GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

GLP10-01-02: Interim Report 24 - Analysis of PFBS. PFHS. and PFOS in Groundwater 

Samples Collected at the Former Sludge Incorporation Area (FSIA) located in Decatur. AL. 

December 2011 

Study Title 

Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and 

Perfluorobutane Sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 

Site-Related Monitoring Program 

Data Requirement 

EPA TSCA Good Laboratory Practice Standards 40 CFR Part 792 

Study Director 

Jaisimha Kesari P.E., DEE 

Weston Solutions, Inc. 

1400 Weston Way 

Westchester, PA 19380 

Phone: 610-701-3761 

Author 

Susan Wolf 

3M Environmental Laboratory 

Interim Report Completion Date 

Date of signing 

Performing Laboratory 

3M Environmental Health and Safety Operations 

Environmental Laboratory 

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

St. Paul, MN 55144 

Project Identification 

GLP10-01-02-24 

Total Number of Pages 

110 

„ The testing reported herein meet the requirements of ISO/IEC 17025-2005 "General Requirements for the 

/ Competence of Testing and Calibration laboratories", in accordance with the A2LA Certificate #2052.01. 

IACCBEDITED I Testing that complies with this International Standard also operate in accordance with ISO 9001:2000. 

Testing Cert #2052.01 

Page 1 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

This page has been reserved for specific country requirements. 

Page 2 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

GLP COMPLIANCE STATEMENT 

Report Title: GLP10-01-02; Interim Report 24 - Analysis of PFBS, PFHS, and PFOS in Groundwater 

Samples Collected at the Former Sludge Incorporation Area (FSIA) in Decatur, AL, December 2011 

Study: Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and 

Perfluorobutane Sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 

Site-Related Monitoring Program. 

This analytical phase was conducted in compliance with Toxic Substances Control Act (TSCA) Good 

Laboratory Practice (GLP) Standards, 40 CFR 792, with the exceptions listed below: 

• These are environmental samples where there is no specific test substance, no specific test 

system and no dosing of a test system. 

• The reference substances have not been characterized under the GLPs and the stability under 

storage conditions at the test site have not been determined under GLPs. 

Gary Hohenstein, Snonsor Representative Date 

Jaisimha Kesan, P.E., DEE, Study Director 

Page 3 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

QUALITY ASSURANCE STATEMENT 

Report Title: GLP10-01-02; Interim Report 24 - Analysis of PFBS, PFHS, and PFOS in Groundwater 

Samples Collected at the Former Sludge Incorporation Area (FSIA) in Decatur, AL, December 2011 

Study: Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and 

Perfluorobutane Sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 

Site-Related Monitoring Program. 

This analytical phase was audited by the 3M Environmental Laboratory Quality Assurance Unit (QAU), 

as indicated in the following table. The findings were reported to the principal investigator (P.I.), 

laboratory management and study director. 

Inspection Dates Phase 

Date Reported to 

Inspection Dates Phase Testing Facility 

Management 

Study Director 

1/16/2012-1/17/2012 Data / Report 1/24/2012 1/24/2012 

QAU Representative Date 

Page 4 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

TABLE OF CONTENTS 

GLP Compliance Statement 3 

Quality Assurance Statement 4 

Table of Contents 5 

List of Tables 6 

Attachments 7 

1 Study Information 8 

2 Summary 9 

3 Introduction 11 

4 Test & Control Substances 11 

5 Reference Substances 12 

6 Test System 13 

7 Method Summary 13 

7.1 Methods 13 

7.2 Sample Collection 13 

7.3 Sample Preparation 13 

7.4 Analysis 14 

8 Analytical Results 15 

8.1 Calibration 15 

8.2 System Suitability 15 

8.3 Limit of Quantitation (LOQ) 16 

8.4 Continuing Calibration 16 

8.5 Blanks 16 

8.6 Lab Control Spikes (LCSs) 16 

8.7 Analytical Method Uncertainty 18 

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8.8 Field Matrix Spikes (FMS) 19 

9 Data Summary and Discussion 19 

10 Conclusion 35 

11 Data/Sample Retention 35 

12 Signatures 36 

LIST OF TABLES 

Table 1. Summarized PFBS, PFHS, and PFOS Results (FSIA Groundwater, December2011).... 10 

Table 2. Sample Description Key Code 13 

Table 3. Instrument Parameters 14 

Table 4. Liquid Chromatography Conditions 14 

Table 5. Mass Transitions 15 

Table 6. Limit of Quantitation (LOQ) 16 

Table 7. Laboratory Control Spike Recovery 17 

Table 8. Analytical Uncertainty 18 

Table 9. Field Matrix Spike Levels 19 

Table 10. DAL GW130R111208 20 

Table 11. DAL GW 130S 111208 20 

Table 12. DAL GW 130L111208 21 

Table 13. DAL GW 131R 111214 21 

Table 14. DAL GW 131S 111214 22 

Table15. DAL GW 131L 111214 22 

Table 16. DAL GW 133R 111214 23 

Table 17. DAL GW 133S 111214 23 

Table 18. DAL GW 133L 111214 24 

Table 19. DAL GW 134R111209 24 

Table 20. DALGW 134S 111209 25 

Page 6 of 110 
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Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Table 21. DAL GW 134L111209 25 

Table 22. DAL GW 135R 111214 26 

Table 23. DAL GW 135S 111214 26 

Table 24. DAL GW 135L 111214 27 

Table 25. DAL GW 136S 111213 27 

Table26. DALGW 136L 111213 28 

Table 27. DAL GW 137S 111209 28 

Table 28. DAL GW 137L 111209 29 

Table 29. DAL GW 138R 111214 29 

Table 30. DAL GW 138S 111214 30 

Table 31. DAL GW 138L 111214 30 

Table 32. DAL GW 140R111213 31 

Table 33. DAL GW141R111214 31 

Table 34. DAL GW 142R 111213 32 

Table 35. DAL GW 143R 111209 32 

Table36. DALGW 144R 111213 33 

Table 37. Trip Blank 1 33 

Table 38. Rinseate Blanks 34 

Table 39. Surrogate Recovery 34 

ATTACHMENTS 

Attachment A: Protocol Amendment 24 37 

Attachment B: Representative Chromatograms and Calibration Curves 45 

Attachment C: Analytical Method ETS-8-044.1 86 

Attachment D: Method Deviation 109 

Page 7 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

1 Study Information 

Sponsor 

3M Company 

Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

Study Director 

Jaisimha Kesari, P.E., DEE 

Weston Solutions, Inc. 

Westchester, PA 19380 

Phone: (610) 701-3761 

Fax: (610)701-7401 

j.kesari@westonsolutions.com 

Study Location 

Testing Facility 

3M EHS Operations 

3M Environmental Laboratory 

Building 260-5N-17 

St. Paul, MN 55144 

Study Personnel 

William K. Reagen, Ph.D., 3M Laboratory Manager 

Cleston Lange, Ph.D., Principal Analytical Investigator, (clanqeOimmm.com): phone (651)-733-9860 

Susan Wolf, 3M Analyst 

Chelsie Grochow, Analyst 

Kelly Ukes, Analyst 

Study Dates 

Study Initiation: March 8, 2010 

Interim 24 Experimental Termination: January 5,2012 

Interim Report Completion: Date of Interim Report Signing 

Location of Archives 

All original raw data and the analytical report have been archived at the 3M Environmental 

Laboratory according to 40 CFR Part 792. The test substance and analytical reference standard 

reserve samples are archived at the 3M Environmental Laboratory according to 40 CFR Part 792 

Page 8 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

2 Sutnmary 

The 3M Environmental Laboratory received groundwater samples from wells located at the Former 

Sludge Incorporation Area (FSIA) in Decatur, AL, representing twenty-seven different sampling 

locations. A total of eighty-eight sample bottles were received at the 3M Environmental Laboratory for 

perfluorooctane sulfonate (PFOS), perfluorohexane sulfonate (PFHS) and perfluorobutane sulfonate 

(PFBS), and included duplicate groundwater samples from each sampling location. Samples also 

included a field matrix spike (FMS) sample for each location, a trip blank set containing Miili-QTM water 

and appropriate trip blank spikes, and two equipment rinseate blanks. The equipment rinseate blanks 

did not have FMS samples prepared for detemnination of PFBS, PFHS, and PFOS recovery. 

The groundwater samples, trip blanks and two equipment rinseate blanks associated with GLP10-01-

02-24 were received from Weston personnel on December 20, 2011. All of the samples were prepared 

and analyzed for PFBS, PFHS, and PFOS following 3M Environmental Laboratory Method ETS-8-

044.1 and conducted under 3M project GLP-10-01-02-24. Many of the groundwater samples required 

dilution to attain PFBS, PFHS, and/or PFOS concentrations within the range of the curve, in some 

instances up to 100-fold dilution were required. The average measured PFBS, PFHS, and PFOS 

concentrations are summarized in Table 1. The equipment rinseate blanks and the trip blank sample 

were below the lower limit of quantitation (LLOQ) for PFBS, PFHS, and PFOS, indicating adequate 

control of sample contamination during shipping and sample collections. 

The PFBS concentration results for all groundwater samples ranged from <0.0250 ng/mL to 64.4 

ng/mL. The PFHS concentration results for all groundwater samples ranged from 0.0594 ng/mL to 827 

ng/mL. The PFOS concentration results for all groundwater samples ranged from 0.420 ng/mL to 1570 

ng/mL. The analytical method uncertainties associated with the reported results are: PFBS + 17%, 

PFHS + 18% and PFOS + 19%. For sample DAL GW 134L, the method uncertainty was expanded for 

PFOS. 

Page 9 of 110 
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Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Table 1. Summarized PFBS, PFHS, and PFOS Results (FSIA Groundwater, December 2011). 

PFBS PFHS PFOS 

Sampling Location 

Avg. Cone. 

(ng/mL) ± RPD 

Avg. Cone. 

(ng/mL) ± RPD 

Avg. Cone. 

(ng/mL) ± RPD 

DALGW 130R 111208 15.1 ±6.6% 119 ±0.84% 467 ± 9.9% 

DALGW 130S 111208 3.27 ±1.8% 25.6 ±1.6% 90.8 ±10% 

DALGW130L111208 1.49 ±2.0% 11.7 ±5.1% 66.3 ±1.4% 

DAL GW131R 111214 36.6 ± 0.55% 182 ±2.2% 1370 ±1.5% 

DAL GW131S 111214 0.688 ±0.15% 4.78 ± 3.6% 4.56 ± 3.7% 

DAL GW131L 111214 2.86 ±1.1% 18.8 ±0.53% 27.9 ± 0.72% 

DALGW133R111214 2.94 ±15% 20.9 ±17% 39.1 ± 10% 

DALGW 133S 111214 11.3 ±0.89% 79.7 ±1.4% 174 ±2.9% 

DAL GW133L 111214 7.90 ± 2.4% 58.7 ±4.1% 252 ±2.8% 

DALGW 134R 111209 47.5 ±0.21% 561 ± 0.54% 1570 ±1.3% 

DALGW 134S 111209 0.364 ±1.6% 4.22 ±1.7% 17.5 ±0.0% 

DAL GW134L 111209 10.5 ±1.9% 109 ±0.0% 436 ± 1.6% 

DALGW 135R 111214 64.4 ±1.6% 827 ±1.6% 1110 ±4.5% 

DALGW 135S 111214 0.991 ± 6.0% 7.90 ± 2.9% 5.81 ± 7.6% 

DALGW135L111214 7.09 ± 0.85% 47.6 ±1.5% 33.8 ± 7.7% 

DALGW 136S 111213 1.77 ±3.4% 11.4 ±3.5% 59.4 ±1.7% 

DAL GW136L 111213 1.91 ±2.6% 12.3 ±0.82% 64.4 ± 3.0% 

DALGW 137S 111209 0.120 ±13% 0.113±21%<^> 0.517 ± 32% 

DAL GW137L 111209 0.0868 ± 14% 0.0992 ± 9.8% 1.62 ± 8.0% 

DALGW 138R 111214 7.40 ± 0.95% 35.3 ±1.4% 300 ± 0.0% 

DALGW 138S 111214 3.64 ±4.1% 17.8 ±1.7% 160 ±1.3% 

DALGW 138L 111214 <0.0250 0.0594 ±12% 0.420 ± 20% 

DALGW 140R 111213 1.27 ±6.3% 14.1 ±2.1% 102 ±3.0% 

DALGW 141R 111214 0.0342 ± 5.3% 0.254 ± 4.3% 4.87 ± 4.1% 

DALGW 142R 111213 1.77 ±7.4% 9.97 ±4.6% 94.4 ± 0.32% 

DALGW 143R 111209 0.715 ±1.7% 2.33 ± 0.0% 15.6 ±6.4% 

DALGW 144R 111213 2.02 ± 3.0% 7.54 ± 0.66% 26.7 ±1.9%® 

Trip Blanks (Milli-QTM Water) <0.0250 <0.0250 <0.0371 

DALGW140R RB 111213 <0.0250 <0.0250 <0.0371 

DALGW133LRB 111214 <0.0250 <0.0250 <0.0371 

All samples reported using extemal standard calibration unless noted otherwise. The analytical method 

uncertainties associated with the reported results are: PFBS ± 17%, PFHS ± 18%, and PFOS ± 19%. 

(1) The analytical uncertainty has been adjusted for PFOS based on FMS recovery for DAL GW 134L to ± 39%. 

(2) The RPD did not meet method acceptance criteria of <20%. 

(3) Sample results reported using intemal standard calibration. 

(4) Sampling location did not have an appropriate FMS spike level to sufficiently evaluate PFOS recovery. 

Page 10 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

3 Introduction 

This analytical study was conducted as part of the Phase 3 Environmental Monitoring and Assessment 

Program for the 3M facility located in Decatur, Alabama. The objective of the overall program is to gain 

information regarding concentrations of perfluorooctane sulfonate (PFOS), perfluorohexane sulfonate 

(PFHS) and perfluorobutane sulfonate (PFBS), in various environmental media such as groundwater, 

soils and sediments that are associated with and near the Decatur facility. This analytical study was 

conducted to analyze groundwater samples collected from various wells located at the Former Sludge 

Incorporation Area (FSIA) in Decatur, AL for PFBS, PFHS, and PFOS in an effort to characterize onsite groundwater conditions. 

The 3M Environmental Laboratory prepared sample containers (250 mL high-density polyethylene 

bottles) which were shipped to Decatur, AL Weston personnel prior to field sampling. Sample 

containers for each sampling location included a field sample, field sample duplicate, and a field matrix 

spike sample. Each empty container was mari<ed with a "fill to here" line to produce a final sample 

volume of 200 mL. Containers designated for field matrix samples were fortified with an appropriate 

matrix spike solution containing PFBS (linear), PFHS (linear), and PFOS (linear) prior to being sent to 

the field for sample collection. See section 8.8 of the report for field matrix spike levels. Sample bottles 

for select sampling locations were fortified with internal standard and surrogate prior to sample collection 

to aid in sample analysis. Where applicable, internal standards were used to aid in the data quality 

objectives. Sampling locations reported for PFOS using internal standard calibraton included: DAL GW 

137S, DAL GW 137L, DAL GW 138L, DAL GW 141R, and DAL GW 144R. 

Samples were prepared and analyzed according to the procedure defined in 3M Environmental 

Laboratory method ETS-8-044.1 "Method of Analysis for the Determination of Perfluorinated 

Compounds In Water by High Perfomriance Liquid Chromatography/Mass Spectrometry Direct 

Injection Analysis". 

Table 1 summarizes the average PFBS, PFHS, and PFOS concentrations for the duplicate samples 

collected, the trip blank, and the aqueous equipment rinseate blank samples. Tables 10-38 summarize 

the individual sample results and the associated field matrix spike recoveries. Surrogate recoveries for 

samples quantitated using internal standard calibration are summarized in Table 39. All results for the 

quality control samples prepared and analyzed with the samples are reported and discussed elsewhere 

in this report. 

4 Test & Control Substances 

There was not a test substance or control substances in the classic sense of a GLP study. This study 

was purely analytical in nature. 

1 

Page 11 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

5 Reference Substances 

Reference Substance 

PFBS 

(predominantly linear 

isomer) 

PFHS 

(linear isomer) 

PFOS 

(branched and linear 

isomers) 

Chemical Name Perfluorobutane sulfonate Perfluorohexane sulfonate Perfluorooctane sulfonate 

Chemical Formula C4F9SO3K' CeFisSO/Na^ CsFiySOs K* 

Identifier Potassium Salt Sodium Salt 

Potassium Salt 

CAS#br-PFOSK 

Use 

Target Analyte Reference 

Standard 

Target Analyte Reference 

Standard 

Target Analyte Reference 

Standard 

Source 3M Wellington Wellington 

Expiration Date 1/10/2017 3/25/2018 3/17/2014 

Storage Conditions Frozen Frozen Frozen 

Chemical Lot Number 101 LPFHxSAMOS brPFOSK0708 

TCP Number TCR-121 TCR08-0018 TCR11-0010 

Physical Description White Powder Crystalline Liquid 

Purity 96.7% 100% NA(^' 

Reference Substance 

PFOS 

(branclied and linear 

isomers) "C4-PFOS Surrogate 

"Cj-PFOS 

Chemical Name Perfluorooctane sulfonate Perfluorooctane sulfonate 

Sodium 

Perfluorooctanesulfonate 

Chemical Formula CsF-iySOs K* CsFiySOa-Na* "CsFiySOaNa' 

Identifier 

Potassium Salt 

CAS #2795-39-3 Sodium Salt CAS#MPFC-C-0511 

Use FMS Reference Standard Sun^ogate Recovery 

Standard Intemal Standard 

Source Aldrich Wellington Wellington 

Expiration Date 2/4/2014 9/8/2013 05/25/2014 

Storage Conditions Room Temperature Frozen Frozen 

Chemical Lot Number 1424328V MPFOS0910 052411 

TCR Number TCR11-0028 TCR10-0044 TCR11-0016 

Physical Description White Powder Liquid Liquid 

Purity 99.7% NA<^> NA<^' 

(1) Reference standard at a concentration of 50 ± 2.5 |jg/mL 

(2) Custom mixture of seven mass-labeled ("C) perfluoroall<ylcaitioxylic adds, two mass labeled ("C) pertiuoroall<ylsulfonates 

and one mass-labeled ('^C) perfluoro-1-octanesulfonamide at a nominal concentration of 5 pg/mL 

Page 12 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

6 Test System 

The test systems for this study are groundwater samples collected from wells located in Decatur, AL by 

Weston Solutions, Inc. personnel. Samples for this study are "real world" samples, not dosed with a 

specific lot of test substance. 

Table 2. Sample Description Key Code. 

String Number String Descriptor Example 

Example DAL GW131R 0111214 

1 Sampling Location DAL = Decatur, Alabama 

2 Well ID GW= Groundwater 

3 Sampling Point Example: 131 

4 Well Level R = Residuum shallow water-bearing zone 

L = Bedrock water-bearing zone 

S = Epikarst middle water-bearing zone 

5 Sampling Date 111214-December 14,2011 

6 Sample Type 0=primary sample 

DB=duplicate sample 

FMS = Field Matrix Spike 

7 Method Summary 

7.1 Methods 

Analysis for all analytes was completed following 3M Environmental Laboratory method ETS-8-044.1 

"Method of Analysis for the Detemnination of Perfluorinated Compounds In Water by High Perfomnance 

Liquid Chromatography/Mass Spectrometry Direct Injection Analysis". 

7.2 Sample Collection 

Samples were collected in 250 mL Nalgene^'^ (high-density polyethylene) bottles prepared at the 3M 

Environmental Laboratory. Sample bottles associated with GLP10-01-02-24 were returned to the 

laboratory at ambient conditions on December 20, 2011. Samples were stored refrigerated at the 

laboratory after receipt. A set of laboratory prepared Trip Blank and Trip Blank field matrix spikes were 

sent with the sample collection bottles. 

7.3 Sample Preparation 

Samples were prepared by removing an aliquot of the well mixed sample and placing it in an autovial for 

analysis. 

Samples that required dilution were prepared by dilutions ImL sample with 9 mLs of Milli-Q water 

(dilution 1:10). Samples that required dilution were prepared by diluting 1mL of sample with 9 mLs of 

Milli Q water (dilution 1:10). Samples requiring a 1:100 dilution were prepared by diluting 0.1 mL of 

sample with 9.9 mLs of MilliQ water 

Sampling locations reported for PFOS using internal standard calibraton: During the preparation of the 

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

laboratory control samples (nominal concentration of 1 ng/mL). The samples bottles were spiked with 

an internal standard mix at a nominal concentration of 1 ng/mL prior to being sent to the field for sample 

collection. 

Page 13 of 110 
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Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

7.4 Analysis 

All study samples and quality control samples were analyzed for PFBS, PFHS, and PFOS using high 

perfomnance liquid chromatography/ tandem mass spectrometry (HPLC/MS/MS). Detailed instrnment 

parameters, the liquid chromatography gradient program, and the specific mass transitions analyzed are 

described in the raw data hard copies placed in the final data packet, and are briefly described below. 

Table 3. Instrument Parameters. 

Instrument Name ETSKirk ETS Buster 

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

Analysis Date 

12/27/11 - PFBS, PFHS, and PFOS 

Extemal standard calibration 

1/4/12 - PFOS 

Intemal standard calibration 

Liquid Chromatograph Agilent 1290 Agilent 1100 

Guard column Betasil C18 (4.6 mm X 100 mm), 5n Prism RP (2.1 mm X 50 mm), 5n 

Analytical column Betasil 018 (4.6 mm X 100 mm), 5n Betasil 018 (2.1 mm X 100 mm), 5n 

Injection Volume 10 nL 10 uL 

Mass Spectrometer Applied Biosystems fiP\ 5500 Applied Biosystems /\Pi 4000 

Ion Source Turbo Spray Turbo Spray 

Electrode Turbo ion electrode Turbo ion electrode 

Polarity Negative Negative 

Software Analyst 1.5.2 Analyst 1.4.2 

Table 4. Liquid Chromatography Conditions. 

step Total Time Flow Rate Percent A PercentB 

Number (min) (fdJmin) (2 mM ammonium acetate) (MethanoO 

ETS-8-044.1 Analyzed 12/27/11 

0 0 750 97.0 3.0 

1 2.0 750 97.0 3.0 

2 14.5 750 5.0 95.0 

3 15.5 750 5.0 95.0 

4 16.5 750 97.0 3.0 

5 20.0 750 97.0 3.0 

ETS-8-044.1 Analyzed 1/4/12 

0 0 300 97.0 3.0 

1 2.0 300 97.0 3.0 

2 14.5 300 5.0 95.0 

3 15.5 300 5.0 95.0 

4 16.5 300 97.0 3.0 

5 20.0 300 97.0 3.0 

Page 14 of 110 
Table 5. Mass Transitions. 

GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Artalyte Mass Transition 

Q1/Q3 

Reference 

Material 

structure 

Intemal 

standard 

Mass Transition 

Q1/Q3 

PFBS 

299/80 

Linear NA NA 299/99 

PFHS 399/80 

Linear NA NA 399/99 

PFOS 

499/80 

Branctiedand 

Linear PFOS 499/99 t^C^PFOS'^' 507/80 Branctiedand Linear PFOS t^C^PFOS'^' 507/80 

499/130 

Branctiedand 

Linear t^C^PFOS'^' 507/80 

["CJPFOS - surrogate 503/80 Linear t^CalPFOS'^^ 507/80 

Dwell time was 20 or 50 msec for each transition. The individual transitions were summed to produce a "total 

ion chromatogram" (TIC), which was used for quantitation. 

(1) Intemal standard and surrogate were only used for PFOS for sampling locations DAL GW 137S, DAL 

GW 137L, DAL GW 138L, DAL GW 141R, and DAL GW 144R. 

8 Analytical Results 

8.1 Calibration 

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 prepared in 

Milli Q water. A total of fifteen spiked standards ranging from 0.025 ng/mL to 100 ng/mL (nominal) were 

analyzed. A quadratic, 1/x weighted, calibration curve of the 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 confimned accuracy of each curve point. 

For sampling locations DAL GW 137S, DAL GW 137L, DAL GW 138L, DAL GW 141R, and DAL GW 

144R for PFOS: Samples were analyzed using a stable isotope intemal standard calibration curve. 

Calibration standards were prepared by spiking known amounts of the stock solution containing the 

target analytes into a laboratory-prepared synthetic groundwater containing calcium and magnesium. A 

separate internal standard spiking solution was prepared and an aliquot was added at the same level to 

all calibration standards and laboratory control samples at a nominal concentration of 1 ng/mL. A 

calibration curve ranging from 0.025 ng/mL to 100 ng/mL (nominal) was analyzed (0.025 ng/mL to 10 

ng/mL for ["CJPFOS surrogate). A quadratic, 1/x weighted, calibration curve of the peak area ratios 

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 confimned accuracy of each curve point. 

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 con-elation coefficient (r) was greater than 0.995 for all analytes. 

8.2 System Suitability 

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

demonstrate overall system suitability. The acceptance criteria of less than or equal to 5% relative 

standard deviation (RSD) for peak area and retention time criteria of less than or equal to 2% RSD was 

met for PFBS, PFHS, PFOS, and f ^C4]PF0S surrogate. 

Page 15 of 110 
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Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

8.3 Limit of Quantitation (LOQ) 

The LOQ for this analysis is the lowest non-zero calibration standard in the curve that meets linearity 

and accuracy requirements and for which the area counts or area ratio are at least twice those of the 

appropriate blanks. The LOQ for all analytes can be found in Table 6. 

Table 6. Limit of Quantitation (LOQ). 

Ana/ys/s Date Dilution PFBS 

LOQ, ng/mL 

PFHS 

LOQ, ng/mL 

PFOS 

LOQ, ng/mL 

12/27/11 Analysisextemal standard 

calibration 

12/27/11 Analysis- 1 0.0250 0.0250 0.0371 

extemal standard 

calibration 

10 0.250 0.250 0.371 

12/27/11 Analysisextemal standard 

calibration 

100 2.50 2.50 3.71 

1/4/12 Analysisintemal standard 

calibration 

1 NA NA 0.0928 

NA = Not Applicable 

8.4 Continuing Calibration 

During the course of each analytical sequence, continuing calibration verification samples (CCVs) were 

analyzed to confinn that the instrument response and the initial calibration curve were still in control. All 

CCVs met method criteria of 100% ± 25% for PFBS, PFHS, PFOS, and ["CJPFOS surrogate. 

8.5 Blanks 

Three types of blanks were prepared and analyzed with the samples: solvent blanks, trip blanks, and 

equipment rinseate blanks. Solvent blank results were reviewed and used to evaluate method 

performance to determine the LOQ for PFBS, PFHS, PFOS, and ["CJPFOS surrogate. Trip blanks 

reflect the shipping and sample collection conditons the sample bottles and samples experience. 

Equipment rinseate blanks are aqueous samples that reflect the efficiency of equipment cleaning in the 

field between different sample collections and are proof of no cross contamination of samples from the 

equipment. 

8.6 Lab Control Spikes (LCSs) 

Low, mid, and high-level lab control spikes were prepared and analyzed in triplicate with each 

preparation set. LCSs were prepared by spiking known amounts of the analyte into Milli Q water or 

synthetic groundwater to produce the desired concentration. The spiked water samples were then 

prepared and analyzed in the same manner as the samples. The method acceptance criteria, average 

of LCS at each level should be within 100% ± 20% with an RSD <20%, were met for PFBS, PFHS, 

PFOS, and [^^C4]PF0S surrogate LCS samples. 

The following calculations were used to generate data in Table 7 for laboratory control spikes. 

LCS Percent Recovery 

Calculated Concentration 

Spike Concentration 

*100% 

LCS% RSD = ^^P"''^*^^ ' 100% 

average LCS recovery 

Page 16 of 110 
Table 7. Laboratory Control Spike Recovery. 

GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

ETS-8-044.1 

Analyzed 12/27/11 

Extemal standard 

calibration PFSS PFHS 

Lab ID 

Spiked 

Concentration 

(ng/mL) 

Calculated 

Concentration 

(ng/mL) YoRecovery 

Spiked 

Concentration 

(ng/mL) 

Calculated 

Concentration 

(ng/mL) YoRecovery 

LCS-111221^ 0.498 0.598 120 0.497 0.506 102 

LCS-111221-5 0.498 0.583 117 0.497 0.496 99.9 

LCS-111221-6 0.498 0.584 117 0.497 0.488 98.2 

Average ±%RSD 118 ±1.5% 100% ±1.9% 

LCS-111221-7 498 5.78 116 4.97 5.03 101 

LCS-111221-6 498 5.70 115 4.97 4.98 100 

LCS-111221-9 498 5.68 114 4.97 5.07 102 

Average ±%RSD 115% ±0.87% 101% ±0.99% 

LCS-111221-10 29.9 26.3 87.9 29.9 24.4 81.5 

LCS-111221-11 29.9 30.2 101 29.9 28.9 96.5 

LCS-111221-12 29.9 28.0 93.8 29.9 29.4 98.3 

Average ± %RSD 94.2% ±7.0% 92.1% ±10% 

ETS-8-044.1 

Analyzed 12/27/11 

Extemal standard 

calibration PFOS( 'Branched and Linear) 

Lab ID 

Spiked 

Concentration 

(ng/mL) 

Calculated 

Concentration 

(ng/mL) YoRecovery 

LCS-111221-4 

LCS-111221-5 

LCS-111221-6 

0.462 

0.462 

0.462 

0.395 

0.383 

0.377 

85.6 

82.9 

81.7 

Average ± %RSD 83.4% ±2.4% 

LCS-111221-7 

LCS-111221-8 

LCS-111221-9 

4.62 

4.62 

4.62 

5.18 

5.11 

5.06 

112 

111 

109 

Average ± %RSD 111% ±1.4% 

LCS-111221-10 

LCS-111221-11 

LCS-111221-12 

27.8 

27.8 

27.8 

23.2 

26.4 

26.1 

83.5 

94.8 

93.8 

Average ± %RSD 90.7% ±6.9% 

Page 17 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Table 7 continued. Laboratory Control Spike Recovery. 

ETS-8-044.1 

Analyzed 1/4/12 

Intemal standard 

calibration PFOS (Branched and Linear) ["C^PFOS sunogat e 

Lab ID 

Spiked 

Concentration 

(ng/mL) 

Calculated 

Concentration 

(ng/mL) YoRecovery 

Spiked 

Concentration 

(ng/mL) 

Calculated 

Concentration 

(ng/mL) YoRecovery 

LCS-120104-1 0.184 0.214 116 0,189 0,201 106 

LCS-120104-2 0,184 0.199 108 0.189 0,209 111 

LCS-120104-3 0.184 0.209 113 0.189 0,212 112 

Average ± %RSD 112 ±3.6% 110% ±2.9% 

LCS-120104-4 1,84 2.14 116 1,89 2,13 113 

LCS-120104-5 1.84 2.05 111 1,89 2,05 109 

LCS-120104-6 1,84 2.08 113 1,89 2,11 112 

Average ± %RSD 113% ±2.2% 111% ±1.9% 

LCS-120104-7 18.4 16.5 89.6 

LCS-120104-8 18.4 17.3 93.8 

LCS-120104-9 18.4 17.2 93.6 

Average ± %RSD 92.3% ± 2.6% 

8.7 Analytical Method Uncertainty 

Analytical 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 

method uncertainty is calculated by multiplying the standard deviation by a factor of 2, which 

con-esponds to a confidence level of 95%. The most recent 50 data points were used to generate the 

method uncertainty values listed in Table 8. 

Table 8. Analytical Uncertainty. 

Analyte Standard Deviation Method Uncertainty 

PFBS 8.51 ±17% 

PFHS 8.98 ±18% 

PFOS 9.29 ±19% 

Page 18 of 110 
GLP10-01-02; interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

8.8 Field Matrix Spikes (FMS) 

A field matrix spike (FMS) was collected at each sampling point to verify that the analytical method is 

applicable to the collected matrix. Field matrix spikes were generated by adding a measured volume of 

field sample to a container spiked by the laboratory with PFBS (linear), PFHS (linear), and PFOS 

(linear+branched) prior to shipping sample containers for sample collection. Field matrix spike 

recoveries within method acceptance criteria of 100±30% confinn that "unknown" components in the 

sample matrix do not significantly interfere with the extraction and analysis of the analytes of interest. 

Field matrix spike concentrations must be 50% of the sample concentration to be considered an 

appropriate field spike. Field matrix spikes are presented in section 9 of this report. 

Table 9. Field Matrix Spike Levels. 

Sampling Location Spike Level PFBS, ng/mL PFHS, ng/mL PFOS, ng/mL 

136R, 137R, 137S, 137L, 138L, 141R FMS 1.01 0,998 0.998 

131S, 134S, 135S 143R FMS 20,2 20.0 20,0 

130L, 142R, 144R FMS 50.5 49.9 49.9 

130S, 131U 133R, 1368, 136L, 140R FMS 101 99.8 99.8 

133S, 133L, 135L, 138R, 138S FMS 202 200 200 

130R, 134L, CW26C, CW26L FMS 503 499 499 

131R, 134R, 135R FMS 2010 2000 2000 

Trip Blank 

Low 1.01 0.998 0,998 

Trip Blank Mid 20,2 20,0 20.0 Trip Blank Mid-High 101 99,8 99,8 Trip Blank 

High 503 499 499 

(Sample Concentration of FMS-Average Concentration : Field Sample & Field Sample Dup.) ^ 

FMS Recovery = — * 100% 

Spike Concentraton 

9 Mats Summary adS Discussion 

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

locations as well as the Trip Blanks and rinseate blanks. Results and average values are rounded to 

three significant figures according to EPA rounding rules. Because of rounding, values may vary slightly 

from those listed in the raw data. Field matrix spike recoveries meeting the method acceptance criteria 

of ± 30%, demonstrate that the method was appropriate for the given matrix and their respective 

quantitative ranges. 

DAL GW 134L - The recovery of the FMS sample for PFOS was 61.2%. Based on the recovery of the 

FMS sample, the analytical uncertainty has been expanded for PFOS to ± 39%. 

DAL GW 137S - The sample/sample duplicate RPD was 21 % for PFHS and 32% for PFOS. 

DAL GW 141R - Sampling location did not have an appropriate FMS spike level for PFOS to 

accurately assess recovery. 

Page 19 of 110 
Table 10. DAL GW 130R 111208 

GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

PFes PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) %Recovery (ng/mL) YoRecovery (ng/mL) YoRecovery 

GLP10-01-02-24-001 DAL-GW-130R-O-111208 14.6 NA 118 NA 444 NA 

GLP10-01-02-24-002 DAL-GW-130R-DB-111208 15.6 NA 119 NA 490 NA 

GLP10-01-02-24-003 DAL-GW-130R-FMS-111208 482 92.8 551 86.7 878 82.4 

Average Concentration (ng/mL) ± YoRPD 15.1 ng/mL ±6.6Yo 119 ng/mL ±0.84Yo 467 ng/mL ±9.9Yo 

NA = Not Applicable 

Samples diluted 1:100 and reported fi-om extemal standard calibration. 

Table 11. DAL GW 1 SOS 111208 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery 

GLP10-01-02-24-004 DAL-GW-130S-0-111208 3.24 NA 25.8 NA 86.1 NA 

GLP10-01-02-24-005 DAL-GW-130S-DB-111208 3.30 NA 25.4 NA 95.4 NA 

GLP10-01-02-24-006 DAL-GW-130S-FMS-111208 97.7 93.5 110 84.6 186 95.4 

Average Concentration (ng/mL) ± YoRPD 3.27 ng/mL ±18% 25.6 ng/mL ±1.6Yo 90.8 ng/mL tlOYo 

NA = Not /Applicable 

Samples diluted 1:10 and reported from extemal standard calibration. 

Page 20 of 110 
Table 12. DAL GW 1 SOL 111208 

GLP10-01-02; Interim Report 24 

/^alysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

PFSS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) %Recovery (ng/mL) YoRecovery 

GLP10-01-02-24-007 DAL-GW-130L-0-111208 1.50 NA 11.4 NA 65.8 NA 

GLP10-01-02-24-008 DAL-GW-130L-DB-111208 1.47 NA 12.0 NA 66.7 NA 

GLP10-01-02-24-009 DAL-GW-130L-FMS-111208 52.1 100 54.7 86.2 110 87.7 

Average Concentration (ng/mL) ± YoRPD 1.49 ng/mL ±2.0Yo 11.7 ng/mL ±5.1Yo 66.3 ng/mL ±1.4Yo 

NA = Not /Applicable 

Samples diluted 1:10 and reported from extemal standard calibration. 

Table 13. DAL GW 131R 111214 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) %Recovery (ng/mL) YoRecovery (ng/mL) YoRecovery 

GLP10-01-02-24-010 DAL-GW-131R-0-111214 36.5 NA 184 NA 1360 NA 

GLP10-01-02-24-011 DAL-GW-131R-DB-111214 36.7 NA 180 NA 1380 NA 

GLP10-01-02-24-012 DAL-GW-131R-FMS-111214 2020 98.7 1970 89.4 2980 80.5 

Average Concentration (ng/mL) ± %RPD 36.6 ng/mL ± 0.55% 182 ng/mL ±2.2Yo 1370 ng/mL ±1.5Yo 

NA = Not /Applicable 

Samples diluted 1:100 and reported from extemal standard calibration. 

Page 21 of 110 
Table 14. DAL GW 1S1S 111214 

GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery 

GLP10-01-02-24-013 DAL-GW-131S-0-111214 0.688 NA 4.86 NA 4.64 NA 

GLP10-01-02-24-014 DAL-GW-131S-DB-111214 0.687 NA 4.69 NA 4.47 NA 

GLP10-01-02-24-015 DAL-GW-131S-FMS-111214 18.3 87.2 21.9 85.6 20.2 78.2 

Average Concentration (ng/mL) ± YoRPD 0.688 ng/mL ± 0.15Yo 4.78 ng//nL± 3.6% 4.56 ng/mL ±3.7Yo 

NA = Not Applicable 

Samples diluted 1:10 and reported from extemal standard calibration. 

Table 15. DAL GW 1S1L 111214 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery 

GLP10-01-02-24-016 DAL-GW-131L-0-111214 2.84 NA 18.8 NA 28.0 NA 

GLP10-01-02-24-017 DAL-GW-131L-DB-111214 2.87 NA 18.7 NA 27.8 NA 

GLP10-01-02-24-018 DAL-GW-131L-FMS-111214 95.7 91.9 112 93.4 103 75.3 

Average Concentration (ng/mL) ± YoRPD 2.86 ng/mL ±1.1Yo 18.8 ng/mL ±0.53% 27.9 ng/mL ±0.72% 

NA = Not /Applicable 

Samples diluted 1:10 and reported from extemal standard calibration. 

Page 22 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Table 16. DAL GW 133R 111214 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) XRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery 

GLP10-01-02-24-019 DAL-GW-133R-0-111214 3.16 NA 22.7 NA 41.1 NA 

GLP10-01-02-24-020 DAL-GW-133R-DB-111214 2.71 NA 19.1 NA 37.1 NA 

GLP10-01-02-24-021 DAL-GW-133R-FMS-111214 95.9 92.0 112 91.3 121 82.1 

Average Concentration (ng/mL) ± YoRPD 2.94 ng/mL ±75% 20.9 ng/mL ±17Yo 39.1 ng/mL ±10% 

NA = Not /Applicable 

Samples diluted 1:10 and reported from extemal standard calibration. 

Table 17. DAL GW 133S 111214 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) %Recovery 

GLP10-01-02-24-022 DAL-GW-133S-0-111214 11.3 NA 80.2 NA 176 NA 

GLP10-01-02-24-023 DAL-GW-133S-DB-111214 11.2 NA 79.1 NA 171 NA 

GLP10-01-02-24-024 DAL-GW-133S-FMS-111214 204 95.4 278 99.2 319 72.8 

Average Concentration (ng/mL) ± YoRPD 11.3 ng/mL ±0.89Yo 79.7ng»nL±14% f74 ng/mL ±2.9% 

NA = Not /Applicable 

Samples diluted 1:10 and reported fi-om extemal standard calibration. 

Page 23 of 110 
Table 18. DAL GW 1S3L 111214 

GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) %Recovery 

GLP10-01-02-24-025 DAL-GW-133L-0-111214 7.80 NA 59.9 NA 248 NA 

GLP10-01-02-24-026 DAL-GW-133L-DB-111214 7.99 NA 57.5 NA 255 NA 

GLP10-01-02-24-027 DAL-GW-133L-FMS-111214 198 94.1 241 91.2 411 79.8 

Average Concentration (ng/mL) ± YoRPD 7.90 ng/mL ±2.4% 58.7ng/mL±4.f% 252 ng/mL ±2.8% 

NA = Not /Applicable 

Samples diluted 1:10 and reported from extemal standard calibration. 

Table 19. DAL GW 134R 111209 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery 

GLP10-01-02-24-028 DAL-GW-134R-0-111209 47.4 NA 559 NA 1580 NA 

GLP10-01-02-24-029 DAL-GW-134R-DB-111209 47.5 NA 562 NA 1560 NA 

GLP10-01-02-24-030 DAL-GW-134R-FMS-111209 1870 90.7 2360 90.0 3080 75.5 

Average Concentration (ng/mL) ± YoRPD 47.5 ng/mL ±0.21Yo 561 ng/mL ±0.54Yo 1570 ng/mL ±1.3Yo 

NA = Not Applicable 

Samples diluted 1:100 and reported from extemal standard calibration. 

Page 24 of 110 
Table 20. DALGW 1S4S 111209 

GLP10-01-02; Interim Report 24 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

PFBS PFHS PFOS 

Concentration Concentration Concerrtration 

3M LIMS ID Description (ng/mL) %Recovery (ng/mL) YoRecovery (ng/mL) %Recovery 

GLP10-01-02-24-031 DAL-GW-134S-0-111209 0.361 NA 4.18 NA 17.5 NA 

GLP10-01-02-24-032 DAL-GW-134S-DB-111209 0.367 NA 4.25 NA 17.5 NA 

GLP10-01-02-24-033 DAL-GW-134S-FMS-111209 18.5 89.8 22.2 89.9 34.5 85.0 

Average Concentration (ng/mL) ± YoRPD 0.364 ng/mL ±7.6% 4.22ng'mL±7.7% 77.5 ng/mL ±0.0% 

NA = Not /Applicable 

Samples undiluted and reported from extemal standard calibration. 

Table 21. DAL GW 134L 111209 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) %Recovery (ng/mL) YoRecovery (ng/mL) YoRecovery 

GLP10-01-02-24-034 DAL-GW-134L-0-111209 10.4 NA 109 NA 432 NA 

GLP10-01-02-24-035 DAL-GW-134L-DB-111209 10.6 NA 109 NA 439 NA 

GLP10-01-02-24-036 DAL-GW-134L-FMS-111209 419 81.2 546 87.6 741 61.2TM 

Average Concentration (ng/mL) ± YoRPD 70.5 ng/mL ±7.9% 709 ng/mL ±0.0% 436 ng/mL ±7.6%'^ 

NA = Not /Applicable 

NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. 

Samples diluted 1:100 and reported fi-om extemal standard calibration. 

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

(2) Sample method uncertainty is expanded to ± 39%. 

Page 25 of 110 
Table 22. DAL GW 135R 111214 

GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) XRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery 

GLP10-01-02-24-037 DAL-GW-135R-0-111214 63.9 NA 820 NA 1130 NA 

GLP10-01-02-24-038 DAL-GW-135R-DB-111214 64.9 NA 833 NA 1080 NA 

GLP10-01-02-24-039 DAL-GW-135R-FMS-111214 1820 87.3 2740 95.7 2580 73.8 

Average Concentration (ng/mL) ± %RPD 64.4 ng/mL ±7.6% 827 ng/mL ±7.6% 7770 ng'mL ±4.5% 

NA = Not /Applicable 

Samples diluted 1:100 and reported from extemal standard calibration. 

Table 23. DAL GW 135S 111214 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) %Recovery 

GLP10-01-02-24-040 DAL-GW-135S-0-111214 0.961 NA 7.78 NA 5.59 NA 

GLP10-01-02-24-041 DAL-GW-135S-DB-111214 1.02 NA 8.01 NA 6.03 NA 

GLP10-01-02-24-042 DAL-GW-135S-FMS-111214 19.1 89.7 26.9 95.0 22.8 85.0 

Average Concentration (ng/mL) ± YoRPD 0.997 ng/mL ± 6.0% 7.90 ng/mL ±2.9% 5.87 ng/mL ± 7.6% 

NA = Not/Applicable 

Samples undiluted and reported fi-om extemal standard calibration. 

Page 26 of 110 
Table 24. DAL GW 135L 111214 

GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) %Recovery (ng/mL) YoRecovery (ng/mL) %Recovery 

GLP10-01-02-24-043 DAL-GW-135L-0-111214 7.06 NA 47.2 NA 32.5 NA 

GLP10-01-02-24-044 DAL-GW-135L-DB-111214 7.12 NA 47.9 NA 35.1 NA 

GLP10-01-02-24-045 DAL-GW-135L-FMS-111214 200 95.5 232 92.2 183 74.6 

Average Concentration (ng/mL) ± YoRPD 7.09 ng/mL ±0.85Yo 47.6 ng/mL ±7.5% 33.8 ng/mL ±7.7% 

NA = Not /Applicable 

Samples diluted 1:10 and reported from extemal standard calibration. 

Table 25. DAL GW 136S 111213 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) %Recovery (ng/mL) %Recovery (ng/mL) %Recovery 

GLP10-01-02-24-049 DAL-GW-136S-0-111213 1.80 NA 11.6 NA 59.9 NA 

GLP10-01-02-24-050 DAL-GW-136S-DB-111213 1.74 NA 11.2 NA 58.9 NA 

GLP10-01-02-24-051 DAL-GW-136S-FMS-111213 106 103 104 92.8 145 85.8 

Average Concentration (ng/mL) ± YoRPD 7.77 ng/mL ±3.4% 77.4 ng/mL ±3.5% 59.4 ng/mL ±7.7% 

NA = Not /Applicable 

Samples diluted 1:10 and reported from extemal standard calibration. 

Page 27 of 110 
Table 26. DAL GW 136L 111213 

GLP10-01-02; Interim Report 24 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery 

GLP10-01-02-24-052 DAL-GW-136L-0-111213 1.88 NA 12.3 NA 65.3 NA 

GLP10-01-02-24-053 DAL-GW-136L-DB-111213 1.93 NA 12.2 NA 63.4 NA 

GLP10-01-02-24-054 DAL-GW-136L-FMS-111213 104 101 106 93.9 153 88.8 

Average Concentration (ng/mL) ± YoRPD 7.97 ng/mL ± 2.6% 72.3 ng/mL ±0.82% 64.4 ng'mL± 3.0% 

NA= Not/Applicable 

Samples diluted 1:10 and reported from extemal standard calibration. 

Table 27. DAL GW 137S 111209 

PFBS PFHS PFOS 

Concerrtration Concerrtration Concerrtration 

3M LIMS ID Description (ng/mL) %Recovery (ng/mL) %Recovery (ng/mL) YoRecovery 

GLP10-01-02-24-058 DAL-GW-137S-0-111209 0.127 NA 0.125 NA 0.601 , NA 

GLP10-01-02-24-059 DAL-GW-137S-DB-111209 0.112 NA 0.101 NA 0.433 NA 

GLP10-01-02-24-060 DAL-GW-137S-FMS-111209 1.09 96.1 0.949 83.8 1.32 80.5 

Average Concentration (ng/mL) ± YoRPD 0.720 ng'mL± 73% 0.773 ng/mL ±27%TM 0.577 ng/mL ±32%'^'^ 

NA= Not Applicable 

Reported results for PFBS and PFHS are from extemal standard calibration. Reported results for PFOS are from intemal standard calibration. 

(1) RPD did not meet acceptance criteria of S20%. 

Page 28 of 110 
Table 28. DAL GW 137L 111209 

GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

PFBS PFHS PFOS 

Concentration Concentration Concerrtration 

3M LIMS ID Description (ng/mL) %Recovery (ng/mL) YoRecovery (ng/mL) %Recovery 

GLP10-01-02-24-061 DAL-GW-137L-0-111209 0.0928 NA 0.104 NA 1.68 NA 

GLP10-01-02-24-062 DAL-GW-137L-DB-111209 0.0807 NA 0.0943 NA 1.55 NA 

GLP10-01-02-24-063 DAL-GW-137L-FMS-111209 1.11 101 1.00 90.3 2.59 97.7 

Average Concentration (ng/mL) ± YoRPD 0.0868 ng/mL ±74% 0.0992 ng/mL± 9.8% 7.62 ng/mL ±8.0% 

NA = Not /Applicable 

Reported results for PFBS and PFHS are from extemal standard calibration. Reported results for PFOS are from intemal standard calibration. 

Table 29. DAL GW 138R 111214 

PFBS PFHS PFOS 

Concerrtration Concentration Concerrtration 

3M LIMS ID Description (ng/mL) %Recovery (ng/mL) YoRecovery (ng/mL) YoRecovery 

GLP10-01-02-24-064 DAL-GW-138R-0-111214 7.36 NA 35.0 NA 300 NA 

GLP10-01-02-24-065 DAL-GW-138R-DB-111214 7.43 NA 35.5 NA 300 NA 

GLP10-01-02-24-066 DAL-GW-138R-FMS-111214 202 96.3 220 92.4 451 75.5 

A\^erage Concentration (ng/mL) ± YoRPD 7.40 n»'mL± 0.95% 35.3 ng/mL ±7.4% 300 ng/mL ±0.0% 

NA = Not /Applicable 

Samples diluted 1:10 and reported from extemal standard calibration. 

Page 29 of 110 
Table 30. DAL GW 138S 111214 

GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

PFBS PFHS PFOS 

Concerrtration Concentration Concerrtration 

3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) %Recovery 

GLP10-01-02-24-067 DAL-GW-138S-0-111214 3.71 NA 17.9 NA 159 NA 

GLP10-01-02-24-068 DAL-GW-138S-DB-111214 3.56 NA 17.6 NA 161 NA 

GLP10-01-02-24-069 DAL-GW-138S-FMS-111214 191 92.8 203 92.6 299 69.5 

Average Concentration (ng/mL) ± YoRPD 3.64 ng/mL ±4.7% 77.8ng/mL± 7.7% 760 ng/mL ±7.3% 

NA = Not /Applicable 

Samples diluted 1:10 and reported from extemal standard calibration. 

Table 31. DAL GW 138L 111214 

PFBS PFHS PFOS 

Concentration Concentration Concerrtration 

3M LIMS ID Description (ng/mL) XRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery 

GLP10-01-02-24-070 DAL-GW-138L-0-111214 <0.0250 NA 0.0630 NA 0.461 NA 

GLP10-01-02-24-071 DAL-GW-138L-DB-111214 <0.0250 NA 0.0558 NA 0.379 NA 

GLP10-01-02-24-072 DAL-GW-138L-FMS-111214 1.00 99.0 0.939 88.1 1.40 98.2 

Average Concentration (ng/mL) ± YoRPD <0.0250 0.0594 ng/mL± 12% 0.420 ng/mL ±20% 

NA = Not /Applicable 

Reported results for PFBS and PFHS are from extemal standard calibration. Reported results for PFOS are from intemal standard calibration. 

Page 30 of 110 
Table 32. DAL GW140R 111213 

GLP10-01-02; Interim Report 24 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

PFBS PFHS PFOS 

Concerrtration Concerrtration Concerrtration 

3M LIMS ID Description (ng/mL) YoRecovery (ng/mLj^ %Recovery (ng/mL) YoRecovery 

GLP10-01-02-24-073 DAL-GW-140R-0-111213 1.23 NA 13.9 NA 100 NA 

GLP10-01-02-24-074 DAL-GW-140R-DB-111213 1.31 NA 14.2 NA 103 NA 

GLP10-01-02-24-075 DAL-GW-140R-FMS-111213 97.7 95.5 109 95.1 181 79.7 

Average Concentration (ng/mL) ± %RPD 7.27 ng/mL ±6.3% 74.7 ng/mL± 2.7% 702 ng/mL ±3.0% 

NA = Not Applicable 

Samples diluted 1:10 and reported from from extemal standard calibration. 

Table 33. DAL GW 141R 111214 

PFBS PFHS PFOS 

Concerrtration Concerrtration Concentration 

3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) %Recovery (ng/mL) YoRecovery 

GLP10-01-02-24-076 DAL-GW-141R-0-111214 0.0351 NA 0.259 NA 4.97 NA 

GLP10-01-02-24-077 DAL-GW-141R-DB-111214 0.0333 NA 0.248 NA 4.77 NA 

GLP10-01-02-24-078 DAL-GW-141 R-FMS-111214 1.00 95.6 1.15 89.8 5.80 NC 

Average Concentration (ng/mL) ± YoRPD 0.0342 ng/mL ±5.3% 0.254 ng/mL± 4.3% 4.87 ng/mL ±4.7%"^ 

NA = Not/Applicable 

NC = Not Calculated; Endogenous sample concentration greater than 2x spil<e level. 

Reported results for PFBS and PFHS are from extemal standard calibration. Reported results for PFOS are from intemal standard calibration. 

(1) Sampling location did not have an appropriate FMS spike level to suflicientiy evaluate PFOS recovery. 

Page 31 of 110 
Table 34. DAL GW 142R 111213 

GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

PFBS PFHS PFOS 

Concerrtration Concerrtration Concerrtration 

3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) XRecovery (ng/mL) YoRecovery 

GLP10-01-02-24-079 DAL-GW-142R-0-111213 1.83 NA 10.2 NA 94.5 NA 

GLP10-01-02-24080 DAL-GW-142R-DB-111213 1.70 NA 9.74 NA 94.2 NA 

GLP10-01-02-24-081 DAL-GW-142R-FMS-111213 48.2 92.0 53.8 87.8 131 73.4 

Average Concentration (ng/mL) ± YoRPD 7.77 ng/mL ±7.4% 9.97 ng/mL± 4.6% 94.4 ng/mL ±0.32% 

NA = Not /Applicable 

Samples diluted 1:10 and reported from extemal standard calibration. 

Table 35. DAL GW 143R 111209 

PFBS PFHS PFOS 

Concentration Concentration Concerrtration 

3M LIMS ID Description (ng/mL) %Recovery (ng/mL) %Recovery (ng/mL) YoRecovery 

GLP10-01-02-24-082 DAL-GW-143R-0-111209 0.709 NA 2.33 NA 16.1 NA 

GLP10-01-02-24-083 DAL-GW-143R-DB-111209 0.721 NA 2.33 NA 15.1 NA 

GLP10-01-02-24-084 DAL-GW-143R-FMS-111209 21.6 103 19.6 86.4 30.2 73.0 

Average Concerrtration (ng/mL) ± YoRPD 0.775 ng/mL ±7.7% 2.33 ng/mL ±0.0% 15.6 ng/mL ±6.4Yo 

NA = Not /Applicable 

Samples diluted 1:10 and reported from extemal standard calibration. 

Page 32 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Table 36. DAL GW 144R 111213 

PFBS PFHS PFOS 

Concentration Concentration Concerrtration 

3M LIMS ID Description (ng/mL) XRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery 

GLP10-01-02-24-085 DAL-GW-144R-0-111213 2.05 NA 7.56 NA 26.4 NA 

GLP10-01-02-24-086 DAL-GW-144R-DB-111213 1.99 NA 7.51 NA 26.9 NA 

GLP10-01-02-24-087 DAL-GW-144R-FMS-111213 55.9 107 47.4 79.9 70.0 86.9 

Average Concerrtration (ng/mL) ± YoRPD 2.02 ng/mL ±3.0% 7.54 ng/mL ±0.66Yo 26.7ng/mL±7.9% 

NA = Not /Applicable 

Reported results for PFBS and PFHS are from extemal standard calibration. Reported results for PFOS are from intemal standard calibration. 

Table 37. Trip Blank 1 

PFBS PFHS PFOS 

Concentration Concerrtration Concentration 

3M LIMS ID Description (ng/mL) XRecovery (ng/mL) %Recovery (ng/mL) YoRecovery 

GLP10-01-02-24-094 DAL-GW-TRIP01-0 <0.0250 NA <0.0250 NA <0.0371 NA 

GLP10-01-02-24-095 DAL-GW-TRIP01-LS 0.994 98.4 0.920 92.2 0.943 94.5 

GLP10-01-02-24-096 DAL-GW-TRIP01-MS 19.6 97.0 18.5 92.5 19.7 98.5 

GLP10-01-02-24-097 DAL-GW-TRIP01-MHS 101 100 93.6 93.8 86.5 86.7 

GLP10-01-02-24-098 DAL-GW-TRIP01-HS 499 99.2 467 93.6 412 82.6 

NA = Not /Applicable 

Reported results from extemal standard calibration. The MHS sample was diluted 1:10, ttieHS sample was diluted 1:100. 

Page 33 of 110 
Table 38. Rinseate Blanks 

GLP10-01-02; Interim Report 24 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

PFBS PFHS PFOS 

Concerrtration Concerrtration Concentration 

3M LIMS ID Description (ng/mL) %Recovery (ng/mL) YoRecovery^ (ng/mL) %Recovery 

GLP10-01-02-24-099 DAL-GW-140R-RB-111213 <0.0250 NA <0.0250 NA <0.0371 NA 

GLP10-01-02-24-100 DAL-GW-133L-RB-111214 <0.0250 NA <0.0250 NA <0.0371 NA 

NA = Not /Applicable 

Reported results from extemal standard calibration. 

Table 39. Surrogate Recovery 

3M LIMS ID Description 

PFOS surrogate 

Yo Recovery 

GLP10-01-02-24-058 DAL-GW-137S-0-111209 93.5 

GLP10-01-02-24-059 DAL-GW-137S-DB-111209 106 

GLP10-01-02-24-060 DAL-GW-137S-FMS-111209 102 

GLP10-01-02-24-061 DAL-GW-137L-0-111209 101 

GLP10-01-02-24-062 DAL-GW-137L-DB-111209 98.5 

GLP10-01-02-24-063 DAL-GW-137L-FMS-111209 91.8 

GLP10-01-02-24-070 DAL-GW-138L-0-111214 94.0 

GLP10-01-02-24-071 DAL-GW-138L-DB-111214 93.4 

GLP10-01-02-24-072 DAL-GW-138L-FMS-111214 97.7 

GLP10-01-02-24-076 DAL-GW-141 R-0-111214 93.7 

GLP10-01-02-24-077 DAL-GW-141 R-DB-111214 95.1 

GLP10-01-02-24-078 DAL-GW-141 R-FMS-111214 97.8 

GLP10-01-01-24-085 DAL-GW-144R-0-111213 102 

GLP10-01-01-24-086 DAL-GW-144R-DB-111213 96.9 

GLP10-01-01-24-087 DAL-GW-144R-FMS-111213 93.9 

Page 34 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

10 Conclusion 

Laboratory control spikes and field matrix spikes were used to determine the analytical method 

accuracy and precision for PFBS, PFHS, and PFOS. Analysis was successfully completed following 

3M Environmental Laboratory method ETS-8-044.1 described herein. 

11 Data/Sample Retention 

All remaining samples and associated project data (hardcopy and electronic) will be archived according 

to 3M Environmental Laboratory standard operating procedures. 

Page 35 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

12 Signatures 

Cleston Lange, Ph.D., 3M Principal Analytical Investigator Date 

William K. Reagen, Ph.D., 3M Environmental Laboratory Department Manager Date 

2-/ 

7-Z 

Gary / Date Hohlenstein, Sponsor Representative 

Jaisimha Kesapf, Study Director pate 

Page 36 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

ATTACHMENT A: PROTOCOL AMENDMENT 

Page 37 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Analytical Protocol: GLP10-01-02 

Amendment 24 

Study Title 

Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and 

Perfluorobutane sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M 

Decatur Phase 3 Site-Related Monitoring Program 

PROTOCOL AMENDMEI^T NO. 24 

Amendment Date: 

December 1, 2011 

Performing Laboratory 

3M Environmental, Health, and Safety Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55144-1000 

Laboratory Project Identification 

GLP10-01-02 

Sampling Event 

Former Sludge Incorporation Area (FSIA) Groundwater 

Page 1 of 7 

Page 38 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Analytical Protocol: GLP10-01-02 

Amendment 24 

This amendment modifies the following portion of protocol: 

"Analysis of PFOS, PFHS and PFBS in Groundwater, Soil and Sediment for the 3M 

Decatur Phase 3 Site-Related Monitoring Program" 

PROTOCOL READS: 

No changes to the wording of the protocol are required. 

AMEND TO READ: 

No changes to the wording of the protocol are required. This amendment only addresses and documents 

the addition of the General Project Outline (GPO) for the collection and analysis of groundwater samples 

from Decatur, AL, and conducted as part of the 3M Decatur Phase 3 Program for PFOS, PFHS and PFBS 

(GLP10-01-02). The anticipated sample collection will occur around the timeframe during the week of 

December 5, 2011. The groundwater samples for this sampling event will be entered into the 3M 

Environmental Laboratory LIMS as project GLP10-01-02-24 and reported as interim report GLP10-01-02-

24, (reflecting study GLP10-01-02 and amendment -24). 

Reason.-

The reason for this amendment is to document the General Project Outline (GPO) which describes the 

anticipate groundwater sample collection event to be conducted for the 3M Decatur, AL facility. 

The GPO is four pages in length and included as attached to this amendment form. 

Page 2 of 7 

Page 39 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Analytical Protocol: GLP10-01-02 

Amendment 24 

Amendment Approval 

Gary Hohensteri, Sponsor Representative Datn e 

Cleston Date C. Lange, Principal Analytical Investigator 

William Reagen, EHSppns Environmental Lab Management Date 

mil 

Jaisimha Kesari f*-^ , DEE, Study Director D^e 

Page 3 of 7 

Page 40 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Analytical Protocol: GLP10-01-02 

Amendment 24 

^IM i Environmental Health & Safety Operations, Environmental Laboratory 

General Project Outline 

To; Gary Hohenstein, 3M EHS&Opns 

From: Susan Wolf, 3M EHS&Opns; Environmental Lab 

cc: William Reagen, 3M EHS&Opns; Environmental Lab 

Cleston Lange, 3M EHS&Opns; Environmental Lab 

Jai Kesari, Weston Solutions 

Date December 1,2011 : 

Subject: Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and 

Perfluorobutane sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur 

Phase 3 Site-Related Monitoring Program; GLP Interim Report 24 - Former Sludge 

Incorporation Area (FSIA) Groundwater - December 2011 Sampling 

1 General Project Information 

3M Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone: (651) 737-3570 

Qahohenstein(5)mmm.com 

3W1 Environmental Laboratory Management 

William K. Reagen 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9739 

Contacts wkreaaen(3!mmm.com 

Principal Analytical Investigator 

Cleston Lange 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9860 

cclanaeOmmm.com 

Sampling Coordinator 

Timothy Frinal< 

Weston Solutions 

Timothy.frinakOwestonsolutions.com 

Phone: (334)-332-9123 

Lab Request Number CLP10-01-02-24 

Six Digit Department Number Dept #530711. Project #0022674449 

Project Schodule/Test Dates Sampling scheduled for the weel< of December 5, 2011 

All verbal and written correspondence will be directed to Gary Hohenstein. 

Page 4 of 7 

Page 41 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Analytical Protocol: GLP10-01-02 

Amendment 24 

2 Background Information and Project Objective(s) 

The 3M EHS Operations Laboratory (3M Environmental Lab) will receive and analyze groundwater 

samples collected from twenty-seven groundwater wells for Perfluorobutanesulfonate (PFBS), 

Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) from the Former Sludge 

Incorporation Area (FSIA). Analyses will be conducted under the GLP requirements of EPA TSCA Good 

Laboratory Practice Standards 40 CFR 792. 

Groundwater samples from Decatur, AL will be collected by Weston Solutions personnel the week of 

December 5, 2011. The 3M Environmental Laboratory v/ill prepare the sample bottles with all required 

spikes to ensure that results for PFBS, PFHS, and PFOS are of a known precision and accuracy. The final 

report will be submitted to Gary Hohenstein and Jai Kesari upon completion under interim report GLP10-

01-02-24. 

3 Project Schedule 

Sample collection bottles will be prepared by 3M Environmental Laboratory for sampling the week of December 

5, 2011. Sample bottles will be shipped in coolers to 3M Decatur for arrival by Monday, December 5, 2011. 

Sample bottles should be stored refrigerated on-site until sample collection. 

Martin Smith \ Weston Trailer 

3M Decatur Plant 

1400 State Docks Road 

Decatur, Alabama 35601 

4 Test Parameters 

The targeted limit of quantitation will be 0.025 ng/mL (ppb) for PFBS, PFHS, and PFOS. 

A total of thirty-one sampling locations have been specified. For each sampling location, a sample, sample 

duplicate and field matrix spike will be collected. Table 1 indicates the well ID and corresponding field spike 

level. The "fill to here" line on each 250 mL Nalgene bottle will be 200 mL. One sets of trip blanks consisting of 

reagent-grade water, a low-level trip blank spike, mid-level field spike, mid-high field spike, and a high-level trip 

blank spike will be prepared at the 3M Environmental Laboratory and sent to the sampling location with the 

other bottles. 

Based on previous sampling of the FSIA (GLP10-01-02-07, GLP10-01-02-011, and GLP10-01-02-18), more 

than half of the sample locations are expected to have PFHS and/or PFOS levels greater than 100 ng/mL. To 

aid in the quantitation of sampling locations with PFBS, PFHS and PFOS levels at expected concentrations of 

<50 ng/mL, sample bottles will contain the addition of internal standards '^02-PFBS, ^^Ca-PFHS, and ^^CgPFOS, as well as '^C4-PF0S surrogate. The trip blank sample, trip blank low and mid spikes will also include 

the addition of internal standard standards '^Oz-PFBS, '^Ca-PFHS, and ^^Cs-PFOS, as well as '^C4-PF0S 

surrogate. Two additional bottles will be prepared to be used for the preparation of the equipment rinseate 

blanks and will also contain the addition of intemal standards '*02-PFBS, ^'Ca-PFHS, and '*CB-PF0S, as well 

as '^C^-PFOS surrogate. A 1 -L bottle of laboratory reagent water will be provided to be used to collect the 

rinseate blanks. 

Page 5 of 7 

Page 42 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Analytical Protocol: GLP10-01-02 

Amendment 24 

Table 1. Sampling Locations and Field Matrix Spike levels. 

Set# Well No. Spike Cone. (ng/mL) 

1 * 136R, 137R, 137S, 137L, 

138L, 141R 

1.0 

2 * 131S,134S,135S,143R 20 

3 * 130L, 142R, 144R 50 

4 1308, 131L, 133R, 136S, 

136L, 140R 

100 

5 1338, 133L, 135L, 138R, 1388 200 

6 130R, 134L, CW26C, CW26L 500 

7 131R,134R,135R 2000 

Trip Blank 1 * 

20 * 

Trip Blank 

100 

Trip Blank 

500 

surrogate. 

5 Test Methods 

Samples will be prepared and analyzed by LC/MS/MS following ETS-8-044.1 "Method of Analysis for the 

Determination of Perfluorinated Compounds In Water by High Perfonnance Liquid Chromatography/Mass 

Spectrometry Direct Injection Analysis". The data quality objectives for these studies are quantitative results for 

the target analytes with an analytical accuracy of 100±30%. Field matrix spikes not yielding recoveries within 

100±30% will be addressed in the report and the final accuracy statement may be adjusted accordingly. Based 

on the results from previously collected samples from the FSIA, most sampling locations will require dilution with 

laboratory reagent water prior to sample analysis by ETS-8-044.1. 

6 Reporting Requirements 

For each sampling location, the report will contain the results for the sample, sample duplicate, and field matrix 

spike. Trip blank and trip blank spikes will be reported for the sampling event as will any equipment/rinseate 

blanks prepared in the field. Laboratory control spikes of reagent water prepared at the time of sample 

preparation will also be reported and used to evaluate the overall method accuracy and precision. Method 

blanks of reagent water prepared at the time of sample preparation will be used to determine the method 

detection limit. For those sampling locations where the field matrix spike level was not appropriate, due to 

higher than expected analyte concentrations, a laboratory matrix spike may be prepared and included in the 

final report. 

7 Email Correspondence 

Attachment A: Sampling Bottle Request 

Page 6 of 7 

Page 43 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Analytical Protocol: GLP10-01-02 

Amendment 24 

Attachment A 

Bollle request for 4lh quarter 2011 FSIA well sampling 

Young, Charles T. 

to:stwolf(^inmm.com 

11/29/2011 03:10 PM 

Cc:"Frinak, Timolhy R.", "SmilL Martin" 

From: "Young, Charles T." <Charles.Young@WestonSolutions.com> 

Sue: 

Tim Frinak and Martin Smith are setting up for groundwater sampling commencing next week at the 

following Former Sludge Incorporation Area monitoring wells: 

130R 133L 136S 140R 

130S 134R 136L 141R 

130L 134S 137R 142R 

131R 134L 137S 143R 

131S 135R 137L 144R 

131L 135S 138R CW26C 

133R 135L 138S CW26L 

133S 136R 138L 

Can you prepare a bottle set for shipment to Martin Smith's attention at Decatur with arrival by Tuesday, 

December 6, 2011? As with eartier rounds, analysis will be performed under GLP10-01-01 and GLP10-

01-02. 

Due to the relatively low GW levels at the site, some of the above wells may be dry and therefore will not 

be sampled. Martin will return any unused bottle sets should some of the locations have insufficient water 

for sampling. 

Thanks, 

Chartie 

Charles T. Young 

Technical Director 

Weston Solutions, Inc. 

1400 Weston Way (5-2) 

West Chester, PA 19380 

(610) 701-3787 

Fax (610) 701-3401 

CONFlDENTIALrrY: This email and attaclmients may contain information which is 

confidential and proprietary. Disclosure or use of any such confidential or proprietciry 

infonnation without the written permission of Weston Solutions, Inc. is strictly prohibited. If you 

received this email in error, please notify the sender by return e-mail and delete this email from 

your system. Thank you. 

Page 7 of 7 

Page 44 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

ATTACHMENT B: REPRESENTATIVE SAMPLE CHROMATOGRAMS AND 

CALIBRATION CURVE(S) 

Page 45 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Workstation: ETSKIRK Results Name: klll227a.rdb 

k111227a.rdb (PFOS): "Quadratic" Regression ("1 / x" weighting): y = -842 x'^2 + 9.99e+005 x + 2.63e+004 (r = 0.9998) 

8.5e7 

8.0e7 

7.5e7 

7.0e7 

6.5e7 

6.0e7 

5.5e7 

5.0e7 

4.5e7 

iu 4.0e7 

< 

3.5e7 

3.0e7 

2.5e7 

2.0e7 

0.0 

15 20 25 30 35 40 45 50 

Concentration, ng/mL 

55 60 65 70 75 80 85 90 

Data worked up by KJU 

Printin g Time: 9:46:02 AM 

Page 1 of 1 

Printin g Date: Wednesday, January 04, 2012 

Page 46 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Workstation : ETSKIRK Result s Name: klll227a.rd b 

Data worked up by KJU 

Printin g Time: 9:46:32 AM 

Page 1 o f 1 

Printin g Date: Wednesday, January 04, 2012 

Page 47 of 110 
GLP10-01-02; Interim Report 24 

Analysts of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Workstation : ETSKIRK Result s Name: klll227a.rd b 

Data worked up by KJU 

Printin g Time: 9:45:16 AM 

Page 1 o f 1 

Printin g Date: Wednesday, January 04, 2012 

Page 48 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

Sample Name 1(11122To018" Sample ID: '11012-10-9- File' "k1 n227a.*tr 

Peak Nan>«. -PF8S' Mass(as): *299.00a«0.000 Oa,299.00a/99.000 DaComment. "2.5 ntj'mL FC std In Milli O Watof" Armotaliofi; ~ 

Sampl e Index : IB 

Data printe d by STW 

Thursday, January 26, 

Page 1 o f 27 

Page 49 of 110 
GLP10-01-02: Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

I

Sample Name,-1(1112270035' SamptelD -LCS-111221-10- File "kl l 

Peak Name: -PFBS- Massfes)- -299.D00/SD.000 Da,299.000/99.000 DaComment.-30ppb LCS" Annolanon -

:ample Index: 3b 

2 9.9 ng/mL 

2 6.3 ng/mL 

12/28/2011 

12-03:55 AM 

Peak-Split. Factoi 

Report Largest Pe; 

Min. Peak Height: 

Hln. Peak Hldth : 

Snoothing Width: 

fir Hindow: 

Expected RT: 

70 

1.00 I 

i Heli ! RT : 

Manual 

•: 12.8 

23S590S3 t 

I

SampleName •k111227aCM2- Sample ID -GLP10-01-02-24-099- Fie, 

Peak Name: 'PFBS" Mass(es): '299.000/80.000 Da,299.000/99.000 DaCommenL "DAL-GW-WOR-RB-" Annotation ~ 

Sample Index' 42 

Sample Type: Unknown 

Concentration: ll/A 

Calculated Cone: < 0 

Acq. Date: 12/2B/2011 

Acq. Time: 2:28-34 AM 

Modified : llo 

Proc. Algorithm- Specify Paramett 

Baae. Sub. Window: 1.00 ain 

Peak-Split. Factei: 3 

Report Largest Peak: Yes 

Hin . Peak Height: 0.OO cpt 

Min. Peak width : 0.00 set 

ng width . 

RT h 

Expected F 

30 C 

12.8 

itlv e BT; llo 

Int . Type: Base To Base 

Retention Time: 12.8 rain 

Area: 3654 counts 

(

Sample Name' -k111227a043- Sample ID: -GLP 10^)1 •02-24-100- RIe 

Poak Name' 'PFBS' M3ss(es)- '299.000/80.000 Da.299.000/99.000 Da' 

CommenL-DAL-GW-lSSL-RB-" Annotation " 

Sample Index; 43 

Sample Type 

Calculated Cone: 

K/A 

Proc. Algorithm: Specif y f 

Base. Sub. Hindou: l.OC 

Peak-Split. Factor: 3 

Report Largest Peak: Ye: 

tlin . Peak Height: O.f 

Min. Peak Width: O.C 

Smoothing width : 3 

RT Kindow; 30.0 

Expected KTi 12.3 

Use Relative RT: No 

Retenti 

Height: 6,51e-*002 CPS 

I

SampleName •kin227a046' SamplelD 'GLP 1CK>1-02-24-096" Flo: 

Peak Name: 'PFBS' Massfes) '299.000/80.000 Da.299.000/99.000 DaComment -DAL-QW-TR1P01-MS-- Annotation' -

Sample Index: i6 

Sample Type: Unknown 

,rs - HQ I 

Modified. llo 

Proc. Algorithm- Specify Parameti 

Noise Percentage: 70 

Base. Sub. Window: 1.00 min 

Peak-Split. Factor: 3 

Report Largest Peak: Yes 

Min. Peak Height: 0.00 cp: 

Hin. Peak width : 0.00 sec 

Smoothing Width- 3 point s 2 0e6' 

RT Window: 30.0 sec 

Expected RT: 12.8 Din 

Use Relativ e RT: Ho 

Int . Type: Valle y 

10.5 11.0 11,5 12,0 12,5 13.0 13.5 

Data printe d by STW 

Thursday, January 26, 2012 

Page 2 of 27 

Page 50 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll22'7 a . rdb 

I

Sample Name: •k111227a049' SamplelD 'GLP10-01-02-24.001- Flte''k111227a.wrfr 

Peak Name "PFBS" Mass{es) '299.000/80.000 Da,299.000/99.000 DaComment- "DAL-GW-130R-0-" Annolation. ~ 

Base. Sub. Window: 

Peak-Split. Factor: 

Report Largest Peak: 

Min. Peak Height; 

Hin. Peak width : 

ing Width: 

2.5e4 

2/4e4 

2.3e4 

2.2e4 

RT Window: 

1.Se4 

1.7e4 

1,6e4' 

1.5e4 

7000.0-

6CK».0' 

SOOO.O4000.0 

3000.0-

2000.0 

1000.0 

0.0-

12.5 13.0 13.! 

I

Sample Name: •k111227B056' Sample ID. 'GLP 1001-02-24-004' Fte' "I 

Peak Name. 'PFBS- Massfes), -299.000/80.000 Da,299.000/99.000 DaComment 'DAL-GW-130S-0-' Annotatron. " 

S.0e4 

4.Sa4' 

4.6e4 

4.4^' 

4.2e4-

4.0e4 

3.8e4' 

3.6e4 

3/4e4 

3.2e4 

3.0*4-

2.8e4-

Proc. Algorithm: Si 

Base. Sub. Window: 

Peak-Split. Factor: 

Report Largest Peal 

Kin . Peak Height: 

Kin . Peak Width: 

Smoothing width : 

RT Window: 

Expected RT: 

Base To Base 

2.4«4 

2.2e4> 

2.0a4 

1.0e4-

BOOO.0-

6000.0-

4000.0-

2000.0-

0.0-

(

Sample Name: 'k111227a0S9* Sample ID' *GLP1041-02-24-007' File ' 

Peak Name. -PFBS" Mass(es). -299.000/B0.000 Da,299.000/99.000 DaComment. "DAL-GW-130L-O-- Annotation, " 

Sample Index: 59 

Sampl e Type : Unknow n 

Calculated Cone: 1.SO ng/mL 

Acq, Date: 12/28/2011 2,3ft4-

Acq, Time: 8:19:51 AM 2.2*4-

Modified : ye s 2.1e4-

Proc. Algorithm- Specify Parameters - HQ 111 

I

SampteNam6;'k111227a062' SamptoID:•GLPHM)1-O2-24-010' Fie:'k111227a.wrfr 

Peak Name. 'PFBS' Mas5(es}, -299.000/80.000 Da,299,000^9.000 Da" 

Comment 'DAL-GW-ISIR-O-' Annotation." 

Sample Index: 62 

ling Midi 

.«d RT: 

152720 cc 

2.41e-f004 

12.6 

1.6»4< 

1.5»4-

1.4e4< 

1.3M1.2e4-

1.1*4-

1.0e4-

9000.0-

6000.0-

5000.0-

4000.0-

3000.0-

2000.0-

1000.0-

co-bftf^ 

10.5 

Data printe d by STW 

Thursday, January 26, 

Page 3 o f 27 

Page 51 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

I

SampleName "kl 11227b0G9" Sample ID: "GLP10-01-02-24-013' File 

Peak Name' "PFBS" Mass(es)' "299.000/60.000 Da,299.000/99.000 Da" 

CommenI "DAL-GW-13 IS* ' Annotation " 

Sample Index: 5 

Sample Type: Unknown 

Concentration: N/A 

Calculated Cone: 0.688 ng/mL 

Acq. Date 12/29/2011 

Acq. Time: 11:10:43 AM 1.6a4 

15e4 

. Algorithm: Specify Parametc 

Peak-: 

Manual 

13.3 

"75363 < 

1.3*4 

12e4-

1.1e4-

1.0e4-

9000.0-

8000.0-

7000.0-

6000.0 

13.0 13.5 14.0 14.5 

I

SampteNaine'"k111227t)072" SamplelD "GLPIMl-02-24-016' Fie' 

Peak Name' "PFBS" Mass(es), "299,000/80.000 Da,299,000/99.000 DaComment: •DAL-GW-131L-0-" Annotation -

Sample Index: S 

Sample Type: Unknown 

Calculated Cone: 2.84 ng/mL 

12/29/2011 

Acq. Tirai 12:12:' 

Modified: Yes 

Proc. Algorithm : Specify Pari 

Noise Percentage: 70 

Base. Sub. Window: 1.00 

Peak-Split. Factor: 3 

Report Largest Peak: Ves 

Hin. Peak Height- 0,00 

Hin. Peak Width: O.OO 

Smoothing Width: 3 

RT * 

Expected RT; 13.3 

Base To E 

:: 13.3 

279073 ci 

13,0 13.5 14.0 14.5 

I

Sample Name: -kl 112271)075' Sample ID. -GLP1CM)1-02-24-019' File: 'k111227b,wir 

Peak Name: TFES' Massfes): '299.000/80.000 Da,299.000/99.000 DaComment:-DAL-GW-133FW>-- Annotattoo:-

Peak-split . Factor: 

Report Largest Peak: 

Min. Peak Height: 

Min. Peak Hldth : 

Base To Base 

Height: 

Start Tl 

End Tim* 

I

SampleName •k111227t)0e2" Sample ID'•GLP1CWH-02-24-022" F<e •k111227b.wtr 

Peak Name "PFBS" Ma»s(e»): "299.000ffl0.000 Da599.000«9.000 DaComment "DAL-GW-133S-0-" Annotation." 

Sample Index; 16 

Sample Type: Unknown 

1.7e5 

1.6e5 

1.505 

1.4e5 

1.3e5 

1.2o5 

l.leS 

1.0a5 

9.0e4 

a.0e4 

7.0e4 

6.0e4 

5.0*4 

4.0e4 

3.0«4 

2.0e4 

1.0«4 

12.5 13.0 13.5 14,0 

Time, min 

Data printe d by STW 

Thursday, January 26, 2012 

Page 4 o f 27 

Page 52 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

Data printe d by STW 

Thursday, January 26, 2012 

Page 5 of 27 

Page 53 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS. and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

(

Sample Name, -k111227bl01" Sempte ID: -GLP10-01-02-24-037- FIte: 

Peak Name: -PFBS- Masses): -299.000ra0.000 Da,299.000/99.000 DaComment: •DAL-GW-135R-0-- Annotation " 

Sample Index: • 37 

Sample Type 

Calculated Cone 

K/h 

63.9 ng/r 

Base. Sub. Window: 

Peak-Split. Factor 

Report Largest Peal 

Kin. Peak Height: 

Min. Peak Width; 

Smoothing Width: 

RT Kindow: 

Sample Name' -V111227b108' Sample tO 'GLPI0-01-02-24-040" FN' 'kl 11227b.wir 

• Peak Name' "PFBS* Massfes): '299,000/BO.OOO Da,299.000i/99.000 Da' 

I Comment "DAL-GW-IKS-O-- Amwtation: " 

Sample Index: 44 

Sample Type: Unknown 

Concentration. ll/A 15eSCalculated Cone: 0.961 ng/mL 

Acq. Date: 12/30/2011 

Acq. Tine- 12:35:50 AM 

Hod I I 

Noi: 

Algorithm: t 

.age: 

. Sub. Mint 

Peak-Split. Factor' 

Peport Largest Peak. 

Hin. Peak Height: 

Hin. Peak width : 

Smoothing Width: 

BT Window: ; 

Expected RT; 

Use Relativ e RT: 

Base To Base 

:: 13.2 lain 

919975 counts 

1.52e+005 cps 

12.5 13.0 13.5 14.0 14.5 15.0 15.5 

I

Sample Name' -k111227b111' Sample ID: 'GLP 1041-02-2' 

Peak Name: -PFBS- Mass(es): -2S9.000/80.000 Da,299.00C 

Commeni "DAL-GW-135L-0-' Annotatkin,-

Moise Percentage: 

Base. Sub. window: 

Peak-Split. Factor; 

Peport Largest Peak; 

Min. Peak Height: 

Min. Peak Width: 

Smoothing width: 

RT Window: 30 

Expected RT; 1. 

Use Relative RT: Ki 

•: •k11l227b.wtfr (Sample Name' "kt11227b114- Sample ID' 'G LP tIM)1-02-24-049* Fie:' 

Peak Name -pFBS" Maas(es]' '299.000/80.000 Da,299.000/99.000 DaComment "DAL-GW-136S-(V" /\nr>otal)Oo: " 

Sample Indejc 50 

Type; Base To Base 

l.05e5-

1.00e5-

9.50e4-

9.00e4-

S.50e4-

8.00e4-

7,SOe4-

7.00e4-

S.50e4-

6.00«4' 

4,50e4 

4.00e4' 

3.50e4-

3.00*4 

2.50e4' 

2,00e4' 

1,50*4-

1.0OM5000.00-

0.00-

Sample Type: 

ll/A 

Base. Sub 

Peak-Split. Factor: 3 

Report Largest Peak; ' 

Hin. Peak Height; I 

Min. Peak Width; I 

Smoothing width ; 

RT Window: 30.0 

Expected RT; 

Specify Parameters - MQ 111 

70 

<: 1.00 min 

! Relal 

Int. Type: 

Retention 1 

Height: 

! RT: llo 

3.0e4 

2.Se4 

2.6e4 

1.8e4 

1.6o4 

1.0e4 

6000.0 

6000.0 

4000.0 

2000.0 

0.0-

12.5 13.0 13.5 14.0 14.5 15.0 15.5 

Tima. min 

Data printe d by STW 

Thursday, January 26, 2012 

Page 6 of 27 

Page 54 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Results Name: klll227a.rd b 

Data printe d by STW 

Thursday, January 26, 2012 

Page 7 o f 27 

Page 55 of 110 
GLPIO-01-02: Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

• SampteNam6:"k111227b13T- Sample ID'•GLP1CW)l-02-24-06r FBe. "kl11227b.wrfr 

• Peak Name:-PFBS" Ma£s(ei):*2e9,000/80.000Da,299.000J99.000Da' 

I Commeni:-DAL-GW>13eS-0-' AnnoOUon:** 

Sanple Index: 73 

Proc. Algorithm: Spec 

Noise Percentage: 

Base. Sub. window; 

Peak-Split. FactorReport Largest Peak; 

Kin . Peak Height: 

Min. Peak width ; 

0.00 cps 

RT Window: 

(idth : 

.0 14.5 15.0 15.5 

(

Sample Name: -kil l 227bl40" Sample ID, •< 

Peak Name. -PFBS' Mass(es). "299.000/80.0( 

Comment "DAL-GW-1381-0-" Anrwtatkin,"" 

Sample Index: 76 

Sanple Type; Unknown 

Concentration: ll/A 

Calculated Cone: 0.0121 ng/mL 

Peak-Split. Factor; 

Hin . Peak Height: 

It Typeftentio n T] 

sight: 

Base To Base 

21591 counts 

1.25e4 

1.20e4 

1.15e4 

1.10e4 

1.05«4 

1.00e4 

9500.00 

9000.00 

&S00.00 

8000.00 

7500.00 

§• 7000.00 

^6500.00 

I 6000.00 

~ 5500.00 

5000.00 

4500.00 

4000.00 

3500.00 

3000.00 

2500,00 

2000.00 

1500.00 

1000.00 

500.00 

0.00 

I

SampteName •kl11227b14r Sample ID:•GLPlOfll-02-24-073* File: 

Peak Name' "PFBS" Mas»(es). "299.000/80.000 Da.299.000«9.000 Da" 

Commenf "DAL-GW-140R-0-" Annotation. ~ 

Sample Index; 83 

Sample Type: Unknown 

Concentration: N/A 

Calculate d Cone: 1.23 ng/RiL 

Acq. Date: 12/30/2011 2.0*4 

Acq. Tine: 2:01;41 PK 

15e4 

Modified : Yes 

I I 1.ee4 

1.704 

•k111227b.viiitr 

Proc. Algoci 

Noise Percer 

hn: Specify Parameteti 

Min. Peak Height; 

Min. Peak Width: 

Smoothing Width; 

5000.0 

4000.0 

3000.0 

2000.0 

1000.0 

0.0 

(

Sample Name: "kl n227b150- Sampte ID: "i 

Peak Name, "PFBS" Ma5S(es), -299.000/80.01 

Comment T)AL-GW-141R-0-- Annotation." 

Sample Index: 36 

0.0351 r 

12/3D/2011 

3:03:4 1 PM 

s"K111227b.wrtr 

. Peak Width. 

.thing 

RT Hindoi 

11,65 

7.65e+003 

1.3»4 

1.3*4-

1.2e4 

1.2»4' 

1.1e4-

1.1e4' 

1.0e4' 

9500.0-

9000.0-

8500.0-

8000 0-

7500.0-

. 7000.0-

6500.0 

6000.0-

5500 0-

5000.0 

4500.0-

4000.0 

3500.0-

3000.0 

2500.0-

2000.0-

L 13.88 

11.5 12,0 12.5 13.0 13.5 14.0 14.5 15.0 

Data printe d by STW 

Thursday, January 26, 2012 

Page 8 of 27 

Page 56 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

I

Sample Name: "k111227bl53- Samplo ID' "GLP10-01-02-24-079" Fite' •kll1227b.wrfr 

Peak Name: "PFBS* Mass{es)' -299,000/80,000 Da,299.000/99.000 DaComment: "DAL-GW-142R-0.* Annotation: "* 

Sample Index: 89 

0.709 r 

12/30/2011 

6; 30;23 PM 

. Peak Height; 

I

Sample Name. •kin227b160- SamplelD "G LP 1 CM)1-02-24-082- Flo: "kil l 227b.wrfr 

Peak Name. "PFBS" Mass{es): "299.000/80,000 Da,299.00IV99.000 Da' 

Comment "DAL-GW-143R-0-- Ajwiotatwn* 

(

Sample Name' "kl l 1227b163- Samplo ID: 'GLP IW)1-02-24-085" File. 

Peak Name: "PFBS" M3*s(es). "299.000/80.000 Da.299.000/99.000 DaComment "DAL-GW-mR-O-- Annotation:"* 

Sample Index: 99 

Sample Type; Unknown 

Concentration; N/A 

Calculated Cone: 2.05 ng/nL 

Acq. Date; 12/30/2011 

Acq. Tine: 7:32:23 PH 

Peak-Split. Factor; 

Peport Largest Peal 

Hin. Peak Height: 

SDOOthlng Hid 

Expected RT; 

Height: 

Star t 1 

End Tin 

(

Sample Name; •k111227a018" Sample ID "11012-10-9" FBe' •k111227a.iiwr 

Peak Name: "PFHS" Maasfes)' '399.000/99.000 Da,399.000/80.000 Da' 

Comment "2.5 ng/mL FC «td in Mili Q Water" Annotation." 

Sample Index: 18 

Sample Type; Standard 

Concentration: 2.50 ng/mL 

Calculated Cone: 2.73 ng/mL 

Acq. Date: 12/27/2011 

Acq. Time: 6:12;<3 PM 

Modified: llo 

Proc. Algorithm: Specify Parameters - MQ II I 

Noise Percentage: 50 

Base. Sub. Window: 1.00 min 

Peak-Split. Factor; 2 

Report Largest Peak; Ves 

Min. Peak Height; 0.00 cps 

Min. Peak Mldth; O.OO sec 

1 RT: 

3.94e-t005 cps 

Data printe d by STW 

Thursday, January 26, 2012 

Page 

Page 57 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

• Sample N8me"k111227a028- Sample ID. "Solvent Blank' Fie. "kl l 1227a wtfT 

I Peak Name, "PFHS" Mas«(es}. "399.000/99.000 Da,399.000/80.000 Da" 

I Comment "MBiQWaterTNll-0437' Annotation -

Sample Index: 2B 

Sample Type; Unknown 

Concentration : H/A 

Calculate d Cone : < 0 

Acq Date: 12/27/2011 

Acq, Tiroe: 9-39:19 PH 8500-

9000 

Min. Peak Height: 

Min Peak Nidth. 

Smoothing Midth: 

0.0 0 se c 

3 point ! 

Area: 269 count: 

Height; 2.71e*002 cp: 

8000 

7500 

7000 

esoo 

6000 

5500 

a 5000 

I" 4500 

- 4000 

3S00 

3000 

2500 

2000 

1500 

1000 

500 

I

SampteName-1(1112278028- SamplelDT.CS-111221-4- Fie: 

Peak Name: 'PFHS' Uass(es) -399.000/99.000 Da,399.000/80.000 Da' 

Comment -O.Sppb LCS- Annotation' " 

Sample Index. 29 

Sample Type; QC 

Concentration; 0.497 ng/mL 

Calculated Cone: 0.506 ng/mL 

Acq. Date; 12/27/2011 

Acq. Time: 9:59:58 PM 

Peak-Split. Factor: 2 

Report Largest Peak; Yei 

Min. Peak Height: O.C 

Min. Peak Width; O.C 

Smoothing Width: 3 

RT Window: 30.0 

Expected RT; li.A 

Use Relative RT: Mo 

mt. Type: Valley 

Retention Time; 11.4 

Area; 42Se56 c< 

Height: 7.54e'O04 

Start Time; H. 2 

End Time; H. 6 

12.0 12.5 13.0 13.5 14.0 14.5 15.0 15.5 16.0 16.5 

I

Sampto Name: -kl 11227a03r Sampte ID: TCS-111221-r Rte: -kl 11 

Peak Name: "PFHS" Mass(as): -asg.OOO^g.OOO Da.399.OOQreO.000 DaComment: -5ppb LCS" Annotation, "* 

Calculated Cone: 

Acq. Time: 

5.03 ng/mL 

1/27/2011 

:01:57 PM 

Modified: No 

Proc. Algorithm; Specify Par; 

Noise Percentage: 50 

Int. Type; Valley 

Retention Time; H. 4 

168553 

7. n e + 005 cps 

I

Sampte Name: 1(111227a035" Sample ID' -LCS-l 11221-10- Fie: "kl 1 

P»ak Name: -PFHS" Mass(es) '399.000/99.000 Da .399.000^0.000 DaComment "30pp6 LCS" Annotation: ~ 

Sample Index: 35 

Proc. Algorithm: Specify Paramet' 

Noise Percentage; 50 

Base. Sub. Window: 1.00 min 

Peak-Split. Factor; 2 

Report Largest Peak: Vsa 

Min. Peak Height: 0.00 

Min. Peak Width; 0.00 

Smoothing Width: 3 

RT Window; 30.0 

Expected RT: H.A i 

15.0 15.5 

Data printe d by STW 

Thursday, January 26, 2012 

Page 10 of 27 

Page 58 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

I

SampteName "kl11227B042" Sampte ID, "GLP10^1-02-24-099" File •k111227a.wir 

Peak Name. "PFHS" Mass{es), "399.000/99.000 Da,38S.000/80.000 DaComment: "DAL-GW-140R-RB-" AnnotaOon, -

Acq. Time: 

Modified ; 

Proc. Algorithm: 

Noise Percentage 

Base. Sub. Hindci 

Peak-Split. Facti 

Report Larg< 

50 

r: 1.00 

Pes) 

: Height; 

Min. Peak width ; 

Smoothing Width: 

RT Window: 

Bas e T o Bas e 

9000-

8500-

8000-

7500-

7000-

6500-

GOOO5500-

5000-

2500 

2000 

14m,J ^^15.08 15 66 ^^^ ^ ^^^ ^ 

12.0 12.5 13.0 13.5 15.0 15.5 16.0 16.5 

I

Sample Name' •kl11227a043" Sampte ID' "(SLPl0-01-02-24-100" Fia: •klll227a.wir 

Peak Name' 'PFHS- Mass(es}' -399.000/99.000 Da,399.000/80.000 Da" 

Comment -DAL-GW-133L-RB-* Annotation' ~ 

7500-

7000-

Smoothing Wit 

RT Window: 

Expected BT: 

6000-

5500-

SOOO4500-

4000-

3500-

3000-

2500-

2000-

15.5 ia.0 

I

Sampte Name:'k111227a046- Sample ID:-GLP10-01-02-24-096- File 

Peak Name. "PFHS' Mas£(es} -399.000/99.000 Da.39g.000/80.000 DaComment, "DAL-GW-TRIPOl-MS-' Annotation' ~ 

Sample Index' 46 

Sampl e Type : Unknow n 

18.5 

Proc Algori Specify 

50 

indow: l.C 

Peak-Split. Factor; 

Report Largest Peak 

Hin . Peak Height: 

Min. Peak width : 

Sxpoctod RT: 

Use Relative 

Retention Tin 

IT: No 

Valley 

!. H. 4 

14759450 ( 

2.516*006 

14.2 

I

Sampte Name: *kl11227a049" Sampte ID: 'GLP 1041-02-24-001' Fie: 

Peak Name, "PFHS- Mass(es) '399.000/99.000 Da,399,000/80.000 Da' 

Comment •DAL-GW-130R-*-* Annotation: ~ 

Sample Index; 49 

sampl e Typ e 

ng/r 

Modified : 

Proc. Algorithn : S] 

Noise Percentage; 

Base. Sub. window; 

Peak-Split. Factor 

Hin . Peak Height: 

Min. Peak Hldth ; 

Smoothing Hldth : 

15,5 18.0 

Data printe d by STW 

Thursday, January 26, 2012 

Page 11 o f 27 

Page 59 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

Sampte Name, "kl l 12Z7a056" Sampte ID "GLP 1041-02-24-004" File, -k111227a.»«r 

I

Peak Name. TFH5" Massfes): -399.000/99.000 Da ,399.000/80.000 Da' 

Comment,-DAL-GW-130S.O-- Annotetion -

Sample Index: 56 

Sample Type 

N/A 

25. 8 

';17:52 / 

Modified; Yes 

Proc. Algorithm: Specify Pars 

Noise Percentage; 50 

Base. Sub. Window; 1.00 

Peak-Split. Factor; 3 

Report Largest Peak; Yas 

Min. Peak Height: 0.00 

Min. Peak Hldth; 0.00 

Smoothing width; 3 

RT Window 30.0 at 

Int . Type: 

Retention 1 

Height: 

Manual 

i e; 14. l 

2154463 c< 

14.0 14.5 

rSampteName •kl11227a059" Sampte ID. "GLP10-01-02-24-007" Fie,-kl11227a.wtfr 

• Pen 

8:19:51 AM 

•ithm: Specify Pai 

Peak-Split. Factor: 

Peport Largest Peak: 

Hin. Peak Height: 

Min Peak Width; 

Smoothing width : 

RT Window: IC 

ielat J i BT: 

I

Sampte Name: "kl 11227a062" Sampte ID: "(JLP10-01-02-24-010" FitoPeak Name: TFHS* Massfes): -399.000/99.000 Da,399.000/80.000 DaComment "D/U.-<JW-131R-<K" Annotation'-

, Window; 

L. Factoi 

Largest Peak: 

Min. Peak Height; 

Min. Peak Width. 

Smoothing Width: 

RT Kindow: 

• Relat I 

1 RT; 

! RT: 

I

Sampte Name: •k11!227b069" Sampte ID: "GLPICKI1-02-24-013" Fie: -k111227b.wtr 

Peak Name -pFHS" Mass(es) "399.000/99.000 Da,399.000/e0.000 Da' 

Comment "DAL-GW-131S-0-" Annotation " 

Sample Index: 5 

Sample Type: Unknown 

Concentration. tl/A 

Calculated Cone; 4.86 ng/mL 

Acq. Date; 12/29/2011 

: Largest Peak 

Data printe d by STW 

Thursday, January 26, 2012 

Page 12 o f 27 

Page 60 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

m SampteName''k111227b072- Sampte ID.-GLP lOJ]1-02-24-016" 

• Peak Name- "PFHS" Mass(es). "399.000/99.000 Da,399.000/80.000 Da' 

m Comment'"DAL-GW-ISIL-O-" Annotation.-

•k111227b.wtr 

• Type: 

N/A 

. Algorithm: Specify Para 

! Percentage' 50 

. Sub Window: 1.00 

-Split . Factor; 2 

- t Largest Peak: Yes 

Peak Height- 0 00 

Peak Hldth; 0 00 

2.4e5 

2.3e5 

2.2 65 

2.1 e5-

2.0e5 

1.9e5' 

1.8e5' 

1.7e5 

1.&e5-

1.5e5 

1.4e5' 

1.3e5-

1Je5 

1.1e5' 

1.0e5' 

9.0e4' 

8.0M' 

7.0e4-

6.0*4-

5.0»4-

4.0e4-

3.0*4-

2.0e4' 

1.0*4-

14.0 14.5 15.0 15.5 16.0 16.5 

I

Sampte Name. •k111227b075- Sampte ID:-GLP10-01-02-24-019" Fie" "k111227b.wi(r 

Peak Name. 'PFHS" Mass(es) "399.000/99.000 Da,399.000/80.000 Da" 

Comment "DAL-GW-133R-0-- Annotatxm -

irithn : Specify Pai 

window; 1.00 

Smoothing width ; 

RT Window: 

Expected RT: 

Use Relative RT. 

Height: 

Start Time 

End Tine : 

I

Sampte Name: *k111227b082" Sanvfie ID' 

Peak Name. -PFHS' Mass(es). 

Comment."DAL-GW-ISSS-O-' Annotation' 

Sample Index: 18 

sampl e Type - Unknow n 

Calculated Cone: 80.2 ng/mL 

Sampte Name: "kl 112271)085' Sampte ID: 'GLP 10J31-02-24-025' Fie 

Peak Name. 'PFHS" Ma»5(Bs): '399.000/99.000 Da.399.000/80.000 Da' 

CommenL •DAL-GW-133L-0-* Annotatian." 

Sample Index: 21 

Sarjpl e Type ' Unknow n 

Data printe d by STW 

Thursday, January 26, 

Page 13 o f 27 

Page 61 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

I SampteName -k111227b08e- Sampte ID'•GLP10-01-02-24-028' File. •k111227b.wtr 

Peak Nam*. "PFHS' Mass{ss)' '399.000/99.000 Da,399.000/80.000 Da' 

I Comment TJAL-GW-134R-*-- Annotatioo ~ 

Calculated Cone: 559. 

Acq. Date: 12/29/21 

Acg Tine ; 5;43;01 

Min. Peak Height: 

Min. Peak Width: 

Sooothmg width : 

. Type: Manual 

intto n Time; 14.7 

i : 4623092 ci 

13.5 14,0 14,5 15.0 15,5 16.0 16.5 

I

Sampte Name, "kl n227b095" Sampte ID 

Peak Name,-PFHS- Mas«(as) '399.000/99, 

Comment •DAL-GW-134&.0-" Annotation: -

Sample Index: 31 

Sample Type; Unknown 

Calculated Cone: 4.18 

Acq. Date: 12/29/2011 

Acg. Tine; 8:07-29 PM 

lOthing Width: 

5.0O5 

4.8e5 

4.6e5 

4.4«5 

4.285 

4.0e5 

3.8e5 

3.6e5 

3.4«5 

3.2e5 

3.0e5 

2.ae5 

2.8e5 

2.4eS 

2.2e5 

2.0o5 

1.8e5 

1.6e5 

8.0e4 

6.0e4 

4.0e4 

2.0*4 

[

Sampte Name: 'kl 11227b098- Sampte ID; 

Peak Name: 'PFHS' Mass(es): •399.f"" ' 

Comment: "DAL-GW-mL-O-- Annotation, 

Sampte Nam*: "kl 11227b101" Sample ID' "GLPI &<I1-02-24-03r Fie 

Peak Name. "PFHS- Masa(es)- '399.000/99.000 Da.399.000/30.000 DaComment "DAL-GW-ISSR-^J." Annotation: ~ 

Sample Index: 37 

Sample Type: Unknown 

Data printe d by STW 

Thursday, January 26, 2012 

Page 14 o f 27 

Page 62 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

*ETS-Kirk Result s Name: klll227a.rd b 

r

Sampte Name, "kl 11227b 108' Sampte ID. 'GLP10-01-02-24-040- Fite* "k111227b 

Peak Name' TFHS" Massfes): "399.000»9.000 Da.399.000/80.000 DaComment "DAL-GW-ISSS-O-- Annotation:" 

Sample Index: 44 

Saople Type; Unknown 

Concentration; N/A 

Calculate d Cone: 7.78 ng/mL 

Acq. Date- 12/30/2011 

Acq. Time- 12:35:50 AM 

.-Split . Factor: 

>rt Largest Peak: 

Peak Height; 

Peak Width: 

Height: 

Star t Ti l 

End Time 

9.0*5 

e.5e5 

e.0e5 

7.5*5 

7.0e5 

6.5e5 

6.0e5 

5.5*5 

S.0e5 

1 4.5*5 

4.0eS 

3.5*5 

3.0*5 

2.5*5 

2.O0S 

1.5*5 

1.0*5 

5.0*4 

3.5 14.0 14,5 15.0 15.5 16.0 16.5 

I

Sampte Name''k111227bl11- Sampte ID.-GLPIOfll-02-24-043' Fie-"kll 1227b. 

Peak Nam*' "PFHS* Mass(*s), "399.000/99.000 Da,399.000/80.000 DaComment "DAL-GW-135L-(^" Annotation. -

Sample Index; 47 

Sample Type: Unknown 

Concentration: ll/A 

Calculated Cone; 47.2 ng/mL 

Acq. Date: 12/30/2011 

Acq. Tine : 1:37;48 AH 

: Largest Peak: 

Smoothing Width: 

RT Window: 

Expected RT; 

Use Relative BT; 

le: 14.e nl n 

3911940 counts 

5.6Se + O05 cps 

I

Sampte Name' *k111227b114' Sampte ID' "GLP10-01-02-24-049' Fito. -kl 11227b,wir 

Peak Name, "PFHS" Ma3S(es): '399.000/99.000 Da,399.000/80.000 DaComment, •DAL-GW-136S-0.- Annotation:-

Sample Index: 50 

sample T-ype - Unknown 

Concentration: N/A 

Calculate d Cone: 11.E ng/nL 

Acq. Date: 12/30/2011 

Acq. Time: 2:39:44 AM 

Modified : Yes 

Proc. Algorithm: Specify Pa. 

Noise Percentage; 50 

Base. Sub. Nindew: 1.00 

Peak-Split. Factor; 2 

Report Largest Peak; Yes 

Hin. Peak Height. 0.00 

Min. Peak Width; 0.00 

Smoothing Width; 3 

RT Window: 30 0 

Expected RT- 14.' 

I

SampleNarrw -k111227b12r Sampte ID''GLP10-01-02-24-052" Fie: 

Peak Name: 'PFHS' Ma5s(e4), "399.000/99.000 Da,399.000/B0.000 DaComment:-DAL-GW-136L-0-* Annotation " 

Sample Index: 57 

Sample Type; Unknown 

Concentration: N/A 

Calculated Cone: 12.3 ng/mL 

Acq. Date: 12/30/2011 

. Tim« 14 ;17 I 

Modified : Yes 

Proc Algorithm; Specify Parameti 

Noise Percentage: 50 

Base. Sub. Window: 1.00 min 

Peak-Split. Factor: 2 

Report Largest Peak; Yes 

i t . Type: Manual 

ea: 1031697 ci 

Data printe d by STW 

Thursday, January 26, 2012 

Page 15 o f 27 

Page 63 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

I

Sani[teName.-k111227b124- Samffa ID:-GLP1CMH.02-24-058- File -k111227b.wir 

Peak Nam*. -PFHS" Mass(BS): '399.000/99.000 Da,399.00fl/80.000 Da" 

Comni«nt.-OAL.CW.137S^- AanotaUofi, -

Sample Index. 60 

Sample Type; Unknown 

Calculated Cone. 0.125 ng/mL 

Acq Date; 12/30/2011 

Acq. Time: 6:0S;15 AH 

1.5*4 

1.4*4 

Modified ; tlo 

Proc. Algorithra: Specify Parameters 

Noise Percentage- 50 

- MO II I 1.3*4 

Base. Sub. window: 1.00 min 

Peak-Split. Factor; 2 

Report Largest Peek: Yes 

Hin. Peak Height: 0.00 cps 

Hin. Peak width : 0.00 see 

Sooothing Width: 3 poin 

RT Window; 30.0 sec 

Expected RT; 14.4 min 

Use Relative RT; Ho 

Int . Type; Valley 

Retention Time: 14.6 min 

Area; 109B97 counts 

1.2*4 

1.1*4 

1.0*4 

9000.0 

& 

" 8000.0 

£• 

Height; 1.52e»004 cps 

1.2*4 

1.1*4 

1.0*4 

9000.0 

& 

" 8000.0 

£1• 7000.0 

6000.0 

50O0.0 

4000.0 

3000.0 

2000.0 

1000.0 J Ll5^5 

13.5 14.0 14.5 15.0 15.5 16.0 16.5 

I

Sampte Name, 'kl11227b127- Sampte ID' -GLP 10-01-02-2< 

Peak Name- -PFHS- MaSE(Bs): -399.000/99.000 Da,399.0r' 

Comment -DAL-GW-137L-0--

Sample Index: 63 

Sample Type: Unknown 

Calculated Cone: 0.10^ 

Acq. Date: 12/30/2011 

Acq. Time; 7:08 ;14 AH 

Proc. Algorithm: Specify 

Koise Percentage: 50 

Baae. Sub. Uindow; I.Oi 

Peak-Spilt. Factor; 2 

Report Largest Peak: Ye: 

Hin . Peak Height: O.i 

Kin . Peak width : O.i 

Smoothing Width: 3 

RT Window: 30.0 

Use Relative RT; llo 

Type; l a l 

9000.0 

8500.0 

8000.0 

g 7500.0-

^ 7000.0 

I 6500.0 

- 6000.0 

5500.0 

5000.0-

4500.0-

4000.0 

3500.0-

3000.0-

2500.0-

2000.0-

1500.0-

1000.0-

500.0-

coistW. 

1.05 

Li 5.09 

12.0 13.5 14.0 14.5 15.0 15.5 18.0 16.5 

I

Sampte Natne: 'kl 11227bl34- Sampte ID: 'GLP1041-02-24-064' Rte 

Peak Nam*' -pFHS' Man(es): -399.000/99.000 Da,399.000/80.000 Da' 

Comment: "DAL-GW-138R-(V' Annotation' ~ 

Sample Index: 70 

Sample Type; Unknown 

Calculated Cone 

Acq. Time; 

Modified : 

Smoothing I 

RT Window: 

12/30/2011 

9;32.5'i AH 

Yes 

Specify Pari 

SampteName'-kl11227b13r Sampte ID''GLP1OO1-02-Z 

Peak Name 'PFHS' Mass[es)' -399.000/99.000 Da.39g.0C 

Commeni:'DAL-GW-138S-(^-' /\nnoiatton:" 

Sample T>-pe: 

Calculated Cone: 

Modifie d Ves 

Proc. Algorithm: Specify Para 

Noise Percentage; 50 

Base. Sub. window; 1.00 

Peak-Split. Factor: 2 

Report Largest Peak; Ves 

Hin . Peak Height: 0.00 

Hin . Peak Width: O.OO 

Smoothing width ; 3 

RT Window: 30.0 se 

Expected RT; li. 4 mi 

Use Relative RT; tlo 

InL Type; Manual 

2.205 

2.1e5' 

2.0e5' 

1.7e5-

1.6*5-

Height; 

Start Ti l 

End Time 

9.0*4 

e,0e4 

7.0e4 

6.0e4 

5.0*4 

4,0*4 

3.0*4 

2.0*4 

1.0*4 

13.5 14.0 14.5 15.0 15.5 16.0 16.5 

Data printe d by STW 

Thursday, January 26, 2012 

Page 16 o f 27 

Page 64 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

Peak-Split. I 

Report Large! 

Min. Peak Hei 

Min. Peak width ; 

RT Windo* 

1 RT: 

I

Sampte Name. 'kl11227b140' Sempte ID, 'GLPI001-02-24-070- Fite: 'k l 11227b.wtfr 

Peak Name. 'PFHS' Massfes): '399.000/99.000 Da,399.000«0.000 DaComment.-DAL-GW-mL-O-- AnnotalKW -

Sample Index: 76 

Sample Typo; Unknown 

Concentration; H/A 

Calculated Cone: 0.0630 ng/mL 

Acq. Date; 12/30/2011 8000 

Acq. Time: 11:36:57 AM 

Hoaiii.d , 

Proc. Algorithm: Specify Parameters - MO II I 

Noise Percentage: 50 7000. 

"0 min 

s 6500 

00 see 6000, 

point s 

i..in 5500-

5000 

ounts & 4500-

m^n 1 <000-

3500 

3000-

2500-

2000-

1500-

1000-

! Relai 

il ,15.27 15.76 

I

SampteName -kl 11227bl47- Sampte ID'•GLP10-01-02-24-073' Fie.-k111227b.wifr 

Peak Name 'PFHS' Mass(es] "399.000/99.000 Da,399.000/80.000 Da' 

Co(nm*nt "DAL-GW-mR-O-' Annotation' " 

Sample Index; 83 

Sample Type: Unknown 

Concentration; ll/A 

Calculated Cone; 13.9 ng/mL 

rithra; Specify Pai 

Base. Sub. Window 

Peak-Split. Facto: 

Report Largest Pei 

Min. Peak Height: 

Min. Peak Hidth . 

Smoothing Width: 

I

Sampte Name: •kl11227b150' Samfie ID: 'GLP 1001-02-24-076- Rte' "k111227b.wifr 

Peak Name: 'PFHS' Mass(es): '399.000/99.000 Da,399,000/80.000 DaComment:-DAL-GW-WIR-O-' Annotation,-

Sample Index: 86 

Sample Type- Unknown 

Concent 1atlon; N/A 

Calculated Cone: 0.259 ng/mL 

Acq. Date; 12/30/2011 

Acq. Tine; 3:03;41 PH 

Modified : Yes 

Proc. Algorithm: Specify Paramett 

Hoise Percentage; 50 

Base. Sub. Window; 1.00 min 

Peak-Split. Factor; 2 

Report Largest Peak; Yes 

Min. Peak Mldth; 0.00 set 

Height: 

Start 1 

End Tin 

3.4*4 

3.2*4 

3.0*4 

2.8e4 

2.6*4 

2.4*4 

2.2*4 

2.0*4 

1.6*4 

1.6*4 

1.4*4-

I5e4 

1.0e4 

8000.0-

6000.0-

4000.0-

2000.0-

0.0 

I

Sampto Name: 'k1l1227bl53' Sampte ID' -GLP 1001-02-: 

Peak Name, 'PFHS' Ma&s(«s) '399 000/99 000 Da.399.0C 

Comment •D/U.-GW-142R-0-* /SjinotaBon -

Sample Index; 89 

Sample Type; Unknown 

Calculi 10.2 ng/mL 

Proc. Algori 

Peal 

NOl! 

Min. Peak Height 

Min. Peak Width; 

Smoothing Hidth : 

RT Hindow; 

in: Specify Par; 

:age: 50 

i Relat 

End Tine : 

! RT: 

14.99 

_ ft 

Data printe d by STW 

Thursday, January 26, 2012 

Page 17 o f 27 

Page 65 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

• SampteNam9:-k111227t)160' Sampte lD"GLP10-01-02-24-082" File*•k111227b.viffl-

• Peak Name: 'PFHS- Mass(as}' -399.000/99.000 Da,399.000/80.000 Da' 

• Comment: •OAL-GW-143R-*-* Annotation'-

Sample Index; 96 

Sanple Type: Unknown 

Concentration: ll/A 

i f y Pai 

50 

1.00 

Use Relativf 

Int. Type; 

2.91e*004 

4000.0 

20O0.O12.0 12.5 13.5 14.0 

I

SampteName:-k111227b163- Sampte ID *G LP10-01-02-24-085' Fie: 

Peak Name, 'PFHS' Mass{es): '399.000/99.000 Da.399.000/B0.000 Da' 

Commenc '0AL-GW-144R-0-- Annotation: ~ 

Sanple Index: 99 

Sampl e Typ e 

Il/A 

ng/mL 

Modi fled: 

Proc. AlgorithmNoise Percentage: 

Base. Sub. Windov 

Peak-Spilt. Facte 

Report Largest P( 

Min. Peak HeightMin. Peak Width: 

Smoothing width: 

RT Window: 

Expected RT: 

I

Sampte Nam*: *kl 11227a018* Sampte ID: '11012-10-9* Fite: "kl 11227a wifT 

Peak Name: 'PFOS- Mass(*s). -499.000/90.000 Da.499.000/99.000 Da.499.000/130.000 Da' 

Comment. "2.5 ng/mL FC std in MilS O Water' Annotation, " 

Sample Index: IS 

Hoi! Per< itage : 

lindow 

Specify Parameti 

Base. Sub 

Poak-Spli' 

Report Largest Pe. 

Hin. Peak Height: 

Mill. Peak width : 

Smoothing Hldth : 

RT Window1 RT; 

; RT: 

I

Sampto Name' It l 11227a028' SiBiipte ID: 'Solvent Blank' Fl*: 'kl 11227a.wltr 

P*ak Hamt TFOS' Mass<es) "499.000/80.000 Da.499.000/99.000 Da.499.000/130.000 Da' 

CommonL "MKi Q Water TNI l-043r Annolatten " 

Concentration; 

Calculated Cone; 

. Window: 

•. Factor: 

Smoothing Mlc 

RT Window: 

Use Relative 

Data printe d by STW 

Thursday, January 26, 2012 

Page 18 of 27 

Page 66 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

• SampteName. "kl l 1227a029" SamptelD.TCS-111221-4" Fite •kl11227a.wrtr 

I Peak Name. "PFOS" Mass(*s) -499.000/80.000 Da,499.OO0/99.OO0 Da.499.000/130.000 Da" 

• Comment' *0.5ppb LCS" Annotation, -

Sample Index: 29 

Saople Type; QC 

Concentration; 0.462 ng/mL 

Calculated Cone: 0.395 ng/mL 

Acq. Date; 12/27/2011 

Acq. TI P 9:59:58 PM 

Yes 

Proc. Algorithm: Specify Par; 

Koise Percentage; 50 

Base. Sub. Window; 1.00 

Peak-Split. Factor: i 

Report Largest Peak' Yes 

Kin. Peak Height; 0.00 

Min. Peak width; 0.00 

Smoothing Width; 3 

RT Hindow: 30.0 si 

Expected RT: IS.4 mi 

Use Relative RT; Ko 

Int Type 

Tine: 15.3 

420664 c< 

14.5 15.0 15.5 16.0 16.5 17 0 17.5 

I

Sampte Name'•k111227a032- Sampte ID'TCS-111221-7" Fle."k111227a.wifr 

Peak Name' 'PFOS* Mass(es)' "499.000/80.000 Da ,499.000/99.000 Da.499.000/130.000 Da" 

Comment "Sppb LCS" Annotation: -

Sample Index; 32 

Samplo Type; OC 

Concentration: 4.62 ng/nL 

Calculated Cone; 5.IB ng/mL 

Acq. Date: 12/27/2011 

Acq. Tine: 11-01:57 PM 

Base. Sub. Window: 

Peak-Split. Factoi 

Report Largest Pe; 

Hin. Peak Height' 

lln . Peak Width; 

RT Windt 

le: 15.3 

5173517 et 

4.5 15.0 15.5 16.0 16.5 17.0 17.5 

I Sampte Name''k111227a035" SamptelD'-LCS-l11221-lO- File: "Ml 1227a. 

Peak Name. -PFOS- Mass{es) -499.000/SO.OOO Da.499.000/99.000 Da,499.000/130.000 Da' 

I Commeni, *30ppb LCS' Annotation: -

2 3.2 ng/mL 

12/28/2011 

12;03;55 AH 

Algol 

Hoi ! Perci 

Base. Sub. window: 

Peak-Split. Factor: 

Report Largest Peak; 

Hin. Peak Height: 

Min. Peak width; 

Smoothing Width; 

BT Hindow; 

Expec 

Use Relat 

Int. Type; 

i RT. 

! RT; 

3.27e+006 

I Sampte Name.-kill 227a042- Sampte ID-GLP1CM)1-02-Z4-099" Fie:* 

Peak Name -PFOS* Mass(es) '499.000/80.000 Da,499.000/39.000 Da,4: 

I Comment •DAL-GW-140R-RB-" Annotation -

Sample Type: 

Smoothing Hidth: 

RT Window: 

Expected RT; 

Use Relative BT: 

Int. Type; 

Area. 

Height: 

2.6*4 

2.5*4 

2.4e4 

2.3a4 

2.2e4 

2.1*4 

2.0*4 

1.9*4-

1.8*4 

1.7*4 

1.6*4-

1.5*4-

- 1.4*4-

1.3*4-

1.2*4 

1.1*4-

1.0*4-

9000.0-

eooo.0-

7000.0 

6000.0 

5000.0-

4000.0-

3000.0-

2000.0-

10OO.0-

0.0 

15.32 J 

17.08 

Data printe d by STW 

Thursday, January 26, 2012 

Page 19 of 27 

Page 67 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

• SampteNam*:'k111227a043' Sampte ID:'GLP10^1-02-24-100' File •k111227a.¥^ 

• P*8k Name: TFOS' Mass(**)' '499.000^0.000 Da,499.000/99.000 Da,499.000/130.000 DaI CofTMii*nt.-DAL-GW-133L-RB-" Amotatwn. " 

Sample Index: 

Sample Type; 

Concentration: 

Calculated Cone; 

H/A 

1. Hindow: 

t . Factor: 

itqest Peak' 

Hanual 

15 3 

12460 ct 

2.3*4 

2.2*4 

2.1*4-

2.0*4-

1.7*4 

1.6*4 

1.5*4-

1.4*4 

1.3*4-

12*4-

1.1*4-

1.0*4-

9000.0 

8000.0 

7000.0-

6000.0 

5000.0 

4000.0 

3000.0 

2000.0 

1000.0 

15.0 15.5 16.0 16.5 17.0 17.5 

I

SampteName •kll12278046- Sampte ID 'GLP10-01-02-24-096' Fie,-k111227a.w1fP 

Peak Nam* -PFOS- Mass{es)' '499.000/80.000 Da,499.000/99.000 Da,499.000/130.000 DaComm*nt -DAL-GW-TRIPOl-MS-' Annotation " 

Sample Index; 46 

Sample Type: Unknown 

ng/mL 

Hodified ; Yes 

Proc. Algorithm ; Specify : 

Moise Percentage: 50 

Peak Height: 

Sinoothing Wic 

RT Hindow; 

Expected RT: 

2.5*6-

2.4e6-

2.3eS 

2.2e6 

2.1e6-

2.0*6-

1.9*6 

1.ee6' 

1.7*6-

1.6*6 

1.5*6 

1.4*6 

1J«6 

1Je6 

1.1e6 

1.0e6 

9.0*5 

8.0*5 

7.0e5 

6.0e5 

5.0e5 

4.0*5 

3.0e5 

2.0e5 

14.5 15.0 15.5 16.0 1B.5 17.0 17.5 

I

SampteName 'kl11227a049' Sampte ID''GLP10^1-02-24-001' FIto: 

Peak Name 'PFOS' Massfes): -499.000/80.000 Da,499.000/99.000 Da.' 

Comment -DAL-GW-ISOR-O-' Annotation' ~ 

Sanple Index; 19 

Sample Type; Unknown 

Concentration; N/A 

Calculated Cone; 444. ng/mL 

Acq. Date: 12/2B/2011 

I

Sample Name' Td 11227a056' Sampte ID: *GLP10-01-02-24-004' Fie: 'kl 11227a.wir 

Peak Name -PFOS" Massfes). "499.000/80.000 Da,499.000/99.000 Da,499.000/130.000 DaComment "DAL-GW-ISOS-O-- Annotation. -

Acq. Tine; 4:53;1' 

It. lypt-^ 

3.6*5 

3.4*5 

32e5 

3.0*5 

2.8*5 

2.6*5 

2.4*5 

2.2*5 

2.0*5 

1.6*5 

1.6*5 

1.4*5 

12*5 

1.0*5 

8.0*4 

6.0*4 

4.0*4 

2.0*4 

12/28/2011 

Sub. Window; 

-t Largest Peak: 

Peak Height; 

Smoothing WidI 

RT Hindow: 

Expected RTManual 

l e; 15.2 

8567243 c< 

m i 

7.0*5-

6.5e5-

6.0e5-

5.5e5-

5.0*5-

4.5*5-

4.0e5-

3.5e5-

3.0eS2.5*5-

2.0*5-

1.5*5-

1.0*5-

5.0*4-

13.0 13.5 14.5 15.0 15.5 16.0 16.5 17.0 17.5 

Data printe d by STW 

Thursday, January 26, 2012 

Page 20 o f 27 

Page 68 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS. and PFOS in Groundwater 

Decatur, AL - December 2011 

*ETS-Kirk Result s Name: klll227a.rd b 

I

Sampte Name, "kl 11227*059" Sempte ID: "GLP 1001-02-24-007" File' "k111227a wtr 

Peak Name: "PFOS" Mass(es). "499.000/80.000 Da.499.000/99.000 Da,499.000/130.000 DaComment "DAL-GW-130L-O-- Annotation: -

Sample Index: 59 

Sample Type; Unknown 

Concentration; M/A 

Calculated Cone: 65.8 ng/mL 

Proc. Algorithm: Specify Pars 

Report Largest Pe 

Hin. Peak width : 

Smoothing Hldth : 

RT WindowExpected RT: 

Use Relativ e RT; 

14.5 15.0 15.5 16.0 16.5 17.0 17.5 

Algorithm- Spec 

Baae. Sub. Hindi 

Kin. Peak HeightMin, Peak Width. 

Smoothing Width. 

RT Hindow: 

i f y Para 

50 

1.00 

I

SampteName:H111227a062- Sampte ID.•GLPlO-01-02-24-010- Fie "I 

Peak Name "PFOS" Mass(es) "499.000/80.000 Da,499.000/99.000 Da,4S 

Comment 'DAL-GW-iaiR-O-" Annotttion.-

Sanple Index: 62 

1.10*6 

1.05e6 

1.00e6 

9.50e5 

9.00*5 

150*5 

8.00*5 

7.50*5 

7.00*5 

6.50*5 

6.00e5 

5.50*5 

5.00*5 

4.50*5 

4,00*5 

3.50*5 

3.00*5 

2.50*5 

2,00*5 

1.50*5 

I.OOeS 

5.00*4 

0.00 

Manual 

lb. 2 

13466185 < 

14.5 15.0 15.5 16.0 16.5 17.0 17.5 

I Pen itage: 

; Specify ParatneC 

Int . Type; 

Retention 1 

Area: 

Start Time: 

End Tims; 

:plit . factor; 

. Largest Peak: 

'eak Height-

'«ak Hidth : 

ling Width; 

idow: 3( 

1 RT; 1 

I

Sampte Name' "kl 11227b069" Sampte ID: "GLP10-01-02-24-013' FIto:' 

Peak Nam*' -pFOS' Mass(»s). '499.000/80.000 Da.499.OO(V99.O00 Da,4< 

Comment "DAL-GW-ISIS-O-- Annotation." 

Sample Index; S 

Sanple Type: Unknown 

5.0*4 

4.8*4 

4.6*4 

4.4*4 

4.2*4 

4.0e4 

3.6*4 

3.6*4 

3.4*4-

3.2*4 

3.0*4 

2.8*4 

2.5*4 

2.4*4 

2.2*4 

2.0*4 

1.BM 

1.6*4 

1.4*4 

1.2*4 

1.0*4 

8000.0 

SampteNamB:"M11227b07r Sampte ID:-GLPlOO1-02-24-016- Fie: •k111227b.wtr 

Peak Nam*. TFOS' Mass(ea) "499.000/80.000 Da ,499.000/99.000 Oa.499.000/130.000 DaComment;-DAL-GW-131L-0-' AnnolaBon:-

Sample Index: 8 

Sample Type; Unknown 

Calcula t 28.0 n^ 

12/29/2011 

12:12:43 PM 

Algorithm : Specify Pars 

Smoothing Hidth ; 3 

RT Hindow; 30.0 

Expected RT; 15.4 

Use Relativ e RT: llo 

Int . Type; Manual 

Retention Time: 15.5 

Area: 2S1912B ct 

Height: 2.96e*005 

-.15.68 

2.8*5-

2.6*5-

2.4eS2.2*5-

2.0*5-

1.8*5-

g- 1.6*5-

g 1.4*5-

15e5-

l.OeS8.0*4 

6.0*4 

Data printe d by STW 

Thursday, January 26, 

Page 21 o f 27 

Page 69 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

• Sampte Nam*: -kl 11227b075" Sampte ID: -( 

• P*Bk Nam*: -PFOS- M3SS(*£)- -499.0DO/80.D( 

I Comm*nt T>AL-GW-133R-t^-- Annotation'" 

Sanple InJex: 11 

Saaple Type: 

N/A 

Calculated Cone; 41.1 

Acq. Date: 12/29/2011 

Acq, Time: 1;14:40 P^ 

Smoothing wtdl 

RT Window: 

Expected RT: 

ng/r 

Hanual 

15.5 

1116483 COL 

3.77e-fO0S 

3.6*5 

3.4*5 

3.2*5 

3.0*5 

2.8*5 

2.6*5 

2A«5 

2.2*5 

2.0*5 

1.2*5-

1.0*5-

eo»4> 

60e4 

4,0*4 

2.0*4-

14,5 15.0 15.5 16.0 16.5 17.0 17.5 

I

Sampte Name: 'K1l1227b082- Sampte ID, -< 

Peak Name 'PFOS- Mass(es):'499.000/80 

Comment: •DAL-GW-133S-0-' Annotation ' 

Sample Index; IB 

Sample Type: Unknown 

Concentration; ll/A 

Calculated Cone: 176. ng/nL 

Acq. Date; 12/29/2011 

Acq. Tine: 3:39:08 PH 

Hodified; Yes 

Kin Peak Height: 

Hin. Peak Hldth; 

Smoothing Hidth; 

RT Window1.6e6 

1.5e6 

1.4e6 

1.3e6 

1.2e6 

1.1e6 

1.0*6 

§• 9.0e5 

t 

1 6.0*5 

7.0e5 

6.0e5 

5.0*5 

4.0*5 

3.0*5 

2.0e5 

1.0e5 

14.5 15.0 15.5 16.0 16.5 17.0 17.5 

I

Sampte Name: "kl 11227b085- Sampte ID: -i 

Peak Name: TFOS- Massfes) -499.000^80.01 

Comment: "DAL-GW-133L-(V" Annotation. 

ample Index: 21 

. Algorithm: : 

. Sub. Window; 

I

Sampte Nam*: "Vl 11227t>088" Sampte ID' "i 

Peak Name "PFOS" Mass(es) "499.000/80.01 

CommenL -OAL-GW.134R.O-' Annotation: -

Sample Index: 24 

Smoothing Hid! 

RT Hindow; 

Expected RT; 

Height. 

Start Time 

End Tlma: 

9.0*5 

8.0*5 

7.0*5 

6,0*5 

5.0*5 

4.0e5 

3.0*5 

2.0*5 

1.0*5 

Hoi: Pert 

Baae. Sul 

Report Lt 

Factor; 

St Peak: 

Hin. Peak Hidth; 

Smoothing Hldth: 

RT Hindow; 3C 

i Relal ! RT: 

1.42e+006 cps 

,33^ ^ 

1.3e6-

1.2e6-

1.1*6-

1.0*6-

9.0e5-

8.0eS7.0e5 

6.0e5 

5.0e5-

4.0*5-

3.0*5-

2.0e5-

4.5 15.0 15.5 16.0 16.5 17.0 17.5 

Data printe d by STW 

Thursday, January 26, 

Page 22 of 27 

Page 70 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

• Sampte Nam*' 'k l 11227b095' Sampte ID: 'GLP 1001-02-24-031' Rte' "kl 11227b w4r 

I P*Bk Nam*. 'PFOS- Mass(*f): -499.000/8a000 Da.499,000/99.000 Da.499.000/130.000 Da' 

• Comment "DAL-GW-134S-0-- Annotatton -

Sample Index; 31 

Sample Type: Unknowr 

H/A 

17.5 

[-Split . Fact; 

. Peak height: 

1.5*6-

1.4*6-

1.3*6-

1.2e6-

1.1*6-

1.0e6-

9.0e5-

8.0*5-

7.0e5-

4.0*5-

3.0*5-

15.0 15.5 16.0 16.5 17.0 17.5 

I

Sampte Nam*. T(111227ti098- Sampte ID: -GLP 1(M)1-02-24-034" Fte: I 

Peak Nam*. "PFOS- M8S5(*s)' -499.000/80^ Da.499.000/g9.000 Oa,4r 

Comm*nt: -DAL-GW-134L-^)-- Annotatton* ~ 

Sanple Index: 34 

Sample Type- Unknowr 

Calci od Cone 

ll/A 

4 32. 

Modified ; Yes 

Proc. Algorithm: Specify Parj 

Base. Sub. window; I.00 

Peak-Split. Factor: 4 

Report Largest Peak Yes 

Min. Peak Height- 0.00 

Hin . Peak Hldth : 0.00 

Smoothing width ; 3 

RT Window: 30.0 at 

Expected RT: 15.4 m] 

Use Relativ e RT; No 

Int . Type; Manual 

Retention Time: 15.6 m: 

Area: 4321849 count 

Beight: 3.65B-*005 C[ 

Start Time: 15.1 lai 

End Time: 15.8 ml 

3.6*5' 

3.4*5-

3.2*5-

3.0e5-

2.8*5-

2.6e5-

2.4*5 

2.2e5-

2.0*5-

1.8*5-

1.6*5-

1.4*5-

1.2*5-

1.0e5-

8.0e4-

6.0*4-

4.0*4-

2.0*4-

15.0 15.5 16.0 16.5 17.0 17.5 

I SampteName--k11l227b101- SamptelD "! 

Peak Nam*''PFOS- Mass(es)''499 000/SO.O( 

I Commeni "D/y.-GW-135ltO-' Annotation:"' 

alculated Cor 

Peak-Split. Fflctt 

Min Peak Height; 

Min. Peak Hidth : 

Smoothing Width: 

RT Hindow: 

Expected RT: 

Use Relative RT; 

Typo; 

Reter 

Area; 

Height: 

Star t 1 

End Tin 

.12e«006 cps 

l.lOee 

1.05*6 

1.00e6 

9.60e5 

9.00*5 

8.50*5 

6.00*5 

7.50*5-

7.00*5-

6.50*5 

6.00*5-

5.50*5-

5.00*5-

4.50e5-

4.00*5-

3.50*5-

3.00*5-

2.50©5-

2.00*5-

1.50*5-

LOOeS5.00*4-

0.00-

I

SampI* Name: 'k111227b108' Sample ID: 'GLPl 041-02-24-040' Fie' 'I 

Peak Name 'PFOS- Mass(as)' '499.000/80 000 Da,499.000/99.000 Da,49 

CommanL ''DAL-GW-135S.C- Annotation'" 

Sample Index; 44 

4.8*5 

4.6*5 

, Algo) 

Moi; : Perc< 

Base. Sub. window; 

Peak-Split. Factor 

Report Largest Pea 

Hin . Peak Height: 

Hin. Peak Width: 

Smoothing width : 

RT Hindow: 

1 RT; 

Hanual 

5581402 counts 

4.92e'005 cps 

4.2*5 

4.0e5 

3.8*5 

3.6*5 

3.4*5-

3.2*5 

3.0*5 

2.8*5 

2.6*5 

2.4*5 

2.2*5 

2.0eS1.8eS 

1.6e5-

1.4e5-

12e5-

1.0*5-

8.0*4 

6.0*4 

15.0 15.5 16.0 16.5 17.0 17.5 

TTm*. min 

15.0 15.5 16.0 16.5 17.0 17.5 

Data printe d by STW 

Thursday, January 26, 2012 

Page 23 o f 27 

Page 71 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

*ETS-Kirk Result s Name: klll227a.rd b 

I

SampteName:"kl11227b111- Sempte ID •GLP10-01-02-24-043* Fite'•k111227b.wrfP 

PeakName -PFOS* Massfes):'499.000/80.000 Da,499.000/9g.OOODa,499.000/130.000 Da' 

Comment'XAL-GW-135L-a-' Annotation ~ 

Sample Index: 47 

inple Type; 

Concentration: H/A 

Calculated Cone; 32.5 r 

Acq. Date; 12/30/2011 

Acq Time' 1;37;48 AH 

lified : 

Noise Pert 

. Sub. 

:age: 

Peak: 

Factoj 

Peport Largi 

Hin. Peak Height; 

Hin. Peak Hidth ; 

Smoothing Hidth ; 

RT Window: 

Expected RT: 

Use Relativ e RT; 

1.00 tnln 

15.0 15.5 16.0 16.5 17.0 17.5 

I Sampte Name: -k1l1227b114- Sampte ID' 'GLP10-01-02-24-049' Fie •kl11227b wffT 

I Peak Nam* "PFOS" M3£S(BS): "499.000/80.000 Da,499.000/99.000 Da,499.000/130.000 Da' 

I Comment: •0AL-GW-136S-0-- Annoiabon:-

I

Sampte Nam*: 'k111227b12r Sampte ID'*GLPlCM)1-02-24-05r Rta:"k111227b.wflr 

Peak Name: "PFOS" Mas»(*s): "499.000/80.000 Da.499.000/99.000 D».499J»0/130.000 DaComment. "DAL-GW-ISeL-O-* AnnoUtion. " 

Calculated Cone; 65.3 r 

Acq. Date; 12/30/2011 

Acq. Time; 5:04:17 AM 

Modified: Yes 

Proc. Algorithm; Specify Para 

Noise Percentage: 50 

Base. Sub. Hindow; 1.00 

Peak-Split. Factor; 4 

Report Largest Peak: Yea 

Hin. Peak Height: 0.00 

Mm. Peak Width: 0.00 

Smoothing Width: 3 

RT Hindow; 30.0 se 

1 RT: 

; RT: 

6.32e->005 eps 

I

Sampte Name: "kl 11227bl24" Sampte ID' "GLP1001-02-24-058" Fte. "kl 11227lJ.wtr 

Peak Nam*' -pFOS" Mass(es): '499.000/80.000 Da,499.000.199.000 Oa.499.000/130.000 Da' 

Conwnent "DAL-GW-137S^>-" Annotation; " 

Sample Index; 60 

Saaple Type: Unknown 

Concern 

CalculB 

Acq. Dai 

Acq. Tin 

0.587 

6;0£:15 t 

ng/mL 

Proc. Algorithm ; Specify Paran 

1 Percf 

Base. Sub. Hindow; 

Peak-Split. Factor: 

Report Largest Peak; 

Min. Peak Height; 

Kin. Peak Midth; 

RT Hindow; 31 

Expected RTUse Relativ e HT; l 

Int . Type; Mai 

Retention Time. 

Area: 61191: 

Height; 6.II1 

5.0 15.5 16.0 16.5 17.0 17.5 

Data printe d by STW 

Thursday, January 26, 

Page 24 of 27 

Page 72 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Results Name: klll227a.rcl b 

Data printe d by STW 

Thursday, January 26, 2012 

Page 25 o f 27 

Page 73 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS. and PFOS in Groundwater 

Decatur, AL - December 2011 

Result s Name: klll227a.rd b 

I

Sample Nam*. "kl11227t>14r Sampl* ID:-GLP10-01-02-24-073' File: •kll1227b.v«r 

Peak Name: "PFOS" Mass(*s): '499.000/80.0DO Da.499.000/99.000 Da,499.000/130.000 Da' 

Comm*nI, "DAL-GW-1401^0-' Armoiatxtn 

Sample Index: 83 

Saaple Type 

Calculal 

H/A 

jrithm: Specify Pai 

, Window; 1.00 

Min. Peak Hidth : 

Smoothing width : 

RT Hindow: 

Manual 

le: 15.3 

9972480 C( 

L5 15.0 15.5 16.0 16.5 17.0 17.5 

I

SampleName -kl11227bl50' Sample ID'"GLP10-01-02-2' 

Peak Nam* 'PROS' M3ss(es)' "499.000/80.000 Da,499.0r 

Commant 'DAL-GW-141R-0-' Anootatton:" 

Algorithm- Specify Pai 

Smoothing width : 

RT Hindow: 

Expected RT: 

3.ae5 

3.6e5-

3.4*5-

3.2*5-

3.0*5-

2.6*5 

2.6*5 

2.4e5-

2.2eS2.0e5-

1.8*5 

1.6e5 

1.4*5-

1J*5-

1.0*5-

60*4' 

60*4' 

4.0*4-

2.0*4-

14.5 15 0 15.5 16.0 16.5 17.0 17.5 

Proc / 

Noise I 

irithm : Specify Par; 

rentage: 50 

. Window: 1.00 

Smoothing width ; 

RT Hindow: 

Expected RT; 

I

Sample Nam*: "kl l 1227b153' Sample ID: *GLP1 CM]1-02-24-079' File: 'I 

Peak Name. TFOS' Mass{*s): •499.000«0.000 Da,499.000i'M.OOO Da.4S 

Commeni: •DAL-GW-142R-0-* Annotation. "* 

Sample Index: S9 

1.10*6 

1.05*6 

1.00*6 

9.50*5 

9.00*5 

B.50*5 

S.00eS 

7.50*5 

7.00*5 

6.50*5 

e.00eS 

5.50*5 

5.00*5 

4.50*5 

4.00*5 

3.50*5 

3.00*5 

2.50*5 

2.0De5 

1.50e5-

1,00*5-

5,00*4-

0.00-

I

Sample Name- 1(111227t>160" Sampl* ID: "GLP 1 CM) 1-02-2' 

Peak Name "PFOS" Mass(es): '499.000/80.000 Oa,499.0f 

Comment "DAL-GW-143R-0-" /Annotation. " 

Sample Type: 

Calci 

n/A 

12/30/2011 

Algorithm ; Spet 

Sub. Window; 

Uln. Peak iight ; 

Width; 

Smoothing Hidth : 

RT Hindow: 

Expected RT; 

Use Relativ e RT: 

Int , Type; 

1.6*5-

1.5*5-

1.4o5-

1.3*5-

1.2e5-

l.leS1.0e5-

g 9.0*4-

t 8.0*4-

I 

7.0*4-

6.0*4-

5.0e4-

4.0*4-

14.5 15.0 15.5 16.0 16.5 17.0 17.5 14.5 15.0 15.5 16.0 16.5 17.0 17.5 

Data printe d by STW 

Thursday, January 26, 2012 

Page 26 o f 27 

Page 74 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

*ETS-Kirk Result s Name: klll227a.rd b 

I

SampleName "klll227l>163" 

Peak Nan>e: "PFOS' Mass(M 

Comment -DAL-GW.144R-0-' 

Sanple Index: 99 

Sanple Type: Unknown 

Report Largest Pei 

Min. Peak Height; 

Min. Peak Width: 

1.15*5-

1.10*5-

1.05*5-

1.00*5-

9.50*4-

9.00*4-

8.50*4-

8.00*4-

7.50*4-

7.00*4-

^ S.50»4-

6.00*4-

I 5 50*4-

" 5.00*»-

4.50*4-

4.00*4-

3.50*4-

3.00*4-

2.50*4-

2.00*4-

1.60*4-i 

1.00*4-

5000.00-

0.00-

13.0 13.5 14.0 14.5 15.0 15.5 16.0 16.5 

Data printe d by STW 

Thursday, January 26, 2012 

Page 27 of 27 

Page 75 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Workstation : ETSBUSTER Batch Name: bl20104a.dab 

*Data worked up by KJU Page l o f 1 

Printin g Time: 3:41:06 PM 

Printin g Date: Thursday, January 05, 2012 

Page 76 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Workstation: ETSBUSTER Batch Name: bl20104a.dab 

*Data worked up by KJU Page 1 of 1 

Printin g Time: 3:41:30 PM 

Printin g Date: Thursday, January 05, 2012 

Page 77 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Buste r J2930203 Batch Name: bl20104a.dab 

I

SampleNamet)120104a0ir Sample ID,'11012-e4' Flei'l 

P*akName -13C4PFOS-SUR' Masses) •503.0W).0amiT 

Ckimmeni;*1.0n9'mLFC stdin Synth. Watai* Annotation'-

3.2e4 

3.0e4 

2.Be4 

Snoothing Hidth ; 3 

RT Window: 30.0 

Use Relative RT; No 

liQuan - 1 

00 cps 

00 sac 

2.4e4 

2.2*4 

2.0*4 

1.4*4 

1.2*4 

1.0*4 

eooo.0 

6000.0 

4000.0 

2000.0 

' 0.0 

1645 16.76 17.13 17.50 

15.5 16.0 

I

Sample Name''b120104a02a' SamplelD'11010^04' F)e-b120104a.wir 

Peak Name: •13C4PFOS-SUR' MaM{es): '503.0/BO.O amo' 

CommenL 'Method Blank' Annotation ** 

Concentratl< 

Calculated C 

Acq. Date: 

Acq. Time: 

: 0.00373 nt 

1/4/2012 

11:21:36 PM 

il, .l.h.i... .iiM, i4ii,.i . 

I

Sampte Name 'b120104a029" Sampte ID. •LCS-120104-1' Fie; •t>120104a.wi(r 

Peak Nam*: •13C4PFOS-SUR' M3ss(es)- '503.0/80.0 amu' 

Comment. '0.2ppb LCS* Annotation -

Sample Index; 29 

Calculated Cone: 0.201 ng 

Acq. Date: 1/4/2012 

Acq. Tine: 11:12:44 PH 

Modified: No 

Proc. Algorithn : IntelliOua n -

Mm. Peak Height: 0.00 cps 

Min. Peak width ; 0.00 sac 

15.4 

Valley 

15.4 

32058 cc 

7.04e+003 

15.3 

15.6 

I

Sampte Name: •bl20104a032" Sampte ID: •LCS-120104-4' File''b120104a.wifr 

PeakName '13C4PFOS-SUR' Massfes):"SOSCBO.Oamu' 

Comment '2ppb LCS' Annotation-" 

SaiDple Index. 32 

Sample Type; QC 

Concentiatlon : 1.89 ng/nL 

Calculated Cone: 2.13 ng/nL 

Acq. Date: 1/5/2012 

Proc. Algorithn : 

Hin. Peak Height: 

Hin. Peak Uldth : 

Snoothing Mldth. 

RT Mindow: 

ixpec 

Height: 

Star t TJ 

End Ti m 

! RT: 

Data printe d by STW 

Printin g Time: 1:29:03 PM 

Printin g Date: Thursday, January 26,- 2012 

Page 1 o f 

Page 78 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Buste r J2930203 Batch Name: bl20104a.dab 

I

San^to Name. "61201048035' Sampl* ID' -LCS-120104-r Fie: 'b120104a.wir 

Peek Nam*. '13C4PFOS-SUR' Mau{tts}' -503.0/BO.O amu" 

Commeni: "20 ppb LCS" Annotation' -

Saople Index: 3b 

Sanple Type; QC 

Concentration: 0.00 ng/nL 

Calculated Cone: 0.00257 ng/nt. 

Acq. Date; l/S/2012 

Acq. Tine; 1;49;11 AM 

Proc. Algorithn; 1 

Min. Peak HeightHin. Peak Width; 

Snoothing Width: 

RT Klndoa; 

Use Relative RT: 

Height; 

Start TJ 

End Timt 

lelliQuan - IDA 

0.00 cps 

0.00 sec 

I

SampteName •bl20104a042' Sampte ID •GLP10-01-02-24-05a' F**t>1201O4a.wrfr 

Peak Name: '13C4PFOS-SUR' Massfes): '5O3.(V80.0 amu' 

Commant •DAL-GVV^137S-0-' Annotation -

I. Peak Height; 

I. Peak Width; 

lOthing Width-

:. Type; 

.elliQuan - IQJ 

14.0 14.5 

16.14 16.51^16.6017.02 17.47.. 17.87..^ 

6.0 16.5 17.0 17.5 

I

Sampte Name: *b12O104aO45' Sampte ID; *GLP10-01-02-24-061* Fie- 'b1201O4a.wtrr 

Peak Nam*.'13C4PFOS-SUR' Mass(*s),'503.0/80.0 

Comment: •DAL-GW-137L-0-' Annotation. -

Sanple Index: 

Sanple Type; Unknown 

Concentration; H/A 

Calculated Cone: 0.0965 

Acq. Date; 1/5/2012 

Acq. Time: 

I

Sampte Name' 'b1201D4BO48* Sampte ID: 'GLP I CM)1-02-24-070' Fite' 'bl20104a.wir 

PeakName'13C4PFOS-SUR' MaM(es)-'503.0/80.0 

Comment:'DAL-GW-13eL-0-* Annotatksn -

RT Mindo-: 

c p s 

1(0 

ntelliQuan 

0.00 

0.00 

3 

30.0 

15.4 

Ho 

1S103 counts 

3. •ieo'003 cps 

15.3 Hin 

Data printe d by STW 

Printin g Time: 1:29:03 PM 

Printin g Date: Thursday, January 26, 2012 

Page 2 o f 

Page 79 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Buste r J2930203 Batch Name: bl20104a.dab 

Data printe d by STW 

Printin g Time: 1:29:03 PM 

Printin g Date: Thursday, January 26, 2012 

Page 3 o f 8 

Page 80 of 110 
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Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Buste r J2930203 Batch Name: bl20104a.dab 

Data printe d by STW 

Printin g Time: 1:29:03 PM 

Printin g Date: Thursday, January 26, 2012 

Page 

Page 81 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Buster J2930203 Batch Name: bl20104a.dab 

Data printe d by STW 

Printin g Time: 1:29:03 PM 

Printin g Date: Thursday, January 26, 2012 

Page 5 o f 8 

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Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Buste r J2930203 Batch Name: bl20104a.dab 

I

Sampte Nam*: 'b120104a017' Sampte ID. "11012-6-8' Fie. 't)120104a.wir 

Peak Nam* 'PFOS' Mass(*£}' '499.0/130.0 amu.499.0/99.0 amu ,499.0/80.0 

Comment '1.0 nglml. FC std In Synth. Water* Annotation. 

0.948 

l/</201Z 

7:29;47 PH 

I

Sampto Narrw 'b120I04a029' Sampte ID: *LCS-120104-1" Fie' 'bl20104a.wir 

Peak Narw 'PFOS' Mass{es)- '499.0/130.0 amu.499.0»9 0 amu,499.0/BO.O amu' 

Commeni-"0.2ppb LCS* Annotatkin'" 

Modified; 

RT Window; 

Expected RT: 

Height; 

Star t Tif 

End Time' 

9.276*003 cps 

I

Sampto Name:'b120104a032' Sampto ID:'LCS-120104-4' F 

Peak Name. 'PFOS' Ma£s(»a)' "499.0/130.0 amu,499.0/99.0 ai 

CommenL '2ppb LCS' Armotatkin' " 

Sample Index; 32 

Sample Type; QC 

Concentration; 1.84 ng/nL 95*4-

Calculated Cone; 2.14 ng/nL 

Acq. Date; 1/5/2012 

»,-<T Tine- I3;*fi:00 IM 9.0*4-

8.5*4-

8.0*4' 

7.5*4-

7.0*4-

6.5e4' 

6.0*4-

5.5*4-

I 5.0*4-

I 4.5*4-

Expected RT: 

Use Relativ e 

Int . Type: 

Retention Tin 

Aiea: 

Height: 

Star t Time; 

End Time: 

: 15.4 

596409 ci 

2.5*4-

2.0*4-

1.5*4-

1.0*4-

5000.0-

0.0-

Data printe d by STW 

Printin g Time: 1:29:03 PM 

Printin g Date: Thursday, January 26, 2012 

Page 6 o f 

Page 83 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Buste r J2930203 Batch Name: bl20104a.dab 

I Sampte Nam*:'b120104a035 ' Sampte ID'TCS-120104. r Fl* . 1)120104a.wvfr 

I _ . .. iu,499.0/99.0amu,499.0/80.0amu ' 

7.5e5 

7.0*5-

6.5*5-

6.0*5 

I t . Type : 

itentio n 1 

5.5*5 

5.0e5 

4.SeS 

§" 4.0*5 -

I 3.5*5-

15.25-.. 

14.5 15.0 15.5 16.0 16.5 17.0 17.5 

I

Sampte Name ; 'bl20104o042 " Sampte ID: 'C3LP10-01-02-24-^)58" Fite: •bl20104a.wi r 

P*a k Nam* : 'PFOS ' Mats(*»). '499.0/130.0 amu.499.0/99.0 amij,499.0/B0.0 amu ' 

Comman L 'DAL-GW-13 7 S-0-" Annotation: -

Sampl e Index : 12 

Sampl e Type : Unknom n 

Calculated Cone. 0.601 r 

1/5/2012 

4:17 :01 AH 

2.1* 4 

2.0e4 

2.19**004 cps 

1.0*4 

9000.0-

8000.0-

7000.0-

6000.0-

5000.0-

4000.0-

3000.0-

2000.0-

1000.0-

0.0-

13.0 13.5 14.0 14,5 15.0 15.5 16.0 16.5 

I Sampte Nam* . •b120104aO45' Sampte ID: 'GLP10^)1-02-24-061 ' fie : "b120104a.wrtr 

Peak Name - "PFOS ' Mass{es): '49 9 0/130.0 ai 

• Commen t "D/U.-GW-137L-0-' Annotation: -

Saiapl e Index : I S 

j,499.0/99.0 amu.4g9.0/S0.0 ar 

I Sampte Nam* : "^201043048 ' Sampte ID: 'GLP10-01-02-24-070* Fito' 'b1201O4a.wl 

I _ . iu.499.0/99.0amu.499.0/80.0amu ' 

Manual 

15.4 

116902 c< 

1.00*5' 

9.50*4-

9.00*4 

8.50*4 -

a.00»t ' 

7.50*4-

7.00*4-

6.50*4-

6.00*4-

^ 5.50*4-

i 5.00e4' 

E 

= 4.50*4 -

4.00*4 ' 

3.50*4-

3.00*4-

2.50*4 -

2.00*4 -

1.50*4-

1.00*4-

5000.00 

0.00-

Hodifled: 

KT Hindow: 

Expected RT: 

0.461 

1/5/2012 

6:23:26 > 

1.30e*004 cps 

1.0*4-

9500.0 ' 

9000.0-

8500.0 ' 

8000.0 ' 

7500.0 ' 

^ 7000.0 ' 

^ 6500.0-

Data printe d by STW 

Printin g Time: 1:29:03 PM 

Printin g Date: Thursday, January 26, 2012 

4.5 15.0 15.5 16.0 16 J 17.0 17.5 

5500.0' 

5000.0' 

4500.0' 

4000.0-

3500.0' 

3000.0' 

2500.0' 

2000.0' 

1500.0' 

500.0' 

0.0' 

J 

Page 7 o f 

Page 84 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Buste r J2930203 Batch Name: bl20104a.dab 

I

SampteName -61201048055' Sampte ID:'GLP10-01-02-24-076' Fie'tj120104a.wir 

Peak Nam*' 'PFOS' Mass(es)- '499.0/130.0 Bmu,499.0«9.0 amu,499.0/80.0 amu' 

Comment: •DAL-GW-141R-0-' Annotation. ~ 

4.97 ng/mL 

Modified; 

RT Window: 

Expected RT; 

Start Time: 

1X1*5' 

9.0*4-

B.0»4-

7.0*4 

6.0*4-

5.0*4 

4.0a4 

3.0*4-

2.0*4-

I

Sampto Name'"61201048058" Sempte ID-•GLP10-01-01-24-085" Fite •b120104a.w(r 

Peak Nam*' 'PFOS' MBSS{*S). '499.0/130.0 amu,499.0/99.0 annu,499.0/BO.O 

Commoni: "DAL-GW-WR-O-" 

Calculated Cone. 

Acq. Time; 

Modified : 

RT MindowUse Relaclue RT: 

Height: 

Star t Ti 

End Ti m 

26.4 

l/S/2012 

9:54:14 M 

^ 3.5*5-

I 3.0e5-

13.0 13.5 14.0 14.5 15 0 15.5 16.0 16.5 17.0 17.5 

Data printe d by STW 

Printin g Time: 1:29:03 PM 

Printin g Date: Thursday, January 26, 2012 

Page 8 of 8 

Page 85 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

ATTACHMENT C: ANALYTICAL METHOD(S) 

Page 86 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

3IVI Environmental Laboratory 

Method 

Method of Analysis for the Determination of Perfluorinated Compounds in Water 

by LC/MS/MS; Direct Injection Analysis 

Method Number: ETS-8-044.1 

Adoption Date: 4/12/07 

Effective Date: /l/f// / 

Approved By: 

William K. Reagen, Technical Director, Environmental Laboratory Date 

ETS-8-044.1 Page 1 of 22 

Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct 

Injection Analysis 

Page 87 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

1 Scope and Application 

This method describes the direct injection analysis of perfluorinated compounds (PFCs) from 

water matrices using high-perfoimance liquid chromatography tandem mass spectrometry 

(HPLC/MS/MS). The method is generally applicable but not limited to the measurement of 

perfluoroalkyl sulfonamides and perfluorinated alkyi acids (PFAAs) such as perfluorosulfonic 

acids (PFSAs) and perfluorocarboxylic acids (PFCAs) (Table 1). Water samples containing 

heavy particulate may require preparation by an alternate method such as ETS-8-154 

"Detennination of Perfluorinated Acids, Alcohols, Amides, and Sulfonates In Water By Solid 

Phase Extraction and High Perfonnance Liquid Chromatography/Mass Spectrometry". The 

method is applicable to both extemal standard and intemal standard calibration V 

Table 1. Representative Target Analytes 

Acronym Analyte 

Chemical Abstract Services 

Registry Number (CASRN) 

PFBA (C4 Acid) Perfluorobutanoic acid 375-22-4 

PFPeA (C5 Acid) Perfluoropentanoic acid 2706-90-3 

PFHxA (C6 Acid) Perfluorohexanoic acid 307-24-4 

PFHpA (C7 Acid) Perfluoroheptanoic acid 375-85-9 

PFOA (C8 Acid) Perfluorooctanoic acid 335-67-1 

PFNA (C9 Acid) Perfluorononanoic acid 375-95-1 

PFDA (CIO Acid) Perfluorodecanoic acid 335-76-2 

PFUnA(C11 Acid) Perfluoroundecanoic acid 2058-94-8 

PFDoA(C12Acid) Perfluorododecanoic acid 307-55-1 

PFTrDA(C13 Acid) Perfluorotridecanoic acid 72629-94-8 

PFBS (C4 Sulfonate) Perfluorobutanesulfonic acid 375-73-5 

PFHS (C6 Sulfonate) Perfluorohexanesulfonic acid 355-46-4 

PFOS (C8 Sulfonate) Perfluorooctanesulfonic acid 1763-23-1 

FBSA (C4 Sulfonamide Perfluorobutanesulfonamide 30334-69-1 

FOSA (C8 Sulfonamide) Pefluorooctanesulfonamide 754-91-6 

The Minimum Reporting Level (MRL) is the Limit of Quantitation (LOQ) that meets Data 

Quality Objectives (DQOs) that are developed based on the intended use of this method. 

Method Flexibility - This is a perfonnance-based method and may be generally applied to the 

determination of perfluorinated compounds in water matrices when analysis batch quality 

control (QC) criteria are met^. Each set of samples are prepared in an analysis batch with 

calibration standards, LCSs, blanks, and continuing calibration check standards analyzed on 

the same instrument during a time period that begins and ends with the analysis of the 

appropriate continuing calibration check standards. The laboratory is pemnitted to modify the 

LC column, mobile phase composition, LC conditions, and MS/MS conditions. Method 

modifications should be considered to improve method perfomnance or to meet data quality 

objectives for the study. In all cases where method modifications are implemented, the batch 

' The method is supported by validation with intemal standard calibration for C4-C13 PFCAs, C4, C6, and C8 PFSAs, 

and C8 perfluoroalkane sulfonamide in laboratory control samples under 3M method validation El 1-0667. 

^ Guidance for establishing method QC Criteria based on a.) FDA May 2001, "Guidance for Industry, Bioanalytical 

Method Validation", b.) EPA Method 537, and c.) European Commission: Guidance for Generating and Reporting 

Methods of Analysis m Support of Pre-registration Data Requirements for Annex II (Part A, section 4) and Annex HI 

(Part A,section 5) of Directive 91/414, SANCO/3029/99 rev. 4 (11/07/00). 

ETS-8-044.1 Page 2 of 22 

Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; 

Direct Injection Analysis 

Page 88 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

analytical QCs (section 9) must be completed and pass QC acceptance criteria (section 13) if 

the data from the analytical batch are to be reported. 

2 Method Summary 

Water samples are analyzed as neat aqueous sample or as solvent diluted aqueous samples 

by direct injection using LC/MS/MS. Samples containing heavy particulate may not be 

suitable for analysis by this method. Samples containing suspended particulate should be 

centrifuged or filtered prior to removing a sample aliquot or diluting with solvent. The water 

sample is mixed well prior to removing an aliquot or diluting, if necessary, with ASTM Type I 

water, HPLC water, other suitable water, or solvent (methanol). 

Quantitation is by stable isotope internal standard calibration in laboratory reagent water. All 

perfluorinated compounds (PFCs) target analyte concentrations of perfluorosulfonic acids 

(PFSAs) and perfluorocarboxylic acids (PFCAs) are reported as anions and corrected for 

their salt or free acid fomns. Alternatively, quantitation may be perfomried by extemal 

standard calibration. 

This is a perfomnance-based method. Method uncertainty for each target analyte is 

detennined for each analytical batch using multiple laboratory control spikes at multiple 

concentrations. This method also requires that the precision and accuracy for each sample 

be determined using field matrix spikes to verify that the method is applicable to each sample 

matrix. 

Calibration standards for PFUnA, PFDoA, PFTrDA, and FOSA have been found to be 

unstable for more than 2 days in 100% water. Samples requiring analysis for these 

compounds by this method should be diluted 1:1 with methanol and analyzed against a 

calibration curve prepared in 1:1 synthetic groundwaterMeOH. 

3 Definitions 

3.1 Analysis Batchi 

A set of study samples that are prepared with calibration standards, laboratory control 

samples, and procedural blanks, and analyzed on the same instrument during a time period 

that begins and ends with the analysis of the appropriate continuing calibration check 

standards. 

3.2 Analytical Sample 

A portion of a laboratory sample prepared for analysis. 

3.3 Calibration Standard 

A solution prepared by spiking a known volume of the Working Standard (WS) into a 

predetemnined amount of ASTM Type I, HPLC grade water, or other suitable water (i.e. 

matrix water), and analyzed according to this method. Calibration standards are used to 

calibrate the instrument response with respect to analyte concentration. 

3.4 Laboratory Duplicate Sample (LDS, or Lab Dup) 

A laboratory duplicate sample is a separate aliquot of a sample taken in the analytical 

laboratory that is analyzed separately with identical procedures. Analysis of LDSs compared 

to that of the first aliquot give a measure of the precision associated with laboratory 

procedures, but not with sample collection, preservation, or storage procedures. 

ETS-8-044.1 Page 3 of 22 

Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; 

Direct Injection Analysis 

Page 89 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

3.5 Field Blank (FB)/Trip Blank (TB) 

ASTM Type 1, HPLC grade water, or other suitable water, placed in a sample container in the 

laboratory and treated as a sample in all respects, including exposure to sampling site 

conditions, storage, preservation and all analytical procedures. The purpose of the TB is to 

detennine if test substances or other interferences are present in the field environment. This 

sample is also referred to as a Trip Blank. 

3.6 Field Duplicate Sample (FDS, Field Dup) 

A sample collected in duplicate at the same time from the same location as the sample. The 

FDS is handled under identical circumstances and treated exactly the same throughout field 

and laboratory procedures. Analysis of the FDS compared to that of the first sample gives a 

measure of the precision associated with sample collection, preservation and storage, as well 

as with laboratory procedures. 

3.7 Field Matrix Spike (FMS) 

A sample to which known quantities of the target analytes, ISs and SRSs are added to the 

sample bottle in the laboratory before the bottles are sent to the field for collection of aqueous 

samples. A known, specific volume of sample must be added to the sample container 

without rinsing. This may be accomplished by making a "fill to this level" line on the outside of 

the sample container. The FMS is analyzed to ascertain if any matrix effects, interferences, 

or stability issues may complicate the interpretation of the sample analysis. 

3.8 Trip Blank Matrix Spike (TBMS) 

An aliquot of ASTM Type 1, HPLC grade water, or other suitable water, to which known 

quantities of the target analytes, ISs and SRSs are added in the laboratory prior to the 

shipment of the collection bottles. The TBMS is analyzed exactly like a study sample to help 

determine if the method is in control and whether a loss of analyte or analytical bias could be 

attributed to sample holding time, sample storage and/or shipment issues. A low and high 

TBMS are appropriate when expected sample concentrations are not known or may vary. 

3.9 internal Standard (IS) 

A compound added to each study sample, calibration standard, laboratory control samples, 

and procedural blanks at a consistent level (typically around 1 ng/mL). The intemal 

standard(s) are stable isotope labeled versions of the target analytes. The area count ratio of 

the target analyte to the internal standard is used for calibration. Surrogate ISs are applied 

when stable isotope ISs of target analytes are unavailable. A surrogate IS is not necessarily 

a stable isotope labeled version of the target analyte, but is treated as an intemal standard for 

quantitation. 

3.10 Laboratory Control Sample (LCS) 

An aliquot of control matrix to which known quantities of the target analytes, ISs and SRSs 

(when applicable) are added in the laboratory at the time when samples are aliquotted. At 

least three levels (two levels for SRSs) in triplicate are included, one generally at the low end 

of the calibration curve and one near the mid range and the upper end of the curve. The 

LCSs are analyzed exactly like a laboratory sample to determine whether the stability of the 

standards. LCSs should be prepared each day samples are aliquoted. 

3.11 Laboratory Matrix Spike (LMS) 

A laboratory matrix spike is an aliquot of a sample to which known quantities of target 

analytes, ISs and SRSs (when applicable) are added in the laboratory. The LMS is analyzed 

exactly like a laboratory sample to detemnine whether the sample matrix contributes bias to 

the analytical results. The endogenous concentrations of the analytes in the sample matrix 

must be determined in a separate aliquot and the measured values in the LMS corrected for 

these concentrations. LMSs are optional for analysis of aqueous samples. 

ETS-8-044.1 Page 4 of 22 

Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; 

Direct Injection Analysis 

Page 90 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

3.12 Laboratory Sample 

A portion or aliquot of a sample received from the field for testing. 

3.13 Limit of Quantitation (LOQ) 

The lower limit of quantitation (LLOQ) for an analytical batch is the lowest concentration that 

can be reliably quantitated within the specified limits of precision and accuracy. The LLOQ is 

generally selected as the lowest non-zero standard in the calibration curve that meets method 

acceptance criteria. The LLOQ for each target analyte is established for each analysis batch 

as the lowest calibration standard with area counts at least twice that of the average area 

counts of the procedural blanks. 

The upper limit of quantitation (ULOQ) for an analytical batch is the highest concentration that 

can be reliably quantitated within the specified limits of precision and accuracy. The highest 

standard in the calibration curve that meets method acceptance criteria is defined as the 

ULOQ. 

3.14 Method/Procedural Blank 

An aliquot of control matrix that is treated exactly like a laboratory sample including exposure 

to all glassware, equipment, solvents, and reagents that are used with other laboratory 

samples. The method blank is used to detennine if test substances or other interferences are 

present in the laboratory environment, the reagents, or the apparatus. 

3.15 Sample 

A sample is an aliquot removed from a larger quantity of material intended to represent the 

original source material. 

3.16 Stock Standard Solution (SSS) 

A concentrated solution of a single-analyte prepared in the laboratory with an assayed 

reference compound. 

3.17 Surrogate Internal Standard 

An IS that is not necessarily a stable isotopically labeled target analyte, but is treated as an 

intemal standard for quantitation. Sun-ogate ISs are used when isotopically labeled 

counterparts of the target analyte are not commercially or readily available. 

3.18 Surrogate Recovery Standard (SRS) 

An isotopically labeled standard, not used as an intemal standard, that is added to each 

sample and appropriate QC sample as a means to evaluate the method performance for a 

chemical class of compounds (e.g., PFSAs, PFCAs). 

3.19 Working Standard (WS) 

A solution of several analytes prepared in the laboratory from SSSs and diluted as needed to 

prepare calibration standards and other required analyte solutions. 

4 Warnings and Cautions 

4.1 Health and Safety 

The acute and chronic toxicity of the standards for this method have not been precisely 

detennined; however, each should be treated as a potential health hazard. The analyst 

should wear gloves, a lab coat, and safety glasses to prevent exposure to chemicals that 

might be present. 

ETS-8-044.1 Page 5 of 22 

Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; 

Direct Injection Analysis 

Page 91 of 110 
GLP10-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

The laboratory is responsible for maintaining a safe work environment and a current 

awareness of local regulafions regarding the handling of the chemicals used in this method. 

A reference file of material safety data sheets (MSDS) should be available to all personnel 

involved in these analyses. 

4.2 Cautions 

The analyst must be familiar with the laboratory equipment and potential hazards including, 

but not limited to, the use of solvents, pressurized gas and solvent lines, high voltage, and 

vacuum systems. Refer to the appropriate equipment procedure or operator manual for 

additional information and cautions. 

5 Interferences 

During sample preparation and analysis, major potential contaminant sources are reagents 

and glassware. All materials used in the analyses shall be demonstrated to be free from 

interferences under conditions of analysis by running method blanks. 

Parts and supplies that contain Teflon® should be avoided or minimized due to the possibility 

of interference and/or contamination. These may include, but are not limited to: wash bottles. 

Teflon® lined caps, autovial caps, HPLC parts, etc. 

The use of disposable micropipettes or pipettes to aliquot standard solutions is recommended 

to make calibration standards and matrix spikes. 

6 Instrumentation, Supplies, and Materials 

6.1 Instrumentation 

Analytical balance capable of reading to 0.0001 g 

HPLC/MS/MS or HPLC/MS system, as described in Section 10. 

6.2 Supplies and Materials 

Sample collection bottles—HDPE (e.g., NalgeneTM) wide-mouth bottles with screw cap. 

Note: Do not use fluorinated or Teflon® bottles or lined caps. 

Coolers or boxes for sample shipment. 

15-mL and 50-mL disposable polypropylene centrifuge tubes. 

Class A pipettes and volumetric flasks, various. 

2 mL HPLC autovials 

Disposable pipettes, polypropylene or glass as appropriate 

Centrifuge capable of spinning 15-mL and 50-mL polypropylene tubes at 3000 rpm. 

7 Reagents and Standards 

Note: Suppliers and catalog numbers are for illustrative purposes only. Equivalent 

perfomnance may be achieved using chemicals obtained from other suppliers. Do not use a 

lesser grade of chemical than those listed. 

7.1 Chemicals 

Water - Milli-Q, HPLC grade, or other suitably appropriate sources 

Calcium Acetate - A.C.S. Reagent Grade 

ETS-8-044.1 Page 6 of 22 

Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; 

Direct Injection Analysis 

Page 92 of 110 
GLPIO-01-02; Interim Report 24 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Magnesium Acetate - A.C.S. Reagent Grade 

Methanol - HPLC grade 

Ammonium Acetate - A.C.S. Reagent Grade 

7.2 Representative Target Analytes, ISs, and SRSs 

PFBA, Heptafluorobutyric Acid, (C4 Perfluorinated Acid) 

PFPeA, Nonafluoropentanoic Acid (C5 Perfluorinated Acid) 

PFHxA, Perfluorohexanoic Acid (Ce Perfluorinated Acid) 

PFHpA, Tridecafluoroheptanoic Acid, (C7 Perfluorinated Acid) 

PFOA, Ammonium perfluorooctanoate, (Cs Perfluorinated Acid) 

PFNA, Heptadecafluorononanoic Acid, (Cg Perfluorinated Acid) 

PFDA, Nonadecafluorodecanoic Acid (C10 Perfluorinated Acid) 

PFUnA, Perfluoroundecanoic Acid, (Cn Perfluorinated Acid) 

PFDoA, Perfluorododecanoic Acid, (C12 Perfluorinated Acid) 

PFTrDA, Perfluorotridecanoic Acid, (C13 Perfluorinated Acid) 

FBSA, Perfluorobutanesulfonamide 

FOSA, Perfluorooctanesulfonylamide 

PFBS, Potassium Perfluorobutanesulfonate 

PFHS, Perfluorohexanesulfonate 

PFOS, Potassium perfluorooctanesulfonate 

PFOA [1,2, 3,4-"C], "C4-isotopically labeled perfluorooctanoic acid (SRS) 

PFOS [1,2, 3,4-"C], "C4-isotopically labeled Perfluorooctanesulfonate (SRS) 

PFUnA [1,2-"C], "C2-isotopically labeled Perfluoroundecanoic acid (SRS) 

A custom mix of ISs in a methanolic solution containing ([1,2,3,4-"C4]PFBA, [1,2 -

"CJPFHxA, [1,2,3,4,5,6,7,8-^^C8lPFOA, [1,2,3,4,5,6,7 8,9-^^C9]PFNA, [1,2 -^^CJPFDA, 

[1,2,3,4,5,6,7-"CyjPFUnA, [1,2 -"CJPFDoA, [1,2,3 -^^CajPFHS, [1,2,3,4,5,6,7,8-^^C8]PFOS, 

and [1,2,3,4,5,6,7,8-"C8]PFOSA (Wellington Laboratories, Guelph, ON) in combination with 

added ([1,2,3,4,5-"C5]PFPeA, ([1,2,3,4-^C4]PFHpA, and [^^OJPFBS can be used to prepare 

a stock IS solution. Alternatively, individual stable isotope ISs can be used to prepare a stock 

IS mixture. 

Other ISs can be applied. 

7.3 Reagent Preparation 

2 mM Ammonium acetate solution (Analysis)—^Weigh 0.3 g of Ammonium acetate and 

dissolve in 2.0 L of reagent water. 

Synthetic Groundwater (containing 25 ppm Ca and Mg) - Weigh 0.61 g of Calcium Acetate 

and 0.92 g of Magnesium Acetate and dissolve in 6.0 L of reagent water. 

Note: Alternative volumes may be prepared as long as the ratios of the solvent to solute rafios 

are maintained. 

ETS-8-044.1 Page 7 of 22 

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Page 93 of 110 
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Decatur, AL - December 2011 

7.4 Stock Standard Solution (SSS) and Working Standard Solution 

Preparation 

The following standard preparation procedure serves as an example. Weighed amounts and 

flnal volumes may be changed to suit the needs of a particular study. For example, pL 

volumes may be spiked into volumetric flasks when diluting stock solutions to appropriate 

levels. 

100 pg/mL target analyte SSSs—Weigh out 10 mg of analytical standard (corrected for 

percent salt, acid [ETS-4-031] and purity) and dilute to 100 mL with methanol or other 

suitable solvent, in a 100 mL volumetric flask. Transfer to a 125 mL LDPE bottle or other 

suitable container. Prepare a separate solution for each analyte. Expiration dates and 

storage conditions of stock solutions should be assigned in accordance with laboratory 

standard operating procedure. An example of purity and salt correction is given below for 

PFOS. 

^. r L molecular weight of anion 

salt correction factor = = 

moclecular weight of salt 

499 PFOS (K-')salt correction factor = — = 0.9275 

538 

10 mg CsFiySOa'K* with purity 90% = 8.35 mg C8F17SO3' (10 mg*0.90*0.9275=8.35 mg) 

10 MQ/mL (10,000 ng/mL) mixed working standard—Add 5.0 mL each of the 100 pg/mL 

SSSs to a 50 mL volumetric flask and bring up to volume with solvent. 

1 (jg/mL (1,000 ng/mL) mixed worl<ing standard—Add 0.5 mL of the 100 pg/mL SSSs to a 

50 mL volumetric flask and bring up to volume with solvent. 

0.1 MQ/mL (100 ng/mL) mixed standard—Add 0.05 mL of the 100 pg/mL SSSs to a 50 mL 

volumetric flask and bring up to volume with solvent. 

Storage Conditions—Store all SSSs and wori<ing standards in accordance with laboratory 

standard operating procedure or in a refrigerator at 4°±2°C for a maximum period of 6 months 

from the date of preparation. 

7.5 Calibration Standards 

Calibration can be perfonned by IS or external calibration. Using the wori<ing standards 

described above, prepare calibration solutions in ASTM Type 1 water, HPLC water, other 

suitable water, or a mixture of solvent and water using the infomnation in Table 2 as a 

guideline. Note: Volumes of water or water/solvent mixtures and wori<ing standards may be 

adjusted to meet the data quality objectives addressed in the general project outline. 

Calibration levels other than those listed below can be prepared as needed. 

For the quantitation of PFOA and PFOS, reference materials of certified mixed linear and 

branched isomer are preferred. Alternately, reference materials of primarily linear isomers of 

PFOA and/or PFOS may be used, however, when quantitating with predominantly linear 

reference standards, additional LCS samples containing both linear and branched isomers of 

PFOA and PFOS are required^. 

7.5.1 Intemal Standard (IS) and Surrogate Recovery Standard (SRS) 

For IS calibration, stable isotope intemal standards of each target analyte or appropriate 

surrogate ISs should be spiked at the same level in all calibration standards. Once the 

calibration standards have been prepared as stated above in Section 7.5, all calibration 

standards are spiked with a separate internal standard spiking solution. Typically the 

' A report summarizing an assessment of the use of reference standards containing certified linear and branched isomers of 

PFOA/PFOS can be found in 3M report Ell-0560. 

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Decatur, AL - December 2011 

concentration of the internal standard is consistent with the internal standard concentration 

expected in the samples being prepared, usually 1 ng/mL. The concentration of the intemal 

standard spiking solution is typically 2 pg/mL. A separate zero point or method blank is 

typically prepared at the same time as the calibration standards, using the same solution 

used to prepare the standards (ASTM Type 1 water, HPLC water, other suitable water, or a 

solvent/water mixture), and is spiked with the intemal standard at the same concentrafion as 

the calibration curve, typically at 1 ng/mL. 

If the samples being analzyed were pre-spiked with SRSs, the calibration curve prepared in 

Section 7.5 is spiked with a separate SRS spiking solution. Typically, the sample bottles are 

spiked with a SRS at 0.1 ng/mL. The final calibration curve must consist of at least six 

calibration points after analysis. The following table provides an example of spike 

concentrations and volumes used to achieve a multi-point extracted calibration curve with 

internal standard and sun'ogate standard. 

Table 1 lists recommended stable isotope internal standards for several PFSA and PFCA 

target compounds. A custom mix of isotopically labeled target analytes in a methanolic 

solution containing ([1,2,3,4-"C4]PFBA, [1,2 -^^CJPFHxA, [1,2,3,4,5,6 7,8-"C8]PFOA, 

[1,2,3,4,5,6,7,8,9-X9]PFNA, [1,2,3,4,5,6 -"CejPFDA, [1,2,3,4,5,6,7 -''XylPFUnA, [1,2 -

"CJPFDoA, [1,2,3-"C3]PFHS, [1,2,3,4,5,6,7,8-"C8]PFOS, and [1,2,3,4,5,6,7,8-"C8]FOSA 

(Wellington Laboratories, Guelph, ON) in combination with added ([1,2,3,4,5-"C5]PFPeA, 

([1,2,3,4-"C4]PFHpA, and [^^OJPFBS can be used to prepare a stock IS solution. 

Alternative sources of certified stable isotope labeled target analytes are applicable. 

Alternatively, individual stable isotope ISs can be used to prepare a stock IS mixture. The 

table below lists the recommended stable isotope ISs and SRSs applied in the method. 

Other stable isotope ISs and SRSs of target analytes not listed in the table may be used if 

supported by validation and/or analysis batch QCs meeting method acceptance criteria (e.g., 

[^^CJ-PFOA). The same intemal standard should be used for a given analyte throughout the 

entire project/study. Note: some of the compounds listed below are appropriate to use as 

surrogate ISs when a stable isotope IS of a target analyte is not available. Generally, 

surrogate isotopically labeled PFCAs are used for PFCAs, and surrogate isotopically labeled 

PFSAs are used for PFSAs. 

Table 2 provides examples of spike concentrations and volumes used to achieve a multi-point 

calibration curve with ISs and SRSs. 

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Decatur, AL - December 2011 

Table 1. Stable Isotope PFCAs and PFSAs used for ISs and SRSs 

Compound Natne Synonym or Acronym Analytical Purpose Reference Standard 

Source 

"C4-Perfluorobutanoic acid [1,2,3,4-"C4]PFBA IS for PFBA 

Wellington Labs 

(Mix or Individual) 

"C4-Perfluoropentanoic acid [l,2,3,4,5-"C5]PFPeA IS for PFPeA 

Wellington Labs 

(Mix or Individual) 

"C2-Perfluorohexanoic acid [l,2-"C2]PFHxA IS for PFHxA 

Wellington Labs 

(Mix or Individual) 

"C4-Perfluoroheptanoic acid [l,2,3,4-"C4]PFHpA IS for PFHpA 

Wellington Labs 

(Mix or Individual) 

'^Cg-Perfluorooctanoic acid [l,2,3,4,5,6,7,8-"C8]PFOA IS forPFOA and [1,2,3,4 

"C4]PFOA 

Wellington Labs 

(Mix or Individual) 

"Cg-Perfluorononanoic acid [1,2,3,4,5,6,7,8,9-"C9]PFNA IS for PFNA 

Wellington Labs 

(Mix or Individual) 

"Ce-Perfluorodecanoic acid [1,2,3,4,5,6-"CslPFDA IS for PFDA 

Wellington Labs 

(Mix or Individual) 

"C7-Perfluoroundecanoic acid [1,2,3,4,5,6,7-"ClPFUnA IS for PFUnA 

Wellington Labs 

(Mix or Individual) 

"C2-Perfluorododecanoic acid [l,2-"C2]PFDoA IS for PFDoA, *PFTA 

Wellington Labs 

(Mix or Individual) 

"Oi-Ammonium Perfluorobutane sulfonate ["02]PFBS IS for PFBS RTI International 

(Individual) 

"Cs-Ammonium Perfluorohexane sulfonate [1,2,3-"C3]PFHS IS for PFHS 

Wellington Labs 

(Mix or Individual) 

"Cs-Sodium Perfluorooctane sulfonate [l,2,3,4,5,6,7,8-"C8]PFOS IS for PFOS and 

PFOS[l,2,3,4 "C4], 

Wellington Labs 

(Mix or Individual) 

''Cs-Perfluorooctanesulfonamide [l,2,3,4,5,6,7,8-"C8]FOSA IS for FOSA 

Wellington Labs (mix) 

RTI International 

(Individual) 

"C4-Perfluorooctanoic acid [l,2,3,4-"C4]PFOA SRS for all PFCAs: C4-C8 Wellington 

"Cj-Perfluoroundecanoic acid [l,2-"C2]PFUnA SRS for all PFCAs C9-C13 Wellington 

"Cg-Perfluorooctane sulfonate [1,2,3,4-"C4]PFOS SRS for all PFSAs: C4, 

C6, and C8 Wellington 

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Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Table 2. Example Preparation of Calibration Curve with ISs and SRSs 

Sample Description Concentration 

ofWS.tig/mL 

Volume of 

WS.fd. 

Volume of IS 

(2 i/g/mL), fd. 

Concentration of 

Surrogate, fig/mL 

Volume of 

Surrogate, id. 

Volume of ASTM Type 1 Water, or 

other suitable solvent mL 

0.025 ng/mL curve point 0.10 25 50 0.20 12.5 100 

0.030 ng/mL curve point 0.10 30 50 0.20 15 100 

0.04 ng/mL curve point 0.10 40 50 0.20 20 100 

0.05 ng/mL curve point 0.10 50 50 0.20 25 100 

0.1 ng/mL curve point 0.10 100 50 0.20 50 100 

0.25 ng/mL curve point 0.10 250 50 0.20 125 100 

0.5 ng/mL curve point 1.0 50 50 0.20 250 100 

1 ng/mL curve point 1.0 100 50 0.20 500 100 

2.5 ng/mL curve point 10.0 25 50 10.0 25 100 

5.0 ng/mL curve point 10.0 50 50 10.0 50 100 

10.0 ng/mL curve point 10.0 100 50 10.0 100 100 

25.0 ng/mL curve point 10.0 250 50 10.0 NA 100 

50.0 ng/mL curve point 10.0 500 50 10.0 NA 100 

75.0 ng/mL curve point 10.0 750 50 10.0 NA 100 

100 ng/mL curve point 10.0 1000 50 10.0 NA 100 

N/A - Not Applicable 

(1) Samples requiring analysis for PFUnA, PFDoA, PFTrDA, and FOSA should be analyzed against a calibration curve prepared in 1:1 synthetic groundvrater:MeOH. 

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8 Sample Collection and Bottle Preparation 

Sample collection bottles are prepared by 3M Environmental Laboratory (or subcontract supplier) personnel for 

shipment at ambient temperature to the collection site. Typically, four separate collection bottles are 

associated with a single collection site: sample, field duplicate sample, low field matrix spike, and high field 

matrix spike. Altematively, the sample and field duplicate sample may contain SRSs in lieu of additional target 

analyte low field matrix spike and target analyte high field matrix spike samples. Depending on the scope of 

the project, additional replicates of the field sample and field matrix spikes may be added. Also, it is not 

uncommon for additional mid-level field matrix spikes to be collected if the expected sample concentrations are 

tnjiy unknown or could span a large concentrafion range. 

High-density polyethylene (HDPE) wide-mouth Nalgene bottles are used for the sample collection containers. 

(Volumes of the bottles may vary depending on how much sample is required to meet data quality objectives.) 

Sample collection volumes are project specific and based on data quality objectives. The Nalgene bottles do 

not require any pretreatment prior to use. Typically, placement of a sample bottle volumetric "fill to here" line is 

done by using a sample bottle marker template. Alternatively, bottles may be weighed prior to bottle 

preparation and weighed again after samples have been collected. 

All bottles should be cleariy labeled to indicate its intended use as a sample, field sample duplicate, low field 

matrix spike, high field matrix spike, sample/SRS field matrix spike, field duplicate sample/SRS field matrix 

spike, trip blank, or trip blank matrix spike. If each location has different designated spike levels, the label 

should also cleariy indicate the sample location designation. Generally, a set of bottles for a given collection 

site are prepared then grouped together in plastic bags for organizational purposes. For each sample 

collection event, at least one set of trip blank and trip blank matrix spikes are prepared. 

Bottle preparation should be documented in a Note to File or on a sample preparation worksheet and should 

include the following infonnation: date prepared, total number of bottles prepared, number of sample sites, the 

standard identification numbers and spike volumes used to prepare spiked bottles, the "fill to here" volume, and 

any other pertinent infomriafion needed for reconstnjctibility of the data. The Note to File will be included in the 

final data package for the project. 

Samples are collected in the field and shipped to the laboratory at ambient temperature. 

8.1 Field Matrix Spike Sample (FMS) 

Field matrix spike samples are a requirement of the method. A FMS sample is defined as a QC sample to 

which known quantities of appropriate target analytes are added to the sample bottle in the field or in the 

laboratory before the bottles are sent to the field. The sample and field duplicate sample may contain 

appropriate SRSs in lieu of target analyte FMS samples. Sample quantities are determined volumetrically or 

gravimetrically. A known, specific volume or weight of sample is added to the sample container without 

rinsing. Volumetric sample measurements may be acquired by a laboratory applied "fill to this level" line on the 

outside of the sample container. Target analyte FMS samples should be spiked at approximately 0.5-10 times 

the expected analyte concentration in the sample. If the expected range of analyte concentrations is unknown, 

multiple spikes at varying levels may be prepared to increase the likelihood that a spike at an appropriate level 

is made. Typically a low and a high target analyte spike are prepared for each sampling location. In those 

instances where SRSs are to be used in lieu of target analyte FMS samples, the sample and field duplicate 

sample are spiked at approximately 2-5 times the target LOQ. The FMS is analyzed to ascertain if matrix 

effects or sample holding time contributes bias to the analytical results. For the sample bottles designated for 

matrix spikes, an appropriate volume of matrix spiking solution is added to the empty bottle prior to sampling. 

The volume of spike solution added should produce the desired final concentration of target analytes once the 

bottle is filled with sample to the "fill to here line". The matrix spiking solution(s) should be prepared in a 

suitable solvent and contain all of the appropriate target analytes, ISs, and SRSs. The target analyte matrix 

spiking solution is often the same as the working standards used to create the calibration standards. An 

example of a bottle spike is given below. 

"Fill to here" volume = 200 mL (A 250 mL Nalgene bottle is used) 

Desired Field Spike Concentrafion = 0.25 ng/mL 

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Decatur, AL - December 2011 

500 nL of a 0.1 ng/mL spiking solution (containing the target analytes) is added to the bottle and the bottle cap 

promptly sealed. 

8.2 Internal Standard and Surrogate Recovery Standard 

If analysis of a sun-ogate recovery standard (SRS) is included in the project objectives, an appropriate volume 

of a surrogate standard solution is added to all the bottles prior to sampling and SPE. Typically sample bottles 

are spiked with surrogate recovery standards at a final desired spike concentration of 0.1 ng/mL. 

If quantitation by intemal standard (IS) is included in the project objective, an appropriate volume of internal 

standard solution is added to all the bottles prior to sampling and SPE. Typically sample bottles are spiked 

with internal standard at a final desired spike concentration of 1 ng/mL. 

For the trip blank, the SRS spike and IS spike is added to the bottle and then ASTM Type I water (HPLC grade 

reagent water or other suitable water may used) is added to the "fill to here" line. The bottle is capped and 

sealing tape may be placed around the outer edge of the cap. Trip blank matrix spikes are prepared by adding 

the appropriate volume of target analyte spiking solution, IS, and SRS spiking solutions and filling the bottle to 

the desired volume with the appropriate water and capping and sealing the cap. 

9 Quality Control and Data Quality Objectives 

9.1 Data Quality Objectives 

This method and required quality control samples is designed to generate data accurate to ±30% with a 

targeted LOQ of 0.025 ng/mL. Any deviations from the quality control measures spelled out below will be 

documented in the raw data and footnoted in the final report. 

9.2 Method/Procedural Blanks 

The method/procedural blank is zero point calibration standard (which includes ISs) analyzed in a regular basis 

with each analysis batch. At a minimum, method blanks are analyzed prior to instalment calibration, prior to 

the analysis of CCV samples, after every 10 sample injections, and at the end of the analytical mn. 

The mean area count or area ratios when using intemal standard calibrafion, for each analyte in the method 

blanks must be less than 50% of the area count counts or area ratios when using internal standard calibration, 

of the LOQ standard. The standard deviation of the area counts, or area ratios when using intemal standard 

calibration, of these method blanks should be calculated. A specific %RSD acceptance criteria is not specified 

but is assessed on an analytical batch basis. If the mean area counts or area ratios when using intemal 

standard calibration, of the method blanks exceed 50% of the LOQ standard, then the LOQ must be raised to 

the first standard level in the curve that meets criteria. Method blanks may be eliminated if technical 

justification can be provided (e.g. the procedural blank was analyzed after an unexpectedly high level sample). 

If any procedural blanks are removed from the LOQ detemninafion, document in the raw data and report as 

appropriate. Laboratory Sample Replicates / Field Duplicate Sample 

Typically, samples are collected in duplicates in the field. The relative percent difference (RPD) of duplicate 

samples should be ^20% for the precision of sample preparafion and analysis to be considered in control. 

Replicate samples not meeting the <20% RPD criteria are flagged and reported as outside of QC acceptance 

criteria. 

9.3 Laboratory Matrix Spikes (LMSs) 

LMSs may be performed in lieu of FMSs if FMSs have previously been perfonned for the sample matrix. 

Additionally, LMSs may be perfonned in lieu of FMSs for a sample matrix if the FMS levels were not 

appropriate for detemnining spike recoveries relative to endogenous levels of target analytes and appropriate 

SRSs. Generally, each sample location represents a different sample and sample matrix. LMSs are prepared 

for each sample and analyzed to detennine the matrix effect on spike recovery efficiency of each target analyte 

and appropriate SRSs. LMSs should be prepared at a minimum of one level and in duplicate. LMS 

concentrations should be prepared at approximately 0.5-10 times the endogenous concentration or 

approximately 4-10 times the LOQ concentration of each target analyte. 

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Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

Lab matrix spike recoveries should fall within ± 30% of expected values. Sample data with LMS recovery 

outside of ±30% but within ±50% of the expected value are fiagged and reported as outside of QC acceptance 

criteria. Data with LMS recovery outside of ±50% of the expected value are reported as NR, where NR is 

defined as "Not Reportable" data outside of QC acceptance criteria. 

9.4 Lab Control Sample 

Lab control spikes are prepared for each analysis batch to detennine method accuracy and precision. LCSs 

should be prepared at three levels in triplicate for each target analyte and at a minimum of two levels in 

triplicate for appropriate SRSs. Low lab control spikes should be prepared at a concentrafion in the range of 

approximately ifour to ten times higher than the targeted lower LOQ, the mid lab control spikes should be 

prepared at a concentration near the mid-point of the calibration curve and the high lab control spikes at 

approximately 80% of the upper LOQ. For each target analyte and SRSs, the percent relative standard 

deviation (method precision) for each control spike level must be less than or equal to 20% and the average 

recovery (method accuracy) for each control spike level must be 80-120%. Sample data for target analytes 

outside of the laboratory control spike acceptance criteria will be handled as follows: 

If the average recovery of a spiking level falls outside method acceptance, but at least 67% (6 out of 9) of LCS 

samples are within 20% of their respective nominal value (33% of the QC samples, not all replicates at the 

same concentration, may be outside 20% of nominal value), the average recovery will be fiagged as outside 

method acceptance criteria. All LCS samples will be control charted as per ETS-4-026. If the average 

recovery of one of the spiking levels exceeded the analytical method uncertainty as determined by ETS-12-

012, that analytical batch uncertainty will be expanded for that particular study. 

If more than 67% of the LCS samples fail to meet method acceptance criteria, the data will not be reported. 

Calibration standards consisting of mixed branched and linear isomer PFOS/PFOA are preferred. However, 

for PFOS/PFOA target analytes, if the calibration standards are comprised of predominantly linear isomers 

only, at least one level of triplicate LCSs should be prepared using PFOS/PFOA which contains a mix of linear 

and branched isomers. These LCSs will be used to demonstrate quantitative equivalency (or quantitative bias) 

of the isomeric mix when using a predominantly linear standard for calibration. The mixed linear and branched 

isomer PFOS/PFOA LCSs recoveries should fall within ± 30% of expected values. Alternatively, in lieu of 

mixed branched and linear isomer PFOS/PFOA LCSs, mixed branched and linear isomer PFOS/PFOA 

TBMSs may be applied to demonstrate method accuracy and precision. 

9.5 Field Matrix Spikes (FMSs) / Surrogate Recovery Standards (SRSs) 

FMSs are prepared for each sampling location and analyzed to determine the matrix effect and sample holding 

time on the spike recovery of each target analyte and/or appropriate SRS. Generally, each sample location 

represents a different sample and sample matrix. 

FMSs are QC samples to which known quantities of appropriate target analytes are added to the sample bottle 

in the laboratory before the bottles are sent to the field. Typically a low and a high target analyte FMS are 

prepared for each sampling locafion. The sample and field duplicate sample may contain appropriate SRSs in 

lieu of target analyte low field matrix spike and target analyte high field matrix spike samples. 

Field matrix spike method acceptance criteria are recoveries within ±30% of the expected value. If FMS 

recovery (target analyte or SRS spike) is outside of ±30% of the expected value or could not be assessed 

because the FMS (target analyte) was spiked at an inappropriate level, the sample result is reported as follows: 

1. ) If target analyte FMS recovery could not be assessed because the FMS's were at an inappropriate level, 

then Laboratory Matrix Spikes (LMS) may be substituted. If LMS recoveries are within ±30% the data are 

reportable and flagged to indicate that the FMS spikes levels were inappropriate. 

2. ) If multiple target analyte FMS's were prepared on a sample and the closest FMS level to the reported 

sample meets the ±30% acceptance criteria but additional FMS's are outside the ±30% acceptance range, the 

data are reportable and flagged to indicate that while there were failing FMS's, the uncertainty will not be 

expanded since the most appropriate spike level passed. 

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Analysis of PFBS, PFHS, and PFOS in Groundwater 

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3. ) If the target analyte FMS recoveries are outside of the ±30% acceptance range but at least 30 acceptable 

historical reportable FMS sample results are available, the data may be reported but flagged with an expanded 

uncertainty and as not meeting FMS criteria. 

4. ) Sample data with FMS recovery outside of ±30% but within ±50% of the expected value are flagged and 

reported as outside of QC acceptance criteria with an expanded uncertainty. 

5. ) If FMS recovery is outside of ±50%, the sample result is reported as NR, where NR is defined as "Not 

Reportable" due to noncompliant QC results. 

The targeted fortification levels should be at least 50% of the endogenous level and less than 10 times the 

endogenous level to be used without justification to determine the statement of accuracy for analytical results. 

Note: It is possible for bottles utilized for Field Matrix Spike samples to be under-filled or over-filled during 

sample collection. Since this scenario will effect the actual concentrafion of the FMS sample (sun-ogate and 

intemal standard concentrations will also be effected, if used), it is important that any obvious under-filling or 

over-filling of sample bottles be documented in the data package and taken into account in the FMS, ISs, or 

SRSs recovery calculations. Samples over-filled or under-filled by more than 10% will be require recalculation 

of the FMS, ISs, and SRS true values. 

The average of the sample and the field duplicate should be used to calculate the recovery. 

10 Procedures 

10.1 Water Sample Preparation 

This method is applicable to water samples. Samples containing heavy particulate may not be suitable for 

analysis by this method. Samples containing suspended particulate should be centrifuge prior to removing a 

sample aliquot, or filtered. 

• Thoroughly mix sample before removing an aliquot and placing in a labeled autovial. 

• Dilute sample, if necessary, with ASTM Type I water, HPLC water, other suitable water, or solvent 

(methanol). 

• Lab control spikes are prepared for each analysis batch to detennine method accuracy and precision. 

LCSs should be prepared at three levels in triplicate for each target analyte and at a minimum of two 

levels in triplicate for appropriate SRSs. Low lab control spikes should be prepared at a concentrafion 

in the range of approximately four to ten times higher than the targeted lower LOQ, the mid lab control 

spikes should be prepared at a concentration near the mid-point of the calibration curve and the high 

lab control spikes at approximately 80% of the upper LOQ. For IS quantitation, stable isotope internal 

standards of each target analyte or appropriate sun'ogate ISs should be spiked at the same level as the 

samples being analyzed, in all LCSs. 

• If LCSs are being prepared using synthetic groundwater, allow the LCSs samples to equilibrate for a 

minimum of 4 hours before aliquoting for analysis or diluting with solvent (methanol). 

11 Sample Analysis - LC/MS/MS 

11.1 Instrument Setup 

Note: In this example, an Applied Biosystems Sciex API 4000 (API 5000 or API 5500) Tandem Mass 

Spectrometer (LC/MS/MS) is used. Other brands/models of LC/MS/MS instruments as well as single 

quadrupole mass spectrometers (LC/MS) may be used as long as the method acceptance criteria are met. 

Brand names, suppliers, part numbers, and models are for illustrative purposes only. Equivalent perfonnance 

may be achieved using apparatus and materials other than those specified here, but demonstration of 

equivalent perfonnance that meets the requirements of this method is the responsibility of the laboratory. The 

operator must optimize and document the equipment and settings used. 

ETS-8-044.1 Page 15 of 22 

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Decatur, AL - December 2011 

Establish the LC/MS/MS system and operating conditions equivalent to the following: 

Mass Spec: Applied Biosystems API 4000, API 5000, or API 5500 

Ion Source: Turbo Ion Spray (ABS) 

Mode: Electrospray Negative 

Scan Type: MRM (Multiple Reaction Monitoring) 

Computer: Dell DHM 

Software: Windows 2000 or Windows XP, Analyst 1.4.2 or higher versions 

HPLC: Agilent Series 1100,1200, or 1290 

Agilent Quaternary Pump 

Agilent Vacuum Degasser 

Agilent Autosampler 

Agilent Column Oven 

Note: One or more C18 HPLC analytical columns (2.1 mm x 100 mm, 5|am or 2.1 mm x 50 mm, 5nm) may be 

attached on-line after the purge valve and before the sample injection port to retard and separate any residue 

contaminants that may be in the mobile phase and/or HPLC system. 

HPLC Column: Betasil C18,4.6mm x 100mm, 5(xm (ThermoElectron Corporafion) 

Column Temperature: 35°C 

Injection Volume: 5pL 

Mobile Phase (A): 2mM Ammonium Acetate in ASTM Type I water (See 7.3) 

Mobile Phase (B): Methanol 

Table 3. Liquid Chromatography Gradient Program. 

Step 

Number 

Total Time 

(min) 

0 

Flow Rate 

(fiUmin) 

Percent A 

(2 mM ammonium 

acetate) 

Percent B 

(Methanol) 

0 

Total Time 

(min) 

0 750 97.0 3.0 

1 2.0 750 97.0 3.0 

2 14.5 750 5.0 95.0 

3 15.5 750 5.0 95.0 

4 16.5 750 97.0 3.0 

5 20.0 750 97.0 3.0 

Note: Other HPLC gradients may be used as long as the method criteria and project data quality objectives are 

met. 

It may be necessary to adjust the HPLC gradient in order to optimize instrument perfonnance. Columns with 

different dimensions (e.g. 2.1mm x 30mm) and columns from different manufacturers (Keystone Betasil C18 

etc.) may be used. 

ETS-8-044.1 Page 16 of 22 

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Analysis 

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Table 4 Suggested MRM Transitions for Target Analytes, Surrogates, and Internal Standards 

Analyte 

Analyte Description Mass Transition 

01 (amu) 

Mass Transition 

03 (amu) 

PFBA (C4 Acid) Target 213 169 

PFPeA (C5 Acid) Target 263 219 

PFHxA (C6 Acid) Target 313 269, 119 

PFHpA (C7 Acid) Target 363 319, 169 

PFOA (C8 Acid) Target 413 369,219,169 

PFNA (C9 Acid) Target 

463 419, 169,219 

PFDA (CIO Acid) Target 513 469,269,219 

PFUnA (C11 Acid) Target 563 519,269,219 

PFDoA (C12 Acid) Target 613 569, 169,319 

PFTA(C13 Acid) Target 663 619, 369,319 

FBSA (C4 Sulfonamide) Target 298 78 

FOSA (C8 Sulfonamide) Target 498 78 

PFBS (C4 Sulfonate) Target 299 99, 80 

PFHS (C6 Sulfonate) Target 399 99, 80 

PFOS (C8 Sulfonate) Target 499 80,99, 130 

[1,2,3,4 -"C4IPFBA IS for PFBA 217 172 

[1,2,3,4,5-"CslPFPeA IS for PFPeA 268 223 

[l,2-"C2lPFHxA IS for PFHxA 315 270 

[1,2,3,4- "C4IPFHPA IS for PFHpA 367 322 

[l,2,3,4,5,6,7,8-"C8lPFOA IS for PFOA 421 376 

[1,2,3,4,5,6,7,8,9-"C9IPFNA IS for PFNA 472 427 

[1,2,3,4,5,6-"CslPFDA IS for PFDA 519 474 

[1,2,3,4,5,6,7-"ClPFUnA IS for PFUnA 570 525 

[l,2-"C2lPFDoA IS for PFDoA and PFTA 615 570 

["O2IPFBS IS for PFBS 303 84 

[l,2,3-"C3lPFHS IS for PFHS 402 80 

[1,2,3,4- "C4IPFOS IS for PFOS 503 80 

[l,2,3,4,5,6,7,8-"C8lFOSA IS for FOSA 507 80 

[l,2,3,4-"C4lPFOA Surrogate (C4-C8 Acids) 417 372 

[1,2,3,4- "C4]PFOS Surrogate(Sulfonates, FOSA) 503 80 

[l,2-"C2lPFUnA Surrogate (C9-C13 Acids) 565 520 

Multiple transitions for monitoring the analytes is an option. The use of one daughter ion is acceptable if data 

sensitivity and selectivity is achieved and provided that retention time criteria are met to assure adequate 

specificity. While the daughter ions may be chosen at the discrefion of the analyst, mass transition 99 is 

suggested for PFOS. Quantitation may be perfonned using the total ion chromatogram (TIC, or summed 

MRMs) for a given analyte. For example, the PFOA TIC would sum all three of the monitored transitions. Use 

of the suggested primary ion is recommended. Retention times may vary slightly, on a day-to-day basis, 

depending on the batch of mobile phase and the gradient, column, guard column(s) used etc. Drift in retention 

fimes is acceptable within an analytical run, as long as the drift continues through the entire analysis and the 

standards are interspersed throughout the analytical run. 

11.2 Calibration Curve 

Quantitation is by intemal standard or extemal standard calibration. Calibration standards may be prepared in 

ASTM Type 1, HPLC water, other suitable water, or a solvent/water mixture. If intemal standard calibration 

does not meet calibration acceptance criteria, extemal calibration can be applied. See Table 1 for 

ETS-8-044.1 Page 17 of 22 

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Analysis of PFBS, PFHS, and PFOS in Groundwater 

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recommended applicafion of available intemal standards. Quantitation of PFOA and PFOS is by summed 

analyte-specific mass transitions. 

Analyze the standard curve prior to each set of samples. If intemal standards were added to the calibration 

standards area ratios are used to generate the calibration curve. The standard curve may be plotted using a 

linear regression (y = mx + b), weighted 1/x or unweighted, or by quadratic fit (y = ax^ + bx + c), weighted 1/x or 

unweighted, using suitable software. The mathematical method used to calculate the calibration curve should 

be applied consistently throughout a study. Any change should be thoroughly documented in the raw data. 

High and/or low points may be excluded from the calibrafion curves to provide a better fit over the range 

appropriate to the data or because they did not meet the pre-determined acceptance criteria. Low-level curve 

points should also be excluded if their area counts (or area rafio if quantitating by IS) are not at least twice that 

of the average area counts (or area ratio if quantitating by IS) of method and/or solvent blanks. The coefficient 

of determination (r^) value for the calibration curve must be greater than or equal to 0.990 (or a con-elation 

coefficient (r) of 0.995). Each point in the curve must be within ±25% of the theoretical concentration with the 

exception of the LLOQ, which may be within ±30%. Justification for exclusion of calibration curve points will be 

noted in the raw data. A minimum of 6 points will be used to construct the calibration curve. 

If the calibration curve does not meet acceptance criteria, perform routine maintenance or prepare a new 

standard curve (if necessary) and reanalyze. 

11.3 Continuing Calibration Verification (CCV) 

Continuing calibration verifications (CCV) are analyzed to verify the accuracy of the calibration curve. Analyze 

a mid-range calibration standard, one of the same standards used to construct the calibration curve, at a 

minimijm after every tenth sample, not including solvent blanks, with a minimum of one per sample set. 

Calibration verification injections must be within ±25% to be considered acceptable. The calibration curve and 

the last passing CCV will then bracket acceptable samples. Multiple CCV levels may be used. Samples must 

be bracketed by passing CCVs or the calibration curve and a passing CCV to be reportable. 

11.4 System Suitability 

A minimum of three system suitability samples should be injected at the beginning of each analytical njn, prior 

to the analysis of the calibration curve. Typically these samples are at a concentration near the mid-level of the 

calibration curve and are repeated injections from one autosampler vial. It is suggested that the system 

suitability injections have area counts or area ratios when using internal standard calibration, with a target RSD 

of <5% and a target retention time RSD of <2%. There is no defined acceptability limit on these results as the 

%RSD value is dependent on the number of MRM transitions being monitored in the LC/MS/MS run or time 

period. Ultimately, any effects on these parameters for the System Suitability samples will also be evident on 

all standards and QC samples analyzed as part of the analysis batch. Any effect of system suitability is 

incorporated within QC acceptance criteria. 

11.5 Sample Analysis and QC s 

For each analysis batch, the instrument analysis run sequence should include an initial calibration curve, 

samples, FDSs, interspersed blanks, interspersed CCVs, appropriate QCs (i.e., LCSs, LMSs, FMSs, TBMSs, 

and TBs), and a final CCV or calibration curve bracketing samples and appropriate QCs 

Inject the same volume (between 5 -10OpL) of each standard, analytical sample and blank into the instrument 

(unless an on-instmment sample dilution is desired). 

Samples containing analytes that are quantitated above the concentration of the highest standard in the curve 

should be further diluted and reanalyzed. 

' 3M Environmental Laboratory study E08-0096 evaluated the effect on these results as a function of the number of MRMs being monitored. 

ETS-8-044.1 Page 18 of 22 

Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection 

Analysis 

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Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

12 Data Analysis and Calculations 

The chromatography analysis software will typically calculate the amount of target analyte in the sample 

extracts using the established calibration curve. 

Calculate the percent recovery of the LCS using the following equation: 

LCS Concentration {—) 

LCS% recovery = ISi ^ * 100% 

ng 

Spike Concentration (—^) 

mL 

Calculate the percent recovery of the LMS using the following equation: 

LMS Concentration {-^) - Concentration of Sample (-^) 

LMS % recovery = * 100% 

Spike Concentration (-2S-) 

mL 

For samples fortified with known amounts of analyte prior to extraction, use the following equation to calculate 

the percent recovery. 

Recovery - analyte found (ng/mL) - Average analyte found in sample (ng/mL) ^ ^ 

Analyte added (ng/mL) 

13 Analysis Batch Method Performance Criteria 

Any method perfonnance parameters that are not achieved must be considered in the evaluation of the data. 

Nonconfonnance to any specified parameters must be described and discussed in the final report if the 

Technical Manager (non-GLP study) or Study Director (GLP study) chooses to report the data. 

If criteria listed in this method perfonnance section are not met, maintenance may be perfonned on the system 

and samples reanalyzed, or other actions taken as appropriate. Document all actions in the raw data. 

If data are to be reported when perfonnance criteria have not been met, the data must be footnoted on tables 

and discussed in the text of the report. 

13.1 System Suitability - Analysis Batch 

A minimum of three system suitability samples should be injected at the beginning of each analytical run. 

These samples are run prior to the calibration curve. It is suggested that the system suitability injections have 

area counts with a target RSD of S5% and a target retention time RSD of 22%. There is no defined 

acceptability limit on these results as the %RSDs are dependent on the number of MRM transitions being 

monitored in the LC/MS/MS run or time period. Any effect of system suitability is incorporated in the QC 

acceptance criteria. 

13.2 Calibration and Limit of Quantitation (LOQ) - Analysis Batch 

Calibration Curve: The coefficient of detennination (r^) value for the calibration curve must be greater than or 

equal to 0.990 con-esponding to a correlation coefficient (r) = 0.995. Each point in the curve must be within 

+25% of the theoretical concentration with the exception of the LLOQ, which may be within ±30%. 

CCV Performance: The calibration standards that are interspersed throughout the analytical sequence are 

evaluated as continuing calibration verifications in addition to being part of the calibration curve. The accuracy 

ETS-8-044.1 Page 19 of 22 

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Analysis 

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Decatur, AL - December 2011 

of each curve point must be within 25% of the theoretical value (within 30% for lowest curve point). Samples 

that are bracketed by CCVs not meeting these criteria must be reanalyzed. 

Limits of Quantitation (LOQ): The lower LOQ (LLOQ) is the lowest non-zero active standard in the 

calibration curve; the peak area of the LLOQ must be at least 2X that of the average area counts for all 

prepared procedural blank(s). By definition, the measured value of the LLOQ must be within 30% of the 

theoretical value. 

Demonstration of Specificity: Specificity is demonstrated by chromatographic retention time (within 4% of 

standard) and the mass spectral response of unique ions. 

13.3 Blanks - Method/Procedural Blanks and Trip 

Method/Procedural Blanks: Multiple procedural blanks should be interspersed throughout the analysis batch 

and the analytical sequence. At a minimum, method blanks are analyzed prior to instalment calibration, prior 

to the analysis of CCV samples, after every 10 sample injections, and at the end of the analytical run. 

The mean area counts (or area ratios when using IS calibration) for each analyte must be less than 50% of the 

area count of the LOQ standard. If the area counts of the procedural blanks exceed 50% of the LOQ standard, 

then the LOQ must be raised to the first standard level that meets criteria. 

Trip Blanic A trip blank of ASTM Type I water (or lab equivalent) is prepared in a sample container in the 

laboratory and treated as a sample, including exposure to shipping, sampling site conditions, storage, 

preservation and all analytical procedures. The trip blanks results for each analyte are included with the 

reported sample results. 

13.4 Data Accuracy and Precision - Analysis Batch 

Lab Control Spil^es: The average recovery at each LCS level for each target analyte and appropriate SRS 

should be within 80-120% and the percent relative standard deviation of the recoveries must be less than or 

equal to 20%. If the average recovery of a spiking level falls outside method acceptance, but at least 67% (6 

out of 9) of LCS samples are within 20% of their respective nominal value (33% of the QC samples, not all 

replicates at the same concentration, may be outside 20% of nominal value), the average recovery will be 

flagged as outside method acceptance criteria. All LCS samples will be control charted as per ETS-12-012. If 

the average recovery of one of the spiking levels exceeded the analytical method uncertainty as determined by 

ETS-12-012, that analytical batch uncertainty will be expanded for that particular study. The average recovery 

at each LCS level for mixed branched/linear isomer PFOA and PFOS should be within 70-130% and the 

percent relative standard deviation of the recoveries must be less than or equal to 20%. 

Field Duplicates: The relative percent difference (RPD) of duplicate samples should be less than 20% for the 

precision of sample preparation and analysis to be considered in control. Replicate samples not meeting the 

20% RPD criteria are flagged and reported as outside of QC acceptance criteria. 

Field IVIatrix Splices: FMS acceptance criteria are recoveries within ±30% of the expected value for each 

target analyte and appropriate SRS. Sample data with FMS recovery outside of ±30% but within ±50% of the 

expected value are flagged and reported as outside of QC acceptance criteria. Data with FMS recovery 

outside of ±50% of the expected value are reported as NR, where NR is deflned as "Not Reportable" data 

outside of QC acceptance criteria. If FMS recovery could not be assessed because FMSs were at an 

inappropriate level, then Laboratory Matrix Spikes (LMSs) may be substituted. If LMS recoveries are within 

±30% for each target analyte and SRSs the data are reportable but flagged as not meeting the FMS method 

acceptance criteria. 

13.5 Analytical Method Uncertainty 

Analytical method uncertainty for each target analyte and SRS is detennined with control charted historical 

analysis batch LCS data for the method and reported with each analysis batch.^ Uncertainty detenninations 

' Method uncertainty based on INTERNATIONAL ANS/ISO/IED STANDARD 17025 reference (GUM, Guide to the Expression of 

Uncertainty in Measurement). Method application demonstrated in ETS-12-012, citing references: a.) EURACHEM/CITAC Guide, 

"Quantifying Uncertainty in Analytical Measurement," Second Edition; Editors: S.L.R. Ellison, M. Rosslein, and A. Williams. 

b.)Georgian, Thomas, "Estimation of Laboratory Analytical Uncertainty Using Laboratory Control Samples," Environmental Testing & 

ETS-8-044.1 Page 20 of 22 

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Analysis 

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are based on INTERNATIONAL ANS/ISO/IED STANDARD 17025 reference (GUM, Guide to the Expression 

of Uncertainty in Measurement) and described in ETS-12-012. At least thirty data points are required for 

determining analytical method uncertainty. The method uncertainty is defined as 2x the standard deviation of 

the percent recoveries of the pooled lab control spikes. While all LCS data points are control charted, only the 

most recent fifty data points are used for detemnining the method uncertainty. 

When less than thirty LCS data points have been generated for a given analyte, the analysis batch LCSs are 

used to detennine the data uncertainty. If FMSs meet the ±30% recovery criteria at a level appropriate to the 

endogenous level, and the LCS meet the ±20% recovery criteria, then the uncertainty of the data is detennined 

as within 100±20%. 

Analysis batch sample data with FMS recovery outside of ±30% but within ±50% of the expected value are 

fiagged and reported as outside of QC acceptance criteria with expanded uncertainties. Data with FMS 

recovery outside of ±50% of the expected value are reported as NR, where NR is defined as "Not Reportable" 

data outside of QC acceptance criteria. If FMS recovery could not be assessed because FMSs were at an 

inappropriate level, then Laboratory Matrix Spikes (LMSs) may be substituted. If LMS recoveries are within 

±30% for each target analyte and appropriate SRSs the data are reportable but flagged as not meeting the 

FMS method acceptance criteria with uncertainties of ±30%. If FMS do not meet the ±30% recovery criteria, 

and historical FMS data does not exist, the analytical uncertainty is evaluated on a sample-by-sample basis, 

the data may be reported with expanded uncertainty and are flagged. 

13.6 Quantitation of PFOA/PFOS - Analysis Batch 

Calibration standards consisting of mixed branched and linear isomer PFOS/PFOA are preferred. 

Quantitation is perfonned by integrating the linear and branched isomers together. Alternately, the linear and 

branched isomers can be integrated separately, applying the appropriate taie value to each calibration curve 

point for each isomer. The LCS and samples are then quantitated by integrating the linear and branched 

isomers separately (requires separate analytical results files) and quantitating the resulting peak against the 

linear or branched calibration curve. The results from both integrations are then summed to produce the final 

result. Integrating the linear and branched isomers separately may be helpful for those samples where the 

linear/branched ratios do not closely match those of the reference standards. 

However, for PFOS/PFOA target analytes, if the calibration standards are comprised of predominantly linear 

isomers only the method requires the addition of LCSs of mixed branched/linear isomer PFOS/PFOA. The 

purpose of including these LCSs is to demonstrate quantitative equivalency (or quantitative bias) of the 

isomeric mix when using a predominantly linear PFOS or PFOA standard for calibration. Altematively, in lieu 

of mixed branched and linear isomer PFOS/PFOA LCSs, mixed branched and linear isomer PFOS/PFOA 

TBMSs may be applied to demonstrate method accuracy and precision. 

An alternate method of quantitation can be perfonned whereby only the linear isomer of PFOS/PFOA is 

integrated and used for generating the calibration curve. The LCS and samples are then quantitated by 

integrating the linear and branched isomers separately (requires separate analytical results files) and 

quantitating the resulting peak against the linear calibration curve. The results from both integrations are then 

summed to produce the final result. Integrating the linear and branched isomers separately reduces the oncolumn concentration for those samples that contain both linear and branched isomers of PFOA/PFOS. This 

ensures that the concentration detected is within the a range of the calibration curve that is comparable 

regardless of whether the calibration curve was generated using predominantly linear isomers of PFOS/PFOA 

or linear plus branched isomers of PFOS/PFOA. 

14 Pollution Prevention and Waste IVIanagement 

Waste generated when perfonning this method will be disposed of appropriately. The original samples will be 

archived at the 3M Environmental Laboratory in accordance with internal procedures. 

Analysis, November/December 2000. c.)Taylor, B.N. and CE. Kuyatt, NIST Technical Note 1297, 1994 Edition: "Guidelines for 

Evaluating and Expressing the Uncertainty of NIST Measurement Resuhs."d.)Adams, T.M., "A2LA Guide for the Estimation of 

Measurement Uncertainty in Testing", July 2002. 

ETS-8-044.1 Page 21 Of 22 

Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection 

Analysis 

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Decatur, AL - December 2011 

15 Records 

Each data package generated for a study must include all supporting infonnation for reconstmction of the data. 

Infonnation for the data package must include, but is not limited to the following items: study or project 

number, sample and standard prep sheets/records, instrument mn log (instrument batch records, instalment 

acquisition method, summary pages), instrument results files, chromatograms, calibration curves, and data 

calculations. 

16 Affected Documents 

None. 

17 Revisions 

Revision 

Number Summarv of Changes 

1 Section 1. Included the use of internal standard calibration by this method. 

Section 2. Included the use of internal standard calibration by this method. Included the 

use of a solvent/water mixture when analyzing for PFUnA, PFDoA, PFTrDA, and FOSA. 

Section 3. Added definitions for internal standard, surrogate internal standard, and 

surrogate recovery standard. 

Section 6. Removed the details regarding the instrument parameters to section 10 of the 

method. 

Section 7. Updated reference standards to include intemal standards and surrogates. 

Changed concentration levels for working standards and included the use of internal 

standards and surrogates. 

Section 8. Inserted a new section on sample bottle preparation. 

Section 9 Quality Control. This section was previously section 10 in ETS-8-044.0. Updated 

QC criteria to be consistent with method ETS-8-154.4. 

Section 10 Procedures. This section was previously section 8 (Sample Handling) in ETS-8-

044.0. Added detail regarding the preparation of LCSs. Included the use of methanol as a 

dilution solvent. 

Section 11 Sample Analysis. This section was previously section 10 in ETS-8-044.0. 

Included the details regarding the instrument parameters. 

Section 12 Data Analysis and Calculations. This section was previously section 11 in ETS8-044.0. Removed the equation for calculating the analytes concentration, indicating that 

this is done by the instrument software. 

Section 13 Method Performance. This section was previously section 12 in ETS-8-044.0. 

Updated QC criteria to be consistent with ETS-8-154.4. Added information on the 

determination of analytical method uncertainty and quantitation of PFO/VPFOS. 

Section 14 Pollution Prevention. This section was previously section 13 in ETS-8-044.0. 

Section 15 Records. This section was previously section 14 in ETS-8-044.0. 

Section 16 Affected Documents. This section was previously section 15 in ETS-8-044.0. 

Section 17 Revisions. This section was previously section 16 in ETS-8-044.0. 

ETS-8-044.1 Page 22 of 22 

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ATTACHMENT D: DEVIATION(S) 

Page 109 of 110 
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Analysis of PFBS, PFHS, and PFOS in Groundwater 

Decatur, AL - December 2011 

RECORD OF DEVIATION/NONCONFORMANCE 

/. Identification 

Study / Project No. 

GLP10-01-02-24 

Date(s) of Occurrence: 

12/27/11, 1/4/12 

Document Number: 

ETS-8-044.1 

Deviation type • SOP • Equipment Procedure 0 Method 

(Check one) • Protocol • GPO • Other: 

/ / . Description (attach extra pages as needed) 

Method Requirements: 

1. FMS recovery within ±30% (section 13.4). 

2. RPD values <20% (section 13.4). 

Actual procedure/process: 

1. The sampling location DAL GW 134L had a PFOS FMS recovery of 61.2%. 

2. The sampling location DAL GW 137S had a sample/sample duplicate RPD of 21% for PFHS and 32% for 

PFOS. 

///. Actions Taken 

(such as amendment issued, SOP revision, etc.) 

Corrective Action ( • Yes 0 No) Reference: 

Acceptability of the nonconforming work: 

1. The sampling location with a FMS recovery outside method acceptance criteria will be flagged in the 

report and the analytical uncertainty for DAL GW 134L will be expanded to ± 39% for PFOS. 

2. The non-compliant RPDs will be flagged in the final report. 

Actions: • Halting of Work • Client Notification • Work Recall • Withholding of Report 

0 Other: Deviations will be noted in final report. 

Project Lead/PAI Approval: 

Study Director (if GLP): 

Sponsor Approval (for GLP protocol deviations): NA 

Date: / i 

Date: 

Date: 

Technical Reviewer (optional): NA Date: NA 

Laboratory Departnnent Manager Approval: Date: 

IV. Authorization to Resume Work 

Where halting of work occurred, resumption of work must first be approved by Laboratory Management 

Laboratory Department Manager Approval: NA Date: NA 

Deviation No. 

(assigned by Study Director or Team Leader at the end of study or project) 

ETS-4-008.7 Page 1 of 1 

Documentation of Deviations and Control of Nonconforming Testing iioof no