GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

GLP10-01-01. Interim Report 18: Analysis of PFOA in Groundwater Samples Collected at 

the Former Sludge Incorporation Area (FSIA) located in Decatur. AL in June 2011 

Study Title 

Analysis of Perfluorooctanoic Acid (PFOA) 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, Bldg 260-05-N-17 

Maplewood, MN 55144 

Project Identification 

GLP10-01-01-18 

Total Number of Pages 

71 

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 A21A Certificate #2052.01. Testing that complies with this intemationai Standard also 

operate in accordance with ISO 9001:2000. 

Testing Cert #2052.01 

Page 1 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

This page has been reserved for specific country requirements. 

Page 2 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

GLP COMPLIANCE STATEMENT 

Report Title: GLP10-01-01, Interim Report 18. Analysis of PFOA in Groundwater Samples Collected 

at the Former Sludge Incorporation Area (FSIA) at Decatur, AL in June 2011 

Study: Analysis of Perfluorooctanoic Acid (PFOA) 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 detennined under GLPs. 

1± 

% ' 2 ^ 

% 

Gary Hobiensteiiif Sponsor Representative Date 

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

Page 3 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

QUALITY ASSURANCE STATEMENT 

Report Title: GLP10-01-01, Interim Report 18. Analysis of PFOA in Groundwater Samples Collected 

at the Former Sludge Incorporation Area (FSIA) at Decatur, AL in June 2011 

Study: Analysis of Perfluorooctanoic Acid (PFOA) in Groundwater, Soil and Sediment for the 3M 

Decatur Phase 3 Site-Related Monitoring Program. 

This report and the accompanying data were audited by the 3M Environmental Laboratory Quality 

Assurance Unit (QAU), as indicated below. The findings were reported to the principal investigator 

(P.I.), laboratory management and study director 

Inspection Dates 

8/4/11-8/5/11 

Phase 

Data / Interim Report 

Date Reported to 

Testing Facility 

Management 

8/18/11 

Study Director 

8/18/11 

QAU Representative 

Page 4 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

TABLE OF CONTENTS 

GLP Compliance statement 3 

Quality Assurance Statement 4 

Table of Contents 5 

List of Tables 6 

1 Study Infomnation 8 

2 Summary 9 

3 Introduction 10 

4 Test & Control Substances 11 

5 Reference Substances 11 

6 Test System 12 

7 Method Summary 12 

7.1 Methods 12 

7.2 Sample Collection 12 

7.3 Sample Preparation 12 

7.4 Analysis 12 

8 Analytical Results 14 

8.1 Calibration 14 

8.2 System Suitability 14 

8.3 Limit of Quantitation (LOQ) 14 

8.4 Continuing Calibration 14 

8.5 Blanks 15 

8.6 Lab Control Spikes (LCSs) 15 

8.7 Analytical Method Uncertainty 18 

8.8 Field Matrix Spikes (FMS) 18 

Page 5 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

9 Data Summary and Discussion 19 

10 Conclusion 31 

11 Data/Sample Retention 31 

12 /\ttachments 31 

13 Signatures 32 

LIST OF TABLES 

Table 1. Summarized PFOA Results (FSIA Groundwater, Decatur, AL, June 2011) 10 

Table 2. Instmment Parameters 13 

Table 3. Liquid Chromatography Conditions 13 

Table 4. Mass Transitions 13 

Table 5. Limit of Quantitation (LOQ) 14 

Table 6. Laboratory Control Spike Recovery 16 

Table 7. Analytical Method Uncertainty 18 

Tables. Field Matrix Spike Levels 18 

Table 9. DALGW130R110630 20 

Table 10. DAL GW130S 110630 20 

Table 11. DALGW130L110630 20 

Table 12. DAL GW131R 110622 21 

Table 13. DAL GW 131S 110622 21 

Table 14. DALGW131 L110622 21 

Table 15. DAL GW 133R110630 22 

Table 16. DAL GW133S 110630 22 

Table 17. DALGW133L110630 22 

Table 18. DAL GW 134R 110628 23 

Table 19. DAL GW134S 110628 23 

Table 20. DALGW 134L110628 23 

Page 6 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Table 21. DALGW135R110628 24 

Table 22. DAL GW135S 110628 24 

Table 23. DALGW135L110628 24 

Table 24. DAL GW136S 110630 25 

Table25. DALGW 136L110630 25 

Table 26. DAL GW137S 110624 25 

Table27. DALGW 137L 110624 26 

Table28. DALGW 138S 110630 26 

Table29. DALGW 138L110630 26 

Table30. DALGW 138R110630 27 

Table31.DALGWCW26C110622 27 

Table 32. DAL GW CW26L110622 27 

Table 33. DAL GW 140R110622 28 

Table34. DALGW 141R110630 28 

Table35. DALGW 142R 110622 28 

Table36. DALGW 143R 110622 29 

Table37. DALGW 144S 110622 29 

Table 38. Trip Blank 1 29 

Table 39. Trip Blank 2 30 

Table 40. Rinseate Blanks 30 

Page 7 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

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 

Maplewood, MN 55106 

Study Personnel 

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

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

Susan Wolf, 3M Analyst 

Chelsie Grochow, Analyst 

Kevin Eich, Analyst 

Kelly Ukes, Analyst 

Jonathan Steege, Analyst 

Study Dates 

Study Initiation: March 8, 2010 

Interim Report 18 Experimental Termination: July 29, 2011 

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 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

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

Sludge Incorporation Area (FSIA) in Decatur, AL, representing thirty different sampling locations. A 

total of one hundred fifty-four sample bottles were received at the 3M Environmental Laboratory for 

perfluorooctanoate (PFOA) analysis, and included duplicate groundwater samples from each sampling 

location. Samples also included at least two field matrix spike (FMS) samples for each location, two trip 

blank sets containing Milli-QTM water and appropriate trip blank spikes, and two equipment rinseates. 

The equipment rinseate blanks did not have FMS samples prepared for detennination of PFOA 

recovery. The groundwater samples, trip blanks, and two equipment rinseate blanks were received 

from Weston personnel on July 8,2011. All of the samples were prepared and analyzed for PFOA 

following 3M Environmental Laboratory Method ETS-8-044.0 under 3M project GLP-10-01-01-18. 

Many of the groundwater samples required dilution to attain PFOA concentrations within the range of 

the curve, in some instances up to 100-fold dilution were required. The average measured PFOA 

concentrations are summarized in Table 1. The equipment rinseates and the trip blanks were below 

the lower limit of quantitation (LLOQ) of 0.0250 ng/mL, indicating adequate control of sample 

contamination during shipping and sample collections. The PFOA concentration results for all 

groundwaters ranged over four orders of magnitude from 0.277 ng/mL to 3520 ng/mL. The analytical 

uncertainty was estimated at 100±15%. 

Page 9 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Table 1. Summarized PFOA Results (FSIA Groundwater, Decatur, AL, June 2011) 

Sample ID 

DALGW130R110630 

DALGW130S110630 

DALGW130L110630 

DAL GW131R 110622 

DAL GW131S 110622 

DAL GW 131L 110622 

DALGW133R110630 

DALGW133S110630 

DALGW133L110630 

DALGW134R110628 

DALGW134S110628 

DALGW134L110628 

DALGW135R110628 

DALGW135S110628 

DALGW135L110628 

DALGW136S110630 

DALGW136L110630 

DALGW137S110624 

DALGW137L110624 

DALGW138R110630 

DALGW138S110630 

DALGW138L110630 

DALGWCW26C110622 

DALGWCW26L110622 

DAL GW140R 110622 

DAL GW141R 110630 

DALGW142R110622 

DAL GW143R 110622 

DAL GW144S 110622 

Trip Blanks (Milli-QTM Water) 

GLP10-01-01-18 Equipment rinseate blanks: 

DAL GW 130L and DAL GW 133S 

Avg. PFOA 

Concentration 

(ng/mL) 

830 

179 

65.1 

2430 

26.2 

95.1 

108 

313 

228 

1800 

9.80 

560 

3520 

21.0 [a] 

278 [a] 

131 

79.0 

0.277 

0.377 

291 

154 

0.893 

426 

645 

129 

1.58 

50.8 

24.1 

50.6 

< 0.0250 

< 0.0250 

Relative 

Percent 

Difference 

1.7% 

1.1% 

5.4% 

9.9% 

3.8% 

2.4% 

0.0% 

1.0% 

1.8% 

0.56% 

2.6% 

12% 

3.1% 

7.2% 

4.0% 

0.0% 

1.8% 

5.4% 

2.4% 

2.1% 

1.3% 

0.34% 

0.47% 

0.16% 

2.3% 

1.3% 

2.6% 

6.2% 

6.1% 

N/A 

N/A 

N/A: not applicable 

The analytical uncertainty for PFOA was estimated at 100+15%. 

[a] Sampling location did not have an appropriate FMS spike level to sufficiently evaluate PFOA 

recovery. 

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 perfluorooctanoate (PFOA) 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 ground water samples collected from various wells located 

at the Fomner Sludge Incorporation Area (FSIA) in Decatur, AL for PFOA in an effort to characterize 

regional groundwater conditions. 

Page 10 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

The 3M Environmental Laboratory prepared sample bottles (250 mL high-density polyethylene) which 

were shipped to Decatur, AL Weston personnel prior to field sampling. Sample bottle sets for each 

groundwater sampling location included a field sample, field sample duplicate, and a minimum of two 

field spike samples. Each empty container for groundwater samplings 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 PFOA prior to being sent to the field for 

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

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

Laboratory method ETS-8-044.0 "Determination of Perfluorinated Compounds in Water by High 

Perfomriance Liquid Chromatography/Mass Spectrometry Direct Injection Analysis". 

Table 1 summarizes the average PFOA concentrations for the duplicate groundwater samples 

collected, the trip blank, and equipment rinseate samples. Tables 9-40 summarize the individual 

sample results and the associated FMS recoveries. All results for the quality control samples prepared 

and analyzed with the samples are reported and discussed elsewhere in this report. 

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

was purely analytical in nature. 

The analytical reference substances used for this study are listed below. 

Reference 

Substance 

Chemical Name 

Chemical Formula 

Identifier 

Use 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFOA (Linear) 

Perfluorooctanoate 

C7F15COOH 

CAS #335^7-1 

Target Analyte 

Reference Standard 

Oakwood Products 

01/17/2018 

Frozen 

3440 

TCR07-0041 

Powder 

99.1% 

PFOA 

(Unear + Branched) 

Perfluorooctanoate 

C7F15COOH 

Ammonium Salt 

CAS #335-67-1 

LCS Reference 

Standard 

3M 

02/27/2017 

Frozen 

332 

TCR-123 

White powder 

95% 

"Cg-PFOA 

Perfluorooctanoate 

^'CsHFisOz 

CAS#MPFC-C-0511 

Intemal Standard 

Wellington 

05/25/2014 

Frozen 

052411 

TCR11-0016 

Liquid 

NA<^' 

"CirPFOA 

Perfluorooctanoate 

^^C8HF1502 

CAS#MPFC-C-0910 

Intemal Standard 

Wellington 

09/28/2013 

Frozen 

092310 

TCR11-0048 

Liquid 

NATM 

(1) Compound is part of a custom mixture of mass-lat)eled perfluorinated compounds at a concentration of 5.0 pg/mL. 

Page 11 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

There was not a test system for this study in the classic sense of a GLP study. This study was 

conducted for analysis of ground water samples collected from wells located in Decatur, AL by Weston 

Solutions, Inc. personnel. Samples for this study are "real worid" environmental samples. 

Sample Description Key Code. 

string Humbec 

Example 

1 

2 

3 

4 

5 

String Descriptor Example 

DAL GW131R 0110622 

Sample Location 

Well ID 

Well Level 

Sampling Date 

Sample Type 

DAL= Decatur, Alabama 

Example: 131 

R = Residum shallow water-ljearing zone 

L = Bedrock water-bearing zine 

S = Epikarst middle water-bearing zone 

110622-June 22,2011 

0=primary sample 

1=duplicate sample 

LS = low spike 

IVIS = mid spike 

HS = high spike 

7.1 Methods 

Analysis for all analytes was completed following 3M Environmental Laboratory method ETS-8-044.0 

"Determination of Perfluorinated Compounds In Water by High Performance Liquid 

Chromatography/Mass Spectrometry Direct Injection Analysis". 

.,TM , 

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 GLP10-01-01-18 were returned to the 

laboratory at ambient conditions on July 8,2011. 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 

each cooler of 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 1mL sample with 9 mLs of Milli-Q water 

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

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

to 9.9 mLs of MilliQ water 

7.4 Analysi s 

All study samples and quality control samples were analyzed for PFOA using high performance liquid 

chromatography/ tandem mass spectrometry (HPLC/MS/MS). Detailed instrument parameters, the 

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

Page 12 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

raw data hard copies placed in the final data packet, and are briefly described below in Table 2, Table 3 

and Table 4. 

Table 2. Instrument Parameters. 

instrument Name 

Analytical Method Followed 

Analysis Date 

Liquid Chromatograph 

Guard column 

Analytical column 

injection Volume 

IVIass Spectrometer 

Ion Source 

Electrode 

Polarity 

Software 

ETSKirH 

ETS-8-044.0 

7/15/11-7/19/11 

Agilent 1200 

Prism RP (2.1 mm X 50 mm), 5 n 

Betasil C18 (2.1 mm X100 mm), 5n 

5or25nL 

Applied Biosystems API 5500 

Turbo Spray 

Turbo ion electrode 

Negative 

Analyst 1.5.2 

ETSKirk 

ETS-8-044.0 

7/28/11-7/29/11 

Agilent 1200 

Betasil CI 8 (4.6 mm X 100 mm), 5n 

Betasil CI 8 (4.6 mm X 100 mm), 5u 

25 nL 

Applied Biosystems API 5500 

Turbo Spray 

Turbo ion electrode 

Negative 

Analyst 1.5.2 

Table 3. Liquid Chromatograpfiy Conditions. 

step 

Number 

Total Time 

(min) 

Flow Rate 

(idJmin) 

Percent A 

(2 mM ammonium acetate) 

Percent B 

(MethanoO 

7/15/11-7/19/11 Analysis 

0 

1 

2 

3 

4 

5 

0.0 

2.0 

14.5 

15.5 

15.6 

20.0 

300 

300 

300 

300 

300 

300 

97.0 

97.0 

5.0 

5.0 

97.0 

97.0 

3.0 

3.0 

95.0 

95.0 

3.0 

3.0 

7/28/11 -7/29/11 Analysis 

0 

1 

2 

3 

4 

5 

0.0 

2.0 

14.5 

15.5 

16.5 

20.0 

750 

750 

750 

750 

750 

750 

97.0 

97.0 

5.0 

5.0 

97.0 

97.0 

3.0 

3.0 

95.0 

95.0 

3.0 

3.0 

Table 4. Mass Transitions. 

Analyte 

PFOA 

Mass Transition 

Q1/Q3 

413/369 

413/219 

413/169 

Intemal Standard ^^' 

t'CJPFOA 

Mass Transition 

Q1/Q3 

421/376 

Dwell time was 20 or 30 msec for each transition. The individual transitions were summed to 

produce a 'total ion chromatogram" (TIC), which was used for quantitation. 

(1) Intemal standard was only used for analysis performed on 7/28/11. 

Page 13 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

8.1 Calibration 

All samples were initially analyzed against an external standard calibration curve. Calibration standards 

were prepared by spiking known amounts of the stock solution containing the target analytes into a 

laboratory-Milli Q water. A total of fifteen spiked standards ranging from 0.025 ng/mL to 100 ng/mL 

(nominal) were prepared. A quadratic, 1/x weighted, calibration curve of the peak area counts was used 

to fit the data for PFOA. The data were not forced through zero during the fitting process. Calculating 

the standard concentrations using the peak area confirmed accuracy of each curve point. 

Sample DAL GW 135S was repeated 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 intemal 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 approximately 0.025 ng/mL to 100 ng/mL was prepared. A quadratic, 1/x 

weighted, calibration curve of the standard peak area/ 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/ peak area ratios and the resultant calibration curve confirmed 

accuracy of each curve point. 

For both analytical mns, 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 PFOA. 

8.2 System Suitability 

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

demonstrate overall system suitability. The acceptance criteria 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 PFOA. 

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 are at least twice those of the appropriate 

blanks. The nominal LOQ for all analytes can be found in Table 5. 

Table 5. Limit of Quantitation (LOQ). 

Analysis Dates 

7/15/11,7/28/11 

PFOA 

LOQ, ng/mL 

0.0250 

8.4 Continuing Calibration 

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

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

CCVs met method criteria of 100% ± 25% for PFOA. 

Page 14 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

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 PFOA. Trip blanks refiect the shipping and sample collection 

conditons the sample bottles and samples experience. Equipment rinseate blanks are aqueous 

samples that refiect 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 10 mL of laboratory 

Milli Q water or synthetic groundwater, to produce the desired concentration. The spiked water samples 

were then 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 the linear PFOA LCS 

samples. 

As the reference materials used for quantitation of PFOA is predominantly linear, and the PFOA present 

in the water samples are comprised of linear and branched isomers, additional LCS samples of linear 

and branched PFOA were prepared at three concentrations to evaluate the potential for analytical bias. 

The linear and branched LCS met method acceptance criteria at all levels. All LCS samples were used 

in the detemnination of method uncertainty in section 8.7. 

The following calculations were used to generate data in Table 6 for laboratory control spikes: 

, ^or. . r. Calculated Concentration , . „„„, 

LCS Percent Recovery = * 100% 

Spike Concentration 

LCS%RSD = Standard deviation LCS replicates .^^py^ 

average LCS recovery 

Page 15 of 71 
Table 6. Laboratory Control Spike Recovery. 

GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

ETS-8-044.0 

Analyzed 7/15/2011 

Lab ID 

LCS-110714-1 

LCS-110714-2 

LCS-110714-3 

Average ±%RSD 

LCS-110714-4 

LCS-110714-5 

LCS-110714-6 

Average ±%RSD 

LCS-110714-7 

LCS-110714-8 

LCS-110714-9 

Average ±%RSD 

Spiked 

Concentration 

(ng/mL) 

0.498 

0.498 

0.498 

LinearPFOA 

Calculated 

Concentration 

(ng/mL) 

0.510 

0.506 

0.547 

%Recovery 

102 

102 

110 

105% ±4.4% 

4.98 

4.98 

4.98 

5.16 

5.26 

5.26 

104 

106 

106 

105% ±1.1% 

29.9 

29.9 

29.9 

28.3 

27.5 

28.4 

94.6 

92.0 

94.9 

93.8%±1.r/o 

ETS-8-044.0 

Analyzed 7/15/2011 

Lab ID 

LCS-110714-10 ECF 

LCS-110714-11 ECF 

LCS-110714-12 ECF 

Average ±%RSD 

LCS-110714-13 ECF 

LCS-110714-14 ECF 

LCS-110714-15 ECF 

Average ±%RSD 

LCS-110714-16 ECF 

LCS-110714-17 ECF 

LCS-110714-18 ECF 

Average ±%RSD 

Urn 

Spiked 

Concentration 

(ng/mL) 

0.498 

0.498 

0.498 

3ar + Branched PF 

Calculated 

Concentration 

(ng/mL) 

0.522 

0.470 

0.491 

•OA 

VoRecovery 

105 

94.4 

98.5 

99.3% ±5.4% 

4.99 

4.99 

4.99 

4.96 

4.99 

5.18 

99.3 

100 

104 

101% ±2.5% 

29.9 

29.9 

29.9 

31.3 

30.3 

30.5 

105 

101 

102 

103% ±2.0% 

Page 16 of 71 
Table 7 continued. Laboratory Control Spike Recovery. 

GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

ETS-8-044.0 

Analyzed 7/28/2011 

Lab ID 

LCS-110726-1 

LCS-110726-2 

LCS-110726-3 

Average ±%RSD 

LCS-110726-4 

LCS-110726-5 

LCS-110726-6 

Average ±%RSD 

LCS-110726-7 

LCS-110726-8 

LCS-110726-9 

Average ±%RSD 

Spiked 

Concentration 

(ng/mL) 

0.199 

0.199 

0.199 

LinearPFOA 

Calculated 

Concentration 

(ng/mL) 

0.210 

0.211 

0.221 

%Recovery 

106 

106 

111 

108%±2.r/o 

1.99 

1.99 

1.99 

2.03 

1.97 

2.02 

102 

98.7 

102 

101% ±1.9% 

19.9 

19.9 

19.9 

19.1 

19.3 

19.3 

96.0 

97.0 

96.8 

96.6% ±0.55% 

ETS-8-044.0 

Analyzed 7/28/2011 

Lab ID 

LCS-110726-10 ECF 

LCS-110726-11 ECF 

LCS-110726-12 ECF 

Average ±%RSD 

LCS-110726-13 ECF 

LCS-110726-14 ECF 

LCS-110726-15 ECF 

Average ±%RSD 

LCS-110726-16 ECF 

LCS-110726-17 ECF 

LCS-110726-18 ECF 

Average ±%RSD 

Lim 

Spiked 

Concentration 

(ng/mL) 

0.199 

0.199 

0.199 

3ar+BrancfiedPF 

Calculated 

Concentration 

(ng/mL) 

0.206 

0.215 

0.217 

•OA 

%Recovery 

104 

108 

109 

10r/o±2.5% 

1.99 

1.99 

1.99 

1.99 

2.01 

2.14 

99.8 

101 

107 

103% ±3.8% 

19.9 

19.9 

19.9 

20.2 

21.7 

22.7 

102 

109 

114 

108% ±5.6% 

Page 17 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

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 

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

corresponds to a confidence level of 95%. 

Table 8. Analytical Method Uncertainty. 

Analyte 

PFOA 

Method 

ETS-8-044.0 

Standard [)eviation 

7.28 

Method 

Uncertainty 

±15% 

8.8 Field Matrix Spikes (FMS) 

A minium of two field matrix spikes were 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 the target analytes prior to shipping 

sample containers for sample collection. Field matrix spike recoveries within method acceptance criteria 

of 100±30% confirm that "unknown" components in the sample matrix do not significantly interfere with 

the extraction and analysis of the analytes of interest. 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 Spil<e Levels. 

Sampling Location 

134S, 135S, 136R, 137R, 137S, 137L, 138L 

130L, 131S, 131L, 133R, 135L, 136S, 136L, 

141R, 142R, 143R, 144S 

130R, 130S, 133S, 133L, 134L, 138R, 138S, 

CW26C, CW26L, 140R 

131R, 134R, 135R 

Trip Blank 

Spike Level 

Low 

Mid 

High 

Low 

Mid 

High 

Low 

Mid 

High 

Low 

High 

Low 

Mid 

Mid-High 

High 

PFOA, ng/mL 

0.0985 

0.985 

9.85 

0.985 

9.85 

98.7 

9.85 

98.7 

494 

98.7 

1956 

0.985 

9.85 

98.7 

494 

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

Spike Concentraton 

100% 

Page 18 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

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 135S110628 - Due to the high concentration of PFOA detected in the sample, this sampling 

location did not have an appropriate FMS spike level to sufficiently evaluate PFOA recovery. 

DAL GW 135L110628 - Due to the high concentration of PFOA detected in the sample, this sampling 

location did not have an appropriate FMS spike level to sufficiently evaluate PFOA recovery. 

Page 19 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Table 10. DAL GW 130R 110630 

3IVIUMSID 

GLP10-01-01-18-006 

GLP10-01-01-18-007 

GLP10-01-01-18-008 

GLP10-01-01-18-009 

GLP10-01-01-18-010 

Description 

DAL GW130R 0110630 

DAL GW130RDB 110630 

DAL GW130RLS 110630 

DAL GW130R MS 110630 

DALGW130RHS110630 

Average Concentration (ng/mL) ± %RPD 

PFOA 

Concentration 

(ng/mL) 

837 

823 

833 

921 

1280 

VoRecovery: 

NA 

NA 

NC 

NC 

91.2 

830 ng/mL ±1.7% 

NA= Not Applicable 

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

Table 11. DAL GW 130S 110630 

3IVIUMSID 

GLP10-01-01-18-011 

GLP10-01-01-18-012 

GLP10-01-01-18-013 

GLP10-01-01-18-014 

GLP10-01-01-18-015 

Average Cone 

Description 

DAL GW130S 0110630 

DAL GW130SDB 110630 

DAL GW130S LS110630 

DALGW130SMS110630 

DAL GW130SHS 110630 

entiytion (ng/mL) ± %RPD 

PFOA 

Concentration 

(ng/mL) 

180 

178 

181 

265 

708 

179 ng/mL 

VoRecovery 

NA 

NA 

NC 

87.1 

107 

±1.1% 

NA= Not Applicable 

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

Table 12. DAL GW 130L 110630 

3IVIUMSID 

GLP10-01-01-18-016 

GLP10-01-01-18-017 

GLP10-01-01-18-018 

GLP10-01-01-18-019 

GLP10-01-01-18-020 

Description 

DAL GW130L 0110630 

DAL GW130LDB 110630 

DAL GW130LLS 110630 

DAL GW1 SOL MS 110630 

DALGW130L HS 110630 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

66.8 

63.3 

68.7 

74.8 

158 

VoRecovery^ 

NA 

NA 

NC 

NC 

94.2 

65.1 ng/mL ±5.4% 

NA= Not Applicable 

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

Page 20 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Table 13. DAL GW 131R 110622 

3IVIUIVIStD 

GLP10-01-01-18-021 

GLP10-01-01-18-022 

GLP10-01-01-18-023 

GLP10-01-01-18-024 

Description 

DAL GW131R 0110622 

DAL GW131RDB 110622 

DAL GW131RLS 110622 

DAL GW131RHS 110622 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

2310 

2550 

2490 

4060 

VoRecovery 

NA 

NA 

NC 

83.3 

2430 ng/mL ±9.9% 

NA= Not Applicable 

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

Table 14. DALGW 131S 110622 

3M LIMS ID 

GLP10-01-01-18-025 

GLP10-01-01-18-026 

GLP10-01-01-18-027 

GLP10-01-01-18-028 

GLP10-01-01-18-029 

Average Cone 

Description 

DAL GW131S 0110622 

DALGW131SDB 110622 

DAL GW131SLS 110622 

DAL GW131S MS 110622 

DAL GW131SHS 110622 

entration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

26.7 

25.7 

26.6 

36.0 

115 

26.2ng/ml 

VoRecovery 

NA 

NA 

NC 

NC 

90.0 

.±3.8% 

NA= Not Applicable 

NO = Not Calculated; Endogenous sample concentration greater than 2x spike level. 

Table 15. DAL GW 131L 110622 

3M LIMS ID 

GLP10-01-01-18-030 

GLP10-01-01-18-031 

GLP10-01-01-18-032 

GLP10-01-01-18-033 

GLP10-01-01-18-034 

Description 

DAL GW131L 0110622 

DAL GW131LDB 110622 

DAL GW131L LS110622 

DAL GW 131L MS 110622 

DALGW131LHS110622 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

93.9 ^ 

96.2 

97.3 

107 

185 

VoRecovery 

NA 

NA 

NC 

NC 

91.1 

95.1 ng/mL ±2.4% 

NA = Not Applicable 

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

Page 21 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Table 16. DAL GW 133R 110630 

3IVILIIVISID 

GLP10-01-01-18-045 

GLP10-01-01-18-046 

GLP10-01-01-18-047 

GLP10-01-01-18-048 

GLP10-01-01-18-049 

Description 

DAL GW133R 0110630 

DAL GW133RDB 110630 

DAL GW133RLS 110630 

DAL GW133R MS 110630 

DALGW133RHS110630 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

108 

108 

96.6 

112 

190 

108 ng/mL 

VoRecovery 

NA 

NA 

NC 

NC 

83.1 

±0.0% 

NA = Not Applicable 

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

Table 17. DAL GW 133S 110630 

SIVILIMSID 

GLP10-01-01-18-040 

GLP10-01-01-18-041 

GLP10-01-01-18-042 

GLP10-01-01-18-043 

GLP10-01-01-18-044 

Description 

DAL GW133S 0110630 

DAL GW133SDB 110630 

DAL GW133SLS 110630 

DALGW133SMS110630 

DAL GW133SHS 110630 

Average Concentration (ng/mL) ± %RPD 

PFOA 

Concentration 

(ng/mL) 

311 

314 

316 

397 

768 

VoRecovery 

NA 

NA 

NC 

NC 

92.3 

313 ng/mL ±1.0% 

NA = Not Applicable 

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

Table 18. DAL GW 133L 110630 

3M LIMS ID 

GLP10-01-01-18-035 

GLP10-01-01-18-036 

GLP10-01-01-18-037 

GLP10-01-01-18-038 

GLP10-01-01-18-039 

Average Cone 

Description 

DAL GW133L 0110630 

DAL GW133LDB 110630 

DAL GW133L LS110630 

DAL GW133L MS 110630 

DAL GW133LHS 110630 

entration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

230 

226 

265 

417 

708 

228 ng/mL 

VoRecovery 

NA 

NA 

NC 

NC 

97.3 

±18% 

NA = Not Applicable 

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

Page 22 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Table 19. DAL GW 134R 110628 

3M LIMS ID 

GLP10-01-01-18-050 

GLP10-01-01-18-051 

GLP10-01-01-18-052 

GLP10-01-01-18-053 

Description 

DAL GW134R 0110628 

DALGW134RDB110628 

DAL GW134R LS110628 

DAL GW134RHS 110628 

Average Concentration (ng/mL) ± %RPD 

PFOA 

Concentration 

(ng/mL) 

1790 

1800 

1870 

3610 

VoRecovery 

NA 

NA 

NC 

92.8 

1800 ng/mL ±0.56% 

NA= Not Applicable 

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

Table 20. DAL GW 134S 110628 

3M LIMS ID 

GLP10-01-01-18-059 

GLP10-01-01-18-060 

GLP10-01-01-18-061 

GLP10-01-01-18-062 

GLP10-01-01-18-063 

Average Cone 

Description 

DAL GW134S 0110628 

DAL GW134SDB 110628 

DAL GW134SLS 110628 

DAL GW134S MS 110628 

DAL GW134SHS 110628 

entration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

9.67 

9.92 

9.60 

10.7 

19.6 

9.80 ng/ml 

VoRecovery 

NA 

NA 

NC 

NC 

99.5 

.±2.6% 

NA = Not Applicable 

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

Table 21. DALGW 134L 110628 

3M LIMS ID 

GLP10-01-01-18-054 

GLP10-01-01-18-055 

GLP10-01-01-18-056 

GLP10-01-01-18-057 

GLP10-01-01-18-058 

Description 

DAL GW134L 0110628 

DAL GW134LDB 110628 

DAL GW134L LS110628 

DAL GW134L MS 110628 

DAL GW134LHS 110628 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

527 

592 

602 

677 

1010 

VoRecovery 

NA 

NA 

NC 

NC 

91.3 

560 ng/mL ±12% 

NA = Not /Applicable 

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

Page 23 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Table 22. DAL GW 135R 110628 

3M LIMS ID 

1 1 1 1 

9 9 9 9 nil 

_j _i _j _i 

CD CD CD CD 

Description 

DAL GW135R 0110628 

DALGW135RDB110628 

DAL GW135RLS 110628 

DAL GW135RHS 110628 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

3570 

3460 

3600 

5250 

VoRecovery 

NA 

NA 

NC 

88.7 

3520 ng/mL ±3.1% 

NA = Not Applicable 

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

Table 23. DAL GW 135S 110628 

3M LIMS ID 

GLP1001-01-18-069 

GLP10-01-01-18-070 

GLP1001-01-18-071 

GLP10-01-01-18-072 

GLP1O01-01-18-073 

Description 

DAL GW135S 0110628 

DALGW135SDB110628 

DALGW135SLS110628 

DAL GW135S MS 110628 

DALGW135SHS110628 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

20.2 

21.7 

NA<^' 

NATM 

44.3 

VoRecovery 

NA 

NA 

NA<^' 

NA'^' 

NC 

21.0 ng/mL ±7.2%' ^ 

NA = Not /Applicable 

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

(1) Sample not analyzed due to spike concentration not being appropriate compared to sample concentration. 

(2) Sampling location did not have an appropriate spike level to evaluate PFOA recovery. 

Table 24. DAL GW 135L 110628 

3M LIMS ID 

GLP10-01-01-18-074 

GLP1001-01-18-075 

GLP1001-01-18-076 

GLP10-01-01-18-077 

GLP10-01-01-18-078 

Description 

DAL GW135L 0110628 

DAL GW135LDB 110628 

DAL GW135LLS 110628 

DAL GW135L MS 110628 

DAL GW135LHS 110628 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

283 

272 

278 

289 

365 

VoRecovery 

NA 

NA 

NC 

NC 

NC 

278 ng/mL ± 4.0%'" 

NA = Not /Applicable 

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

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

Page 24 of 71 
GLP10-01-01; Interim Report 18 

/Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Table 25. DAL GW 136S 110630 

3M LIMS ID 

GLP10O1-01-18-088 

GLP10-01-01-18-089 

GLP10-01-01-18-090 

GLP10-01-01-18-091 

GLP10-01-01-18-092 

Description 

DAL GW136S 0110630 

DALGW136SDB110630 

DAL GW136SLS 110630 

DAL GW136S MS 110630 

DAL GW136SHS 110630 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

131 

131 

132 

136 

217 

VoRecovery 

NA 

NA 

NC 

NC 

87.1 

131 ng/mL ±0.0% 

NA = Not /Applicable 

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

Table 26. DAL GW 136L 110630 

3M LIMS ID 

GLP1001-01-18-084 

GLP1001-01-18-085 

GLP1001-01-18-086 

GLP10-01-01-18-155 

GLP10-01-01-18-087 

Description 

DAL GW136L 0110630 

DALGW136LDB110630 

DAL GW136LLS 110630 

DAL GW136L MS 110630 

DAL GW136LHS 110630 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

79.7 

78.3 

79.6 

89.1 

170 

VoRecovery 

NA 

NA 

NC 

NC 

92.2 

79.0 ng/mL ±1.8% 

NA = Not Applicable 

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

Table 27. DAL GW 137S 110624 

3M LIMS ID 

GLP10-01-01-18-093 

GLP10-01-01-18-094 

GLP10-01-01-18-095 

GLP10-01-01-18-096 

GLP1O01-01-18-097 

Description 

DAL GW137S 0110624 

DALGW137SDB110624 

DAL GW137SLS 110624 

DALGW137SMS110624 

DALGW137SHS110624 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

0.284 

0.269 

0.383 

1.18 

9.32 

VoRecovery 

NA 

NA 

NC 

91.7 

91.8 

0.277 ng/mL ±5AVo 

NA= Not Applicable 

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

Page 25 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Table 28. DAL GW 137L 110624 

3M LIMS ID 

GLP10-01-01-18-098 

GLP10-01-01-18-099 

GLP10-01-01-18-100 

GLP10-01-01-18-101 

GLP10-01-01-18-102 

Description 

DAL GW137L 0110624 

DAL GW137LDB 110624 

DAL GW137LLS 110624 

DALGW137LMS110624 

DAL GW137LHS 110624 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

0.372 

0381 

0.477 

1.35 

9.98 

VoRecovery 

NA 

NA 

NC 

98.8 

97.5 

0.377 ng/mL ±2.4% 

NA = Not/Applicable 

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

Table 29. DAL GW 138S 110630 

3M LIMS ID 

GLP10-01-01-18-113 

GLP10-01-01-18-114 

GLP10-01-01-18-115 

GLP10-01-01-18-116 

GLP10-01-01-18-117 

Average Cone 

Description 

DAL GW138S 0110630 

DAL GW138SDB 110630 

DAL GW138S LS110630 

DAL GW138S MS 110630 

DAL GW138SHS 110630 

entration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

155 

153 

161 

231 

610 

154 ng/mL 

VoRecovery 

NA 

NA 

NC 

78.0 

92.4 

±13% 

NA = Not /Applicable 

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

Table 29. DAL GW 138L 110630 

3M LIMS ID 

GLP10-01-01-18-108 

GLP10-01-01-18-109 

GLP10-01-01-18-110 

GLP10-01-01-18-111 

GLP10-01-01-18-112 

Description 

DAL GW138L 0110630 

DAL GW138LDB 110630 

DAL GW138LLS 110630 

DAL GW138L MS 110630 

DAL GW138LHS 110630 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

0891 

0.894 

0.974 

1.69 

9.14 

VoRecovery 

NA 

NA 

NC 

810 

83.7 

0.893 ng/mL ±0.34% 

NA = Not Applicable 

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

Page 26 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Table 30. DAL GW 138R 110630 

3M LIMS ID 

GLP10-01-01-18-103 

GLP1OO1-01-18-104 

GLP10-01-01-18-105 

GLP10-01-01-18-106 

GLP10-01-01-18-107 

Description 

DAL GW138R 0110630 

DAL GW138RDB 110630 

DAL GW138RLS 110630 

DAL GW138R MS 110630 

DAL GW138RHS 110630 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

294 

288 

292 

370 

709 

291 ng/mL 

VoRecovery 

NA 

NA 

NC 

NC 

84.7 

±2.1% 

NA = Not Applicable 

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

Table 31. DAL GW CW26C 110622 

3M LIMS ID 

GLP10-01-01-18-118 

GLP10-01-01-18-119 

GLP10-01-01-18-120 

GLP10-01-01-18-121 

GLP10-01-01-18-122 

Average Cone 

Description 

DAL GWCW26C 0110622 

DAL GW CW26C DB 110622 

DAL GW CW26C LS 110622 

DAL GW CW26C MS 110622 

DAL GW CW26C HS 110622 

entration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

427 

425 

436 

502 

841 

426 ng/mL 

VoRecovery 

NA 

NA 

NC 

NC 

84.1 

±0.47% 

NA= Not Applicable 

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

Table 32. DAL GW CW26L 110622 

3M LIMS ID 

GLP10-01-01-18-123 

GLP10-01-01-18-124 

GLP10-01-01-18-125 

GLP1OO1-01-18-126 

GLP10-01-01-18-127 

Description 

DAL GWCW26L 0110622 

DAL GW CW26L DB 110622 

DAL GWCW26L LS110622 

DAL GW CW26L MS 110622 

DAL GW CW26L HS 110622 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentiation 

(ng/mL) 

645 

644 

667 

723 

1060 

VoRecovery 

NA 

NA 

NC 

NC 

84.2 

645 ng/mL ±0.16% 

NA= Not Applicable 

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

Page 27 of 71 
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Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Table 33. DAL GW 140R 110622 

3M LIMS ID 

GLP10-01-01-18-128 

GLP10-01-01-18-129 

GLP10-01-01-18-130 

GLP10-01-01-18-131 

GLP10-01-01-18-132 

Description 

DAL GW140R 0110622 

DAL GW140RDB 110622 

DAL GW140RLS 110622 

DAL GW140R MS 110622 

DALGW140RHS110622 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

127 

130 

141 

223 

567 

VoRecovery 

NA 

NA 

NC 

95.7 

88.9 

129 ng/mL ±2.3% 

NA = Not /Applicable 

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

Table 34. DAL GW 141R 110630 

3M LIMS ID 

GLP10-01-01-18-135 

GLP10-01-01-18-136 

GLP10-01-01-18-137 

GLP10-01-01-18-138 

GLP10-01-01-18-139 

Description 

DAL GW141R 0110630 

DALGW 141 RDB 110630 

DALGW141RLS 110630 

DAL GW141R MS 110630 

DAL GW141RHS 110630 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

1.59 

1.57 

2.50 

10.6 

91.6 

VoRecovery 

NA 

NA 

93.4 

91.6 

91.2 

1.58 ng/mL ±1.3% 

NA= Not Applicable 

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

Table 35. DAL GW 142R 110622 

3M LIMS ID 

GLP10-01-01-18-140 

GLP10-01-01-18-141 

GLP10-01-01-18-142 

GLP10-01-01-18-143 

GLP10-01-01-18-144 

Description 

DAL GW142R 0110622 

DAL GW142RDB 110622 

DAL GW142RLS 110622 

DAL GW142R MS 110622 

DAL GW142RHS 110622 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

50.1 

51.4 

50.9 

57.5 

144 

VoRecovery 

NA 

NA 

NC 

NC 

94.5 

50.8 ng/mL ±2.6% 

NA = Not Applicable 

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

Page 28 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Table 36. DAL GW 143R 110622 

3M LIMS ID 

GLP10-01-01-18-145 

GLP1001-01-18-146 

GLP10-01-01-18-147 

GLP10-01-01-18-148 

GLP10-01-01-18-149 

Description 

DAL GW143R 0110622 

DAL GW143RDB 110622 

DALGW143RLS 110622 

DAL GW143R MS 110622 

DAL GW143RHS 110622 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

23.3 

24.8 

25.5 

33.1 

117 

VoRecovery 

NA 

NA 

NC 

NC 

94.2 

24.1 ng/mL ± 6.2% 

NA = Not /Applicable 

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

Table 37. DAL GW 144S 110622 

3M LIMS ID 

GLP10-01-01-18-150 

GLP10-01-01-18-151 

GLP10-01-01-18-152 

GLP10-01-01-18-153 

GLP10-01-01-18-154 

Description 

DAL GW144S 0110628 

DAL GW144SDB 110628 

DAL GW144SLS 110628 

DAL GW144S MS 110628 

DAL GW144SHS 110628 

Average Concentration (ng/mL) ± VoRPD 

PFOA 

Concentration 

(ng/mL) 

52.1 

49.0 

51.2 

60.3 

138 

VoRecovery 

NA 

NA 

NC 

NC 

88.6 

50.6 ng/mL ±6.1 % 

NA = Not Applicable 

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

Table 38. Trip Blank 1 

3M LIMS ID Ilil l 

9 9 9 9 9 5 5 5 5 5 CD C

D C

D C

D CD 

Description 

Trip Blank Set 1 Sample 

Trip Blank Set 1 LS 

Trip Blank Set 1 MS 

Trip Blank Set 1 MHS 

Trip Blank Set 1 HS 

PFOA 

Concentration 

(ng/mL) 

<0.0250 

0981 

10O 

95.5 

493 

VoRecovery 

NA 

99.6 

102 

96.8 

99.9 

NA = Not Applicable 

Page 29 of 71 
Table 39. Trip Blank 2 

NA = Not Applicable 

Table 40. Rinseate Blanks 

GLP10-01-01; Interim Report 18 

/Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

3M LIMS ID 

GLP1001-01-18-001 

GLP10-01-01-18-002 

GLP1001-01-18-003 

GLP10-01-01-18-004 

GLP10-01-01-18-005 

Description 

Trip Blank Set 2 Sample 

Trip Blank Set 2 LS 

Trip Blank Set 2 MS 

Trip Blank Set 2 MHS 

Trip Blank Set 2 HS 

PFOA 

Concentration 

(ng/mL) 

<0.0250 

0.954 

9.29 

89.7 

443 

VoRecovery 

NA 

96.9 

94.3 

90.9 

89.8 

3M LIMS ID 

GLP10-01-01-18-133 

GLP10-01-01-18-134 

Description 

DAL GW130LRB 110630 

DAL GW133S RB110630 

PFOA 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

VoRecovery 

NA 

NA 

NA= Not/Applicable 

Page 30 of 71 
GLP10-01-01; Interim Report 18 

/Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

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

accuracy and precision for PFOA. Analysis was successfully completed following 3M Environmental 

Laboratory method ETS-8-044.0 described herein. 

All remaining samples and asscx:iated project data (hardcopy and electronic) will be archived according 

to 3M Environmental Laboratory standard operating procedures. 

Attachment A: Protocol Amendment 18 (General Project Outline) 

Attachment B: Representative Chromatograms and Calibration Curves 

Attachment C: Analytical Method - ETS-8-044.0 

Page 31 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

n^£-2^» 'h4^ ) 

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

p9Jf^o^sr^oj/ 

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

Gary Hohenstein, 3M Sponsor Representative Date 

ML 

Jaisimha Kesari, Study Director jate 

Page 32 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

ATTACHMENT A : PROTOCOL AMENDMENT 

Page 33 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

Analytical Protocol: GLPi^f-W" ''""^ 

Amendment 18 

Study Title 

Analysis of Perfluorooctanoic Acid (PFOA) in Groundwater, Soil and Sediment for the 

3M Decatur Phase 3 Site-Related Monitoring Program 

PROTOCOL AMENDMENT NO. 18 

Amendment Date: 

June 15, 2011 

Perfonning Laboratory 

3M Environmental, Health, and Safety Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55144-1000 

laboratory Project Identification 

GLP10-01-01 

Sampling Event 

Fomner Sludge Incorporation Area (FSIA) Groundwater 

Page 1 of 8 

Page 34 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

Analytical Protocomp^m'-&h- -"""^ ^oi i 

Amendment 18 

This amendment modifies the foilowing portion of protocol: 

"Analysis of Perfluorooctanoic Acid (PFOA) 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 

at Decatur, AL, and conducted as part of the 3M Decatur Phase 3 Program for PFOA (GLP10-01-01). 

The anticipated sample collection will occur around the timeframe during the week of June 20. 2011. The 

groundwater samples for this sampling event will be entered into the 3M Environmental Laboratory LIMS 

as project GLP10-01-01-18 and reported as interim report GLP10-01-01-18, (reflecting study GLP10-01-

01 and amendment-18). 

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 five pages in length and included as attached to this amendment fbmi. 

Page 2 of 8 

Page 35 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

Analytical Protocoimtf^m^ ' '""^ '°^ ' 

Amendment 18 

Amendment Approval 

^ / 

mi/j Jp^Am/'ri 

Gary Hohenstein, Sponsor Representative Date 

0/,d 'zo/V 

Cleston C. Lange, Principal Analytical Investigator Date 

/ S " J c/^' ^ ^O/ / 

William Reagen, EHS Opns Environmental Lab Management 

U/Mv/. 

Date 

£/^/il 

D6te Jaisimha KesafrPt., DEE, Study Director 

Page 3 of 8 

Page 36 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Analytical Protocol: GW10-01-01 

Amendment 18 

Environmental Health & Safety Operations, Environmental Laboratory 

General Project Outline 

To: Gary Hohenstein, 3M EHS&Opns 

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

cc: V\/illiam Reagen, 3M EHS&Opns; Environmental Lab 

Cleston Lange, 3M EHS&Opns; Environmental Lab 

Jai Kesari, Weston Solutions 

Date: June 15,2011 

Subject: Analysis of Perfluorooctanoic Acid (PFOA) in Groundwater, Soil and Sediment for the 3M 

Decatur Phase 3 Site-Related Monitoring Program; GLP Interim Report 18 - Former Sludge 

Incorporation Area (FSIA) Groundwater - June 2011 Sampling 

1 General Project Information 

Contacts 

Lab Request Number 

Six Olslt Department Number 

1 Project Schedule/Test Dates 

3H Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3IVI Building 224-5W-03 

Saint Paul. MN 55144-1000 

Phone: (651) 737-3570 

Qahohenstein@mmm.com 

3M Environmental Laboratory Management 

William K. Reagen 

3M EHS Opns, Environmental 1 aboratory 

260-5N-17 

651 733-9739 

wkreaqenP!mmm.com 

Principal Analytical Investigator 

Cleston Lange 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9860 

cclanae@mmm.com 

Sampling Coordinator 

Timothy Frinak 

Weston Solutions 

Timothv.frinak@westonsolutions.com 

Phone: (334}-332-9123 

QLP1(M)1-01-18 

Dept #530711. Project #0022674449 

Sampling scheduled fbr the week of June 20,2011 

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

Page 4 of 8 

Page 37 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL: June 2011 

Analytical Protocol: GLP10-01-01 

Amendment 18 

2 Background information and Project Objective(s) 

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

samples collected from thirty-one groundwater wells for Perfluorooctanoic Acid (PFOA) 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 June 

20, 2011. The 3M Environmental Laboratory will prepare the sample bottles with all required spikes to 

ensure that results for PFOA are of a known precision and accuracy. The final report will be submitted to 

Gary Hohenstein and Jai Kesari upon completion under interim report GLP10-01-01-18. 

3 Project Schedule 

Sample collection bottles will be prepared by 3M Environmental Laboratory for sampling the week of June 20, 

2011. Sample bottles will be shipped in coolers to 3M Decatur for anival by Friday, June 17, 2011. Sample 

botdes 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 PFOA. 

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

duplicate and a minimum of two field mabix spikes will be collected. Table 1 indicates tiie well ID and 

corresponding field spike levels. The "fill to here" line on each 250 mL Nalgene botde will be 200 mL. Two sets 

of trip blanks consisting of reagent-grade water, a low-level tip blank spike, micMevel field spike, mid-high field 

spike, and a high-level trip blank spike will be prepared at the 3M Environmental Laboratory and sent to tiie 

sampling location witii tiie other bottles. Two additional bottles will be prepared to be used for the preparation 

of the equipment rinseate blanks. A1-L container of laboratory reagent water will be provided for the collection 

of tine equipment rinseate blanks. 

Based on the results from previously collected samples from the FSIA {GLP10-01-01-07 and GLP10-01-01-11), 

most sampling locations will require dilution wiUi laboratory reagent water prior to sample analysis. However, 

sampling locations identified in Set 1 of Table 1 are expected to contain PFOA concentiration <10 ng/mL. For 

samples collected firom Uiese sampling locations, the sample, sample duplicate and field mabix spikes will 

contain ttie addition of intemal standard Ca-PFOA at a nominal concentration of 1 ng/mL, as will the tiip blanks 

samples, trip blank low spikes, and two equipment rinseate blanks. The additional of intemal standard will be 

used to aid in the analysis of tiie samples. A total of 169 sample bottles \N\\\ be prepared. 

Page 5 of 8 

Page 38 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

Analytical Protocompmf-4^'''"' ' ^'' ' 

Amendment 18 

Table 1. Sampling Locations and Field Matrix Splice levels. 

Set# 

1 

2 

3 

4 

5 

Well No. 

1348,1358,136R,137R. 

137S, 137Land138L 

130L. 1318,131L. 133R, 

135L. 1368,136L, 141R, 

142R, 143R and 144R 

130R. 1308,1338,133L. 

134L, 138R, 1388. CW26C. 

CW26L and 140R 

131R. 134Rand135R 

Trip Blank Sets 1 and 2 

Sample Level 

Low 

Mid 

High 

Low 

Mid 

High 

Low 

Mid 

High 

Low 

High 

Low 

Mid 

Mid-High 

High 

Spike Cone. (ng/mL) 

0.1 

1.0 

10 

1 

10 

100 

10 

100 

500 

100 

2000 

1 

10 

100 

500 

5 Test IMethods 

Samples will be prepared and analyzed by LC/MS/MS following ETS-8-044.0 "Determination of Perfluorinated 

Compounds In Water by High Performance Liquid Chromatography/Mass Spectrometry Direct Injection 

Analysis". The data quality objectives for tiiese studies are quantitative results for the target analytes with an 

analytical accuracy of 100±30%. Field matrix spikes not yielding recoveries wittiin 100t30% will be addressed 

in tiie report and tiie final accuracy statement may be adjusted accordingly. Based on the results from 

previously collected samples firom the FSIA (GLP10^1-01-07 and GLP10-01-01-11), most sampling tocations 

will require dilution with laboratory reagent water prior to sample analysis by ETS-8-044.0. 

For samples containing intemal stendard: samples will be analyzed against an intemal standard calibration 

curve. Each cun/e point will contein isotopically-labeled perfluorocarisoxylic acids and perfluorosutfonic acids at 

a nominal concentiation of 1 ng/mL The calibration curve will be generated by taking tiie ratio of tiie standaixl 

peak area counts over the intemal stendard peak area counte to fit the date for each analyte. 

Alternately, samples may be analyzed by ETS 8-154.3 "Determination of Perfluorinated Adds, Alcohols, 

Amides, and Sulfonates In Water By Solid Phase Exbraction and High Performance Liquid 

Chromatography/Mass Spectrometiy or ETS-8-110.1 "Method of Analysis for tiie Detemnination of 

Perfluorinated Compounds in Water, Soil and Sediment by LC/MS/MS". 

6 Reporting Requirements 

For each sampling location, the report will contein the results for tiie sample, sample duplicate, and field matirix 

spikes. Trip blank and trip blank spikes will be reporiied for tiie sampling event as will any equipment/rinseate 

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

preparation will also be reported and used to evaluate tiie overall metiiod accuracy and precision. Metiiod 

blanks of reagent water prepared at tiie time of sample preparation will be used to detenriine tiie metiiod 

detection limit For those sampling locations where tiie fiekl matrix spike level was not appropriate, due to 

higher tiian expected analyte concentiBtions, a laboratory matrix spike may be prepared and included in tiie 

final report 

Page 6 of 8 

Page 39 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

Analytical Protocol: GLPi^f-lil" """"^ 

Amendment 18 

7 Email Correspondence 

Quarterly GW sampling - Decatur Former Sludge Incorporation Area Wells 

Young, Charles T. to: stwolf@mmm.com 06/13/201102:14 PM 

Cc: "Frinak, Timothy R.", "Smith, Martin" 

Sue: 

WESTON will be performing quarterly groundwater sampling of the former sludge incorporation area (FSIA) wells 

beginning on June 20,2011. The attached word document shows the FSIA wells (highlighted in yellow) that will be 

sampled for fluorochemlcal analyses.under GLP 10-01-01 and GLP 10-01-02. It also shows sampling schedule for 

other quarterly sampling (and conventional parameters) 

Mso attached is a spreadsheet summary table from the most recent (Nov-2010) round at the FSIA wells. 

In addition to the primary/dupllcate/spike bottles, we will need bottles and Milli-Q water for the two equipment 

rinseate blanks that will be collected. 

Thanks, 

Charlie 

Charles T. Young 

Technical Director 

Weston Solutions, Inc. 

1400 Weston Way (5-2) 

West Chester, PA 19380 

(610) 701-3787 

Fax (610) 701-3401 

Page 7 of 8 

Page 40 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Analytical Protocol: GLP10-01-01 

Amendment 18 

Quarteriy GW Monitoring 

First and Tliird Quarter Rflonitoring Program 

201L 

203L* 

204L 

206L 

209L 

211R 

212R 

212D 

213R 

213S 

215R 

215D 

216R 

217R 

217S 

217D 

218R 

218L 

220R* 

220L* 

221R 

222R* 

223R 

225R 

225L 

226R 

226L 

227R* 

227L* 

228R 

228L 

229R 

229L 

305R 

307L 

308R 

31 OR* 

311R 

313R 

315R 

317L* 

319L 

324L* 

325L 

328R* 

328L* 

330R* 

330L* 

332S 

335R* 

501 

503 

507 

51 OR 

51 OL 

511S 1 

512R 

512L 

GRS04*^ 

RW312R* 

RW327R* 

RW331S* 

Second and Fourtfi Quarter (Monitoring Program 

201L 

203L 

211R 

212R 

212D 

213R 

213S 

217R 

217S 

217D 

Monitoring wells ui 

(^ Monitoring wel 

(**) Monitoring we 

"One sample Willi 

analysis. 

RW indicate reoo\ 

218R 

218L 

??2R 

223R 

229R 

229L 

305R 

307L 

313R 

315R 

rillbeanalyredforV 

swill be analyzed fc 

Us will be analyzed f 

3e collected from tin 

« 7 wells used In ac 

324L 

325L 

332S 

335R 

512R 

512L 

130R** 

130S** 

130L** 

131.R** 

'OCs and isopropyi 

)r PFOA, and VOCs 

or PFOA. 

J closed landfiH(SW 

:tiva groundwater e> 

131S** 

131L** 

133R** 

1338** 

133L** 

134R** 

134S** 

134L** 

135R** 

135S** 

135L** 

ether using EPA Me 

/ Isopropyi ether us 

MIM) groundwater 

(traction systems. 

136R** 

1363** 

136L** 

137R** 

137S** 

137L** 

138R** 

138S** 

138L** 

CW26C** 

CVV26L** 

»od ^6 0 unless ol 

ing EPA Metiiod 82 

extraction system fb 

140R** 1 

141R** 

142R** 

143R** 

144R** 

[herwiselndk»ted. 

SO. 

rVOC and PFOA 

Page 8 of 8 

Page 41 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

ATTACHMENT B: REPRESENTATIVE SAIVIPLE CHROMATOGRAMS AND 

CALIBRATION CURVE(S) 

Page 42 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Results Name: kllOTlSa.rdb 

k110715a.rdb (PFOA): "Quadratic" Regression ("1 / x" weighting): y = -6.93e+003 x*2 + 1.82e+006 x + 3.65e+004 (r = 0.9998) 

45 50 55 

Concentration, ng/mL 

100 

Data printe d by STW 

Printin g Time: 10:17:59 AM 

Printin g Date: Tuesday, August 23, 2011 

Page 1 of 1 

Page 43 of 71 
GLP10-01-01; InteriiTi Repoil 18 

Analysis of PFOA in water samples 

FSIA - Decatur. AL; June 2011 

Results Name: kll0715a.rdb 

• Sample Name:-k110715a020r Sample tO;*11003-2&-iar 

• PMk Name:'PFOA' Uaw(e():'413^XXV369.000Da,413.0( 

• Comment-5.0no/mLFCitdkiMaQWWer Anrtotafcn:'' 

Sample Index: 30 

Sample Type : 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modified : 

Pcoc . Algorithm: 

Hois e Percentag e 

Standar d 

5.00 ng/mL 

5 . H ng/mL 

7/15/201 1 

10:28:2 2 PM 

Yes 

Specif y Paramet e 

90 

Base . Sub. Window: 1.00 min 

Peak-Split . Fact r : 3 

Report Largest Peot : Yes 

Min. Peak Heigh t 

Min. Peak Illdth : 

Smoothing Width: 

RT Hindo«: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

Area : 92 

Height : 

Star t Time: 

End Time: 

0.0 0 cp s 

0.0 0 se c 

30. 0 se c 

15.4 min 

No 

Manual 

15.4 min 

7151 counts 

.2l6t00 6 cps 

15.3 min 

15. 7 min 

1.20»6-

1.15*6-

1.10e6-

1J)5»6-

IJXM -

9.50e5-

ajXtoS8.50e5-

SJXJeS7.50e5-

7J)0e5-

' 6.50e5-

exoes5J0e5-

5.00e5 

4.50e5' 

4J00t5-

3.50*5-

3.00e5-

2.50eS' 

2.00a5-

130e5-

1.00eS5.00e4' 

0.00-

135 14.5 15.0 15.5 16.0 

I

SHnpteName:-V110715a029- Sampla ID: "Solvent Blanir FUe:-k110715a.wir 

P«ak Name: TFOA' MaM(et): "413.000/369.000 Da ,413.000219.000 01,413.000/1 G9.000 Oa" 

Comment:-MliQWaterTN11-0234' Arvtotsfion:' 

Sample Index: 29 

Sample Type: Unknown 

Concentration: N/A 

Cal c 

Acq. 

Acq. 

ulate d Cone: 

Dat e 

Time 

Modified : 

Proc 

Base 

Peak 

Repo 

Min. 

Min. 

Alg rithm: 

Percentag e 

Sub 

-Spl i 

t La 

Peak 

Peak 

Smoothing 

RT Window 

Expe 

Use 

Int . 

Kete 

< 0 

7/16/201 1 

1:39:13 AM 

No 

Specif y Pa 

90 

Window: 1.00 

- Factor: 3 

qest Peak: Yes 

Height 

Width: 

Width: 

:t6 d RT: 

lela t 

Type 

itio n 

Height : 

Sta r 

ve RT: 

Time: 

End Time: 

0.0 0 

0.0 0 

0 

30. 0 

15-7 n 

No 

Base To Ba 

15. 5 

5415 co'j 

.536*003 

15. 5 

15. 6 n 

[

Sample Name: 1(1107158030' Sample ID: 'LCS-110714-1- File: 'V1107lSa.Vi4r 

P««k Name: 'PFOA' Hau(e«): -413.00(V3e9.000 03,413.000/219.000 Oa ,413.000^69.000 DaComment 'D.Sppb LCS" Annotation:"" 

lamplt Index : 30 

I

Saniple Name: 1(110715a03T Sample ID: "LCS-110714-

Peak Name: -PFQA" Ma««<e«): "413.00Cra69.000 D8.413.a 

Comment:-Sppb LCSConcentiati c 

Calculate d t 

Acq. Date : 

Acq. Time: 

Modified : 

Ptoc . Algo r 

Nois e Percei 

n : 0.49 8 

one ; O.510 

7/16/201 1 

1:59:18 AM 

Ves 

thm: Specif y Pa 

tage : 90 

Base . Sub. Window: 1.00 

Peak-Split . 

Report Largi 

Min. Peak He 

raetor : i 

St Peak: Yes 

i^ht : 0.0 0 

Min. Peak Hidth : 0.0 0 

Smoothing W; 

RT Hindow: 

Expecte d RT 

Use Relativ e 

!nt . Type: 

Retentio n T: 

Area : 

Height : 

Star t Time: 

dth : 0 

30. 0 

ng/mL 

ng/mL 

amete 

min 

c p s 

15. 5 min 

RT: No 

Base To Ba e 

(16: 15.5 min 

963879 cou 

1.38etO05 cp s 

15.3 n in 

Concentiati o 

Calculate d C 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algoc i 

Nois e Perce r 

1.96 

5.16 

7/16/201 1 

3:02:3 8 AM 

N^ 

Specif y Pa r 

90 

Base . Sub. Window: 1.00 

Peak-Split . 

Report Large 

Min. Peak He 

•act r : 3 

St Peak: Yes 

qhr 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e 

Int . Type : 

Retentio n Ti 

Height : 

Star t Time: 

End Time : 

KT: 

0.0 0 

0.0 0 

0 

30. 0 ; 

15. 7 m 

No 

Valle y 

15.4 n 

9252077 eoun 

.27e+006 c 

15-3 n 

15. 7 m 

ng/mL 

ig/mL 

c p s 

po 

.n 

.n 

:s 

pa 

in 

in 

13^ 13.5 14.0 

125e6' 

120e6' 

1.15o6 

1-10e6 

1.05e6 

1.00e6 

9.50e5 

9-0Oe5 

8-50e5 

8.00e5 

7.50e5 

. 7.00B5 

: 6.50e5 

6.00e5 

550e5 

5-00*5 

4.50e5 

4XX)e5 

3.50e5 

3.00a5 

2-50e5 

2.00e5 

1.50e5 

1.0005 

5J)0e4 

0.00 •-t^4BMi^>i*NMm>ipl*-^ 

14.5 15.0 155 16.0 16.5 17.0 17.5 18.0 

Data printed by STW 

Printing Time: 10:27:35 AM 

Printin g Date: Tuesday, August 23, 2011 

Page 1 of 10 

Page 44 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

*ETS-Kirk Results Name: kll0715a.rdb 

I SatnplaNanw:'V110715a03tr Samfte ID:-LCS-110714-r Rle:*V110715a.M«r 

I PeakNaiTM:-PFOA- Ma««<e«):-413.000/369.000Da,413.00Qr219J]CODa,413.00(V169.000DaI Comment-SOpt^ LCS' 

Sample IndcK: 36 

Sample Type : QC 

Concentcation : 29. 9 

Calculate d Cone: 28. 3 

Acq. Date : 7/16/2011 

Acq. Time : 4:06:0 3 AM 

Modified : Yes 

Pcoc . Algorithm: Specify Pa 

Uois e Percentage : 90 

Base . Sub. Window: 1.00 

Peak-Split . Factor: 2 

Report Largest Peak: Yes 

Min. Peak Height : O.OC 

Min. Peak Width: O.OC 

Smoothing Width: 0 

RT Window: 30. 0 

Expecte d RT: 15.7 

Us6 Relativ e RT: Ho 

Int . Type : Manual 

Retentio n Time: 15.5 

ng/nl. 

ng/mL 

lamet e 

min 

c p s 

aln 

Area : ^6053927 counts 

Height : S.84e*006 

Star t Time : 15. 3 

End Time: lo.O 

c p s 

Din 

min 

135 14.0 15.0 15.5 16.0 16.5 1' l o 17.5 

I

Sample Name: 1(110715a04r S«mplB ID: TCS-110714-10" Fie: 1(110715a.wHT 

Peak Hame: TFOA" Haas(M): "413.000/369.000 Oa .413.000/219.000 Da ,413.000/169.000 Da' 

Comment:-0.5ppb LCS ECF- Annolatlon:"" 

Sample Index : t 3 

Sample Type: QC 

Concentration : 0.4 98 ng/mL 

Calculate d Cone; 0.522 ng/mL 

Acq. Date : 7/16/201 1 

Acq. Time: 6:31:0 1 AM 

Modified : 

Perr: :entage : 

. Hindow: 

Yes 

90 

Peak-Split . Factor: 3 

Repiort Largest Peak; Yi 

Min. Peak Height : 0. 

Min. Peah Width: 0. 

Smoothing Width: 0 

RT Window: 30. 0 

Expecte d RT: 15,7 

Use Relativ e RT: No 

Retentio n 1 

Height : 

Manu; 

I

Satrtile Name: "k110715a046r Sample IO:-LCS-110714-13' Fie: ''I(1107l5a.w4r 

Peak Name: "PFOA" Mattes): '413.000/369.000 Da,413.000/219.000 Da,413.000/169.000 Da" 

Comment'5ppb LCS ECr Annotatton:-

Sample Index: 46 

Sample Type: OC 

Concentration : 4.99 ng/mL i rawR 

Calculate d Cone: 4.96 ng/mL '•'~~ ' 

9.50eS9.00e5-

5 - MQ II I 

8.50e5-

8.00e5-

7.50e5-

^'= 7.00e5-

6.50e5-

6.00e5-

I 5.50e5-

f 5.00o5-

4.00e5 

3.50 ^ 

3.00eS 

2-50*5 

2.00e5 

1.50e5 

1-00*5 

5.00M 

0.00 

I

Sample Name: "kl 107l5a049- Samite ID: "LCS-110714-16" Fie: -fc110715a.st«r 

Peak Name: TR3A" MaM(e«): '413.000/369.000 Da,413.000/319.000 Da .413.00^169.000 Da' 

Comment: '30ppb LCS ECP Amotation: ~ 

Sample Index : 49 

Sample Type: QC 

Acq. 

Modi 

Proc 

Base 

Peak 

Min. 

Min. 

Smoo 

RT W 

Date 

Time 

led : 

Algorithm 

Sub Windo 

7/16/201 1 

7:37 

Y 

Split . Factor: 

t Largest Peak: 

Peak 

Peak 

hin g 

ndow 

Hcighi 

Hidth 

Width 

Expecte d RT: 

Use Rela c 

Int . 

Retentio n 

Area 

Height : 

ve RT 

Tlmt,: 

8) 

26 AM 

^ tV Pa 

90 

1.00 

3 

Yes 

0.0 0 

0.0 0 

0 

No 

Man a i 

15.5 

9B047 

1.02e 006 

Concentration : 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Nois e Percentage : 

Base . Sub- Hindoi. 

Peak-Split . Fact o 

Min. Peak Height : 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expecte d RT: 

L'se Relativ e RT: 

Int . Type : 

Retentio n Time: 

Area : 502 

Height : 5 

Star t Time: 

End Time: 

29. 9 ng/mL 

31. 3 ng/mL 

7/16/201 1 

8:40:4 6 AM 

Yes 

Specif y Paramet e 

90 

1.00 min 

a k : Yes 

0.0 0 cp s 

0.0 0 se c 

0 po 

30. 0 se c 

15. 7 min 

No 

Manual 

15-5 rain 

17005 counts 

39e^006 cps 

IS.O min 

16. 0 min 

15.0 15.5 16.0 16.5 17.0 175 14.5 15.0 15.5 16.0 16-5 17.0 17.5 18.0 

Data printe d by STW 

Printing Time: 10:27:35 AM 

Printin g Date: Tuesday, August 23, 

Page 2 of 10 

Page 45 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur. AL; June 2011 

Results Name: kll0715a.rdb 

I

Sampto Name: 1(1107158185" Sampto ID:"GLP1CW)1-01-ie-093" FUB: "k110715a.»«r 

PaakNaiM:'PFQA' Mats(M):"413.00(V369.000Da.413.000/219.000Da,413.00(yi69.000Da' 

Comment "DAL GW 1375 0110624' Annotation:" 

Sample Index: IBS 

Sample Type: Unknown 

Concentration: H/A 

Calculated Cone: 

Acq. Date: 

Acq. Tin*: 

Modified: 

Proc. Algorithm: 

Noise Percentage 

0.284 

7/18/2011 

8:35:05 AM 

Yes 

Specify Pa 

90 

Base, Sub, Window: 1.00 

Peak-Split. Factor: 3 

Report Largest Peak: Y«9 

Min. Peak Height 

Min. Peak width: 

Smoothing Width: 

RT Window; 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

0.00 

0.00 

0 

30.0 

15.5 n 

No 

Base To Ba 

IS.E D 

Area: 553876 cou 

Height: 

Start Time: 

End Time: 

.21e«0O4 

15-2 n 

15-6 B 

I

San4)leName:*k110715a194^ SamplalD:"OLP1(>O1-01-1M}98- Fle:'k1l0715a.wHr 

Peak Name: "PFOA' MaH(ea): "413.000/369.000 Da ,413.000/219.000 Da ,413.000/169X00 Da" 

Comment:-DALGUV137L0l10e2r Arwwtatkin;" 

Sample Index: 194 

Sample Type: Unknown 

Calculated Cone: 0.372 ng/mL 

Acq. Date: 7/18/2011 

Acq. Time: 11:16:14 AM 

)ifie< 

Proc. Algorithm: 

Hoise Per 

Baae. Sub 

Peak-Spll 

entage 

. Fact 

Specify 

90 

Parame 

-: 1.00 m 

St: 4 

Report Largest Peah: Yes 

Min. Peak 

Hln. Peak 

Smoothing 

RT Window 

Height 

Width: 

Width: 

Expected RT: 

Use Relat 

Int. Type 

Retention 

Area: 

Height: 

Start Tlmi 

End Time: 

ve RT: 

Time: 

0 

0 

0 

30.0 

15.4 

No 

Base To 

15.4 

396B 

00 c 

00 a 

min 

Base 

ounts 

;.90e-f004 cps 

15.2 

15.6 min 

tecs -

e c 

9.0M 

8.5e4' 

8.0e4' 

7.5e4-

7.0e4 

6.5e4 

e.0»4 

5.5e4 

5.0»4 

4.5e4' 

4.0e4' 

3.5e4 

3.0M 

2,5M' 

2.0e4' 

1.5e4 

1.0e4-

5000.0-

o.oV>*4(«f«««!^ 

13.0 135 

I

Sampto Namo: 'kl1071Sa20r Sample ID: "OLP1001-01-18-108^ FUe: 'V1107l5a.wHr 

Peak Name:"PFOA- Mata<e«):"413.00(y369.000Da,413.00Q/219JX»Da,413.00(Vl69.000DaComment-DAL GW138L 0110630" Amotatfan:"" 

Satnple Index: 208 

Sample Type: Unknown 

Concentration: N/A 

Calculated Cone: 0.891 ng/mL 

Acq. Date: 7/ie/;01 ] 

Acq. 

Modi 

Ptoc 

Hols 

Base 

Peak 

Time 

led: 

Algorithm: 

Pe r 

Sub 

Spll 

Windo 

. Fact 

4:43 

Y« 

Spec 

Report Largest Peak: 

Peak 

Peak 

Smoothing 

RT Hindow 

Expe 

Use 

Int. 

Rete 

Area 

Height 

Width: 

Width: 

,ted RT: 

-.elat 

Type 

tlon 

Height: 

Stat 

ve RT: 

Time: 

1 

44 

fY 

90 

PM 

Pa 

1.00 

3 

Y 

<f> ' 

f> 

.4 

No 

Base 

1 

165S909 

Time: 

End Time: 

.04e^ 

1 

To 

.4 

s 

DO 

00 

Ba 

005 

.6 

I

Sampto Name:'k110715al99" Sample ID:N3LP1OO1-01-18-103' Fle:-k1107lSa.wtr 

Peak Name: TFOA" MaM(ea): '413.OOCV369.000 Da.4l 3.000319.000 Da.413.000/169.000 DaComment "DAL OWISSR 0110630 (dl 1:10)" AnnotBtkin: "^ 

Sample Index: 199 

Sample Type: Unknown 

Concentration: H/A 

Calculated Cone: 294. ng/mL 

Acq. Date: 7/19/2011 

Acq. Time: 1:32:30 PM 

Proc- Alg 

Noise Per 

Base. Sub 

Peak-Spll 

Report La 

Min. Peak 

Min. Peak 

Smoothing 

RT Window 

rithm 

entag' 

Windc 

Spec 

. Factor: 

gest 

Heigh 

Width 

Width 

Expected RT: 

Use Relat 

Int. Type 

Retention 

Area: 

Height: 

ve RT 

Time: 

eak: 

30 

1 

fY 

90 

Pa 

1.00 

4 

0 

0 

0 

0 

.4 

No 

Base 

1 

4758369 

Start Time: 

End Time: 

5.33e* 

1 

To 

.4 

00 

.0 

00 

on 

Ba 

13.0 13J 19.0 10.5 17.0 17.5 

Data printe d by STW 

Printin g Time: 10:27:35 fiM 

Printin g Date; Tuesday, August 23, 

Page 3 of 10 

Page 46 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Results Name: kll0715a.rdb 

TM

Sample Name:'V110715a139' San^to ID:'OLP10«1-O1<l8.05g" File:VI107l5a.vrir 

Peak Name: "PFOA" Ma«a{e«): '413.000369.000 Da,413.000/219.000 Da,413.000/169.000 Da' 

Comment:"OALGW134S011062Gr Annotation:' 

Sample !nde>r: 139 

Sample Type: Unknown 

Concentration : N/A 4Je5 -

Calculate d Cone: 9.o7 ng/mL 

Acq. Date : 7/17/;01 1 4.0o5-

Acq. Time: 4:ZZ:16 PM 

3.8e5-

3.605-

3.4*5-

3.205-

3.0e5-

2.8e5-

2.6e5-

2.4e5-

I 2.0e5-

I 

1Ae5-

1.6«5-

1.4e5-

1.2e5 

1-0e5 

8.0e4' 

e.0e4' 

4.0e4' 

Z0e4 

IT 

Modlf 

Ptoc. 

(Jolse 

Bare. 

PeakRe por 

Min. 

Min. 

led : 

A l g 

P e r 

<;pli 

- U 

=pak 

Smoothing 

RT Wl 

Ex pec 

Y 

srlthm: Spec 

entage: 

Window: 

. Factor 

gest Pea 

Height: 

Width: 

Width: 

;ed RT: 

Use Relat 

Int . 

Retei 

Area: 

Heigh 

Sta n 

End T 

Type 

Lion 

ve RT: 

B 

Time: 

3535 

4 . 

Time: 

ine : 

: 

10 

1 

q 

I V 

9 0 

Parameters -

1.00 n 

Y e s 

0 

0 

0 

. 4 

Ho 

s e T o 

15.4 

9 3 

0 0 

0 0 

m i n 

Base 

m i n 

6e-t00S cps 

1 

1 

- 1 

. 6 

m i n 

m i n 

n 

p s 

point s 

0.0 

13.0 13.5 14.5 15.0 155 

lOiM,. 

I

SaiTpleName:"k1l0715a08Sr Sample ID:"GLI»HM1-01-1W12S" Flte:"k110715».wW 

Peak Name: 'PFOA" MaM(M): "413.000/369.000 Da.413.000/219.000 Da.413.000^69.000 Da" 

Conment*DAL0W131S 0110622 (dlt 1:10)-

5ampleName:lc1107l5a076" Sampto ID:-OLP1OO1-D1-18-0l6r ne:'kll0715a.Mir 

Peak Name: TFOA' MaM(o«}: "413-000/369.000 Da .413.000^19.000 Da.413.000/16S.000 Da" 

Comment:'DALGWl30L0110S30(dil1:10r Amwtatkin:"" 

Sample Index : 76 

Sample Type : Unknown 

Concentcation : N/A 

Calculate d Cone: 66. 8 ng/mL 

Acq. Date : 7/16/2011 

Acq- Time: 6:11 :26 PM 

Percentage : 

Sub. Wind! 

Nolsi 

Base 

Peak-Split . Facto i 

Report Largest Pe: 

Min. Peak Height : 

Min. Peak width : 

Smoothing width : 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type: E 

: Specify ParametE 

. .39e+006 cps 

15.B min 

1.4e6' 

1.3e6' 

1.3e6' 

1.2e6-

1-2e6-

1.1e6-

1.1e6-

1.0»6-

9.5e5-

9.0e5-

e.5e5-

6.0e5 

7.5e5-

7.0e5-

6.5e5-

6.0e5-

S.5e5-

5.0e5-

4.5e5-

4.0e5-

3.5e5-

3.0B5-

2.505-

2.0e5-

1.5e5-

I.OeS13.0 13.5 

I

SanvleHame:"k1107lSa098r Sampto ID:-OLPlOO1-01-1&«30^ Fle:'kl10715a.wifr 

PMk N<me: 'PFOA" MaM(et); "413.000^69.000 Da.413.000/219.000 Da,413.000/169.000 Da" 

Commert:"DALGW131L0110622{dai:10r " -

Sample Index : 98 

Sample Type : 

H/A 

Ai:q. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Nois e Percentag e 

Base . Sub. Windo 

Peak-Split . Fac t 

7/16/;01 1 

10:4S:2 7 PM 

Yes 

Specif y Par 

90 

: 1.00 

t : 3 

Report Largest Peak: Yes 

Min. Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Hindow: 

Expected RT: 

Use Relativ e RT: 

Int . Type: 

Retentio n Time: 

0.0 0 

0.0 0 

0 

30. 0 s 

15. 7 m 

No 

Manual 

15.4 m 

Area : 1006429 coun 

Height : 

Star t Time: 

End Time: 

-21e-f005 CF 

15. 1 m 

15. 6 m 

120e5 

1.15e5 

1.10e5 

1.05e5 

1.00e5-

9.50ft4 

9.00e4' 

850e4' 

a00e 4 

7-50*4-

7JX>e4-

6.50e4-

6.00e4-

5.50*4-

5.00*4-

450*4-

4.00e4 

3.50*4 

3.00*4 

2.50*4 

2.00e4 

1.50M 

Sample Type : 

Concentl a Ion : 

Calculate d Cone: 

Acq. Oate 

Acq. Time 

Modified: 

Proc . Algorithm: 

Nois e Per 

Base . Sub 

Peak-Spll 

Re|)ort La 

Min. Peak 

Min. Peak 

Smoothing 

RT Window 

entag e 

Unknown 

H/A 

S3.9 

7/17/2 0 

1:55:56 

Yes 

Specif y 

90 

AM 

Pa 

Window: 1.00 

. Fact 3 t: 4 

gest Peak: Y 

Heigh t 

Width: 

Width: 

Expected RT: 

l'se Rela t 

Int . Type 

Retentio n 

Area : 

Height: 

Star t Tim 

End Time: 

ve RT: 

Time: 

0 

0 

0 

30. 0 

15.4 

No 

Base To 

15.4 

1654B643 

.87e*00 

15. 1 

15. 9 

00 

00 

Bas 1.1*6-

1.0e6-

7.0*5 

6.0e5 

5.0*5 

4.0*5 

3.0B5 

Z0*S 

1.0*5 

15.0 155 16.0 16-5 17.0 175 

Data printed by STW 

Printing Time: 10:27:35 AM 

Printin g Date: Tuesday, August 23, 2011 

Page 4 of 10 

Page 47 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Results Name: kll0715a.rdb 

I

San^Nam:-k110715a1ir Sample IO:-GLP1(M)1-01-1MH5- FilB:"1c110715a. 

PMk NanM: -PFOA- MaM(«a): '413.000/369.000 Da.413.OaQr219.0OO Oa.413.00Wie9.000 Da' 

Cotim«*-nALGW133R0110630(dfl1:10)" -

Sample Index : 

Sample Type : 

Calculate d Cone: 

Acq. Date : 

Acq- Tin« : 

Modified : 

Proc . Algorithm: 

Nois e Percentag e 

Base . Sub. Windc 

Peak-Split . Fac t 

Report Largest P 

Min. Peak Heigh t 

Mlh. Peak Width: 

Smoothing Width: 

RT Window: 

Elxpected RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

117 

Unknown 

N/A 

loe. 

7/17/201 1 

8:36:5 5 AM 

Yes 

Specif y Pa 

90 

i: 1.00 

o r : 3 

,ak: Yes 

: 0.0 0 

0.0 0 

30. 0 

15.4 n 

No 

Base To Ba 

15.4 1 

Area : 1B890925 co 

Height : 

Star t Time: 

End Time: 

2.10et00 6 

15.1 J 

15.8 a 

13.0 13-5 14.5 15-0 15.5 KJO IBS 17.0 17.5 

I

Sample Name: •V110715a112' Sample ID:'0LP1OO1-01-1ftO4Q^ Fae:-k110715a.wtr 

Peak Name: "PFOA- Mae«(es):-413XXXV369.000 Oa ,413.000219.000 Da,413.00CV1Ga.0OO Da" 

Comment:"DALGW133S0110630(dil1:10)" Amotatton:-

Sample Index: 112 

Sample Type 

Cal c 

Acq. 

Acql a te d Cone 

Date : 

Time: 

Modlfled : 

Proc 

Nois 

Base 

Peak 

Repo 

Min. 

Algor. 

Percen 

thm 

tag e 

Unknown 

7 

b 

N/A 

311 . 

17/20 

51:4 9 

Yes 

Specif y 

Sub. Window: 

Split . 

t Largi 

Peak HI 

Peak H 

Smoothing H 

RT Window: 

Expecte d RT 

Faci 

3 t Pea 

Igh' 

d t h 

d t h 

90 

1 

AM 

Pa 

1.00 

3 

: Yes 

0 

0 

0 

30. 0 

15.4 

00 

00 

13.0 13-5 14.5 15.0 15-5 16-0 165 17.0 ^^ S 

I

Sanv)le^ame:'Vl10715a13O' Sample ID:'OLP10«1.«1-1»4)54- Fae:-k110715a.viirr 

Peak Name: "PFOA- liAaM(e(): -413-000^369.000 Da,413.000219.000 Da ,413.000/169.000 Da' 

Comment:-DALQW134L0110628(diI1:10}- Amotatkm:*" 

Sample Index : 130 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 527. ng/mL 

Acq. Date : 7/17/201 1 

Acq. Time: 1:12:27 PM 

I

SanpleName:i(1107lSal03r Sample ID:-GLP 1001-01-18-035" FUe:-k1l0715a.wHr 

Peak Name:'PFOA' MaM(e*):'413.0DtV369.000Oa,413.000/219.0O0 Da,413.00CV169.000 DaComment "DALGWl33L0110630{dl 1:10)" -

Sainple Index : 103 

Sample Type : 

N/A 

Calculate d Cone: 

A^q. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Nois e Percentage : 

Base . Sub. Wlndoi 

Peak-Split . Fact o 

Report Largest P( 

Min. Peak Height : 

Min. Peak Width: 

Smoothing Width: 

RT window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

230. 

7/17/201 1 

:':42:0 1 AM 

Yes 

Specif y Pa 

90 

: 1.00 

r : 4 

a k : Yes 

0 

30. 0 

15.4 n 

No 

Manual 

15.4 1 

Area : 8260473 cou 

Height : £ 

Star t Time: 

End Time: 

.4 9e-f005 

15.0 n 

15.7 n 

ng/mL 

9.0*5-

8.5*5-

8.0eS' 

7.5*5-

7.0*5-

6.5*5-

6.0*5-

53*5-

5.0e5-

4.5e5-

4.0e5-

3.5*5-

3.0*5-

2.5*5-

2.0e5-

1-5e5 

1.0e5' 

5.0e4-

0.0-

Modified : 

Proc . Algorithm: 

Nois e Pe r 

Base . Sub 

Peak-Spl l 

Reiiort La 

Min. Peak 

Min. Peak 

Smoothing 

. Windc 

Yes 

Specif y Pa 

:. Facto r 

rgast Pea 

Heigh t 

Width: 

Width: 

iT: 

Use Relativ e RT: 

Int . Type 

Retentio n 

Area : 

Height : 

Star t Tim 

End Time: 

Time: 

IB 

90 

1.00 

4 

: Yes 

0.0 0 

0.00 

0 

30. 0 

15. 1 n 

No 

Base To Ba 

7 

-

15.4 

4 22 CO 

6e-^006 

15. 0 D 

15. 9 n 

fcjl'l ',1, 1 iii|i|i|,il|IMiHlli(i|i| HH, , 

145 15.0 15.5 la O 16.5 17.0 17.5 

Data printe d by STW 

Printing Time: 10:27:35 AM 

Printin g Date: Tuesday, August 23, 2011 

Page 5 of 10 

Page 48 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Results Name: kll0715a.rdb 

(

Sample Name: 'Vt10715a18ff' Sample ID: "GLPl&01-01-18-08tf- File: -k1l0715a.viilrr 

Peak Nam*: "PFOA" Ma*a<as): "413.000/369.000 Oa.413.000/219-000 Da,413.000/169.000 Da" 

CorTnMnt-DALGW136S011063D<<ai1:10)" Annotation:' 

Sampl. " 

Sample Type : Ur,kn< 

im: Specif y Paramet* 

Report Largest Peak: Ye: 

Min. Peak Height : O.t 

Min. Peak Width: O.C 

Smoothing Width: 0 

RT Window: 30. 0 

Expecte d RT: 15,4 

Use Relativ e RT: No 

Retentio n Time: 15.4 

Area : 22653047 ; 

Height : 2,o2o-t006 

Star t Time: 15. 0 

End Time: 15. 0 

I

Sample Name:'Tc110715a171" Sample ID:-GLP1WI1*1.1W)84" Fle:-k110715a.wMr 

Peak Name: "PFOA" M&*s(e*): "413.000/369.000 Da ,413.000/219.000 Da .413.000/169.000 Da" 

Commert:"DALGW136L0110630{dai:10)- AnnotaOon:" 

3.4*5-

3.2*5-

3.0*5-

2.8*5-

2.GeS' 

2.4*5 

2.2e5 

2.0eS1.ee5-

1.6*5-

1.4*5-

1.2*5-

1.0*5-

8.0*4-

6-0e4-

4.0*4-

2.0*4-

Sample Type: 

Concentration : 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Nois e fercentag e 

Unknown 

N/A 

79. 7 

7/ia/201 1 

3:39:4 7 AH 

Yes 

Specif y Pa 

90 

Base . Sub. Window: 1.00 

Peak-Split - Factor: 3 

Report Largest PeaK: Yes 

Hin . P«alc Height 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

0.0 0 

0.0 0 

0 

30. 0 

lS- 7 i; 

No 

Manual 

15.4 1 

Area : Z92501S cou 

Height : 

Star t Time: 

End Time: 

.4ee-tOOS 

15. 1 n 

15. 6 D 

13.5 

^.,t,m,0mtmiimmmf i m ^^MMIMV^ ^ 

I

Sample Name: •V1107l5a2l3f Sample ID; "QIP1&01-01-18-113- Rle:1(110715a.wtr 

Peak Name: "PFOA" Mat«(e«): '413.000/369.000 Da.413.000/219JX)0 Da.413-00(V169.000 Da' 

Commert"DALGW138S0110630(dil1:lO)" Annotatton:-

Sample Index : 213 

I

SanvleName:"k110715a22r SamplBlD:-GlPl(W)l-01-l8-1ir Fl*:"k1l0715a.vi*fr 

Peak Name: TFOA' hlaM(e(): "413-000/369.000 Da.4l3.00(V219.000 Da,413.000/169.000D«" 

Camnient"OALGWCW26C0110622{dai:l0)" Amotatkm:-

Sample Index: 222 

Sample Type: 

Concentration : 

Calculate d Cone: 

Acq. Time: 

Kodllled : 

Proc . Algorithm: 

Nois e Percentag e 

H/A 

155 . 

7/18/201 1 

6:30:0 4 PM 

Ye« 

Specif y Pa 

: 90 

Base . Sub. Window: 1.00 

Peak-Split . Facl 

Report Largest 1 

Hln. Peak Height 

Min. Peak Hidth : 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

o r : 3 

lak : Yes 

: 0.0 0 

0.0 0 

0 

30. 0 

15.4 

No 

Base To Ba 

15.4 D 

Area : 5604 337 cou 

Height : 

Star t Time: 

End Time: 

7.07e*OO5 

15. 1 n 

15. 7 r. 

N/A 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modified : 

Proc - Algorithm: 

Hois e Percentag e 

4 27 . 

7/18/201 1 

&:40:19 P 

Yes 

ng/mL 

Specif y Paramet e 

90 

Base - Sub. Window: 1.00 

Peak-Split . Fact r : 4 

ReiMct Largest Peak: Yes 

Min. Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

L'se Relativ e RT: 

Int . Type : 

Retentio n Time: 

min 

0.0 0 cp s 

0.0 0 se c 

0 

30. 0 

15-4 

No 

Manual 

15.4 

Area : 15087641 c 

Height : 

Star t Time: 

End Time: 

.89e*006 

15. 0 

IS. a 

cps 

min 

1.8*6 

1.7*6 

1.6*6-

1.5*6-

1.4*6-

1.3ee< 

1.2e6 

1.1e6-

1.0e6-

9.0*5-

8.0*5-

7.0*5-

6-0*5-

5.De5-

4.0*5-

3.0*5-

2.0*5-

1.0*5-

0.0 

145 15.0 15.5 16.0 16.5 17.0 17.5 

Data printed by STW 

Printing Time: 10:27:36 AM 

Printin g Date: Tuesday, August 23, 

Page 6 of 10 

Page 49 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Results Name: kll0715a.rdb 

T

SarTpleNBme:'k110715a22r Sample ID: "OLP1O4)1-01-18-123* FUe:-k110715a.wtfr 

Peak Name: 'PFOA" Ma*a<ae): '413.000/369.000 Da,413.000/219.000 Da,413.00(V169.000 Da" 

Co(Tvnent"DALGWCVV26L0110622(<lM:10)" AnwtalNn: ~ 

Sample Indei-.: 227 

Sample Type: Unknown 

N/A 

Calculate d L 

Acq. Time: 

Peak-Split . Factoi 

Report Largest Pe; 

Min. Peak Height : 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Elxpected RT; 

Vst, Relativ e RT: 

Int . Type: 

Retentio n Time: 

Area : 223! 

Height : 2. 

leters - MQ II I 

I

S«[TpleN«m*:Tcl107l5b24r Sample ID: "GLPIOOWI-IS-ISS" Hle:'V110715a.wii«r 

Peak Name: "PFOA" MaM(e«): "413.000/369.000 Da.413.000/219-000 Da,41S-OOIVI69.000 Da' 

CornnenfOALOWUIROlloeao r Aimotatton:"" 

Sample Index : 251 

I

Sample Name:'V110715a23ff- SamplalD:"GLJ>l(M)1-01-18-128- Fle:"k110715a.w4r 

Peak Nam*: TFOA" Maea(e«): "413.000/369.000 Da ,413.000/219.000 Da ,413.000/169.000 Da' 

Comment:"DALGWl40R0110622(dl1:10r Annotatk>n:~ 

Sample Inde.-i: 236 

Sample Type 

Cone. ratlo i N/A 

Cal c 

Acq. 

Acq. 

lat e 

Oate 

Time 

Modified : 

Pto c 

Nols 

Base 

Peak 

Repo 

Min. 

Min. 

i Cone 

Algorithm 

Pe r 

Sub 

Spl i 

entag 

Wine 

- Fac 

t Largest 

Peak 

Peak 

Smoothing 

RT W 

Expe 

ndow 

Heigh 

Width 

Width 

t e d RT: 

Use Rela t 

Int . 

Ret e 

Area 

Tvpe 

Height : 

Sta r 

ve RT 

Time: 

: 127. 

7/19/201 1 

3:16:5 1 AM 

Yes 

Specif y Pa 

r: 90 

ow: 1.00 

'eak : Yes 

0.0 0 

0 

30. 0 

15.1 n 

No 

Valle y 

15.4 n 

46044B7 cour 

Time: 

End Time: 

5.e6e-t005 

15. 1 1 

15. 6 n 

1^.0 15.5 16.0 165 ^^si 17 5 

Sample Name: 'Vl10715b2Sr Sample ID: "OLP 10^1-01-18-140" Pie: 'k110715a.Jrr 

Peak Nam*: TFOA' lite«s(ea): "413.000/369.000 Oa.413.00CU219.000 Da,413.000/169.000 DaComment "DALGW 142R0 110622 (dl 1:10)' Amotatkin:-" 

Sample '. 

Sample Type: 

Calculate d Cone. 

Acq. Time: 

Modified : 

Proc . AlgorithmNois e Percentag . 

Unknown 

H/A 

1.59 ng/ 

7/19/:01 1 

10:07:2 7 AM 

Yes 

Specif y Parame 

: 90 

Base . Sub. Window: 1.00 mi 

Peak-Split - Facl 

Report Largest 1 

Min. Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type: 

Retentio n Time: 

o r : 3 

eak : Yes 

: 0.0 0 c 

0.0 0 s 

0 

30. 0 se c 

15.4 min 

No 

Manual 

15.4 min 

Sample Type : Unkf 

Concentration : 

Calculate d Cone: 

N/A 

50. 1 n 

Acq. Date : 7/19/201 1 

Acq. Time: 1 

Modified : 

;53:1 7 AM 

Yes 

Proc - Algcrithro : Specif y Par a 

Nois e Percentage : 

Base . Sub. Window: 

Peak-Split . Facto r 

Report Largest Pea 

Min. Peaf. Height : 

Min. Peak Width: 

Smoothing Width: 

RT Window; 

Expecte d RT: 

Use Relativ e RT: 

int . Type: B 

Retentio n Time: 

Area : 1857 

Height : 2 . 

Star t Time: 

End Time: 

90 

1.00 

4 

: Yes 

0.0 0 

0 

30. 0 s e 

15-4 inl 

No 

s e To Base 

15-4 ml 

78 count 

le-tOOS cp 

15-1 ml 

15. 6 ml 

2.4*5 

2.3*5-

2.2e5-

2.1eS 

2.0e5-

1.9*5-

1.8*5-

1.7*5-

1.6*5-

1.5*5-

1.4*5-

1.3e5-

1.2e5-

l.leS1.0*5-

9.0*4-

8.0*4-

7.0*4-

6.0*4-

5.0*4-

4.0*4-

3.0*4-

2.0*4-

1.0*4-

m^t^mlttfi^Sia^afi 

'e;73 17.06 17.39.^1751 

Data printe d by STW 

Printing Time: 10:27:36 AM 

Printin g Date: Tuesday, August 23, 2011 

Page 7 of 10 

Page 50 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Results Name: kll0715a.rdb 

n

SanvIa Name: "^107151)261- Sanqile ID:-GLP1(V01-O1-18-14r FUe: "k110715a.vrir 

Peak Name: "PFOA" Ma**<**): "413.000i369.000 Da.413.0O0i/219.0OODa.413.O0CV169.00O Da' 

ConvtMrt:"OALGW143ROll0622<dil1:10r Annotatkm; 

Sample Type : 

Concentration : 

Calculate d Com 

Acq. Time: 

23. 3 r 

7/19/201 1 

3:03:0 2 PM 

Modified : Yes 

Proc . Algorithm: Specif y Parameters - KQ II I 

Nois e Percentage : 90 

Bafe . Sub. Window: 1.00 min 

Peak-Split . Factoc : 5 

Report Largest Peak: Yes 

Min. Peak Height : 0.0 0 cps 

Min. Peak V?idth; O.OO se c 

Smoothing Width: 0 points 

RT Window; 30. 0 se c 

Expected RT: 15.4 min 

Vsb Relativ e RT: No 

Int . Type: Base To Base 

Retentio n Time: 15.4 min 

Acea: 4252765 counts 

Height : 5.S3e»O05 cp s 

Star t Time: 15. 1 min 

End Time: 15. 7 min 

I

S«n¥l*Name:"k110715a06r SaF(^>leP:-GIJ>1(«1-01-1W)06- Flle:1c11071^.«ir 

Peak Name: "PFOA" Maca<ea): "413.00(V369JMO D«.413.00CV219.000Da,413.00(V169-000 Da* 

Comnent-DALCW130R0110630<dai:100)- Arawtatkm:-

Sanpl e Index : 62 

Sample Type : 

• Sample Name:-kl10715b266^ Sample ID:"VLPIOOI-Ol-IS-ISO" Ple:-k110715a.wHr 

I Peak Name: "PFOA* MaM<aa): "413.000ir3e9.000 Da,413.00(V219.000 Oa.413.000/169.000 Da" 

• Comment:*DALGW144S0110828Mai;10r Annotatton:"" 

Sample Index : 270 

Sample Type : Unknown 

N/A 

Calculate d C 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . AlgotI 

Nois e Perce r 

one : 52. 1 ng/mL 

7/19/201 1 

4:49:1 2 PH 

Yes 

:hm: Specif y Paramete 

:age : 90 

Base . Sub. Window: 1.00 min 

Peak-Split . 

Report Large 

Min. Peak He 

Min. Peak Wl 

factor: 4 

St Peak : Yes 

ght : 0.0 0 cp s 

1th: 0.0 0 se e 

Smoothing Width: 0 po 

RT Window: 

Expected RT: 

Use Relativ e 

Int . Type : 

Retentio n Tl 

Area : 

Height : 

Star t Time: 

End Time: 

30. 0 se c 

15.4 min 

RT: No 

Base To Base 

lae: 15.4 min 

1927318 counts 

2.3Se*005 cps 

15. 1 min 

15. 6 min 

2.3*5 

2.2e5 

2.1e5-

2.0*5 

1.9e5 

1.8e5 

1.7*5 

1.6*5' 

1.5*5-

1.4*5 

1.3*5 

1.2*5 

1.1*5 

1.0e5' 

g.0e4' 

8.0*4 

7.004-

6.0*4-

5.0*4 

4.0*4-

3.0*4-

2-0*4-

1.0e4-

0.0 

13.0 ;wti 

:entratli N/A 

I

Sampl*N*me:1c110715a071" Samp|e|D:-GLJ>1OO1-01-1fr011" Fi*:"k110715a.wttr 

Peak Name: "PFOA" Maa»(es): '413.000/369.000 Da.413.000/219.000 Da ,413.000/169.000 Da' 

C(Knmen(:*DALGW130S0110630(dHl:10)" Anrwtatkin:~ 

Sample Index : 71 

Sample Type : 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Nois e Percentag e 

7/16/201 1 

1:15:18 PM 

Yes 

Specif y Param 

90 

Base . Sub. Window: 1.00 ra 

Peak-Split . Fact r : 3 

Report Largest Peak: Yes 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type: 

Retentio n Time; 

0.0 0 

0.0 0 

0 

30. 0 se c 

15. 7 min 

No 

Manual 

15.5 min 

Area : 14802990 count 

Height : 

Star t Time: 

End Tine : 

.72e*006 cps 

15.1 min 

15. 7 min 

1 

1.7*6 

1.6*6 

15*6 

1.4*6 

1-3*6 

1J2e6 

1-1*6 

1 ^ 

9J)e5 

8.0e5 

7-OeS 

e^5 

5.0e5 

4-0e5 

3.0e5 

2.0e5 

1.0e5 

15. 

J 

M/A 

ng/mL 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Nois e Percentag e 

7/16/201 1 

4:25:4 3 PM 

Yes 

Specif y Parame 

90 

Base . Sub. Window: 1.00 ml 

Peak-Split . Fact r : 3 

Report Largest Peak: Yea 

Min. Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type: 

Retentio n Time: 

0.00 c 

0.00 s 

0 

30. 0 se c 

15. 1 min 

No 

Valle y 

15.4 min 

Area : 30524073 count* 

Height : 

Star t Time: 

End Time: 

.46e-i-00o cps 

15. 1 min 

15. 6 min 

13.5 14.0 U S 15.0 15.5 10.0 15.0 155 16.0 16.5 17.0 175 

Data printe d by STW 

Printing Time: 10:27:36 AM 

Printin g Date: Tuesday, August 23, 2011 

Page 8 of 10 

Page 51 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA In water samples 

FSIA - Decatur, AL; June 2011 

Results Name: kll0715a.rdb 

I

Sample Name: 'k1107l5a085' Sampis ID: -GLP1CM)1-01-1&«21" FUe: "kl10715a.wir 

Peak Name: "PFOA" Mat*<e«): "413.000069-000 D«.413.00ar219-000 Da.413-00CV169.000 Da" 

Coirm*rt:"DAL<5W131R0110622<(iai:100r Amotaton:-

Sample Index: 65 

Sample Type: Unknown 

Concentration ; N/A 

Calculate d Cone: 2310. ng/mL 4.2*6-

Acq. Date : 7/16/2011 

Acq. Time: 9:21:44 PM 4.0*6-

Modi fit 

Ptoc . I 

Yes 

Ithm: Specif y Paramet 

Peak. 

Base . Sub. Hlndo' 

Peak-Split . Facti 

Report La. 

Min. Peak Height : 

Min. Peak Width; 

Smoothing Width; 

RT I • • 

i RT; 

: Relat H 

, Type: 

Re tent ] 

Area : 

Height; 

le : 15.4 min 

38390775 counts 

4.34e400e cps 

15. 0 min 

3.Be6 

3.eee 

3.4*6-

3.2*6-

3.0*6' 

2-8*6 

2.6e6 

2.4e6' 

2.2e6-

2.0*6 

1.6e6' 

1.6e6' 

1.4e6< 

12*6-

1-0e6-

8.0e5-

6.0*5< 

4.0*5-

2.0*5-

0.0-

13-0 13.5 14.0 145 15.0 155 16.0 165 17-0 175 

I

Sample Hame:-kll07lSal6r Sample ID: "GLP1001-01-18-079" FUe:"k1107lSa.v)i4r 

Peak Name: "PFOA" Ma«*(*s): *413.000069.000 Da ,413.000219.000 Da ,413.000^69.000 Da" 

Comment "DALGW 1%R 0 110628 <<ia 1:100)" Annotatbn:-

Sample Index; 167 

Sample Type: 

Sub. Wlni 

:age: 

Specif y Parami 

90 

1.00 ra: 

I

Sample Name:'k110715a12Cr SaiT^ID:^LP1&01-01-18-050- Fle:"k110715a.M«r 

Peak Nam*: TFOA' Ma*s(**): "413.000069.000 D*,413J»0>'219-000 Da.413.00(V1GS.OOO Oa" 

Comment:"DALGW134R0110628(dl1:100r Armotabon:-

Satnple Inde.-t: 126 

Sample Type : Unknown 

Concentiation : N/A 

Calculate d Cone: 1790. ng/mL 3 2«fi 

Acq. Date : 7/17/201 1 " 

Acq. Time: 11:17:1 3 AM 

3.0*6-

MQ II I 

2.8*6' 

Z6e6-

Z4e6-

2.2e6-

2.006-

& 1.6*6-

1 1.6*6-

I 

1.4e6< 

1.2*6 

1.0*6 

Nolst 

Base. 

Peak-Split , Facto r 

Report Largest Peal 

Min. Peak Height : 

Kin . Peak Hidth : 

Smoothing Width: 

RT Window: 30.0 

Expected RT: 

Use Relativ e RT: 

Int . Type: Base To Bas' 

Retentio n Time: 15. 5 m: 

Area : 30420430 coui 

Height : 3.32e-f00d cj 

5.5 

14.5 15.0 15.5 16-0 165 17.0 175 

I SanvleName:'V110715a158' Sample ID:'OLP1(M>1-01-18-074" Fie: *1c11071 Sa.wHT 

Peak Nam*: TFOA' M«ta(*«):'413.00Q069.000Da,413.00Q/219.000Da,4l3.000/l6aj>DODa' 

I CoinnenL'DALGWl^LOll0628(dOl:10)" Annotatkm:' 

5.0*6-

4.8*6-

4.6*6-

4.4*6-

4.2*6-

4.0*6-

3.8e6< 

3.6e6< 

3.4*6-

3.2*6-

3.0*6-

2.8*6-

2.6*6-

2.4*6-

2.2*6-

2.0*6-

1.8*6-

1.6*6-

1.4*6-

1.2*6 

1.0*6 

6.0*5 

6.0*5-

4.0*5-

Z0*5' 

0.0-

N/A 

Calculate d 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algor 

Hois e Perc e 

Base . Sub. 

Peak-Split . 

one 

thm 

3570 . 

7/18/201 1 

2:13:5 0 AM 

Yes 

Specif y Pa 

tage : 90 

Indow: 1.00 

Report Largest Peak: Yes 

Min. Peak H igh 

Min. Peak Hidth 

Smoothit,g Hidth 

RT Hindow: 

Expecte d RT 

Use Relati v 

Retentio n T 

Area : 

Height : 

Star t Time: 

End Tine : 

RT 

0.0 0 

0.0 0 

0 

30. 0 s 

15. 7 n 

No 

Manual 

15.5 n 

56222974 COu 

5.BOe-.006 c 

15. 1 rr 

IS.O rr 

Sample Index ; 

Sample Type : 

Concentration : 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Nois e Percentag e 

158 

Unknown 

H/A 

283 . 

7/17/2 0 

11:03: 0 

Yes 

Specif y 

90 

P 

Pa 

Base . Sub. Hindow: 1.00 

Peak-Split . Fact ^r: 3 

Rei>ort Largest Peak: Y 

Min. Peak Heigh t 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Vso Relativ e RT: 

Int . Type: 

Retentio n Time: 

Area : 46 

Height : 

Star t Time: 

End Time: 

0 

0 

0 

30. 0 

15. 7 

No 

Manual 

15. 5 

22156 

.ISe.OO 

15. 0 

16-0 

00 

00 

145 15.0 15.5 16J) 165 17X) 175 la O 15.0 155 16.0 165 17X) 17.5 18.0 

Data printe d by STW 

Printing Time: 10:27:36 AM 

Printin g Date: Tuesday, August 23, 2011 

Page 9 of 10 

Page 52 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur. AL; June 2011 

Results Name: kll0715a.rdb 

• Sarn)leNam*:"K110715a144' Sample ID: "GLP1tMH-01-18-064" Rle:"»t110715a-»«r 

• Peak Name:-PFOA" Ma*«<e«):-413.00QQ69.000Da,413.00Q'2ig.00ODa,413.00(V169.00OOa' 

I Comment Trip Blank S«l 1 Sample" Anrwtatkm: ~ 

Sample Index: 144 

Sample Type: 

•atioi N / A 

Calculated Cone: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Base. Sub. Windo 

Peak-Split. Fact 

Report Largest P 

Min. Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

Acea: 

Height: 

Start Time: 

End Time: 

< 0 

7/17/2011 

6:07:22 PM 

Yes 

Specify Pa 

90 

^: 1.00 

sr: 3 

..ak: Yes 

0.00 

0 

30.0 

15.4 n 

No 

Base To Ba. 

15.4 1 

9552 cou: 

5.21e+003 

15.4 1 

15.5 n 

I

SampteN*m*:"k110715a23€r Sainple ID: "GLPI001-01-18-133" Fte:"kl10715a.wir 

Peak Name: "PFOA" MB«*(e*): "413.000/369.000 Da ,413.000/219.000 Da ,413.000/169JXW Da" 

Coffiment:-DALGW130LRB110630r Annotatton:" 

Sample lnde:<: 236 

Sample Type: 

ratio; N/A 

Calculated Cone: 

Acq. Date: 

Acq- Time: 

Modified: 

Proc. Algorithm: 

Hoise Percentage: 

Base. Sub. Window 

Peak-Split. Facto 

< 0 

7/19/2011 

2:36:20 AM 

Yes 

Specify Pa 

90 

1.00 

r: 4 

Report Largest Peak: Yes 

Min. Peak Height: 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

Area: 1 

Height: 6 

Start Time: 

End Time: 

0.00 

0.00 

0 

30.0 = 

15.5 r. 

Ho 

Manual 

15.5 n 

= 418 cour 

30et003 c 

15.4 n 

15.5 n 

Data printe d by STW 

Printin g Time: 10:27:36 AM 

Printin g Date: Tuesday, August 23, 

Page 10 of 10 

Page 53 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Results Name: kll0728a.rdb 

kl 10728a.rdb (PFOA): "Quadratic" Regression ("1 / x" weighting): y = -0.00307 x*2 + 1.09 x + 0.0166 (r = 0.9998) 

80, 

75-

40 45 50 55 65 70 75 80 85 90 95 100 

Analyte Cone. / IS Cone. 

Data printed by STW 

Printing Time: 10:26:11 AM 

Printing Date: Tuesday, August 23, 

Page 1 of 1 

2011 

Page 54 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur. AL; June 2011 

*ETS-Kirk Results Name: kll0728a.rdb 

I

Sample Name: •V110728a01S- Sampto ID: "1100M5«" 

Peak Name: "13CaPfOA-IS(IS}* Maaa<»c}: -421.000/376.C 

Comment "1.0 ng/mL FC itd In Synth. VVat*i- Annotatton: 

Sample Inde>;: 16 

Sample Typie: Standard 

Concentration: 1.00 ng/mL 

Calculated Cone: N/A 

Acq. Date: 7/28/2011 

Acq. Time: 3:16:32 PM 

Proc. Algorithm: S 

Noise Percentage: 

Base. Sub. Window 

Peak-Split. Factor 

Report Largest Pei 

Min. Peak Height: 

Min. Peak Width: 

Smoothing Hidth: 

RT Window: 

Expected RT: 

Use Relative RT: 

int. Type: 

Retention Time: 

Area: 150S 

Height; 2 

Start Time: 

End Time: 

pec: 

t: 

1.S 

Ho 

Vail 

IS 

*1 / 

b2e* 

lb 

l b 

fy Pa 

50 

..00 

2 

Yes 

0.00 

ey 

.7 

105 

.6 

.0 n 

I

S»iTpleN»m*:-k110728a028" Sample |D:"LCS-I10y26-1" FUe:n(110728*.wtr 

Peak Name: "13C8PRDA-IS0S)- Ma*i(e*): "421.000/376.000 Da' 

Comm*nt "0.2ppb LCS* Annotatton: ~ 

I

Sanv(eName:-V110728a02r San ^ ID; "11 005*9" Rle:-k1 

PeakNama:*13C8PFOA-l3(l5r Maaa(e*):"421.000376.000Da* 

Comment: "Pitothod Blanir Annotatton: " 

Sample Index: 27 

Sample Type; Unknown 

Concentration: 1.00 ng/mL 

Calculated Cone: N/A 

Noi; ;aqe: 

. 141 ndc 

Peak-Split. Factor 

Report Largest Peal 

Min. Peak Height; 

Min- Peak Width: 

Smoothing Width: 

RT Vlindow: 

Expect 1 RT: 

Int. Type: 

Retention Time: 

Area: !7i 

Height: 

Start Time: 

Valley 

15.7 

5882 c 

.016*005 

15.6 

Sample Type: QC 

Concentration: 0.993 

Calculated Cone: N/A 

Acq. Date: 7/28/2011 

Acq. Time: 7:29:32 PM 

Modified: Yes 

Proc. Algorithm: Specify Par 

Hoise Percentage: 50 

Base. Sub. Hindow: 1.00 

Peak-Split. Factor: 3 

Report Largest Peak: Yes 

Min. Peak Height: 0.00 

Min. Peak Width: 0.00 

Smoothing Width: 0 

RT Hlndo«: 30.0 s 

Expected RT: 15.9 in 

Use Relative RT: No 

ig/mL 

imeters - MO III 

min 

cps 

s e c 

points 

Int. Type: Base To Base 

Retention Tims: 15.8 it 

Area: 1666277 coun 

Height: 2.93e+005 cps 

Start Time: 15.6 m 

End Time: 16.1 m 

n 

n 

I

Sample Name: 1(110726*031" Sample ID: "LCS-110726-4" Fle:1(11073aa.wifr 

Peak Name: "13C8R=OA^S{(S)" MaH(e*): *421.000076.000 Da' 

Comment: '2ppb LCS* Annotatton:" 

Sample Index: 31 

Sample Type: 

Concentratic 

QC 

i: 0.993 ng/m. 

Calculated Cone: H/A 

Acq. Date: 

Acq. Time: 

Modified: 

7/28/2011 

8:32:51 PM 

No 

Proc. Algorithm: Specify Paramet 

Hoise Percen age: 50 

Base. Sub. tJindow: l. 00 min 

Peak-Split. 

Report Large 

Min. Peak He 

•actor: 2 

St Peak: Yes 

ght: O.OO cp 

Min. PeaK Width: 0.00 se 

Smoothing wl 

RT Window: 

Expected RT: 

Use Relative 

Int. Type: 

Retention Tl 

Area: 

Height: 

Start Time: 

End Time: 

:th: 0 p. 

30.0 sec 

15.8 min 

RT: Ho 

Valley 

le: 15.8 min 

1665098 counts 

2.70e+005 cps 

15.6 min 

16.0 min 

Data printe d by STW 

Printin g Time: 10:30:02 AM 

Printin g Date: Tuesday, August 23, 2011 

Page 1 of 5 

Page 55 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

*ETS-Kirk Results Name: kll0728a.rdb 

I

S«ni|)le Name:-k110728a03r Sample ID:'LCS-110726-7' File:-kl 10728«.viir 

Peak Name:-laCUPFCWWSflS)" Haaa(ea):"421.00Q'376.0CODaCetnnert: "ZOppb LCS' Annotation:" 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modified: 

Proc . Algorithm; 

Nois e Percentag e 

Base . Sub. Windo 

Peak-Split . Fact 

N/A 

7/28/201 1 

9:36:14 PM 

No 

Specif y Pa 

50 

•i: 1.00 

a r: 2 

Report Largest Peak: Yes 

Min. Peak Heigh t 

Min. Peak Vlidth: 

Smoothing Hidth : 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type: 

Retentio n Time: 

0.0 0 

0.0 0 

0 

30. 0 

15.8 n 

Ho 

Base To Ba 

15.8 B 

Acea : 1593904 cour 

Height : 

Star t Time: 

End Time: 

.516*005 c 

15. 6 n 

15. 9 n 

I

SanpleName:1(110728a044- San^le ID: "LCS-110726-13* Rle:1(110728a.w(r 

PeakNam*:*13CePFQA4S(lS)" MaM(e«J; "421.000076.000Da" 

Comment'2ppb LCS EC r Annotatton:' 

Sample Index : 44 

Sample Type: QC 

Concentration : 0.994 ng/mL 2.8*5i 

Calculate d Cone: H/A 

I

Sample Nam*: "k1l0726sO41" Sample ID: TCS-110726-10- Fle:*k110728a.<Mr 

Peak Name: "13C6PFCA-I3{IS)" Maaa{e*): "421.000/376.000 Oa" 

Cemm*nt:*0.2ppbLCSECP Annotatton:"" 

Sample Type : 

Concentration : 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Kois e Percentag e 

Base . Sub. Windo 

Peak-Split . Fact 

Report Largest P 

Min. Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

QC 

0.993 

N/A 

7/29/201 1 

12:04:0 8 AM 

Yes 

Specif y Par 

' : 1.00 

o r : 2 

.ak: Yes 

: 0.0 0 

0.0 0 

0 

30. 0 s 

15.8 m 

Ho 

Valle y 

15.7 m 

Area : 1679052 coun 

Height : 

Star t Time: 

End Time: 

2.62et00 5 c 

15. 6 m 

16. 0 m 

I

Sampt*Name:'V11072BaO4r Sample ID: "LCS-110726-16- Fie: 1(110728a.wtr 

Peak Name: "13C8PFOA4S{IS)* Man{*«):'421.00CV376.000Da" 

Comnwnt: "20ppb LCS ECF" Amotatton: ~ 

Sample Index : 47 

Z5*5 

2.4*5 

2.3*5 

2.2*5 

2.1*5 • 

2.0*5 

1.Se5 

1.8*5 

1.7*5 

1.6*5-

1.5*5-

1.4*5-

1.3*5-

1.2*5-

1.1*5-

1.0*5-

g.0e4-

8.0*4-

7.0*4 

6.0*4 

5.0*4 

4.0e4 

3.0*4 

Z0e4' 

Acq. Date : 

Acq. Time: 

Modified: 

Proc . Algorithm: 

Nois e Feccecitage 

Base . Sub. Hlndo 

Peak-Split . Fac t 

Report Largest P 

Min. Peak Height 

Min. Peak Vlidth: 

Smoothing Width: 

RT Hindow: 

Expected RT; 

Use Relativ e RT: 

Int . Type: 

Retentio n Time: 

7/29/201 1 

1:07:32 AM 

Yes 

Specif y Pa 

SO 

/ : 1.00 

r : 2 

a k : Yes 

0.0 0 

0 

30. 0 s 

15. 8 n 

No 

Valle y 

15. 7 1 

Area : 1627025 cour 

Height : 

Star t Time: 

End Time: 

.Ble-f005 c 

15. 6 a 

15. 9 B 

Sample Type : 

Ion : 

Calculate d Cone: 

Acq. Date 

Acq. Time 

Modified : 

Proc . Algorithm: 

Hois e Pe r 

Base . Sub 

Peak-Spl l 

entag e 

QC 

0.99 3 

N/A 

7/29/2 0 

2:10:5 0 

Yes 

specif y 

50 

1 

AM 

•ig/tti 

Paramet 

Window: 1.00 

. Fact 

Re|»r t Largest P 

Min. Peak 

Min. Peak 

Smoothing 

RT Window 

Height 

width : 

width : 

Expecte d RT: 

Use Relativ e RT: 

Int . Type 

Retentio n 

Area : 

Height ; 

Star t Tim 

End Time: 

Time: 

a r: 2 

tak : Yes 

0 

0 

30. 0 

15.8 

Ho 

Valle y 

15.7 

00 

00 

m1n 

cp 

P< 

1597202 coun 

.53et00 5 cp s 

15.6 

15. 9 m 

n 

n 

1M «.o 

Data printe d by STW 

Printing Time: 10:30:03 AM 

Printin g Date: Tuesday, August 23, 2011 

Page 2 of 5 

Page 56 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Results Name: kll0728a.rdb 

I

Sample Name: •V110728a07?' Sample ID: "GLP1&«1-01-1W)69' Rto:*kll072ea.wtr 

Peak Name: "13C8PFOA4S(IS}" Ma*a{ea): "421.00Ck'376.000 Da" 

Coirmenk"DALGW 1353 0110628- Anrntstton:' 

Sample Index: 75 

Sample Type: Unknown 

Concentration; 1.00 ng/mL 

Calculated Cone: H/A n 

Acq. Date: 7/29/2011 

Acq. Time: 12:02:36 PM 

Modified : Yes 

Peak-Split . Fac o r : 2 

Report Largest Peak: Yes 

Min. Peak Heigh 

Min. Peak Hidth 

Smoothing Hidth 

RT Window: 

Expected RT: 

Use Relativ e RT 

Int . Type: 

Retentio n Time: 

: 0.0 0 

0.0 0 

0 

15.8 min 

Ho 

Base To Base 

15.8 min 

Area : 1725937 counts 

Height ; 

Star t Time: 

End Time: 

2.90e-fO05 eps 

15. 6 min 

15. 0 min 

135 

I

SsnplaName:~k110728a02r Sample ID: "1100&«9^ Fle:'V110728a.w4r 

Peak Name: "PFOA" Ma*a(e*): "413.OOCV369.000 Da ,413.000/219.000 Da,413.00(V169.DOO DaComment "Method Blank" Arvwtatran: ~ 

Sample Index: 27 

Sample Type: Unknown 

Concentration: N/A 

T

Sample Name: "kl10728aO16r S8n^lD:-1 1 00»^&«" FUe:"lc1107a8a.wtfr 

Peak Nam*: "PFOA* MaM<*s): "413.OOCV369.000 Da .413.00(V219.000 Da,413.00(Vt68JXn Da' 

Comnent:"1.0ng/mLFCetdkfSyntti.Wat*;' Annotaflon:"" 

Sample Inde^: 16 

Sample Type: Standard 

Concentration: 1.00 ng/mL 

Calculated Cone: 0.999 ng/mL 

Acq. Date: 7/28/2011 

Acq, Time: 3:16:32 PM 

Modified : 

Proc . Algorithm: 

Hois e Percentage : 

Base . Sub. Window 

Peak-Split . Fact o 

Report Largest Pe 

Min. Peak Height : 

Min. Peak Width: 

Smoothing width : 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

Yes 

Specify Pa 

50 

1.00 

r; 2 

k: Yes 

0.0 0 

0.0 0 

0 

30. 0 

15.8 

No 

Manual 

15.7 

Area : 1661714 cou 

Height : 2 

Star t Time: 

End Time: 

65e+005 

15.6 

15. 9 

(

Sample Name: "k110726a028" Sampto ID: TC&-110726-r Fle:1(1l0728a.wtfr 

Peak Name: "PFOA" Ma*a(ea): -413.00(V369.000 Da,413.O0a'219.O0O Da,413.000/169.000 Da* 

ConuTMnt: *0.2ppb LCS* Annotatton: *" 

Calculate d Cone: 

Acq. Date ; 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Hois e Percentag e 

Base . Sub. Windo 

Peak-Split . Fac t 

0.00359 

7/28/20 1 

7:08:2 8 

Yes 

Specif y 

50 

w: 1.0 

o r: 2 

Report Largest Peak: Ye 

Min. Peak Height 

Min. Peak Width: 

Smoothing width : 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type: 

Retentio n Time: 

Area : 

Height : 

Star t Time: 

End Time: 

0. 

0. 

0 

30. 0 

15. 8 

Ho 

Manual 

15.8 

'678 9 c 

5.10e-tOO3 

15.7 

15. 0 

1.7e4 

1.6e4 

1.5*4 

1.4*4 

1Je4 

1.2e4 

1.1*4 

1.0e4 

9000.0 

8000.0 

70oao 

6000.0 

5000.0 

4000.0 

3000.0 

2000.0 

1000.0 

0.0 

14.2 

TIW.'T'.".'T? 

14.54 

;i U.S9 ' " 

WLuki 

15.78 

1 

t^TM iP 

16.16 1 f 

k \ 1 } 

17J6 

IN IIIL 

UikiUi 

PiiPf 

18.12 

II 

iii"A ||I||]||M If 

" l|f 

Sample Type: OC 

Concentr e ion : 

Calculate d Cone: 

Acq- Date 

Acq. Time 

Modified : 

Proc . Algorithm: 

Base . Sub 

Peak-Spl l 

0. 99 

10 

7/28/201 1 

7:29 32 PM 

Yes 

Spec 

Window: 

. Factor: 

ReiJort Largest Peak: 

Min. Peak 

Min. Peak 

Smoothing 

RT Window 

Heigh t 

Width: 

Width: 

Expected RT: 

Use Rela t 

Int . Type 

Retentio n 

Area : 

Height : 

Star t Tim 

End Time: 

ve RT: 

Time: 

30 

ty Pa 

SO 

1.00 

3 

Yes 

0.0 0 

0.0 0 

0 

0 

15. 8 n 

No 

Man 

2430 

.98e 

a l 

. 8 : 

004 c 

15.7 n 

1 .0 n 

7.0e4' 

leters - MC II I 

f 3.5*4 

I 

3.0a4 

Data printe d by STW 

Printing Time: 10:30:03 AM 

Printin g Date: Tuesday, August 23, 

Page 3 of 5 

2011 

Page 57 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

*ETS-Kirk Results Name: kll0728a.rdb 

I San¥leNam*:"W10728a031* San^)le ID: "LCS-110726-4" FUe:1c110728a. 

I P*akNam*:"PFOA" Ma*«(*«):*413.DOQQ69.000Da,413.000i/219.0000a,413.00a/l69.000Da' 

I Convnant "2ppb LCS" Annotatton:"" 

:ulate d C 

. Date : 

. Time: 

2.0 3 n 

7/28/201 1 

8:32:54 PM 

Modlfl . 

Proc, 

Noisi 

Algol 

, Window: 

Peak-Split . Factor: 

Report Largest Peak: 

Min. Peak Height : 

Specif y Parameters - MO II I 

Min. : Hldl 

Smoothing VIIdl 

RT Window: 

Expected RT: 

Use Relal . RT: 

Int . Type : Valle y 

Retentio n Time: 15. 8 

Area : 3727598 cov 

Height : 5.93e+005 

Star t Time: 15. 7 

End Time: 15. 0 

I Sanvie Nam*: "kl 10728*041" Sample ID:-LCS-110726-ia' Fle:1c110728a!w(F 

Peak Name:-PFOA" Mau(*t):*413.00a/369.000Da,413.000ir219.0DODa.413.00Qn69.000DaI Comnwnt •X).2ppb LCS ECP Amotatton:" 

I

Sampto Name:'V11072Sa034' Sample ID:-LCS-110726-r Fle:"k110728a.wfrr 

Peak Name: "PFOA" Ma*a(at): -413.000/369.000 Da,413.00a'219.000 Da ,413.000/169.000 D*" 

Commant: -20ppb LCS' Annotation: ~ 

4.8*6-

4.6e6-

4.4e6-

4.2*6-

4.0*6-

3.8e6-

3.6*6-

3.4*6-

3.2*6-

3.0*6-

2.8*6-

2.6*6-

2.4*6-

2.2*6-

2.0*6-

1.6*6-

1.6*6-

Sample Type: 

Concentratio n 

Calculate d Co 

Acq. Date : 

Acq. Time; 

Modified : 

Proc . Algori t 

Hois e Percen t 

Base . Sub. Wl 

QC 

19. 9 

19. 1 

7/28/2 0 

9:36:14 

No 

Specif y 

50 

PM 

g/mL 

g/mL 

Paramet e 

ndow: 1.00 

Peak-Split . Fac t 

Report Large s 

Min. Peak Kei 

Min. Peak Wid 

Smoothing Wld 

RT Window: 

Expected RT: 

Use Relativ e 

Int . Type: 

P 

li: 

•h: 

ItT: 

Retentio n Time: 

Area : 

Height : 

Star t Time: 

End Time: 

r : 2 

a k : Yes 

0 

0 

0 

30. 0 

15.8 

No 

Valle y 

31707235 

.92e''00o 

15. 7 

16. 0 

00 

00 

mir, 

po 

s e c 

m n 

c 

m 

n 

n 

1.0*6 

8.0*5 

6.0*5 

4.0e5' 

2.0e5 

13.5 14.0 I 

(

Sample Name: -k11072Sa04<' Sample ID: -LCS-110726-13" Fie: "k1l0728a.wir 

Peak Name: "PFOA" Ma««(e*): '413.000/369.000 Da,413.00(V2ig.OOO Da ,413.000/169.000 Da' 

Commant: "2ppb LCS ECF" /Annotatton: 

Sample Index : 

Concentration : 

Calculate d Cone: 

Acq, Date : 

Acq- Time: 

Modified : 

Ptoc . Algorithm: 

Hois e Percentag e 

41 

QC 

0.19 9 

0.206 

7/29/2011 

12:04:0 8 

Yes 

ng/mL 

AM 

Specif y Paramet e 

Base . Sub. Window; l.Ot 

Peak-Split . Factor : 2 

Report Largest P 

Min. Peak Height 

Min. Peak Vlldth: 

Smoothing tlldth : 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

ak: Yes 

O.C 

O.C 

0 

30. 0 

15.8 

Ho 

Manual 

15.8 

Area : 408715 co 

Height : 5.61e*O0A 

Star t Time: 

End Time: 

15. 5 

15. 9 

min 

) cp s 

) se e 

po 

s e c 

min 

ops 

min 

imple Type: QC 

Concentration : 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modified : 

Proc , Algorithm: 

Hois e Percentag e 

1.99 ng/mL 

1.99 lig/mL 

7/29/201 1 

1:07:32 AM 

Yes 

Specif y Paramet e 

50 

Base . Sub. Window: 1.00 min 

Peak-Split . Fac t a r: 2 

Report Largest Peak: Yes 

Min. Peak Heigh t 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type; 

Retentio n Time: 

0.0 0 cp s 

0.0 0 se c 

0 po 

30. 0 se e 

15.8 min 

Ho 

Manual 

15.7 min 

Acea: 3558803 counts 

Height : 

Star t Time: 

End Time; 

5.01e*005 cps 

15.4 rain 

16. 0 min 

15.0 155 16.0 16.5 17.0 17.5 18.0 

Data printe d by STW 

Printing Time: 10:30:03 AM 

Printin g Date: Tuesday, August 23, 2011 

Page 4 of 5 

Page 58 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

Results Name: kll0728a.rdb 

I San«)te Name: 1(1107283047- S«mF4e ID:-108-110726-16^ FI«:*k110728a.wHr 

I Peak Name:-PFOA- MaM<ea):*413.00IV369.0000a^13.0aQr219.000Da,413.00tf1€9.000Da' 

I Comment-20ppb LOS ECP Annotation:--

Sample Inde>-

Sample Type: 

Concentrati o 

Calculate d C 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algor: 

Hois e Percen 

:hm: 

Base . Sub. Windc 

Peak-Split . 

Report Large 

••act 

St P 

Min. Peak Height 

Min. Peak w: 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e 

Int . Type : 

Retentio n Ti 

Area ; 

Height : 

KT: 

47 

QC 

19. 9 

20. 1 

7/29/201 1 

2:10:5 0 AM 

Yes 

Specif y Pat 

50 

i: 1.00 

o r : 2 

eak : Yes 

0 

30. 0 s 

15.8 m 

Ho 

Manual 

15.8 m 

33487411 cou 

.33e+006 c 

amete 

min 

c p s 

ps 

Sample Name: "k110728aO75" SampI* ID:"OLP1&01-01-1&06g^ Fle:"k110728a.w<rr 

Peak Name: "PFOA" Maw(*a}: "413.000/369.000 Da.413.000^19.000 Da.413.000/169J}00 Da" 

CommMil:"DALGW135S0110B2r Annotation:" 

Sample Index : 75 

Sample Type: 

Concentration : 

Calculate d Cone: 

Acq. Time : 

Modified : 

Proc . Algorithm: 

Nois e Percentag e 

Base . Sub. Windo 

Unknown 

N/A 

20. 2 

7/29/201 1 

12:02:3 6 PM 

Yes 

Specif y Par 

50 

-: 1.00 

Peak-Split . Factor: 2 

Report Largest Peak: Yes 

Min. Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Tvpe : 

Retentio n Time: 

Area ; 35 

Height : 

Star t Time : 

End Time: 

0.0 0 

0 

30. 0 s 

15. 6 m 

No 

Manual 

15. 8 m 

58578 cou 

.46et00 6 e 

15. 3 m 

16. 0 m 

Data printe d by STW 

Printing Time: 10:30:03 AM 

Printin g Date: Tuesday, August 23, 

Page 5 of 5 

Page 59 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

ATTACHMENT C: ANALYTICAL METHOD(S) 

Page 60 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

3M Environmental Laboratory 

Metiiod 

Mett)od of Analysis for ttie Determination of Perfluorinated Compounds in Water 

by LC/MS/MS; Direct Injection Analysis 

Method Number: ETS-8-044.0 

Adoption Date: Upon Signing 

Effective Date: Q <//(^ / o "l 

Approved By: 

^/>^/o y 

William K. Reagen, Laboratory Manager Date 

ETS-8-044.0 Page 1 of 11 

Method of Analysis for ttie Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct 

Injection Analysis Page 61 of 71 
GLP10-01-01; Interim Report 18 

Analysis of PFOA in water samples 

FSIA - Decatur, AL; June 2011 

1 Scope and Application 

This method is to be used to quantify Perfluorobutanoic Acid (PFBA), Perfluoropentanoic Acid (PFPeA), 

PerfiuorohexanoicAcid (PFHA), Perfluoroheptanoic Acid (PFHpA), Perfluorooctanoic Acid (PFOA), 

Perfluorononanoic Acid (PFNA), Perfluorodecanoic Acid (PFDA), Perfluoroundecanoic Acid (PFUnA), 

Perfluorododecanoic Acid (PFDoA), Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), 

and Perfiuorooctanesulfonate (PFOS) by High Performance Liquid Chromatography coupled to a tandem 

Mass Spectrometric Detector (LC/MS/MS) in clean water samples. Water samples containing heavy 

particulate may require preparation by an alternate method such as ETS-8-154 "Determination of 

Perfluorinated Acids, Alcohols, Amides, and Sulfonates In Water By Solid Phase Extraction and High 

Performance Liquid Chromatography/Mass Spectrometry". 

This method is considered a performance-based method. Data is considered acceptable as long as the 

defined QC elements are satisfied. 

Sample collection is not covered under this analytical procedure. 

2 IVIethod Summar y 

Clean aqueous samples are analyzed 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 centrifuge prior to removing a sample aliquot, or filtered. 

This is a performance-based method. Method accuracy is detennined for each sample set 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. Sample results for spikes outside of 70% to 130%, may be flagged as such (with 

expanded accuracy statements), or will not be reported due to non-compliant quality control samples. 

Fortification levels for field matrix spikes and for laboratory matrix spikes should be at least 50% of the 

endogenous level and less than 10 times the endogenous level to be used to determine the statement of 

accuracy for analytical results. 

3 Definitions 

3.1 Calibration Standard 

A solution prepared by spiking a known volume of the Worthing Standard (WS) into a predetermined 

amount of ASTM Type I, HPLC grade water, or other suitable water, and analyzed according to this 

method. Calibration standards are used to calibrate the instmment response with respect to analyte 

concentration. 

3.2 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. 

3.3 Field Blanit (FB)/Trip Blanl( 

ASTM Type I, 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 FB is to determine if test substances or 

other interferences are present in the field environment. This sample is also refen'ed to as a Trip Blank. 

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3.4 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. 

3.5 Field Matrix Spike (FMS) 

A sample to which known quantities of the target analytes 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 should be spiked between 

approximately 50% and 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. The FMS is analyzed to ascertain if any matrix 

effects, interferences, or stability issues may complicate the interpretation of the sample analysis. 

3.6 Trip Blank Spike (Field Spike Control Sample, FSCS) 

An aliquot of ASTM Type I, HPLC grade water, or other suitable water, to which known quantities of the 

target analytes are added in the laboratory prior to the shipment of the collection bottles. The FSCS is 

extracted and analyzed exactly like a study sample to help determine if the method is in control and 

whether a loss of analyte could be attributed to holding time, sample storage and/or shipment issues. A 

low and high FSCS are appropriate when expected sample concentrations are not known or may vary. At 

least one separate, un-spiked sample must be taken at the same time and place as each FMS. 

3.7 Laboratory Control Sample (LCS) 

An aliquot of control matrix to which known quantities of the target analytes are added in the laboratory at 

the time of sample extraction. At least two levels are included, one generally at the low end of the 

calibration curve and one near the mid to upper range of the curve. The LCSs are extracted and analyzed 

exactly like a laboratory sample to detennine whether the method is in control. LCSs should be prepared 

each day samples are extracted. 

3.8 Laboratory Matrix Spike (LMS) 

A laboratory matrix spike is an aliquot of a sample to which known quantities of target analytes are added 

in the laboratory. The LMS is analyzed exactly like a laboratory sample to detennine whether the sample 

matrix contributes bias to the analytical results. The endogenous concentrations of the analytes in the 

sample matrix must be detennined in a separate aliquot and the measured values in the LMS con'ected 

for these concentrations. LMSs are optional for analysis of aqueous samples. 

3.9 Laboratory Sample 

A portion or aliquot of a sample received from the field for testing. 

3.10 Limit of Quantitation (LOQ) 

The lower limit of quantitation (LLOQ) for a dataset is the lowest concentration that can be reliably 

quantitated within the specified limits of precision and accuracy during routine operating conditions. To 

simplify data reporting, the LLOQ is generally selected as the lowest non-zero standard in the calibration 

curve that meets method criteria. Sample LLOQs are matrix-dependent. 

The upper limit of quantitation (ULOQ) for a dataset is the highest concentration that can be reliably 

quantitated within the specified limits of precision and accuracy during routine operating conditions. The 

highest standard in the calibration curve that meets method criteria is defined as the ULOQ. 

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3.11 Method 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. 

3.12 Sample 

A sample is an aliquot removed from a larger quantity of material intended to represent the original source 

material. 

3.13 Stock Standard Solution (SSS) 

A concentrated solution of a single-analyte prepared in the laboratory with an assayed reference 

compound. 

3.14 Surrogate 

A compound similar in chemical composition and behavior to the target analyte(s), but is not normally 

found in the sample(s). A sunogate compound is typically a target analyte with at least one atom 

containing an isotopically-labeled substitution. If used, sun-ogate(s) are added to all samples and quality 

control samples. Surrogate(s) are added to quantitatively evaluate the entire analytical procedure 

including sample collection, preparation, and analysis. Inclusion of a sun'ogate analyte is an optional 

quality control measure and is NOT required. 

3.15 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 detemnined; 

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. 

The laboratory is responsible for maintaining a safe wori< environment and a cun-ent awareness of local 

regulations 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 ^miliar 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. 

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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 Equipment 

6.1 Instrumentation and Equipment 

A high performance liquid chromatograph capable of pumping up to two solvents and equipped with a 

variable volume injector capable of injecting 5-100 |JL connected to a tandem Mass Spectrometer 

(LC/MS/MS). I 

Analytical balance capable of reading to 0.0001 g 

A device to collect raw data for peak integration and quantitation 

15-mL and 50-mL disposable polypropylene centrifuge tubes. 

Gas tight syringes, 25|JL, SOJJL, 100|JL, 250|JL, 500|JL, 1000|JL. 

1 mL plastic HPLC autovial. 

Disposable pipettes, polypropylene or glass as appropriate 

Centrifuge capable of spinning 15-mL and 50-mL polypropylene tubes at 3000 rpm. 

6.2 Chromatographi c System 

Guard Column: Prism RP, 4.6 mm x 50 mm, 5 |jm 

Analytical Column: Betasil C18,4.6 mm x 100 mm, 5 |jnri 

Temperature: 10°C 

Mobile Phase (A): 2 mM Ammonium Acetate in Water 

Mobile Phase (B): Methanol 

Gradient Program: 

Time (min) 

0.0 

0.5 

11.0 

13.5 

13.6 

17.0 

%A 

97 

97 

5 

5 

97 

97 

%B 

3 

3 

95 

95 

3 

3 

Flow Rate 

(mL/min) 

1.0 

1.0 

1.0 

1.0 

1.0 

1.0 

Injection Volume: 100 JJL 

Quantitation: Peak Area - quadratic curve fit, 1/x weighted. 

Run Time: ~ 17 minutes. 

The previous information is intended as a guide; alternate conditions and equipment may be used 

provided that data quality objectives are met. 

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6.3 MS/MS System 

6.3.1 Mode: Electrospray Negative ion, MRM mode, monitoring the following transitions: 

Analyte 

PFBA 

PFPeA 

PFHA 

PFHpA 

PFOA 

PFNA 

PFDA 

PFUnA 

PFDoA 

PFBS 

PFHS 

PFOS 

Transition Monitored 

213^169 

263-^219 

313 ^269 and 313-^119 

363 -^ 319, 363 -^ 169 and 363 -^ 119 

413 ^ 369, 413 -» 219 and 413 ^ 169 

463 -^ 419, 463 -^ 169 and 463 -^ 219 

513 ^ 469, 513 ^ 219 and 513 ^ 269 

563 -^ 519, 563 ^ 269 and 563 ^219 

613 ^ 569, 613 -^ 169 and 613 ^ 319 

299 -^ 80 and 299 -^ 99 

399 -^ 80 and 399 -^ 99 

499 -^ 80, 499 -^ 99 and 499 -^ 130 

Multiple transitions for monitoring the analytes is an option, as summing multiple transitions may provide 

quantitation of isomers that more closely matches NMR data and may have the added benefit of 

increased sensitivity. The use of one daughter ion is acceptable if method sensitivity is achieved, 

provided that retention time criteria are met to assure adequate specificity. 

The previous information is intended as a guide, alternate instmments and equipment may be used. 

7 Reagents and Standards 

7.1 Chemicals 

Water - Milli-Q, HPLC grade, or other suitably appropriate sources 

Methanol - HPLC grade 

Ammonium Acetate -A.C.S. Reagent Grade 

7.2 Standards 

Perfluorobutanoic Acid (PFBA - C4 acid); Oakwood Products, Inc 

Perfluoropentanoic Acid (PFPeA - C5 acid, also known as NFPA, nonafluoropentanoic acid); Alfa Aesar 

PerfiuorohexanoicAcid (PFHA-C6 acid); Oakwood Products, Inc 

Perfluoroheptanoic Acid (PFHpA - C7 acid, also known as TDHA, tridecafluoroheptanoic acid); Oakwood 

Products, Inc 

Perfluorooctanoic Acid (PFOA - C8 acid); 3M 

Perfluorononanoic Acid (PFNA-C9 acid); Oakwood Products, Inc 

Perfluorodecanoic Acid (PFDA-C10 acid); Oakwood Products, Inc 

Perfluoroundecanoic Acid (PFUnA-C11 acid); Oakwood Products, Inc 

Perfluorododecanoic Acid (PFDoA-CI 2 acid); Oakwood Products, Inc 

Perfluorobutanesulfonate (PFBS - C4 sulfonate); 3M 

Perfluorohexanesulfonate (PFHS - C6 sulfonate); 3M 

Perfiuorooctanesulfonate (PFOS - C8 sulfonate); 3M 

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The previous information is intended as a guide. Reagents and standards from alternate sources may be 

used. 

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. 

Note: Altemative volumes may be prepared as long as the ratios of the solvent to solute ratios are maintained. 

7.4 Stock Standard Solution (SSS) and Working Standard Solution Preparation 

The following standard preparation procedure serves as an example. Weighed amounts and final volumes may be 

changed to suit the needs of a particular study. For example, |JL volumes may be spiked into volumetric flasks 

when diluting stock solutions to appropriate levels. 

100 |jg/mL target analyte SSSs—Weigh out 10 mg of analytical standard (corrected for percent salt and 

purity) and dilute to 10OmL with methanol or other suitable solvent, in a 10OmL volumetric flask. Transfer to a 

125mL 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 con-ection is given below for PFOS. 

,. , , molecular weight of anion 

salt correction factor = = 

moclecular weight of salt 

499 PFOS (K^ )salt correction factor = ^^ ^ = 0.9275 

538 

10 mg CsFiySOsK" with purity 90% = 8.35mg CsFiySOs"(10 mg*0.90*0.9275=8.35 mg) 

5 (jg/mL (5000 ng/mL) mixed working standard—^dd 0.5mL each of the 100|jg/mL SSSs to a lOmL volumetric 

flask and bring up to volume with solvent. 

250 ng/mL mixed working standard—Add 1.25mL of the 5 |jg/mL -mixed worthing standard solution to a 25mL 

volumetric flask and bring up to volume with solvent. 

125 ng/mL mixed standard^Add 625pL of the 5 jjg/mL-mixed wori<ing standard solution to a 25mL volumetric 

flask and bring up to volume with solvent. 

Storage Conditions—Store all SSSs and working 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. 

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7.5 Calibration Standards 

Using the wori<ing standards described above, prepare calibration solutions in ASTM Type I water, HPLC water, or 

other suitable water, using the following table as a guideline. Note: Volumes of water 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. 

Concentration 

of WS, ng/mL 

125 

125 

125 

125 

250 

250 

250 

250 

5000 

5000 

5000 

Volume of WS.fiL 

10 

15 

20 

30 

20 

50 

100 

200 

25 

50 

100 

Final Volume of 

Calibration Standard (mL 

Of ASTM Type 1 Water, or 

ottier suitable water) 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

Final Concentration of 

Calibration Standard, ng/mL 

(ppb) In ASTM Type 1 Water, 

or other suitable water 

0.025 

0.0375 

0.050 

0.075 

0.100 

0.250 

0.500 

1.00 

2.50 

5.00 

10.0 

8 Sample Handling 

8.1 Water Sample Preparation 

This method is applicable to clean 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 plastic autovial. Plastic is 

prefen'ed over the use of glass autovials, to prevent the possibly of fluorochemlcal sticking to the glass. 

Dilute sample, if necessary, with ASTM Type I, HPLC water, or other suitable water. 

Prepare method QC samples and multiple method blanks and aliquot into labeled plastic autovials. 

Prepare at least five method blanks. 

9 Sample Analysis - LC/MS/MS 

Analyze the standard curve prior to each set of samples. The standard curve may be plotted using a linear fit, 

weighted 1/x or unweighted, or by quadratic fil (y = ax^ + bx + c), weighted 1/x or unweighted, using suitable 

software. The calibration curves may include but should not be forced through zero. 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 firom the calibration curves to provide a better fit over the range 

appropriate to the data or because they did not meet the pre-detennined acceptance criteria. Low-level curve 

points should also be excluded if their area counts are not at least twice that of the method and/or solvent blanks. 

The coefficient of determination (r^) value for the calibration curve must be greater than or equal to 0.990. Each 

point in the curve must be within ±25% of the theoretical concentration with the exception of the LLOQ, which may 

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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 constmct 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. 

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 minimum 

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 containing analytes that are quantitated above the concentration of the highest standard in the 

curve should be further diluted and reanalyzed. 

10 Quality Control 

10.1 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. 

10.2 Method Blanks 

Method blanks must be prepared with each analysis batch. At least five method blanks must be prepared. 

Method blanks may be injected multiple times, but no more than 3 injections should be removed fi'om a single 

method blank. At a minimum, method blanks are analyzed prior to instrument calibration, prior to the analysis of 

CCV samples, and at the end of the analytical mn. 

The mean area count for each analyte in the method blanks must be less than 50% of the area count of the LOQ 

standard. The standard deviation of the area counts of these method blanks should be calculated and reported. If 

the mean area counts 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, or altematively, the method blanks must be evaluated 

statistically to determine outliers, or technical justification to eliminate one or more results should be made. 

10.3 Sample Replicates 

Samples duplicates are collected in the field. The relative percent difference, RPD, should be reported. RPD 

results greater than 20% will be flagged in the report, but will not be excluded firom reporting. The requirement for 

replicates excludes field blanks. 

10.4 Surrogate Spikes 

Sun'ogate spikes are not required but may be used on project specific requirements. 

10.5 Lab Control Sample 

Triplicate lab control spikes at a minimum of two different concentrations are to be prepared with each preparation 

batch. Low lab control spikes should be prepared at concentrations in the range of five to ten times higher than the 

targeted LOQ and high lab control spikes should be prepared at concentrations near the mid-point of the curve. 

The relative standard deviation of the control spikes evaluated independently at each concentration level must be 

less than or equal to 20% and the average recovery must be 80-120%. If the above criteria are not met, the entire 

set of samples should be re-injected or re-prepared as appropriate. 

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10.6 Field Matrix Spikes / Lab Matrix Spikes 

Recoveries of field matrix spikes and laboratory matrix spikes are anticipated to be between 70% and 130% of the 

fortified levels. Sample results for spikes outside of 70% to 130%, may be flagged as such (with expanded 

accuracy statements), or will not be reported due to non-compliant quality control samples. 

The targeted fortiflcation levels should be at least 50% of the endogenous level and less than 10 times the 

endogenous level to be used without justification to detemnine the statement of accuracy for analytical results. 

The average of the sample and the field duplicate should be used to calculate the recovery. 

11 Data Analysis and Calculations 

Use the following equation to calculate the amount of analyte found (in ng/mL, based on peak area) using the 

standard curve (linear regression parameters) generated by an appropriate software program: 

Analyte found (ng/mL) = (Peak Area - Intercept) ^ ^ ^ 

Slope 

DF = factor by which the final volume was diluted, if necessary. 

For samples fortified with known amounts of analyte prior to extraction, use the following equation to calculate the 

percent recovery. 

_ Total analyte found (ng/mL) - Average analyte found in sample (ng/mL) 

Analyte added (ng/mL) 

12 Method Performance 

Any method perfomnance parameters that are not achieved must be considered in the evaluation of the data. 

Nonconfonnance to any specified parameters must be described and discussed if the Technical Manager (nonGLP study) or Study Director (GLP study) chooses to report the data. 

If criteria listed in this method performance section are not met, maintenance may be performed 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 pert'omriance criteria have not been met, the data must be footnoted on tables and 

discussed in the text of the report. 

12.1 System Suitability 

System Suitability standards are not a required component of this method. If required by protocol or by the 

technical manager, a minimum of three system suitability samples are injected at the beginning of each analytical 

run prior to 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. The system suitability injections must 

have area counts with an RSD of ^5% and a retention time RSD of S2% to be compliant. 

12.2 Quantitation 

Calibration Curve: The coefficient of detennination (r^) value for the calibration curve must be greater than or 

equal to 0.990. 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 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. 

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Demonstration of Specificity: Specificity is demonstrated by chromatographic retention time (within 4% of 

standard) and the mass spectral response of unique ions. 

12.3 Sensitivity 

The targeted limit of quantitation for all analytes is 0.025 ng/mL. The LOQ for any specific analyte may vary 

depending on the evaluation of appropriate blanks and the accuracy of the low-level calibration curve points. Refer 

to Section 10 for additional details. 

12.4 Accurac y 

This method and required quality control samples are designed to generate data that are accurate to +/-30%. 

Section 10 contains additional infomnation regarding the required accuracy of laboratory control spikes, field matrix 

spikes and laboratory matrix spikes. 

12.5 Precision 

Samples should be collected in duplicate in the field. The relative percent difference, RPD, should be reported. 

RPD results greater than 20% will be flagged in the report, but will not be excluded from reporting. The 

requirement for replicates excludes field blanks or rinse blanks. 

Section 10 contains additional infomnation regarding the required precision of laboratory control spikes. 

13 Pollution Prevention and Waste Management 

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 intemal procedures. 

14 Records 

Each data package generated for a study must include all supporting infomnation for reconstmction of the data. 

Infomnation 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 (instalment batch records, instmment acquisition 

method, summary pages), instrument results files, chromatograms, calibration curves, and data calculations. 

15 Affected Documents 

None. 

16 Revisions 

Revision 

Number Summary of Changes 

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