GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

GLP10-01-02: Interim Report 18 - Analysis of PFBS. PFHS. and PFOS in Groundwater 

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

in June 2011 

Study Title 

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

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

Site-Related Monitoring Program 

Data Requirement 

EPA TSCA Good Laboratory Practice Standards 40 CFR Part 792 

Study Director 

Jaisimha Kesari P.E., DEE 

Weston Solutions, Inc. 

1400 Weston Way 

Westchester, PA 19380 

Phone:610-701-3761 

Author 

Susan Wolf 

3M Environmental Laboratory 

Interim Report Completion Date 

Date of signing 

Performing Laboratory 

3M Environmental Health and Safety Operations 

Environmental Laboratory 

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

St. Paul, MN 55144 

Project Identification 

GLP10-01-02-18 

Total Number of Pages 

113 

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

Competence of Testing and Calibration L^lx>ratories", in accordance with the A2LA Certificate #2052.01. 

^ED I Testing that compiies with this International Standard also operate in accordance witti ISO 9001:2000. 

Testing Cert #2052.01 

Page 1 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

This page has been reserved for specific country requirements. 

Page 2 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

GLP COMPLIANCE STATEMENT 

Report Title: Interim Report 18 Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

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

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

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

Site-Related Monitoring Program. 

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

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

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

system and no dosing of a test system. 

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

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

' - ^ 

Gary Hof)enstein,Sponsor Representative Date 

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

Page 3 of 113 
GLP10-01-02; Interim Report 18 

/^alysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

QUALITY ASSURANCE STATEMENT 

Report Title: Interim Report 18 Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

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

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

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

Site-Related Monitoring Program. 

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

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

laboratory management and study director. 

Inspection Dates 

8/18/11-8/19/11 

Phase 

Data / Report 

Date Reported to 

Testing Facility 

Management 

8/25/11 

Study Director 

8/25/11 

n ^ L 

'^-l- K 

QAU Representaive Date 

Page 4 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

TABLE OF CONTENTS 

GLP Compliance statement 3 

Quality Assurance Statement 4 

Table of Contents 5 

List of Tables 6 

1 Study Infomriation 8 

2 Summary 9 

3 Introduction 11 

4 Test & Control Substances 11 

5 Reference Substances 12 

6 Test System 13 

7 Method Summary 13 

7.1 Methods 13 

7.2 Sample Collection 13 

7.3 Sample Preparation 13 

7.4 Analysis 14 

8 Analytical Results 15 

8.1 Calibration 15 

8.2 System Suitability 15 

8.3 Limit of Quantitation (LOQ) 16 

8.4 Continuing Calibration 16 

8.5 Blanks 16 

8.6 Lab Control Spikes (LCSs) 16 

8.7 . Analytical Method Uncertainty 20 

8.9 Field Matrix Spikes (FMS) 21 

9 Data Summary and Discussion 21 

Page 5 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

10 Conclusion 39 

11 Data/Sample Retention 39 

12 Attachments 39 

13 Signatures 40 

LIST OF TABLES 

Table 1. Summarized PFBS, PFHS, and PFOS Results (FSIA Groundwater, June 2011) 10 

Table 2. Sample Description Key Code 13 

Table 3. Instrument Parameters 14 

Table 4. Liquid Chromatography Conditions 14 

Table 5. Mass Transitions 15 

Table 6. Limit of Quantitation (LOQ) 16 

Table 7. Laboratory Control Spike Recovery 18 

Table 8. Analytical Uncertainty 20 

Table 9. Field Matrix Spike Levels 21 

Table 10. DAL GW130R 110630 23 

Table 11. DAL GW130S 110630 23 

Table 12. DAL GW1 SOL 110630 24 

Table 13. DAL GW 131R 110622 24 

Table 14. DAL GW131S 110622 25 

Table 15. DALGW131L 110622 25 

Table 16. DAL GW133R 116030 26 

Table 17. DAL GW133S 110630 26 

Table 18. DALGW133L110630 27 

Table 19. DALGW134R110628 27 

Table 20. DALGW134S 110628 28 

Table 21. DALGW134L110628 28 

Page 6 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Table 22. DALGW135R110628 29 

Table 23. DAL GW135S 110628 29 

Table 24. DALGW135L110628 30 

Table 25. DAL GW136S 110630 30 

Table 26. DALGW136L110630 31 

Table 27. DAL GW137S 110624 31 

Table 28. DAL GW137L 110624 32 

Table 29. DAL GW138S 110630 32 

Table 30. DALGW138L110630 33 

Table 31. DAL GW138R 110630 33 

Table32. DALGWCW26C 110622 34 

Table33. DALGWCW26L110622 34 

Table34. DALGW 140R 110622 35 

Table35. DALGW 141R 110630 35 

Table36. DALGW 142R 110622 36 

Table37. DALGW 143R 110622 36 

Table38. DALGW 144S 110628 37 

Table 39. Trip Blank 1 37 

Table 40. Trip Blank 2 38 

Table 41. Rinseate Blanks 38 

Page 7 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

ii.i^ ' 

Sponsor 

3M Company 

Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

Study Director 

Jaisimha Kesari, P.E., DEE 

Weston Solutions, Inc. 

Westchester, PA 19380 

Phone:(610)701-3761 

Fax:(610)701-7401 

j.kesari@westonsolutions.com 

Study Location 

Testing Facility 

3M EHS Operations 

3M Environmental Laboratory 

Building 260-5N-17 

St. Paul, MN 55144 

Study Personnel 

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

Cleston Lange, Ph.D., Principal Analytical Investigator, (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 18 Experimental Termination: August 3,2010 

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 113 
GLP10-01-02; interim Report 18 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

FSIA-June 2011 

g mmrnM^ 

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

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

locations. A total of one hundred fifty-four sample bottles were received at the 3M Environmental 

Laboratory for perfluorooctane sulfonate (PFOS), perfluorohexane sulfonate (PFHS) and 

perfluorobutane sulfonate (PFBS), and included duplicate groundwater samples from each sampling 

location. Samples also included 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 rinseate 

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

PFBS, PFHS, and PFOS recovery. 

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

02-18 were received from Weston personnel on July 8, 2011. Ail of the samples were prepared and 

analyzed for PFBS, PFHS, and PFOS following 3M Environmental Laboratory Method ETS-8-044.0 

and conducted under 3M project GLP-10-01-02-18. Many of the groundwater samples required 

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

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

concentrations are summarized in Table 1. The equipment rinseate from DAL GW 1 SOL and the trip 

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

adequate control of sample contamination during shipping and sample collections. The equipment 

rinseate from sample DAL GW 133S for PFOS was just above the LLOQ at 0.0478 ng/mL, while PFBS 

and PFHS were below the lower limit of quantitation (LLOQ). 

The PFBS concentration results for all groundwater samples ranged from 0.0391 ng/mL to 74.3 ng/mL. 

The PFHS concentration results for ail groundwater samples ranged from 0.0806 ng/mL to 844 ng/mL. 

The PFOS concentration results for all groundwater samples ranged from 0.483 ng/mL to 1510 ng/mL. 

The analytical method uncertainties associated with the reported results are: PFBS + 11 %, PFHS + 

14% and PFOS + 36%. For some samples, the method uncertainty was expanded for PFOS. 

Page 9 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

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

Sampling Location 

DAL GW130R 110630 

DALGW 1308 110630 

DAL GW1 SOL 110630 

DAL GW 131R 110622 

DAL GW131S 110622 

DAL GW 131L110622 

DAL GW133R 110630 

DALGW 1338 110630 

DAL GW133L 110630 

DAL GW134R 110628 

DALGW 1348 110628 

DALGW134L110628 

DAL GW135R 110628 

DALGW 1358 110628 

DAL GW135L 110628 

DALGW 1368 110630 

DALGW136L110630 

DALGW 1378 110624 

DAL GW137L 110624 

DAL GW138R 110630 

DALGW 1388 110630 

DALGW138L110630 

DAL GWCW26C 110622 

DAL GWCW26L 110622 

DAL GW140R 110622 

DAL GW 141R 110630 

DAL GW142R 110622 

DAL GW143R 110622 

DALGW 1443 110628 

Trip Blanks (Milli-QTM Water) 

DAL GW130LRB 110630 

DALGW 1338 RB110630 

PFBS 

Avg. Cone. 

(ng/mL) ± RPD 

16.3 ±1.8% 

353 ±00% 

1.67 ±1.8% 

54.9 ± 3.5% 

0894 ±4.6% 

3.42 ±1.2% 

4.79 ±3.8% 

9.08 ±1.4% 

6.67 ±0.45% 

51.4 ±1.4% 

0.258 ±2.3% 

11.8 ±6.8% 

74.3 ±1.6% 

1.21 ±0.83% 

9.69 ±0.83% 

3.69 ±1.1% 

2.33 ± 0.43% 

0.107 ±2.8% 

0.0826 ±1.9% 

8.01 ±0.0% 

4.57 ± 0.66% 

00391 ±2.8% 

8.23 ±073% 

13.5 ±0.74% 

1.59 ±1.3% 

0.0431 ±2.8% 

1.69 ±0.0% 

1.66 ±2.4% 

1.66 ±4.2% 

<0.0250 

<0.0250 

<0.0250 

PFHS 

Avg. Cone. 

(ng/mL) ± RPD 

125 ± 0.0% 

29.8 ± 0.34% 

13.6 ±2.2% 

304 ±4.6% 

5.07 ±7.5% 

21.6 ±1.9% 

331 ±3.0% 

67.2 ±0.74% 

46.9 ±1.7% 

483 ± 0.62% 

3.09 ± 2.3% 

111 ±13% 

844 ±3.7% 

8.06 ±2.2% 

71.0 ±2.5% 

25.8 ±0.78% 

16.0 ±1.3% 

0.0806 ±2.0% 

0.107 ±094% 

39.2 ±0.26% 

23.2 ±0.0% 

0113 ±0.89% 

67.8 ±1.6% 

105 ±1.0% 

17.8 ±1.1% 

0.296 ±1.7% 

10.2 ±3.0% 

6.06 ±3.8% 

7.14 ±3.9% 

<0.0250 

<0.0250 

<0.0250 

PFOS 

Avg. Cone. 

(ng/mL) ± RPD 

450 ±4.4% 

97.6 ±5.0% 

63.7 ± 5.3% 

1510 ±3.3% 

5.37 ±2.1 % 

32.4 ± 1.5% <" 

42.6 ±7.3% 

195 ±1.0% 

146 ± 4.8% <^' 

1060 ±13% 

13.3 ±0.0% 

493±22%<^' 

969 ±11 % 

NR<^> 

57.6 ± 7.3% <^' 

116 ±0.87% 

69.0 ±10%'^' 

0.483 ±6.4% 

1.96 ±2.6% 

347 ± 0.58% 

199 ±4.5% 

0.851 ± 2.6% 

398 ±00 % 

934 ±4.9% 

128 ±13% 

3.00 ± 3.0% 

85.5 ±6.8% 

23.8 ±3.4% 

29.0 ± 38% '^' 

<0.100 

<0.0400 

0.0478 

TTie analytical method uncertainties associated with the reported results are: PFBS ± 11 %, PFHS ± 14%, and PFOS ± 36%. 

(1) The analytical uncertainty has been adjusted for PFOS based on FIVIS recovery for DAL GW 131L to ± 39%, D/M. GW 135L 

to±37%, DALGW136Lto±41%, and DAL GW 144S to ± 37%. 

(2) The low field matrix spike for PFOS had a recovery that >200%, while the high field matrix spike met method acceptance 

criteria. 

(3) The RPD did not meet method acceptance criteria of s20%. 

(4) NR = Not Reported; Recovery of the only appropriate field matrix spike was >200%. See section 9 of the report for additional 

information. 

Page 10 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

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

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

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

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

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

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

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

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

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

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

two field matrix spike samples. Each empty container was mari<ed with a "fill to here" line to produce a 

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

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

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

Sample bottles for select sampling locations were fortified with intemal standard prior to sample 

collection to aid in sample analysis. These included sampling locations: DAL GW 134S, DAL GW 135S, 

DAL GW 136R, DAL GW 137R, DAL GW 137S, DAL GW 137L, DAL GW 138L, Trip Blank samples, 

and equipment rinseate blanks. Where applicable, intemal standards were used to aid in the data 

quality objectives. 

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

Laboratory method ETS-8-044.0 "Detennination of Perfluorinated Compounds In Water by High 

Perfonnance Liquid Chromatography/Mass Spectrometry Direct Injection Analysis". 

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

collected, the trip blank, and the aqueous equipment rinseate blank samples. Tables 10-41 summarize 

the individual sample results and the associated field matrix spike 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. 

Page 11 of 113 
GLP10-01-02; Interim Report 18 

/^alysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Reference Substance 

Chemical Name 

Chemical Formula 

Identifier 

Use 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFBS 

(predominantly linear) 

Perfluorobutane sulfonate 

C4F9SO3" 

Potassium Salt 

Target Analyte Reference 

Standard 

3M 

1/10/2017 

Frozen 

41-2600-8442-5 

TCR-121 

White Powder 

96.7% 

PFHS 

(lineal) 

Perfluorohexane sulfonate 

CeFisSOa' 

Sodium Salt 

Target Analyte Reference 

Standard 

Wellington 

4/2/2013 

Frozen 

LPFHxSAMOS 

TCR08-0018 

Crystalline 

98% 

Chemical Name 

Chemical Formula 

Identifier 

Use 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFOS 

(linear) 

Perfluorooctane sulfonate 

CsFiySOs' 

Potassium Salt 

CAS #2795-39-3 

Target Analyte Reference 

Standard 

Wellington 

10/18/2013 

Frozen 

LPFO8KBM06 

TCR08-0001 

Crystalline 

98% 

PFOS 

(linear + branclied) 

Perfluorooctane sulfonate 

C8F17SO3" 

Potassium Salt 

CAS #2795-39-3 

LCS Reference Standard 

3M 

12/14/2016 

Frozen 

171 

TCR-696 

White Powder 

86.4% 

"CB-PFOS 

Sodium 

Periluorooctanesulfonate 

"CsFiySOaNa" 

CAS#MPFC-C-0511 

Intemal Standard 

Wellington 

05/25/2014 

Frozen 

092310 

TCR11-0016 

Liquid 

5 |jg/mL <^' 

( C) periluoroalkylsulfonates and one mass-labeled ("C) perfluoro-1-octanesulfbnamide. 

Page 12 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

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

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

specific lot of test substance. 

Table 2. Sample Description Key Code. 

string Number 

Example 

1 

2 

3 

4 

5 

6 

string Descriptor Example 

DAL GW131R 0110622 

Sampling Location 

Well ID 

Sampling Point 

Well Level 

Sampling Date 

Sample Type 

DAL = Decatur, Alabama 

GW= Groundwater 

Example: 131 

R = Residum shallow water-bearing zone 

L = Bedrock water-bearing zone 

S = Epikarst middle water-bearing zone 

110622 = June22,2011 

0=primary sample 

DB=duplicate sample 

LS = low spike 

MS = 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 Perfonnance 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 GLP10-01-02-18 were retumed 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 of 1 mL 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 MillJQ water. 

Samples associated with sampling locations DAL GW 143R and DAL GW 144S were spiked with 

intemal standard by adding an aliquot of intemal standard stock solution into 10 mLs of sample. Internal 

standard was added to aid on the quanitation of the samples. 

Page 13 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA - June 2011 

7.4 Analysis 

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

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

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

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

Table 3. Instrument Parameters. 

Instrument Name 

Analytical Method Followed 

Analysis Date 

Liquid Chromatograph 

Guard column 

Analytical column 

Injection Volume 

lUlass Spectrometer 

Ion Source 

Electrode 

Polarity 

Software 

ETSKir1< 

ETS-8-044.0 

7/20/11 - PFBS, PFHS, and PFOS 

Agilent 1200 

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

Betasil 018 (2.1 mm X 100 mm), 5\i 

2 or 10 ^L 

Applied Biosystems PP\ 5500 

Turtx) Spray 

Turtx) ion electrode 

Negative 

Analyst 1.5.2 

ETS Kirk 

ETS-8-044.0 

7/29/1 land 8/2/11-PFOS 

Agilent 1200 

Betasil 018 (4.6 mm X 100 mm), 5n 

Betasil 018 (4.6 mm X 100 mm), 5n 

25 nL 

Applied Biosystems API 5500 

Turbo Spray 

Turtx) ion electrode 

Negative 

Analyst 1.5.2 

Table 4. Liquid Chromatography Conditions. 

Step 

Number 

Total Time 

(min) 

Flow Rate 

(fiUmin) 

Percent >4 

(2 mM ammonium acetate) 

PercentS 

(Methanol) 

ETS-8-044.0 Analyzed 7/20/11 

0 

1 

2 

3 

4 

5 

0 

2.0 

14.5 

15.5 

16.5 

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 

ETS-8-044.0 Analyzed 7/29/11 and 8/2/11 

0 

1 

2 

3 

4 

•5 

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 

Page 14 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA - June 2011 

Table 5. Mass Transitions. 

Analyte 

PFBS 

PFHS 

PFOS 

Mass Trarjsition 

Q1/Q3 

299/80 

299/99 

399/80 

399/99 

499/80 

499/99 

499/130 

Reference 

Material 

structure 

Linear 

Linear 

Linear 

Intemal Standard 

NA 

NA 

t^Cel-PFOS'^' 

Mass Transition 

Q1/Q3 

NA 

NA 

507/80 

Dwell time was 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 PFOS for sampling locations DAL GW 1358, DAL GW 1378, 

DAL GW 137L, DAL GW 138L, DAL GW 144R and DAL GW 1438. 

8 Analytical Results 

8.1 Calibration 

Samples were analyzed against an external standard calibration curve. Calibration standards were 

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

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

analyzed. A quadratic, 1/x weighted, calibration curve of the peak area counts was used to fit the data 

for each analyte. The data were not forced through zero during the fitting process. Calculating the 

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

For sampling locations DAL GW 135S, DAL GW 137S, DAL GW 137L, DAL GW 138L, DAL GW 143R, 

DAL GW 144R and rinseate blanks for PFOS: Samples were analyzed using a stable isotope intemal 

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

solution containing the target analytes into a laboratory-prepared synthetic groundwater containing 

calcium and magnesium. A separate 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 peak area counts was used to fit the 

data for each analyte. The data were not forced through zero during the fitting process. Calculating the 

standard concentrations using the peak area ratios and the resultant calibration curve confirmed 

accuracy of each curve point. 

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 PFBS, PFHS, and PFOS. 

8.2 System Suitability 

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

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

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

met for PFBS, PFHS, and PFOS with the exception of the external calibration of the synthetic water 

curve which had an area count RSD of 9.3%. Other QC items were used to assess data accuracy 

Page 15 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

including calibration curve point accuracy, curve fit criteria, CCVs, and LCS, all meeting method 

acceptance criteria. A method deviation is included with the raw data. 

8.3 Limit of Quantitation (LOQ) 

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

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

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

Table 6. Limit of Quantita tion (LOQ). 

Analysis Date 

7/20/11 Analysisexternal calibration 

7/29/11 Analysisexternal calibration 

7/29/11 Analysisinternal standard 

calibration 

8/2/11 Analysis -

internal standard 

calibration 

Dilution 

1 

5 

10 

50 

100 

1 

10 

100 

1 

1 

PFBS 

LOQ, ng/mL 

0.0250 

0.125 

0.250 

1.25 

2.50 

NA 

NA 

NA 

NA 

NA 

PFHS 

LOQ, ng/mL 

0.0250 

0.125 

0.250 

1.25 

2.50 

NA 

NA 

NA 

NA 

NA 

PFOS 

LOQ, ng/mL 

0.100 

0.500 

1.00 

5.00 

10.0 

1.00 

10.0 

100 

0.100 

0.0400 

NA = Not Applicable 

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 PFBS, PFHS, and PFOS except for the external 

calibration of the synthetic water curve where two CCVs had recoveries outside method acceptance 

criteria of 100% ± 25% for PFOS. The two non-compliant CCVs did not bracket any samples reported 

herein. 

8.5 Blanks 

Two types of blanks were prepared and analyzed with the samples: method blanks and field/trip blanks. 

Method blank results were reviewed and used to evaluate method perfonnance and to determine the 

LOQ for each analyte 

8.6 Lab Control Spikes (LCSs) 

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

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

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

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

of LCS at each level should be within 100% ± 20% with an RSD <20%. 

7/20/11 Analysis: All LCSs met acceptance criteria for PFBS, PFHS, and PFOS. 

Page 16 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

7/29/11 Analysis - intemal calibration: The low set of LCS samples for PFOS had an average recovery 

of 126%. The mid and high sets of LCS samples met acceptance criteria for PFOS. 

7/29/11 Analysis - external calibration: The low set of LCS samples for PFOS were spiked below the 

LOQ. The mid and high sets of LCS samples met acceptance criteria for PFOS. 

8/2/11 Analysis -All LCSs met acceptance criteria for PFOS. 

As the reference material used for quantitafion of PFOS is predominantly linear, and the PFOS present 

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

PFOS (linear and branched) were prepared at three concentrations in triplicate to evaluate the potential 

for analytical bias. 

7/20/11 Analysis: All linear and branched PFOS LCSs met acceptance criteria. 

7/29/11 Analysis - intemal calibration: The low set of LCS samples (linear and branched) for PFOS had 

an average recovery of 136% and the high set had an average recovery of 122%. The mid set of LCS 

samples met acceptance criteria for PFOS. 

7/29/11 Analysis - external calibration: The low set of LCS samples (linear and branched) for PFOS 

were spiked below the LOQ. The mid and high sets of LCS samples met acceptance criteria for PFOS. 

8/2/11 Analysis: The low, mid, and high linear and branched LCSs had average recoveries of 129%, 

122%, and 122%. 

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

, „ „ _ . _, Calculated Concentration , . .„„, 

LCS Percent Recovery = * 100% 

Spike Concentration 

LCS% RSD = standard deviation LCS replicates .., ^^y^ 

average LCS recovery 

Page 17 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA - June 2011 

Table 7. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Analyzed 7/20/11 

External standard 

calibration 

Lab ID 

LCS-110714-1 

LCS-110714-2 

LC8-110714-3 

Average ±%RSD 

LCS-110714-4 

LC8-110714-5 

LC8-110714-6 

Average ± %RSD 

LC8-110714-7 

LCS-110714-8 

LCS-110714-9 

Average ±%RSD 

PFBS 

Spiked 

Concentsdon 

(ng/mL) 

0.498 

0.498 

0.498 

Calculated 

Concentration 

(ng/mL) 

0.507 

0.514 

0.514 

VoRecovery 

102 

103 

103 

103 ±0.56% 

4.98 

4.98 

4.98 

5.14 

5.14 

5.13 

103 

103 

103 

103% ±0.0% 

29.9 

29.9 

29.9 

29.9 

29.0 

29.5 

100 

96.8 

98.8 

98.5% ±1.6% 

PFHS 

Spiked 

Concentration 

(ng/mL) 

0.498 

0.498 

0.498 

Calculated 

Concentration 

(ng/mL) 

0.524 

0.526 

0.537 

VoRecovery 

105 

106 

108 

106% ±1.4% 

4.98 

4.98 

4.98 

5.21 

5.30 

5.20 

105 

106 

104 

105% ±1.0% 

29.9 

29.9 

29.9 

30.1 

28.6 

29.8 

101 

95.6 

99.7 

98.8% ±2.9% 

ETS-8-044.0 

Analyzed 7/20/11 

External standard 

calibration 

Lab ID 

LCS-110714-1 

LC8-110714-2 

LC8-110714-3 

Average ±%RSD 

LC8-110714-4 

LC8-110714-5 

LCS-110714-6 

Average ±%RSD 

LCS-110714-7 

LCS-110714-8 

LC8-110714-9 

Average ±%RSD 

PFOS (linear) 

Spiked 

Concentration 

(ng/mL) 

0.498 

0.498 

0.498 

Calculated 

Concentration 

(ng/mL) 

0.427 

0.432 

0.448 

VoRecovery 

85.8 

86.8 

89.9 

87.5% ±2.4% 

4.98 

4.98 

4.98 

4.93 

4.92 

4.72 

98.9 

98.8 

94.7 

97.5% ±2.5% 

29.9 

29.9 

29.9 

30.5 

28.5 

29.6 

102 

95.2 

98.9 

98.7% ±3.4% 

Lab ID 

LC8-110714-10 

LC8-110714-11 

LCS-110714-12 

Average ±%RSD 

LC8-110714-13 

LCS-110714-14 

LC8-110714-15 

Average ±%RSD 

LC8-110714-16 

LC8-110714-17 

LCS-110714-18 

Average ±%RSD 

PFOS (linear+branclied) 

Spiked 

Concentration 

(ng/mL) 

0.495 

0.495 

0.495 

Calculated 

Concentration 

(ng/mL) 

0.469 

0.460 

0.437 

VoRecovery 

94.7 

92.9 

88.3 

92.0% ±3.6% 

4.96 

4.96 

4.96 

4.14 

4.33 

4.46 

83.5 

87.3 

89.9 

86.9% ±3.7% 

29.8 

29.8 

29.8 

29.4 

29.3 

28.5 

98.6 

98.3 

95.6 

97.5% ±1.7% 

Page 18 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Table 7 continued. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Analyzed 7/29/11 

Intemal standard 

calibration 

Lab ID 

LC8-110726-1 

LC8-110726-2 

LCS-110726-3 

Average ± %RSD 

LC8-110726-4 

LC8-110726-5 

LCS-110726-6 

Average ± %RSD 

LC8-110726-7 

LC8-110726-8 

LC8-110726-9 

Average ±%RSD 

PFOS (linear) 

Spiked 

Concentration 

(ng/mL) 

0.199 

0.199 

0.199 

Calculated 

Concentration 

(ng/mL) 

0.257 

0.248 

0.250 

VoRecovery 

129 

125 

125 

126% ±1.8%*^' 

1.99 

1.99 

1.99 

2.11 

2.00 

2.11 

106 

101 

106 

104% ±2.8% 

19.9 

19.9 

19.9 

20.8 

21.4 

21.1 

105 

107 

106 

106% ±0.94% 

Lab ID 

LCS-110726-10 

LCS-110726-11 

LCS-110726-12 

Average ±%RSD 

LCS-110726-13 

LCS-110726-14 

LCS-110726-15 

Average ±%RSD 

LCS-110726-16 

LC8-110726-17 

LC8-110726-18 

Average ± %RSD 

PFOS (linear+branched) 

Spiked 

Concenbation 

(ng/mL) 

0.198 

0.198 

0.198 

Calculated 

Concentration 

(ng/mL) 

0.272 

0.264 

0.271 

VoRecovery 

137 

133 

137 

136%±1.7%<" 

1.98 

1.98 

1.98 

2.26 

2.34 

2.47 

114 

118 

125 

119% ±4.7% 

19.8 

19.8 

19.8 

22.9 

241 

25.6 

116 

122 

129 

122% ±5.3%TM 

ETS^044.0 

/sjialyzed 7/29/11 

External standard 

calibration 

Lab ID 

LCS-110726-4 

LCS-110726-5 

LC8-110726-6 

Average ± %RSD 

LCS-110726-7 

LCS-110726-8 

LCS-110726-9 

Average ±%RSD 

PFOS (linear) 

Spiked 

Concentration 

(ng/mL) 

1.99 

1.99 

1.99 

Calculated 

Concentration 

(ng/mL) 

2.07 

2.08 

2.04 

VoRecovery 

104 

104 

103 

104% ±0.56% 

19.9 

19.9 

19.9 

21.4 

21.7 

20.1 

107 

109 

101 

106% ±3.9% 

Lab ID 

LC8-110726-13 

LC8-110726-14 

LCS-110726-15 

Average ±%RSD 

LC8-110726-16 

LC8-110726-17 

LCS-110726-18 

Average ±%RSD 

PFOS (linear+branched) 

Spiked 

Concentration 

(ng/mL) 

1.98 

1.98 

1.98 

Calculated 

Concentration 

(ng/mL) 

2.04 

2.04 

2.27 

VoRecovery 

103 

103 

115 

107% ±6.5% 

19.8 

19.8 

19.8 

17.2 

19.2 

17.2 

87.1 

97.1 

86.6 

90.3% ±6.6% 

(1) The average recovery did not meet method acceptance criteria of 100% ± 20%. 

Page 19 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA - June 2011 

Table 7 continued. Laboratory Control Spike Recovery. 

ETS^044.0 

Analyzed 8/2/11 

Intemal standard 

calibration 

Lab ID 

LCS-110726-1 

LCS-110726-2 

LCS-110726-3 

Average ±%RSD 

LCS-110726^ 

LC8-110726-5 

LC8-110726-6 

Average ±%RSD 

LCS-110726-7 

LCS-110726-8 

LCS-110726-9 

Average ±%RSD 

PFOS (linear) 

Spiked 

Concentration 

(ng/mL) 

0.199 

0.199 

0.199 

Calculated 

Concentration 

Jng/mL) 

0.219 

0.211 

0.226 

VoRecovery 

110 

106 

114 

110% ±3.6% 

1.99 

1.99 

1.99 

2.15 

2.04 

2.13 

108 

103 

107 

106% ±2.5% 

19.9 

19.9 

19.9 

21.1 

21.7 

21.4 

106 

109 

107 

107% ±1.4% 

Lab ID 

LCS-110726-10 

LCS-110726-11 

LC8-110726-12 

Average ±%RSD 

LC8-110726-13 

LC8-110726-14 

LC8-110726-15 

Average ±%RSD 

LCS-110726-16 

LCS-110726-17 

LCS-110726-18 

Average ±%RSD 

PFOS (linear+branched) 

Spiked 

Concentration 

(ng/mL) 

0.198 

0.198 

0.198 

Calculated 

Concentration 

(ng/mL) 

0.252 

0.254 

0.264 

VoRecovery 

127 

128 

133 

129% ±2.5%*^' 

1.98 

1.98 

1.98 

2.29 

2.39 

2.53 

l i 6 

121 

128 

122% ±5.0%TM 

19.8 

19.8 

19.8 

23.0 

24.3 

25.3 

116 

123 

128 

122% ±4.9%TM 

(1) The average recovery did not meet method acceptance criteria of 100% ± 20%. 

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%. The most recent 50 data points were used to generate the 

method uncertainty values listed in Table 8. The method uncertainty for PFOS by ETS-12-012-2 was 

found to be ± 28%, however, since the low set of linear and branched LCS had an average recovery of 

136%, the analytical uncertainty assigned to this study for PFOS will be ± 36%. 

Table 8. Analytical Uncertainty. 

Analyte 

PFBS 

PFHS 

PFOS 

Standard Deviation 

5.59 

7.12 

NA 

Method Uncertainty 

±11% 

±14% 

±36% 

NA = Not Applicable 

Page 20 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

FSIA-June 2011 

8.8 Field Matrix Spikes (FMS) 

Low, mid, and high field matrix spikes (FMS) were collected at each sampling point (low and high FMS 

only at 131R, 134R, and 135R) to verify that the analytical method is applicable to the collected matrix. 

Field matrix spikes were generated by adding a measured volume of field sample to a container spiked 

by the laboratory with PFBS (linear), PFHS (linear), and PFOS (linear) 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 IVIatrix Spike Levels. 

Sampling Location 

1348,1358,136R, 137R, 1378,137L 138L 

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

141R, 142R, 143R, 1448 

130R, 1308,1338,133L 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 

PFBS, ng/mL 

0.102 

1.02 

10.2 

1.02 

10.2 

102 

10.2 

102 

510 

102 

1972 

1.02 

10.2 

102 

510 

PFHS, ng/mL 

0.102 

1.02 

10.2 

1.02 

10.2 

102 

10.2 

102 

510 

102 

2000 

1.02 

10.2 

102 

510 

PFOS, ng/mL 

0.0985 

0.985 

9.85 

0.985 

9.85 

98.5 

9.85 

98.5 

493 

98.5 

2000 

0.985 

9.85 

98.5 

493 

(Sample Concentration of FMS - Average Concentration: Field Sample & FieldSample Dup.) .„,„„„, 

FMS Recovery = -^^ ^-^* 100% 

Spike Coneentraten 

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 njles. 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 1 SOL - The recovery of the high FMS sample for PFOS was 68.3%. The high spike, the only 

appropriate spike level as compared to the sample concentration, is still within the analytical uncertainty 

of 100% ± 36%. No additional adjustment will be made to the analytical uncertainfy. 

DAL GW 131L - The recovery of the high FMS sample for PFOS was 61.2%. Since the high spike 

was the only appropriate spike level as compared to the sample concentration, the analytical 

uncertainty has been adjusted for PFOS to 100% ± 39%. 

Page 21 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

DAL GW 133L - The recovery of the mid FMS sample for PFOS was 231 %. The high FMS sample 

met acceptance criteria with a recovery of 92.1%. Since both spiking levels were appropriate as 

compared to the sample concentration, the sample set will be reported and footnoted. 

DAL GW 134L - The sample RPD was 22% for PFOS. 

DAL GW 135S - The recovery of the high FMS sample for PFOS was 224%. Since the high spike 

was the only appropriate spike level as compared to the sample concentration, the sample set will not 

be reported since the FMS recovery was greater than 100% ± 50%. 

DAL GW 135L - The recovery of the high FMS sample for PFOS was 63.4%. Since the high spike 

was the only appropriate spike level as compared to the sample concentrafion, the analytical 

uncertainty has been adjusted for PFOS to 100% ± 37%. 

DAL GW 136L - The recovery of the high FMS sample for PFOS was 58.9%. Since the high spike 

was the only appropriate spike level as compared to the sample concentration, the analytical 

uncertainty has been adjusted for PFOS to 100% ± 41 %. 

DAL GW 141R - The recovery of the high FMS sample for PFOS was 65.6%. The mid FMS sample 

met method acceptance criteria. Since the mid spike was the most appropriate spike level as 

compared to the sample concentration, the analytical uncertainty will not be iadjusted for PFOS. 

DAL GW 142R - The recovery of the high FMS sample for PFOS was 68.5%. The high spike, the only 

appropriate spike level as compared to the sample concentration, is still within the analytical uncertainty 

of 100% ± 36%. No additional adjustment will be made to the analytical uncertainty. 

DAL GW 144S - The recovery of the high FMS sample for PFOS was 63.5%. Since the high spike 

was the only appropriate spike level as compared to the sample concentration, the analytical 

uncertainty has been adjusted for PFOS to 100% ± 37%. 

Page 22 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Table 10. DAL GW 130R110630 

3MUMSID 

GLP10-O1-O2-1&<306 

GLP10-01-02-18-007 

GLP10-01-02-18-008 

GLP10-01-02-18^09 

GLPIO^I-02-18-010 

Average Concenti 

Description 

DAL GW130R 0110630 

DAL GW130RDB 110630 

DAL GW130R LS110630 

DALGW130RMS110630 

DALGW130RH8110630 

ration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

16.4 

16.1 

25.0 

110 

501 

VoRecovery 

NA 

NA 

85.8 

91.9 

95.0 

16.3 ng/mL ±1.8% 

PFHS 

Concentration 

(ng/mL) 

125 

125 

131 

218 

629 

VoRecovery 

NA 

NA 

NC 

91.2 

98.8 

125 ng/mL ±0.0% 

PFOS 

Concentration 

(ng/mL) 

440 

460 

501 

492 

853 

VoRecovery 

NA 

NA 

NC 

NC 

81.8 

450 ng/mL ±4.4% 

NA = Not Applicable 

NC = Not Calculated; the endogenous sample concentration is greater than 2x the spike level. 

Reported results from external standard calibration. 

Table 11. DAL GW 1 SOS 1106S0 

3MUMSiD 

GLP10-01-02-18-011 

GLP10-01-02-18-012 

GLP10-01-02-18-013 

GLP10-01-02-18-014 

GLP10-01-02-18-015 

Average Concenti 

Description 

DALGW 1308 0110630 

DALGW130SDB110630 

DALGW130SL8110630 

DALGW130S MS 110630 

DALGW130SHS 110630 

•ation (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

3.53 

3.53 

13.7 

102 

504 

VoRecovery 

NA 

NA 

100 

96.5 

98.4 

3.53 ng/mL ±0.0% 

PFHS 

Concentration 

(ng/mL) 

29.8 

29.7 

39.9 

130 

577 

%Recovery 

NA 

NA 

NC 

983 

107 

29.8 ng/mL ±0.34% 

PFOS 

Concentration 

(ng/mL) 

100 

95.1 

113 

185 

466 

%Recovery 

NA 

NA 

NC 

88.8 

74.8 

97.6 ng/mL ±5.0% 

NA = Not Applicable 

NC = Not Calculated; the endogenous sample concentration Is greater than 2x the spike level. 

Reported results from external standard calibration. 

Page 23 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Table 12. DAL GW 130L 110630 

3M LIMS ID 

GLP10-01-02-18-016 

GLP10-01-02-18-017 

GLP10^1-02-18-018 

GLP1O-01-O2-18-019 

GLP10-01-02-18-020 

Description 

DAL GW130L 0110630 

DAL GW130LDB 110630 

DAL GW130LLS 110630 

DAL GW130L MS 110630 

DALGW130L HS 110630 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

1.68 

1.65 

2.77 

12.4 

98.2 

VoRecovery 

NA 

NA 

108 

105 

94.6 

1.67 ng/mL ±1.8% 

PFHS 

Concentration 

Jng/mL) 

13.7 

13.4 

15.2 

241 

114 

VoRecovery 

NA 

NA 

NC 

103 

98.5 

13.6 ng/mL ±2.2% 

PFOS 

Concentration 

(ng/mL) 

62.0 

65.4 

72.0 

72.4 

131 

VoRecovery 

NA 

NA 

NC 

NC 

683 <^' 

63.7 ng/mL ±5.3% 

NA = Not Applicable 

NC = Not Calculated; the endogenous sample concentration is greater than 2x the spike level. 

Reported iBsults from extemal standard calibration. 

(1) FMS did not ineet acceptance criteria of 100±30%. The recovery Is within the analytical uncertainty. 

Table 13. DALGW 131R110622 

3M LIMS ID 

GLP10-01-02-18-021 

GLP10-01-O2-18-022 

GLP10^1-02-18-023 

GLP10-01-02-18^24 

Description 

DAL GW131R 0110622 

DAL GW131RDB 110622 

DAL GW131RL8 110622 

DAL GW131RHS 110622 

Average Concentrati'on (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

53.9 

55.8 

157 

1880 

VoRecovery 

NA 

NA 

100 

92.6 

54.9 ng/mL ±3.5% 

PFHS 

Concentration 

(ng/mL) 

297 

311 

414 

2200 

VoRecovery 

NA 

NA 

NC 

94.8 

304 ng/mL ±4.6% 

PFOS 

Concentration 

(ng/mL) 

1530 

1480 

NA<^' 

3200 

VoRecovery 

NA 

NA 

NA<^' 

84.8 

1510 ng/mL ±3.3% 

NA = Not Applicable 

NC = Not Calculated; the endogenous sample concenfration is greater than 2x the spike level. 

Reported iBsults from extemal standard calibration. 

(1) FMS not analyzed since spike level was not appropriate in comparison to the sample concentration. 

Page 24 of 113 
GLP10-01-02; Interim Report 18 

/^alysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Table 14. DAL GW 131S 110622 

3M LIMS ID 

GLP10-01-O2-18-025 

GLP10-01-02-18-026 

GLP10-01-02-18-027 

GLP10^1-02-18-028 

GLP10-01-02-1&O29 

Average Concenti 

Description 

DALGW 1318 0110622 

DALGW131SDB 110622 

DALGW131SLS 110622 

DALGW1318 MS 110622 

DALGW1318HS 110622 

^ o n (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

0.914 

0.873 

1.93 

109 

98.9 

VoRecovery 

NA 

NA 

102 

981 

96.1 

0.894 ng/mL ±4.6% 

PFHS 

Concentration 

(ng/mL) 

5.26 

4.88 

6.07 

15.2 

104 

VoRecovery 

NA 

NA 

NC 

99.3 

97.0 

5.07 ng/mL ±7.5% 

PFOS 

Concentration 

(ng/mL) 

5.31 

5.42 

6.27 

13.1 

80.3 

VoRecovery 

NA 

NA 

NC 

78.5 

76.1 

5.37 ng/mL ±2.1% 

NA = Not /Vpplicable 

NC = Not Calculated; the endogenous sample concentration is greater than 2x the spike level. 

Reported results from extemal standard calibration. 

Table 15. DALGW131L 110622 

3MUMSID 

GLP10-01-02-18-030 

GLP10^1-02-18-031 

GLP10-01-02-18-032 

GLP10^1-02-18-033 

GLP10-01-02-18-034 

Average Concenti 

Description 

DAL GW131L 0110622 

DAL GW131LDB 110622 

DAL GW131LLS 110622 

DAL GW131L MS 110622 

DAL GW131LHS 110622 

ration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

340 

3.44 

444 

138 

102 

VoRecovery 

NA 

NA 

NC 

102 

96.6 

3.42 ng/mL ±1.2% 

PFHS 

Concentration 

(ng/mL) 

21.4 

21.8 

22.8 

32.8 

120 

VoRecovery 

NA 

NA 

NC 

NC 

96.5 

21.6 ng/mL ±1.9% 

PFOS 

Concentration 

(ng/mL) 

32.6 

32.1 

30.5 

42.0 

92.6 

%Recovery 

NA 

NA 

NC 

NC 

61.2TM 

32.4 ng/mL ±1.5% ^^> 

NA = Not /\pplicable 

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

Reported results litim extemal standard calibration. 

(1) FMS did not meet acceptance criteria of 100±30%. The analytical uncertainty for PFOS has been adjusted for FMS recovery to ± 39%. 

Page 25 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Table 16. DAL GW133R116030 

3MUMSiD 

GLP10-01-02-18-045 

GLP10-01-02-18^>46 

GLP10-01-O2-18O47 

GLP10-01-02-18-048 

GLP10-01-02-18-049 

Average Concenti 

Description 

DAL GW133R 0110630 

DALGW133RDB110630 

DAL GW133R LS110630 

DALGW133RM8110630 

DALGW133RHS110630 

ation (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

4.70 

488 

5.62 

143 

989 

%Recovery 

NA 

NA 

NC 

93.2 

92.3 

4.79 ng/mL ±3.8% 

PFHS 

Conceittration 

(ng/mL) 

32.6 

33.6 

32.0 

41.7 

130 

VoRecovery 

NA 

NA 

NC 

NC 

95.0 

33.1 ng/mL ±3.0% 

PFOS 

Concentration 

(ng/mL) 

44.1 

41.0 

37.5 

51.3 

111 

%Recovery 

NA 

NA 

NC 

NC 

69.5TM 

42.6 ng/mL ±7.3% 

NA = Not Applicable 

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

Repotted results from extemal standard calibration. 

(1) FMS did not meet acceptance criteria of 100±30%.. The recovery is within the analytical uncertainty 

Table 17. DAL GW 13SS 110630 

3M LIMS ID 

GLP10-01-O2-1&O40 

GLP10^1-02-18-041 

GLPIO^I-02-18^2 

GLP10-01-02-18-043 

GLP10-01-02-18-044 

Average Concenti 

Description 

DALGW 1338 0110630 

DALGW1338DB 110630 

DAL GW 1338 LS 110630 

DALGW 1338 MS 110630 

DALGW1338HS 110630 

ration (ng/mL) ±VoRPD 

PFBS 

Concentration 

(ng/mL) 

9.01 

9.14 

18.9 

105 

487 

VoRecovery 

NA 

NA 

96.3 

94.0 

93.7 

9.08 ng/mL ±1.4% 

PFHS 

Concentration 

(ng/mL) 

66.9 

67.4 

76.2 

167 

551 

VoRecovery 

NA 

NA 

NC 

97.9 

94.9 

67.2 ng/mL ±0.74% 

PFOS 

Concentration 

(ng/mL) 

196 

194 

202 

265 

585 

VoRecovery 

NA 

NA 

NC 

71.1 

79.2 

195ng/mL±1.0Vo 

NA = Not Applicable 

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

Reported results from extemal standard calibration. 

Page 26 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Table 18. DAL GW1 SSL 110630 

3M LIMS ID 

GLP10-01-02-18-035 

GLP10-01-02-18-036 

GLP10-01-02-18-037 

GLP10-01-02-18-038 

GLP10-01-02-18-039 

Average Concent 

Description 

DAL GW133L 0110630 

DAL GW133LDB 110630 

DAL GW133L LS110630 

DALGW133LMS110630 

DALGW133LH8110630 

ration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

6.68 

6.65 

17.2 

107 

487 

VoRecovery 

NA 

NA 

103 

98.4 

94.2 

6.67 ng/mL ±0.45% 

PFHS 

Concentration 

(ng/mL) 

47.3 

46.5 

61.6 

164 

543 

VoRecovery 

NA 

NA 

NC 

115 

97.3 

46.9 ng/mL ±1.7% 

PFOS 

Concentration 

(ng/mL) 

149 

142 

NA« 

373 

599 

VoRecovery 

NA 

NA 

NATM 

231 <"' 

92.1 

146 ng/mL ±4.8% 

NA = Not Applicable 

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

Reported results Irom extemal standard calibration. 

(1) Not Analyzed; The LS was not analyzed since it was not expected to be appropriate as compared to the sample concentration. 

(2) Field mabix spike did not meet method acceptance criteria of 100±30%. No adjusfrnent was made to the analytical uncertainty since both spike levels were appropriate as compared to 

the sample concentration. 

Table 19. DAL GW134R110628 

3MUMSID 

GLP10-01-02-18-050 

GLP10-01-02-18-051 

GLP10-01-02-18-052 

GLP10-01-02-18-053 

Description 

DAL GW134R 0110628 

DALGW134RDB110628 

DAL GW134RL8 110628 

DAL GW134RH8 110628 

Average Concerrtration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

51.7 

51.0 

150 

1890 

VoRecovery 

NA 

NA 

96.7 

932 

51.4 ng/mL ±1.4% 

PFHS 

Concentration 

(ng/mL) 

484 

481 

588 

2360 

VoRecovery 

NA 

NA 

NC 

93.9 

483 ng/mL ±0.62% 

PFOS 

Concentration 

(ng/mL) 

996 

1130 

1040 

2870 

VoRecovery 

NA 

NA 

NC 

90.4 

1060 ng/mL ±13% 

NA = Not Applicable 

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

Reported results from extemal standard calibration. 

Page 27 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Table 20. DALGW 1S4S 110628 

3M LIMS ID 

GLP10-01-02-18-059 

GLP10-01-02-18-060 

GLP10-01-02-18-061 

GLP10-01-02-18-062 

GLP10-01-02-18-063 

Average Concent 

Description 

DALGW 1348 0110628 

DALGW134SDB110628 

DALGW 1348 LS110628 

DALGW134SMS110628 

DALGW1348HS110628 

ration (ng/mL) ±VoRPD 

PFBS 

Concentration 

(ng/mL) 

0.255 

0.261 

0.371 

1.23 

10.8 

VoRecovery 

NA 

NA 

NC 

95.3 

103 

0.258 ng/mL ± 2.3% 

PFHS 

Concentration 

(ng/mL) 

3.05 

312 

312 

4.08 

140 

VoRecovery 

NA 

NA 

NC 

NC 

107 

3.09 ng/mL ±2.3% 

PFOS 

Concentration 

(ng/mL) 

13.3 

13.3 

12.6 

14.6 

24.9 

VoRecovery 

NA 

NA 

NC 

NC 

118 

13.3 ng/mL ±0.0% 

NA = Not Applicable 

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

Reported results \com extemal standard calibration. 

Table 21. DAL GW 1S4L 110628 

3MUMSID 

GLP1CW)1-02-18-054 

GLP10-01-O2-18-055 

GLP1001-02-18-056 

GLP10-01-02-18-057 

GLP1OO1-02-18-058 

Average Concenti 

Description 

DAL GW134L 0110628 

DAL GW134LDB 110628 

DAL GW134LLS 110628 

DAL GW134L MS 110628 

DAL GW134LHS 110628 

'ation (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

11.4 

12.2 

22.0 

108 

479 

VoRecovery 

NA 

NA 

100 

94.3 

91.6 

11.8ng/mL±6.8Vo 

PFHS 

Concentration 

(ng/mL) 

104 

118 

127 

216 

586 

VoRecovery 

NA 

NA 

NC 

103 

93.1 

111 ng/mL ± 13% 

PFOS 

Concentration 

(ng/mL) 

438 

547 

469 

534 

897 

VoRecovery 

NA 

NA 

NC 

NC 

82.1 

493 ng/mL ± 22% <^> 

NA= Not/Vpplicable 

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

Reported results from extemal standard calibration. 

(1) RPD did not meet acceptance criteria of s20%. 

Page 28 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Table22. DALGW 135R 110628 

3M LIMS ID 

GLP10-01-02-18-079 

GLP10-01-02-18-080 

GLP10-01-O2-18-081 

GLP10-01-02-18-083 

Description 

DAL GW135R 0110628 

DALGW135RDB110628 

DAL GW135R LS110628 

DAL GW135RH8 110628 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

74.9 

73.7 

172 

1840 

VoRecovery 

NA 

NA 

95.8 

89.5 

74.3 ng/mL ±1.6% 

PFHS 

Concentration 

(ng/mL) 

859 

828 

927 

2620 

VoRecovery 

NA 

NA 

NC 

88.8 

844 ng/mL ±3.r/o 

PFOS 

Concentration 

(ng/mL) 

1020 

917 

1070 

2480 

VoRecovery 

NA 

NA 

NC 

75.6 

969 ng/mL ±11% 

NA = Not Applicable 

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

Reported results from extemal standard calibration. 

Table 23. DALGW 135S 110628 

3M LIMS ID 

GLP10-01-02-18-069 

GLP10-01-02-18-070 

GLP1001-02-18-071 

GLP10-01-02-18-072 

GLP10-01-02-18-073 

Average Concent 

Description 

DALGW 1358 0110628 

DALGW 1358 DB 110628 

DALGW 1358 LS 110628 

DALGW 1358 MS 110628 

DALGW 1358 HS 110628 

ration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

1.20 

1.21 

1.41 

2.21 

10.5 

VoRecovery 

NA 

NA 

NC 

98.5 

91.1 

1.21 ng/mL ±0.83% 

PFHS 

Concentration 

(ng/mL) 

7.97 

8.15 

886 

9.22 

19.1 

VoRecovery 

NA 

NA 

NC 

NC 

108 

8.06 ng/mL ±2.2% 

PFOS 

Conceittration 

(ng/mL) VoRecovery 

Not Reported '^' 

NA = Not Applicable 

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

Reported results for PFBS and PFHS are from external standard calibration. PFOS was analyzed by both intemal standard and extemal standard calibration with the results from both 

analyses being not reportable. 

(1) Not Reported; ttie most appropriate field mafrix spike recovery was greater than 100% ±50%. 

Page 29 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Table 24. DAL GW 135L 110628 

3M LIMS ID 

GLP1OO1-02-18-074 

GLP10-01-02-18-075 

GLP10-01-02-18-076 

GLP10-01-02-18-077 

GLP10-01-02-18-078 

Average Concent 

Description 

DAL GW135L 0110628 

DAL GW135LDB 110628 

DAL GW135LL8 110628 

DAL GW135L MS 110628 

DAL GW135LH8 110628 

'ation (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

9.73 

9.65 

10.6 

19.9 

109 

VoRecovery 

NA 

NA 

NC 

100 

97.4 

9.69 ng/mL ±0.83% 

PFHS 

Concentration 

(ng/mL) 

71.9 

70.1 

73.9 

84.0 

176 

VoRecovery 

NA 

NA 

NC 

NC 

103 

71.0 ng/mL ±2.5% 

PFOS 

Concentration 

(ng/mL) 

55.5 

59.7 

48.1 

57.8 

120 

VoRecovery 

NA 

NA 

NC 

NC 

63.4TM 

57.6 ng/mL ±7.3%'^' 

NA= Not/Vpplicable 

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

Reported results from extemal standard calibration. 

(1) FMS did not meet acceptance criteria of 100±30%. The analytical uncertainty for PFOS has been adjusted tor FMS recovery to ± 37%. 

Table 25. DAL GW 136S 110630 

3M LIMS ID 

GLP10-01-02-18-088 

GLP10-01-02-18-089 

GLP10-01-02-18-090 

GLP10-01-02-18-091 

GLP10-01-02-18-092 

Average Concent 

Description 

DALGW 1368 0110630 

DALGW136SDB110630 

DALGW1368LS110630 

DALGW 1368 MS 110630 

DALGW136SH8110630 

'ation (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

371 

367 

461 

13.2 

99.8 

VoRecovery 

NA 

NA 

NC 

932 

94.2 

3.69 ng/mL ±1.1% 

PFHS 

Concentration 

(ng/mL) 

25.9 

25.7 

26.7 

35.2 

125 

VoRecovery 

NA 

NA 

NC 

NC 

97.3 

25.8 ng/mL ±0.78% 

PFOS 

Concentration 

(ng/mL) 

115 

116 

120 

118 

187 

%Recovery 

NA 

NA 

NC 

NC 

72.6 

116 ng/mL ±0.87% 

NA= Not Applicable 

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

Reported results from extemal standard calibration. 

Page 30 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Table 26. DAL GW 136L 110630 

3MUMSID 

GLP10-01-02-18-084 

GLP10-01-02-18-085 

GLP10-01-02-18-086 

GLP10-01-02-18-155 

GLP1OO1-02-18-087 

Average Concent 

Description 

DAL GW136L 0110630 

DAL GW136LDB 110630 

DAL GW136L LS110630 

DAL GW136L MS 110630 

DAL GW136LHS 110630 

ration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

2.33 

2.32 

3.32 

12.5 

101 

%Recovery 

NA 

NA 

NC 

99.8 

96.7 

2.33 ng/mL ±0.43% 

PFHS 

Concentration 

(ng/mL) 

15.9 

16.1 

17.0 

26.3 

115 

VoRecovery 

NA 

NA 

NC 

101 

97.1 

16.0 ng/mL ±1.3% 

PFOS 

Concentration 

(ng/mL) 

72.4 

65.5 

73.6 

84.8 

127 

VoRecovery 

NA 

NA 

NC 

NC 

58.9TM 

69.0ng/mL±10%'^> 

NA = Not Applicable 

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

Reported results from extemal standard calibration. 

(1) FMS did not meet acceptance criteria of 1 oa±30%. The analytical uncertainty for PFOS has been adjusted ft)r FMS recovery to ± 41 %. 

Table 27. DAL GW 1S7S 110624 

3MUMSID 

GLP10-01-02-18-O93 

GLP10-01-02-18-094 

GLP10-01-02-1&O95 

GLP10-01-02-18-096 

GLP10-01-02-18-097 

Average Concent 

Description 

DALGW 1378 0110624 

DALGW1378DB 110624 

DAL GW137SL8 110624 

DALGW 1378 MS 110624 

DALGW137SH8110624 

ration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

0.108 

0.105 

0.215 

1.05 

9.68 

VoRecovery 

NA 

NA 

106 

92.5 

93.9 

0.107 ng/mL ±2.8% 

PFHS 

Concentration 

(ng/mL) 

0.0814 

0.0798 

0.184 

1.06 

9.86 

VoRecovery 

NA 

NA 

101 

96.0 

95.9 

0.0806 ng/mL ±2.0% 

PFOS 

Concentration 

(ng/mL) 

0.498 

0.467 

0.569 

1.42 

10.2 

VoRecovery 

NA 

NA 

NC 

95.2 

98.7 

0.483 ng/mL ±6.4% 

NA= Not Applicable 

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

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

Page 31 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Table 28. DAL GW1 STL 110624 

3M LIMS ID 

GLP10-01-02-18-098 

GLP10-01-02-18-099 

GLP10O1-02-18-100 

GLP10-01-O2-18-101 

GLP10-01-02-18-102 

Average Concenti 

Description 

DAL GW137L 0110624 

DALGW137LDB110624 

DAL GW137L LS110624 

DALGW137LM8110624 

DALGW137LH8110624 

-ation (ng/mL) ± VoRPD 

PFBS 

Concentiation 

(ng/mL) 

0.0834 

0.0818 

0.189 

1.06 

9.70 

VoRecovery 

NA 

NA 

104 

95.8 

94.3 

0.0826 ng/mL ±1.9% 

PFHS 

Concentration 

(ng/mL) 

0.106 

0.107 

0.213 

1.10 

10.0 

VoRecovery 

NA 

NA 

104 

97.4 

97.0 

0.107 ng/mL± 0.94% 

PFOS 

Concentiation 

(ng/mL) 

1.93 

1.98 

2.01 

2.96 

12.0 

%Recovery 

NA 

NA 

NC 

102 

102 

1.96 ng/mL ±2.6% 

NA= Not Applicable 

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

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

Table 29. DAL GW 138S 110630 

3MUMSID 

GLP10-01-02-18-113 

GLP10-01-02-18-114 

GLP10-01-02-18-115 

GLP10-01-02-18-116 

GLP10-01-02-18-117 

Average Concenti 

Description 

DAL GW138S 0110630 

DALGW138SDB110630 

DALGW138SLS110630 

DALGW138SM8110630 

DALGW138SH8110630 

-ation (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

4.55 

4.58 

145 

96.8 

488 

%Recovery 

NA 

NA 

97.4 

90.4 

94.8 

4.57 ng/mL ±0.66% 

PFHS 

Concentration 

(ng/mL) 

23.2 

23.2 

33.4 

117 

528 

VoRecovery 

NA 

NA 

NC 

92.0 

99.0 

23.2 ng/mL ±0.0% 

PFOS 

Concentiation 

(ng/mL) 

194 

203 

221 

269 

593 

VoRecovery 

NA 

NA 

NC 

NC 

80.1 

199 ng/mL ±4.5% 

NA = Not Applicable 

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

Reported results from extemal standard calibration. 

Page 32 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

FSIA-June 2011 

Table 30. DALGW1S8L 1106S0 

3M LIMS ID 

GLP1001-02-18-108 

GLP10-01-02-18-109 

GLP10-01-02-18-110 

GLP10-01-02-18-111 

GLPiaOI-02-18-112 

Average Concent 

Description 

DAL GW138L 0110630 

DAL GW138LDB 110630 

DAL GW138LL8 110630 

DAL GW138L MS 110630 

DALGW138LHS110630 

-ation (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

0.0385 

0.0396 

0.135 

0.973 

9.06 

VoRecovery 

NA 

NA 

94.1 

91.6 

88.4 

0.0391 ng/mL ±2.8% 

PFHS 

Concentration 

(ng/mL) 

0.112 

0.113 

0.213 

1.08 

9.82 

%Recovery 

NA 

NA 

98.5 

94.9 

95.2 

0.113 ng/mL± 0.89% 

PFOS 

Concentration 

(ng/mL) 

0.840 

0.862 

1.04 

1.82 

10.8 

VoRecovery 

NA 

NA 

NC 

98.4 

101 

0.851 ng/mL ±2.6% 

NA = Not Applicable 

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

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

Table S1. DAL GW 1S8R110630 

3MUMSID 

GLP1OO1-02-18-103 

GLP10-01-02-18-104 

GLP10-01-02-18-105 

GLP10-01-02-18-106 

GLPiaO1-02-18-107 

Average Concent 

Description 

DAL GW138R 0110630 

DAL GW138RDB 110630 

DALGW138RLS110630 

DAL GW138R MS 110630 

DALGW138RHS110630 

ration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

8.01 

8.01 

17.7 

97.8 

462 

VoRecovery 

NA 

NA 

95.0 

88.0 

89.0 

8.01 ng/mL ±0.0% 

PFHS 

Concentration 

(ng/mL) 

39.1 

39.2 

48.8 

134 

515 

VoRecovery 

NA 

NA 

NC 

93.0 

93.3 

39.2 ng/mL± 0.26% 

PFOS 

Concentration 

(ng/mL) 

348 

346 

340 

405 

731 

VoRecovery 

NA 

NA 

NC 

NC 

78.0 

347 ng/mL ±0.58% 

NA = Not /Applicable 

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

Reported results from extemal standard calibration. 

Page 33 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Table 32. DAL GW CW26C 110622 

3MUMSID 

GLP10-01-02-18-118 

GLP10-01-02-18-119 

GLP10-01-O2-18-120 

GLP10-01-02-18-121 

GLP10-01-02-18-122 

Description 

DAL GWCW26C 0110622 

DAL GW CW26C DB 110622 

DAL GW CW26C LS 110622 

DAL GW CW26C MS 110622 

DAL GW CW26C HS 110622 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentiation 

(ng/mL) 

8.26 

8.20 

18.1 

106 

480 

VoRecovery 

NA 

NA 

96.8 

95.9 

92.5 

8.23 ng/mL ±0.73% 

PFHS 

Concentration 

(ng/mL) 

68.3 

67.2 

77.0 

166 

563 

VoRecovery 

NA 

NA 

NC 

96.3 

97.1 

67.8 ng/mL± 1.6% 

PFOS 

Concentiation 

(ng/mL) 

398 

398 

384 

499 

839 

VoRecovery 

NA 

NA 

NC 

NC 

89.5 

398 ng/mL ±0.0% 

NA = Not Applicable 

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

Reported results from extemal standard calibration. 

Table 33. DAL GW CW26L 110622 

3MUMSID 

GLP10-01-02-18-123 

GLP10-O1-02-18-124 

GLP10-01-02-18-125 

GLP10-01-02-18-126 

GLP10-01-02-18-127 

Description 

DAL GWCW26L 0110622 

DAL GW CW26L DB 110622 

DAL GW CW26L LS 110622 

DAL GW CW26L MS 110622 

DAL GWCW26LHS 110622 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

13.4 

13.5 

23.0 

107 

501 

VoRecovery 

NA 

NA 

93.6 

91.7 

95.6 

13.5 ng/mL ±0.74% 

PFHS 

Concentration 

(ng/mL) 

104 

105 

115 

202 

599 

VoRecovery 

NA 

NA 

NC 

95.6 

97.0 

105ng/mL±1.0% 

PFOS 

Concentration 

(ng/mL) 

911 

957 

925 

985 

1410 

%Recovery 

NA 

NA 

NC 

NC 

96.6 

934 ng/mL ±4.9% 

NA= Not Applicable 

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

Reported results from extemal standard calibration. 

Page 34 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Table 34. DAL GW 140R 110622 

3MUMSID 

GLP10-01-02-18-128 

GLP10-01-02-18-129 

GLP10-01-02-18-130 

GLP10-01-02-18-131 

GLP10-01-O2-18-132 

Description 

DAL GW140R 0110622 

DAL GW140RDB 110622 

DAL GW140R LS110622 

DAL GW140R MS 110622 

DAL GW140RH8 110622 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

1.58 

1.60 

11.3 

101 

477 

VoRecovery 

NA 

NA 

95.2 

97.5 

93.2 

1.59ng/mL±1.3% 

PFHS 

Concentration 

(ng/mL) 

17.7 

17.9 

27.8 

119 

508 

VoRecovery 

NA 

NA 

98.0 

99.2 

96.1 

17.8 ng/mL± 1.1% 

PFOS 

Concentration 

(ng/mL) 

119 

136 

125 

210 

598 

VoRecovery 

NA 

NA 

NC 

83.8 

95.5 

128 ng/mL ±13% 

NA = Not Applicable 

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

Reported results from extemal standard calibration. 

Table 35. DAL GW 141R 110630 

3M LIMS ID 

GLP1001-02-18-135 

GLP10-01-02-18-136 

GLP10-01-02-18-137 

GLP10-01-02-18-138 

GLP1OO1-02-18-139 

Average Concent 

Description 

DAL GW141R0 110630 

DALGW 141 RDB 110630 

DAL GW 141RLS 110630 

DALGW 141 RMS 110630 

DAL GW 141RHS 110630 

-ation (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

0.0437 

0.0425 

0.992 

9.49 

94.7 

VoRecovery 

NA 

NA 

93.0 

92.6 

92.8 

0.0431 ng/mL ±2.8% 

PFHS 

Concentration 

(ng/mL) 

0.298 

0.293 

1.30 

10.0 

99.1 

VoRecovery 

NA 

NA 

98.5 

95.1 

96.9 

0.296 ng/mL ±1.7% 

PFOS 

Concentiation 

(ng/mL) 

3.04 

2.95 

3.94 

10.0 

67.6 

VoRecovery 

NA 

NA 

NC 

71.1 

65.6TM 

3.00 ng/mL ±3.0% 

NA = Not Applicable 

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

Reported results from extemal standard calibration. 

(1) FMS did not meet acceptance criteria of 100±30%. The recovery is wittiin the analytical uncertainty. 

Page 35 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Table 36. DAL GW 142R110622 

3MUMSID 

GLP10-01-02-18-140 

GLPiaO1-02-18-141 

GLP10-01-02-18-142 

GLP10-01-02-18-143 

GLP10-01-02-18-144 

Average Concent 

Description 

DAL GW142R 0110622 

DAL GW142RDB 110622 

DAL GW142RL8 110622 

DAL GW142R MS 110622 

DALGW142RHS 110622 

ration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

1.69 

1.69 

2.62 

11.4 

97.0 

VoRecovery 

NA 

NA 

91.2 

95.2 

93.4 

1.69 ng/mL ±0.0% 

PFHS 

Concentration 

(ng/mL) 

10.0 

10.3 

11.1 

19.6 

109 

VoRecovery 

NA 

NA 

NC 

92.6 

96.9 

10.2 ng/mL ±3.0% 

PFOS 

Concentration 

(ng/mL) 

82.6 

88.4 

89.3 

85.2 

153 

VoRecovery 

NA 

NA 

NC 

NC 

685TM 

85.5 ng/mL ±6.8% 

NA = Not Applicable 

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

Reported results from extemal standard calibration. 

(1) FMS did not meet acceptance criteria of 100t30%. The recovery is within the analytical uncertainty. 

Table 37. DAL GW 143R110622 

3MUMSID 

GLP10-01-02-18-145 

GLP10-01-02-18-146 

GLP10-01-02-18-147 

GLP10-01-02-18-148 

GLP10-01-02-18-149 

Average Concent 

Description 

DAL GW143R 0110622 

DALGW143RDB 110622 

DALGW143RLS 110622 

DAL GW143R MS 110622 

DALGW143RHS 110622 

ration (ng/mL) ±VoRPD 

PFBS 

Concentration 

(ng/mL) 

1.64 

1.68 

2.62 

10.9 

96.0 

%Recovery 

NA 

NA 

94.1 

90.6 

92.5 

1.66 ng/mL ±2.4% 

PFHS 

Concentration 

(ng/mL) 

5.94 

6.17 

7.04 

15.4 

106 

VoRecovery 

NA 

NA 

NC 

91.6 

98.0 

6.06 ng/mL ±3.8% 

PFOS 

Concentration 

(ng/mL) 

23.4 

242 

NA<^> 

32.3 

123 

VoRecovery 

NA 

NA 

NA<^' 

NC 

101 

23.8 ng/mL ±3.4% 

NA= Not Applicable 

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

Reported results from extemal standard calibration. 

(1) FMS not analyzed since spike level was not appropriate in comparison to the sample concentration. 

Page 36 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Table 38. DAL GW 144S 110628 

3MUMSID 

GLP10-01-02-18-150 

GLP10-01-02-18-151 

GLP10-01-02-18-152 

GLP10-01-02-18-153 

GLP10-01-O2-18-154 

Average Concent 

Description 

DAL GW144S 0110628 

DAL GW144SDB 110628 

DALGW 1448 LS 110628 

DAL GW144S MS 110628 

DAL GW144SHS 110628 

ation (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

1.69 

1.62 

2.55 

11.4 

91.4 

VoRecovery 

NA 

NA 

87.7 

95.5 

88.0 

1.66 ng/mL ±4.2% 

PFHS 

Concentiation 

(ng/mL) 

7.28 

7.00 

7.99 

17.1 

98.5 

VoRecovery 

NA 

NA 

NC 

97.6 

89.6 

7.14 ng/mL ±3.9% 

PFOS 

Concentration 

(ng/mL) 

29.5 

28.4 

NA<^' 

37.0 

91.5 

VoRecovery 

NA 

NA 

NA*^' 

NC 

63.5 <^' 

29.0 ng/mL ±3.8%^^ 

NA = Not Applicable 

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

Reported results from extemal standard calibration. 

(1) FMS not analyzed since spike level was not appropriate in comparison to the sample concentration. 

(2) FMS did not meet acceptance criteria of 100t30%. The analytical uncertainty for PFOS has been adjusted for FMS recovery to ± 37%. 

Table 39. Trip Blank 1 

3MUMSID 

GLP10-01-02-18-064 

GLP10-01-02-18-065 

GLP10-01-02-18-066 

GLP10-01-02-18-067 

GLP10-01-02-18-068 

Description 

Trip Blank Set 1 Sample 

Trip Blank Set 1 LS 

Trip Blank Set 1 MS 

Trip Blank Set 1MHS 

Trip Blank Set 1HS 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

1.05 

10.3 

102 

508 

VoRecovery 

NA 

103 

101 

100 

99.6 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

1.10 

10.9 

105 

523 

%Recovery 

NA 

108 

107 

103 

103 

PFOS 

Concentration 

(ng/mL) 

<0.100 

1.01 

9.45 

102 

381 

%Recoveiy 

NA 

103 

95.9 

104 

77.4 

NA= Not Applicable 

Reported results from extemal standard calibration. 

Page 37 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Table 40. Trip Blank 2 

3MUMSID 

GLP10-01-02-18-001 

GLP10-01-02-18-O02 

GLP10-01-O2-18-O03 

GLP10-O1-O2-18-004 

GLP10-01-02-18-005 

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 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

0.995 

9.62 

93.0 

459 

VoRecovery 

NA 

97.5 

94.3 

91.2 

90.0 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

1.01 

9.98 

95.2 

477 

VoRecovery 

NA 

99.0 

97.8 

93.3 

93.5 

PFOS 

Concentration 

(ng/mL) 

<0.100 

0.903 

8.39 

91.2 

344 

%Recovery 

NA 

91.7 

85.2 

92.6 

69.8 

NA = Not Applicable 

Reported results from extemal standard calibration. 

Table 41. Rinseate Blanks 

3MUMSID 

GLP10-01-02-18-133 

GLP10-01-02-18-134 

Description 

DALGW130LRB 110630 

DALGW133SRB 110630 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

VoRecovery 

NA 

NA 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

VoRecovery 

NA 

NA 

PFOS 

Concentration 

(ng/mL) 

<0.0400 

0.0478 

VoRecovery 

NA 

NA 

NA= Not Applicable 

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

Page 38 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA - June 2011 

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

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

3M Environmental Laboratory method ETS-8-044.0 described herein. 

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

to 3M Environmental Laboratory standard operating procedures. 

Attachment A: Protcx:ol Amendment 18 (General Project Outline) 

Attachment B: Representative Chromatograms and Calibration Curves 

Attachment C: Analytical Method 

Attachment D: Method Deviation 

Page 39 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Date 

'zeJ) 

Cleston Lange,i^h.D., 3M Principal Analytical Investigator 

2jf£i^r^// 

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

u 

Gary , Spcifisor Representative 

OM/Jy 

Date 

Jaisimha Kesari,^tudy Director / Date 

Page 40 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

ATTACHMENT A: PROTOCOL AMENDMENT 

Page 41 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Analytical Protocol: GLPIO-01-02 

Amendment 18 

Study Tide 

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

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

Decatur Phase 3 Site-Related Monitoring Program 

PROTOCOL AMENDMENT NO. 18 

Amendment Date: 

June 15,2011 

Performing Laboratory 

3M Environmental, Health, and Safety Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55144-1000 

Laboratory Project Identification 

GLPIO-01-02 

Sampling Event 

Former Sludge Incorporation Area (FSIA) Groundwater 

Page 1 of 8 

Page42of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

AnalyScal Protocol: GLPIO-01-02 

Amendment IB 

This annendment modifies the following portion of protocol: 

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

Decatur Phase 3 Site-Related Monitoring Program" 

PimTocoL READS: 

No changes to the wording of the protocol are required. 

AUEND TO READ: 

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

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

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

(GLPIO-01-02). 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 GLP10-01-02-18 and reported as interim report GLP10-01-02-

18, (reflecting study GLP10-01-G2 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 form. 

Page 2 of 8 

Page 43 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA - June 2011 

Analytical Protocol: GLPIO-01-02 

Amendment 18 

Amendment Approval 

J^H W^1^^. 

% , 

(( 

Gary Hohenstein, Sponsor Representative 

^/^s/'Z.C) , } 

Cleston C. Lange, Principal Analytical Investigator Date 

^ ^ ^ /j-Jz// ^ ^O/J 

William Reagen, EHS Opns Environmental Lab Management 

iM.A// 

Date 

Jaisimha Kesari P.&rDEE, Study Director 

Page 3 of 8 

Page44of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Analytical Protocol: GLPIO-01-02 

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: William Reagen, 3M EHS&Opns; Enwonmental Lab 

Cleston Lange, 3M EHS&Opns; Environmental Lab 

Jai Kesari, Weston Solutions 

Date: June 15,2011 

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

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

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

Incorporation Area (FSIA) Groundwater - June 2011 Sampling 

1 General Project Information 

Contacts 

1 Lab Request Number 

1 Six Digit Department Number 

1 Project Scheduien'Mt Dates 

3M Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

aaliohenstein(S)mmm.com 

3M Envirormtentai Laboratory Management 

William K. Reagen 

3M EHS Opns. Environmental l.at}oratofy 

26(WN-17 

651 733-9739 

vi*reaqen(a)mmm.com 

Principal Analytical Investigator 

aeston Lange 

3M EHS Opns, Environmental Laboratory 

26(«N-17 

651 733-9860 

cclanQe(3)mmm.com 

Sampling Coordinator 

Timothy Frinak 

Wisston Solutions 

Timothv.frinak<aiwestonsolutions.com 

Phone: (334)-332-9123 

GLP10-01-02.18 

Dept #530711. Project #0022674449 

Sampling scheduled for the weel< of June 20,2011 

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

Page 4 of 8 

Page 45 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Analytical Protoa>t: GLP10-01-02 

Amendment 18 

2 Background Information and Project Objective(s) 

The 3M EHS Operations Laboratory (3M Environmental Lab) will receive and analyze gn>und\ivater 

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

Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) from the Fomier 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 

15,2011. The 3M Environmental Laboratory will prepare the sample bottles with all required spikes to 

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

will be submitted to Gary Hohenstein and Jai Kesari upon completion under interim report GLP10-01-02-

18. 

3 Project Schedule 

Sample collectbn bottles will be prepared by 3M Environmental Laboratory for sampling the w^ c of June 20, 

2011. Sample bottles will be shipped in coolers ovemight to 3M DK:atur for arrival on Friday, June 17,2011. 

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

Martin Smith \ Weston Trailer 

3M Decatur Plant 

1400 State Docks Road 

Decatur, Alabama 35601 

4 Test Parameters 

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

A total of ttiirty-one sampling kxations have been specified. For each sampling tocation, a sample, sample 

duplicate and a minimum of two fiekj matrix spikes will be collected. Table 1 indicates the well ID and 

corresponding field spike levels. The lill to here° line on each 250 mL Nalgene botOe will be 200 mL. Two sets 

of trip blanks consisting of reagent-grade water, a low-level trip blank spike, mid-l&«l fidd spike, mid-high field 

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

sampling k>cation with tiie other botU^ Two addffionatbotUes will be prepared to be used for the preparation 

of the ^uipment rinseate blanks. A1 -L container of laboratory reagent water will be provkJed for the collectk>n 

of the equipment rinseate blanks. 

Based on the results fixan previously collected samptes from tiie FSIA (GLP10-01-02-O7 and GLP10-01-02-11), 

most sampRng bcations will require dilution with latxuaiDiy reagent water prior to sample aredysis. However, 

sampling kxstions identified in S ^ 1 of Table 1 are expec t to contain PFBS, PFHS, and PFOS 

concentrations <10 ng/mL For samples collected firom tiiese sampling locations, tiie sample, sample duplicate 

and field matrix spikes will contain the addition of internal standard '"Oz-PFBS, "Ca-PFHS, and ^^CVPFOS, at a 

nominal concentration of 1 ng/mL as will the trip blanks samples, trip blank low spik^, and two equipment 

rinseate blanks. The additional of intemal standards will be used to aki m the analysts of the sampiss. A totel of 

169 sample botties will be prepared. 

Page 5 of 8 

Page 46 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

FSIA-June 2011 

AnalyUcal Protocol: GLPIO-01-02 

Amendment 18 

Table 1. Sampling Locations and Field Matrix Spike levels. 

Set# 

1 

2 

3 

4 

5 

Well No. 

134S, 135S. 136R, 137R, 

137S. 137Land138L 

130L. 131S, 131L, 133R, 

135L.136S, 136L,141R, 

142R. 143R and 144R 

130R, 130S, 133S, 133L. 

134L, 138R, 138S, CW26C. 

CW26L and 140R 

131R, 134Rand136R 

Trip Blank Sets 1 and 2 

Sample Level 

Low 

Mkl 

High 

Low 

Mid 

Hiflh 

Low 

Mki 

HkJh 

Low 

High 

l-OW 

Mid 

Mid-Hiqh 

High 

Spike Cone. (ng/mL) 

0.1 

1.0 

10 

1 

10 

100 

10 

100 

500 

100 

2000 

1 

10 

100 

500 

5 Test Metiiods 

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

Compounds In Water by High Perfonnance Liquid Chromatography^ass Spa^bnomeby Direct injection 

Analysis'. The date quality objectives for tiiese studies are quantitetive results for tiie target analytes witti an 

analytical accuracy of 100±30%. RekJ matrix spkes not yieMing recoveries within 100±30% will be addressed 

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

previously collected samples fiom the FSIA (GLP10-01-02-07), most sampling kx:ations will require dilution witti 

laboratory reagent water prior to sample analysis by ETS-8-044.0. 

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

curve. Each curve point will contain isotopically-labeied perfluorocart}Oxyiic ackJs and perftuorosutfonic acids at 

a nominal concenb^ation of 1 ng/mL. The calibration curve will be generated by taking ttie ratio of tt^ stendard 

peak area counts over ttie intemal standard peak area oounte to fit tt« date for each analyte. 

Alternately, samples may be analyzed by ETS 8-154.3 "Detenminatic«i of Perfluorinated Adds, Akxjhols, 

Amktes, and Sulfonates In \A^ter By Solid Phase Extiaction and High F^erfbmiance LK|uk] 

Chromatography/Mass Spectiomety" or ETS-8-110.1 "Mettwd of Analysis for ttie D^armination of 

Perfluorinated Compounds in V\^ter, Soil and Sediment by LC/MS/MS*. 

6 Reporting Requirements 

For each sampling location, ttie report will contain ttie resutts for ttie sample, sample duplicate, and field nnatrix 

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

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

preparation will also be reported and used to e\raluate ttie overall mettKxJ acoiracy and predsion. M^od 

blanks of reagent water prepared at ttie time of sample preparation wiB be used to d^ermine ttie mettiod 

detection limit For those sampling kx^tions wtiere the fieki matrix spice \&im\ was not appropriate, due to 

higher than expects anatyte concentrations, a laboratory matrix spike may be prepared mxi will be included in 

tiie final report. 

Page 6 of 8 

Page 47 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA - June 2011 

Analytic^ Protocol: GLP10-01-02 

Amendment 18 

7 Email Correspondence 

Quarterly GW sampling - Decatur Former Sludge Incorporation Area Wells 

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

Cc: "Frinaic, Timothy R.'", "Smitii, 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 fluorochemical analyses-under GLP 10-01-01 and GLP 10-01-02. It also shows sampling schedule for 

other quarterly sampling (and conventional parameters) 

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

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

rinseate blanks that will be collected. 

Thanks, 

Charlie 

Charies 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 

Page48of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Analytical Protocol: GLPIO-01-02 

Amendment 18 

Quarteriy GW Monitoring 

1 Rrst and Third Quarter IMonitoring Program 

201L 

203L* 

204L 

206L 

209L 

211R 

212R 

212D 

213R 

213S 

215R 

215D 

216R 

217R 

217S 

217D 

218R 

218L 

220R* 

220L* 

221R 

222R* 

223R 

226R 

225L 

226R 

226L 

227R* 

227L* 

228R 

228L 

229R 

229L 

306R 

307L 

308R 

310R* 

311R 

313R 

315R 

317L* 

319L 

324L* 

325L 

328R* 

328L* 

330R* 

330L* 

332S 

335R* 

501 

503 

507 

510R 

51OL 

511S 1 

512R 

512L 

GRS04*^ 

RW312R* 

RW327R* 

RW331S* 

Second and Fourth Quarter Monitoring Program 

201L 

203L 

211R 

212R 

212D 

213R 

213S 

217R 

217S 

217D 

218R 

218L 

222R 

223R 

22gR 

229L 

305R 

307L 

313R 

315R 

324L 

325L 

332S 

335R 

512R 

512L 

130R** 

130S** 

130L** 

131R** 

131S** 

131L** 

133R** 

133S** 

133L** 

134R** 

134S** 

134L** 

135R** 

135S** 

135L** 

136R** 

136S** 

136L** 

137R** 

137S** 

137L** 

138R** 

138S** 

138L** 

C\A/26C** 

CW26L** 

140R** 1 

141R** 

142R** 

143R** 

144R** 

Monitoring wells will be analyzed for VOCs and isopfopyl efth^ using EPA Method 8260 unless othenMise indica ^ 

O Monitoring wells will be analyaal for PFOA and VOCs / isopropyl ether using EPA Melhod 8260. 

( ^ Monitoreig wells will be analyzed for PFOA 

"One sample will be collected from the ctosed landfai (SWVMU4) groundwater «clraclk>n system for VOC and PFOA 

analysis. 

RW indicate recovery wells used in active gromdwater extraction systems. 

Page 8 of 8 

Page 49 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

ATTACHMENT B: REPRESENTATIVE SAMPLE CHROMATOGRAMS AND 

CALIBRATION CURVE(S ) 

Page 50 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Workstation: ETSKIRK Results Name: kll0720a.rdb 

k110720a.rdb (PFBS): "Quadratic" Regression ("1 / x" weighting): y = -4.75e+003 x'*2 + 1.39e+006 x + 3.69e+003 (r = 0.9999) 

10 15 20 25 30 35 40 45 50 55 60 

Concentration, ng/mL 

65 70 75 80 85 90 95 100 

Data worked up by KJU Page 1 of 1 

Printing Time: 2:05:58 PM 

Printing Date: Wednesday, July 27, 2011 

Page 51 Of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Workstation: ETSKIRK Results Name: kll0720a.rdb 

Data worked up by KJU Page 1 of 1 

Printing Time: 2:07:54 PM 

Printing Date: Wednesday, July 27, 2011 

Page 52 Of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Workstation: ETSKIRK Results Name: kll0720a.rdb 

45 50 55 

Concentration, ng/mL 

Data worked up by KJU Page 1 of 1 

Printing Time: 2:07:19 PM 

Printing Date: Wednesday, July 27, 2011 

Page 53 Of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS. PFHS. and PFOS in Water Samples 

FSIA-June 2011 

*ETS-Kirk Results Name: kll0720a.rd b 

I

SomptB Namo: 1(1107208018- Sampto ID: •11003-26*" 

Paak Namt: "PFBS' Masqat): *299.000/80.000 Oa.299.0Dl 

CommeM:-2.5 r>9/mLFCd(J In Mill Q Water- Annotation: " 

Sample Type ; Standar d 

Concentration : 2.5 0 ng/mL 

Calculate d Cone : 2.5 1 ng/mL 

7/20/201 1 

3:17:05 PM 

Modified : 

Proc. Algorl t 

•r.tage 

Base . Sub. 

Peak-Split . Facto r 

Report Largest Peal 

Min. Pflak Height : 

Min. Peak Mldth : 

Smoothing Width : 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

3503854 COL 

6.38et00 5 

13. 0 

13.S 

5.2a5 

5.0eS 

4.8«S 

4,6«5 

4.4a5 

4.2e5 

4.0«5 

3 * « 

3.Se5 

3.4«S 

3.2*5 

3,0«5-

2.8*5 • 

2.6a5 

2.4«5 

2.2a5 

2.005 

1.8*5 

1.6*5-

1.4*5-

1.2*5-

1.0*5-

8.0*4 

6.0*4-

4.0*4-

2.0*4-

0.0-

12.0 125 13fl 13.5 

I

Sampla Nam*: M 10720a028- Sampl* 10: 'Solvent Blanir File: 1(110720a.w<r 

Peal( Name:-PFBS- M«w(ea):-299.000/80JX»Da.299.00(V99.000i3aCommentTX«QV\UerTN11-0238' Anr>otatton:-

Sample Type: 

600 

:<jla 

Acq. Dat e 

Acq. Time 

Modified : 

Proc . Algorithm : 

Noir e Percentag e 

Base . Sub 

Peak-Spl l 

7/20/201 1 

6:4 e 26 PH 

Ko 

Spec 

Window: 

. Fac t 

Report Largest P 

Min. Peak 

Min. Peak 

Smoothing 

RT Window 

Heigh t 

Width : 

Width : 

Expecte d RT: 

Use Rela t 

Int . Type 

Retentio n 

Area : 

Height : 

ve RT: 

Time: 

eak : 

30 

1 

fy Pa 

50 

1.00 

2 

Yes 

0.0 0 

0.0 0 

0 

0 

. : n 

Mo 

Base 

3013 

To Ea 

•^.STe+OO: c 

11.0 

I

SampteName:"V110720a029- SamptelD:-LCS-110714-r 

Paak Name: 'PFBS- Massfee): -299^)00/80.000 Da.299.00a 

Comment: "O.Sppb LCS' Anrxitatlon: " 

Sample Index : 29 

I San ^ Name: 1(1107208037 Samp4etD:-LCS-110714-4- t^le:-k110720a.wtr 

P*al( Name: TFBS- Ms3s(es}: -299.000/80.000 Da,299.000/99.000 Da' 

I CommenfSppb LCS* Anrmtation: " 

ample Index : 32 

Sample Type: 

Concentration : 

Calculate d Cone : 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Nois e Percentag e 

Base . Sub. Windo 

OC 

0.19 8 

0.507 

7/20/201 1 

ng/mL 

ng/mL 

7:07:2 1 PM 

Yes 

Specif y P 

SO 

*: 1.00 

Peak-Split . Factor : 1 

Report Largest Peak: Yes 

Min. Peak Heigh t 

Min. Peak Width : 

Smoothing Width : 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

camet e 

mln 

c p s 

0.0 0 se c 

0 

30. 0 

13. 2 

No 

Manual 

13. 2 

Area : 707520 co 

Height : 

Star t Time: 

.086+005 

13. 0 

a e o 

mii^ 

c p s 

1.05*5 

1.00e5 

9.S0e4' 

9.00e4-

8.S0e4-

8.00*4 

7.50*4 

7.00e4: 

6.50*4: 

e 6.00*4-

I 5.00»4-

4.50*4-

4.00*4: 

3.50*4-

3.00*4-

2.50*4-

2.00*4-

1.50*4^ 

1.00*4-

5000.00^ 

0.00-

Sampla Type 

Concontrati o 

Calculate d i 

Acq. Time: 

Modified : 

Proc . Algor: 

Nois e Perce n 

Base . Sub. h 

Peak-Split . 

Report Large 

Kin . Peak He 

QC 

1.98 

5.1 1 

7/20/201 1 

8:10:1 2 PM 

No 

Specif y Par 

50 

Indow: 1.00 

Fact r : 2 

St Pe4k: Yes 

Igh t 

Kin . Peak Width : 

Smoothing W: 

RT Window: 

Expecte d RT 

Use Relativ e 

Int . Type : 

Retentio n Ti 

Area : 

Height : 

dth : 

RT: 

0.0 0 

0.0 0 

30. 0 3 

13. ? m 

No 

Valle y 

13. 2 . 

7021088 coun 

.07e+006 c 

nq/mL 

ng/mL 

rain 

c p s 

po 

I n 

p s 

1J)5e6 

1.00*6 

9.S0eS9.00*5 

850* 5 

8.00*5-

750*5 

7.00*5 

650* 5 

6.00*5 

o 5.50*5 

1 5.0OB5 

4.50e5 

4.00e5 

3.S0a5 

3.00a5 

2.50e 

2.00*5 

1.50*5' 

1.00*5 

5.00*4 

15^ 1S.5 

Data printe d by STW 

Printin g Time: 12:06:00 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 1 of 29 

Page 54 Of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rd b 

I

Sampl* Name: >110720*035" Sample 10: •LCS-110714-r Fl*: l(11D720a.wiir 

Paak Name: "PFBS" Man(as): *299.00Q/80.000 Da,299.000i/99.000 Da' 

Commert: *30pt3fa LCS* Annotation: -

Sample Index : 35 

Saniple Type: QC 

Concentratlor,! 29.9 

Calculate d Cone: 29.9 

Acq. Date: 7/20/2011 

Acq. Time: 9:13:06 PM 

Modified : Yes 

Proc. Algorithm : Specif y Pa 

Noise Percentage: 50 

Base. Sub. Window: 1.00 

Peak-Split . Factor: 2 

Report Largest Peak: Yes 

Min. Peak Height : 0.00 

Mln. Peak Width: 0.00 

Smoothing Width: 0 

ng/mL 

ng/mL 

a mete 

mln 

cp3 

po 

Retentio n 

Area : 

Height : 

Star t Tim 

End Time: 

T me: 13 

"37344691 

5.63e t 

12 

13 

7 

106 

0 

a 

11.0 12.0 12.5 13.0 

I

Sampt* Nam*: 1(110720*045- Sample iD:-LCS-110714-ir File:lc110720a.w«r 

P*aK Nama: 'PFBS- Masses): -2d9.OOCV60.000 Da.299.000if99.000 Oa" 

Comm*nt: "Sppb LCS ECP Annotation: " 

Sample 

I

Sample Name:l(110720a047 Sample ID:*LC5-110714-1fr File:-k110720a.wtr 

Peak Name:-pFBS- Massfea):-299.000/80JXIODa.299.000/9g.000 DaComment •0.5pf* LCS Ec r Annotalkin; ~ 

Sampl e Index : 12 

Sample Type : QC 

Concentration : 0.0 0 ng/mL 

Calculate d Cone: 0.0037 7 ng/mL 

Acq. Date : 7/20/201 1 

Acq. Time : 11:39:5 3 p« 

Modified : 

Proc . Algorithm : 

Nois e Percentag e 

Base . Sub. Windov. 

Peak-Split . Fact e 

Report Largest Pe 

Mln. Peak Heigh t 

Min. Peak Width : 

Smoothing Width : 

RT Windov: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

Area : 

Height : 

Star t Time: 

End Time: 

No 

Specif y Pa 

50 

: 1.00 

r : 2 

0.0 0 

0.0 0 

0 

30. 0 

13. 2 

No 

Valle y 

13. 2 

8923 cou 

.55e+00 3 

13. 0 

13. 3 n 

11.0 

I

Sample Name:l(110720aO48- Sample ID:-LCS-110714-1S' File:l(110720a.wir 

Peak Name: "PFBS- Ma39<*a): -299.00<VS0.000 Da.299.000/99.000 DaComment "SOppb LCS EC r AwKrtaUon: -

Sample Index : 18 

Sample Type : QC 

Concentration : 0.0 0 ng/mL 

Calculate d Cone : 0.32 3 na/mL 6.5*4-

Acq. Date : 7/21/201 1 

rims: 1:15:1 1 AM 

6.0*4-

s - MQ II I 

5.5*4 

5.0*4-

4.Se4-

4.0e4-

I 3.5*4-

I 

I 3.0e4-

Z5*4-

2.0*4-

1.5*4-

1.0*4-

Samplo Type : QC 

Concentration : 0.0 0 ng mL 

Calculate d Cone : 0.053 9 ng/mL 

Acq. Date : 7/21/201 1 

Acq. Time : 12:42:1 9 AM 

Modified : No 

Proc . Algorithm : Specif y Param 

Moise Percentage : 60 

Base . Sub . Window: 1.00 m 

Peak-Split . Factor : 2 

Report Largest Peak : Yes 

ter s 

n 

Min. Peak Height : 0.0 0 cp s 

Min. Peak Width : 0.0 0 

RT Window: 30. 0 se c 

Expecte d RT: 13. 2 min 

Use Relativ e RT: No 

Retentio n Time: 13. 2 mln 

Height : 1.17e+0O4 cp s 

Star t Time : 13. 0 mln 

End Time : 13. 5 mln 

- MQ II I 

1.10e4-

1.05*4-

9000.C 1-

7500.00-

7000.00-

£:6000.CO: 

1 5500.00: 

~ 5000.00: 

4500.00: 

4000.00: 

3500.00^ 

3000.00^ 

2500.00-: 

2000.00^ 

1500.00-i 

1000.00-^ 

500.00 j 

0.0OJ 

Acq. Tims 

Modified : 

Proc . Algorithm : 

Nois e Pe r 

Base . Sub 

Peak-Spl i 

Report La 

Min. Peak 

Min. Peak 

RT Window 

rentage : 

Window 

. Fact o 

ges t Pe 

Height : 

Width : 

Width : 

Expecte d RT: 

Use Rela t 

int . Type 

Area : 

Height : 

ve RT: 

Time : 

15 

6 

Star t Time: 

End Time: 

:15:1 1 

No 

Specif y 

AM 

Pa 

1.00 

r: 2 

k: Y 

0 

0 

30. 0 

13. 2 

No 

Valle y 

13. 2 

662 

69e-^00 

12. 9 

13. 1 

(10 

flO 

Data printe d by STW 

Printin g Time: 12:06:00 PM 

Printin g Date : Tuesday, September 06, 

Page 2 of 29 

2011 

Page 55 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

*ETS-Kirk Results Name: kll0720a.rd b 

I

Sampi*Name:l(110720a06r Sampla iD:-GLP1(W)1-02-1WXW" File: 1(110720a.w 

Peait Name: -PFBS' Maaa(ea): -299.000/80.000 Da,299.000/99.000 DaCommont:-DALGW130R0110630((iai:100)- AnnotaUon:-

Sample Index: 61 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 

Acq. Date : 

Acq. Time : 

Modified : 

Proc . Algorithm : 

Nois e Percentage : 

Base . Sub. Windo* 

Peak-Split . Fact o 

Report Largest Pe 

Mln. Peak Height : 

Min. Pea t Width : 

Smoothing Width : 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time : 

16. 1 

7/21/201 1 

6:18:0 6 AM 

No 

ng/mL 

Specif y Parameters 

50 

: 1.00 

r : 2 

a k : Yes 

0.0 0 

0.0 0 

0 

30. 0 a 

13. 2 m 

No 

Valle y 

13. 2 m 

Area : 231879 coun 

Height : 2 

Star t Time : 

End Tlmo: 

min 

c p s 

s e c 

poin t 

n 

n 

s 

.52e«004 cp s 

12. 9 m 

13. 5 m 

n 

h 

- MQ II I 

2.0*4 

1.8*4 

1.0*4 

aooo.0 

6000.0 

4000.0 

2000.0 

0.0 

11.0 

•,'"S"i-'|-| ,"1 1 '•( r ^ 

12.0 12.5 13.0 13.5 14.0 14.5 15.0 15.5 

I

SafiH)l*Mame:l(110720a07S- Sample iD:-GLP1tM)1-02-18-016- File:lt110720a,wir 

Pealt Name: -PFBS' M8*s(es): -299.O00A0.000 Da.299.000/99.000 Da' 

Commert:"DALGW130L0110630(cIi|l:10)" AnFiotaBon:" 

Sample Index : 75 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 1.68 ng/mL ^e» ^ 

Acq. Date : 7/21/201 1 3.6*4-

Acq. Time : 11:11:5 2 AM 

3.4*4-

Modified : Yes 

• Sample Name: l(110720a070- Sample ID: 'GLPI041-02-1 frOI V File: -i(110720a.wir 

I Pealt Name: 'PFBS- Ma3a(*s): -299.000/80.000 Da.299.O0CV99.OOO Da-

• Comment-DALGW130SD110630{di)1:10)- AnnoUtlon:-

Sample Index: 70 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 3.&3 ng/mL 

Acq. Pate: 7/21/2011 

Acq. Time: 9:27:02 AM 

Modified : 

Proc . Algorithm : 

Nois e Percentage : 

Base . Sub . Window 

Peak-Split . Fact o 

Report Largest Pe 

Min. Peak Height : 

Min. Peak Width : 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

Yes 

Specif y 

50 

Parame t 

1.00 min 

rt 3 

- k : Y« 

0 

0 

0 

30. 0 

13. 2 

No 

Manual 

13. 2 

Area : 493659 c 

Height : 7 

Star t Time : 

End Tine : 

59et00 ' 

12. 9 

13. 1 

00 cp 

00 s e 

mln 

ounts 

c p s 

mln 

min 

7.5*4 

7.0*4 

6.5*4 

6.0*4 

5.5*4 

5.0*4 

4.5*4 

4.0e4 

3.5*4 

3.0*4 

2.5*4 

Z0»4' 

1.5*4 

1.0*4 

5000.0 

- i 

11.0 11.5 IZO 12.S 13J) 13.5 14.0 14.5 15.0 15.5 

I

Sarr^Nam*:l(110720a08r Sampla ID: *&LP1CM}1.Q2.1M)25' FDa: I d 10720a.wir 

Peak Nam*: *PFBS- Mass{*a): -299.00a'80.000 Da,299.000199.000 Da' 

Convn*nt-DALGW131S0110622(ciai:10)* Annotation:-

Sample Index : 38 

Sample Type: Unknown 

Proc . Algorithm : Specif y 

Nois e Percentage : 50 

Param 

Base . Sub . Window: 1.00 m 

Peak-Split . Factor : 2 

Report Largest Peak: Yes 

Mln. Peak Height : 0 

Mln. Peak Width : 0 

Smoothing Width : 0 

RT Window: 30. 0 

Expecte d RT: 13. 2 

Use Relativ e RT: No 

Int . Type : Manual 

Retentio n Time : 13. 2 

Area : 237023 c 

Height : 3.75e+00. 

Star t Time : 12. 9 

t e r 

n 

00 cp s 

00 se c 

mln 

ounts 

opa 

mln 

p o l 

- MO II I 

ts 

% 

3.2e4 

3.0*4 

Z4* 4 

2.2*4 

2.0*4 

1.8*4 

Calculate d Cone: 0.91 1 na/mL 

Acq. Date : 7/21/201 1 

Acq. Time : 3:14:4 5 PM 

Modified : Yes 

Proc . Algorithm : Specif y Parameters 

Nois e Percentage : 50 

Base . Sub . Window: 1.00 mln 

Peak-Split . Factor : 3 

Report Largest Peak: Yes 

Mln. Peak Height : 0.0 0 cp s 

Mln. Peak Width : 0.0 0 se e 

Smoothing Width : 0 pol n 

RT Window: 30. 0 Sec 

Expecte d RT: 13. 2 mln 

Use Relativ e RT: No 

Int . Type : Base To Bas e 

Retentio n Time: U. 2 mln 

Height : 1.91e+001 cp s 

Star t Time : 12. 9 mln 

- MQ II I 

J 

f 

1.7*4 

1.6e4 

1.5e4 

1.4e4 

1.3*4 

1.2*4^ 

1.2*4 

1.0*4 

8000.0 

6000.0 

4000.0 

2000.0 

9000.0' 

8000.0 

7000.0-

6000.0-

5000.0-

4000.0-

0,0 ViW'^UJ»(M**fiv,>u*'44i^.iiii iWiyw i 

13.07.^1 

iaijUalJ^^HUuLUL«u.Mu 

14.0 14.5 15.0 15.5 

Data printe d by STW 

Printin g Time: 12:06:00 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 3 of 29 

Page 56 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rd b 

I Pealt Nam*: -PFBS" Mas9(es}: '299.000/60.000 Da,299.000/99.000 Da 

Sample Index: 97 

Sample Type: Unknown 

Concentration : N/A 7=- ^ 

Calculate d Cone: 3.10 ng/mL ''^^ ^ 

Acq. Date: 7/21/2011 

Acq. Time: 6:53:17 PM yQ ^ 

Modified : No 

Proc. Algorithm : Specif y Parameters - MQ II I 65*4 

Noise Percentage! 50 

Base. Sub. Window: 1.00 mln 

Peak-Split . Factor: 2 6.0*4 

Report Largest Peak: Yes 

Mln . Peak Height : 0.00 cps 

Min . Peak Width : 0.00 sec 5.5*4 

Smoothing Width: 0 point s 

RT Window: 30.0 sec 

Expected RT: 13.2 min 5.0*4 

Use Relativ e RT: No 

Int . Type: Valle y *-5«4 

Retention Time: 13.2 mln * 

Area: 176229 counts g" . ^ 

Height: 7.fi2e*O01 cps >: '"" " 

Star t Time: 12.9 min S 

End Time: 13.1 mln J 35 ^ 

3.0*4 

2.5*4 

2.0*4 

1.5*4 

1.0*4 

5000.0 

11.0 li. 5 12.0 

• Ssii<pleName:i(110720a111- Sample lD:'GLhMI1-02-1&O40- t^lle 

1 I Peak Nam*: -PFBS- Mass<es}: "299.000^0.000 Da.299.00W99.000 Da" 

• Comm*nt:-0ALGW133S0110630(dil1:10)- Annotation:-

Sample Index: 111 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 9.01 ng/mL ^-^ ^ 

Actj. Date: 7/21/2011 

Actj. Time: 11:17:51 PM 3.6*4 

Modified : No 3,4«4. 

Proc. Algorithm : Specif y Parameters - MO II I 

Noise Percentage: 50 3 3*4 

Base. Sub. Window: 1.00 min 

Peak-Split . Factor: 2 

Report Largest Peak: Yes o.u*^' 

Mln . Peak Height : 0.00 cps 

Mln . peak Width : 0.00 sec 2-6*4-

Smoothing Width : 0 point s 

RT Window: 30.0 see 2.6*4-

Ej;pected RT: 13.2 min 

Use Relativ e RT: No 24*4-

Int . Type: Valle y 

Retention Time: 13.1 min « ^-J*4-

Area: 251016 counts fr 

Height: 3.B8e»001 cps ^ 2.0*4-

Star t Time: 12.9 mln 11 

End Time: 13.3 mln % 1.8*4-

1.6*4-

1.4*4-

1.2e4-

1.0*4-

8000.0-

6000.0-

4000.0-

2000.0-

Tc110720a.wlfr 

11.0 1l'.5 12.0 

13.16 

1 1 

12.5 13. i 0 13.5 14.0 14.5 15.0 15.5 

1 3 1 4 

1 1 • A 

125 13,0 13.5 14.0 14.5 15.0 15.5 

l"sa-;;?;Tl'a-;;;;"-k110720a1iy S«mp>;ii5r^LPiMi--0gltU)45- File:-V110720a.wtr "^ ^ ' ~"" ^ ^ 

I Peak NarDe: "PFBS" Mas»{e«):-299.00080.000 Da.299.000»9.000 Da' 

• Comment-DALGW133R0il0630(dU1:10)- Annotatton:-

Sample Index : 116 

: Sample Type: Unknown ,3, . 

concentration : N/A ^ „ , j |"* 

Calculate d Cone: 4.70 ng/mL i.uuoa-i 

Acq. Date: 7/22/2011 i 

Acq. Time: 1:32:35 AM 9.50*4^ 

Modified : No 9.00*4 

Proc. Algorithm : Specify Parameters - MQ II I 

Nolso Percentage: 50 850*4 

Base. Sub. Window: 1.00 min 

Peak-Split . Factor: 2 8.00*4 

Report Largest Peak: Yes 

Min . Peak Height : 0.00 cps 750*4 

Min . Peak Width : 0.00 sec 

Smoothing Width : 0 point s T/WWJ 

RT Window: 30.0 sec '•"* * 

Ss^RetatW e RT: Ko"' "' " 6.50e4 

Int . Type: Valley 6.00e4 

Retention Time: 13.2 mln « 

Area : 656572 count s g" 5.50*4 

Height: 1.02et005 cps >; 

Start Time: 12.8 min S 5.00*4 

End Time: 13.4 min g 

•E 4.50*4 

4.00*4 

3.50*4 

3.00*4 

ZS0e4 

Z00e4 

• 1.50*4 

1.00e4 

5000.00 

0.00 

1 1 1 1 1 

11.0 li. 5 12.0 li s 13.J 0 13.5 14.0 14.S 15.0 15.5 j 

1 SampteNam*:'V110720a102- Sample ID: •GU'iai1^-1(W35 - File Trt 10>20a.««r 

I Peak Name: -PFBS" MBSs{es): -299.000/BO.OOO Da,299.000/99.000 Da" 

• CorwnBnfDALGW133L0110630(<«1:10)" Annotation:" 

Sample Index : 102 

Sample Type: Unknown ni c 

concentration : N/A ,4^5 , ' V 

Calculate d Cone: €.68 na/mL ' 1 1 

Acq. Date: 7/21/2011 \ 1 

Acq. Time: 8:38:52 PM 1 3e5-^ 1 

Modified : Yes 

Proc. Algorithm : Specify Parameters - MQ II I ^ 

Noise Percentage: 50 '"* ' 

Base. Sub. Window: 1.00 min 

Peak-Split . Factor: 1 

Report Largest Peak: Yes ''" • 

Mln . Peak Height : 0.00 cps 

Mln . Peak Width ; 0.00 sec 

Smoothing Width : 0 point s '•'*= • 

RT Window: 30.0 sec 

Expected RT: 13.2 min 

Use Relativ e RT: No 9-0e4-

Int . Type: Base To Base 

Retention Time: 13.2 min - 8.0*4-

Area: 930117 counts 9 

Height: 1.42e+00S cps >; 

Start Time: 12.9 min I I 7.0e4-

End Time: 13.6 rain | 

6.0*4 

5.0*4 

' 4.0*4-

3.0*4-

2.0e -

1.0e4-

1 1 1 • 

IIJ ) 11.5 IZO 12.5 13. i 0 13.5 14.0 14.5 15.0 15.5 

Data printe d by STW 

Printin g Time: 12:06:01 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 4 of 29 

Page 57 Of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rd b 

r

SamplaName:"k110720a084- Sample ID:-GLP1(>O1-02-1fr421' 

Peak Name: 'PFBS- Mass<ea): -299.000/80.000 Da,299.000/99.000 DaComment: -DAL GW 131R 0 110622 (dB 1:1M)- Annotation:" 

Sampl e Index : . 81 

Sampl e Type : Unknown 

Concentration : N/A 

Calculate d Cone: 53. 9 ng/mL 

Acq. Date : 7/21/201 1 

Acq. Time : 2:20:4 4 PM 

Proc . Alqc 

Nois e Per< 

Base . Sub. 

Peak-spli t 

Report Lai 

Mln. Peak 

Smoothin g Mldtl 

RT Window; 

Use Relativ e Rl 

No 

lecif y Parameters - MO II I 

. Factor : 

12.5 13.0 13.5 

I

San^Name:'V110720a129 - Sample ID: 

Peak Name:-PFBS- Mas9(es):-299.000/80. 

Comment: "DAL GW 134L 0110628 (da 1:10)' 

Sampl e Index : 129 

Sampl e Type : Unknown 

Concentration : N/A 

Calculate d Cone: 11. 4 ng/mL 

Acq. Date : 7/22/201 1 

Acq. Time : 5:05:1 4 AM 

GLPtfrOI -Oa-1 &054" File: 

.000 Da.299.000/99.000 Da' 

Annotatton:" 

I

S«mpleNam*:T<110720a125- Sample ID: "GLP1CM)1-02.1W>50- File: •k110720a.wir 

Peak Name: -PFBS" Ma3s{ea): -299.000^0.000 Da.299.000/99.000 Oa' 

Comment'DALGW134R0110628(dai:100)' Annotathm:-

Sampl e Index : 125 

Sampl e Type : Unknown 

N/A 

Calculate d Cone: 

Acq. Date : 

Acq. Time : 

Modified : 

Proc . Algorithm : 

Nois e Percentag e 

51. 7 ng/mL 

7/22/201 1 

4:41:4 9 AM 

Yes 

Specif y Paramet e 

50 

Base . Sub. Window: 1.00 mln 

Peak-Split . Fact e 

Report Largest Pe 

Min. Peak Heigh t 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

Area : 72 

Height : 

Star t Time: 

End Time : 

r : 3 

a k : Yes 

0.0 0 cp s 

0.0 0 se c 

30. 0 ae c 

13. 2 min 

No 

Manual 

13. 2 mln 

1694 counts 

.lOetOOS cp s 

12. 9 mln 

13. 5 mln 

1.05e5 

1.00e5 

9.50e4 

9.00a4' 

8.50*4 

8.00e4 

7.50*4 

7.00e4: 

6.50*4-

§. 6.00*4' 

^ 5.50*4 

I 5.00*4 

450e4 ' 

4.00*4 

3.50*4 

3.00*4-

2.50*4 

2.00*4 

1.50*4' 

1.00e4 

5000.00-

0.00 

12.0 12.5 13.0 13.5 14.0 14.5 15.0 15.5 

f^ile: i d 1072ba.wir 

.000 Dallfle . No 

Proc , Algorithm : Specif y Parameters -

Nots e Percentage : 50 

Base . Sub. Window: 1.00 mln 

Peak-Split . Factor : 2 

Report Largest Peak: Yes 

ght : 

Min. Peak Width : 

Smoothing Widtl 

RT Window: 

Expecte d RT: 

0.00 

! Relai : RT: No 

Int . Type : Valle y 

Retentio n Time: 13. 1 mln 

Area : 321580 counts 

Height : 5.07e-f004 cp s 

Star t Time: 12. 8 mln 

End Time : 13. 3 mln 

I

SarT4]4eNam*:'V110720a13r Sample ID: *GLP1(K)1-02-1 

Peak Name: -PFBS' Masa(*s): -299.00(V80.000 Da,299.000/99. 

Co[iwnent'OALGW134S011062r Annexation:"' 

Sample Type: 

Concentration : 

Calculate d Cone: 

Acq. Date : 

Acq. Time : 

Modified : 

Proc . Algorithm : 

Nois e Percentag e 

Bas« . Sub. Klndo 

Peak-Split . Fac t 

Unknown 

N/A 

0.25 5 

7/22/201 1 

9:14:2 5 AM 

Yes 

Specif y Pa 

50 

*: 1.00 

r : 4 

Report Largest Peak: Yes 

Mln, Peak Heigh t 

Min, Peak Width : 

Smoothin g Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Retentio n Time: 

0.0 0 

0.0 0 

30. 0 a 

13- 2 B 

No 

Valle y 

13. 2 « 

Area : 358398 cour 

Height : 5.S4e+004 e 

Star t Time : 

End Time : 

12. 9 n 

13. 5 n 

12.5 13.0 13.5 

5.4e4-

5.2e4 

5.0e4 

4.8*4 

4.6*4-

4.4*4-

4.2*4-

4.0*4-

3.8e4-

3.6*4-

3.4*4-

3.2*4-

3.0*4-

' 2.8*4-

Z6e4-

2.4*4-

2.2e4-

2.0*4-

1.8*4-

1.6*4-

1.4*4-

1.2*4-

1.0*4-

S000.0-

6000.0-

4000.0-

2000.0-

0.0-

12.0 12.5 13.0 13.5 14.0 14.5 15.0 15.5 

Data printe d by STW 

Printin g Time: 12:06:01 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 5 of 29 

Page 58 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

*ETS-Kirk Results Name: kll0720a.rd b 

I I I Sampl* Name:-k110720a15r Sample b:-QLP1«>t-02-1&«69- Flle:1c11D720a.Mr 

I P*ak Nam*: -PFBS" Hae»(»«): •299.O0Om0.DO0 Da,299.000^9.000 Da-

• Comment: -DAL GW 13SS 0110628" Annotation: ~ 

Sample Index: 152 

Sample Type: Unknown 

Concentration : N/R 

Calculate d Cone: 1.20 ng/mL ,4* 5 

Acq. Date: 7/22/2011 

Acq. Time: 2:08:07 PM 2.3e5 

Modified : yes 2Je5 

Proc. Algorithm : Specif y Parameters - MO II I 

Noise Percentage: 50 ^•^' ^ 

Base. Sub. Window: 1.00 min 2.QaS 

Peak-Split . Factor: 4 

Report Largest Peak:- Yes 1,9«5 

Min . Peak Height: 0.00 cps 

Min . Peak Width: 0.00 sec I.SeS 

Smoothing Width: 0 point s 

RT Window: 30.0 sec '-'• ' 

Expected RT: 13.2 mln . g^c 

Use Relativ e RT: No 

1.5eS 

Int . Type: Base To Base 

Retentio n Time: 13.1 mln « 1.4*5 

Area: 1666292 counts g" ., , 

Height : 2.50e + 005 cps <. •••*" 

Star t Time: 12.9 mln | ,^ ^ 

End Time: 13.7 mln fe 

£ 1.1*5 

1.0*5 

9.0*4 

8.0*4 

7.0*4 

6.0e4 

5.0e4 

4.0e4 

3.0*4 

2.0*4 

1.0*4 

11.0 11.5 12.0 

I Sampl*N8m«:T(110720a166- Sample ID: •GLP1{M)l-02-1W)79- File:T(110720a.wHr 

I Comment:"DALGW135R0110628(dai:100)* Annotatton:" 

Sample Index : 166 

1 Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 74. 9 ng/mL 1 JaS 

Acq. Date: 7/22/2011 

Acq. Time: 7:01:56 PM 

1.6*5 

Modified : Yes 

Proc. Algorithm : Specif y Parameters - MQ II I .c- c 

Noise Percentage: SO '^ ^ 

Base. Sub. Window: 1.00 min 

Peak-Split . Factor: 3 1.4*5 

Report Largest Peak: Yes 

Kin . Peak Height: 0.00 cps ^ 3tS 

Mln . Peak Width: 0.00 sec 

Smoothing Width: 0 point s 

RT Window: 30.0 sec 1-2«5 

Expected RT: 13.2 mln 

Use Relativ e RT: No 1_,,5 

Int . Type: Base To Base 

Retentio n Time: 13.2 mln t, ••0«5 

Area: 1041957 counts fr 

Height : 1.76et005 cps ^ 9.0*4 

Star t Time: 12.8 min H 

7.0*4 

6.0*4 

5.0e4 

4.0*4 

3.0*4 

Z0*4 

1.0*4 

11.0 11.5 12.0 

1 

1 .14 

1 

1 • 1 1 

125 13.X 0 13.5 14.0 14.S 

T^m*. min 

1318 

I 

12.5 13.0 13.5 14.0 14.5 

Time, mln 

1 1 Sample Name: •k110720a15r Sample ID:-GLP1W)1-02-1WJ74- Fae:-k11O720a.wtr 

1 • Peak Name: -PFBS' Ma3a(**): -299.00a«0i)00 Da.299.00CV99.000 Da15.0 15.5 

15.0 15.5 

• CommcntT)AlGW135L0110628<dl1:10)- Annotatton:" 

Sample Index: 157 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 9.73 ng/mL 

Acq. Date: 7/22/2011 2.2e5 

Acq. Time: 3:53:03 PM 

Modified : No ,( . -

Proc. Algorithm : Specif y Parameters - MQ II I ^"' ^ 

Noise Percentage: 50 . g^c 

Base. Sub. Window: 1.00 min 

Peak-Split . Factor: 2 ig^ g 

Report Largest Peak: Yes 

Min . Peak Height : 0.00 cps u^ S 

Mln . Peak Width : 0.00 sec 

Smoothing Width: 0 point s 1.6e5 

RT Window: 30.0 see 

Expected RT: 13.2 mln 1.5*5 

Use Relativ e RT: No 

1.4*5 

Int . Type: Valle y 

Retention Tlms: 13.2 mln a '•3e5 

Area: 1352313 counts 9 . - -

Height: 2.3OetO05 cps >l '-^ ^ 

Star t Time: 12.9 mln 1 i i «: 

End Time: 13.5 min • '''" ^ 

- 1.0*5 

9.0e4 

8.0*4 

7.0*4 

6.0*4 

S.0e4 

4.0*4 

3.0e4 

2.0*4 

1.0*4 

11.0 11.5 ii o 

1 Sample^3me:-k110720alV Sample ID:-GLP1&O1-02-1M>8r t'ile:-k110720a.wir 

I Peak Name:-PFBS- MaB9(ea):-299.000>f80.000 Da,299.D00i^.OOO Da' 

• Comment'DALGW136S0110630{dai:10)'' Annotation:' 

Sample Index: 179 

Sample Type: Unknown 

Concentration : M/A 

Calculate d Cone: 3.71 na/mL 

Acq. Dale: 7/22/2011 8.0B4 

Acq. Time: 11:35:01 PM 

7.5*4 

Modified : Yea 

Proc. Algorithm : Specif y Parameters - MQ II I 

Noise Percentage: 50 7.0*4 

Base. Sub. Window: 1.00 mln 

Peak-Split . Factor: 2 

Report Largest Peak: Ves ''•'* ^ 

Min . Peak Height : 0,00 cps 

Min . Peak Width: 0,00 sec 6.0e4 

Smoothing Width: 0 point s 

RT Window: 30,0 sec 

Expected RT: 13.2 min 5.5*4 

Use Relativ e RT: No 

5.0*4 

Int . Type: Manual 

Retention Time: 13.2 mln « 

Area: 518916 counts fr 4.5*4 

Height : 8.39e+004 cps >; 

Star t Time: 12.9 mln 1 

End Time: 13.4 mln g *-'* ^ 

3.5*4 

3.0*4 

Z5e4 

2.0e4 

1.5e4 

1.0*4 

5000.0 

11,0 11.5 120 

13.22 1 

f 

12.5 13.0 

Time 

i. 

13.5 14.0 14.5 15.0 15.5 

• mh 

1317 1 

•,., ,-.-,,- A 

12.5 13.0 13.5 14.0 14.5 15.0 15.5 

Data printe d by STW 

Printin g Time: 12:06:01 PM 

Printin g Date: Tuesday, September 06, 2011 

Page 6 of 29 

Page 59 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rd b 

i*:"k110720a170- Sample ID: •GLP1(W)1-02-18O84" Flle:"k110720a.wir 

Peak Name: -PFBS' Maaa<es>: -299.000/80.000 Da,299.000/99,000 DaComm*nt:-DALGW136L0 110630 (dll 1:10)" Annotatton:-

Sample Index: 170 

5,2*4 

5,0*4 

4.8*4 

4.6*4 

4.4*4 

4.2*4 

4.0*4' 

3.8e4 

3.6*4 

3.4*4-

3.2*4-

3.0*4-

2^*4-

2.6*4-

2.4*4-

2.2*4-

1.4*4 

1.2*4 

1.0*4 

8000.0 

6000.0 

4000.0 

2000.0 

Sample Type : 

Concentration : 

Calculate d Cone: 

Acq. Date : 

Acq. Time : 

Modified : 

Proc , Algorithm : 

Nois e Percentag e 

Base . Sub . Windo 

Peak-Split . Fac t 

Unknown 

N/A 

2.3 3 

7/22/201 1 

B:25:5 7 PM 

No 

Specif y Pa 

: 50 

w: 1.00 

o r : 2 

Iseport Largest Peak: Yes 

Min. Peak Heigh t 

Min. Peak Width : 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

: 0.0 0 

0.0 0 

0 

30. 0 

13. 2 n 

No 

Valle y 

13. 2 n 

Area : 327996 cour 

Height : 

Star t Time: 

End Time : 

5.61e+004 c 

12. 9 n 

13. 4 n 

0.0 

11.0 13.0 13.5 

I

Sampl*Nam*:'K110720a19r Sample ID:-GLPlOo4-02-18^ - ^lie:-k11O720a.wir 

Peak Name: -PFBS" MaBs(e3): -299,000^0.000 Da,299.000/99.000 Da" 

Comment:-DAL GW137L 0110624- Annotatton: " 

Sample Index : 193 

Sample Type : 

Sampl* Nam*: 1(110720a184- Sampis ID:-GLP1tHll.02-18-09r Flle:-k110720a.vrir 

P*ak Name: 'PFBS- Ma9S<es): -299.000/80.000 Da.299.000/99.000 DaComment "DAL GW137S0110624- Annotation;-

Sample Index: 184 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 0.108 ng/mL 

Acq. Date: 7/23/2011 

Acq. Tims: 1:20:03 AM 

Modified : 

Proc. Algorithm : 

Noise Percentage 

Base. Sub, Klndou 

Peak-Split . Facto 

Report Largest Pe 

Min . Peak Height 

Mln . Peah Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type: 

Retention Time: 

No 

Specif y Paramete 

50 

: 1,00 min 

r: ? 

0-00 cps 

0.00 sec 

0 po 

30.0 sec 

13.2 mln 

No 

Base To Base 

13.2 mln 

Area: 153922 counts 

Height : 2 .42et0O4 cps 

2.4*4 

Z3*4 

Z2o4 

2.1 e4 

2.0e4 

1.9e4 

1.8e4 

1.7e4 

1.6e4 

1.Se4 

1.4*4 

1 1.3e4 

§• 1.2e4 

1 1.1*4 

1.0*4 

9000.0 

80DO.O 

70O0.0 

6000.0 

5000.0 

4000.0 

3000.0 

2000.0 

1000.0 

0.0 

11.0 

14S2 

WN»^iM''Wll*<*!M>M 

12.5 13.0 135 14.0 14.5 IS.O 15.5 

I

SampleName:*1(110720s196- Sample ID:-GLP1CM)l-02-18-10r Flle:-kll0720a.wir 

Peak Name: -PFBS" Maaa(ea): -299.000re0,000 Da.299.00CV99.000 Da* 

Comm*nt-DALGW138R0110630(d01:10)- Annotation:'*-

Sampl e Index : 19B 

Sampl e Type: 

Calci 

N / A 

nq/mL 2.0*4 

Modified : No 

Proc . Algorithm : Specif y Pa 

Nois e Percentage ; 

Base . Sub . Window: 

Peak-Split . Facto r 

Report Largest Pea 

Hln . Peak Height : 

Mln. Peak Width : 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : B 

Retentio n Time: 

50 

1.00 

2 

: Yes 

0.0 0 

0.0 0 

0 

30. 0 

13. 2 

No 

s e To Ba 

13. 2 

Area : 119551 cou 

Height : 2.03e+004 

Calculate d Cone: 

Acq. DatQ: 

Acq, Tlmfl: 

N / A 

Nolsi Pert itage 

Basi 

Peak-Split . Factor: 4 

Report Largest Peak: 

Mln . Peak Height: ( 

Mln . Peak Width: ( 

Smoothing Width: ( 

RT Window: 30.0 

Specif y Parametei 

50 

•: 1.00 min 

.ela ' ! RT: 

Base To Base 

4 68 9 counts 

Height : 

Star t Time: 

End Time: 

14.0 14.5 15.0 15.5 . 

Data printe d by STW 

Printin g Time: 12:06:01 PM 

Printin g Date : Tuesday, September 06, 

Page 7 of 29 

2011 

Page 60 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Sarriples 

FSIA-June 2011 

*ETS-Kirk Results Name: kll0720a.rd b 

I

Ssmpl*Nam*:-k110720a207' Sample ID:-GLPiaO1-O2-18-106- Flle:1(110720a.w()r 

Peak Name: 'PFBS- Ma*8<*8}: -299.000/60.000 Da,299.000il99,000 DaComment:-OALGW138L0110630r Annotatton:" 

Sample Index : 207 

Sample Type : Unknown 

Concentration : N/A 

Calculate d Cone: 0.038 5 ng/mL 

Acq. Date : 7/23/201 1 

Acq. Time: 9:22:5 4 AM 

Hod i f 

Proc. 

Noise 

Base. 

^eakRepor 

Mln . 

Min . 

ird : 

A l g 

P e r 

Siih 

Spl l 

: La 

'eak 

'ealr 

Smoothing 

RT Wi 

Expee 

Use R 

Int . 

Reten 

Area: 

Heigh 

Star t 

t e d 

ela t 

Type 

I o n 

3rithm 

:entag. 

Windo 

. Fact 

•gest 1 

Heighi 

Width 

Width 

T : 

ve RT 

Time: 

Time: 

End Time: 

No 

Specif y 

: 50 

P a r 

w: 1.00 

o r : 2 

eak: Y. 

: 0 

0 

0 

30.0 

13.2 

No 

Base To 

13.2 

57277 c 

9.49e+00, 

13.1 

13.4 

OU 

(Kl 

m n 

Base 

m 

o u n s 

c p s 

m n 

I

San^Name : 1(1107203221- Sample ID:'GLPiaO1-02^1S-1ir Flle:1(110720a.w(rr 

Peak Name: -PFB r Masa(*s): *299.000/80.000 Da,299.000/99.000 DaComment: "DAL GWCW26C0110622(cia 1:10)* Annotatk>n:~ 

Sample Index : 221 

3.2*4-

3,0*4-

25*4 

2.0*4 

1A*4-

1.6*4' 

14.0 14.5 15.0 15.5 

I

Sampl* Name:-k11D720a2ir Sample lD:-GLP1W)l.02-18-1ir Fl»e:-k110720a.wir 

Peak Name: -PFBS- Mass<es): -299.000/80.000 Da,299.000/99.000 DaComment "DALGW 138S0 110630(da 1:10)- Annotatlon:'-

Sample Index : 212 

Sample Type ; Unknown 

Noll :age 50 

Base . Sub. window r: 1.00 

Peak-Split . Factor : 4 

Report Largest Peak: Yes 

Min. Peak Height : 0.0 0 

Min. Peak Width : 0.0 0 

Smoothing Width : 0 

RT Window: 30, 0 sf 

i Reli 

Rctent l 

Height : 

• RT: 

Base To Base 

•: 13. 2 min 

$35583 counts 

9,44e+004 cp s 

12, 9 min 

13, 5 min 

9,0e4-

8.5*4-

8.0e4' 

7.5*4-

7.0*4-

6.5*4-

6.0*4-

5.5*4-

5.0e4-

4.5*4-

4.0e4-

3.Se4: 

3.0e4 

2.Se4 

2.0e4 

1.5*4; 

1.0*4-

5000.0-

0.0-

12.5 13.0 13.5 14.0 14.5 15.0 15.5 

I

Sample Name: 1(110720a226: Sample 1D:*GLP1U)1-02-18-123 - File: 

Peak Nam*: 'PFBS- MB>a(es): -299.000/80XWO Da39.00a^.00 0 DaComment-DAL eWCW26L0110622(dU 1:10)" Annotatton:-

Samp 

Cone 

.e Type 

entrati c 

Un 

Calculate d Cone: 

Acq. 

Acq. 

Modi 

Pro c 

Nois 

Base 

Peak 

Repo 

Min. 

Min. 

Date : 

Time: 

fled : 

Algor 

e Percei 

7 / 

2 : 

thm: Sp 

Sub. Window: 

-Split . 

r t Large 

Peak He 

Factor : 

St Peak 

ight : 

Peak width : 

Smoothing width : 

RT K 

E^ipe 

Use 

Int . 

Ret e 

Are a 

ndow: 

=ted RT 

Relativ e 

Type : 

itlo n T 

Height : 

Sta r Time: 

RT: 

M 

2333 

3 . 3 

kno wn 

N/A 

2 3 / 

l b : 

Y26 

2011 

52 PM 

s 

eclf y Fa 

3 0 . 

1: 

1 

1 

l e t 

y^ 

50 

1.00 

Yes 

0.0 0 

0.0 0 

0 

D a 

a l 

, 2 1 

)04 C 

, 9 n 

ample Type : 

8000.0 

6000.0 

4000.0 

2000.0-

N/A 

12.0 12.5 13.0 13.5 

Calculate d Cone 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algori 

Nois e Peccen 

Base . Sub. K 

Peak-Split . 

Report Large 

Mln. Peak He 

hm 

13. 4 

7/23/201 1 

4:01:3 9 PM 

Yes 

Specif y Pa 

age : 50 

ndow: 1.00 

•ac 

t Peak : Yes 

(Th 

Kin , Peak Width 

Smoothing wl 

RT Window: 

Expecte d RT: 

Use Relativ e 

Int . Type : 

Retentio n Tl 

Area : 

Height : 

Star t Time: 

RT 

: 0.0 0 

0.0 0 

0 

30, 0 3 

13, 2 n 

No 

Valle y 

13. 1 p 

37 6650 eoun 

5,28e+004 c 

12, 9 n 

^J..)!..' , fit: , i »,l4«miM i 

14.0 14.5 15.0 15.5 12.5 13.0 13.5 14.0 14.5 15.0 15.5 

Data printe d by STW 

Printin g Time: 12:06:01 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 8 of 29 

Page 61 Of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

*ETS-Kirk Results Name: kll0720a.rd b 

||Sampl*Name:-K110720a237- Sample ID:-GLP1(M1-02-18-128- FlU:^110720a,wir 

I Peak Name: "PFBS" Maes(*s): "299,000«),000 Da,299.000«9,000 Da" 

• Comment:-DALGW140R0110e22(dm:10)- Annotatton:-

Sample Index: 237 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 1.58 ng/mL 

Acq. Date: 7/23/2011 3,0*4 

Acq. Time: 7:52:16 PM 

Modified : Yes 2.8*4 

Proc. Algorithm : Specif y Parameters - MQ l U 

Noise Percentage: 50 oc. ^ 

Base. Sub. Window: 1,00 min ^'" ^ 

Peak~Spllt, Factor: 2 

Report Largest Peak: Yes 2.4*4 

Min . Peak Height : 0.00 cps 

Min , Peak Width: 0,00 sec 

Smoothing Width: 0 point s 2.2*4 

RT Window: 30,0 sec 

Expected RT: 13,2 mln 

Use Relativ e RT: No 2.0*4 

Int . Type: Manual 

Retention Time: 13.2 mln . '••' ^ 

Area: 222582 counts g" 

Height: 3,16e + 004 cps <. ,- ^ 

Star t Time: " 12.9 min % 

End Time: 13.4 min | 

•£ 1,4*4 

1,2*4 

1,0*4 

8000.0 

6000.0 

4000.0 

2000,0 

j m ^ 

11.0 11.5 12.0 125 

1 SamptefJame:^110720a25r Sample lb:'•GLP1(W1-02-18-140^ l=lle:i(11D720a.**r 

I Peak Nam*: -PFBS- Mas3(e3): -299.000/80.000 Da.299.000/99,000 Da" 

• Commen(:'DALGW142R0110622(dil1:10)- Annotation:"" 

Sample Index : 251 

Sample Type: Unknown 

1 Concentration : N/A 3.4*4 

Calculate d Cone: 1.69 ng/mL 

Acq. Date: 7/24/2011 - - . 

Acq, Time: 12:46:29 AM ^"^' ^ 

Modified : No 3,0*4' 

Proc. Algorithm : Specif y Parameters - MQ II I 

1 Nolae Percentage: 50 

Base. Sub. Window: 1,00 mln ^^*^ ' 

Peak-Split . Factor: 2 

Report Largest Peak: Yes 2.6*4-

Min. Peak Height : 0.00 cps 

Mln. Peak Width : 0.00 sec 

Smoothing Width: 0 point s 2.4*4-

RT Window: 30.0 see 

Expected RT: 13.2 mln 22*4-

Use Relativ e RT: No 

Int . Type: Valle y 2,0*4-

Retentlon Time: 13.2 mln -

Area: 236351 counts § , g^ . 

Height : 3.426^^004 cps ^ 

Star t Time: 12.9 mln B 

End Time: 13.4 mln | 1.6*4-

1,4*4' 

1.2*4' 

1J)e4-

60O0.Oeooo. • 

4000. -

2000. -

11.0 115 12.0 12.5 

1 

13-17 

^ 

13,0 13,5 14,0 145 15.0 155 

13,16 

• A 

13.0 

1 

135 14.0 145 15.0 155 

1 Peak Name: 'PFBS' Mas*{*s): -299,000/80.000 Da,299,000/99.000 Da' 

' • Comment-OALGWUlROIIoeSO" Annotation:-" 

Sample Index: 246 

; Sample Type: Unknown 

1 Concentration : N/A 

Calculate d Cone: 0,0437 ng/mL 9500 

Acq. Date: 7/23/2011 

Acq, Time: 11:01:17 PM gooQ 

Modified : No -- -

Proc. Algorithm : Specif y Parameters - MQ II I "^^ ^ 

Noise Percentage: 50 

Base, sub. Window: 1.00 min 8000 

Peak-Split . Factor: 2 

Report Largest Peak: Yea 7500 

Min . Peak Height: 0.00 cps 

Mln . Peak Width: 0.00 sec 70OO 

Smoothing Width: 0 point s 

RT Window: 30, 0 sec ^COQ 

Expected RT: 13.2 mln 

Use Relativ e RT: No ^ ^ 

Int , Type: Base To Base 

Retention Time: 13,2 min « 5500 

Area: 64395 counts & 

Height: 9.e0e+003 cps ^ 5000 

Star t Time: 13.0 min •» 

End Time: 13.4 min • 450Q 

4000 

3500 

3000 

2500 

2000 

1500 

1000 

SOO 

10,85 

1319 1 

12.96,. 

11.0 11.5 120 12.5 13,0 

1 Sample Name: •K110720a2eo- Sample ID: "GLPI&OI^2-18-145" File:Sdl0720a.wir 

I Peak Nam*: "PFBS" MaBS(ea): •299,000i«).000 Da.299,000«9,000 Da" 

• Comment-DALGW143R0110622{dai:10)- Annotation:-

Sample Index: 260 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 1.64 ng/mL 

Acq. Date: 7/24/2011 3-*^ ' 

Acq, Time: 3:55:39 AM 

3.204 

Modified : Yea 

Proc. Algorithm : Specif y Parameters - MQ II I 

Noise Percentage: 50 ^-°'* ' 

Base. Sub. Window: 1.00 min 

Peak-Split . Factor: 3 Z8*4-

Report Largest Peak: Yes 

Mln . Peak Height: 0.00 cps _„, . 

Min . Peak Width: 0.00 aec ^'^ ^ 

Smoothing Width: 0 point s 

RT Window: 30.0 aec 2.4*4-

Expected RT: 13.2 mln 

Use Relativ e RT: No 2,2*4-

Int , Type: Base To Base 

Retention Time: 13.2 mln « 2.0*4-

Area: 231480 counts g" 

Height : 3,55e*004 Cps >; , n^ . 

Star t Time: 12.9 min % 

End Time: 13-4 mln 0 

c 1.6e4' 

1.4*4-

1,2*4-

1.0*4-

8000,0-

6000.0-

4000.0-

2000.0-

Tim* 

i 

i 

1 13.91 14,59,. 14,8015.07 \ ^ 

^^13. 5 14,0 ^ l4.S lt! o 15.5 

.mln 

131A II 

11.0 115 12,0 12,5 13.0 

•""^ 

135 14.0 145 15.0 15.5 

i^5 —^ ^ = U 

Data printe d by STW 

Printin g Time: 12:06:01 PM 

Printin g Date : Tuesday, September 06, 2011 

Page of 29 

Page 62 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS. PFHS, and PFOS in Water Samples 

FSIA-June 2011 

*ETS-Kirk Results Name: kll0720a.rd b 

I

SampleName:"k110720a265- Sampl* ID: "GLP1(M1.02-18-150" FU*: 

P*ak Nam*: 'PFBS- Man<*9): -299,000/80.000 Da.299.000/99.000 DaComment: "DAL GW144S0 11062S(dll 1:10)- Annotatton:"" 

Sample Index : 265 

Sample Type : Unknown 

Concentration : N/A 

Calculate d Cone : 1.69 ng/mL 

Acq. Date : 7/24/201 1 

Acq. Time: 40:4 3 AM 

Modified : 

Proc 

Nois e 

Base. 

PeakMin . 

Mln . 

Smoot 

RT WJ 

Expec 

Use R 

Int . 

Reten 

Area : 

Heig h 

Star t 

End T 

Y e s 

Algorithm : Specif y Pa 

P e r 

S u b 

Spl l 

: La 

F-eak 

Sflak 

iln q 

Led 

ela t 

Type 

:T i : m 

Ime : 

centaqe : 

Window: 

. Facto r 

rges t Pea 

Height : 

Width : 

Width : 

! T : 

ve RT: 

B 

Time : 

2 3 8 

SO 

1.00 

3 

0.0 0 

0.0 0 

0 

30. 0 

13. 2 

No 

se To Ba 

13. 2 n 

36 cou 

3.78et00 4 

12. 9 

13. 5 B 

3.6*4 

3,4*4 

3,2*4 

3.0*4 

za*4 

Z6*4 

2.4*4 

2.2*4 

2J3a4 

15*4 

1.6*4 

1.4*4 

1.2*4 

1.0*4 

8000.0 

4000.0 

2000.0 

0.0 ..nil ^iHii^.l. ti(W^i4ii.wV*>M,n(*e*^*^rt 

12.5 13.0 135 14.0 145 15.0 155 

I

Sampl* Nam*: •kl10720a145" Sampla ID: •GLP1&O1.02-18O6F Fil*: "kl 10720a.wMr 

P*Bk Nam*: "PFBS" Maaa<*s): "299.000/80.000 D8,299.000i99.000 DaComment Trip Blank Set 1 MS' Annotation:"" 

Sampl e Index : 145 

Sample Type: Unknown 

tlOi N/A 

Calculate d Cone 

Acq. Time : 

Modified : 

Proc . Algorithm 

10. 3 ng/mL 

7/22/201 1 

11:41:1 5 AM 

Yes 

Specif y Parameters 

Nois e Percentage : 50 

Base . Sub. Windc 

Peak-Split . Fac 

Report Largest 

Min. Peak Heigh 

Min . Peak Width 

Smoothing Width 

RT Window: 

Expecte d RT: 

Use Relativ e RT 

Int . Type : 

Retentio n Time: 

w: 1.00 mln 

o r : 2 

eak : ye s 

: 0.0 0 cp s 

0.0 0 se c 

0 poin t 

30. 0 se c 

13. 2 mln 

No 

13. 1 rain 

Area ; 13921158 counts 

Height : 

Star t Time: 

End Time: 

2.15e*00 6 cp s 

13. 0 mln 

13. 6 Bin 

- MQ II I 

1 

1 

2.1 e6 

1.9*8 

1.7*6 

1.5*6 

1.4*6 

1.3e5 

1,2e6 

1.1*6 

1.0*6 

9.0*5 

8.0*5-

7.0*5-

6,0eS 

5,0*5 

4,0*5 

3.0*5 

2,0*5 

1.0eS 

UJQ 13.0 135 14.0 14.5 15.0 155 

I

Sample Name: 1(110720a018- Sample ID:-11003.2fr9- Fle:-kll0720a.wir 

Peak Name: -PFHS* Msss(es): -399.000/99.000 Da,399.000nK).000 DaComment; "25 nflftnL FC rid h MO Q Water" AnnoUtton:-

Sample Index : 18 

Sample Type : 

Concent rati o 

Calculate d Cone 

Acq. Date : 

Acq. Time : 

Modified : 

Proc . Algori 

Nola e Perce r 

Base . Sub. V 

Peak-Split . 

Report Larg e 

Min. Peak He 

Mln. Peak Wi 

Smoothing Wi 

RT Window: 

Expecte d RT: 

Use Relativ e 

Int . Type : 

Retentio n Tl 

Area : 

Height : 

Star t Time: 

End Time: 

.hm 

.nd 

Standar d 

2.5 0 ng/mL 

2.6 2 ng/mL 

7/20/201 1 

3:17:0 5 PM 

No 

Specif y Paramet e 

: 50 

w: 1.00 mln 

"actor : 2 

St 

• q h 

fith 

d t h 

RT 

eak : Yes 

: 0.0 0 cp s 

0,0 0 se c 

0 po 

30. 0 se c 

14, 9 min 

No 

valle y 

14, 8 min 

20105 counts: 

6.19e-f005 cp s 

14. 7 mln 

15. 2 mln 

I

Sample Name: 1(110720a6S^ Sample lo;'SolveniBlank- t^ite:'Tc110720a.*lfr 

Peak Name: 'PFHS" Masates): -399.000/99,000 Da.399,000/80,000 DaComment -Mm Q V\Mer TNI 1-0238" Annotatton;"" 

Sanpl e Type: Unki 

Concentration : 

Calculate d Cone : 

Acq. Date : - 7/ : 

Acq, Time ; 6:. 

Modified : 

Proc , Algorithm : Spi 

Base , Sub. Window: 

Peak-Split , Factor : 

Report Largest 

N/A 

Smoothing i 

RT Window: 

Expecte d R^ 

Area : 

Height : 

Star t Time: 

End Time: 

:ak Height : c p s 

165 17.0 

Data printe d by STW 

Printin g Time: 12:06:01 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 10 of 29 

Page 63 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rd b 

• SampleNamB:-k110720a029" Sample ID:'LCS-110714-1" Fle;"k110720a.wir 

I Peak Name: "PFHS" Mas9{ea): "399.000*9.000 Da.399.000«).000 Da" 

I Comment: '05pt>b LCS" Annotation:" 

Sample Index : 29 

Sample Type : QC 

Concentration : 0,49 8 ng/mL 

Calculate d Cone: 0.524 ng/mL 

Acq, Date : 7/20/201 1 

Acq. Time : 7:07:2 1 PM 

Modified : Yes 

Proc . Algorithm : Specif y Parameters - MQ II I 

Base . Sub . Window: 1,00 mln 

Peak-Split , Factor: 2 

Report Largest Peak: Yes 

Mln, Peak Height : 0,0 0 cp s 

Mln, Peak Width : 0.0 0 se c 

Smoothing Width: 0 points 

RT Window: 30, 0 se e 

Expecte d RT: 14. 9 mln 

Use Relativ e RT: No 

Int , Type : Manual 

Retentio n Time: 14, 8 mln 

Area : 94.1775 counts 

Height : 1.24et00 5 cp s 

Star t Time : 14. 7 mln 

1 

1.20e5 

1.15e5 

1.1065 

1.05e5 

9.50e4^ 

8.50e4 

8,00e4 

7.50*4 

7.00*4 

6.50*4 

5.50*4 

5.00*4 

4.50*4 

4,00*4 

3.50*4 

3.00*4' 

2,50*4-

2.00*4 

1.50*4 

1,00*4 

sooaoo 

0.00' 

I

Sampl* Name:'\11D720a03S- Sample 10: *LC&-110714-7- Fl*:'k110720a.wifr 

Peak Name: 'PFHS' Mas9(es>: -399.000/99.000 Da.399.000/80.000 Da' 

Conunent: -30ppb LCS- Annotation:" 

Sample Index : 35 

Sample Type : QC 

Concentration : 29. 9 ng/mL 

Calculate d Cone : 30. 1 nq/mL 

Acq. Date : 7/20/201 1 

I Sample Name: 1(110720a032- SamplelD:TCS-110714-4' Fie: "k110720a,wtfr 

I Peak Name: 

• Comment "Sppb LCS" Annotatton: -

Sample Inde: 

Sample Type 

Concentrati o 

Calculate d i 

Acq, Date : 

Acq, Time: 

Modified : 

Proc . Algor: 

Nois e Perce r 

Base . Sub, 1 

Peak-Split . 

32 

OC 

n: 4.9 8 

one : 5.2 1 

7/20/201 1 

8:10:1 2 P 

Ko 

ng/mL 

ng/mL 

thm: Specif y Parameters 

tage : 50 

indow: 1.00 

Factor : 2 

St Peak: Yes 

Min. Peak Height : 0. 0 

Min. Peak Wl 

Smoothing W: 

RT Window: 

Use Relativ e 

Int , Type : 

Area : -

Height : 

Star t Time: 

End Time : 

dth : 0, 0 

30. 0 

RT: No 

Valle y 

8107342 CO 

].19et00 6 

14. 7 

15. 4 

c p s 

s e c 

n ts 

cp s 

mln 

mln 

- MQ 111 

a 

t 

1.15*6 

I.IOeO1.05*6 

1.00*6 

9.00e5 

7.50*5 

7.0065 

6.00B5 

5.50*5 

5.00*5 

450* 5 

4.00*5 

3506 5 

3.0065 

2.5065 

2.00e5 

1.5065 

I.OOaS 

5.0064 

0.00 

12.5 14.5 15.0 15.5 16.0 16.5 17.0 

I

Sample Name:-V110720a042- Sample ID:'LCS-110714-10" Fl)e:-k110720a.w«r 

Peak Name: "PFHS" Ma«e(ea}: -3g9.00(V99.000 Da,399,000/80.000 DaComment -O.Sppb LCS ECP- Annotation:"" 

Sample Index: 42 

Sample Type: ("C 

Concentration : 0.00 ng/mL 6500-

Calculate d Cone: 0.0245 no/mL 55e6 Acq. Date: 7/20/2011 

Acq. Time : 

Modified : 

Proc . Algorithm : 

Nois e Percentag e 

Base . Sub . Windo 

9:13:0 S PM 

No 

Specif y Pa 

50 

J: 1.00 

Peak-Split . Factor : 2 

Report Largest Peak: Yes 

Min. Peak Heigh t 

Min. Peak Width : 

Smoothing Width : 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

0.0 0 

0.0 0 

0 

30- 0 

14. 9 n 

No 

Valle y 

14. 8 

Area : 41799969 CO 

Height : 5.74e-t006 

Star t Time : 

End Time : 15. 2 It 

Acq. Time 

Modified : 

Proc . Algorith m 

Nois e Per 

Base . Sub 

11:39:5 3 PM 

No 

Spe c 

Window: 

Peak-Split . Faci 

Report La 

Hln . Peak 

Min. Peak 

Smoothing 

RT Window 

gest 1 

Helghi 

Width 

Width 

Expecte d RT: 

Use Rela t 

Int . Type 

Retentio n 

Area : 

Height : 

ve RT 

Tlmft: 

eak : 

30 

1 

tv 

SO 

Parame 

1.00 ml 

7 

Y 

0 

0 

0 

0 

. 9 

No 

Bas e 

54992 

To 

s 

00 c 

00 3 

s e c 

mln 

Base 

mln 

6.49e-f003 cp s 

Data printe d by STW 

Printin g Time: 12:06:01 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 11 of 29 

Page 64 Of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rd b 

|l|5.mpl.Nam*:-K110720a045 - Sampl* ID:-LC5-110714-ir Flle:-k110720a,vrir 

I Peak Nama: "PFHS" Ma3S<*a): •399,000»9.000 D».399.000ra0,000 Da* 

• Comm*nt: "Sppb LCS ECF" Annotatton: " 

Sample Index : 45 

Sample Type : QC ,48 2 

Concentration : 0.0 0 ng/mL 5/4*4 

Calculate d Cone : 0.25 7 ng/mL 

Acq, Date : 7/21/201 1 '-^ M 

Acq. Time : 12:42:4 9 AM 50, 4 

Modified : Yes 4,8*4 

Proc . Algorithm : Specif y Parameters - MQ II I 4- ^ 

Nois e Percentage : 50 '-^" ^ 

Base . Sub . Window: 1,00 mln 4.4*4 

Peak-Split . Factor : 4 

Report Largest Peak: Yes 'tuv t 

Mln. Peak Height : 0.0 0 cp s ' 40 ^ 

Mln. Peak Width : 0.0 0 se e 

Smoothing Width : 0 points 3,8*4 

RT Window: 30. 0 se c ,- . 

Expecte d RT: 14. 9 mln •^•'*** 

Use Relativ e RT: No 3.4M 

Int . Type : Base To Base 3.2*4 

Retentio n Time: 14.B rain « 30 ^ 

Area:- 42391S counts & 

Height : &.47et004 cp s ^ 2.8*4 

Star t Time : 14. 5 min V 

End Time : 15, 2 Bi n S 

•E Z4*4 

25*4 

2.0*4 

1.8*4 

1.6*4 

1.4*4 

1.2*4 

1.0*4 

8000.0 

6000.0 

4000.0 

2000,0 

14.75 

II u n 

1 

. J ' li s 13.0 13 5 14,0 14 5 

1 

15.0 15 5 16.0 16 5 17.0 

1 Time mln 

• Sample Name:-kll07203061" Sample ID:-GLP1W)1-02-18.00e" FUe:1(110720a.w<ir 

1 Peak Nam*: -PFHS" M«ss(e8): -399,000/99.000 Da,399.000/80.000 Da-

• Comment: "DAL GW 130R 0110630 (dll 1:100)- Annotatton:" 

Sample Index : 61 

Sample Type : Unknown 1483 

Concentration : N/A 

Calculate d Cone: 125 . ng/mL ^.665 

Acq. Date : 7/21/201 1 ,56 5 

Acq. Time : 6:18:0 6 AM 

2.465 

Modified : Ves -i-i-i: 

Proc . Algorithm : Specif y Parameters - MQ II I ^.365 

Nois e Percentage : 50 2.2*5 

Base . Sub . Window: 1.00 min 

Peak-Split . Factor : 3 2.1*5 

Report Largest Peak: Yes •>«-•; 

Min. Peak Height : 0.0 0 cp s ^" ^ 

Min. Peak Width : 0.0 0 se c I.905 

Smoothing Width : 0 point s 

RT Window: 30. 0 se c 1565 

Expecte d RT: 14, 9 mln , ,. -

Use Relativ e RT: Wo '''* * 

1.665 

Int . Type : Manual 

Eetentior, Time : 14. 8 min « '-^ ^ 

Area : 1990580 counts g- 14 ^ 

Height : 2.65e-f005 cp s >L 

Star t Time : 14. 6 min 'S 1.3e5 

UndTi.. , ,S. l .i n 1 _^ ^ 

1.165 

1,065 

9,0e4 

8.0e4 

7,0e4 

6,0e4-

5,0*4-

4,0*4 

3.0e4' 

2.064 

1.0*4 

14.69,, 

1 

1 

12.5 13.0 13 5 14.0 14.5 

= _ _ __ _ • -^ 

1 I 15.0 15 5 16.0 16 5 17.0 

|isampt*N»m*:T.110720a048 " Sampfe to:-LCS-110714-16" FBe: "k110720a.v»!r 

I Peak Nam*: 'PFHS" Ma3S<*a}: -399.000/99.000 Da.399.000/80.000 Da-

• Conunent -30ppb LCS ECP Annotatton: "* 

Sample Index : 48 

Sample Type: QC 

Concentration : 0.0 0 ng/mL 3.4*5 

Calculate d Cone : 1.6 3 ng/mL 

Acq. Date : 7/21/201 1 ,-. ^ 

Acq. Time: 1:45:4 1 AM ^^ ^ 

Modified : Yes 3.0*5 

Proc . Algorithm : Specif y Parameters - MQ II I 

Nois e Percentage : 90 

Base . Sub. Window: 1,00 min •^'* ' 

Peak-Split . Factor : 5 

Report Largest Peak: Yes 2,6*5 

Min. Pealc Height : 0.0 0 cp s 

Min. Peak Width : 0.0 0 se e 

Smoothing Width : 0 point s 2.4*5 

RT Window: 30. 0 se c 

Expecte d RT: 14. 9 min 2.2*5 

Use Relativ e RT: No 

Int . Type : Base To Base 2.0*5 

Retentio n Time: 14. 8 mln -

Area : 2590175 counts ^ 1 o-B 

Height : 3-40et00 5 cp s j ^ '^' ^ 

Star t Time: 14. 6 min » 

End Time : 15. 2 mln g ^-^ ^ 

•E 

1.4*5 

1.2*5 

1.0*5 

8.0*4 

6.0*4 

4.0*4 

Z0*4 

1 2 5 13.0 135 

1 SampleName;T(110720a070- Sample lb:-GLHtW)i^- 1 (WI T File:-k110y20a.wtfr 

I Peak Name: -PFHS- Mass(ea): •399.000^9.000 Da,399.O0O«O.0OO Da' 

• Comment-DALGW130S0110630{(ai:10)- Annotatton:" 

Sample Index : 70 

Sample Type : Unknown 

Concentration : N/A 

Calculate d Cone : 29. 8 ng/mL 

Acq. Date : 7/21/201 1 6 0e5-

Acq. Time: 9:27:0 2 AM 

Modified : " Yes =c- l 

Proc . Algorithm : Specif y Parameters - MQ II I '•'"' ' 

Nois e Percentage : 50 

Base . Sub. Window: 1.00 mln 

Peak-Split . Factor : 6 5.065 

Report Largest Peak: Yes 

Mln, Peak Height : 0,0 0 ' cp s 

Min. Peak Width : 0.0 0 se c .=^ 5 

Smoothing Width : 0 point s ^'^ ^ 

RT Window: 30. 0 se e 

Expecte d RT: 14. 9 mln 

Use Relativ e RT: No 4.065 

Int . Type : Base To Base 

Retentio n Time: 14. 8 rain « 3S«S 

Area : 4683837 counts fr 

Height : 6.35e+00 5 cp s >; 

Star t Time: 14. 5 mln f 

End Time : 15. 4 mln | 3-0e5 

2.565 

2.0*5 

1,Se5-

1,0e5-

5,0e4 

1 2 5 13.0 13 5 

14.83 

14.68. • 

km 

• m 

m 14.0 14.5 15.0 15,5 16.0 16.5 17.0 | 

Tlme.min 

1481 

14.67v 1 

i 1 

mm , 

14.0 14.5 15.0 1S.5 16.0 16.5 17.0 | | 

Jl 

Data printe d by STW 

Printin g Time: 12:06:0 1 PM 

Printin g Date: Tuesday, September 06, 

Page 12 of 29 

Page 65 Of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS. PFHS. and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rd b 

I SampleNama:-\110720a075- Sample ID: "GLP1(K}1-02-ia-016- Fae:-k110720a,M)r 

I Peak Name: -pFKS* Mass^es): -399.000/99.000 Da.399.000/80,000 Da-

• Comment:-DAL(3W130L0110630{dai:10)- Annotatton:" 

Sample Index : 75 

Sample Type: Unknown 

Concentration 

Calculated Coi 

Acq, Date: 

Acq, Time: 

N/A 

13, 7 ng/mL 

7/21/201 1 

11:11:5 2 AM 

Spei 

Noise Percentage: 

Base. Sub, Window: 

Peak-Split . Factor: 

Report Largest Peak: 

Min . Peak Height : 

Mln . Peak Width: 

ng Width: 

Lfy Parametei 

50 

1.00 ni n 

RT I 

I RT: 

Use RelaCl> 

Retention "; 

Area: 

Height : 

Star t Time: 

End Time: 

2.8*5 

2.6*5 

2.465 

2,265 

2,065-

15*5 

1,6*5 

1.4*5 

1.2*5 

1.0*5 

8.0*4 

6.0*4 

4.0*4 

14.0 14.5 15.0 15.5 16.0 16.5 17.0 

I

Sample Name:-V110720a097' Sample ID:-GLPllM)1-02-

Peak Nam*: 'PFHS' Ma33(as); -399,000/99,000 Da, 

Comment:-DAL OW131L0110622 (dl 1:10)- Annotation: 

Sample Index : 97 

e Type: Unknown 

itratlon : H/A 

ng/mL 

I

5ampl*Nam*:1(110720a088- Sampl* 10:-GLP1CM11-02-18«25- Rle:-K110720a.wtr 

Peak Nam*: 'PFHS- M83a(*a}: "399,00099,000 Da.399,000/80,000 OaCommont -DAL GW 131S 0110622 (dil 1:10)- Annotatton: -

1.1065 

1.05*5-

1.00e5 

950*4 

9.00e4 

8.5064 

8.00e4< 

7.5064 

7.00e4 

6.5064 

a- 6,00e4 

* 55064-

5 

£ 5J)0e4-

4,S0e4-

4,0064-

3,50e4-

3,0064: 

2.50e4-

2,0064: 

1.S0e4-

1.00e4-

5000.00: 

0.00 

Sample Tyjje: 

Concentration: 

Calculated Cone: 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Noise Percentage 

Base. Sub, Windo 

Peak-Spilt. Fact 

Unknown 

N/A 

5.26 ng/mL 

7/21/2011 

3:44:45 PM 

No 

Specify Paramete 

SO 

rf: 1,00 min 

3r: 2 

Report Largest Peak: Yes 

Mln. Peak Height 

Mln. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

0.00 cps 

0.00 sec 

0 po 

30.0 sec 

14.9 min 

No 

Valley 

14.8 mln 

Area: B49123 counts 

Height: .13et005 cps 

125 13.0 

I

SaiT4)leNam6:'V110720al16r Sampla ID:-GLP1CM)1-02-l&«45- File:-kl 10720a.wir 

Peak Name: -PFHS- M8ss<6s): -399.000/99.000 Da,399.000/80.000 Da' 

CommenfDALGW133R0110630(<ai:10)- Annotation:-

Sample Index: 116 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 32.6 na/mL 

7/22/2011 

Sample Type: 

Concentration: 

Calculated Cone: 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Noise Percentage 

Unknown 

N/A 

21.4 

7/21/2011 

6:53:47 PM 

Yes 

Specify Pa 

SO 

Base. Sub. Window: 1.00 

Peak-Split. Fact ar: 3 

Report Largest Peak: Yes 

Mln. Peak Height 

Mln. Peak Width: 

Smoothing Width: 

0.00 

0.00 

0 

Area: 

Height: 

Start Time: 

End Time: 

3387165 c 

4.69^-^005 

14.5 

15.2 

6.565 

Acq. Timi 1:32:35 AM 

Peak-Split . Factor: 

Report Largest Peal 

Mln . Peak Height: 

Mln . Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

c p s 

Use Rela( : RT: 

14.0 14.5 15.0 15.5 16.0 16.5 17,0 125 13,0 135 14,0 14,5 15,0 15.5 16.0 165 17,0 

Data printe d by STW 

Printin g Time: 12:06:01 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 13 of 29 

Page 66 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rd b 

I

Samp*6Nam6:-k110720»lir Sample ID:"GLPKMI^-IWMO" File:T<110720a.«*fr 

Peak Name: -PFHS* M3S3(6S}: -399,000/99.000 Da.399,000ffl0,000 Da' 

Comnwnt: ^ALGW133S0 110630 (da 1:10)- Annotation: "• 

Sample Index : 111 

Sample Type : Unknown 

Concentration : N/A 25*5 -

Calculate d Cone : 66. 9 ng/mL 

Acq. Date : 7/21/201 1 

Acq. Time : 11:47:5 4 PM Z6e5 -

Modified : 

Proc . Algo r 

Nois e Perc e 

thm: 

tage : 

Base , Sub . Window 

Peak-split , 

Report Larqi 

Min, Peak He 

Min. Peak Wi 

RT Window: 

Expecte d RT 

Int . Type : 

Retentio n T 

Area : 

star t Time : 

End Time : 

Fact o 

ight : 

dth : 

RT. 

Yes 

Specif y P 

50 

1.00 

r : 4 

r 

0.0 0 

0.0 0 

30. 0 

14. 9 

Manual 

14. 8 

2128157 CO 

2 

14. 5 

15. 1 

m 

mete r 

min 

c p s 

s e c 

- MQ 

n 

n t s 

m 

m 

n 

n 

I I I 

1 

% ^ 

2.2*5 

2.0*5 

1 8*5 

1.6*5 

12.5 13.0 14.0 14.5 15.0 15.5 16.0 16,5 17.0 

I

Sample Name:-kl 10720*084' Sample ID:-GLP1041-02-18-O2r File:K11D720a.wirr 

Peak Name: -PFHS" Mas9<6s): -399.000^9.000 Da,399.000ffi0.000 DaComment: "DAL GW131R 0110622 (dlll:100)- Annotatton: ~ 

Satafl e Index : 64 

Sample Type : Unknown 

Concentration : N/A 

Calculate d Cone : 297 . ng/mL 

Acq. Date : 7/21/201 1 

Acq. Time : 2:20:4 4 PM 

I

SampleName:n(110720a102- Sample ID:'GLPl(H>1-02-18-035' File: 

Peak Name: -pFHS" Man<ea): -399.000/99,000 Da,399.000/80.000 Da' 

Comment "DAL GW 133L 0110S30<dl 1:10)' Annotatton: ~ 

Sample Index: 102 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 47.3 ng/mL 

Acq. Pate: 7/21/2011 

Acq. 

Modi 

Pro c 

Nols 

Base 

Peak 

Kepo 

Mln. 

Mln, 

Time 

fled : 

Algorithm : 

e Pe r 

Sub 

-Spl l 

c t La 

Peak 

hln q 

RT Window 

Expecte d 

Use 

Int , 

Ret e 

Are a 

^ela t 

Type 

tio n 

Height : 

Sta t Tim 

ventage -

Window 

, Fact e 

gest Pe 

Height : 

Width: 

Width: 

^T: 

ve RT: 

Time: 

736 

9 

8:38 

Y 

Spec 

r : 

a k : 

30 

1 

N< 

Val 

1 

7649 

,80 e 

14 

52 

g 

tv 

50 

PM 

Pa 

1.00 

3 

Yes 

0 

0 

0 

a 

. 9 

ey 

. 8 

00 

00 

OOS t 

. 5 

145 14.5 15,0 15.5 16J) 165 17,0 

I

'Sampleriame:-kl10720a125' Sample ID:-GLPlO«1-02-1(M»ff- FUe: 

Peak Name: 'PFHS* Mass(es): -399.000,«9,000 Da,399.000/80.000 DaComment "DAL GW134R 0 110628(dll1:100)- Annotatton:" 

Sample Index : 125 

Sample Type : Unknown 

Concentration : N/A 

Calculate d Cone: 484 . na/mL 

Acq. Date : 7/22/201 1 

Acq. Time: 4:41:4 9 AM 

6.065 

Modified : Yes 

Proc , Algorithm : Specif y 

Nois e Percentage : 50 

Peak-Split . Factor : 3 

Report Largest Peak: Ve 

Mln, Peak Height : 0 

Min, Peak Width : 0 

Smoothing Width : 0 

RT Window: 30. 0 

Expecte d RT: 14, 9 

Use Relativ e RT: No 

Int , Type : Manual 

Retentio n Time : 14, 8 

Area : 4668318 C 

Height : 6.27e-t005 

Star t Time: 14. 5 

End Time : 15. 2 

Parameters -

s 

00 cp s 

00 

s e c 

mln 

c p s 

mln 

rain 

Mt' H I 

^ 

1 

45*5 

4.0*5 

3.5*5 

3.0e5 

Modified : 

Proc . Algor] 

Nois e Perce n 

Base . Sub. W 

Peak-Split . 

Report Large 

:hm: 

:aqe 

indo 

Tact 

It P 

Min. Peak Heigh t 

Min. Peak Width : 

Smooching Width: 

RT Window: 

Expecte d RT: 

Use Relativ e 

Int . Type : 

Retentio n Ti 

Area : 

Height : 

Star t Time : 

End Time : 

RT: 

75 

r e s 

Specif y Parame 

50 

*: 1.00 ml 

r : 5 

a k : Yes 

0.0 0 c 

0,0 0 s 

0 

30, 0 se c 

14. 9 min 

No 

Valle y 

14. 8 mln 

5296 counts 

.68(,-f00S cp s 

14. 5 min 

15. 3 min 

14.0 14.5 15.0 15.5 16.0 16.5 17.0 14.0 .14.5 15.0 15.5 16.0 16.5 17.0 

Data printe d by STW 

Printin g Time: 12:06:02 PM 

Printin g Date : Tuesday, September 06, 

Page 14 of 29 

Page 67 Of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

*ETS-Kirk Results Name: kll0720a.rd b 

• Sample Name: 1(110720*129' Sampte ID:-GLP10O1-0M8-054- File: 

I Peak Name:-PFHS- Ma8e(*s): "399,000/99.000 Da,399.000/80,000 Da' 

• Comm*nt:*DAL6W134L0110628(cfil1:10)' AnnoUtion:" 

Sample Index: 129 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 104, ng/mL 

Acq. Date: 7/22/2011 

Acq, Time: 5:05:44 AM 

Modified : 

Proc . Algotithn : 

Nois e Percentag e 

Base . Sub . Windo 

Peak-Split . Fact 

Repcirt Largest P 

Min. Peak Heigh t 

Hln . Peak Width : 

Smoothin g Width : 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time : 

Area : 32 

Height : 

Star t Time : 

End Time : 

Yes 

Specif y Parame t 

: 50 

w: 1.00 mln 

o r : 3 

eak : Yes 

: 0-0 0 cp 

0.0 0 St 

30. 0 se c 

14. 9 mln 

No 

Manual 

14. 8 min 

i8908 counts 

I.21et00 6 cp s 

14. S min 

15. 1 min 

12,S 13,0 14,0 14,5 15.0 15.5 16.0 16.5 17.0 

(

Sample Name: 1c110720a15r Sample ID: 'GLP 1041^02-18'«69- File: "kl 10720a.wirr 

Peak Nam*: 'PFHS- Ma9s(es): -399,000/99.000 Da,399,000/80.000 Da' 

Comment "DAL GW135S0 110628' Annotaflon: " 

Sample Index : 152 

Sample Type: Unknown 

Concentration : N/A 

ng/mL 

I SampleNam*:1i110720al38- Sample ID:•GLP1W)1-02-l&4558r Flle:"kl10720a.wir I

- . 

Paak Nam*: -pFHS- ktaestes): -399.000/99.000 Da,399.000/80.000 DaCon¥nent"DALGW134S0110628- Annotation:"" 

Sample Index: 138 

culat 

Typei 

N/A 

Cone: 3.OS i 

Acq. Date: 7/22/2011 

Acq, Time: 9:14:25 AM 

Modified : Yes 

Proc. Algorithm : Specif y Pat; 

Noise Percentage: 50 

Base. Sub. Window: 1.00 

Peak-Split . Factor: 2 

Report Largest Peak: Yes 

Min . Peak Height : 0.00 

Mln , Peak Width: 0.00 

Smoothing Width: 0 

RT Window: 30,0 St 

Expected RT: 

Use ! RT: 

6.23e*005 eps 

0.0 

I

SampteName:-k110720a15r Sample ID:-GLP1tM)1.02-1W)74" File: 

Peak Nam*: 'PFHS" Mass(es): "399.000/99.000 Da,399.000/80.000 Da' 

Comm*nt-DALGW135L0110628(dl 1:10)- Annotatton:TM 

jample Index; 157 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algo r 

Base . Sub. 

Peak-Split . 

Report Larg 

thm: 

'Indo 

7 

7/22 / 

2:0 8 

YSpe c 

Factor : 

St P 

Min. Peak Heigh t 

Mln. Peak Width : 

Smoothing W 

RT Window: 

Expecte d RT 

dth : 

Use Relativ e RT: 

Int . Type : 

Retentio n T 

Area : 

Height : 

Star t Time : 

End Time : 

iak : 

30 

1' 

NC 

Bas e 

1 

1224576-

.57e * 

1 

IE 

97 

20 

u; 

„ 

fv 

so 

PM 

Pa 

1.00 

Yes 

0 

0 

0 

. 9 

To 

00 

. 5 

, 5 

00 

Ba 

Sample Type : 

Calculate d Cone: 

Acq, Date : 

Acq. Time: 

Modified : 

Proc . Algorithm : 

Nois e Percentag e 

Base . Sub. Windo 

Peak-Split . Fac t 

Unknown 

K/A 

71, 9 

7/22/201 1 

3:53:0 3 PM 

Yes 

Specif y Par 

50 

f. 1.00 

t : 6 

Report Largest Peak: Yes 

Mln. Peak Heigh t 

Min. Peak Width : 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type: 

Retentio n Time: 

0,0 0 

0,0 0 

30. 0 3 

14- 9 m 

Mo 

Bas e To Bas 

14. 9 m 

Area : 11080246 cou 

Height : ,77e+00 6 c 

14.0 14.5 15.0 15.5 16.0 16.5 17.0 

Data printe d by STW 

Printin g Time: 12:06:02 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 15 of 29 

Page 68 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rd b 

isampl*Nam*:-1(110720.166- Sampla ID:-GLP1(K)1-02-1IM)79- Flle:-kl10720a.»lfr 

I Peak Name: 'PFHS' Ma93(*«>: '399.000/99.000 Da,399.000^0,000 Da-

• Comm*nt:'DALGW13SR0110628(dll1:100)- AnnoUtkin:-

Sample Index: 166 

Sample Type: Unknown 1484 

Concentration : N/A 

Calculate d Cone: 859. ng/mL 1.8*6 

Acq. Date: 7/22/2011 

Acq. Time: 7:01:56 PM 1.7B6 

Modified : Yes 

Proc. Algorithm : Specif y Parameters - MO II I '-" ^ 

Noise Percentage: 50 

Base. Sub. Window: 1.00 min 1,5*6 

Peak-Split . Factor: 4 

Report Largest Peak: Yes 14*6 

Mln . peak Height : 0.00 cps 

Mln . Peak Width : 0.00 sec 

Smoothing Width: 0 point s '•2* ° 

RT Window: 30.0 see 

Expected RT: 14.9 min 1.2*6 

Use Relativ e RT: No 

1.1*6 

Int . Type: Base To Base 

Retention Time: 14,8 min . 

Area: 13153795 counts & ^' ^ 

Height: l,8Set006 cps ^ 

Star t Time: 14.5 mln | fl.0e5 

End Time: 15.6 min g 

- 6.0.5 

7.0*5 

6.0*5 

5.0*5 

4.0*5 

1 ^'^2.0*^ 5 

1.0*5 

^ 

1 

1 1 

,4.6^ 1 • • ^^•- • 

l i s iT o 135' 14.0 14,5 15.0 15,5 16,0 16.5 17.0 

• Samp»eName:T<110720al70- Sample ID: •GLP10^1-02.1(W)84- Flle:-\110720a.wtr 

I Peak Name: -pFHS" hla«s(ee}: "399.000/99.000 Da,399.000/80.000 Da' 

• Commert:-DALGW136L0110630(dil1:10)- Annotatten:-

Samplo Index: 170 

Sample Type: Unknown 1482 

Concentration : N/A 

Calculate d Cone: 15.9 ng/mL 

Acq. Date: 7/22/2011 •»•*" 

Acq. Time: 8:25:57 PM 

32e5 

Modified : Yes 

Proc. Algorithm : Specif y Parameters - MQ II I - - ^ 

Noise Percentage: SO ^"* ^ 

Base. Sub, Window: 1-00 mln 

Peak-Split , Factor: 4 2.8e5 

Report Largest Peak: Yes 

Hln . Peak Height : 0.00 cps -fleS 

Mln , Peak Mldth : 0,00 sec 

Smoothing Width: 0 point s 

RT Window: 30.0 sec 2.4e5 

Expected RT: 14.9 mln 

Use Relativ e RT: No 2.2e5 

Int . Type: Manual 

Retention Time: 14.8 min - 2.0e5-

Area: 2518549 counts g" 

Height : 3.56e + 005 eps ^ ,_8a5-

Star t Time: 14.5 min Tl 

End Time: 15.3 min « 

1 1.6*5-

1.4*5 

1,2*5 

1,0e5' 

8,0e4-

6,0*4 

4.0*4-

2.0*4-

1 

1 

1 14.67 I 

• II 

l i 5 13,0 135 14.0 14.5B 15. . 0 15,5 16.0 16.5 17.0 

1 S.mpl*Name:K110720al7r Sample lD:'GLP1CK>1-02-1»)8r Fil.:"kl 10720..vrir 

I Peak Name: 'PFHS' Ma«s(*s}: -399,000i«9.000 Da.399,000/80,000 Da' 

• Comment-DALOW13eS0ll0630<dll1:10)- Annotatton:" 

Samrile Index: 179 

Sample•Type: Unknown 

Conoentration : N/A 

Calculate d Cone: 25.9 ng/mL 54*S 

Acq. Date: 7/22/2011 

Acq. Time: 11:35:0 1 PM 5,2e5 

Modified : Yea *°* ^ 

Proc. Algorithm : Specif y Parameters - MQ II I 4.8*5 

Noise Percentage: 50 

Base, Sub, Window: 1,00 min ^-^ ^ 

Peak-Split . Factor: 3 4,4*5 

Report Largest Peak: Ves 

Min . Peak Height: 0.00 cps 4.2*5 

Mln . Peak Width: 0.00 sec 40, 5 

Smoothing Width: 0 point s 

RT Window: 30. 0 sec 3,8*5 

Expected RT: 14.9 mln •»«.«; 

Use Relativ e RT: No ^'^ ^ 

3.4*5 

Int . Type: Valle y 

Retention Time: 14.8 mln - •'•^ ' 

Area: 4077196 counts fr 3.0*5 

Height : 5,60e.005 eps ^ l 

Star t Time: 14.5 mln H ^'^ ^ 

End Time: 15.2 mln | 2,6*5 

2.4*5 

2,2*5 

2.0*5 

1,8*5 

1,0*5 

1.4e5 

1.2e5 

1.0e5 

8,0e4-

6.0*4 

4.0*4 

Z0*4 

• li s 13.0 13.5 

|SampleName:1<110720«184- Sampie ID: "GLt>1CM)1.02-l&W3^ FU*:-kl10720a.wir 

I Peak Nam*: -PFHS- Ma8a(*a): -399.000^9.000 OB.399.000«0.000 Da" 

Sample Index: 184 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 0,0814 na/mL . g^ . 

Acq- Date: 7/23/2011 

Acq. Time: 1:20:03 AM 

Modified : No 

Proc. Algorithm : Specif y Parameters - MQ II I 1-7*4 

Noise Percentage: 50 

Base. Sub. Window: 1.00 mln 1.6*4-

Peak-Split . Factor: 2 

Report Largest Peak: Yes ^ 5^4. 

Min . Peak Height: 0.00 cps 

Mln . Peak Width: 0.00 sec , ^ . 

Smoothing Width: 0 point s ''^ ^ 

RT Window: 30.0 sec 

Expected RT: 14.9 mln '•3»* 

Use Relativ e RT: No 

1.2*4 

Int . Type: Base To Base 

Retention Time: 14.8 mln « 1.1B4-

Area: 145246 counts g" 

Height : 1.96e-t004 cps >L 1 o«4. 

Star t Time: 14.6 min 1 

End Time: 15.0 mln | g^„ -

6000.0 

7000.0 

6000,0-

5000.0 

4000.0-

3000.0 

2000.0-

1000.0-

125 13.0 13.5 

1460 ' 1 

i \ 

j J 14.0 14.5 15.0 15,5 16.0 16,5 17,0 

Tim*, min 1 

1489 II 

L 

1 I 

14.0 14.5 

1 1 , , J 

15.0 15.5 16.0 16.5 17,0 

Data printe d by STW 

Printin g Time: 12:06:02 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 16 of 29 

Page 69 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS. and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rd b 

*Nam*:1<110720a19r Sample ID: •GLP10O1-02-1B-098- Flle:"k110720a.wir 

Peak Name: "PFHS' Mass{e9}: -399.000/99,000 Da,399.000/80.000 DaComment: 'DAL GW 13A 0 110624' Annotatton: ~ 

Sample Index : 193 

Sample Type : 

Concentration : 

Calculate d Cone : 

Acq. Date : 

Acq. Time : 

Modified : 

Proc . Algorithm : 

Nois e Percentag e 

Base . Sub , Windov 

unknown 

N/A 

0.10 6 ng/m 

7/23/201 1 

4:28:5 7 AM 

Yes 

Specif y Parame t 

50 

: 1.00 mln 

Peak-Split . Factor : 4 

Report Largest Peak: Yes 

Min. Peak Heigh t 

Min. Peak Width : 

Smoothing Width : 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time : 

Atea : - 1 

Height : i 

Star t Time : 

End Time: 

0.0 0 cp 

0.0 0 s e 

0 PC 

30. 0 se c 

14. 9 mln 

No 

Base To Base 

14. 8 min 

4872 counts 

.See+004 cp s 

15. 0 min 

2.3*4-

2.2*4 

2.1 e4 

2.0*4 

1,9*4 

1,8*4 

1.7*4 

1.6*4 

1.5*4 

; 1.3*4 

1.2*4 

1.1* 

1J)»4-

9000.0 

6000.0 

7000.0 

6000.0 

5000.0-

4000.0-

3000.0 

2000,0-

1000,0-

0,0 »Hni'*""**»*''?"^^WO 

12.5 13.0 

V^t«wMMi!V^ *f^^Mt4,^W^4J*^ ^ 

13.5 14.0 14.5 15J) 15.5 16.0 16.5 17,0 

I

Sample Name: T<110720s20r Sample ID: -6LP1CM)1-02-18-108" File: 1(110720a.wirr 

Peak Name: -PFHS- Mass(es): -399.000/99.000 Da.399.000/80.000 DaComment:-DALGW 138L 0110630- Annotation:-

Sample Index : 207 

Sample Type: Unknown 

c.„„„.„.,o,.: »,A ^ 

Z4e4 

2.3e4 

M^i II I 2.2*4 

2.1e4 

2.0e4 

1.9e4 

1.8*4 

1.7*4 

1.6*4-

1.5*4-

Molsi 50 

. Kin! 

Peak-Split . Factor: 3 

Report Largest Peak: V* 

Mln. Peak Height: 0. 

Mln . Peak Width: 0, 

Smoothing Width: 0 

RT Window: 30.0 

I RT: 

Relativ e RT: 

14 . 9 

I

SampleNam*:-k110720a19r Sampl* ID:'GLP10«1-O2-18-103- Flle:-k110720a.wtr 

Paak Name: 'PFHS- Masa<*8): -399.000/99.000 Da.399.000/80.000 Da' 

Comm*nt-DALGW138R0110630(dil1:10)" Annotation;-

Sample Index: 188 

Sample Type: Unknown 

7.SeS 

7.0e5 

6.5*5 

6,0eS5,5e5-

5.0e5 

4.5eS4.0eS; 

3.5e5-

3.0e5-

2.5e5-

ZOeS1.SeS1.0eSlal 

Time: 14.8 

Area: 6119555 coi 

Height: 8.01etOO5 

Start Time: 14.5 

End Time: 15.4 

14.0 14.5 15.0 15.5 16.0 16.5 17.0 

I

Sample Name:-Vt10720a2ir Sample ID:'GLPICMJI-02-18-1 

Peak Name: 'PFHS' Mas9{es}: "399.000/99.000 Da,399.0a0/80. 

Commant 'DAL OW138S 0110630 (dO 1:10)- Annotation: -

Sample Index: 212 

Sample Type: Unknown 

Calculate d Cone : 

Acq. Date : 

Acq, Time: 

Modified : 

Proc . Algorithm : 

Nois e Percentag e 

Base . Sub . Windo 

Peak-Split . Fac t 

Report Largest P 

Min. Peak Heigh t 

Min. Peak Width : 

Smoothing Width : 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int , Type : 

Retentio n Time : 

Area : 1 

Height : 

Star t Time: 

End Time: 

0,112 ng 

7/23/201 1 

9:22:5 4 AM 

Y-a 

Specif y Param 

50 

eak : Yes 

0-00 

0,0 0 

0 

30, 0 se c 

14. 9 min 

No 

Manual 

14.3 min 

94 4 65 counts 

2.5£e+004 cp s 

14. 5 min 

15. 0 min 

1.4*4-

1.3*4 

1.2*4 

1.1*4-

1.0*4-

9000.0-

8000.0-

7000.0-

6000.0-

5000,0-

4000.0-

3000.0 

2000.0 

1000.0 

0.0 

•cif y Parameters - MQ II I 

Base. Sub. 

Peak-Split . 

Report La re 

3661875 counts 

4.47e+00 5 cp s 

14. 5 min 

15. 3 min 

irt,ii|ti|i jiMi |.i^ \>^,,iiy'^mi^)^^¥\Hu_JUK^'fMmitt^M^^^ 

13.5 14,0 14.5 15,0 15.5 16.0 16.5 17.0 14.0 14.5 15.0 1 S.5 16.0 16.5 17.0 

Data printe d by STW 

Printin g Time: 12:06:02 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 17 of 29 

Page 70 Of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

*ETS-Kirk Results Name: kll0720a.rdb 

Sampl* Nam*: "kl10720B221' Sampl* ID: •GLP1(H31-02-18-118- FIIe:1(110720a.«*(ir 

P*ak Nam*: "PFHS" MBS9<*S): -399.000/99.000 Da.399.00affl0.000 Da' 

Commant -DAL GW CVU26C 0 110622 (da 1:10)' Annotatton: ** 

Sample Index : 221 

Sample Type : Unknown 

Concentration : K/A 2.8*5-

Calculate d Cone: 68. 3 ng/mL 

Aeg, Date : 7/23/201 1 

Acq, Time : 2:16:5 2 PM 2.6*5 

Modified: Yea 

Proc, Algorithm: Specify Parame 

Noise Percentage: 50 

Base, Sub, Window: 1.00 m: 

Peak-Split. Factor: 3 

Report Largest Peak: Yes 

ter 

n 

Min. Peak Height: 0.00 cps 

Min, Peak Width: 0.00 s 

Smoothing Width: 0 

RT Window: 30.0 see 

Expected RT: 14,9 mln 

Use Relative RT: No 

Int. Type: Manual 

Retention Time: 14,8 mln 

Atea: 2171579 counts 

Height: 2.82e*005 cps 

Start Time: 14.5 mln 

End Time: 15.2 min 

poi 

- MQ III 

ts 

» 

s 

2.2e5 

2J)e5 

1.8*5 

Sanrqil«Nam*:1(110720a237- Sample lD:'Gt.PiaO1-02-18-128- FUe: 

Peak Name: -PFHS- ltfaaa(*s}: *399.000/99.000 Da,399,000/80.000 Da' 

Cwnment: *DAL 6W140R 0110622 (cQ 1:10)- Annotation: ~ 

Sanpl e Index : 237 

Sample Type : Unknown 

Concentration : N/A 

Calculate d Cone: 17. 7 ng/mL 

Acq. Date : 7/23/201 1 

• SampU Name: 1(110720*226- Sampl* ID:'GLP1(K)l-02-18-123- File: 

• Peak Name: 'PFHS* Mass(ea}: '399.000(99.000 Da.399.000/80.000 Da' 

• Comment'DALGWCW26L0110622{tlII1:10)- Awiotatkin: * 

Sample Index : 22G 

Sample Type : Unknown 

Acq, Date: 

Acq. Time: 

Modified: 

Proc. Algori 

Noise Percen 

Base. Sub, W 

Peak-Split. 

Report Large 

Min. Peak He 

Min. Peak Wi 

7/23/2011 

4:01:39 PM 

No 

Specify Param 

50 

ndow: 1.00 m 

•act r: 2 

St Peak: Yes 

ght 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative 

Int. Type: 

Retention Tl 

Area: 

Height: 

Start Time: 

End Time: 

BT: 

0,00 

0,00 

0 

30.0 sec 

14.9 mln 

Mo 

Valley 

14.8 mln 

3287679 counts 

.04e+005 eps 

14.5 mln 

15.2 min 

125 13.0 

I

San^Nanrt*:'k110720a24ff- Sampl* ID:-GLP1MI1-02-1S-135- FUe:-k110720a.w«r 

P*ak Name: -PFHS- Masa(es): -399.OOCV99.000 Da,399.000/80.000 Da' 

Comment'DAL GW141R 0110630- Annotation:-

Sample Index : 246 

Unknown 

N/A 

6.5e4 

6.0e4-

5.5*4-

5.0*4-

4.5*4-

4.0*4-

3.5*4-

3.0*4-

Acq. Tlmi 7:52:1 6 PM 

Modified: Y 

Proc. Algorithm: Spec 

Noise Percentage: 

Base. Sub. Window: 

Peak-Split. Factor: 

Report Largest Peak: 

Min. Peak Height: 

Mln. Peak Width: 

Smoothing Width: 

RT Window: 30 

s 

fy Param 

50 

1.00 m 

4 

Yes 

0,00 

0.00 

0 

0 sec 

Expected RT: 14.9 mln 

Use Relative RT: N 

Int. Type: Base 

Retention Time: 1 

Area: 2800911 

Height: 3.76e 

To Base 

.8 min 

005 cps 

Calculated Cone 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algorithm 

Molse Percentag 

Base. Sub. Klndc 

Peak-Split. Fac 

Report Largest 

0.298 ng/ 

7/23/2011 

11:01:17 

Yes 

Specify 

: SO 

w: 1.1 

eak: Yi 

Mln. Peak Height: 0 

Mln. Peak Width 

Smoothing Width 

RT Window: 

Expected RT: 

Use Relative RT 

Int. Type: 

Retention Time: 

Area: 

Height: 

Start Time: 

End Time: 

0 

0 

30.0 

14.9 

NO 

Manual 

14.8 

87939 c 

6.68e'f004 

14.6 

15.1 

PM 

Parame 

0 ml 

00 c 

DO 3 

min 

mln 

cps 

mln 

mln 

.0 14.5 15.0 15.5 16J) 16.5 17.0 12.5 13.0 16.5 17.0 

Data printed by STW 

Printing Time: 12:06:02 PM 

Printing Date: Tuesday, September 06, 

Page 18 of 29 

Page 71 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS. and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rd b 

• Sampt*Nwn*:T<110720a251' Sample ID: •GLP1(M>1-02-18.140' File: 

• Peak Name:-PFHS- Masa{e»): "399.000/99.000 Da,399.000/80.000 Da' 

• Cominent-DALGW142R0110622(dil1:10)' Annotatk>n:-

Sample Index: 251 

Sample Type: Unknown 

Conetntration: N/A 

Calculated Cone: 10.0 ng/mL 

Acq. Date: 7/24/2011 

Acq. Time: 12:46:29 AM 

Modified: Y 3 

Proc. Algorithm: Specify Pa 

Noise Percentage: 

Base. Sub, Window: 

Peak-Split. Factor: 

Report Largest Peak: 

Mln. Peak Height: 

Mln, Peak Width: 

Smoothing Width: 

RT Window: 30 

50 

1.00 

3 

Yes 

0.00 

0.00 

0 

0 

Atea: 

Height: 

Start Time: 

End Time: 

1599070 count 

2.13et005 cp 

14.5 mi 

15.3 mi 

Data printe d by STW 

Printin g Time: 12:06:02 PM 

Printin g Date : Tuesday, September 06, 

Page 19 of 29 

Page 72 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rd b 

• Sample Nam*:'K110720a018- Sampl* ID:'11003-2ft«- Fl*:-W10720a.v««r 

• Paak Nama:-pFOS- Ma3S<es):-499.000^.000 Da.499.000W>.OOODa,499.000/130.000Da-

• Comment: *2.5 r^fmL FC atd In Mm Q Wat*^ Annotation:" 

Sample Index : 18 

Sample Type : Standar d 

Concentration : 2.5 0 ng/mL 

Calculate d Cone : 2.4 0 ng/mL 

Aeg. Date : 7/20/201 1 

Acq. Time: 3:17:0 5 PM 

Base . Sub . Window. 

Peak-Split . FactoJ 

Report Largest Pe, 

Mln. Peak Height : 

Min. Peak Width : 

Smoothing Width : 

RT Window: 

Expecte d RT: 

• Sampl* Nam*:'V110720a028' Sampl* ID:-SoN*nt BfanlT Flle:-k110720a.nir 

• Peak Name:'PFOS' lrtass{**):'499.000/99.000 Da.499.000/SO.OOODa,499.000/130.000Da-

• Comn*nt'VllQWatarTN11-023 r AnnoUtlon:*" 

Sample Index : 28 

Sample Type : Unknown 

Concentration : N/A 

Calculate d Cone ; 0.019 1 ng/mL 

Acq. Date : 7/20/201 1 

13.5 14.0 1 5 5 16.0 16.5 17.0 17.5 16.0 

I

SamplsName:1(110720a029- Sample IO:''LC^1l0714-r Fl*:-kll0720a. 

Paak Nam*: 'PFOS' Massfes): -499.00099.000 Da.499.000/80.000 Da,499,000/130.000 DaComment: t}.5ppb LCS' Annotation: ~ 

Sample Index : 29 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Noise Percentage 

Base. Sub. Windo 

6:46:26 

No 

Specify 

50 

PM 

param 

•f: 1.00 m 

Peak-Split. Factor: 2 

Report Largest P 

Mln. Peak Height 

Min. Peah Width: 

Smoothing Width: 

BT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

Area: 

Height: 

Start Time: 

End Time: 

ak: Y 

0 

0 

0 

30.0 

15.9 

No 

Valley 

15.8 

1167 c 

.90efO0 

15.7 

15.9 

00 

00 

sec 

min 

min 

cps 

min 

min 

13.5 14.0 1 6 5 17.0 

Sample Name:-kll0720a032' SamplelD:-LCS-110714-4* Fle:-k110720a.vrir 

Peak Name: 'PFOS* M8a3(eB): '499.000/99.000 Da,499,000/80.000 Da,499.000/130.000 Da' 

Comment "Sppb LCS- Annotatton:" 

Sample Index ; 32 

Sample Type : OC 

Concentration : 4.9 8 ng/mL 

Calculate d Cone: 4.9 3 ng/mL 5,ZB5-

Acq. Date : 7/20/201 1 5 0*5-

4.8*5-

s - MQ II I ^-^•5 -

4.4*5-

4.2*5-

4.0*5-

3.8*5-

3.6*5-

3.4*5-

3.2e5-

3.0e5-

H 2.8*5-

I 2.6a5-

I 2.4a5-

2.2e5-

2.0*5-

l.ae5-

1.6e5-

1.4e5-

1.2e5-

1,0*5-

8,0*4-

6.0*4-

4.0e4' 

2.0*4 

Sample Type: 

Concentration: 

Calculated Cone: 

Acq. Date: 

Acq. Tine: 

Modified: 

Proc. Algorithm: 

Noise Percentage 

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: 

QC 

0.498 nq/mL 

0.4 27 ng/mL 

7/20/2011 

7:07:21 PM 

Yes 

Specify Paramete 

50 

J: 1.00 min 

;r: 1 

-ak: Yes 

0.00 eps 

0.00 3«C 

0 po 

30.0 sec 

15.9 mln 

No 

Valley 

15.9 mln 

Area: 30534 3 counts 

Height: 

Start Time; 

End Time: 

.47e+004 cps 

15.7 min 

16.1 mln 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Noise Percentage: 

Base. Sub. Window 

Peak-Split. Facto 

Report Largest Pe 

Mln. Peak Height: 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

8:10:12 PM 

No 

Specify Pa 

: 1.00 

r: 2 

ak: Yes 

0.00 

0.00 

0 

30.0 

15.9 n 

No 

Valley 

15.e r. 

Area: 3510539 cour 

Height: 5 

Start Time: 

End Time: 

31etO05 c 

IS.7 K 

16.4 R 

0.0 

15.0 15.5 16.0 1 6 5 17.0 

Data printe d by STW 

Printin g Time: 12:06:02 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 20 of 29 

Page 73 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rd b 

I

Sample Nam*:-1(110720*035' Sample ID:-LCS-1107l4-r Fle:-k110720a.vritr 

P*ak Nam*: -PFOS" M8ss{*s}: '499.00CV99.000 Da,499.000/80.000 Da.499.000/130.000 Da' 

Comment: "SOppb LCS' Annotation; ~ 

Sample Index : 35 

Sample Type: QC 

Concentration : 2 9.9 ng/mL 

Calculate d Cone: 30.5 ng/mL 

Acq. Date: 7/20/2011 

Acq. Time: 

Modified: 

Proc. Algorithms 

Noise Percentage: 

Base. Sub. Window 

Peak-Split. Facto 

9:13:06 

Yes 

Specify 

50 

PM 

Par 

1.00 

c: 1 

Report Largest Peak: Y( 

Min. Peak Height: 

Mln. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

Area: 204 

Height: 2 

Start Time: 

End Time: 

0 

0 

0 

30.0 

15,9 

Mo 

Manual 

15,8 

3796 

95e*00' 

15,7 

16.4 

OU 

00 

3 

COU 

meters 

min 

c p s 

s e e 

poln 

t s 

m 

m n 

13.5 14.0 15.0 155 16.0 16.5 17.0 17.5 18.0 

Sample Name :-k110720a045- Sample ID:-LCS-110714-ir Flle:-kll0720a.w(rr 

Peak Name: -PFOS* Masa(*>): "499.000/99.000 Da.499.000/80.000 Da,499.00(V130.000 Da' 

Comment: ^p b LCS ECF" Annotation: ~ 

Sample Index : 45 

Sample Type: QC 

Concentration: 4.96 ng/mL 

Calculated Cone: 4.14 ng/mL 

Acq. Date: 7/21/2011 2.8e5 

Acq. Time: 12:42:49 AM 

Modified : Yes 

Ptoc . Algorithm : Specif y Parametei 

Noise Percentage: 50 

Base. Sub. Window: 1.00 min 

Peak-Split . Factor: 4 

Report Largest Peaki 

I

SamplaName:-kl10720a042' Sample ID:'LCS-110714-10- File:-kl10720a.wtr 

Peak Name: -pFOS" Masa<ea}: '499.000/99.000 Da.499.000/80.000 Da.499.000/130.000 Da' 

Comment "O.Sppb LCS ECP Annotatton: ~ 

3.2e4 

3.0e4 

2.6e4 

2.6*4 

2.4*4 

2.2*4 

2.0*4 

1,8*4 

1.6*4 

1.4*4 

1.2*4 

1.0*4' 

8000.0 

6000.0 

4000.0 

2000.0-

..^mtt. i o ^ ,MeiyS.m... 

1S.( 

i .l.^'M.J M|i>i II i<i4ii'^r''T*^*f''*nitifttih>'rlHt* 

15,0 15.5 16.0 165 17.0 175 18.0 

I

San:v<«NanM:-V110720a048- Sample ID:'LCS-110714-16- Flle:1(110720a.wtr 

Peak Name: "PFOS" IAia3(ea): -499.000/99.000 Da.499.000/80.000 Da.499.00a/130.000 Da' 

Comment -30ppb LCS ECP Annotation: ~ 

Sample Index: 46 

Sample Type: QC 

Concentration : 29.S ng/mL 

Calculate d Cone: 29-4 ng/mL 

Acq. Date: 7/21/2011 

Acq. Time: 1:45:41 AM 

, Algoj 

.age: 50 

Height: 

Mln. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

eps 

I Rela • RT: No 

Manual 

le: 15.8 rain 

295504 9 counts 

2.93et005 cpa 

Base. Sub. Window: 

Peak-Split , Factor: 2 

Report Largest Peak: ' 

Min , Peak Height : ( 

Mln . Peak Width : ( 

Smoothing Width: ( 

RT Window; 30.0 

Expected RT: 5 . 9 

! Reli ! RT: 

15,0 15.5 16.0 16.5 17.0 17.5 18.0 15.0 15.5 16.0 16.5 17.0 175 18.0 

Data printe d by STW 

Printin g Time: 12:06:02 PM 

Printin g Date : Tuesday, September 06/ 2011 

Page 21 of 29 

Page 74 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rd b 

I

SampleName:-k110720e061- Sample ID:'GLP1CKI1-02-18-006- Flle:1 

Peak Name: 'PFOS' Ms3a(*a): -499.00af99,000 Da.499.000/80.000 Da.49 

Comment:'DALGW130R0110630((£l1:100)- Annotatton:' 

Sample Index : 61 

Type : Unknown 

2.2*5 

2.1*5 

2.0*5 

MO II I l-9^ -

1.8*5 

1.7*5 

1.6e5 

1.5*5 

1.4*5 

1.3*5 

& 1-2»5 

# 1.1*5 

I 1.0e5-

9.0*4-

8.0*4 

7.0*4-

6.0*4-

5.0*4-

4.0e4-

3.0e4-

2.0*4-

1.0*4-

Sample Type : 

Concentration : 

Calculate d Cone : 

Acq. Date : 

Acq. Time : 

Modified : 

Proc . Algorithm : 

Nois e Percentag e 

Base . Sub . Windo 

Peak-Split . Fac t 

Report Largest P 

Min. Peak Heigh t 

Min. Peak Width : 

Smoothing Width : 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time : 

Area : 31 

Height : 

Star t Time : 

End Time: 

Unknown 

N/A 

440. ng 

7/21/201 1 

e:18:o e AM 

Yes 

Specif y Param 

50 

><: 1.00 m 

3 r: 2 

lak: Yes 

O.OO 

0.0 0 

0 

30-0 se c 

15. 9 mln 

No 

Manual 

15. 7 mln 

0308 counts 

.21et00 5 cp s 

15.4 min 

16. 1 mln 

0.0 

135 14.0 

I

Sample Nam*:-k110720a075- Sample ID:-GLP1(K)1-«2-18-016- Rte:-V11D720a.wtr 

Peak Name: "PFOS' M833(es): '499.000199.000 Da,499.000ffl0.000 Oa,499.00(V130.000 Da" 

Comment:'DALGW130L0110630(dill:10)' Annotation; " 

Sample Index : 75 

SampleNama:'V110720a070' Sample ID:'GLP1fr01-02-18-011- FUe:1 

I

P*ak Nam*; 'PFOS* Mass(e9}: '499.000/99.000 D8,499.000n0.000 Da,4! 

Conm»ent-DALGW130S0110630(dil1:10)' AnnoUtlon:"' 

Sample Index : 70 

5.2*5 

5.0*5-

4.8*5-

4.6e5-

4.4*5-

4.2e5 

4.0e5< 

3,8e5 

3.6*5-

3.4e5-

3.2*5-

3.0*5-

2.Be5-

2.ee5-

2.4*5 

2.2e5 

2.0*5 

1.8*5 

1.6*5 

1.4*5 

1.2*5 

1.0*5-

8.0*4-

6.0*4-

4.0*4 

2.0*4 

0.0 

Acq. Date 

Acq. Time 

Modified : 

Proc . Algorith m 

Nois e Per 

Base . Sub 

Peak-SplI 

Report La 

Min. Peak 

Min. Peak 

RT Window 

Expecte d 

Use Rela t 

Retentio n 

Area : 

Height : 

Star t Tim 

7/21/2 0 

9:27:0 2 

Yes 

Specif y 

centage : 50 

. Fac 

rgest 

Heigh 

Width 

Width 

T : 

ve RT 

Time: 

w: 1. 

o r : 6 

1 

AM 

Parame 

0 ml 

eak : Yes 

: 0 

0 

0 

30. 0 

15. 9 

No 

Base To 

15-7 

7070817 

00 c 

00 3 

rain 

Base 

5.24e+00 5 cp s 

15. 3 mln 

15.0 15.5 16.0 16 5 17.0 17.5 18.0 

I

Samp*eName:T(110720a06y Sample ID: •GLP1(M)l-02-18-025- FUe :-kl10720a .wHT 

Peak Name: -PFOS- Mass(*s): '499.000/99.000 Da,499.000/80.000 Da,499.000/130.000 DaComment-OALGW131SO11O622{d01:1O>" AnnoUtfan:-

ample Index: 88 

Sample Type : Unknown 

Concentration : N/A 

Calculate d Cone : 62. 0 ng/mL 

Acq. Date : 7/21/201 1 

Acq. Time : 11:11:5 2 AM 

Proc . Algorithm : Specif y Parameters - MO II I 

Nois e Percentage : 50 

Base . Sub . Window: 1.00 min 

Peak-Split . Factor : 8 

Report Largest Peak: Yes 

Min. Peak Height : 0.0 0 cp s 

Min. Peak Width : 0.0 0 se c 

Smoothing Width : 0 point s 

RT Window: 30. 0 se c 

Expecte d RT: 15, 9 rain 

Use Relativ e RT: No 

Int . Type : Base To Bas e 

Retentio n Time : 15, 8 mln 

Area : 4402593 counts 

Height : 3.36at00 5 cp s 

End Time: 16.4 mln 

A 

1 

3.2B5 

2.4 ^ 

Z0e 5 

1.8e5 

1.4e5 

4.0*4 

2.0*4 

Concentr a 

Calculat e 

Acq. Dat e 

Acq. Time 

Modified : 

Ion : 

Cone 

Proc , Algorith m 

Moise Pe r 

Base . Sub 

entag e 

Unkr.c wn 

H/A 

5 31 

7/21/2 0 

3:44 45 

Yea 

Spec 

Window: 

Peak-Split , Fac t 

Report La 

Min. Peak 

Min. Peak 

Smoothing 

RT Window 

gest 1 

Helghi 

Width 

Width 

Expecte d RT: 

Use Rela t 

Int . Type 

Retentio n 

Area : 

Height : 

ve RT: 

Time: 

; 

Star t Time: 

End Time: 

o r : 

eak : 

30 

15 

Base 

15 

30336 

fy 

90 

1 

PM 

Par a 

1.00 

3 

0 

0 (' 

0 

. 9 

To 

.h 

3.37et0 0 

15 

16 

.4 

.0 

00 

s e 

mi 

Base 

ml 

cp 

mi 

mi 

15.0 15.5 16.0 16.5 17.0 175 18.0 

I^T' I Vi'nri-'*«***<^***«-JVS**''*V 

15.0 15.5 16.0 16 5 17.0 17.5 18.0 

TTme. mh 

Data printe d by STW 

Printin g Time: 12:06:02 PM 

Printin g Date : Tuesday, September 06, 

Page 22 of 29 

Page 75 Of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rdb 

I

Sampl*Nam*:-k110720a09r Sample ID:-6LP1CM1-02>16<I30- Fik 

Peak Nam*: -PFOS' !*««(•»): •499.000«9.000 Da,499.000/80.000 Da,< 

Comment -DAL GW 131L 0 110622 (dU 1:10)' Annotation:' 

Sample Index: 97 

Pert 

N/A 

;hm: Specif y Pai 

Sub. Window: 1.00 

Peak-Split . Factor: A 

Report Largest Peak: Ves 

Min . Peak Height : 0.00 

Mln . Peak Width : 0.00 

Smoothing Width: 0 

RT Window: 30.0 st 

Expected RT: 15.9 mJ 

Jse Rel ! RT: 

2.14et005 cps 

2.1*5 

2.0e5 

1.9*5 

1.8eS 

1.7e5-

1.6e5' 

1.5e5 

1.4*5 

1.3*5 

1.2*5 

1.1*5 

1.0e5-

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-

15.0 155 16.0 16.5 MO 175 18.0 

I

Sampl*Nam*:-k110720allff' Sampla ID:'GLP 10-01-02-1 

P*ak Nam*: "PFOS" Ma33(fls): "499.000/99.000 Da.499.a 

Comment-DALGW133R011063D(dll1:10)- Annotation: 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 44.1 ng/mL 

Acq. Date: 7/22/2011 

Acq. Time: 1:32:35 AM 

Modified : 

Proc . Algorithm : 

Nois e Percentag e 

Base . Sub. Windo 

Peak-Split . Fac t 

Report Largest P 

Mln. Peak Heigh t 

Mln. Peak Width : 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

Ye s 

Specif y 

50 

Param 

J : 1.00 m 

:.r: 2 

-ak : Yes 

0 

0 

0 

30. 0 

15. 9 

No 

Manual 

15. 7 

Area : 3145634 c 

Height : 2.45et00 5 

Star t Time: 

End Time: 

15. 3 

16. 1 

00 

00 

s e e 

mln 

ounts 

c p s 

mln 

min 

8-045" Fll»:1 

.OOODa.4 

2.4*5 

2.3*5 

2ito5 

Zl* 5 

2.0*5-

1.9*5-

1.8*5-

1.7*5 

1.6*5' 

1.Se5 

1.4*5-

1.3*5-

1.2e5 

l.leS 

1.0e5 

g.0e4 

e.0e4 

7.0e4 

6.0*4' 

5.0*4 

4.0*4 

3.0*4 

2.0*4 

1.0e4-

0.0-

13.5 14.0 15.0 15.5 16.0 165 17,0 17.5 18,0 

[

SampleMame:'V110720a102' Sample ID:-GLP1&O1-02-18-O35- File:-kl10720a.wltr 

Peak Name: "PFOS- hlaa3(*t}: '499.000A9.000 Da,499.000/80.000 Da,499.000/130.000 Da" 

Comment-OALGW133L0110630{dl1:10)- Annotatkin:-

an^le Index: 102 

I

SampleName:'V110720a1ir Sample ID:"GLP1(K)1-02-18-O40- File; 

Peak Name: -PFOS- htasa(**): '499.OOCV99.000 Da,499.000/80.000 Da, 

Comment:-DALGW133S0110630{dai:10}- Amotation:-

Sample Index : 111 

Sampl e Type : Unknown 

Concentration : N/A 

Calculate d Cone: 196. ng/mL 19*5 

Acq. Date: 7/21/2011 

Acq. Time: 11:47:54 PM 

9 - MO II I 1-7*5 

1.6*5 

1.5*5 

I t s '-^ ^ 

1.3*5 

1.2*5 

^ 1.0*5 

I 9.0*4 

8.0*4-

6.0*4 

5.0*4 

4.0*4' 

Modified : 

Ptoe . Alg 

Nois e Pe r 

Base . Sub 

Peak-Epl l 

Report La 

Min . Peak 

Min. Peak 

Smoothing 

RT Window 

Expecte d 

Int . Type 

Retentio n 

Area : 

Height : 

Yes 

jrithm : Specif y Pa 

rentage : 90 

Window: 1.00 

. Factor : A 

rgest Peak: Yes 

Height : 0.0 0 

Width : 0.0 0 

Width : 0 

30. 0 a 

T: 15. 9 n 

ve RT: No 

Bas e To Ba;3 

Time: 15. 6 n 

2B06295 cou 

1.97e+005 c 

Sanpl e Type 

Coneentratl i 

Unknown 

n: N/A 

Calculate d Cone : 137 . n 

Acq. Date : 

Acq. Time : 

Modified : 

Proc . Algor: 

Nois e Percei 

Base . Sub . W 

Peak-Split . 

Report Large 

7/21/201 1 

B:3B:52 PM 

Yes 

thm: Specif y Par a 

tage : 50 

indow: 1.00 

Factor : 5 

St Peak: Yes 

Hln . Peak Height : 0.0 0 

Mln. Peak Width: 0.0 0 

Smoothin g Width : 0 

RT Window: 

Elxpected RT: 

Use Relativ e 

Retentio n Tl 

Area : 

Height : 

Star t Time: 

End Time: 

30. 0 s e 

15. 9 mi 

RT: No 

Bas e To Base 

me: 15. 7 mi 

9686760 coun t 

7.27e+00 5 cp 

15. 3 mi 

16. 4 ml 1 3.5*5 

2.5e5-

ZOeS 

15.0 155 16.0 16.5 17,0 175 18.0 135 14.0 15.0 15.5 16J) 165 17.0 175 18.0 

Data printed by STW 

Printing Time: 12:06:02 PM 

Printing Date: Tuesday, September 06, 

Page 23 of 29 

2011 

Page 76 Of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rd b 

• SamplaName:T<110720a084- Sample ID: •GLP1(M1-02-1ftO21- File;-k110720a.*ytr 

• Peak Nam*: "PFOS' Mass(*B): '499.00099.000 Da,499.000/80.000 Da.499.00a'130.000 Da' 

• Comm*nt:'DALGW131R0110622(dai:100)- Annotatton:"' 

Sample Index: 84 

! Type: Unknown 

Concentr e N/A 

.4B0. 

Base . Sub. Window: 

Peak-Spilt . Factor : 

Report Largest Peak 

Min. Peak Height : 

Kin . Peak Width : 

Smoothing Width : 

RT Window: 

Expecte d RT: 

End Time: 

:lf y Pai 

50 

1.00 

6.0*5 

75*5 

7.0*5 

6.5*5 

6.0*5 

55*5 

5.0*5 

4.5*5 

4.0*5-

3.5*5-

3.0*5-

15.0 15 5 16.0 16.5 17.0 17 5 18.0 

I

SampleNam*:-k110720a129- Sample ID:'GLP1001-02-

Peak Nam*: 'PFOS' Ma3s(*s): "499.000/99.000 Da,499.a 

Comment:'DALGW134L0110626(da 1:10)- Annotatkin 

Sample Index : 129 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 438 . ng/mL 

Acq. Date : 7/22/201 1 

Acq. Time : 6:05:4 4 AH 

Modified : Yes 

Proc . Algorithm: Specif y Parameters - HQ II I 

Base . Sub. Window 

Peak-Split . Facto i 

Report Largest Pei 

Mln. Peak Height : 

Kin . Peak Width : 

Smoothing Width : 

RT Window: 

Expecte d RT: 

•18-054- Fllo:1 

,000/80.000 Da.4l 

I

SaiT^Nam*:-k110720sl25- Sampl* ID:-GLP1M}1-O2-18-0G0- Fa*:' 

Paak Nam*: -pFOS* Masst**): '499.000/99.000 Da.499.000/80.000 Da,4.' 

Connmant 'DAL GW 134R 0110628 (dll 1:100)' Annotation:' 

Sample Type : 

N/A 

Acq, Date : 

Acq. Time : 

Modified : 

Proc . Algorithm : 

Nois e Percentage : 

Base . Sub . Window 

Peak-Split . Fact o 

Report Largest Pe 

Min. Peak Height : 

Min. Peah Width : 

Smoothing Width : 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

7/22/2 0 

4:41:4 9 

Yea 

50 

1 

AM 

Parame 

1.00 ml 

a k : Y 

0 

0 

0 

30. 0 

15. 9 

No 

Manual 

15. 7 

Area : 7011803 

Height : 5 

Star t Time: 

3 

OO c 

00 s 

s e c 

min 

.SBe-tOOS cp s 

15. 3 min 

End Time : 

5.4*5' 

5.2e5-

5,0*5-

4,8*5-

4.6e5-

4.4*5-

4.2*5-

4.0*5-

3.8*5-

3.6*5-

3.4*5-

3.2*5-

3.0*5-

2.8e5-

2.6*5-

2.4*5-

2.2*5-

Z0e5-

1.8*5 

1.6*5-

1,4*5 

1.2*5-

1.0*5-

8.0*4 

6.0*4-

4.0*4-

2.0*4-

0.0 

1 3 5 14.0 15.0 15 5 16.0 16 5 17.0 17 5 16.0 

I

SampteNam*:T(110720a138" Sample ID:'GLPUMI-02-1 &059r FUe: "k110720a.wttr 

Peek Nama: 'PFOS' M8ts(e9): *499J)0Q/99.000 Da,499.000/80.000 Da,499.000/130.000 DaComment "DAL GW134S0 110628r Annotation:-

Sample Index : 138 

1.00 

: RT: No 

Int . Type : Manua l 

Retentio n Time: 15.B 

Area : 6180078 coi 

Height : 4.40e-t00 5 

Star t Time: 15. 3 

End Time: 16. 3 

4.4a5 

4,2*5 

4,0*5 

3.6*5-

3.6*5 

3.4*5 

3.2*5 

3,0*5 

25*5 

2.6*5-

^ 2.4*5-

^ 2.2*5-

I 2.0*5-

15*5-

1.6*5-

1.4*5-

1.2*5-

1.0*5-

8.0*4-

6.0*4-

4.0*4-

Z0*4-

0.0-

Sample Type : Unkno 

N/A 

Calculate d Cone : 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm : 

Nois e Perce n 

Base . Sub. W 

Peak-Split . 

Report Large 

Mln. Peak He 

a g e 

13. 3 

7/22/201 1 

9:14:2 5 AH 

Yes 

Specif y Pa 

50 

ndow: 1.00 

-act c 

g h t 

Mln. Peak Width : 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e 

Int . Type : 

Retentio n Ti 

Area : 

Height : 

Star t Time : 

End Time : 

RT: 

r : 2 

0.0 0 

0.0 0 

0 

30. 0 3 

15. 9 n 

No 

Manual 

15. 7 rt 

9277060 cour 

.77e-t005 c 

15. 3 n 

16. 3 rr 

6.5*5-

6.0*5-

5.5*5-

5.0e5-

4.5e5-

4.0e5-

3,5e5-

3.0e5-

2.5e5-

2.0e5-

1.5e5-

1.0e5-

15.0 15.5 16.0 16.5 17.0 17 5 18.0 14.0 145 15.0 15 5 16.0 16 5 17.0 17 5 18.0 

Data printe d by STW 

Printin g Time: 12:06:02 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 24 of 29 

Page 77 Of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS. PFHS. and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rd b 

Modified : 

Proc . Algori 

Nois e Percentage : 

Base . Sub . Windov 

Peak-Split . Facto i 

Report Largest Pei 

Kin . Peak Height : 

Min. Peak Width: 

Smoothin g Width : 

•3605106 count ! 

2.71e+00 5 ep ! 

15. 3 mir 

16. 3 mlt 

2.6e5 

25*5 

2.4*5 

25*5 

2.2*5 

Z1*5 

2.0*5 

1.9*5-

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-

9.0*4-

8.0*4-

7.0*4-

6.0*4-

5.0*4-

4.0e4-

3.0e4-

Z0e4-

1.0*4-

0.0 

135 14.0 

I

S3mpleN3me:-1(110720a16r Sample ID:-GLP1(K)1-02-18-079- File:'V110720a.wir 

Peak Nam*: -PFOS- Masa(*»): -499.00099.000 Da,499.000/BOJMO Da.499.00(V130.000 DaComment: -DAL GW135R 0 110628 (dU 1:100)' Annotation; " 

Sample Index : 166 

15.0 15 5 16.0 16.5 17.0 17 5 18.0 

TTme. mln 

I

SampleName:"k110720«15r Sample ID:'GLP1W)1^-18-074- File 

Peak Name: "PFOS- Maes{e9): -499.000/99.000 Da.499.000ffi0.000 Da, 

Comment*DALGWl%L0110628(dll:10)' Annotatton:" 

Sample Index : 157 

Sample Type ; Unknown 

N/A 

late d Cone : 55. 5 ng/mL 

7/22/201 1 

3:53:03 PM 

Modified : 

Proc . Algor i 

Nois e Pe r 

Base . Sub w 

Peak-Split . 

Report La 

Min. Peak 

Mln. Peak 

Smoothing 

RT Window 

Expecte d 

Use Rela t 

Area : 

Height : 

Star t Tim 

End Time : 

rge 

Lhm: 

^aet 

St P 

Heigh t 

Width: 

Width: 

T: 

ve 

Tl 

KT: 

Ye 

Spec : 

sak : 

3 0 . 

15 

No 

Ma nu 

15 

3951624 

.26eH 

15 

16 

s 

Ey Pa 

50 

1.00 

4 

Yes 

0.0 0 

0.0 0 

0 

.) 9 

a l 

.6 

cou 

)05 

. 3 

.0 

4.2eS 

4,0e5 

3.8e5 

3.6e5 

3.4*5 

3.2*5-

3.0e5-

Z8*5-

2.6*5-

2.4*5-

2.2e5-

2.0e5-

1.8e5-

1.6e5-

1.4eS1.265-

1.0e5-

8.0e4-

6.0e4-

4,0e4-

Z0e4-

0.0-

15.0 15,5 16.0 16 5 17.0 17 5 18.0 

I

Sample Name: *V110720a1>r Sample ID:-GLP1CM)1-02-lK)a6* Faa:tcll0720a.wttr 

Peak Name: -PFOS" Masa(es}: *499.000/99.000 Da,499.000/80.000 Da,499.000/130.000 Da' 

Comment -DAL GW 136S 0 110630 (dU 1:10)' Annotatkin: " 

Sanpl e Type : 

ion : 

Calculate d Cone : 

Acq. Dat e 

Acq. Time 

Modified : 

Proc . Alg 

Nois e Pe r 

Base . Sub 

rlthm : 

Window 

Unknown 

N/A 

1020 . n 

7/22/201 1 

7:01:5 6 

Yes 

Specif y 

50 

PM 

: 1.00 

Peak-Split . Factor: 7 

Report Largest Pe 

Min. Peak 

Min. Peak 

Smoothing 

RT Window 

Expecte d 

Use Rela t 

Int . Type 

Retentio n 

Area : 

Height : 

Star t Tim 

End Time : 

Heigh t 

Width : 

Width : 

T: 

ve RT: 

Time : 

71i 

( 

ak: Ye 

0 

0 

0 

30. 0 

15. 9 

No 

Base To 

15. 7 

1513 c 

.BOetOOS 

15. 3 

16. 4 

5 

00 

00 

s e 

mi 

Bas e 

mi 

mi 

Calculate d Cone 

Acq. Date : 

Acq. Time : 

Modified : 

Proc . Algorith m 

115 . 

7/22/201 1 

11:35:0 1 

Yes 

Specif y P 

Nois e Percentage : 50 

Base . Sub . Wind 

Peak-Split . Fac 

w: l.OC 

o r : 2 

Report Largest Peak: Yes 

Min. Peak Heigh 

Mln. peak Width 

Smoothing Width 

RT Window: 

Expecte d RT: 

Use Relativ e RT 

Int . Type : 

Retentio n Time: 

ng/mL 

PM 

aramet 6 

mln 

: 0.0 0 cp s 

0.0 0 se c 

30. 0 

15. 9 

No 

Manual 

15. 6 

Area : 8095614 co 

Height : 

Star t Time : 

End Time : 

6.40et-00S 

15. 4 

16. 4 

po 

mln 

c p s 

mln 

mln 

15.0 15 5 16.0 165 17j) 175 18.0 1 3 5 14J1 14 5 15.0 15.5 16J) 16 5 17.0 17 5 18.0 

Data printe d by STW 

Printin g Time: 12:06:03 PM 

Printin g Date: Tuesday, September 06, 2011 

Page 25 of 29 

Page 78 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: Icll0720a.rdb 

I Peah Name: -PFOS- Ma3a(es): -499.000/99.000 Da,499.000/80.000 Da,499.00CV130.000 Da' 

• Comment:'OALGW136L0110630(dill:10)- Annotatkjn:-

Sample Index : 170 

Sample Type : Unknown 1582 

Concentration ; N/A 

Calculate d Cone : 72. 4 ng/mL 42e 5 

Acq. Date : 7/22/201 1 

Acq. Time : 8:25:5 7 PM 4.0e5 

Modified : Yes 3^ 5 

Proc . Algorithm : Specif y Parameters - MQ II I 

Nois e Percentage : SO 3.6«5 

Base . Sub . Window: 1.00 min 

Peak-split . Factor : 4 3.4«j5 

Report Largest Peak: Yes 

Mln. Peak Height : 0.0 0 cp s 3.2eS 

Mln. Peak Width : 0.0 0 se c 

Smoothing Width : 0 points 30e 5 

RT Window: 30. 0 se c 

Expected RT: 15. 9 min 25e 5 

Use Relativ e RT: No 

2.6*5 

Int . Type : Manual 

Retentio n Time : 15. 8 mln - 2.4*5 

Area : 5129333 counts g" 

Height : 4.33 e + 005 cp s >; 2.2e5 

Star t Time : 15.4 mln 5 

End Time: 16. 2 mln » 2.0*5 

1.8*5 

1.6*5 

1.4^ 

1.2*5 

1.0e5 

6.0e4 

6.0e4 

4.0*4 

2.0*4 

15.67.S. 

1 1 

15.51 J 1

1 3 5 14.0 14 5 15.0 15 1 5 

i 

16.0 16 5 17.0 17 5 18.0 

|Sampl*Name:"kll0720a193 - Sample ID:"GLPHWI-02-1 W)98" File:1<110720a.wlfr " 

I Peak Name: "PFOS" Mass(es): -499.00CI«9.000 Da,499.000/80.000 Da,499.00Q/l 30.000 Da" 

• Comment:'DALGWl37L0110624- Annotatfen:"" 

Sample Index : 193 

Sample Type : Unknown , 5 82 

Concentration : K/A -105 ^ 

Calculate d Cone : 1.43 ng/mL 

Acq. Date : 7/23/201 1 1 OOeS 

Acq. Time : 4:23:5 7 AM "^ ^ 

M.di,l.d , V „ »•=< " 

Proc . Algorithm : Specif y Parameters - MQ II I o no-j 

Noise Percentage : 50 *'•'" " 

Base . Sub . Window: 1.00 min awi- j 

Peak-Split . Factor : 2 8.t)0e4 

Report Largest Peak: Yes anA ^ 

Min. Peak Height : 0.0 0 ep s o.wflw 

Min. Peak Width : 0.0 0 se c , en .1 

Smoothing Width : 0 points 7.50*4 

RT Window: 30. 0 se c 

Expecte d RT: 15. 9 mln 7.00*4 

Use Relativ e RT: No 

6.50*4 

Int . Type : Manual 

Retentio n Time : 15. 8 min „ 6.00*4 

Area : 1025031 counts §• 

Height : l.O6e-f0O5 cp s ^ 5.50*4 

Star t Time : 15.4 min f 

End Time : 16. 0 min | 5.00*4 

4.50*4-

400*4-

3.50*4-

3.0064-

250e4-

200*4-

1.50*4 

1.00*4-

5000.00-

15,66-,^ 

1 

1 1 1 J 1 3 5 14.0 145 15.0 15 5 

1 ... . Tm 

\ . , ,,, 

16.0 165 17.0 17 5 16.0 

^^m = ^ ! 

• Sampl6Nam*:'k110720a184- Sampl*ID:'GLP10-01~02-16-093- Flle:'k110720a.wtr 

I Peak Name: "PFOS- Ma*s(es):'499.000/99.000 Da.499.000/80.000 Da.499.000/130.000 Da" 

• Comment-DALGW137S0110624- Annotation:' 

Sample Index : 184 

Sample Type: Unknown 

Conoentration : N/A 

Calculate d Cone : 0.33 0 ng/mL 

Acq. Pate : 7/23/201 1 ^'^ ^ 

Acq. Time: 1:20:0 3 AM j.,^ ^ 

Modified : Yes 21e 4 

Proc . Algorithm : Specif y Parameters - MO ii i 

Moise Percentage : 50 2.0e4 

Base . Sub. Window: 1.00 min 

Peak-Split . Factor : 2 1.9e4 

Report Largest Peak: Yes 

Mln. Peak Height : 0.0 0 cp s ''•°* ^ 

Mln. Peak Width : 0.0 0 se c ,_ . 

Smoothing Width: 0 point s '•' " 

RT Window: 30. 0 se c ,5, 4 

Expecte d RT: 15. 9 min '"'^ ^ 

Use Relativ e RT: No 1.5e4 

Int . Type : Manual 1.4e4 

Retentio n Time: 15.B min -

Area : 235407 counts & 1-3«4 

Height : 2.40et00 4 ep s ^ , _ , 

Star t Time: 15. 4 min 5 ^-^ ^ 

End Time : 16. 1 min | ,,^ 4 

1.0e4 

9000.0 

6000.0 

7000.0 

6000.0 

5000.0 

4000.0 

3000.0 

2000.0 

1000.0 

15.82 

1557.„ 

• 1 1 • • 

iJ^I'^- ' .,4k**W*v^ >k.. 

1 3 5 14.0 14 5 15.0 15 5 16.0 16 5 17.0 17.5 18.0 | 

1 SampteName:-k110>26a198- Sample ID: "GLP1Wl1.02-18-10y File:-kll0720a.wir 

I Peak Name: "PFOS" Mas»(ea):'499.000/99.000 Da,499.000/80.000Da.499.000fl30.000 Da" 

• Comment'DALGW138R0110630{dil1:10)" Annotatton:-

Sample Index : 1S8 

Sample Type : Unknown 

Concentration : N/A 

Calculate d Cone: 348 . na/mL 2.1*6-

Acq. Date : 7/23/201 1 

Acq. Time : 6:13:5 8 AM 2.0*6-

Modified : Yes 1.9*6-

Proc . Algorithm : Specif y Parameters - MQ II I 

Nois e Percentage : 50 1.8*6-

Base . Sub. Window: 1.00 mln 

Peak-Split . Factor : 2 1.7*6 

Mln. Peak Height : 0.0 0 cp s 1,6*6-

Mln. Peak Width : 0.0 0 se c 

Smoothing Width: 0 point s 1,5*6 

RT Window: 30. 0 se e 

Expecte d RT: 15. 9 min 1.4*6 

Use Relativ e RT: No 

1.3*6 

Int . Type : Manual 

Retentio n Time: 15.B min „ 1^ 6 

Area : 23006663 counts g" 

Height : 2.15et00 6 ep s >; 1.1e6 

Star t Time: 15. 3 mln » 

End Time : 16. 6 mln | l.0e6 

9.0e5 

8.0*5 

7.0*5 

6.0e5 

5.0e5 

4.0e5 

3.0e5 

2.0e5-

1.0e5-

Thne mh 

15 81 1 

15.66,. 

1 1 1 • • • • m. 

1 3 5 14.0 14 5 15.0 15 5 16.0 16 5 17.0 17 5 18.0 |1 

Data printed by STW 

Printing Time: 12:06:03 PM 

Printing Date: Tuesday, September 06, 2011 

Page 26 of 29 

Page 79 Of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

•ETS-Kirk Results Name: kll0720a.rd b 

l i Sampl*Nam*:-k110720a207' Sample ID: "GLP(frO1-02-16-10r Fil*:-k110720a.vKtr 

I Paak Nam*: 'PFOS- Maas(es>: -499JXXV99.000 Da,499X00/80.000 Da,499,000/130.000 Da" 

• Comm*nt:-DALGW138L011063a- /Annotatton:-

Sample Index: 207 

Sample Type: Unknown 

Concentration: N/A 

Calculated Cone: 0.339 ng/mL 1.9*4 

Acq. Date: 7/23/2011 

Acq, Time: 9:22:54 AM ,_g^ 

Modified: Yes 

Proc. Algorithm: Specify Parameters - MQ III '•'** 

1 Noise Percentage: 50 

Sase. Sub. Window: 1.00 min 1.6*4 

Peak-Split. Factor: 4 

Report Largest Peak: Yes 1.5*4 

Min. Peak Height: 0.00 cps 

Min. Peak Width: 0.00 sec i4«4 

1 Smoothing Width: 0 points 

RT Window: 30.0 sec ,- . 

Expected RT: 15.9 mln '-* ^ 

Use Relative RT: No 

1.2*4 

Int. Type: Base To Base 

Retention Time: 15.8 min « 1.1*4 

Area: 241597 counts & 

Height: 1.97e + 004 cps >L 10*4 

Start Time: 15.4 mln 1 

End Time: 16.2 mln | ^QQQQ 

8000.0 

7000.0 

6000.0 

5000.0 

4000.0 

3000.0 

2000.0 

1 1000.0 

...M.MUL,,M.L.,,,iMl<^^ 

135 14.0 145 15.0 

1 Sample ^Jame:4<110720a22r Sampte ID:'-GI>1W)1^18-118-' t= Be: i<110^20*.«*r 

1 Peak Name: "PFOS- Mass(*»): "499.OOW99.000 Da.499.000BO.000 Da.499.000/130.000 Da" 

• Comment:-DALGWCWi6C0110622(dll1:10)- AnnotaUon:-

Sample Index: 221 

1 Sample Type: Unknown 

Concentration: N/A 

Calculated Cone: 398. ng/mL 36*5 

Acq. Date: 7/23/2011 

Acq. Time: 2:16:52 PM g^ g 

Modified: Yes 

Proc. Algorithm: Specify Parameters - MQ III 3.2e5 

Noise Percentage: 50 

Base. Sub. Window: 1.00 mln 3_0e5 

Peak-Spilt. Factor: 6 

Report Largest Peak: Yes 

Min. Peak Height: 0.00 cps ^-" ^ Min. Peak Width: 0.00 sec 

Smoothing Width: 0 polnla 2.6*5 

RT Window: 30.0 sec 

Expected RT: 15.9 min 2_4«5 

Use Relative RT: No 

int. Type: Base To Base ^,2*5 

Retention Time: 16.B mln « 

Area: 5630287 counts & 2.0*5-

Height: 3.74e*0O5 cps ^ 

Start Time: 15.4 min S ^ g^ . 

End Time: 16.4 min g 

~ 1.6*5-

1.4*5-

1.2*5-

1.0*5-

8.0*4-

6.0*4 

4.0*4-

2.0*4-

135 14.0 145 15.0 

1553 

1 

15.69.,. 

1 1 • • • 1 • 

i5.5a.^^i J15L 5 16.0 

Tlme.min 

1579 

15.te,^ 

H 

^H 

^ H 

^ H • • • • • m J15L 5 16,0 

17.10,, 17.31 

1«.5 17,0 175 18.0 

16.5 17.0 175 18.0 

I Peak Name: "PFOS" Man<*B}: '499.000/99.000 Da,4a9.000/S0.000 Da,499.000/130.000 Da" 

• Conr«i*nt-DALGW138S0110630((fil1:10)" Annotatkm;-

Sample Index: 212 

Sample Type: Unknown 

Concentration: N/A 

Calculated Cone: 194. ng/mL 1 1Se6 

Acq. Date: 7/23/2011 

Acq. Time: 11:08:02 AM 1,10*6 

Modified: Yea l.OSeS 

Proc. Algorithm: Specify Parameters - MQ III 

Noise Percentage: 50 1.00*6 

Base. Sub. Window: 1.00 min ocive 

Peak-Split. Factor: 2 9.50e& 

Report Largest Peak: Yes ' oonul 

Mln. Peak Height: 0.00 cps w.uueo 

Mln. Peah Width: 0.00 sec 850*5 

Smoothing Width: 0 points 

RT Window: 30.0 aec 8.00*5 

Expected RT: 15.9 mln 

Use Relative RT: No 750e5 

Int. Type: Manual ' 7.00*5 

Retention Time: IS.8 min » «KA-C 

Atea: 13359050 counts g" ^-'**° 

Height: 1.19e*006 cps >; ar««^ 

Start Time: 15.3 mln f **-"^^ 

End Time: 16.3 min g 5.50*5 

5.00*5 

4.50*5 

4.00*5 

3.50*5 

3.00*5 

2.50e5 

2.00*5 

150*5 

1.00e5 

5.00e4 

15.81 1 

15.67-^ 1 

1 1 1 

• • 1 • • 

13.5 14.0 145 15.0 15. M5 16. ^ 0 165 17.0 175 18.0 1 

Thne.mh 1 

|Sampl*Nam*:'k1l0^26a226' Sample ID:-Gi>1(M]1-02-18-12r File:-k110720a.wir 

I Peak Name: "PFOS" Mass(e«): •499.000«9.000 Da.499.000«0.000 DB.499.000/1 30,000 Da" 

• Comment "DAL GW CW26L 0110622 (dQ 1:10)- Annotatkin:"" 

Sanple Index: 226 

Sanple Type: Unknown 

Concentration: N/A 95e5 

Calculated Cone: 911. no/mL 

Acq. Date; 7/23/2011 

Acq. Time: 4:01:39 PM a.ueo-' 

Modified: Yes 8.5e5 

Proc. Algorithm: Specify Parameters - MQ III 

Noise Percentage: 50 B.OeS 

Base. Sub. Window: 1.00 mln 

Peak-Split. Factor: 6 y g^g. 

Report Largest Peak: Yes 

Mln. P*ak Height: 0.00 cps 

Mln. Peak Width: 0.00 sec '•''*'' 

Smoothing Width: 0 points 

RT Window: 30.0 sec 6.5e5 

Expected RT: 15.9 mln 

Use Relative RT: No 6.0*5 

Int. Type: Base To Base S5»S 

Retention Time: 15.8 mln « " 

Area: 12573911 counts & ^„ ^ 

Height: 9.58e + 005 cps >; '•"*• 

Start Time: 15.4 min 1 

End Time: 16.4 mln g 4.Se5-

- 4.0*5 

3.5*5 

3.0*5 

2.5*5 

2.0eS 

1.5*5 

1.0e5 

5.0e4-

15.81 

15.65,. 

., 

y 

•H • • 1 1 

M I 

m^ 135 14.0 145 15.0 155 16,0 165 1^.0 175 18.0 || 

^*"""' =u 

Data printe d by STW 

Printin g Time: 12:06:03 PM 

Printin g Date : Tuesday, September 06, 

Page 27 of 29 

Page 80 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS. and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0720a.rd b 

T

Sarrvl* Nanw: l(110720a237- Sample (D: "C^PI 04)1-02-18-128- File: "kl 10720B.Mir 

P*ak Nam*: 'PFOS' Ma8s(*s): "499.00099.000 Da,499.000/80.000 Da,499.000/130.000 Da" 

Comment:-DALGW140R0110622{dU1:10)- Annotatton:"" 

Sample Index : 237 

Sample Type: Unknown 

IT 

Acq. Dat e 

Acq. Time 

Modified ; 

Proc . Alg 

Nois e Pe r 

Base . Sub 

Peak-Spl i 

Report La 

Min. Peak 

Min. Peak 

Smoothing 

RT Window 

Expecte d 

Use Rela t 

Int . Type 

Retentio n 

Area : 

Height : 

Star t Tim 

End Time : 

rlthm : 

entag e 

7/23/201 1 

7:52:1 6 PM 

Yes 

Specif y Par a 

SO 

Window: 1.00 

. Fact e r : 2 

ges t Peak: Yes 

Heigh t 

Width : 

Width : 

ve RT: 

Time : 

0.0 0 

0.0 0 

0 

30. 0 s e 

15. 9 mi 

No 

Manual 

15.7 mi 

8325647 coun t 

5.91e+005 c p 

15. 3 mi 

16. 4 mi 

15,0 15,5 16.0 16.5 

I

Sanvil*N3m*:-fcl10720a25r Sample ID:-GLPl(M)1-02-18-14a' FSe:' 

Peak Name: "PFOS" Ma»(*s): "499.000il99.000 Da ,499.000/80,000 Da.49 

Comment: "DAL GW 142R 0110622 (dU 1:10}- Annotatkin: "" 

Sample Index : 251 

^: Unknown 

5.2*5 

5.0*5 

4 5 ^ 

4.6*5 

MQ II I 

4.4*5 

4.2*5 

4.0*5 

35e 5 

3.6 ^ 

3.4*5 

3.2*5 

3.0*5 

& 25* 5 

f 2.6*5 

2.2*5 

2.0*5 

15*5 

1.6*5 

1.4*5-

1.2*5-

1.0*5-

ei)*4-

6J>*4' 

4.0*4-

2.0*4-

S8mpl*Nam«:-1(110720a246' Sampl* ID:-GLP1(M)1-02-

P*ak Nam*: 'PFOS- Masst*a): "499.000/99.000 Da,499.~ 

Camm*nt-OALGW141R0110630- Annotation:' 

Sample Index : 246 

Sampl e Type: Unknown 

Concentration : N/A 

Calculate d Cone: 3.04 ng/mL 

Acq. Pate : 7/23/201 1 

Acq. Time: 11:01:1 7 PM 

Noli Pert 

Ye s 

SO 

Base . Sub. Window: l. ( 

Peak-Split . Factor : 2 

Report Largest Peak: Y< 

Mln. Peak Height : 0. 

Mln. Peak Width : 0, 

Smoothing Width: 0 

RT Window: 30. 0 

Expecte d RT: 15. 9 

Use Relativ e RT: No 

, t . Type : 

Height: 

Start Tin 

End Time; 

Mam 

2.18e+00 5 cp s 

•18-135" Fil*:1 

.000/80.000 Da,4! 

2.1*5 

2.0*5 

1.9*5 

1.8*5 

1.7*5 

1.6*5 

1.5*5 

1.4*5 

1.3*5 

1.2*5-

l.leS ' 

1.0*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-

0.0 

15.0 15.5 16.0 16 5 17.0 17.5 18.0 

Sample Type : Unknown 

Concentration : N/A 

Calculate d Cone : 82. 6 

Acq. Date : 7/24/20 1 

Acq. Time : 12:46:2 9 

Modified : Yes 

Proc . Algorithm : Specif y 

Nois e Percentage : 50 

. AM 

Base . Sub . Window: 1.00 m 

Peak-Split . Factor : 2 

Report Largest Peak: Yes 

Mln. Peak Height : 0. 

Mln. Peak Width : 0. 

Smoothing Width : 0 

RT Window: 30. 0 

Expecte d RT: 15. 9 

Use Relativ e RT: No 

Int . Type : Manual 

Retentio n Time : 15. 8 

Area : 5838738 e 

Height : S.27e+005 

Star t Time: 15. 4 

End Time: 16. 2 

)0 

10 

s e e 

min 

c p s 

mln 

mln 

I

SampteName:'l(110720a26a' Sample ID: "GLPI (Mil •02-18-145- File:*! 

Peak Nam*: TFOS" Mass(es): -499.000/99.000 Da,499.000/80.000 Da,49 

Comnwnt -DAL GW 143R 0110622 (dB 1:10)- Annotation: " 

Sample Index : 260 

Sample Type ; 

0.0 

N/A 

Calculate d Cone: 

Acq. Date : 

Acq. Tims: 

Modified : 

Pcoc . Algorithm : 

Molse Percentag e 

Base . Sub. Windov 

Peak-Split . Fact e 

17. 8 

7/24/2 0 

3:55:3 8 

Yes 

Specif y 

ng/ 

1 

AM 

Parame 

: 1.00 ml 

r : 6 

Report Largest Peak: Y 

Mln. Peak Heigh t 

Mln. Peak Width : 

Smoothing Width : 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

Area : 12' 

Height : 

Star t Time : 

0 

0 

0 

30. 0 

15. 9 

No 

Manual 

15. 7 

4550 c 

.82e+0 0 

is. 4 

00 e 

00 a 

a « e 

mln 

mln 

epH 

mln 

15.0 155 16,0 16.5 

Tlme.min 

9.5e4 

9.0*4-

8.5*4-

6.0*4-

7.5*4-

7.0*4-

6.5e4: 

6.0*4^ 

5.5*4: 

5.0*4-

4.5*4; 

4.0*4: 

3.5*4: 

3.0*4; 

Z5*4-

2.0*4: 

t.5*4-

1.0*4' 

5000.0' 

0.0 

15.0 1S.5 18,0 16 5 17.0 17 5 18.0 

Data printe d by STW 

Printin g Time: 12:06:03 PM 

Printin g Date : Tuesday, September 06, 

Page 28 of 29 

2011 

Page 81 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

*ETS-Kirk Results Name: kll0720a.rd b 

r

S«m;fcName:1<110720a265- Sample ID:-GLP1(H)1-02-1& 

Peak Nanw: -PFOS* Mass(as): -499.000/99.000 Da,499.000/ 

Comnient:"OALGW1**S0110628(dai:10)- AiwotaUon:" 

Sample Ir.dex: 265 

Sample Type: Unknown 

Concentration: N/A 

Calculated Cone: 8,69 

Acq. Date: 7/24/2011 

Acq. Time: 5:40:48 AM 

Modified: Yes 

Proc. Algorithm: Specify Par 

Base. Sub. Window: 1.00 

Report Largest Peak: Yes 

Hin. Peak Height: 0.00 

Mln. Peak Width: 0.00 

Smoothing Width: 0 

RT Window: 30.0 3 

Expected RT: 15.9 m 

Use Relative RT: No 

Int. Type: Base To Ba; 

Retention Time: 15.7 m 

Area: 623012 coun 

ng/mL 

ameters 

min 

e p s 

polr 

In 

Height: 4.£5e-t004 cps 

End Time: 16.2 m i n 

- MQ III 

t s 

& 

i 

4.4*4 

4,2*4 

3.4*4 

2.8*4 

2.4*4 

2.2*4 

2.0*4 

1.4e4 

1.2*4 

1.0e4 

8000.0 

6000.0 

400D.O' 

2000.0 

0.0 •i^-vM^ttiefj^Maitop 

I

SamptoNam*:-kl10720a145" Sampl* 10:-GLP1&O1-02-1&O66' FUe:1 

Peak Nam*: 'PFOS- Mass(*s): '499.000/99.000 Da,499.000/80.000 0a,4' 

Commant -Trip Blank S*t 1 MS- Annotation: ~ 

9.5*5 

9.0*5 

8.5*5 

8.0*5 

7.5*5 

7.0*5 

6.5*5-

6.0*5-

5.5*5-

5.0*5-

4.5*5 

4.0*5 

3.5*5: 

3.0*5: 

2.5*5: 

2.0e5: 

1.5*5-

1.0*5: 

5.0*4: 

Sample Type: 

Concentratio 

Calculated C 

Acq. Pate: 

Acq. Time: 

Modified: 

Proc. Algori 

Noise Percer 

thm: 

-aqe 

Base. Sub- Windo 

Peak-Split. 

Min. Peak He 

Mln. Peak 'Hi 

Smoothing Wi 

RT Window: 

Expected RT: 

Use Relative 

Int. Type: 

Retention Ti 

Height: 

Unknown 

N/A 

9.45 

7/22/2011 

11:41:15 AM 

No 

Specify Par 

50 

: 1.00 

factor: 2 

St Peak: Yes 

iqht 

dth: 

dth: 

RT: 

0.00 

0.00 

0 

30.0 s 

15.9 m 

No 

Valley 

15.8 m 

6661651 coun 

.OOe+006 cp 

0.0 

13.S 14.0 14.S 15.0 15.5 16.0 16.5 17.0 17.5 18.0 

Data printe d by STW 

Printin g Time: 12:06:03 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 29 of 29 

Page 82 Of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0729b.rdb 

(0 

0) 

< 

w 

• — 

m 

g> 

< lU 

CO 

c 

< 

55 

50 

45 

40 

35 

30 

25 

45 50 55 60 

Analyte Cone. / IS Cone. 

Data printed by STW 

Printing Time: 12:08:22 PM 

Printing Date: Tuesday, September 06, 

Page 1 of 1 

2011 

Page 83 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

*ETS-Kirk Results Name: kll0729b.rd b 

• S«mpl*Nam*:T(110729b0ir Samf** ID: "11 005-25^ Fl*: •k110729b.wtr 

I Paak Nam*:-13CSPF0S^S(IS)- Man(M):''507.0001/80.000 Da' 

I Comnwnt: "2.5 ng/mL FC etd In Synth. Water Annotation: ~ 

Sample Index : 17 

Sample Type: standard 

Concentration: 0.960 ng/mL 

Calculated Cone: N/A 

Acq. Date: 7/30/2011 

Acq. Time: 10:52:40 PH 

Modified: Yes 

Proc. Algorithm: intelllQuan - IQA II 

Mln. Peak Height: 0.00 cps 

Mln. Peak Width: 0.00 sec 

Smoothing Width: 0 points 

BT Window: 30.0 sec 

Expected RT: 16.2 mln 

Use Relative RT: Mo 

Int. Type: Valley 

Retention Time: 16.1 mln 

Area: 697115 counts 

Height: l.lSe'OOS cps 

Start Time: 16.0 mln 

End Time: 16.A nIn i 

1.15*5 

1.10*5 

1.05*5 

1.00*5 

9.00*4 

8.50*4 

8.00*4 

7,50*4 

7.00*4 

6.50*4 

6.00*4 

5.50*4 

5.00*4 

4.50*4 

4.00*4 

3.50*4 

3.00*4-

2.50*4 

2.00*4 

1.50*4 

1.00*4 

5000.00 

0.00' 

I

Sampt*l4am*:'k110729b028' Sample ID:'LCS-110726-1' Fie:'V110729b.w(r 

P«>kNam*:'13C8PFOS-tS(ISr Mss3<«a): "SOT.OOCVBO.OOO Da' 

Comm*nt: t)J2ppb LCS" Annotation: ~ 

Sample Index : 28 

Sample Type : OC 

Concentration : 0.95 3 ng/mL 

Calculate d Cone ; N/A 

Acq. Date : 7/31/201 1 

Acq. Time: 2:44:3 3 AM • 

Modified : Ho 

Sampt*Nam*:-1(110729b02r Sampt* ID:'11 002-243' FO*:-kl10729b.wtr 

P*ak Nam*: -13C8PFOS-IS(IS)- Ma«3<es): "507.000/80.000 DaComment *M*thod Blanir Annotatkin: 

SampJ' 

Sample Type: 

ng/mL 

Calculated Cone: 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Mln. Peak Height 

Mln. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

N/A 

7/31/201: 

2:23:30 AM 

IntelllQu 

: 0.00 

0.00 

0 

30.0 

16.2 

an - IQA II 

cps 

aec 

points 

mln 

1.2*5 

Use Belatlv . 

valley 

16.1 

03 331 cc 

1.50e+005 

16.0 

16.3 

mln 

cpn 

mln 

mln I 

^ 

1 

1.0*5 

9.0*4 

8.0*4 

7.0*4 

14.0 14.5 

Proc. Algorithm: 

Hln. Peak Height: 

Mln. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

ntelllQ 

0.00 

0.00 

0 

30.0 

16.2 

No 

Valley 

16.2 

Area: 573071 cc 

Height: 9 

Start Time: 

End Time: 

17et00* 

16.0 

16.1 

an -

sec 

mln 

mln 

mln 

mln 

Modified: 

Proc. Algorithm: 

Mln. Peak Height 

Mln. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

No 

IntelllQ.! 

0.00 

0.00 

0 

30.0 

16.2 

No 

Valley 

16.2 

Area: 629190 CO 

Height: 

Start Time: 

.07e+005 

16-1 

I

SampteNam*:1<110729b03r Sampl*ID:-LCS-110726-4' FI*:'V110729b,\»Wr 

P*akNam*:'13C8PFOS-IS{IS)' Uas9(*a): ^5O7.00(V80.000 Da' 

Comment *2ppb LCS" Annotation:" 

Sample Index: 31 

Sample Type; QC 

Concentration : 0.953 ng/mL 

Calculate d Cone: N/A 1.05*5' 

Acq. Date: 7/31/2011 

Acq. Time: 3:47:55 AH 1.00*5' 

9.50*4' 

8.50*4-

8.00e4-

7.50*4-

7.00*4-

6.50*4-

« 6.00*4-

^ 5.50e4-

g 5.00*4-

4.50*4-

4.00*4-

3.50*4-

3.00*4-

2.50*4-

2.00*4-

1.50*4-

1.00*4' 

5000.00 

0.00 .J^r^,. 

Data printe d by STW 

Printin g Time: 12:10:58 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 1 of 7 

Page 84 Of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0729b.rd b 

• SampleNam*:1(110729b034- Sample ID:'LCS-11072&-r Fl*:'k110729b.w 

• Paak Name:'13C8PFOS-IS05}' Mass(*s):'507.000/BO.OOO Da" 

I Comment '20ppb LCS" Annotatkm:'" 

Sample Index : 34 

Sample Type; QC 

Concentration : 0.953 ng/mL 

CalcuUte d Cone: N/A 

Acq. Date: 7/31/2011 14 ^ 

Acq. Tine : 4:51:17 AM 

Modified: 1.3*5 

Proc. Algorithm: 

Min. Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

Yes 

IntelllQuan 

: 0.00. c 

0.00 3 

0 po 

30.0 s 

16.2 m 

No 

Valley 

16.2 m 

Area: 900961 coun 

Height: 

Start Time: 

L.48et005 c 

16.0 m 

8.0*4 

7.0*4 

6.0*4 

5.0*4 

4.0*4' 

3.0*4 

Z0e4 

1.0*4-

0.0-

14.0 14.5 

../TVlH.. 

I

Samp4*Nam*:Tc110729bO44' Samp** tD:'LCS-110726-13^ File:'k110729b.w4r 

P*akName:'13C8PFOS^S05)- Mass<*s):'5O7XO0/BO.OO0 Da' 

Comm*nt: "2ppb LCS ECF" Annotatton;" 

Sample Index: 44 

Sample Type: QC 

Concentration: 0.954 ng/mL 

Calculated Cone: N/A 

Acq. Date: 7/31/2011 

Acq. Time: 8:22:25 AM 

Sampl* Nam*; "k110729b04r Sample ID:'LCS-110726-10' FJl*:-k110729b.w 

P*ak Nam*: '13C8PFOS-IS(IS)' Ma«s<Bs): -S07JX)0/80.000 Da' 

Comment •0.2ppb LCS ECP Annotatfen:" 

Sample Index: 41 

Sample Type: QC 

Concentration: 0,953 ng/mL _ ^ 

Calculate d Cone: N/A S-5«4-

Acq, Date: 7/31/2011 

Acq. Time: 7:19:05 AM 9.0*4-

8.5*4-

A II 

8.0*4-

7.5*4-

7.0*4-

6.5*4-

6.0*4-

- 5.6e4-

S. 

i '•°"-

I 4.5*4-

4.0*4-

3.5*4-

3.0*4-

Modified: 

Proc. Algorithm: 

Mln. P-ak Height: 

Mln. Paak Width: 

Smoothing Width: 

RT Window; 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

Yes 

ntelllQ-j 

0.00 

0.00 

0 

30.0 

16.2 

No 

Valley 

16.1 

Area: 589221 co 

Height: 9 75e+004 

I ,./s».. 

Modified: 

Proc. Algori 

Mln. Peak He 

hm; 

ght: 

Min. Peak Width: 

Smoothing Width; 

RT Window: 

Expected RT; 

Use Relative 

Int. Type: 

Retention Tl 

Area: 

Height: 

Start Time: 

End Time: 

RT: 

Yes 

intelllQL 

0.00 

0.00 

0 

30.0 

16.2 

No 

Valley 

16.1 

577343 CO 

1 OOe-tOOS 

16.0 

16.3 

an - 1 

cps 

points 

mln 

min 

cps 

min 

I

SBn«)leName:'V11072gb04r SamptelD:' 

P*akNam*:'13C8PFOa4S(IS>' Mas9(*s):' 

Comment '20ppb LCS ECP Annotatkin: ~ 

Sample Index: 4 7 

Sample Type; QC 

Concentration: 0.953 ng/mL 

Calculated Cone: N/A 

Acq. Date: 7/31/2011 

Acq. Time: 9:25:45 AM 

Modified: 

Proc. Algorithm 

Mln, Peak Heigh 

Mln. Peak Width 

Smoothing Width 

RT Window: 

Expected RT: 

Use Relative RT 

Int. Type: 

Retention Time: 

Yea 

IntelliOuan - I 

: 0.00 

0.00 

0 

30.0 

16.2 

No 

Valley 

16.1 

Area: 666352 c 

Height: 

Start Time: 

End Time; 

1.07et005 

16.0 

16.4 

cps 

points 

sec 

mln 

cps 

mln 

mln 

16J) 16.5 

1.05*5 

l.OOeS 

9.50e4 

9.00e4 

S.50e4-

8.00*4-

7.50*4 

7.00*4 

6.50*4 

6.00*4 

% 5.50*4-

f 

I 5.00*4-

4.50*4-

4.00*4-

3.50*4-

3.00*4-

2.50*4-

Z00*4-

1.S004-

1.00*4-

5000.00-

0.00-

,.A?s».>., 

Data printe d by STW 

Printin g Time: 12:10:58 PM 

Printin g Date : Tuesday, September 06, 

Page 2 of 7 

2011 

Page 85 Of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

*ETS-Klrk Results Name: kll0729b.rd b 

I

SampteName:"k110729b072' Sample ID:-GLP1(K}1-02-1&093- File:-k110729b.wirr 

Paak Nama; '•13CSPF0&^S<IS}' Ma89(es): '507J)OQ/80.000 Da* 

Comment:-DALGW137S0110624- Annotatton:" 

Sampl e Type ; 

Calculate d Cone 

Acq. Date : 

Acq. Time : 

Modified : 

Proc . Algorith m 

Mln. Peak Heigh' 

Min. Peak widt h 

Smoothin g WldthRT Window; 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

Unknown 

0.96 0 

N/A 

7/31/201 1 

6:14:2 7 P 

Yes 

IntelliQ u 

: 0.0 0 

0.0 0 

30. 0 

16. 2 

No 

valle y 

Area : 733901 co 

Height ; 

Star t Time: 

End Time : 

1.25e'(-005 

16. 0 

16. 4 

1.20*5 

1,15*5' 

1.10*5 

1.05e5 

1.00*5-

9.50*4-

9.00*4-

8.50*4-

8.00e4-

750e4-

7.00e4 

6.50e4-

6.00*4-

5.50*4 

5.00*4 

4.50*4 

4.00*4 

3.50e4 

3.00*4-

2.50*4 

2.00*4 

1.50B4 

1.0Oe4 

5000.00 

0.00' 

16.14 

14.0 14,5 

• ,/VS,—,.. 

SampieName:1c110729b086' Sample ID:'GLP1041-02-18-108 - File: 1(110729b.wir 

Peak Nam*: -13C8PFOS-(S(IS)' Mass{ee): '507.000/80.000 DaComment:-OALGW138L0 110630' Annotatnn:-

Sampl e Index : 86 

Sampl e Type : Unknown 

Conctntratlon : 0.96 0 ng/mL 

N/A 

I SampleNam*:'k110729b08r Sampt*ID:'GLP1001-02-18-098' File:-1(110729b.wir I

P*ak Name: -13C8PFOS-IS0S)' Ma«{*9): "507.000/80.000 Da' 

CommenfDALGW137L0110624' Annotatton:" 

Sample Index : 81 

Sample Type ; Unknown 

Concentration : 0.96 0 

Calculate d Cone ; N/A 

Acq. Date ; 7/31/201 : 

ng/mL 

Acq. Time : 9:24:5 9 PM 

Modified : Yes 

Proc . Algorithm ; IntelllQ ' 

Mln. Peak Height : 0.0 0 

Mln. peak «idth : 0.0 0 

Smoothing Width : 0 

RT Window; 30. 0 

Expecte d RT: 16. 2 

Use Relativ e RT: No 

Int . Type : Valle y 

Retentio n Time: 16. 1 

Area : 1004652 co 

Height : l.BletOOS 

Star t Time ; 16. 0 

End Time : 16. 5 

cp s 

a e c 

poin t 

mln 

c p s 

min 

IQA 11 

= 

& 

1.8*5-1 

1.7*5-

1.6*5-

1.4*5-

1.3*5-

1.2* -

1.1*5-

1.0*5-

9.0*4-

8.0*4-

7.0*4-

6.0*4-

5.0*4-

4.0e4-

3.0*4-

Z0e4-

1.0*4-

I

San ^ Nam*: "kll0729b095* Sample ID: 'GLPI0^1-02-18-145* File: 'k110729b.>vtr 

P*ak Name: -13C8PFOS-IS(IS}- Mass{*a): '507.000/80.000 Da' 

Comment'DALGW143R 0110622-ISaddacT Annotatton:"" 

Sanpl e Index : 95 

Sample Type : Unknown 

Concentration : O.960 ng/mL 

Calculate d Cone: N/A 

Acq. Date : 8/1/201 1 

Acq. Time: 2:21:2 5 AM 

lulate d Cone: 

Acq. 

Acq. 

Dat e 

Time 

Modified : 

Mln . 

Algor i 

Peak 

Peak 

Smoothin g 

RT W ndow 

Expecte d 

He 

hm: 

• gh t 

Width : 

Width ; 

;T: 

Use Relativ e 

Int . Type 

Retentio n 

Are a 

Ti 

KT; 

7/31/201 1 

11:10:4 7 

Yes 

IntelliQ u 

0.0 0 

0.0 0 

0 

30. 0 

16. 2 

No 

Valle y 

16. 1 

598907 CO 

Star t Time : 

1.05*5-

LOOeS9.50e4-

9.00*4-

6.50*4-

6.00*4-

7.50*4-

7.00*4-

6.50*4-

« 6.00*4-

* 5.50*4-

I 5.00*4-

4.50*4-

4.00*4-

3.50*4-

3.00*4-

2.50*4-

2.00e4-

1.50*4-

1.00*4-

5000.00 

0.00 

Modified : 

Proc . Algorith m 

Mln. Peak Heigh 

Mln. Peak Width ; 

Smoothing Width ; 

RT Window: 

Expecte d RT: 

Use Relativ e RT 

Int . Type : 

Retentio n Time : 

Yes 

IntelII Q 

: 0.0 0 

0.0 0 

0 

30. 0 

16. 2 

No 

Valle y 

16. 1 

Area : 852592 cc 

Height ; 1.52et00 5 

i ../Vs^^, 

Data printe d by STW 

Printin g Time: 12:10:58 PM . 

Printin g Date : Tuesday, September 06, 2011 

Page 3 of 7 

Page 86 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0729b.rd b 

T

Sampl*NBm*:>110729t>100' Sample 10:'GLP1041-02-1B-150' Fll*:'k110729b.wlr 

Paak Nam*: '13C8PFOS-IS0S)' Maaa(*8): "507.000/80.000 Da' 

Comniant:'DALGW144S0110628-ISBdd«d- Annotatkin:" 

Sample Type: 

Calculated Coi 

Acq. Date: 

Acq, Time: 

Min. Peat Width: 

Smoothing Width: 

RT Window: 

Unknc 

0.960 ng/mL 

itelliQuai 

0.00 • 

0.00 : 

6 Relatlv. 

it. Type: 

Height: 

Start Tlm( 

End Time: 

l.38e+0O4 cps 

8.0*4-

7,5*4-

7.0*4-

6.5*4 

6.0*4 

5.5*4 

5.0*4 

4.5*4 

4.0*4 

2.5*4 

2.0*4 

14.0 14.5 1 ./rs„, 

I

Sampl* Name: l(110729b027' Sampl* ID:'11 002.243' Fle:1d10729b.w<r 

Peak Name: 'PFOS* Massf**); '499.OCW99.000 Da,499.000/80.000 Da.499.0D(V130.000 DaComment: "Matttod Blank' Annotatton: 

Sample Index: 27 

Sample Type: Unknown 

ng/mL 

7/31/2011 

30 AM 

4000 

I

SampleName:'k110729bOir Sampl*ID:'11 00»2&«' Fil*:'k1l0729b.»flr 

P*ak Nam*; 'PFOS* Masa<*B): "499.000/99.000 Da,499.000/80.000 Da,499.000/130.000 Da' 

Comment *2.5 rqjAnL FC etd In Synth. VVM*r Annotafion:"" 

Sample Type: 

Calculated Cone: 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Noise Percentage 

Standard 

2.50 ng/mL 

2.SA ng/mL 

7/30/2011 

10:52:40 PM 

Yes 

Specify Paramete 

50 

Base. Sub. Window: 1.00 mln 

Peak-Split. Fact 

Report Largest P 

Mln. Peak Height 

Mln, Peak Width: 

Smoothing Width: 

RT Window: 

Expected KT: 

Use Relative RT: 

int. Type; 

Retention Time: 

:ak: Yes 

0.00 cps 

0.00 aec 

0 po 

30.0 sec 

16.2 mln 

No 

llanual 

16.2 mln 

Atea: 1980062 counts 

Height: 

Start Time: 

End Time: 

i.27e+005 cps 

16.1 mln 

16.A mln 

Modified: 

Proc. Algorithm: S| 

Noise Percentage: 

Base. Sub. Window: 

Peak-Split. Factor 

f y Pai - MQ II I 

Hln Peak Height: 

Mln. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Height: 

Start Tli 

End Time: 

16.2 

22841 COI 

t.lSe-tOOS 

16.1 

I

Sampl* Name: •k110729b028- Sampl* ID: "LCS-110726-1- F(e:*V110729b.wir 

P*ak Nam*: 'PFOS' Mas*(fls): '499.000/99.000 Da,499.000/80,000 Da,499.000/130.000 Da" 

Commant '0.2ppb LCS' Annotation:" 

2.6*4 

2.5*4 

2.4*4-

2,3*4-

2.2*4-

2.1*4-

2.0*4-

1.9*4-

1.8*4-

1.7*4-

1,6*4-

1,5*4-

Sample Index: 

Sample Type: 

Calculated Cone: 

Acq. Date: 

Acq. Time: 

Modified: 

Ptoc. Algorithm: 

Noise Percentage 

Base. Sub. Windo 

28 

QC 

0.199 

0.257 

7/31/2011 

2:44:33 AM 

No 

Specify Par 

50 

J: 1.00 

Peak-Split. Factor: 2 

Report Largest Peak: Yes 

Mln. Peak Height 

Mln. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

0.00 

0.00 

0 

30.0 a 

16.2 m 

No 

Valley 

16.2 r 

Area: 1695J5 coun 

Height: 

Start Time: 

.6<e+004 c 

16.1 m 

ng/mL 

ng/mL 

amete 

c p s 

e c 

I n 

Ln 

I n 

1.4*4' 

1.3*4 

1,2*4 

1.1*4 

1.0*4 

9000.0 

aooo.0 

7000.0 

6000.0 

5000.0-

4000.0-

3000.0 

2000.0 

1000.0-

0.0 i.fi»nl«H<*i|i<lDil>*H(ii*i|li| 

16.0 16.5 

Tim*, mln 

Data printe d by STW 

Printin g Time: 12:10:58 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 4 of 7 

Page 87 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS. PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0729b.rdb 

r

Sample Nam*:"k11072aj03r Sample ID:'LCS-11072S-»' Fl*:'1<110729b.wir 

P*ak Nam*: 'PFOS' htas3(*8): '499.000/99.000 Da,499.000/80.000 Da.499.000>'130.000 Da' 

Comntent '2ppb LCS' /knnotatton:" 

Sample Index: 31 

Sample Type: QC 

Concentration: 1.9 9 

Calculated Cone: 2.11 

Acq. Date: 7/31/2011 

Acq. Time: 3:47:55 AM 

Modified: No 

Proc. Algorithm: Specify Par 

Noise Percentage: 50 

Base. Sub. Window: 1.00 

Peak-Split. Factor: 2 

Report Largest Pe«k: Yes 

Min. Peak Height: 0.00 

Min. Peak Width: 0.00 

Smoothing Width: 0 

RT Window: 30.0 3 

Expected RT: 16.2 m 

Use Relative RT: No 

Int. Type: Valley 

Retention Time: 16.2 m 

Area: 1494748 coun 

ng/mL 

ng/mL 

amete 

mln 

s 

Height: 2.53etO05 cps 

Start Time: 16.1 m 

End Time: 16.4 mln 

16.5 17.0 18.0 16.5 

Sampl*Nam*:"k110729b041' Sampl* ID: •LCS-110726-10" File:'"1(110729b.yiiifr' 

P*ak Name: "PFOS' Maa3(*9): '499.000/99.000 Da,499.O0O/SD.O00 Da,499.000/130.000 DaComment: "0.2pp6 LCS ECF" Arewtatton:-

Sample Indi 

I

Sampl* Nam*: 1(1107291)034- Sample ID:'LCS-110726-7" Fta:-k110729l].«tfr 

P*ak Nam*: "PFOS" Mseatee): '499.000/99.000 Da,499.000/80.000 Da.499.000/130.000 DaComment '20ppt> LCS" Annotation: ~ 

Sample Index: 

Sample Type; 

Concentration: 

Calculated Cone: 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Noise Percentage; 

Base. Suta. Windo* 

Peak-Split. Facto 

Report Largest Pe 

Min. Peak Height: 

Min. Peak Width: 

Smoothing Width: 

RT Window; 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

Area: 2 0; 

Height: 2 

Start Time: 

End Time: 

34 

OC 

19.9 

20.8 

7/31/2011 

4:51:17 AM 

Yes 

Specify Pa 

50 

: 1.00 

c: 2 

ak; Yes 

0.00 

0.00 

0 

30.0 

16.2 

No 

Manual 

16.1 n 

79566 cot 

.3Set006 c 

16.4 R 

I

Sample Nam*: "k110729b04*- Sample ID: •lCS-110726-ir Fil*: •k110729b.»tfr 

P*ak Name: "PFOS" Ma3s(ee): '499.000/99.000 Da.499.000/80.000 Da,499.000/130.000 DaComment '2ppb LCS ECF" Annotation: ~ 

SaDq:>le Index: 44 

Sample Type: QC 

Concentration: 

Calculated Cone: 

Acq. Date: 

Acq. Time: 

Modified: 

Proc, Algorithm: 

Noise Percentage 

0.198 

0.272 

7/31/2011 

7:19:05 

Yes 

Specify 

50 

ng/mL 

ng/mL 

AM 

Paramete 

Base. Sub. Window; 1.00 

Peak-Split. Factor: 2 

Report Largest Peak: Yes 

Hln. Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Window; 

Expected RT: 

Use Relative RT: 

Int, Type: 

Retention Time: 

Height: 2 

Start Time; 

End Time: 

0 

0 

30.0 

16.2 

No 

Manual 

16.1 

4644 

.lle+00 

15.9 

16.3 

min 

00 cps 

00 sec 

po 

mln 

mln 

c p s 

mln 

mln 

2.1*4 

2.0*4 

1.9*4 

1.8*4 

1.7e4 

1.6*4 

1.5*4 

1.4*4 

1,3*4 

1,2*4 

1.1*4 

1,0*4 

9000.0 

8000.0 

7000.0 

6000.0 

5000.0 

4000.0 

3000.0 

2000.0 

1000.0 

0.0 •MhM i 

16,15 

15.99s. 

II 11 • H 

^B^ie ^ 

',''"lfl ilfk JA^HAI , 

Sample Type: 

Concentratio 

Calculated C 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algori 

Noise Percen 

Base. Sub. W 

Peak-Split. 

hm: 

a g e 

OC 

1.98 

2.26 

7/31/2011 

8:22:25 Al 

Yes 

Specify P 

50 

ndow: 1.00 

3r: 2 

Report Largest Peak; Yes 

Mln. Peak He g h t 

Min. Peak Width: 

Smoothing Ml 

RT Window: 

Expected RT: 

Use Relative 

Int. Type: 

Retention Tl 

Area: 

Height: 

Start Time: 

End Time: 

ith: 

RT: 

14 

ng/mL 

ng/mL 

aramete 

min 

0.00 cps 

0.00 sec 

0 

30.0 

16.2 

No 

Kanual 

16.1 

5570 CO 

.E3e+005 

15.8 

16.3 

po 

mln 

mln 

n ts 

c p s 

mln 

mln 

14.0 14.5 155 lao 16.5 17.0 17.5 18.0 185 

Data printed by STW 

Printing Time: 12:10:58 PM 

Printing Date: Tuesday, September 06, 

Page 5 of 7 

Page 88 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

FSIA-June 2011 

*ETS-Kirk Results Name: kll0729b.rd b 

l||Samp<*Nam*:"k110729lfl4 r Sampte ID:-t.CS-110726-16r Fli*:1c110729b.wifr 

• Peak Nam*: "PFOS' Irias3(«s): '499.000/99.000 Da,499.000/80.000 Oa,499.00a'130.000 Da' 

• Comment: '20ppb LCS Ec r Annotatkm: -

Sample Index ; 47 

Sample Type : QC 

Concentration : 19. 8 ng/mL 

Calculate d Cone : 22. 9 ng/mL 16*6 

Acq. Date : 7/31/201 1 

Acq. Time: 9:25:4 5 AM 

15*6 

Modified : Yes 

Ptoc . Algorithm : Specif y Parameters - MO II I , . ^ 

Nois e Percentage : 50 '•** ^ 

Base . Sub. Window: 1.00 mln 

Peak-Split . Factor : 2 )_3 ^ 

Report Largest Peak: Yes 

Mln. Peak Height : 0.0 0 cp s 

Min. Peak Width : 0.0 0 se c 1-2*6 

Smoothing Width : 0 point s 

RT Window: 30. 0 se c . . ^ 

Expecte d RT: 16. 2 min '•'" ° 

Use Relativ e RT; No 

1.0*6 

Int . Type : Manual 

Retentio n Time : 16. 1 rain , 

Area : 16527493 counts g" S-'* ' 

Height : 1.66e*006 cp s >: 

Star t Time: 15. a mln | g( ^ 

End Time : 16. 4 min | 

7.0*5 

6.0*5 

5.0*5 

4.0*5 

3.0*5 

2.0*5 

1.0*5 

16.15 

16.01^ 

II 

• 1 

M. 14.0 14.5 15.0 15.5 16.0 16.5 17.0 175 18.0 18 5 

1 SampleName:-k110729b08r Sampkt ID:"GLP1CKI1-02-1U»8- File: "kl 10729b.wtr ~~ " T\m^.nir\ 

1 P*ak Name: 'PFOS' hta3S{*s): "499.00099.000 Da.499.000/80.000 Da,499.00(V130.000 Da* 

• Comment:"DALGW137L0110624' Afmotatbn:" 

Sample Index : 81 

Sample Type : Unknown 

Concentration ; N/A 24B S 

Calculate d Cone: 1.93 ng/mL 

Acq. Date : 7/31/201 1 2 3*5 

Acq. Time: 9:24:5 9 PM 

2.2e5 

Modified : Yes 

Proc . Algorithm : Specif y Parameters - MQ II I 2.1B5 

Nois e Percentage : 50 

Base . Sub. Window: 1.00 min ^"" ^ 

Peak-Split . Factor : 2 ^ g ^ 

Report Largest Peak: Yes 

Mln. Peak Height ; 0.0 0 cp s 18* 5 

Mln. Peak Width : 0.0 0 se c 

Smoothing Width : 0 points 1.7*5 

RT Window: 30. 0 se c 

Expecte d RT: 16. 2 min l-*«5 

Use Relativ e RT: No ^ 

1 Int . Type: Manual 4 j ^ 

Retentio n Time : 16- 1 mln « 

Area : 2172452 counts & 1.3*5 

Height : 2.43etO0 5 cp s ^ 

Star t Time: 15. 8 min "W 1.2*5 

End Time: 16.4 min g 

1 1.1*5 

1.0*5 

9.0*4 

6.0*4 

7.0*4 

6.0*4 

5.0*4 

4.0*4 

3.0*4 

2.0*4-

1.0*4-

1614 

16.00^ 

• II • • 

14.0 14.5 15,0 15 5 16. M0 18. . 5 17.0 175 18.0 18 5 

1 Tlme.mtn 

I P*ak Nam*: -PFOS" Iltas3<*8): '499.000/99.000 De,499.000/80.000 Da,499.000/130.000 Da' 

Sample Index : 72 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone : 0.49 8 ng/mL ^^ * 

Acq. Date : 7/31/201 1 

Acq, Time: 6:14:2 7 PM *'^ * 

Modified : Yes 3.8«4 

Proc . Algorithm : Specif y Parameters - MQ II I 

Nois e Percentage : 50 3.6*4 

Base . Sub. window: 1.00 mln 

Peak-Split . Factor : 2 3.4«* 

Report Largest Peak: Yes 

Min. Peak Height : 0.0 0 cp s 3.2*4 

Mln. Peak Width : 0.0 0 se c 

Smoothing Width ; 0 point s 3.0*4 

RT Window: 30. 0 se c 

Expecte d RT; 16. 2 min 2.8*4 

Use Relativ e RT: No 

Z6*4 

Int . Type : Manual 

Retentio n Time: 16- 1 mln j , Z4*4 

Area : 414083 counts g" 

Height ; 1.29e-t004 cp s >: 2,2*4 

Star t Time: 15- 8 mln ft 

End Time: 16. 3 rain J 2.0*4 

1.8*4 

1.6*4 

1.4*4 

1.2e4 

1.0*4 

8000,0 

6000.0 

4000,0 

2000.0 

1614 

15,99.. 

1 

1 15.65..M 

14.0 14 5 15.0 15 ^^j 5 16. m 0 

I Peak Name; "PFOS- Mas9(*s): •499.000«9.000 Da,499.000/80.000 Da.499.000/130.000 Da' 

• Comm*nt'DALGW138L011063ff' Annotatton:" 

Sample Index : 86 

Sample Type: Unknown 

Concentration : N/A , . , 

Calculate d Cone ; 0.84 0 na/mL "•'" ^ 

Acq. Date : 7/31/201 1 50, 4 

Acq. Time: 11:10:4 7 PM 

4.8e4 

Modified : Yes 

proc . Algorithm ; Specif y Parameters - MQ II I ^•°" * 

Nois e Percentage : 50 4.404. 

Base . Sub. Window: 1.00 mln 

Peak-Split . Factor : 2 4.2*4-

Report Largest Peak: Yes .^ ^ 

Min. Peak Height : 0.0 0 cp s 

Min. Peak Width : 0.0 0 se c 3.8*4 

Smoothing Width : 0 point s 

RT Window: 30. 0 se c 3-6»4 

Expecte d RT: 16. 2 min -> ^ J 

Use Relativ e RT: No ^'^ ^ 

3.2e4 

Int . Type : Manual 

Retentio n Time: 16. 2 mln „ ^•"' * 

Area : 566383 counts & 2.8e4 

Height : 5.25e+00 4 cp s ^ 

Star t Time: 15. 8 mln f 2.6e4 

End Time : 16. 3 mln S 

1 24e4 

2 A 4 

2.0e4 

1.8e4 

1.6e4 

1.4*4 

1.2e4 

1.064 

8000.0 

6000.0 

4000.0-

2000.0-

16.52 17J 4 

w/V,..,.,^ ^mJK.^.f.^ 

1 6 5 17.0 175 18.0 

16.1A 

16.0U 

1 1 

• I

• I 

ll 

14.0 14 5 15.0 15..5 16. M 0 

I 17.77 

l\. J-Jv ... 

1 6 5 17.0 17 5 18.0 

' y ^ 1 

185 j 

1 8 5 

Data printe d by STW 

Printin g Time: 12:10:58 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 6 of 7 

Page 89 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0729b.rd b 

• Sample Name:'k11072Sb095' Sampto ID:'GLP1(K}1-02-18-145' 

I Peak Nam*: 'PFOS' Iillas3(ett): '499.000/99.000 Oa,499.000/80,000 Da.4 

• Comment:'DALGW143R0110622-ISadd*<r Annotatkin: "^ 

Sample Index: 95 

Sample Type: 

Con< atloE N/A 

Calculated Conc: 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Noise Percentage 

23.4 

8/1/2011 

2:21:25 AM 

Yes 

Specify Pa 

SO 

Base. Sub. Window: 1.00 

Peak-Split. Factor: 2 

Report Largest p 

Mln. Peak Height 

Mln. Peak Width: 

Smoothing Width; 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

Area: 21 

ak: Yes 

0.00 

0.00 

0 

30.0 3 

ng/mL 

min 

cp s 

e c 

16.2 min 

Ko 

Manual 

16.0 n 

63806 cot 

i n 

n t s 

1.7*6 

1.6*6 

1,5*6 

1.4*6 

13*6 

1.2*6 

1.1*6-

1.0*6 

9.0*5 

8.0*5 

7.0*5 

6.0e5-

5.0e5-

4.0e5-

3.0e5 

2.0e5-

1.0e5-

0.0-

14.0 145 1S.0 155 16.0 16.5 17.0 175 18.0 165 

1 Sampl*Nam*:n<110729t>10(r Sampla ID:-GLP1&O1-02-18.150- FB. -wia729b.wir 

I Paak Nam*:'PFOS- Masa{*a):-499.000/99J}00Oa,499.000/80.00ODa,499.0D0/13D.000Da" 

• Commant'DALGW144S0110628-lSadd*d' 

Sample Index: 100 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Conc: 29.5 ng/mL 

Acq. Datft: 8/1/2011 

Acq. Tlmo: 4:07:21 AM 

Modified : Yes 

Proc. Algorithm : Specif y Parameters -

Kolse Percentage: 50 

Base. Sub. Window: 1.00 min 

Peak-SplU . Factor: 2 

Report Largest Peak: Yea 

Mln . Peak Height: 0.00 cps 

Mln . PeaK Width: 0.00 sec 

Smoothing Width: 0 point s 

RT Window: 30.0 sec 

Expected RT: 16.2 min 

Use Relativ e RT: No 

Int . Type; Manual 

Retention Time: 16.0 mln 

Area: 15004231 counts 

Height : 1.24et006 cps 

Star t Time: 15.7 min 

End Time! 16.4 min 

Annotatton:" 

MQ II I 

1.20*6 

1.15*6 

i.ioee 

1.05eB 

1.00e6 

9.S0e5 

9.00*5 

850*5 

6.00eS 

750*5 

.00. 5 

^ . 650*5 

1 6.00*5 

1 550*5 

SJOOeS 

450*5 

4,00*5 

350*5 

3.00*5 

250e5 

2.00e5 

1.50e5 

1.00B5 

5.00e4 

0.00 

^5A^ 

14.0 14.5 15.0 15.5 16.0 165 17.0 175 18.0 185 

Tlnw. mh 

Data printe d by STW 

Printin g Time: 12:10:58 PM 

Printin g Date : Tuesday, September 06, 

Page 7 of 7 

Page 90 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Workstation: ETSKIRK Results Name: kll0729b ext.rdb 

Data worked up by KJU Page 1 of 1 

Printing Time: 12:04:36 PM 

Printing Date: Wednesday, August 03, 2011 

Page 91 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS. PFHS, and PFOS in Water Samples 

FSIA-June 2011 

Results Name: kll0729b ext.rd b 

Sanv>leName:l(11072gb019' Sample 10: 

Peak Name: 'PFOS' Mss9(*e); '499.00Q'99 J 

Comnwnt 1 0 t^ML FC Od h Syrth, Wat*^ 

Calcu 

Acq. 

15.0 15 5 16.0 16 5 

SamF'eNBine:*kll0729l>02r Sampt*ID:"11 002-243' File:*k110729b.wnr 

Peak Name: -pFOS* Mass(*s): '499^)0/99,000 Da .499.000/60.000 Ds.499.00a/130.000 Da* 

Comm*nt "Method Btank" Annotatkin: ~ 

Sample Index : 27 

Sample Type : 

Concentration ! N/A 

Calculate d Conc : 0.65 3 ng/mL 

Acq. Date : 7/31/201 1 

Acq. Time : 2:23:3 0 AM 

Modified : Yes 

Proc . Algorithm : Specli y Parameters 

Noir e Percentage : 50 

Base . Sub. Window: 1.00 mln 

Peak-Split . Factor : 2 

Report Largest Peak : Ves 

Min. Peak Height : 0.0 0 cp s 

Min. Peak Sldth : 0.0 0 ae c 

Smoothing Width : 0 poin t 

RT Window: 30. 0 ae c 

Expecte d RT: 16. 2 mln 

Use Relativ e RT: No 

Int . Type : Manual 

Area : 23923 counts 

Height : 4.26e+00 3 cp s 

Star t Time: 16. 1 mln 

- MQ II I 

1 

1 

4400-) 

4200-

4000-

3600-

2600-

2400-

2200-

1800-

1600-

1400-

1200-

1OO0-

I

Sample Name: 1(110729l>034- Sample ID: XCS-110726-r Fi*:-k110729b.w4r 

Peak Nam*: -PFOS" Maaa(*8): '499.000/99,000 Da ,499.000/80.000 Da .499.000/130.000 Oa* 

Comment "TOppb LCS' Annotation: ~ 

Sanpl e Index : 34 

Sample Type : OC 

Concent ra t Ion : 19. 9 ng/mL 

Calculate d Conc : 21. 4 ng/mL 

Acq. Date : 7/31/201 1 

Acq, Time : 4:51:1 7 AM 

18.0 185 

I

Sample Name: 1(1107291)031- Samp 

Paak Nam*: 'PFOS* Mas9{*«); '499. 

Comm*nt: '2ppb LCS' Annotatton:" 

Sample Index : 3 1 

Sample Type : 

Calculate d Conc: 

Acq. Date : 

Acq. Time: 

1,99 ng/mL 

2,0 7 ng/mL 

7/31/201 1 

3:47:5 5 AM 

No 

; Pen 

Peak-Split . Factor : 

Report Largest Peak: 

Kin . Peak Height : 

Mln. Peak Width : 

Smoothing Width : 

RT Window: 31 

Expecte d RT: 

Use Relativ e RT: r 

Height : 

Star t Time; 

[4 9474 8 C( 

2.53e+00 5 

16. 1 

2.5eS 

Z4*5 

2.3*S 

2.2*5 

2.1*5 

2.0*5-

15*5-

1.8*5-

1.7*5-

1.6*5 

1.5*5 

1.4e5 

1,3*5-

1.2*5-

l.leS1.0*5-

9.0*4-

8.0*4 

7.0*4 

6.0*4-

5.0e4-

4.0e4-

3,0e4-

2.0*4-

1.0*4-

Modified : Y 

Proc. Algorithm ; Spec 

Noise Percentage: 

Base. Sub. Window; 

Peak-Split . Factor: 

Report Largest Peak: 

Mln . Peak Height: 

Mln . Peak Width: 

Smoothing Width: 

RT Window: 30 

ea 

f y Pa 

50 

1.00 

2 

Ves 

0.00 

0.00 

0 

0 

Area : 20377770 

Height : 3.35e+0C 

Star t Time: 16. 1 

15.0 15 5 16.0 165 

Tkne.mtn 

18.0 1B5 

Data printe d by STW 

Printin g Time: 12:13:00 PM 

Printin g Date : Tuesday, September 06, 2011 

Page 1 of 2 

Page 92 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS. and PFOS in Water Samples 

FSIA-June 2011 

*ETS-Kirk Results Name: kll0729b ext.rd b 

I

Sampla Nam*: "k110729t)044' Sample ID: •LCS-110726-13" File: •k110729b.wir 

Peak Name: "PFOS* Ms9s{*8); *499.00Q/99.000 D*,499.000/80.000 Da.499.00CV130.000 Da' 

Conunent "^p b LCS ECF~ Annotation:" 

1.98 I 

2.04 r 

7/31/2011 

8:22:25 AM 

Modified : 

Proc. Algorithm : 

Noise Percentage: 

Base. Sub. Window 

Peak-Split . Facto 

Report Largest Peak: ' 

Mln . Peak Height : i 

Mln . Peak Width : ( 

Smoothing Width : I 

RT Window: 30.0 

Expected RT: 16.: 

Use Relativ e RT: No 

;lfy Pa] 

50 

1.00 

, Type Mani. 

16. 1 

Area: 1464074 cc 

Height: 1.53e»005 

Star t Time: 15.8 

End Time: 16.3 

1.Se5 

1.4*5 

15*5 

1.2*5 

1.1*5 

iJOtS 

9.0e4 

8.0e4 

7.0e4 

6.0e4 

S,0*4 

I

San4)leName:K110729b055- Sampis ID:-GLP1(M>1-02-18-021 

Peak Nam*: 'PFOS' Ma>a(**): -499.000i99.000 Da,499.000/80.000 Da, 

Comment: "DAL GW 131R 0110622 (dll 1:100)" Annotation: -

Sample Index : 55 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Conc: 1530. ng/mL .--^ . 

1.20*6 

1.15*6 

' - " ^ ' " 1.10*6 

1.05*6 

1.00*6 

9.50*5-

nt s 9.00e5 

8.S0eS 

8.00*5 

7.50*5 

§- 7.00e5 

^ 6.S0e5 

I &00*S 

5.50*5 

5.00*5-

4.50*5 

4.00*5 

3.50*5 

3.00*5 

Z50*S 

Z00e5 

1.50*5 

l.OOeS 

5.00*4 

O.O0 

M10729b.*lfr 

,499.000/130.000 DaI

Sampl* Nam*:T<110729W>4r Sampl* ID: "LCS-110726-ie" Fil*: "k110729b.wir 

P*ak Nam*: 'PROS' Mas9(*s): '499,000/99.000 Da.499.000/80.000 Da.499.000/130.000 Da' 

Conunent '20ppb LCS EC r Arawtafion:" 

Sample Index: 47 

1.5*6 

1.4*6 

1.3*6 

l,2e6 

l.leS1,0 

Sample Type: 

Concentration: 

Calculated Conc: 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Noise Percentage 

QC 

19.8 

17.2 

7/31/2011 

9:25:45 AM 

Yes 

Specify Par 

50 

Base. Sub. Window: 1.00 

Peak-Split. Fact r: 2 

Report Largest Peak: Yes 

Mln. Peak Height 

Mln. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

0.00 

0.00 

0 

30.0 a 

16.2 m 

No 

ig/mL 

ng/mL 

min 

cps 

sec 

po 

,n 

Height: 

Star t Ti 

End Tim< 

.G6e*00e cps 

9.0*5-

8.0*5 

7.0*5 

6.0e5 

5.0e5 

4.0*5-

3.0*5 

2.0*5 

1.0*5 

0,0 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Noise Percentage 

7/31/2011 

12:14:44 P 

Yes 

Specify Pa 

50 

Base. Sub. Window: 1.00 

Peak-Split, Fact or: 2 

Report Largest Peak: Yes 

Min. Peak Height 

Mln. Peak Width: 

Smoothing Width: 

RT Window: 

E>:pected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

Area: 14 

Height: 

0.00 

0.00 

0 

30.0 

16.2 n 

No 

Manual 

16.0 n 

187265 CO 

,30e+006 

Data printe d by STW 

Printin g Time: 12:13:00 PM 

Printin g Date : Tuesday, September 06, 

Page 2 o f 2 

2011 

Page 93 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

*ETS-Kirk Results Name: kll0802a.rdb 

m 

1 

w 

CO 

< 

i 

CO 

c 

< 

27 J 

26-

25-

24-

23-

22-

2 1-

20-

19-

18-

17-

16-

15-

14-

13-

12-

11-

10-

9 

8-

7-

6-

5-

4-

3-

2 

1-

0-

12 14 

Analyte Gone. / IS Conc. 

Data printed by STW 

Printing Time: 12:14:09 PM 

Printing Date: Tuesday, September 06, 2011 

Page 1 of 1 

Page 94 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

*ETS-Kirk Results Name: kll0802a.rdb 

li|sampl*Nam*:'k110802a013- Sample ID:'11 003.2M- F^:-k110802a.«4r 

I Peak Nam*: '13C8PF0S-IS(IS)- Ma«s(*s): -S07.000ffl0.000 Da' 

• Commant: "0.1 ng/mL FC M in Synth. Wat*!* Annotatkin: ~ 

Sample Index : 14 

Sample Type: Standard , 8 20 

Concentration : 0.960 ng/mL 100*5 

Calculate d Conc: N/A 

Acq. Date: 8/2/2011 950«4 

Acq. Time: 7:35:09 PM 

Modified : NO ^"" ^ 

Proc. Algorithm : intelllQua n - IQA I I 

Mln. Peak Height : 0.00 cps 8.50*4 

Mln. Peak Width: 0.00 sec 

Smoothing Width : 0 point s 8.00*4 

RT Window: 30.0 sec 

Expected RT: 16.2 mln 7.50e4 

Use Relativ e RT: No 

7.00e4 

Int . Type: Valle y 

Retention Time: 16.2 mln 650*4 

Area: 626671 count s 

Height : l.OletOOS cp» g^ . 

Star t Time: 16.1 mln "•"*"* 

End Time: 16.4 min ^^ ^ 

f 5.00e4 

1 4.50e4 

4.00e4 

3.50e4 

3.00e4 

2.50e4 

2.00e4-

1.S0e4-

1.00e4-

5000.00 

14.0 14.5 1^.0 15.5 16.0 

L, i-''*'^^' 

16.5 17.0 17.5 18.0 16,5 

• Sample Mam*:T(110802a025" Sampl* ID:-LCS-110726-1" Fle:-k110802a.«ir 

I Peak Name: "13C8PFOS-IS{IS)- Maas^ea):-507.00are0.000 Da' 

I Comment •0.2ppb LCS" Annotatbn:" 

Sample Index : 26 

Sample Type: QC ia2 0 

Concentration : 0,953 ng/mL 115*5 

Calculate d Conc: N/A 

Acq. Date: B/2/2011 110*5 

Acq. Time: 11:48:15 PM 

1.05*5 

Modified : No 

Proc. Algorithm : IntelllQua n - IQA I I 1,00*5 

Min. Peak Height : 0.00 cps 

Mln. Peak Width : 0.00 sec 950*4 

Smoothing Width: 0 point s 

RT Window: 30.0 sec 9.00e4 

Expected RT: 16.2 mln „ 

use Relativ e RT: No '^•^°»* 

Int . Type: Valle y 8.00*4' 

Retention Time: 16.2 min TtOi,^ 

Area: 693975 count s 

Height: 1.16e+005 cpa 700*4-

Star t Time: 16.1 mln 

End Time: 16.4 mln „ 650e4. 

g ; 6.00*4. 

1 5.50*4-

5.00*4-

4.50*4-

4.00e4-

3.50e4 

3.00*4 

^50*4 

2.00*4 

1.50*4 

1.00*4-

5000.00-

14.0 14.5 15.0 15.5 16X) 

1 Tim* 

165 17,0 17.S 18.0 18.5 

m l n 

HsampUName:T.110S02a02r Sampte ID:'11 OOS-129- Fle:-k110802a.v>tr 

I PeaK Nam*:-13C8PFOaJS(IS)- Ma»(*s):'507.000/80.000 Da' 

• Comment "Method Btank" Annotatkin: " 

Sample Index: 24 

Sample Type: Unknown ,623 

Concentration : 0.960 ng/mL 

Calculate d Conc: N/A 

Ac;q. Date: 6/2/2011 1.4e5 

Acq. Time: 11:06:09 PM 

Modified : Yea 1.3e5 

Proc. Algorithm : IntelllQua n - IQA I I 

Mln. Peak Height: 0.00 cps 

Mln . PeaK Width: 0.00 sec 1.2e5 

Smoothing Width: 0 point s 

RT Window: 30.0 sec 

Expected RT: 16.2 mln LloS 

Use Relativ e RT: No 

Int . Type: Valle y I.OeS 

Retentio n Time: 16.2 mln 

Area: 957170 counts 

Height : 1.47e-l-005 cps H-°«^ 

Star t Time: 16.1 mln 

End Time: 16.5 mln « 

1 8.0e4 

1 ^-0 ^ 

£ 

6.0*4 

5.0*4 

4.0*4 

3.0*4 

2.0e4^ 

1.0e4-

14.0 14.5 15.0 15.5 16.0 16.5 17.0 17.5 18.0 18.5 1 

• Sampl*Name:1(110802a028' Sample ID:TCS-11072fr4- Fle:1<110802a.wlfr 

• Peak Name: '13C8PFOS-IS{1S)' Mas9(es): "507.000/80,000 Da' 

• Comment '2ppb LCS* Annotatton:" 

Sample Index: 29 

Sample Type: QC ,6, 0 

Concentration : 0.953 ng/mL 

Calculate d Conc: N/A 1.15*5 

Acq. Date: 8/3/2011 

Acq. Time: 12:51:45 AM l.lOeS 

Modified : No ^^^ ^ 

Ptoc. Algorithm : IntelllQaa n - IQA I I 1 nn.s 

Mln . Peak Height: 0.00 cps ''" " 

Mln . Peak Width : 0.00 sec 9 50*4 

Smoothing Width: 0 point s 

RT Window: 30.0 sec 900*4-

Expected RT: 16.2 mln 

Use Relativ e RT: No 8.S0e4-

Int . Type: Valle y 8.O0e4-

Retentio n Time,: 16.2 mln 

Area: 742792 counts 7.S0e4-

Height: l.iee+00 5 cps 

Star t Time: 16.1 mln (.u« t 

End Time: 16.4 mln g_ ^^^ . 

1 5.50*4 

S.00e4-

4.S0e4-

4.00e4-

3.S0e4 

3.00e4 

2.50e4 

Z0ae4 

1.50e4 

1.00e4-

5000.00-

14.0 14.5 15.0 15.5 16,0 

L 

16.S 17.0 17.5 18.C 

Time, mm 

18.5 

Data printed by STW 

Printing Time: 12:15:38 PM 

Printing Date: Tuesday, September 06, 2011 

Page 1 of 5 

Page 95 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS. PFHS. and PFOS in Water Samples 

FSIA-June 2011 

*ETS-Kirk Results Name: kll0802a.rd b 

1

Sanv)t*Name:-k1108O28O3r Sampl*lD:'LCS-110726-r Fl*:1(110802a.w(ir 

P*ak Nam*: '13C8PFOS-IS(IS)' Mas9(c«): '507,000/80.000 Da* 

Commerd: '20ppb LCS" Annotation: ~ 

Sample Index : 32 

Sample Type: • QC 

Concentratio 

Calculated C 

Acq. Date: 

Acq, Time: 

Modified: 

Proc. Algori 

Mln. Peak He 

hm 

qh 

Mln. Peak Width 

Smoothing Wl 

RT Window: 

Expected RT: 

Use Relative 

Int. Type: 

Retention Tl 

Area: 

Height: 

Start Time: 

End Time: 

RT 

0.953 

N/A 

e/3/201] 

1:54:58 

No 

n g / 

AM 

IntelllQuan -

! 0.00 

0.00 

0 

30.0 

16.2 

Ho 

Valley 

16.2 

9S8423 c 

1.59e-f005 

16.1 

16.4 

point 

mln 

mln 

ountB 

c p s 

mln 

mln 

I

SampleName:'k110802a041" Sample ID:*LCS-110726-13- Fie: "kit 0602a. wi r 

Peak Nam*; -13C8PFOS-IS(IS}' MBSS<*S): "507.000/60.000 Da' 

Common!: "2ppb LCS ECF" Annotatton:"" 

Sample Index: 42 

Sample Type: QC 

0.954 ng/mL 

I

SampleName:'k11O802a044" Sampl* ID:'LCS-110726-16^ ^ile:'kl10802a.wir 

P*ak Nam*: '13C8PFOS-IS(IS}' Mess(«s}: ''507.000re0.000 Da' 

Comment'20ppb LCS EC r AnnoUtton:" 

Sample Index: 45 

Calculated Conc: N/A 

Acq. Date: 8/3/2011 

Acq. Time: 5:26:11 AM 

Modified: Yes 

Proc. Algorithm: IntelllQuan - IQA II 

Mln. Peak Height; 0.00 

Min. Peak Width: 0.00 

Smoothing Width: 0 

RT Window: 30.0 

Expected RT: 16.2 

Use Relative RT: No 

Int. Type: Valley 

Retention Time: 16.2 

Area: 639828 c 

Height: 1.08et005 

Start Time: 16.1 

End Time: 16-4 

cp s 

points 

min 

mln 

c p s 

mln 

mln i 

1.0S*S 

9.50e4 

0.00e'-

8.50*'-

8.00*'-

7.50*4-

7.00*--

6.S0e'-

6.00e4-

5.50e4-

5.00e4-

4.S0e4: 

4.00e4: 

3.S0e4^ 

3.00*4 

2,50*4 

2,00*4 

1.50e4 

1.00e4-i 

5000.00-i 

0.00^ 

Sample Type; 

Concentration: 

Calculated Conc: 

Ac;q. Date: 

Acq. Tlma: 

Modified: 

Proc. Algorithm: 

Mln. Peak Height 

Mln. Peak Width: 

Smoothing Width: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

OC 

0.953 

N/A 

B/3/2011 

6:29:30 AM 

Yes 

IntelllQua 

0.00 

0.00 

30.0 s 

16.2 n 

No 

Base To Bas 

16.2 n 

Area: 699327 cour 

Height: 

Start Time: 

,14e+005 t 

16,1 n 

15.5 16.0 16.5 

I.IOeS 

1.05*5 

1.00*5 

S.50*4 

S.00*4-

6.50e4< 

8.00e4< 

7.50e4-

7.00*4-

6.50*4-

'{ 6.00*4 

I 5.50*4' 

= 5.00*4-

4.50*4-

4.00*4-

3,50*4-

3.00*4-

2.50*4-

2.00e4-

1.50*4-

1.00*4-

5000.00-

0.00-

Data printe d by STW 

Printin g Time: 12:15:38 PM 

Printin g Date: Tuesday, September 06, 

Page 2 of 5 

Page 96 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

*ETS-Kirk Results Name: kll0802a.rd b 

Modified: 

Proc. Algorithm: 

Mln. Peak Height 

Mln. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Ye» 

IntelllQuan 

0.00 c 

0.00 3 

0 po 

30.0 s 

16.2 m 

Saii^Nam*:'k110602a07r Sampl* ID: "GLP10O1-0M6-133' File:"kl10802a.wlT 

P*sk Nam*: "13C8PFOSJS(IS^ Ma33{*s): •507.000re0.000 Da' 

Commant "DAL GW130L RB110630" Annotatton:-

Sample Index: 73 

Sample Type: Unknown 

Concentration : 0.96 0 ng/mL 

Calculate d Conc: N/A 

Acq- Date: 8/3/2011 2,0*5-

Acq. Time: 4:21:05 PM 

1.9e5-

I I 1.8*5-

1.7*5-

1.6*5-

1.5*5-

1.4*5-

1.3eS1.2e5-

k l.leS 

I 

9.0e4-

8.0e4-

7.0e4-

6.0e4-

5.0e4-

4.0e4-

3.0e4-

2.0e4-

1.0e4-

Helght : 

Star t Tlmi 

End Time: 

0.0 

14.0 14.5 

Sampt* Name:-1(11O8O2B013- Sample ID:'11 00^25-5" Rle;"kl10802a.wtir 

Paak Nam*: "PFOS" Mass(*s): "499.000/99.000 Da,499,000/80.000 Da,499.00CV130.000 Da' 

ComnMnt: T).1 ng/mL FC std in Syntt). Water" Annotatton:"" 

Sample Index: 14 

Standard 

0.100 nq/mL 

0.0965 ng/mL 1.25*4-

1.20*4 

1.1S*4-

s - MQ II I 1.10*4 

1.05*4 

1.00*4 

95oaoo 

nts 9000.00 

8soaoo 

8000.00 

75oaoo 

S. 7000.00 

^6500.0 0 

I 6000.00 

~ 5500.00 

5000.00 

4500,00 

4000,00 

3500.00 

3000.00 

2500,00' 

2000.00 

isoaoo 

1000.00' 

5oaoo 

0.00-

I

Sampl* Name: "k1108CCa073' Sampla ID: "GLP1IW)1-02-18-134" File: "k110802a.wir 

Peak Name: "13C8PFOS4S(IS}' Mas3<ea); -507.000/80.000 Da" 

Comm*nt'OALGW133SRB11063ff' Annotatton:' 

Sample Index: 74 

Sample Type: Unknown 

0.96 0 ng/mL 

N/A 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algor: 

Mln. Peak He 

thm: 

ight; 

Min. Peak Width: 

Smoothing W 

RT Window: 

Expected RT 

Uss Relative 

Int. TiT.e: 

Retention T: 

Area: 

Height: 

RT: 

128 

2 

8/3/2011 

:42:16 PM 

Yes 

ntBlllQ 

0.00 

0.00 

0 

30.0 

16.2 

No 

Valley 

16.1 

341 C 

12«-t005 

an 

ml 

ml 

cp 

2,1*5 

Z0e5 

1.9e5 

1.8e5-

1.7*5 

1.6*5 

1.5e5-

1.4*5 

1.3*5 

1.2*5 

1.1*5 

1.0*5< 

9.0*4-

8.0*4-

7.0*4-

6.0*4-

5.0*4-

4.0e4-

3.0e4-

2.0e4< 

1.0e4-

0.0-

14.0 14.5 

SanvileName:*k110802s02r Samp4elD:'11 005-129" Flle:-kl10802a.wtr 

Peak Name: 'PFOS- Mass<*s); '499.000/99,000 Oa,499.000/80.000 Da.499.000/130.000 DaComment -Mettwd BtanlT Annotatton:"" 

Sample Index : 24 

Sampl e Type : Unknown 

Concentration : N/A 

16.0 16.5 17.0 

Tlme.min 

17.5 18.0 18.5 

Sample Type : 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algor 

Holse Perce 

thm: 

Base. Sub. Windo 

Peak-Split. 

Report Larg 

Fact 

St P 

Min. Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT 

Use Relative RT: 

Int. Type: 

Retention T 

Height: 

Start Time: 

End Time: 

a/2/2011 

7:35:09 PM 

No 

Specify Pa 

50 

J: 1.00 

ak: Yes 

0.00 

0.00 

0 

30.0 a 

16.3 n 

No 

Valley 

16.2 n 

7724 2 cour 

.30e-f004 c 

16.1 n 

16.3 a 

••^i^..^ » thili*«l<ii*^H^*««|iM<> 

Calculated Conc: 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Holse Percentage 

< 0 

8/2/2011 

11:06:09 PM 

Yes 

Specify Par 

50 

Base. Sub. Window: 1.00 

Peak-Split. Facte 

Report Largest Pe 

Mln. Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

t: 2 

ak: Yes 

0.00 

0.00 

0 

30.0 3 

16.3 m 

No 

Manual 

16.2 m 

Area: 16450 coun 

Height: 2 

Start Time: 

End Time: 

.16e•^003 cp 

16.0 m 

16.3 m 

16.0 16.5 

Tim*, mln 

16.0 16.5 

Time, mk) 

Data printe d by STW 

Printin g Time: 12:15:39 PM 

Printin g Date : Tuesday, September 06, 

Page 3 of 5 

Page 97 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

•ETS-Kirk Results Name: kll0802a.rd b 

|||SamplaNam.:-K110e02a025' Samp). ID:"LCS-11072ft-r Fie:-k110802a.»lir 

I Peak Nam*: -PFOS" Ma9s(*«): '499.OOCW9.000 Da,499.000ffl0.000 Da,499.000/130.000 Da' 

• Commant: "0.2ppb LCS" Annotatton: " 

Sample Index : 26 

1 Sample Type: QC 

Concentration : 0.199 ng/mL 

Calculate d Conc: 0.219 ng/mL 

Acq. Date: 8/2/2011 Z8*4 

Acq. Time: 11:48:18 PM 

Modified : No 2.6*4 

Proc, Algorithm : Specif y Parameters - MO II I 

Noise Percentage: 50 

Base. Sub. Window: i.OO min 2.4e4 

Peak-Split . Factor: 2 

Report Largest Peak: Yes 

Min. Peak Height: 0.00 cps 2.2*4 

Mln . Peak Width: 0.00 sec 

Smoothing Width: 0 point s 

RT Window: 30.0 sec 2.0*4 

Expected RT: 16.3 mln 

Use Relativ e RT: No 

Int . Type: Valle y 

Retention Time: 16-2 mln . 

Area: 179532 counts fr '*" * 

Height: 2.93e4'004 cps ^ 

Star t Time: 16.1 mln %.... . 

End Time: ' 16.3 mln | '- ^ 

~ 1,2*4 

1.0*4 

6000.0 

6000.0 

4000.0 

2000.0 

14.0 14.5 15.0 

1 SampleName:-k110802a03r Sample ID:-LCS-110726->* »'i*:i(110802a.vrin" 

1 Peak Name: 'PFOS' Mass<e8}: "499.OOCV99.000 Da.499.000/80.000 Da.499.00tV130.000 Da" 

1 Comment: "20ppb LCS" Annotatton: -

Sample Index : 32 

Sample Typ.e: QC 

Concentration : 19.9 ng/mL 

Calculate d Conc: 21.1 ng/mL 3.4*6 

Acq. Date: 8/3/2011 

Acq. Time: 1:54:5B AM g^jee 

Modified : No 

Proc. Algorithm : Specif y Parameters - MQ H I 3.0e6 

Noise Percentage: 50 

Base. Sub. Window: 1.00 min -.8*6 

Peak-Split . Factor: 2 

Report Largest Peak: Yes 

Min . Peak Height: 0-00 cps 2.6*6-

Mln. Peak Width: 0.00 sec 

Smoothing Width: 0 point s 2.4*6 

RT Window: 30.0 aec 

Expected RT: 16.3 mln 

Use Relativ e RT: No 2,2*6-

Int . Type: Valle y -Q^ . 

Retention Time: 16.2 min - *•'"" 

Area: 22570284 counts gHeight: 3.49e-f0O6 cps ^ 1,e«6-

Start Time: 16. 1 mln % 

End Time: 16.5 mln £ ^g^ . 

1.4*6 

1.2*6 

1.0*6-

8.0*5 

6.0*5-

4.0*5-

Z0*5-

0.0 ' • • 1 1 • • < 

14.0 14,5 15.0 

16.19 

1 .,1656 

1 .1 

ll/t"'' ' 

15.5 16.0 16.5 17.0 175 18.0 185 

16.18 

I 

155 16.0 165 17.0 17.5 18.0 185 

1 P*ak Nam*: "PFOS" Ma«9(*s): "499.000/99.000 Da,499.DOO/80.000 Da.499.000/130.000 Da" 

• Commant-2ppb LCS" Annotatton:-

Sample Index: 29 

Sample Type: <y: 

Concentration : 1.99 ng/mL 

Calculate d Conc: 2.15 ng/mL ,7 5 

Acq. Pate: 6/3/2011 * 

Acq. Time: 12:51:45 AM 2.6*5 

Modified : No ^^ ^ 

Proc. Algorithm : Specif y Parameters - MQ II I 2.4*5 

Kol«e Percentage: 50 

Base. Sub. Window: 1.00 min 2.3*5 

Peak-Split . Factor: 2 2.2*5 

Report Largest Peak: Yes 

Min. Peak Height : 0.00 cps 2.1*5 

Min . Poah Width : 0.00 sec 2.0*5 

Smoothing Width: 0 point s 

RT Window: 30.0 sec 1.9*5 

Expected RT: 16.3 min , g^g 

Use Relativ e RT: No 

1.7*5 

Int . Type: Valle y 

Retention Time; 16.2 mln « '•°" ' 

Area: 1769247 counts §• 1.5*5 

Height: 2.80e-t005 cps ^ 

Star t Time: 16.1 mln 'S '•* = 

End Time: 16.4 min | l.JeS 

1,2*5 

1.1*5 

1.0*5 

g.te4 

8.0*4 

7.0e4 

6,0*4 

5,0*4 

4,0*4 

3.0*4 

2,0*4 

1.0*4 

14.0 145 15.0 

1 Sampl* Nam*: "kll0802a03(r Sampl* ID:'LCS-110726-10" |:|le:'k1l6802a,wtfr 

I Peak Name: "PFOS- Haea(es): "499.000/99.000 Da,499.000fflO.OOODa,499.00a/130,000 Da" 

• Comment "0.2ppb LCS ECP Annotatton:" 

Sample Index: 39 

Sample Type: QC 

Concentration : 0.198 ng/mL 

Calculate d Conc: 0.252 na/mL 

Acq. Date: 8/3/2011 '-^" ^ 

Acq. Time: 4:22:49 AM 

1.7e4 

Modified : Yes 

Proc. Algorithm : Specif y Parameters - MQ II I . yj^ ^ 

Noise Percentage: 50 

Base. Sub. Window: 1.00 mln 

Peak-Split . Factor: 2 '•'• * 

Report Largest Peak: Yes 

Mln . Peak Height : 0.00 cps 1.4*4-

Kin . Peak Width : 0.00 sec 

Smoothing Width: 0 point s 13,4 . 

RT Window: 30.0 sec 

Expected RT: 16.3 mln , . , 

Use Relativ e RT: No ^^ ^ 

Int . Type: Manual 1.1*4-

Retention Time: 16.2 mln _ 

Area: 184609 counts % 10*4-

Height : 1.86e-f004 cps ^ 

Star t Time: 15.8 min 1 TM«n . 

End Time: 16.3 mln | «»°- ° 

8000,0 

7000.0-

6000,0' 

S000.0-

4000.0-

3000.0-

2000.0-

1000.0-

14.0 145 15.0 

16,21 

_f 155 16.0 165 17.0 175 

Tlm*.mln 

16.17 

16.04., 1 

^• H 16.51 

^ B ,Ll657 

• 1 

18.0 185 

,.,,^,.iMl^^^ l \|fcifiYi^i^iitf^')'tiiW'^*^*it^iinht>j^i 1 1 

155 16.0 165 17.0 175 18.0 185 

Data printe d by STW 

Printin g Time: 12:15:39 PM 

Printin g Date: Tuesday, September 06, 2011 

Page 4 of 5 

Page 98 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS. and PFOS in Water Samples 

FSIA-June 2011 

*ETS-Kirk Results Name: kll0802a.rdb 

I

Sample Name: 1(1106028041* Sample ID: -LCS-110726-ir FUe: 'kll0802a.Mir 

Peak Name: 'PFOS' Mas3<e*): -499.OOCV99.000 Da,499.00Q/80XX)0 Oa.499,000^130.000 Da' 

Comment: *2ppb LCS ECF* Annotation: ~ 

Sample Index : 42 

Sample Type : QC 

Concentration : 1.98 ng/mL 

Calculate d Conc : 2.2 9 ng/mL 

Acq. Date : 8/3/201 1 

Acq. Time : 5:26:1 1 AM 

Per< 

Window: 

Peak-Split . Factor : 

Report Largest Pea)i 

Min. Peak Height : 

Min . Peak Width : 

Smoothing Width: 

RT Window: 

rlthm: Specif y Pat; 

ntage i 

1.7e5 

1.6*5 

1.5*5 

1.4eS 

1.3e5 

1.2e5 

1.1*5 

1.0*5 

6.0*4 

5.0*4 

14.0 145 15.0 15 5 16.0 16 5 17,0 17 5 18.0 18 5 

I

Sample Name:-1(110802*072' Sample ID;-GLP1(U>l-02-18-133" File: 1(110802a.wir 

Peak Nam*: 'PFOS' Ma3s(es): '499.00099.000 Oa,499.000/80.000 Da.499.000/130.000 DaComment: "DAL GW130LRB 110630" Annotatlon:-

I

Sampl*Nam*:-V110802a044- Sampl*ID:'LCS-110726-16- Fil*:'k110802a,wHr 

Peak Name: 'PFOS^ Maa3(*a}: '499.000/99.000 D8,499.000/80iXX) Da.499.00Q/130.000 Oa' 

Comnwnt '20ppb LCS ECF" Annotation; ~ 

19. 8 r 

23. 0 r 

8/3/201 1 

6:29:3 0 AM 

Modified : 

Proc . Algorithm: 

Nois e Percentag ' 

Base . Sub . Kindi 

Peak-Split . Factor: 2 

Report Largest Peak: Y 

Min. Peak Height : 0 

Min. Peak Width : 0 

Smoothing Width : 0 

RT Window: 30. 0 

Expecte d RT: 16. 3 

Specif y Parameter! 

50 

-: 1.00 min 

• RT: 

Int. Type: 

Retention T 

Height: 

Start Time: 

End Time: 

15.0 15 5 16.0 16 5 17.0 17 5 18.0 185 

Sample Type: Unki 

(

SampleName:*k110a02a073' Sampl*ID:'GLPl001-02-11 

P*ak Name: 'PFOS' Maa3{*a): '499.000/99.000 Da.499.0r 

Comment: "DAL GW133S RB 11063ff' Annotatkin: "" 

Sample Index : 74 

N/R 

Acq. Date : 

Acq. Time : 

Modified : 

Proc . Algo r 

Nois e Perc e 

thm: 

8/3/201 1 

4:21:0 5 PM 

Yes 

Specif y Pa 

50 

Base . Sub . window: 1.00 

Peak-Split . Factor : 2 

Report Largest Peak: Yes 

Mln. Peak H« igh t 

Mln. Peak Width : 

Smoothing Width: 

RT Window: 

Expecte d RT 

Use Relativ e 

int . Type : 

Retentio n T 

Area : 

Height : 

Star t Time: 

End Time : 

RT: 

0.0 0 

0.0 0 

0 

30. 0 

16. 3 n 

No 

Manual 

16. 2 1 

7067 cou 

.200*003 c 

15. 9 1 

16. 2 n 

Sample Type : 

Concentration : 

Calculate d Conc : 

Acq. Time : 

Modified : 

Proc . Algorithm : 

Base . Sub. Windo 

Unknown 

N/A 

0.047 8 

e/3/201 1 

4:42:1 6 PM 

Yes 

Specif y Pa 

50 

: 1.00 

Peak-Split . Factor : 2 

Report Largest P 

Mln. Peak Heigh t 

Mln. Peak Width : 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

Atea : 

Height : 

Star t Time : 

End Time : 

a k : Yes 

0.0 0 

0.0 0 

0 

30. 0 3 

16. 3 n 

No 

Manual 

16. 1 R 

9847 cour 

.08e+004 c 

15. 9 : 

16. 3 It 

• ts - MQ II I 

1.05e4 

1.00e4 

9500.00 

9000.M; 

8500.00-

8000.00-

7500.00 

7000.00 

650a00 

| . 6000,00 

^5500.00 -

I sooaoo^ 

45oaoo 

4000.00; 

3500.00-

3000.00-

2500.00-

2000.00 

1500.00 

1000.00 

500.00-

0.00 ii4"f L^m^ifaiartiKijIIJii^i 

Data printed by STW 

Printing Time: 12:15:39 PM 

Printing Date: Tuesday, September 06, 

Page 5 of 5 

2011 

Page 99 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

ATTACHMENT C: ANALYTICAL METHOD 

Page 100 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA'- June 2011 

Mettiod 

Mettiod 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 *^ I n f o "} 

Approved By: 

^/^j/a y 

William K. Reagen, Laboratory Manager Date 

ETS-8-044.0 Page 1 of 11 

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

Injection Analysis Pagel0lofll3 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA - June 2011 

1 Scope and Application 

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

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

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

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

and Perfluorooctanesulfonate (PFOS) by High Perfonnance 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 Method 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 detemnined 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 Blank (FB)/Trip Blank 

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. 

ETS-8-044.0 Page 2 of 11 

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

Injection Analysis 

Page 102 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

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 detemnine 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 determine 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 detemiine whether the sample 

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

sample matrix must be determined in a separate aliquot and the measured values in the LMS corrected 

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

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. 

ETS-8-044.0 Page 3 of 11 

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

Injection Analysis 

Page 103 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA - June 2011 

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 determine 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 surrogate compound is typically a target analyte with at least one atom 

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

control samples. Sun'ogate(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 determined; 

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 woric 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 familiar with the laboratory equipment and potential hazards including, but not limited 

to, the use of solvents, pressurized gas and solvent lines, high voltage, and vacuum systems. Refer to the 

appropriate equipment procedure or operator manual for additional infonnation 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. 

ETS-8-044.0 Page 4 of 11 

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

Injection Analysis 

Page 104 of 113 
GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

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 perfonnance 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, 50|JL, lOOpL, 250|jL, 500^JL, lOOOpL. 

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 Chromatographic System 

Guard Column: Prism RP, 4.6 mm x 50 mm, 5 pm 

Analytical Column: Betasil CI 8,4.6 mm x 100 mm, 5 ijm 

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 pL 

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. 

ETS-8-044.0 Page 5 of 11 

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

Injection Analysis 

Page 105 of 113 
GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

6.3 MS/MS System 

6.3.1 Mode: Electrospray Negative on, 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 

Perfluorohexanoic Acid (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-CIO 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 

Perfluorooctanesulfonate (PFOS - C8 sulfonate); 3M 

ETS-8-044.0 Page 6 of 11 

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

Analysis 

Page 106 of 113 
GLP10-01-Q2; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

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: Alternative 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, pL 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 correction is given below for PFOS. 

^. , . molecular weight of anion 

salt correction factor = = 

moclecular weight of salt 

4Qd PFOS (K-^ )salt correction factor = ^^ ^ = 0.9275 

538 

10 mg CsFiySOs'K* with purity 90% = 8.35mg C8F17SO3" (10 mg*0.90*0.9275=8.35 mg) 

5 |jg/mL (5000 ng/mL) mixed working standard—Add 0.5mL each of the lOOpg/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 pg/mL -mixed wori<ing standard solution to a 25mL 

volumetric flask and bring up to volume with solvent. 

125 ng/mL mixed standard—Add 625pL of the 5 pg/mL-mixed woricing standard solution to a 25mL volumetric 

flask and bring up to volume with solvent. 

Storage Conditions—Store all SSSs and wori<ing standards in accordance with laboratory standard operating 

procedure or in a refrigerator at 4°±2°C for a maximum period of 6 months from the date of preparation. 

ETS-8-044.0 Page 7 of 11 

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

Analysis 

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GLP10-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

7.5 Calibration Standards 

Using the worthing 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 woridng 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, fd. 

10 

15 

20 

30 

20 

50 

100 

200 

25 

50 

100 

Final Volume of 

Calibration Standard (mL 

of ASTM Type 1 Water, or 

other suitable water) 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

Final Concentration of 

Calibration Standard, ng/mL 

(ppb) in ASnH 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 

preferred over the use of glass autovials, to prevent the possibly of fluorochemical 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^ -H 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 from the calibration curves to provide a better fit over the range 

appropriate to the data or because they did not meet the pre-detemnined 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 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 

ETS-8-044.0 Page 8 of 11 

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Analysis 

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Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

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, perfomn 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 constnjct 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 firom a single 

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

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

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 detennine 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 relafive percent difference, RPD, should be reported. RPD 

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

replicates excludes field blanks. 

10.4 Surrogate Spikes 

Surrogate 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. 

ETS-8-044.0 Page 9 of 11 

Method of Analysis for the Detennination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection 

Analysis 

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Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

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 fiagged as such (with expanded 

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

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

endogenous level to be used without justification to detennine 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: 

. ,^ , ., , ,, (Peak Area-Intercept) ^ ^ 

Analyte found (ng/mL) = -^^ ^-^ x DF 

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 perfonnance parameters that are not achieved must be considered in the evaluation of the data. 

Nonconfomnance 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 perfomnance section are not met, maintenance may be perfonned on the system and 

samples reanalyzed, or other actions taken as appropriate. Document all actions in the raw data. 

If data are to be reported when perfomnance 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 

mn 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 S5% and a retention time RSD of <2% to be compliant. 

12.2 Quantitation 

Calibration Curve: The coefficient of detenninafion (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 Perfonnance: 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 meefing these criteria must be reanalyzed. 

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Analysis 

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Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

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 Accuracy 

This method and required quality control samples are designed to generate data that are accurate to +1-30%. 

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

13 Pollution Prevention and Waste Management 

Waste generated when perfomning 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 infonnation for reconstruction of the data. 

Infonnation for the data package must include, but is not limited to the following items: study or project number, 

sample and standard prep sheets/records, instmment run log (instrument batch records, instrument acquisition 

method, summary pages), instmment results files, chromatograms, calibrafion curves, and data calculations. 

15 Affected Documents 

None. 

16 Revisions 

Revision 

Number Summary of Changes 

ETS-8-044.0 Page 11 of 11 

Method of Analysis for the Detennination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection 

Analysis 

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GLPIO-01-02; Interim Report 18 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

FSIA-June 2011 

ATTACHMENT D: DEVIATION(S) 

Page 112 of 113 
GLPIO-01-02; Interim Report 18 

RECORD OF DEVIATI0N/N0N^e^r6iMtV"^'TM'?sr;uSi ? 

/. Identification 

study / Project No. 

GLP10-01-02-18 

Date(s) of Occurrence: 

kll0729b, l<110802a 

Document Number: 

ETS-8-044.0 

Deviation type • SOP D Equipment Procedure 0 Metliod 

(Check one) D Protocol D GPO n Other: 

//• Descriptio n (attach extra pages as needed) 

Method Requirements: 

1. LCS average recoveries wntiiin ±20% (section 10.5). 

2. FIVIS recovery within ±30% (section 10.6). 

3. RPD within ±20% (section 10.3). 

4. System suitability peak area RSD S5% and retention time RSD <2%>. 

Actual procedure/process: 

1. I<110729b (internal calibration): The low set of PFOS ECF LCS sannples had an average recovery of 136% 

and the high set of ECF LCS samples had an average recovery of 122%. I<110802a: The low, mid, and 

high PFOS ECF LCS samples had average recoveries of 129%, 122%, and 122%. 

2. The following samples had FMS recoveries less than 70% for PFOS: 130L, 131L, 135L, 136L, 141R, 

142R, and 1443. Samples 133L and 135S had FMS samples greater than 150% for PFOS. 

3. Sample 134L had an RPD of 22% for PFOS. 

4. k110729b (external calibration): The peak area RSD for PFOS was 9.3%. 

///. Actions Taken 

(such as amendment issued, SOP revision, etc.) 

Corrective Action (D Yes IZI No) Reference: 

Acceptability of the nonconforming work: 

1. The recoveries for the non-compliant LCSs (linear + branched) will be flagged in the final report. AN of the 

LCSs prepared with this study were evaluated by ETS-12-012 to determine the method analytical 

uncertainty. The analytical uncertainty when evaluated by ETS-12-012 was determined to be ±28% for 

PFOS. However, the analytical uncertainty for this study will be set at ±36%, based on the recovery of the 

low set of linear + branched LCS from run kl l 0729b. 

2. The non-compliant FMS recoveries for PFOS vAW be flagged in the final report. If necessary, the method 

uncertainty will be expanded for samples with FMS recovery less than 64%. Samples 133L and 1353 will 

not be reported for PFOS due to the FMS recoveries being outside the £50% acceptance criteria. 

3. The PFOS RPD for sample 134L will be flagged in the final report. 

4. Other QC items were used to assess data accuracy for PFOS - calibration curve point accuracy, curve fit 

criteria, CCVs, and LCS, all meeting method acceptance criteria. 

Actions: D Halting of Work D Client Notification D Work Recall D Withholding of Report 

0 Other: Deviations will be noted in final report. 

Project Lead/PAI Approval: "'%- In 

Study Director (if GLP): Date: 

Sponsor Approval (for Q>VP protocol deviations): NA Date: 

Technical Reviewer (optional): NA Date: NA 

Laboratory Department,Manager Approval: Date: 

IV. Authorization to Resume Work 

Where halting of work occurred, resumption of work must first be approved by Laboratory Management 

Laboratory Department Manager Approval: NA Date: NA 

Deviation No. 

(assigned by Study Director or Team Leader at the end of study or project) 

ETS-4-008.7 Page 1 of 1 

Documentation of Deviations and Control of Nonconforming Testing 

Page 113of 113