.3

ISO13-05-01-035 DAL-GW-RW327R-0-130328 711 65.3 140 344

ISO13-05-01-036 DAL-GW-RW327R-DB-130328 715 63.7 140 348

Average 713 (5) 64.5 140 346

%RPD Sample/Sample Dup 0.56 2.5 0.0 1.2

ISO13-05-01-039 DAL-GW-328R-0-130321 321 32.2 50.8 185

ISO13-05-01-040 DAL-GW-328R-DB-130321 323 32.3 50.1 174

Average 322 (5) 32.3 50.5 180

%RPD Sample/Sample Dup 0.62 0.31 1.4 6.1

ISO13-05-01-043 DAL-GW-328L-0-130321 91.4 45.6 16.8 0.905

ISO13-05-01-044 DAL-GW-328L-DB-130321 91.0 44.6 16.8 0.855

Average 91.2 45.1 16.8 0.880

%RPD Sample/Sample Dup 0.44 2.2 0.0 5.7

ISO13-05-01-047 DAL-GW-330R-0-130322 265 1560 147 498

ISO13-05-01-048 DAL-GW-330R-DB-130322 284 1640 156 547

Average 275 1600 152 523

%RPD Sample/Sample Dup 6.9 5.0 5.9 9.4

ISO13-05-01-051 DAL-GW-330L-0-130322 167 549 300 176

ISO13-05-01-052 DAL-GW-330L-DB-130322 164 545 288 187

Average 166 547 294 182

%RPD Sample/Sample Dup 1.8 0.73 4.1 6.1

ISO13-05-01-054 DAL-GW-RW331S-0-130328 765 843 299 653

ISO13-05-01-055 DAL-GW-RW331S-DB-130328 750 841 291 630

Average 758 (6) 842 295 642

%RPD Sample/Sample Dup 2.0 0.24 2.7 3.6

ISO13-05-01-057 DAL-GW-335R-0-130328 3670 1340 1540 4860

ISO13-05-01-058 DAL-GW-335R-DB-130328 3860 1410 1600 4920

Average 3770 1380 1570 4890

%RPD Sample/Sample Dup 5.0 5.1 3.8 1.2

ISO13-05-01-060 DAL-GW-GRS04-0-130328 3190 2080 6680 2800

ISO13-05-01-061 DAL-GW-GRS04-DB-130328 3300 2040 6950 3380

Average 3250 2060 6820 3090

%RPD Sample/Sample Dup 3.4 1.9 4.0 19

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 ± 13%, PFBS ± 14%, PFHS ± 15%, and PFOS ± 22%.

(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: PFOS ± 25%.

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

(4) The analytical method uncertainty has been expanded to ±32% for PFOA. See section 4 for further discussion.

(5) The analytical method uncertainty has been expanded to ±31% for PFOA. See section 4 for further discussion.

(6) The analytical uncertainty has been expanded to ±34% for PFOA. See section 4 for further discussion.
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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 March 21, March 22, March 27, and March 28, 

2013 and returned to the 3M Environmental Laboratory on March 29, 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. 

Sample Description Key Code.

String Number String Descriptor Example

Example DAL-GW-317L-0-130322

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 130322 – March 22, 2013

6 Sample Type 0 =primary sample 

DB =duplicate sample

FMS = Field Matrix Spike

LS = Low field matrix spike

HS = High field matrix spike

2.3 Sample Preparation

4/2/13: Solvent dilution / external standard analysis. All samples and laboratory control spikes were 

diluted with methanol prior to sample analysis. Samples requiring a 1:10 dilution were prepared by 

removing a 1.0 mL aliquot of the well mixed sample and diluting it with 9.0 mL of methanol. Samples 

requiring a 1:20 dilution were prepared by removing a 0.5 mL aliquot of the well mixed sample and 

diluting it with 9.5 mL of methanol. Samples requiring a 1:50 dilution were prepared by removing a 0.2 

mL aliquot of the well mixed sample and diluting it with 9.8 mL of methanol. 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. Samples requiring a 1:200 dilution were prepared by removing a 0.05 mL aliquot of 
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-01

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the well mixed sample and diluting it with 10 mL of methanol. Sample injection values were increased 

for some samples if a smaller dilution factor (i.e.2 or 5) was desired.

4/5/13: Solvent dilution / external standard analysis. Samples and laboratory control spikes were 

diluted with methanol prior to sample analysis and spiked with surrogate recovery standards (SRSs) 13C4-PFOA and 13C4-PFOS to be used in lieu of target analyte matrix spikes. Sample sets LCS130405a, 203L, and 220R required a 1:10 dilution and were prepared removing 1.0 mL of the well 

mixed sample and diluting it with 8.9 mL of methanol and 0.1 mL of a solution containing SRSs (spiked 

at a nominal concentration of 1 ng/mL). The 203L samples were spiked with SRSs in lieu of 

appropriate target analyte field matrix spike samples. The 220R samples were spiked with SRSs since 

it was noted on the chain of custody for the field matrix spike that the cap was loose upon arrival at the 

sampling site thus making the recovery of this sample questionable. Sample set GRS04 required a 

1:1000 dilution and were prepared by removing a 0.01 mL aliquot of the well mixed sample and diluting 

it with 10 mL of methanol. Due to high recoveries for PFBS, PFHS, and PFOS determined during the 

initial analysis of the samples, a laboratory matrix spike (LMS) was prepared by spiking an aliquot of 

the primary sample at the same level as the target analyte field matrix spike (nominal concentration of 

5000 ng/mL). 

4/5/13: Direct injection/ internal standard analysis. Sample set 317L was 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. The following analytical runs were processed and reported herein:

4/2/13: Solvent dilution / external standard analysis for PFOA, PFBS, PFHS, PFOS; locations 220L, 

222R, 227R, 227L, 310R, RW312R, 317L, 324L, RW327R, 328R, 328L, 330R, 330L RW331S, 335R, 

GRS04, Trip Blanks and Rinseate Blank sample.

4/5/13: Solvent dilution / external standard analysis for PFOA, PFBS, PFHS, PFOS, 13C4-PFOA and 

13C4-PFOS; locations 203L, 220R, and GRS04.

4/6/13: Direct injection / internal standard analysis for PFOS; location 317L.

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.
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Table 3. Instrument Parameters

Instrument Name ETS Buster

Analysis Dates 4/2/13, 4/5/13, 4/6/13

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 5, 10, 25, 50 μL

Mass Spectrometer Applied Biosystems API 4000

Ion Source Turbo Spray

Polarity Negative

Software Analyst 1.6.1

Table 4. 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 5. Mass Transitions

Analyte

Mass Transition

Q1/Q3

Internal Standard Mass Transition

Q1/Q3

Reference Material 

Structure

PFOA

413/369

413/219 NA NA Linear and Branched

413/169

PFBS

299/80

NA NA Linear

299/99

PFHS

399/99

NA NA Linear

399/80

PFOS

499/99

[

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

499/130

[

13C4]-PFOA surrogate 417/372 NA NA Linear

[

13C4]-PFOS surrogate 503/80 NA NA Linear

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.

NA = Not Applicable

(1) Internal standard was used for the analysis of sampling location 317L for PFOS on 4/6/13.
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3 Data Analysis

3.1 Calibration

4/2/13: Solvent dilution / external standard calibration.

Diluted samples were analyzed against an external standard calibration curve for PFOA, PFBS, PFHS, 

and PFOS. Calibration standards were prepared by spiking known amounts of stock solutions 

containing the analytes of interest into 50 mL of 90:10 methanol: laboratory Milli-QTM water. A total of 

thirteen calibration standards ranging from 0.02 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.

4/5/13: Solvent dilution / external standard calibration.

Diluted samples were analyzed against an external standard calibration curve for, PFOA, PFBS, 

PFHS, PFOS, 13C4-PFOA and 13C4-PFOS. Calibration standards were prepared by spiking known 

amounts of stock solutions containing the analytes of interest into 50 mL of 90:10 methanol: laboratory 

Milli-QTM water. A total of thirteen calibration standards ranging from 0.02 ng/mL to 150 ng/mL 

(nominal) were analyzed (0.02 ng/mL to 25 ng/mL for the SRSs). 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.

4/6/13: 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 ng/mL. A total of ten curve points were analyzed with the samples ranging from 

0.025 ng/mL to 5.0 ng/mL. A quadratic, 1/x weighted, calibration curve of the ratio of the standard peak 

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

data were not forced through zero during the fitting process. 

For all analyses, each curve point was quantitated using the overall calibration curve and reviewed for 

accuracy. Method calibration accuracy requirements of 100±25% (100±30% for the lowest curve point) 

were met for all analytes. The correlation coefficient (r) was greater than 0.995 for all analytes.

3.2 System Suitability

A calibration standard was analyzed four times at the beginning of the analytical sequence to 

demonstrate overall system suitability. The acceptance criteria for system suitability samples is less 

than or equal to 5% relative standard deviation (RSD) for peak area or peak area ratio and retention 

time criteria of less than or equal to 2% RSD. These criteria were met for all analytes.

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.
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Table 6. LOQ

Analysis 

Date Calibration Dilution Factor

PFBA

LOQ, ng/mL

PFOA

LOQ, ng/mL

PFBS

LOQ, ng/mL

PFOS

LOQ, ng/mL

4/2/13 External standard

2 0.0384 0.0400 0.0400 0.0370

5 0.0960 0.100 0.100 0.0925

10 0.192 0.200 0.200 0.185

20 0.384 0.400 0.400 0.370

50 0.960 1.00 1.00 0.925

100 1.92 2.00 2.00 1.85

200 3.84 4.00 4.00 3.70

4/5/13

External standard 10 0.192 0.200 0.200 0.185

1000 19.2 20.0 20.0 18.5

4/6/13 Internal standard NA 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 with each sample preparation batch for the target 

analytes and analyzed in triplicate, while only low and high lab control spikes were prepared for the 

surrogates. LCSs were prepared by spiking known amounts of the analytes into synthetic groundwater 

or laboratory Milli Q water to produce the desired concentration. The LCS samples were then diluted in 

a similar manner as the samples (if diluted) prior to sample analysis. The method acceptance criteria, 

average of each level of LCS should be within 100% ± 20% with an RSD ≤20%, was met for all LCSs

with the following exceptions: 

4/5/13 analysis: The acceptance criteria for accuracy were met with the exception of the high set of 

LCS for PFOS (122%).

4/6/13 analysis: The acceptance criteria for accuracy were met with the exception of the low and mid

set of LCS for PFOS (123% and 125% respectively).

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

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

The following calculations were used to generate data in Table 7.

* 100%

Spike Concentration

Calculated Concentration LCSPercent Recovery =

* 100%

average LCS recovery

standard deviation LCS replicates LCS% RSD =
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Table 7. Lab Control Spike Results

ETS-8-044.1

Analyzed 4/2/13

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-130402-1 0.958 1.00 104 1.00 1.07 107

LCS-130402-2 0.958 0.981 102 1.00 1.05 105

LCS-130402-3 0.958 1.01 105 1.00 1.03 103

Average ± %RSD 104% ± 1.5% 105% ± 1.9%

LCS-130402-4 9.58 10.9 113 10.0 11.7 117

LCS-130402-5 9.58 10.6 110 10.0 11.8 118

LCS-130402-6 9.58 10.8 113 10.0 11.8 118

Average ± %RSD 112% ± 1.5% 118% ± 0.49%

LCS-130402-7 38.2 41.6 109 39.8 44.7 112

LCS-130402-8 38.2 41.8 109 39.8 44.9 113

LCS-130402-9 38.2 43.0 113 39.8 45.5 114

Average ± %RSD 110% ± 2.1% 113% ± 0.88%

ETS-8-044.1

Analyzed 4/2/13

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-130402-1 1.00 1.05 105 0.927 0.967 104

LCS-130402-2 1.00 1.03 103 0.927 0.948 102

LCS-130402-3 1.00 1.02 102 0.927 0.950 102

Average ± %RSD 103% ± 1.5% 103% ± 1.1%

LCS-130402-4 10.0 11.3 113 9.27 10.4 112

LCS-130402-5 10.0 11.2 112 9.27 10.7 115

LCS-130402-6 10.0 11.3 113 9.27 10.6 115

Average ± %RSD 113% ± 0.51% 114% ± 1.5%

LCS-130402-7 39.8 43.1 108 36.9 42.1 114

LCS-130402-8 39.8 43.3 109 36.9 42.3 115

LCS-130402-9 39.8 44.3 111 36.9 43.0 117

Average ± %RSD 109% ± 1.4% 115% ± 1.3%
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Table 7 continued. Lab Control Spike Results 

ETS-8-044.1

Analyzed 4/5/13

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-130405a-1 0.958 0.954 99.6 1.00 1.05 105

LCS-130405a-2 0.958 0.973 102 1.00 1.03 103

LCS-130405a-3 0.958 0.974 102 1.00 0.975 97.5

Average ± %RSD 101% ± 1.4% 102% ± 3.8%

LCS-130405a-4 9.58 10.8 113 10.0 10.9 109

LCS-130405a-5 9.58 10.3 107 10.0 10.9 109

LCS-130405a-6 9.58 10.6 111 10.0 11.1 111

Average ± %RSD 110% ± 2.8% 110% ± 1.1%

LCS-130405a-7 38.2 43.2 113 39.8 45.6 114

LCS-130405a-8 38.2 44.7 117 39.8 46.4 117

LCS-130405a-9 38.2 45.0 118 39.8 46.1 116

Average ± %RSD 116% ± 2.3% 116% ± 1.3%

ETS-8-044.1

Analyzed 4/5/13

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-130405a-1 1.00 1.10 110 0.927 0.939 101

LCS-130405a-2 1.00 1.02 102 0.927 0.948 102

LCS-130405a-3 1.00 0.997 99.7 0.927 0.947 102

Average ± %RSD 104% ± 5.2% 102% ± 0.57%

LCS-130405a-4 10.0 11.3 113 9.27 10.5 113

LCS-130405a-5 10.0 11.1 111 9.27 10.4 112

LCS-130405a-6 10.0 11.5 115 9.27 10.5 114

Average ± %RSD 113% ± 1.8% 113% ± 0.88%

LCS-130405a-7 39.8 45.3 114 36.9 44.5 121

LCS-130405a-8 39.8 47.0 118 36.9 44.8 121

LCS-130405a-9 39.8 46.6 117 36.9 45.6 124

Average ± %RSD 116% ± 1.8% 122% ± 1.4% (1)

(1) Average LCS recovery did not meet method acceptance criteria of 100 ± 30%.
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REPORT NO. ISO13-05-01

PAGE 12 OF 28

Table 7 continued. Lab Control Spike Results 

ETS-8-044.1

Analyzed 4/5/13

External 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-130405a-1 0.998 0.969 97.1 0.956 1.01 106

LCS-130405a-2 0.998 0.992 99.4 0.956 1.02 107

LCS-130405a-3 0.998 0.971 97.3 0.956 1.00 105

Average ± %RSD 97.9% ± 1.3% 106% ± 0.94%

LCS-130405a-4 9.98 10.2 103 9.56 9.87 103

LCS-130405a-5 9.98 10.1 101 9.56 9.79 102

LCS-130405a-6 9.98 10.1 101 9.56 9.83 103

Average ± %RSD 102% ± 1.1% 103% ± 0.56%

ETS-8-044.1

Analyzed 4/6/13

Internal Standard 

Calibration PFOS (Linear and Branched)

Lab ID

Spiked 

Concentration 

(ng/mL)

Calculated 

Concentration 

(ng/mL) %Recovery

LCS-130405b-1 0.0921 0.110 120

LCS-130405b-2 0.0921 0.108 118

LCS-130405b-3 0.0921 0.121 132

Average ± %RSD 123% ± 6.1%(1)

LCS-130405b-4 0.921 1.15 125

LCS-130405b-5 0.921 1.11 121

LCS-130405b-6 0.921 1.18 129

Average ± %RSD 125% ± 3.2%(1)

LCS-130405b-7 2.30 2.64 115

LCS-130405b-8 2.30 2.57 112

LCS-130405b-9 2.30 2.68 116

Average ± %RSD 114% ± 1.8%

(1) Average LCS recovery did not meet method acceptance criteria of 100 ± 30%.
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REPORT NO. ISO13-05-01

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%. 

• The analytical method uncertainty as calculated by ETS-12-012.2 for PFOS by external 

standard calibration was ± 14%. The recovery of the high set of LCS analyzed on 4/5/13 

was 122% for PFOS by external standard calibration for the samples analyzed on this 

date. The analytical method uncertainty was expanded to ± 22%.

• The analytical method uncertainty as calculated by ETS-12-012.2 for PFOS by internal 

standard calibration was ± 19%. The recovery of the mid set of LCS analyzed on 4/6/13 was 

125% for PFOS by internal standard calibration for the samples analyzed on this date. The 

analytical method uncertainty was expanded to ± 25%.

Table 8. Analytical Method Uncertainty

Analyte Calibration Standard Deviation (%) Method Uncertainty

PFOA External 6.64 ±13%

PFBS External 6.93 ±14%

PFHS External 7.25 ±15%

PFOS External NA ±22%

PFOS Internal NA ±25%

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 Concentraton

(Sample Concentration of FMS Average Concentration:FieldSample & FieldSample Dup.) FMS Recovery − =
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REPORT NO. ISO13-05-01

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Table 9. Field Matrix Spike Concentrations

Sampling location

Spike 

Level

PFOA

ng/mL

PFBS

ng/mL

PFHS

ng/mL

PFOS

ng/mL

203L Low 1.05 0.996 0.986 1.00

High 10.5 9.96 9.86 10.0

220R and 220L FMS 52.7 49.8 49.3 50.0

22R Low 105 99.6 98.6 100

High 527 498 493 500

227R and 328R Low 52.7 49.8 49.3 50.0

High 527 498 493 500

227L and 330R Low 527 498 493 500

High 1054 996 986 1000

310R, RW312R, and RW331S FMS 1054 996 986 1000

317L FMS 1.05 0.996 0.986 1.00

324L FMS 211 199 197 200

RW327R Low 105 99.6 98.6 100

High 1054 996 986 1000

328L Low 1.05 0.996 0.986 1.00

High 105 99.6 98.6 100

330L FMS 527 498 493 500

335R and GRS04 FMS 5270 4980 4930 5000

Trip Blank

Low 1.05 0.996 0.986 1.00

Mid 105 99.6 98.6 100

High 1054 996 986 1000

4 Data Summary and Discussion

Tables 10-29 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 lab matrix spike and surrogate recovery standards. 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, surrogate recovery standard laboratory matrix spikes, and 

laboratory matrix spikes met method acceptance criteria with the following exceptions:

• Location 203L; The low and high field matrix spikes prepared for the sample set was not 

appropriate as compared to the sample concentrations detected. The sample and sample 

duplicate were re-analyzed and spiked with surrogate recovery standard at a nominal 

concentration of 1 ng/mL and acceptable recoveries were obtained. 

• Location 220R; It was noted on the chain of custody that the FMS sample container arrived 

with a loose cap prior to sampling. In lieu of a target analyte matrix spike, the sample and 

sample duplicate were spiked with surrogate recovery standard at a nominal concentration of 1 

ng/mL and acceptable recoveries were obtained.
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REPORT NO. ISO13-05-01

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• Location 324L; The FMS recovery for PFOA was 68.8%. The analytical uncertainty for this 

location was expanded to ± 32%.

• Location RW327R; The FMS recovery for PFOA was 69.0%. The analytical uncertainty for this 

location was expanded to ± 31%.

• Location 328R; The FMS recovery for PFOA was 69.3%. The analytical uncertainty for this 

location was expanded to ± 31%.

• Location RW331S; The FMS recovery for PFOA was 66.7%. The analytical uncertainty for this 

location was expanded to ± 34%.

• Location GRS04; The FMS recovery was outside the method acceptance criteria for PFBS 

(238%), PFHS (407%), and PFOS (610%). A laboratory matrix spike (LMS) was prepared on 

the primary sample (ISO13-05-01-60) at the same spike level as the FMS sample (nominal 

concentration 5000 ng/mL). The LMS sample met method acceptance criteria. The sample 

results for GRS04 for this sampling event are similar to results observed for this location during 

previous sampling events in 2010, 2011, and 2012. FMS recoveries for these previous 

sampling events met method acceptance criteria, demonstrating that the method is 

appropriate for the sample matrix. Therefore, the recovery of the LMS was used to assess 

method accuracy for GRS04.
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REPORT NO. ISO13-05-01

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Table 10. DAL GW 203L

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-001 DAL-GW-203L-0-130328 220 NA 35.3 NA

ISO13-05-01-002 DAL-GW-203L-DB-130328 219 NA 35.9 NA

ISO13-05-01-003 DAL-GW-203L-LS-130328 NR NR NR NR

ISO13-05-01-004 DAL-GW-203L-HS-130328 NR NR NR NR

Average Concentration (ng/mL) ± %RPD 220 ng/mL ± 0.46% 35.6 ng/mL ± 1.7%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-001 DAL-GW-203L-0-130328 233 NA 796 NA

ISO13-05-01-002 DAL-GW-203L-DB-130328 241 NA 760 NA

ISO13-05-01-003 DAL-GW-203L-LS-130328 NR NR NR NR

ISO13-05-01-004 DAL-GW-203L-HS-130328 NR NR NR NR

Average Concentration (ng/mL) ± %RPD 237 ng/mL ± 3.4% 778 ng/mL ± 4.6%

13C4-PFOA (1) 13C4-PFOS (1)

3M LIMS ID Description %Recovery %Recovery

ISO13-05-01-001 DAL-GW-203L-0-130328 93.1 102

ISO13-05-01-002 DAL-GW-203L-DB-130328 98.9 97.0

Average Concentration (ng/mL) ± %RPD 96.0% ± 6.1% 99.5% ± 5.1%

NA = Not Applicable

NR= Not Reported; Spike levels were less than 0.5x the endogenous sample concentration.

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

(1) Surrogate recovery standards were added to the samples during sample preparation.
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REPORT NO. ISO13-05-01

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Table 11. DAL GW 220R

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-005 DAL-GW-220R-0-130327 40.8 NA 7.01 NA

ISO13-05-01-006 DAL-GW-220R-DB-130327 41.3 NA 7.00 NA

ISO13-05-01-007 DAL-GW-220R-FMS-130327 NR NR NR NR

Average Concentration (ng/mL) ± %RPD 41.1 ng/mL ± 1.2% 7.01 ng/mL ± 0.14%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-005 DAL-GW-220R-0-130327 30.2 NA 62.0 NA

ISO13-05-01-006 DAL-GW-220R-DB-130327 31.9 NA 59.8 NA

ISO13-05-01-007 DAL-GW-220R-FMS-130327 NR NR NR NR

Average Concentration (ng/mL) ± %RPD 31.1 ng/mL ± 5.5% 60.9 ng/mL ± 3.6%

13C4-PFOA (1) 13C4-PFOS (1)

3M LIMS ID Description %Recovery %Recovery

ISO13-05-01-005 DAL-GW-220R-0-130327 98.9 106

ISO13-05-01-006 DAL-GW-220R-DB-130327 94.2 99.6

Average Concentration (ng/mL) ± %RPD 96.5% ± 4.9% 103% ± 5.9%

NA = Not Applicable

NR= Not Reportable; Note on chain of custody form indicated that the sample cap was loose prior to sampling, thus making the 

FMS recovery questionable. 

Samples were diluted 1:10 and analyzed using external standard quantitation. The injection volume was increased to produce a 

dilution factor of 5.

(1) Surrogate recovery standards were added to the samples during sample preparation.
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REPORT NO. ISO13-05-01

PAGE 18 OF 28

Table 12. DAL GW 220L

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-008 DAL-GW-220L-0-130327 45.0 NA 7.89 NA

ISO13-05-01-009 DAL-GW-220L-DB-130327 44.8 NA 7.99 NA

ISO13-05-01-010 DAL-GW-220L-FMS-130327 85.7 77.4 51.0 86.5

Average Concentration (ng/mL) ± %RPD 44.9 ng/mL ± 0.45% 7.94 ng/mL ± 1.3%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-008 DAL-GW-220L-0-130327 37.4 NA 63.8 NA

ISO13-05-01-009 DAL-GW-220L-DB-130327 36.4 NA 66.5 NA

ISO13-05-01-010 DAL-GW-220L-FMS-130327 76.4 80.1 108 85.7

Average Concentration (ng/mL) ± %RPD 36.9 ng/mL ± 2.7% 65.2 ng/mL ± 4.1%

NA = Not Applicable

Samples were diluted 1:10 and analyzed using external standard quantitation. The injection volume was increased to produce a 

dilution factor of 5.

Table 13. DAL GW 222R

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-011 DAL-GW-222R-0-130328 219 NA 41.8 NA

ISO13-05-01-012 DAL-GW-222R-DB-130328 232 NA 42.8 NA

ISO13-05-01-013 DAL-GW-222R-LS-130328 313 NC 132 90.1

ISO13-05-01-014 DAL-GW-222R-HS-130328 606 72.2 571 106

Average Concentration (ng/mL) ± %RPD 226 ng/mL ± 5.8% 42.3 ng/mL ± 2.4%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-011 DAL-GW-222R-0-130328 246 NA 406 NA

ISO13-05-01-012 DAL-GW-222R-DB-130328 258 NA 422 NA

ISO13-05-01-013 DAL-GW-222R-LS-130328 345 NC 513 NC

ISO13-05-01-014 DAL-GW-222R-HS-130328 828 117 932 104

Average Concentration (ng/mL) ± %RPD 252 ng/mL ± 4.8% 414 ng/mL ± 3.9%

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. 
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REPORT NO. ISO13-05-01

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Table 14. DAL GW 227R

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-015 DAL-GW-227R-0-130321 273 NA 16.5 NA

ISO13-05-01-016 DAL-GW-227R-DB-130321 273 NA 17.1 NA

ISO13-05-01-017 DAL-GW-227R-LS-130321 320 NC 59.4 85.5

ISO13-05-01-018 DAL-GW-227R-HS-130321 650 71.5 422 81.4

Average Concentration (ng/mL) ± %RPD 273 ng/mL ± 0.0% 16.8 ng/mL ± 3.6%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-015 DAL-GW-227R-0-130321 69.4 NA 574 NA

ISO13-05-01-016 DAL-GW-227R-DB-130321 72.5 NA 577 NA

ISO13-05-01-017 DAL-GW-227R-LS-130321 113 85.3 655 NC

ISO13-05-01-018 DAL-GW-227R-HS-130321 488 84.6 1070 98.9

Average Concentration (ng/mL) ± %RPD 71.0 ng/mL ± 4.4% 576 ng/mL ± 0.52%

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 227L

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-019 DAL-GW-227L-0-130321 76.7 NA 198 NA

ISO13-05-01-020 DAL-GW-227L-DB-130321 81.7 NA 204 NA

ISO13-05-01-021 DAL-GW-227L-LS-130321 483 76.6 615 83.1

ISO13-05-01-022 DAL-GW-227L-HS-130321 877 75.7 1020 82.2

Average Concentration (ng/mL) ± %RPD 79.2 ng/mL ± 6.3% 201 ng/mL ± 3.0%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-019 DAL-GW-227L-0-130321 37.4 NA 238 NA

ISO13-05-01-020 DAL-GW-227L-DB-130321 37.0 NA 244 NA

ISO13-05-01-021 DAL-GW-227L-LS-130321 430 79.7 634 78.6

ISO13-05-01-022 DAL-GW-227L-HS-130321 814 78.8 1050 80.9

Average Concentration (ng/mL) ± %RPD 37.2 ng/mL ± 1.1% 241 ng/mL ± 2.5%

NA = Not Applicable

Samples were diluted 1:50 and analyzed using external standard quantitation. 
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Table 16. DAL GW 310R

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-023 DAL-GW-310R-0-130322 925 NA 1190 NA

ISO13-05-01-024 DAL-GW-310R-DB-130322 917 NA 1190 NA

ISO13-05-01-025 DAL-GW-310R-FMS-130322 1680 72.0 1990 80.3

Average Concentration (ng/mL) ± %RPD 921 ng/mL ± 0.87% 1190 ng/mL ± 0.0%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-023 DAL-GW-310R-0-130322 289 NA 647 NA

ISO13-05-01-024 DAL-GW-310R-DB-130322 278 NA 641 NA

ISO13-05-01-025 DAL-GW-310R-FMS-130322 1090 81.8 1560 91.6

Average Concentration (ng/mL) ± %RPD 284 ng/mL ± 3.9% 644 ng/mL ± 0.93%

NA = Not Applicable

Samples were diluted 1:50 and analyzed using external standard quantitation. 

Table 17. DAL GW RW312R

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-026 DAL-GW-RW312R-0-130328 1160 NA 1160 NA

ISO13-05-01-027 DAL-GW-RW312R-DB-130328 1080 NA 1070 NA

ISO13-05-01-028 DAL-GW-RW312R-FMS-130328 1860 70.2 1900 78.8

Average Concentration (ng/mL) ± %RPD 1120 ng/mL ± 7.1% 1120 ng/mL ± 8.1%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-026 DAL-GW-RW312R-0-130328 501 NA 809 NA

ISO13-05-01-027 DAL-GW-RW312R-DB-130328 475 NA 738 NA

ISO13-05-01-028 DAL-GW-RW312R-FMS-130328 1300 82.4 1600 82.7

Average Concentration (ng/mL) ± %RPD 488 ng/mL ± 5.3% 774 ng/mL ± 9.2%

NA = Not Applicable

Samples were diluted 1:50 and analyzed using external standard quantitation. 
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REPORT NO. ISO13-05-01

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Table 18. DAL GW 317L

PFOA (1) PFBS (1)

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-029 DAL-GW-317L-0-130322 0.244 NA <0.0400 NA

ISO13-05-01-030 DAL-GW-317L-DB-130322 0.240 NA <0.0400 NA

ISO13-05-01-031 DAL-GW-317L-FMS-130322 1.06 77.6 0.824 82.7

Average Concentration (ng/mL) ± %RPD 0.242 ng/mL ± 1.7% <0.0400 ng/mL

PFHS (1) PFOS (2)

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-029 DAL-GW-317L-0-130322 0.0809 NA 0.155 NA

ISO13-05-01-030 DAL-GW-317L-DB-130322 0.0918 NA 0.207 NA

ISO13-05-01-031 DAL-GW-317L-FMS-130322 0.859 78.4 0.931 75.0

Average Concentration (ng/mL) ± %RPD 0.0864 ng/mL ± 13% 0.181 ng/mL ± 29% (3)

NA = Not Applicable

(1) Samples were diluted 1:10 and analyzed using external standard quantitation. The injection volume was increased to produce 

a dilution factor of 2.

(2) Samples were analyzed using internal standard quantitation. 

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

Table 19. DAL GW 324L

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-032 DAL-GW-324L-0-130321 254 NA 67.0 NA

ISO13-05-01-033 DAL-GW-324L-DB-130321 260 NA 76.4 NA

ISO13-05-01-034 DAL-GW-324L-FMS-130321 402 68.8 (1) 243 86.0

Average Concentration (ng/mL) ± %RPD 257 ng/mL ± 2.3% (2) 71.7 ng/mL ± 13%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-032 DAL-GW-324L-0-130321 71.0 NA 203 NA

ISO13-05-01-033 DAL-GW-324L-DB-130321 73.6 NA 212 NA

ISO13-05-01-034 DAL-GW-324L-FMS-130321 234 82.0 394 93.3

Average Concentration (ng/mL) ± %RPD 72.3 ng/mL ± 3.6% 208 ng/mL ± 4.3%

NA = Not Applicable

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

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

(2) The analytical uncertainty for PFOA was expanded to ± 32%.
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REPORT NO. ISO13-05-01

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Table 20. DAL GW RW327R

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-035 DAL-GW-RW327R-0-130328 711 NA 65.3 NA

ISO13-05-01-036 DAL-GW-RW327R-DB-130328 715 NA 63.7 NA

ISO13-05-01-037 DAL-GW-RW327R-LS-130328 815 NC 156 91.9

ISO13-05-01-038 DAL-GW-RW327R-HS-130328 1440 69.0 (1) 871 81.0

Average Concentration (ng/mL) ± %RPD 713 ng/mL ± 0.56% (2) 64.5 ng/mL ± 2.5%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-035 DAL-GW-RW327R-0-130328 140 NA 344 NA

ISO13-05-01-036 DAL-GW-RW327R-DB-130328 140 NA 348 NA

ISO13-05-01-037 DAL-GW-RW327R-LS-130328 230 91.3 435 NC

ISO13-05-01-038 DAL-GW-RW327R-HS-130328 952 82.4 1200 85.4

Average Concentration (ng/mL) ± %RPD 140 ng/mL ± 0.0% 346 ng/mL ± 1.2%

NA = Not Applicable

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

Samples were diluted 1:20 and analyzed using external standard quantitation. 

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

(2) The analytical uncertainty for PFOA was expanded to ± 31%. 
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REPORT NO. ISO13-05-01

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Table 21. DAL GW 328R

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-039 DAL-GW-328R-0-130321 321 NA 32.2 NA

ISO13-05-01-040 DAL-GW-328R-DB-130321 323 NA 32.3 NA

ISO13-05-01-041 DAL-GW-328R-LS-130321 364 NC 76.4 88.7

ISO13-05-01-042 DAL-GW-328R-HS-130321 687 69.3 (1) 449 83.7

Average Concentration (ng/mL) ± %RPD 322 ng/mL ± 0.62% (2) 32.3 ng/mL ± 0.31%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-039 DAL-GW-328R-0-130321 50.8 NA 185 NA

ISO13-05-01-040 DAL-GW-328R-DB-130321 50.1 NA 174 NA

ISO13-05-01-041 DAL-GW-328R-LS-130321 95.0 90.4 226 NC

ISO13-05-01-042 DAL-GW-328R-HS-130321 459 82.9 626 89.3

Average Concentration (ng/mL) ± %RPD 50.5 ng/mL ± 1.4% 180 ng/mL ± 6.1%

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. 

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

(2) The analytical uncertainty for PFOA was expanded to ± 31%
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-01

PAGE 24 OF 28

Table 22. DAL GW 328L

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-043 DAL-GW-328L-0-130321 91.4 NA 45.6 NA

ISO13-05-01-044 DAL-GW-328L-DB-130321 91.0 NA 44.6 NA

ISO13-05-01-045 DAL-GW-328L-LS-130321 98.2 NC 46.0 NC

ISO13-05-01-046 DAL-GW-328L-HS-130321 170 74.8 128 83.2

Average Concentration (ng/mL) ± %RPD 91.2 ng/mL ± 0.44% 45.1 ng/mL ± 2.2%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-043 DAL-GW-328L-0-130321 16.8 NA 0.905 NA

ISO13-05-01-044 DAL-GW-328L-DB-130321 16.8 NA 0.855 NA

ISO13-05-01-045 DAL-GW-328L-LS-130321 18.2 NC 1.72 84.0

ISO13-05-01-046 DAL-GW-328L-HS-130321 96.0 80.3 75.9 75.0

Average Concentration (ng/mL) ± %RPD 16.8 ng/mL ± 0.0% 0.880 ng/mL ± 5.7%

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. The injection volume was increased to produce a

dilution factor of 2 (0, DB, and LS) or 5 (HS).

Table 23. DAL GW 330R

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-047 DAL-GW-330R-0-130322 265 NA 1560 NA

ISO13-05-01-048 DAL-GW-330R-DB-130322 284 NA 1640 NA

ISO13-05-01-049 DAL-GW-330R-LS-130322 740 88.3 2110 NC

ISO13-05-01-050 DAL-GW-330R-HS-130322 1140 82.1 2410 81.3

Average Concentration (ng/mL) ± %RPD 275 ng/mL ± 6.9% 1600 ng/mL ± 5.0%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-047 DAL-GW-330R-0-130322 147 NA 498 NA

ISO13-05-01-048 DAL-GW-330R-DB-130322 156 NA 547 NA

ISO13-05-01-049 DAL-GW-330R-LS-130322 586 88.1 1020 99.5

ISO13-05-01-050 DAL-GW-330R-HS-130322 1010 87.1 1350 82.8

Average Concentration (ng/mL) ± %RPD 152 ng/mL ± 5.9% 523 ng/mL ± 9.4%

NA = Not Applicable

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

Samples were diluted 1:50 and analyzed using external standard quantitation. 
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-01

PAGE 25 OF 28

Table 24. DAL GW 330L

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-051 DAL-GW-330L-0-130322 167 NA 549 NA

ISO13-05-01-052 DAL-GW-330L-DB-130322 164 NA 545 NA

ISO13-05-01-053 DAL-GW-330L-FMS-130322 589 80.4 969 84.7

Average Concentration (ng/mL) ± %RPD 166 ng/mL ± 1.8% 547 ng/mL ± 0.73%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-051 DAL-GW-330L-0-130322 300 NA 176 NA

ISO13-05-01-052 DAL-GW-330L-DB-130322 288 NA 187 NA

ISO13-05-01-053 DAL-GW-330L-FMS-130322 726 87.6 622 88.1

Average Concentration (ng/mL) ± %RPD 294 ng/mL ± 4.1% 182 ng/mL ± 6.1%

NA = Not Applicable

Samples were diluted 1:20 and analyzed using external standard quantitation. 

Table 25. DAL GW RW331S

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-054 DAL-GW-RW331S-0-130328 765 NA 843 NA

ISO13-05-01-055 DAL-GW-RW331S-DB-130328 750 NA 841 NA

ISO13-05-01-056 DAL-GW-RW331S-FMS-130328 1460 66.7 (1) 1600 76.1

Average Concentration (ng/mL) ± %RPD 758 ng/mL ± 2.0% (2) 842 ng/mL ± 0.24%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-054 DAL-GW-RW331S-0-130328 299 NA 653 NA

ISO13-05-01-055 DAL-GW-RW331S-DB-130328 291 NA 630 NA

ISO13-05-01-056 DAL-GW-RW331S-FMS-130328 1060 77.6 1370 72.9

Average Concentration (ng/mL) ± %RPD 295 ng/mL ± 2.7% 642 ng/mL ± 3.6%

NA = Not Applicable

Samples were diluted 1:50 and analyzed using external standard quantitation. 

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

(2) The analytical uncertainty for PFOA was expanded to ± 34%
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-01

PAGE 26 OF 28

Table 26. DAL GW 335R

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-057 DAL-GW-335R-0-130328 3670 NA 1340 NA

ISO13-05-01-058 DAL-GW-335R-DB-130328 3860 NA 1410 NA

ISO13-05-01-059 DAL-GW-335R-FMS-130328 7550 71.8 5770 88.3

Average Concentration (ng/mL) ± %RPD 3770 ng/mL ± 5.0% 1380 ng/mL ± 5.1%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-057 DAL-GW-335R-0-130328 1540 NA 4860 NA

ISO13-05-01-058 DAL-GW-335R-DB-130328 1600 NA 4920 NA

ISO13-05-01-059 DAL-GW-335R-FMS-130328 5980 89.5 9890 100

Average Concentration (ng/mL) ± %RPD 1570 ng/mL ± 3.8% 4890 ng/mL ± 1.2%

NA = Not Applicable

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

Table 27. DAL GW GRS04

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-060 DAL-GW-GRS04-0-130328 3190 NA 2080 NA

ISO13-05-01-061 DAL-GW-GRS04-DB-130328 3300 NA 2040 NA

ISO13-05-01-062 DAL-GW-GRS04-FMS-130328 9010 109 13900 238 (1)

ISO13-05-01-060 DAL-GW-GRS04-0-130328 LMS NA NA 8040 121

Average Concentration (ng/mL) ± %RPD 3250 ng/mL ± 3.4% 2060 ng/mL ± 1.9%

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-060 DAL-GW-GRS04-0-130328 6680 NA 2800 NA

ISO13-05-01-061 DAL-GW-GRS04-DB-130328 6950 NA 3380 NA

ISO13-05-01-062 DAL-GW-GRS04-FMS-130328 26900 407 (1) 33600 610 (1)

ISO13-05-01-060 DAL-GW-GRS04-0-130328 LMS 13000 129 9250 130

Average Concentration (ng/mL) ± %RPD 6820 ng/mL ± 4.0% 3090 ng/mL ± 19%

NA = Not Applicable

Samples were diluted 1:1000 and analyzed using external standard quantitation. 

(1) FMS did not meet acceptance criteria of 100 ± 30%. The LMS sample was used to demonstrate method accuracy for PFBS, 

PFHS, and PFOS.
3M ENVIRONMENTAL LABORATORY

REPORT NO. ISO13-05-01

PAGE 27 OF 28

Table 28. Trip Blank

PFOA PFBS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-063 DAL-GW-TRIP01-0 (1) <0.0384 NA <0.0400 NA

ISO13-05-01-064 DAL-GW-TRIP01-LS (1) 0.808 76.7 0.814 81.7

ISO13-05-01-065 DAL-GW-TRIP01-MS 87.6 83.1 89.2 89.6

ISO13-05-01-066 DAL-GW-TRIP01-HS 750 71.2 828 83.1

PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL) %Recovery

Concentration 

(ng/mL) %Recovery

ISO13-05-01-063 DAL-GW-TRIP01-0 (1) <0.0400 NA <0.0370 NA

ISO13-05-01-064 DAL-GW-TRIP01-LS (1) 0.761 77.2 0.782 78.2

ISO13-05-01-065 DAL-GW-TRIP01-MS 83.3 84.5 85.4 85.4

ISO13-05-01-066 DAL-GW-TRIP01-HS 925 93.8 926 92.6

NA = Not Applicable

Samples were diluted 1:10 and analyzed using external standard quantitation. The injection volume was increased to produce a

dilution factor of 2 for select samples.

(1) Samples were analyzed using a dilution factor of 2. 

Table 29. Rinseate Blank

PFOA PFBS PFHS PFOS

3M LIMS ID Description

Concentration 

(ng/mL)

Concentration 

(ng/mL)

Concentration 

(ng/mL)

Concentration 

(ng/mL)

ISO13-05-01-067 DAL-GW-RB-222R-0-130328 <0.0384 <0.0400 <0.0400 <0.0370

. 

Samples were diluted 1:10 and analyzed using external standard quantitation. The injection volume was increased to produce a

dilution factor of 2 for select samples.
3M ENVIRONMENTAL LABORATORY 

REPORT NO. IS013-05-01 

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 I 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 

Id 

Susan T. Wolf, 3M Rrinfcipal Analytical Investigator Date 

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

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

project. 

Quality Assur^ce Representative Date 

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

Environmental Laboratory. 

PAGE 28 OF 28