GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

GLP10-01-02: Interim Report 17 - Analysis of PFBS. PFHS. and PFOS in 

Groundwater Samples Collected from Decatur. AL. 1^* Quarter 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 

GLP10-01-02-17 

Total Number of Pages 

98 

The testing reported herein meet the requirements of ISO/IEC 17025-200S "General Requirements for the 

Competence of Testing and Calibration L^lx>ratories", In accordance with the A2I^ Certificate #2052.01. 

Testing that complies with this International Standard also operate In accordance with ISO 9001:2000. 

Testing Cert #2052.01 

Page 1 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

This page has been reserved for specific country requirements. 

Page 2 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

GLP CoiviPLiANCE STATEMENT 

Report Title: Interim Report 17 Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Collected from Decatur, AL, 1^ Quarter 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. 

"S 

Gary Hohenstein, Sfconsor Representative Date 

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

Page 3 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

QUALITY ASSURANCE STATEMENT 

Report Title: Interim Report 17 Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Collected from Decatur, AL, 1^' Quarter 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 

6/15/2011-6/29/2011 

Phase 

Data / Interim Report 

Date Reported to 

Testing Facility 

lUlanagement 

7/16/2011 

Study Director 

7/14/2011 

~?-^^'^ ^ 

QAU Represertstive Date 

Page 4 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

TABLE OF CONTENTS 

GLP Compliance statement 3 

Quality Assurance Statement 4 

Table of Contents 5 

List of Tables 6 

1 Study Information 8 

2 Summary 9 

3 Introduction 11 

4 Test & Control Substances 11 

5 Reference Substances 12 

6 Test System 13 

7 Method Summary 14 

7.1 Methods 14 

7.2 Sample Collection 14 

7.3 Sample Preparation 14 

7.4 Analysis 14 

8 Analytical Results 16 

8.1 Calibration 16 

8.2 System Suitability 17 

8.3 Limit of Quantitation (LOQ) 17 

8.4 Continuing Calibration 17 

8.5 Blanks 17 

8.6 Lab Control Spikes (LCSs) 18 

8.7 Analytical Method Uncertainty 22 

8.8 Laboratory Matrix Spikes (LMS) 22 

8.9 Field Matrix Spikes (FMS) 22 

Page 5 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

9 Data Summary and Discussion 23 

10 Conclusion '. 36 

11 Data/Sample Retention 36 

12 Attachments 36 

13 Signatures 37 

LIST OF TABLES 

Table 1. Summarized PFBS, PFHS, and PFOS Results (Decatur Groundwater-01 2011). ...10 

Table 2. Instmment Parameters 15 

Table 3. Liquid Chromatography Conditions 15 

Table 4. Mass Transitions 16 

Table 5. Limit of Quantitation (LOQ) 17 

Table 6. Laboratory Control Spike Recovery ..19 

Table 7. Analytical Uncertainty 22 

Table 8. Field Matrix Spikes 23 

Table 9. GW203LQ1 Y11 LF 25 

Table 10. GW 220R Q1 Y11 LF 25 

Table 11. GW220LQ1 Y11 LF 26 

Table 12. GW222RQ1 Y11 LF 26 

Table 13. GW227RQ1 Y11 LF 27 

Table 14. GW227LQ1 Y11 LF 27 

Table 15. GW 310R 01 Y11 CP 28 

Table 16. GW312RQ1 Y11 CP 28 

Table 17. GW317LQ1 Y11 CP 29 

Table 18. GW 324L 01 Y11 CP 29 

Table 19. GW 327R 01 Y11 CP 30 

Table 20. GW 328R 01 Y11 CP 30 

Page 6 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

Table 21. GW328LQ1 Y11 CP 31 

Table 22. GW330RQ1 Y11 CP 31 

Table 23. GW330LO1 Y11 32 

Table 24. GW331S01 Y11 32 

Table 25. GW 335S 01 Y11 CP 33 

Table 26. GWGRS04Q1 Y11 CP 33 

Table27. Trip Blank 1 34 

Table 28. Trip Blank 2 34 

Table 29. GLP10-01-02-17 Equipment Rinseate Blank 35 

Table 30. GLP10-01-02-15 Soil Equipment Rinseate Blanks 35 

Page 7 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

i 1 Study Information 

Sponsor 

3M Company 

Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

Study Director 

Jaisimha Kesari, P.E., DEE 

Weston Solutions, Inc. 

Westchester, PA 19380 

Phone:(610)701-3761 

Fax:(610)701-7401 

j.kesari@westonsolutions.com 

Study Location 

Testing Facility 

3M EHS Operations 

3M Environmental Laboratory 

Building 260-5N-17 

St. Paul, MN 55144 

Study Personnel 

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

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

Susan Wolf, 3M Analyst 

Chelsie Grochow; analyst 

Jonathan Steege; analyst 

Study Dates 

Study Initiation: March 8,2010 

Interim 17 Experimental Termination: May 18, 2011 

Interim Report Completion: Date of Interim Report Signing 

Location of Archives 

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

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

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

Page 8 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1 St Quarter Sampling - 2011 

2 Summar y 

The 3M Environmental Laboratory received groundwater samples from wells located in Decatur, AL, 

representing eighteen (18) different sampling locations collected March 23 - April 1, 2011. A total of 

eighty-one 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 field 

matrix spike (FMS) samples for each location, two trip blanks containing Milli-QTM water and 

appropriate trip blank spikes, and one equipment rinseate blank. The equipment rinseate blanks did 

not have FMS samples prepared for determination of PFBS, PFHS or PFOS recovery. All groundwater 

samples for this project were logged under GLP10-01-02-17. In addition, four aqueous soil equipment 

rinseate blanks for GLP10-01-02-15 were analyzed and reported herein. The aqueous soil equipment 

rinseate blanks were collected on January 26 - 27,2011. As with the groundwater equipment rinseate 

blanks, the soil equipment blanks did not have FMS samples prepared for detemnination of PFBS, 

PFHS or PFOS recovery. 

The groundwater samples, trip and equipment rinseate blanks for GLP10-01-02-17 were received from 

Weston personnel on April 5, 2011. The aqueous soil equipment rinseate blanks for GLP10-01 -02-15 

were received from Weston personnel on Febmary 2, 2011. All of the samples were prepared and 

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

Many of the groundwater samples required dilution to attain PFBS, PFHS, and PFOS concentrations 

within the range of the curve, in some instances up to a 200-fold dilution were required. The average 

measured PFBS, PFHS, and PFOS concentrations are summarized in Table 1. Equipment rinseate 

and the trip blanks were below the lower limit of quantitation (LLOQ), indicating adequate control of 

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

groundwaters ranged from 0.0246 ng/mL to 3020 ng/mL. The PFHS concentration results for all 

groundwaters ranged from 0.119 ng/mL to 5360 ng/mL. The PFOS concentration results for the 

reported groundwaters ranged from 0.250 ng/mL to 6010 ng/mL. The analytical uncertainties 

associated with the reported results are as follows: PFBS 100% ± 17%, PFHS 100% ± 17%, and 

PFOS 100% ±22%. 

Page 9 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

Table 1. Summarized PFBS, PFHS, and PFOS Results (Decatur Groundwater - 01 2011). 

Sampling Location 

GW203LQ1 Y11 LF 

GW 220R Q1 Y11 LF 

GW220LQ1 Y11 LF 

GW 222R 01 Y11 LF 

GW227RQ1 Y11 LF 

GW227LQ1 Y11 LF 

GW310RQ1Y11CP 

GW312RQ1 Y11 CP 

GW317LQ1 Y11 CP 

GW324LQ1 Y11 CP 

GW327RQ1 Y11 CP 

GW328RQ1 Y11 CP 

GW 328L Q1 Y11 CP 

GW330RQ1 Y11 CP 

GW330LQ1 Y11 CP 

GW331SQ1 Y11 CP 

GW 335S 01 Y11 CP 

GWGRS04Q1 Y11CP 

Trip Blank (Milli-QTM Water) 

GLP10-01-02-17 Equipment Rinseate 

Blank 

GLP10-01-02-15; Four Aqueous Soil 

Equipment Rinseate Blanks 

PFBS 

Avg. Cone. (ng/mL) 

± %RPD 

105 ±2.9% 

8.41 ± 0.83% 

11.5 ±2.6% 

97.6 ± 2.8% 

19.6±24%<^> 

292 ±4.1% 

840 ± 0.83% 

1190 ±3.4% 

0.0246 ± 21% <^' 

112 ±1.8% 

93.3 ± 2.7% 

39.0 ±5.1% 

71.9 ±3.3% 

3020 ± 1.7% <"> 

545 ± 17% 

558 ± 29% '2' 

1080 ±3.7%'^' 

2020 ± 6.9% 

<0.0200 

<0.0200 

<0.0250 

PFHS 

Avg. Cone. (ng/mL) 

± %RPD 

595 ± 2.0% 

34.3 ± 4.7% 

52.0 ± 4.8% 

607 ± 2.8% 

106±23%<^' 

62.2 ±1.8% 

485 ± 8.0% 

629 ± 26% <^' 

0.119 ±3.4% 

111 ±5.4% 

168 ± 1.8% <^' 

63.1 ±5.1% 

22.3 ± 3.6% 

259 ±1.5% 

625 ±17% 

292 ±15% 

2030 ± 2.5%'"' 

5360 ± 6.9% 

<0.0400 

<0.0400 

<0.0250 

PFOS 

Avg. Gone. (ng/mL) 

± %RPD 

861 ±12<^* 

51.5 ±3.1% 

83.5 ±11% 

781 ± 6.7% 

740 ± 23% <^* 

363 ±1.4% 

1020 ±14% 

1010±34%<^> 

0.250 ±15% 

316 ±10% 

617 ±8.4% 

217 ±6.0% 

1.33 ±14% 

720 ±1.4% 

223 ± 9.0% 

642 ± 8.3% 

6010 ± 6.7% <'" 

NR<^' 

<0.500 

<0.500 

<0.0250 

The analytical method uncertainties associated with the reported results are as follows: PFBS 100% ± 16%, PFHS 100% ± 18%, 

and PFOS 100% ±21%. 

(1) The analytical uncertainty for PFOS has Iseen adjusted to ± 38% based on FMS recovery. 

(2) Ttie RPD did not meet method acceptance criteria of s20%. 

(3) The analytical uncertainty for PFHS has been adjusted to ± 41 % based on FMS recovery. 

(4) Sampling location did not contain an appropriate spike level to assess recovery. 

(5) The analytical uncertainty for PFBS has been adjusted to ± 34% based on FMS recovery. 

(6) NR = Not Reportable. Recovery ofthe most appropriate FMS sample was <50%. See section 9 of the report for additional 

information. 

Page 10 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1 St Quarter Sampling - 2011 

3 Introduction 

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

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

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

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

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

conducted to analyze ground water samples collected from various wells located in Decatur, AL for 

PFBS, PFHS, and PFOS in an effort to characterize on-site 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 field spike 

samples. Each empty container was marked 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. 

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

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

Performance Liquid Chromatography/Mass Spectrometry Direct Injection Analysis". 

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

collected, trip blanks and equipment rinseate samples. Tables 9-27 summarize the individual sample 

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

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

\4 Test & Control Substances 

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

was purely analytical in nature. 

Page 11 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

5 Reference Substances 

Reference Substance 

Chemical Name 

Chemical Formula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFBS 

(predominantly linear) 

Perfluorobutane sulfonate 

C4F9SO3" 

Potassium Salt 

3M 

1/10/2017 

Frozen 

41-2600-8442-5 

TCR-121 

White Powder 

96.7% 

PFHS 

(linear) 

Perfluorohexane sulfonate 

C6F13SO3" 

Sodium Salt 

Wellington 

4/2/2013 

Frozen 

LPFHxSAMOS 

TCR08-0018 

Crystalline 

98% 

Reference Substance 

Chemical Name 

Chemical Formula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFOS 

(linear) 

Perfluorooctane sulfonate 

C8F17SO3" 

Potassium Salt 

CAS #2795-39-3 

Wellington 

10/18/2013 

Frozen 

LPFOSKBM06 

TCR08-0001 

Crystalline 

98% 

PFOS 

(linear -i- branched) 

Perfluorooctane sulfonate 

C8F17SO3" 

Potassium Salt 

CAS #2795-39-3 

3M 

12/14/2016 

Frozen 

171 

TCR-696 

White Powder 

86.4% 

Page 12 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1 st Quarter Sampling - 2011 

Reference Substance 

Chemical Name 

Chemical Formula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

"C,-PFOS 

(linear) 

Sodium 

Perfluorooctanesulfonate 

''C8Fi7S03-Na" 

CAS#MPFC-C-0910 

Wellington 

09/28/2013 

Frozen 

092310 

TCR10-0048 

Liquid 

5 |jg/mL '^' 

(1) Custom mixture of seven mass-labeled ("C) perfluoroalkylcartjoxylic adds, two 

mass-labeled ("C) perfluoroalkylsulfonates and one mass-labeled ("C) 

perfiuoro-l -octanesulfonamlde. 

The test system for this study are ground water samples collected from wells located in Decatur, AL by 

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

specific lot of test substance. 

Sample Description Key Code. 

Example GW330L Q1 Y11 CP 1 

String Number 

1 

2 

3 

4 

5 

6 

String Descriptor 

Sample Type 

Well Identmer 

Well Level 

Sampling Date 

Sampling Location 

Sample Type 

Example 

GW= Ground water 

Example: 330L 

R = Residuum shallow water-bearing zone 

L = Bedrock water-bearing zone 

S = Epikarst middle water-bearing zone 

01^ 1 = 1 " quarter, 2011 

CP = Chemical Plant 

FL = Former Landfill 

0=primary sample 

1=duplicate sample 

LS = low spike 

HS = high spike 

Page 13 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

7 Method Summary 

7.1 Methods 

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

"Determination of Perfluorinated Compounds In Water by High Performance Liquid 

Chromatography/Mass Spectrometry Direct Injection Analysis". 

7.2 Sample Collection 

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

Environmental Laboratory. Sample bottles were retumed to the laboratory at ambient conditions on 

October 1, 2010. Samples were stored refrigerated at the laboratory after receipt. A set of laboratory 

prepared Trip Blank and Trip Blank field matrix spikes were sent with the sample collection bottles. 

7.3 Sample Preparation 

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

analysis. 

Samples that required dilution were prepared as follows: 

1:5 dilutions were prepared by diluting 2mL sample with 8 mL of Milli 0 water, 

1:10 dilutions were prepared by diluting 1 mL sample with 9 mL of Milli 0 water, 

1:20 dilutions were prepared by diluting 0.5mL sample with 9.5mL of Milli 0 water, 

1:50 dilutions were prepared by diluting 0.2mL sample with 9.8mL of Milli 0, and 

1:100 dilutions were prepared by diluting 0.1 mL sample with 9.9mL of Milli 0 water. 

1:200 dilutions were prepared by diluting 0.05mL sample with 9.95mL of Milli 0 water. 

Samples may also have been diluted further by varying the injection volume during analysis. 

Sampling locations GW 317L and GW 328L were prepared for PFOS by removing a 10 mL aliquot and 

adding an aliquot of a separate intemal standard spiking solution (nominal concentration of 1 ng/mL). 

This same procedure was followed for the laboratory control samples. 

7.4 Analysis 

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

performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). Detailed instrument 

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

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

4/19/11 Analysis: All samples analyzed for PFBS, PFHS, and PFOS. 

4/24/11 Analysis: Analyzed re-diluted sample set GW 222R 01 Y11 LF for PFBS, PFHS, and PFOS. 

5/12/11 Analysis: Analysis of GLP10-01-02-15 soil equipment rinseate blanks for PFBS, PFHS. 

5/14/11 Analysis: Analysis of sampling location GW 317L 01 Y11 CP and GW 328L 01 Y11 for PFOS 

with intemal standard. 

5/16/11 Analysis: Analysis of GLP10-01-02-15 aqueous soil equipment rinseate blanks for PFOS. 

5/17/11 Analysis: Analysis of re-diluted sample set GW GRS04 01 Y11 CP for PFOS with laboratory 

matrix spike. 

Page 14 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

Table 2. Instrument Parameters. 

Instrument Name 

Analytical Method Followed 

Analysis Date 

Liquid Chromatograph 

Guard column 

Analytical column 

Injection Volume 

Mass Spectrometer 

Ion Source 

Electrode 

Polarity 

Soflware 

ETS Ginger 

ETS-8-044.0 

4/19/11 and 4/24/11 

Agilent 1100 

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

Betasll 018 (2.1 mm X 100 mm), 5u 

2or5nL 

Applied Blosystems API 5000 

Turbo Spray 

Turbo Ion electrode 

Negative 

Analyst 1.4.2 

ETS McCoy 

ETS-8-044.0 

5/12/11,5/14/11,5/16/11,5/17/11 

Agilent 1290 

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

Betasll 018 (2.1 mm X 100 mm), 5n 

10,25or5|iL 

Applied Blosystems/^Pl 5500 

Turbo Spray 

Turtjo ion electrode 

Negative 

Analyst 1.5.2 

Table 3. Liquid Chromatography Conditions. 

step 

Number 

Total Time 

(min) 

Flow Rate 

(fiL/min) 

PercentA 

(2 mM ammonium acetate) 

Percent S 

(Methanol) 

ETS-8-044.0 Analysis 4/13/11 and4/24/11 

0 

1 

2 

3 

4 

5 

0 

1 

2 

3 

4 

5 

0 

1.0 

11.0 

13.5 

14.0 

17.0 

ETS-8-04 

0 

2.0 

14.5 

15.5 

16.5 

20.0 

300 

300 

300 

300 

300 

300 

90.0 

90,0 

10.0 

10.0 

90.0 

90.0 

4.0 Analysis 5/12/11,5/14/11,5/16/11, and 5/17/11 

300 

300 

300 

300 

300 

300 

90.0 

90.0 

5.0 

5.0 

90.0 

90.0 

10.0 

10.0 

90,0 

90.0 

10.0 

10.0 

10.0 

10.0 

95.0 

95.0 

10.0 

10.0 

Page 15 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

Table 4. Mass Transitions. 

Analyte 

PFBS 

PFHS 

PFOS 

Reference Material 

Structure 

Unear 

Unear 

Linear 

Mass Transition 

Q1/Q3 

299/80 

299/99 

399/80 

399/99 

499/80 

499/99 

499/130 

Intemal Standard 

NA 

NA 

fC^PFOS^ 

Mass Transition 

Q1/Q3 

NA 

NA 

507/80 

Dwell time was 50 msec (4/19/11,4/24/11,5/14/11,5/16/11, and 5/17/11 analysis) or 20 msec (5/12/11 analysis) for each 

transition. Ttie Individual transitions were summed to produce a "total Ion chromatogram" (TIC), which was used for 

quantitation, 

NA = Not/Applicable 

(1) Intemal standard was only used for the analysis of locations: GW 317L, GW 328L, and GLP10-01-02-15 soil 

equipment rinseate blanks for PFOS, 

8 Ama^yticat Results 

8.1 Calibration 

4/19/11,4/24/11,5/12/11, and 5/17/11 analysis: 

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

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

water. A total of frfteen spiked standards ranging from 0.020 ng/mL to 100 ng/mL were prepared, 

however, not all analytical runs included all fifteen standards. Low curve points were disabled to meet 

accuracy or method blank criteria. 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 iforced through zero during the fitting 

process. Calculating the standard concentrations using the peak area confimned accuracy of each curve 

point. 

Each curve point was quantitated using the overall calibration curve and reviewed for accuracy. Method 

calibration accuracy requirements of 100±25% (100±30% for the lowest curve point) were met for all 

analytes. The con-elation coefficient (r) was greater than 0.995 for PFBS, PFHS, and PFOS for each 

analytical batch. 

5/14/11 analysis: Sampling locations GW 317L, GW 328L, and GLP10-01-02-15 soil equipment rinseate 

blanks for PFOS. 

Samples were analyzed against a matrix-matched stable isotope intemal standard calibration curve. 

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

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

The calibration standards contained an intemal standard mix at a nominal concentration of 1 ng/mL. A 

total of ten spiked standards ranging from 0.050 ng/mL to 25 ng/mL were analyzed for PFOS. A 

quadratic, 1/x weighted, calibration curve of the ratio of the standard peak area counts over the intemal 

standard peak area counts was used to fit the data for each analyte. The data were not forced through 

zero during the fitting process. 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 PFOS. 

5/16/11 analysis: Sampling locations GLP10-01-02-15 soil equipment rinseate blanks for PFOS. 

Samples were analyzed against a matrix-matched stable isotope intemal standard calibration curve. 

Page 16 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

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. 

The calibration standards contained an intemal standard mix at a nominal concentration of 1 ng/mL. A 

total of nine spiked standards ranging from 0.0250 ng/mL to 2.5 ng/mL were analyzed for PFOS. A 

quadratic, 1/x weighted, calibration curve of the ratio of the standard peak area counts over the internal 

standard peak area counts was used to fit the data for each analyte. The data were not forced through 

zero during the fitting process. 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 PFOS. 

8.2 System Suitability 

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

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

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

met for PFBS, PFHS, and PFOS for each analytical batch. 

8.3 Limit of Quantitation (LOQ) 

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

and accuracy requirements and for which the area counts are at least twice those ofthe appropriate 

blanks. The LOQs associated with the sample analysis are listed in the table below. 

Table 5. Limit of Quantitation (LOQ). 

Analysis Date 

4/19/11 

4/24/11 

5/12/11 

5/14/11 

5/16/11 

5/17/11 

Dilution 

1 

5 

10 

20 

50 

100 

20 

50 

1 

1 

1 

200 

PFBS 

LOQ, ng/mL 

0.0200 

0.100 

0.200 

0.400 

1.00 

2.00 

0.400 

1.00 

0.0250 

NA 

NA 

NA 

PFHS 

LOQ, ng/mL 

0.0400 

0.200 

0.400 

0.800 

2.00 

4.00 

5.00 

12.5 

0.0250 

NA 

NA 

NA 

PFOS 

LOQ, ng/mL 

0.500 

2.50 

5.00 

10.0 

25.0 

50.0 

5.00 

12.5 

NA 

0.0500 

0.0250 

20 

NA = Not Applicable; analytical results for were not reported from the run. 

8.4 Continuing Calibration 

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

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

reported samples were bracketed by CCVs that met method criteria of 100% ± 25%. 

8.5 Blanks 

Three types of blanks were prepared and analyzed with the samples: method procedural blanks, 

field/trip blanks, and equipment blanks. Method procedural blank results were reviewed and used to 

evaluate method perfomriance and to detennine the LOO for each analyte. 

Page 17 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

8.6 Lab Control Spikes (LCSs) 

A minimum of two lab control spike levels were prepared and analyzed in triplicate with each preparation 

set. LCSs were prepared by spiking known amounts of the analyte into 10 mL of Milli 0 water to 

produce the desired concentration. The spiked water samples were then analyzed in the same manner 

as the samples. The method acceptance criteria, average of LCS at each level should be within 100% ± 

20% with an RSD 220%. 

4/19/11 Analysis: Three levels of LCS were prepared and met method acceptance criteria for PFBS, 

PFHS, and linear PFOS. 

4/24/11 Analysis: Three levels of LCS were prepared and met method acceptance criteria for PFBS. 

The low set of LCS samples were BLOO for PFHS and PFOS, while the mid and high set of LCS 

samples met method acceptance criteria. 

5/12/11 Analysis: Two levels of LCS were prepared and met method acceptance criteria for PFBS and 

PFHS. 

5/14/11 Analysis: Three levels of LCS were prepared and met method acceptance criteria for linear 

PFOS. 

5/16/11 Analysis: Two levels of LCS were prepared and met method acceptance criteria for PFOS. 

5/17/11 Analysis: Two levels of LCS were prepared and met method acceptance criteria for PFOS. 

As the reference materials used for quantitation 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 + branched) were prepared to evaluate the potential for analytical bias. 

4/19/11 Analysis: Three levels of linear and branched PFOS LCS were prepared and met method 

acceptance criteria. 

4/24/11 Analysis: Three levels of linear and branched PFOS LCS were prepared. The low set of LCS 

samples were BLOO, while the mid and high set of LCS samples met method acceptance criteria, 

and met method acceptance criteria. 

5/14/11 Analysis: Three levels of linear and branched PFOS LCS were prepared and met method 

acceptance criteria. 

5/16/11 Analysis: Two levels of linear and branched PFOS LCS were prepared and met method 

acceptance criteria. 

5/17/11 Analysis: Two levels of linear and branched PFOS LCS were prepared and met method 

acceptance criteria. 

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

1 ,^o 1^ . r. Calculated Concentration ,.... , 

LCS Percent Recovery = * 100% 

Spike Concentration 

LCS% RSD = standard deviation LCS replicates . ^ Q^^^ 

average LCS recovery 

Page 18 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

Table 6. Laboratory Control Spike Recovery. 

ETS^-044.0 

Analyzed 4/19/11 

Lab ID 

LCS-110412-1 

LCS-110412-2 

LCS-110412-3 

Average ±%RSD 

LCS-110412-4 

LCS-110412-5 

LCS-110412-6 

Average ±%RSD 

LCS-110412-7 

LCS-110412-8 

LCS-110412-9 

Average ±%RSD 

Spiked 

Concentration 

(ng/mL) 

2.00 

2.00 

2.00 

PFBS 

Calculated 

Concentration 

(ng/mL) 

2.17 

2.16 

2.23 

%Recovery 

109 

108 

111 

109% ±1.4% 

20.0 

20.0 

20,0 

20.6 

23.6 

22.5 

103 

118 

112 

111% ±6.8% 

50.0 

50.0 

50.0 

52.2 

56.9 

57.0 

104 

114 

114 

111% ±5.2% 

Spiked 

Concentration 

(ng/mL) 

2.00 

2.00 

2.00 

PFHS 

Calculated 

Concentration 

(ng/mL) 

2.22 

2.30 

2.29 

%Recoveiy 

111 

115 

114 

113% ±1.8% 

20.0 

20.0 

20.0 

21.1 

23.5 

22.7 

106 

118 

113 

112% ±5.4% 

50.0 

50.0 

50.0 

51.9 

56.0 

56.9 

104 

112 

114 

110% ±4.8% 

ETS-8-044.0 

Analyzed 4/19/11 

Lab ID 

LCS-110412-1 

LCS-110412-2 

LCS-110412-3 

Average ±%RSD 

LCS-110412-4 

LCS-110412-5 

LCS-110412-6 

Average ±%RSD 

LCS-110412-7 

LCS-110412-8 

LCS-110412-9 

Average ±%RSD 

Spiked 

Concentration 

(ng/mL) 

2.00 

2.00 

2.00 

PFOSOineai) 

Calculated 

Concentration 

(na/mU 

2.21 

2.51 

2.10 

%Recovery 

111 

125 

105 

114% ±9.0% 

20.0 

20.0 

20.0 

21.7 

24.3 

23.0 

108 

122 

115 

115% ±6.1% 

50.0 

50.0 

50.0 

52.7 

56.7 

57.7 

105 

113 

115 

111% ±4.8% 

Lab ID 

LCS-110412-10 

LCS-110412-11 

LCS-110412-12 

Average ±%RSD 

LCS-110412-13 

LCS-110412-14 

LCS-110412-15 

Average ±%RSD 

LCS-110412-16 

LCS-110412-17 

LCS-110412-9 

Average ±%RSD 

PFOS Oinear+branched) 

Spiked 

Concentration 

(ng/mL) 

2.02 

2.02 

2.02 

Calculated 

Concentration 

(ng/mL) 

2.14 

2.03 

2.31 

YoRecovery 

106 

101 

114 

107% ±6.1% 

20.2 

20.2 

20,2 

21.8 

23.3 

22.3 

108 

115 

110 

111% ±3.2% 

50,5 

50.5 

50.5 

61.5 

60.0 

52.7 

122 

119 

104 

115% ±8.4% 

Page 19 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Table 6 continued. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Analyzed 4/24/11 

Lab ID 

LCS-110422-1 

LCS-110422-2 

LCS-110422-3 

Average ±%RSD 

LCS-110422-4 

LCS-110422-5 

LCS-110422-6 

Average ±%RSD 

LCS-110422-7 

LCS-110422-8 

LCS-110422-9 

Average ±%RSD 

Spiked 

Concentration 

(ng/mL) 

0.200 

0.200 

0.200 

PFBS 

Calculated 

Concentration 

(ng/mL) 

0.189 

0.200 

0.231 

%Recovery 

94.3 

99.8 

115 

103% ±10% 

2.00 

2.00 

2.00 

1.91 

2.12 

2.23 

95.6 

106 

112 

105% ±7.9% 

20.0 

20.0 

20.0 

19.6 

21.5 

23.4 

97.9 

107 

117 

10r/.±8.9% 

Spiked 

Concentration 

(ng/mL) 

0.200 

0.200 

0.200 

PFHS 

Calculated 

Concentration 

(ng/mL) 

<0.250 

<0.250 

<0.250 

VoRecovery 

NA 

NA 

NA 

NA'^' 

2.00 

2,00 

2,00 

1.82 

2.23 

2.01 

91.1 

112 

101 

101% ±10% 

20,0 

20,0 

20,0 

17.6 

18.9 

20.6 

88.2 

94.7 

103 

95.3% ±7.8% 

ETS-8-044.0 

Analyzed 4/24/11 

Lab ID 

LCS-110422-1 

LCS-110422-2 

LCS-110422-3 

Average ±%RSD 

LCS-110422-4 

LCS-110422-5 

LCS-110422-6 

Average ±%RSD 

LCS-110422-7 

LCS-110422-8 

LCS-110422-9 

Average ±%RSD 

Spiked 

Concentration 

(ng/mL) 

0.200 

0,200 

0,200 

PFOS (linear) 

Calculated 

Concentration 

(ng/mL) 

<0,250 

<0,250 

<0,250 

%Recovery 

NA 

NA 

NA 

NA<^' 

2,00 

2,00 

2.00 

1.75 

1.97 

1.95 

87,7 

98,4 

97,3 

94.5% ±6.2% 

20.0 

20.0 

20.0 

20,5 

23,7 

24,1 

103 

118 

121 

114% ±8.5% 

Lab ID 

LCS-110422-10 

LCS-110422-11 

LCS-110422-12 

Average ±%RSD 

LCS-110422-13 

LCS-110422-14 

LCS-110422-15 

Average ±%RSD 

LCS-110422-16 

LCS-110422-17 

LCS-110422-18 

Average ±%RSD 

PFOS (linear+branched) 

Spiked 

Concentration 

(ng/mL) 

0,202 

0,202 

0,202 

Calculated 

Concentration 

(ng/mL) 

<0,250 

<0,250 

<0,250 

VoRecovery 

NA 

NA 

NA 

NA<'' 

2,02 

2,02 

2.02 

1,84 

1,82 

1,69 

90,8 

89,9 

83,5 

88.1% ±4.5% 

20.2 

20.2 

20.2 

21,0 

22,1 

21,9 

104 

110 

108 

107% ±2.8% 

(1) The sample result was BLOO, A recovery could not be calculated. 

Page 20 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

Table 6 continued. Laboratory Control Spike Recovery. 

ETS-8-044,0 

Analyzed 5/12/11 

Lab ID 

LCS-110509-1 

LCS-110509-2 

LCS-110509-3 

Average ±%RSD 

LCS-110509-4 

LCS-110509-5 

LCS-110509-6 

Average ±%RSD 

PFBS 

Spiked 

Concentration 

(ng/mL) 

0.198 

0.198 

0.198 

Calculated 

Concentration 

(ng/mL) 

0.185 

0.202 

0.212 

%Recovery 

93.2 

102 

107 

101% ±6.9% 

1.98 

1.98 

1.98 

1.70 

2.22 

2.40 

85,7 

112 

121 

106% ±17% 

PFHS 

Spiked 

Concentration 

(ng/mL) 

0,198 

0,198 

0,198 

Calculated 

Concentration 

(ng/mL) 

0,201 

0,221 

0,223 

%Recovery 

101 

111 

112 

108% ±5.6% 

1,98 

1,98 

1,98 

1,74 

2,19 

2,25 

88,0 

111 

113 

104% ±13% 

ETS^-044,0 

Analyzed 5/14/11 

Lab ID 

LCS-110513-1 

LCS-110513-2 

LCS-110513-3 

Average ±%RSD 

LCS-110513-4 

LCS-110513-5 

LCS-110513-6 

Average ±%RSD 

LCS-110513-7 

LCS-110513-8 

LCS-110513-9 

Average ±%RSD 

Spiked 

Concentration 

(na/mU 

0,199 

0,199 

0,199 

PFOS (lineal) 

Calculated 

Concentration 

(ng/mL) 

0.188 

0.183 

0.182 

VoRecovery 

94.6 

92.0 

91.4 

92.7% ±1.8% 

1.99 

1.99 

1,99 

2.22 

2.12 

2.36 

111 

107 

118 

112% ±5.0% 

9,94 

9,94 

9,94 

9.09 

9.25 

8.19 

91.5 

93.0 

82.4 

89.0% ±6.4% 

Lab ID 

LCS-110513-10 

LCS-110513-11 

LCS-110513-12 

Average ±%RSD 

LCS-110513-13 

LCS-110513-14 

LCS-110513-15 

Average ±%RSD 

LCS-110513-16 

LCS-110513-17 

LCS-110513-18 

Average ±%RSD 

PFOS (linear+branched) 

Spiked 

Concentration 

(ng/mL) 

0.201 

0.201 

0.201 

Calculated 

Concentration 

(ng/mL) 

0.196 

0.209 

0.207 

%Recovery 

97,6 

104 

103 

102% ±3.4% 

2.01 

2.01 

2.01 

2.05 

2.01 

2.14 

102 

100 

106 

103% ±3.0% 

10.0 

10.0 

10.0 

9.96 

9.85 

9,84 

99,6 

98.5 

98.4 

98.8% ±0.67% 

ETS-8-044,0 

Analyzed 5/16/11 

Lab ID 

LCS-110509-1 

LCS-110509-2 

LCS-110509-3 

Average ±%RSD 

LCS-110509-4 

LCS-110509-5 

LCS-110509-6 

Average ±%RSD 

PFOS (linear) 

Spiked 

Concentratmn 

(ng/mL) 

0,198 

0,198 

0,198 

Calculated 

Concentration 

(ng/mL) 

0.152 

0.164 

0.182 

%Recoverv 

76.6 

82.6 

91,7 

83.6% ±9.1% 

1,98 

1,98 

1,98 

1.52 

1.99 

2.06 

76,7 

100 

104 

93.6% ±16% 

Lab ID 

LCS-110509-10 

LCS-110509-11 

LCS-110509-12 

Average ±%RSD 

LCS-110509-13 

LCS-110509-14 

LCS-110509-15 

Average ±%RSD 

PFOS Oinear+branched) 

Spiked 

Concentration 

(ng/mL) 

0,200 

0,200 

0,200 

Calculated 

Concentration 

(ng/mL) 

0.199 

0.207 

0.207 

%Recovefy 

99,6 

103 

103 

102% ±1.9% 

2.00 

2,00 

2.00 

2.03 

2,15 

2,05 

102 

108 

103 

104% ±3.1% 

Page 21 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 St Quarter Sampling - 2011 

Table 6 continued. Laboratory Control Spike Recovery. 

ETS-8-044,0 

Analyzed 5/17/11 

Lab ID 

LCS-110517-1 

LCS-110517-2 

LCS-110517-3 

Average + %RSD 

LCS-110517-4 

LCS-110517-5 

LCS-110517-6 

Average ±%RSD 

PFOS (linear) 

Spiked 

Concentration 

(ng/mL) 

4,98 

4,98 

4,98 

Calculated 

Concentration 

(ng/mL) 

5,82 

5.73 

5,69 

VoRecovery 

117 

115 

114 

115% ±1.3% 

40,0 

40,0 

40,0 

44,5 

45,3 

45.6 

111 

113 

114 

113% ±1.4% 

Lab ID 

LCS-110517-7 

LCS-110517-8 

LCS-110517-9 

Average ± %RSD 

LCS-110517-10 

LCS-110517-11 

LCS-110517-12 

Average ± %RSD 

PFOS (linear + branched) 

Spiked 

Concentration 

(ng/mL) 

5,04 

5,04 

5,04 

Calculated 

Concentration 

(ng/mL) 

4.79 

5.04 

4.90 

VoRecovery 

95,1 

100 

97,2 

97.4% ±2.5% 

40.4 

40.4 

40.4 

40,3 

41,9 

41,7 

99,8 

104 

103 

102% ±2.1% 

8.7 Analytical Method Uncertainty 

Analytical uncertainty is based on historical LCS 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 LCS samples. 

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

corresponds to a confidence level of 95%. A minimum ofthe 50 data points were used to generate the 

method uncertainty values. 

Table 7. Analytical Uncertainty. 

Analyte 

PFBS 

PFHS 

PFOS 

Standard Deviation 

8,72 

8,43 

11,0 

Method Uncertainty 

±17% 

±17% 

±22% 

8.8 Laboratory Matrix Spikes (LMS) 

Two laboratory matrix spikes were prepared for sample set GW GRS04 01 Y1 CP for PFOS, The high 

FMS at 5000 ng/mL was not meeting method acceptance criteria for PFOS, therefore, a 5000 ng/mL 

LMS sample was prepared on both the primary sample and the sample duplicate. It was noted at the 

time of sample preparation, that the primary sample for this sampling set contained significantly more 

sediment in the sample bottle as compared to the other sample bottles collected for this location. The 

color of the sample was similar to the color of dark tea and had a strong petroleum odor. 

The LMS sample was prepared by removing a 0.05 mL aliquot of both the primary sample and the 

sample duplicate, adding an aliquot of spiking solution, and adding laboratory reagent water for a final 

volume of 10 mL. The dilution factor for the LMS samples was 200x. The LMS samples met method 

acceptance criteria with recoveries for 106% and 107% respectively. 

8.9 Field Matrix Spikes (FMS) 

Field matrix spikes were collected at each sampling point to verify that the analytical method is 

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

field sample to a container spiked by the laboratory with 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 

Page 22 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1 St Quarter Sampling-2011 

concentrations must be 50% ofthe sample concentration to be considered an appropriate field spike. 

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

Table 8. Field Matrix Spikes. 

Sampling Location 

317L 

220R, 220L, 328L 

203L, 222R, 227L, 227R, 31 OR, 324L, 

327R, 330L''', 3318 and 335S 

GRS04, 312R, 330R<^> 

328R 

Trip Blank Sets 1 and 2 

Spike Level 

Low FMS 

High FMS 

Low FMS 

High FMS 

Low FMS 

High FMS 

Low FMS 

High FMS 

Low FMS 

High FMS 

Low FMS 

Mid FMS 

High FMS 

PFBS 

(ng/mL) 

1,00 

10,0 

10,0 

100 

100 

1000 

1000 

5000 

100 

500 

10,0 

100 

1000 

PFHS 

(ng/mL) 

1,00 

10,0 

10,0 

100 

100 

1000 

1000 

5000 

100 

500 

10,0 

100 

1000 

PFOS 

(ng/mL) 

1,00 

10,0 

10,0 

100 

100 

1000 

1000 

5000 

100 

500 

10,0 

100 

1000 

(1) The sample collection tx)ttles used to collect location GW 330R were Intended for location GW 330L, The sample 

collection bottles used to collect location GW 330L were Intended for location GW 330R, 

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

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

Spike Concentraton 

9 Data Summary and Discussion 

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

locafions as well as the Trip Blanks and rinseate blank. 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 203L Q1 Y11 LF (Table 9) - The recovery of the HS for PFOS was 138%. Since this was 

the only appropriate spike level, the analytical uncertainty has been adjusted for PFOS to ± 38%. 

DAL GW 327R Q1 Y11 CP (Table 19) - The recovery of the LS for PFHS was 141 % and the recovery 

of the HS was 96.3%. Since the LS is the most appropriate spike level, the analytical uncertainty has 

been adjusted for PFHS to ± 41 %. 

DAL GW 330R Q1 Y11 CP (Table 22) - The wrong sample bottles were used to collect this sampling 

location. As a result, an appropriate field matrix spike was not available for PFBS. 

Page 23 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

DAL GW 335S Q1 Y11 CP (Table 25) - The recovery of the HS for PFBS was 134%. Since this was 

the only appropriate spike level, the analytical uncertainty has been adjusted for PFBS to ± 34%. An 

appropriate field matrix spike was not available for PFHS and PFOS. 

DAL GW GRS04 Q1 Y1 CP (Table 26) - The sample set was initially analyzed on 4/19/11. The 

sample/sample duplicate RPD for PFOS did not meet method acceptance criteria at 50%, and the 

recovery of the HS for PFOS did not meet method acceptance criteria with a recovery 23.7%. The 

sample set was re-diluted and analyzed on 5/17/11. The sample/sample duplicate RPD for PFOS did 

not meet method acceptance criteria at 48%, and the HS for PFOS still outside method acceptance 

criteria with a recovery of 32.9%. The LMS samples prepared on the primary sample and sample 

duplicate did meet method acceptance criteria with recoveries of 106% and 107% respectively. 

However, due to both the RPD and FMS recovery not meeting method acceptance criteria for PFOS, a 

result for PFOS will not be reported for this sampling location. 

Page 24 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

Table 9. GW 203L Q1 Y11 LF 

3M LIMS ID 

GLP10-01-02-17-053 

GLP10-01-02-17-054 

GLP10-01-02-17-055 

GLP10-01-02-17-056 

Description 

GW 203L Q1 Y11 LF 0 

GW 203L Q1 Y11 LF 1 

GW203LQ1 Y11 LF LS 

GW203LQ1 Y11 LF HS 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

106 

103 

232 

1300 

VoRecovery 

NA 

NA 

128 

120 

105 ng/mL ±2.9% 

PFHS 

Concentration 

(ng/mL) 

601 

589 

689 

1610 

VoRecovery 

NA 

NA 

NC 

102 

595 ng/mL ±2.0% 

PFOS 

Concentration 

(ng/mL) 

914 

808 

974 

2240 

VoRecovery 

NA 

NA 

NC 

138 <^' 

861 ng/mL ±12%<^ 

NA = Not Applicable 

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

Samples diluted 20x and analyzed 4/19/11. 

(1) Field matrix spike did not meet method acceptance criteria of 100% ± 30%. 

(2) The analytical uncertainty has been adjusted for PFOS to ± 38%. 

Table 10. GW 220R Q1 Y11 LF 

3MUMSID 

GLP10-01-02-17-033 

GLP10-01-02-17-034 

GLP10-01-02-17-035 

GLP10-01-02-17-036 

Description 

GW220RQ1 Y11 LFO 

GW220RQ1 Y11 LF1 

GW220RQ1 Y11 LF LS 

GW220RQ1 Y11 LF HS 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

8.44 

8.37 

19.4 

125 

VoRecovery 

NA 

NA 

110 

117 

8.41 ng/mL ±0.83% 

PFHS 

Concentration 

(ng/mL) 

35.1 

33.5 

45.4 

144 

VoRecovery 

NA 

NA 

NC 

110 

34.3 ng/mL ±4.7% 

PFOS 

Concentration 

(ng/mL) 

52.3 

50.7 

61.5 

134 

VoRecovery 

NA 

NA 

NC 

82.5 

51.5 ng/mL ±3.1% 

NA = Not /\ppllcable 

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

Samples diluted 5x and analyzed 4/19/11. 

Page 25 of 98 
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/Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

Table 11. GW 220L Q1 Y11 LF 

3M LIMS ID 

GLP10-01-02-17-037 

GLP10-01-02-17-038 

GLP10-01-02-17-039 

GLP10-01-02-17-040 

Description 

GW220LQ1 Y11 LFO 

GW220LQ1 Y11 LF 1 

GW220LQ1Y11LFLS 

GW220LQ1 Y11 LF HS 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

11,3 

11.6 

23.1 

127 

%Recovery 

NA 

NA 

117 

116 

11.5 ng/mL ±2.6% 

PFHS 

Concentiation 

(ng/mL) 

50.7 

53.2 

64.0 

158 

VoRecovery 

NA 

NA 

NC 

106 

52.0 ng/mL ±4.8% 

PFOS 

Concentration 

(ng/mL) 

79.0 

87.9 

92.2 

161 

VoRecovery 

NA 

NA 

NC 

77.6 

83.5 ng/mL ±11% 

NA = Not /Applicable 

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

Samples diluted 5x and analyzed 4/19/11. 

Table 12. GW 222R Q1 Y11 LF 

3M LIMS ID 

GLP10-01-02-17-041 

GLP10-01-02-17-042 

GLP10-01-02-17-043 

GLP10-01-02-17-044 

Description 

GW222RQ1 Y11 LFO 

GW222RQ1 Y11 LF 1 

GW222RQ1 Y11 LF LS 

GW222RQ1 Y11 LF HS 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

96.2 

98.9 

203 

1150 

VoRecovery 

NA 

NA 

105 

105 

97.6 ng/mL ±2.8% 

PFHS 

Concentration 

(ng/mL) 

615 

598 

859 

1540 

VoRecovery 

NA 

NA 

NC 

93.4 

607 ng/mL ±2.8% 

PFOS 

Concentration 

(ng/mL) 

755 

807 

829 

1620 

VoRecovery 

NA 

NA 

NC 

83.9 

781 ng/mL ± 6.7% 

NA = Not /Applicable 

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

Samples diluted 20x .with the exception ofthe HS which was diluted 50x, and analyzed 4/24/11. 

Page 26 of 98 
GLP10-01-02; Interim Report 17 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Table 13. GW 227R Q1 Y11 LF 

3MUMSID 

GLP10-01-02-17-029 

GLP10-01-02-17-030 

GLP10-01-02-17-031 

GLP10-01-02-17-032 

Description 

GW227RQ1 Y11 LFO 

GW227RQ1 Y11 LF 1 

GW227RQ1 Y11 LF LS 

GW227RQ1 Y11 LF HS 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

21,9 

17.2 

131 

1130 

VoRecovery 

NA 

NA 

111 

111 

19.6 ng/mL ±24%^' 

PFHS 

Concentration 

(ng/mL) 

118 

93.6 

234 

1190 

VoRecovery 

NA 

NA 

128 

108 

106 ng/mL ±23%^^' 

PFOS 

Concentration 

(ng/mL) 

826 

653 

1000 

1970 

VoRecovery 

NA 

NA 

NC 

123 

740 ng/mL ± 23% (^> 

NA = Not/Applicable 

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

Samples diluted 20x and analyzed 4/19/11. 

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

Table 14. GW 227L Q1 Y11 LF 

3M LIMS ID 

GLP10-01-02-17-025 

GLP10-01-02-17-026 

GLP10-01-02-17-027 

GLP10-01-02-17-028 

Description 

GW227LQ1 Y11 LFO 

GW227LQ1 Y11 LF 1 

GW227LQ1 Y11 LF LS 

GW227LQ1 Y11 LF HS 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

286 

298 

389 

1280 

VoRecovery 

NA 

NA 

NC 

98.8 

292 ng/mL ±4.1% 

PFHS 

Concentration 

(ng/mL) 

61.6 

62.7 

165 

1010 

VoRecovery 

NA 

NA 

103 

94.8 

62.2 ng/mL ±1.8% 

PFOS 

Concentration 

(ng/mL) 

365 

360 

477 

1190 

VoRecovery 

NA 

NA 

NC 

82.8 

363 ng/mL ±1.4% 

NA = Not/Applicable 

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

Samples diluted 20x and analyzed 4/19/11. 

Page 27 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

Table 15. GW 31 OR Q1 Y11 CP 

3M LIMS ID 

GLP10-01-02-17-021 

GLP10-01-02-17-022 

GLP10-01-02-17-023 

GLP10-01-02-17-024 

Description 

GW310RQ1 Y11 CPO 

GW310RQ1 Y11 CP 1 

GW310RQ1 Y11 CPLS 

GW310RQ1 Y11 CPHS 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

836 

843 

982 

1890 

VoRecovery 

NA 

NA 

NC 

105 

840 ng/mL ±0.83% 

PFHS 

Concentration 

(ng/mL) 

465 

504 

573 

1570 

VoRecovery 

NA 

NA 

NC 

109 

485 ng/mL ±8.0% 

PFOS 

Concentration 

(ng/mL) 

943 

1090 

1050 

1810 

%Recovery 

NA 

NA 

NC 

79.4 

1020 ng/mL ±14% 

NA = Not /Applicable 

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

Samples diluted 10Ox and analyzed on 4/19/11. 

Table 16. GW312RQ1 Y11 CP 

3MUMSID 

GLP10-01-02-17-077 

GLP10-01-02-17-078 

GLP10-01-02-17-079 

GLP10-01-02-17-080 

Description 

GW312RQ1 Y11 CPO 

GW312RQ1 Y11 CP1 

GW312RQ1 Y11 CPLS 

GW312RQ1 Y11 CPHS 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

1170 

1210 

2370 

7050 

VoRecovery 

NA 

NA 

118 

117 

1190 ng/mL ±3.4% 

PFHS 

Concentration 

(ng/mL) 

710 

547 

1480 

5330 

VoRecovery 

NA 

NA 

85.2 

94.0 

629ng/mL±26%^> 

PFOS 

Concentiation 

(ng/mL) 

1180 

833 

1980 

b//0 

VoRecovery 

NA 

NA 

97.4 

95.3 

1010 ng/mL ±34%^^ 

NA = Not /Applicable 

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

Samples diluted 10Ox and analyzed 4/19/11. 

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

Page 28 of 98 
GLP10-01-02; Interim Report 17 

/Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

Table 17. GW 317L Q1 Y11 CP 

3M LIMS ID 

GLP10-01-02-17-017 

GLP10-01-02-17-018 

GLP10-01-02-17-019 

GLP10-01-02-17-020 

Description 

GW317LQ1 Y11 CPO 

GW317LQ1 Y11 CP1 

GW317LQ1 Y11 CPLS 

GW317LQ1 Y11 CPHS 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

0.0272 

0.0220 

1.15 

10.8 

VoRecovery 

NA 

NA 

113 

108 

0.0246 ng/mL ±21%'^' 

PFHS 

Concentration 

(ng/mL) 

0.121 

0.117 

1.24 

11.3 

VoRecovery 

NA 

NA 

112 

112 

0.119 ng/mL±3.4Vo 

PFOS 

Conceirtration 

(iig/mL) 

0.268 

0.231 

1.33 

8.77 

VoRecovery 

NA 

NA 

108 

85.2 

0.250 ng/mL ±15% 

NA = Not /Applicable 

Results for PFBS and PFHS reported fi^m 4/19/11 analysis. Results for PFOS reported from 5/14/11 analysis. 

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

Table 18. GW 324L Q1 Y11 CP 

3M LIMS ID 

GLP10-01-02-17-045 

GLP10-01-02-17-046 

GLP10-01-02-17-047 

GLP10-01-02-17-048 

Description 

GW 324L Q1 Y11 CP 0 

GW 324L Q1 Y11 CP 1 

GW 324L Q1 Y11 CP LS 

GW 324L Q1 Y11 CP HS 

Average Concentration (ng/mL) ± VoRPD . 

PFBS 

Concentration 

(ng/mL) 

113 

111 

236 

1210 

VoRecovery 

NA 

NA 

124 

110 

112 ng/mL ±1.8% 

PFHS 

Concentration 

(ng/mL) 

114 

108 

226 

1080 

VoRecovery 

NA 

NA 

115 

96.9 

111 ng/mL±5.4Vo 

PFOS 

Concentration 

(ng/mL) 

332 

299 

414 

1280 

VoRecovery 

NA 

NA 

NC 

96.5 

316 ng/mL ±10% 

NA = Not /Applicable 

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

Samples diluted 20x and analyzed 4/19/11. 

Page 29 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Table 19. GW 327R Q1 Y11 CP 

3M LIMS ID 

GLP10-01-02-17-073 

GLP10-01-02-17-074 

GLP10-01-02-17-075 

GLP10-01-02-17-076 

Description 

GW327RQ1 Y11 CPO 

GW327RQ1 Y11 CP 1 

GW327RQ1 Y11 CPLS 

GW327RQ1 Y11 CPHS 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

92.0 

94.5 

216 

1290 

VoRecovery 

NA 

NA 

123 

120 

93.3 ng/mL ±2.7% 

PFHS 

Concentration 

(ng/mL) 

169 

166 

308 

1130 

VoRecovery 

NA 

NA 

141(1) 

96.3 

168 ng/mL ±1.8%^ 

PFOS 

Concentration 

(ng/mL) 

591 

643 

652 

1480 

VoRecovery 

NA 

NA 

NC 

86.3 

617 ng/mL ±8A% 

NA = Not Applicable 

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

Samples diluted 50x and analyzed 4/19/11. 

(1) Field matrix spike did not meet method acceptance criteria of 100% ± 30%. 

(2) The analytical uncertainty has been adjusted for PFHS to ± 41 %. 

Table 20. GW 328R Q1 Y11 CP 

3M LIMS ID 

GLP10-01-02-17-061 

GLP10-01-02-17-062 

GLP10-01-02-17-063 

GLP10-01-02-17-064 

Description 

GW328RQ1 Y11 CPO 

GW328RQ1 Y11 CP 1 

GW328RQ1 Y11 CPLS 

GW328RQ1 Y11 CPHS 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

38.0 

40.0 

152 

612 

VoRecovery 

NA 

NA 

113 

115 

39.0 ng/mL ±5.1% 

PFHS 

Concentration 

(ng/mL) 

64.7 

61.5 

161 

516 

VoRecovery 

NA 

NA 

97.9 

90.6 

63.1 ng/mL ±5.1% 

PFOS 

Concentration 

(ng/mL) 

223 

210 

323 

677 

VoRecovery 

NA 

NA 

NC 

92.1 

217 ng/mL ±6.0% 

NA = Not /Applicable 

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

Sample, sample duplicate, and LS diluted lOx, HS diluted 20x, and analyzed 4/19/11. 

Page 30 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Table 21. GW 328L Q1 Y11 CP 

3MUMSID 

GLP10-01-02-17-057 

GLP10-01-02-17-058 

GLP10-01-02-17-059 

GLP10-01-02-17-060 

Description 

GW 328L Q1 Y11 CP 0 

GW328LQ1 Y11 CP 1 

GW 328L Q1 Y11 CP LS 

GW 328L Q1 Y11 CP HS 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

73.1 

70.7 

82.7 

189 

%Recovery 

NA 

NA 

NC 

117 

71.9 ng/mL ±3.3% 

PFHS 

Concentration 

(ng/mL) 

22.7 

21.9 

32.4 

123 

VoRecovery 

NA 

NA 

NC 

101 

22.3 ng/mL ±3.6% 

PFOS 

Concentration 

(ng/mL) 

1.42 

1.24 

9.38 

NA<^' 

VoRecovery 

NA 

NA 

80.5 

NA<^' 

1.33 ng/mL ±14% 

NA = Not /Applicable 

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

Samples diluted lOx and analyzed for PFBS and PFHS on 4/19/11. Results for PFOS reported firom undiluted samples analyzed on 5/14/11. 

(1) Sample was not analyzed since the spike level was not expected to be appropriate as compared to the sample concentration. 

Table 22. GW 330R Q1 Y11 CP 

3MUMSID 

GLP10-01-02-17-009 

GLP10-01-02-17-010 

GLP10-01-02-17-011 

GLP10-01-02-17-012 

Description 

GW330RQ1 Y11 CPO 

GW330RQ1 Y11 CP 1 

GW330RQ1 Y11 CPLS 

GW330RQ1 Y11 CPHS 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

2990 

3040 

3130 

4130 

%Recovery 

NA 

NA 

NC 

NC 

3020 ng/mL ±1.r/o^> 

PFHS 

Concentration 

(ng/mL) 

257 

261 

383 

1390 

VoRecovery 

NA 

NA 

NC 

113 

259 ng/mL ±1.5% 

PFOS 

Concentration 

(ng/mL) 

725 

715 

771 

1790 

VoRecovery 

NA 

NA 

NC 

107 

720 ng/mL ±1.4% 

NA = Not /Applicable 

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

Samples diluted 50x, with the exception of the HS sample which was diluted 10OX, and analyzed on 4/19/11. 

(1) Samples were coDected in bottles intended for GW 330L, which contained FMS samples at 100 ng/mL and 1000 ng/mL Bottles intended for GW 330R contained FMS samples at 1000 

ng/mL and 5000 ng/mL. /As a result, an appropriate field matrix spike was not available for PFBS. 

Page 31 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1 st Quarter Sampling - 2011 

Table 23. GW330LQ1 Y11 

3M LIMS ID 

GLP10-01-02-17-013 

GLP10-01-02-17-014 

GLP10-01-02-17-015 

GLP10-01-02-17-016 

Description 

GW 330L Q1 Y11 CP 0 

GW 330L Q1 Y11 CP 1 

GW 330L Q1 Y11 CP LS 

GW 330L Q1 Y11 CP HS 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

590 

499 

1670 

6290 

%Recovery 

NA 

NA 

113 

115 

545 ng/mL ±ir/o 

PFHS 

Concentration 

^ng/mL) 

677 

572 

1810 

6630 

VoRecovery 

NA 

NA 

119 

120 

625 ng/mL ±17% 

PFOS 

Concentration 

(ng/mL) 

233 

213 

1100 

5270 

VoRecovery 

NA 

NA 

87.7 

101 

223 ng/mL ±9.0% 

NA = Not/Applicable 

Samples diluted 20x, with the exception ofthe HS sample, which was injected at a volume to simulate a dilution of 125X, and analyzed on 4/19/11. 

Samples wsie collected in bottles intended for GW 330R, which contained FMS samples at 1000 ng/mL and 500 ng/mL Bottles Intended for C3W 330L contained FMS samples at 100 ng/mL 

and 1000 ng/mL 

Table 24. GW331SQ1 Y11 

3MUMSID 

GLP10-01-02-17-069 

GLP10-01-02-17-070 

GLP10-01-02-17-071 

GLP10-01-02-17-072 

Description 

GW331SQ1 Y11 CPO 

GW331SQ1 Y11 CP1 

GW331SQ1 Y11 CPLS 

GW331SQ1 Y11 CPHS 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

640 

476 

614 

1570 

%Recovery 

NA 

NA 

NC 

101 

558 ng/mL ±29%'^' 

PFHS 

Concentration 

(ng/mL) 

314 

269 

367 

1160 

VoRecovery 

NA 

NA 

NC 

86.9 

292 ng/mL ±15% 

PFOS 

Concentration 

(ng/mL) 

668 

615 

714 

1530 

VoRecovery 

NA 

NA 

NC 

88.9 

642 ng/mL ±8.3% 

NA = Not /Applicable 

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

Samples diluted 50x and analyzed on 4/19/11. 

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

Page 32 of 98 
GLP10-01-02; Interim Report 17 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Table 25. GW 335S Q1 Y11 CP 

3M LIMS ID 

GLP10-01-02-17-049 

GLP10-01-02-17-050 

GLP10-01-02-17-051 

GLP10-01-02-17-052 

Description 

GW 335S Q1 Y11 CP 0 

GW 335S Q1 Y11 CP 1 

GW 335S Q1 Y11 CP LS 

GW 335S Q1 Y11 CP HS 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

1100 

1060 

1220 

2420 

VoRecovery 

NA 

NA 

NC 

134'^' 

1080ng/mL±3.r/o^ 

PFHS 

Concentration 

(ng/mL) 

2050 

2000 

2130 

3310 

VoRecovery 

NA 

NA 

NC 

NC 

2030 ng/mL ± 2.5% f^' 

PFOS 

Concentration 

(ng/mL) 

5810 

6210 

5870 

7690 

VoRecovery 

NA 

NA 

NC 

NC 

6010ng/mL±6.7Vo^* 

NA = Not Applicable 

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

Samples diluted 50x for PFBS and PFHS, while samples were injected at a volume to simulate a dilution of 125x for PFOS and analyzed on 4/19/11. 

(1) Field matrix spike did not meet method acceptance criteria. 

(2) Tfie analytical uncertainty has been adjusted for PFBS to ± 34%. 

(3) /An appropriate spike level was not available to assess accuracy for PFHS and PFOS. 

Table 26. GW GRS04 Q1 Y11 CP 

3MUMSID 

GLP10-01-02-17-065 

GLP10-01-02-17-066 

GLP10-01-02-17-067 

GLP10-01-02-17-068 

Description 

GW GRS04 Q1 Y11 CP 0 

GW GRS04 Q1 Y11 CP 1 

GW GRS04 Q1 Y11 CP LS 

GW GRS04 Q1 Y11 CP HS 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

2090 

1950 

3290 

8310 

VoRecovery 

NA 

NA 

NC 

126 

2020 ng/mL ±6.9% 

PFHS 

Concentration 

(ng/mL) 

5540 

5170 

6510 

11800 

VoRecovery 

NA 

NA 

NC 

129 

5360 ng/mL ±6.9% 

PFOS 

Concentration 

(ng/mL) VoRecovery 

Not Reported 

Not Reported'^' 

NA = Not /Applicable 

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

Samples diluted 10Ox for PFBS and PFHS and analyzed on 4/19/11. Samples diluted 200x for PFOS and analyzed on 5/17/11. 

(1) Both the RPD and FMS recovery did not meet method acceptance criteria for PFOS. A result for PFOS will not be reported for this sampling location. See discussion in section 9 ofthe 

report for additional information. 

Page 33 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

Table 27. Trip Blank 1 

3M LIMS ID 

GLP10-01-02-17-001 

GLP10-01-02-17-002 

GLP10-01-02-17-003 

GLP10-01-02-17-004 

Description 

Trip Blank 1 Sample 

Trip Blank 1 Low 

Trip Blank 1 Mici 

Trip Blank 1 High 

PFBS 

Concentration 

(ng/mL) 

<0.0200 

10.5 

112 

1060 

VoRecovery 

NA 

105 

112 

106 

PFHS 

Concentration 

(ng/mL) 

<0.0400 

11.1 

116 

1110 

VoRecovery 

NA 

111 

116 

111 

PFOS 

Concentration 

(ng/mL) 

<0.500 

10.9 

103 

945 

VoRecovery 

NA 

109 

103 

94.5 

NA = Not Applicable 

FMS Mid diluted 10x, FMS High diluted 50x, and analyzed on 4/19/11. 

Table 28. Trip Blank 2 

3M LIMS ID 

GLP10-01-02-17-005 

GLP10-01-02-17-006 

GLP10-01-02-17-007 

GLP10-01-02-17-008 

Description 

Trip Blank 2 Sample 

Trip Blank 2 Low 

Trip Blank 2 Mid 

Trip Blank 2 High 

PFBS 

Concentrati'on 

(ng/mL) 

<0.0200 

10.4 

105 

1050 

VoRecovery 

NA 

104 

105 

105 

PFHS 

Concentration 

(ng/mL) 

<0.0400 

10.8 

108 

1120 

VoRecovery 

NA 

108 

108 

112 

PFOS 

Concentrati'on 

(ng/mL) 

<0.500 

11.0 

88.2 

962 

VoRecovery 

NA 

110 

88.2 

96.2 

NA = Not /Applicable 

FMS Mid diluted 10x, FMS High diluted 50x, and analyzed on 4/19/11. 

Page 34 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 2011 

Table 29. GLP10-01-02-17 Equipment Rinseate Blank 

3M LIMS ID 

GLP10-01-02-17-081 

Description 

Equipment Blank GRS04 

PFBS 

Concentration 

(ng/mL) 

<0.0200 

PFHS 

Concentration 

(ng/mL) 

<0.0400 

PFOS 

Concentration 

(ng/mL) 

<0.500 

Sample was analyzed on 4/19/11. 

Table 30. GLP10-01-02-15 Soil Equipment Rinseate Blanks 

3MUMSID 

GLP10-01-02-15-013 

GLP10-01-02-15-017 

GLP10-01-02-15-019 

GLP10-01-02-15-078 

Description 

DALSSSS15RB 

DALSSSS18RB 

DALSSSS10RB 

DAL SS SS26 RB 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

<0.0250 

<0.0250 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

<0.0250 

<0.0250 

PFOS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

<0.0250 

<0.0250 

Samples analyzed for PFBS and PFHS on 5/12/11. 

Samples analyzed for PFOS on 5/16/11. 

Page 35 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

10 Qamc^ion 

Laboratory control spikes and field matrix spikes were used to detennine the ana!ytic:al method 

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

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

\11 BatafBamipte Retention 

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

to 3M Environmental Laboratory standard operating procedures. 

12 /i0ac/mi&nts 

Attachment A: Protocol Amendment 17 (General Project Outline) 

Attachment B: Representative Chromatograms and Calibration Curves 

Attachment C: Analytical MethcxI 

Attachment D: Method Deviation 

Page 36 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1 st Quarter Sampling - 2011 

\13^^atttres 

M zoiL 

ClestonCange, Ph.D., 3M Principal Analytical Investigator Date 

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

-7/2 

Gary Hohenstein, Sponsor Representative Date 

Jaisimha Kes^, Study Director ' Date 

Page 37 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

ATTACHMENT A: PROTOCOL AMENDMENT 

Page 38 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

Analytical Protocol: GLP10-01-02 

Amendment 17 

Study Title 

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

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

Decatur Phase 3 Site-Related Monitoring Program 

PROTOCOL AMENDMENT NO. 17 

Amendment Date: 

March 14,2011 

Performing Laboratory 

3M Environmental, Health, and Safety Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55144-1000 

Laboratory Project Identification 

GLP10-01-02 

Sampling Event 

Decatur 1^' Quarter Groundwater Sampling 

Page 1 of 7 

Page 39 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Samolina - 2011 

Analytical Protocol: GLPf0^1-02 

Amendment 17 

This amendment modifies the following portion of protocol: 

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

Decatur Phase 3 Site-Related Monitoring Program" 

PROTOCOL READS: 

No changes to the wording ofthe protocol are required. 

AMEND TO READ: 

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

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

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

{GLP10-01-02). The anticipated sample collection will occur around the timeframe ofthe week of March 

21, 2011. The groundwater samples for this sampling event will be entered into the 3M Environmental 

Laboratory LIMS as project GLP10-01-01-17 and reported as interim report GLP10-01-02-17, (reflecting 

study GLP10-01-02 and amendment-17). 

Reason: 

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

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

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

Page 2 of 7 

Page 40 of 98 
Analysis of 

1st Quarter S^tJUfiif^rgfftfit 1 7 

Amendment Approval 

imi WM?^H 

Gary Hohenstein, Sponsor Representative Date 

^/f^k<DJ) 

Cleston C. Lange, Principal Analytical Investigator Date 

////9^0lC//^O// 

William Reagen, EHS Opns Environmental Lab Management 

\ihL 

Date 

2k\\\\ 

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

Page 41 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

Analytical Protocol: GLPlO-Ol-02 

Amendment 17 

Ki ' Environmental Health & Safety Operations, Environmental Laboratory 

C^s-Qsrn; ?i*o;2Gj 'Dcitlme 

To: Gary Hohenstein, 3M EHS&Opns 

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

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

Cleston Lange, 3M EHS&Opns; Environmental Lab 

Jai Kesari, Weston Solutions 

Charles Young, Weston Solutions 

Date: March 14,2011 

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 09- Decatur 1*'Quarter 2-11 

Groundwater Sampling 

1 General Project information 

Contacts 

Lab Request Number 

Six Digit Department Number 

Project Schedule/Test Dates 

3M Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

aahohenstein@mmm.com 

3M Environmental Laboratory Management 

William K. Reagen 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9739 

wkreaaenOmmm.com 

Principal Anaiyticai Investigator 

Cleston Lange 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9860 

cclanae(a)mmm.com 

Sampling Coordinator 

Timothy Frinak 

Weston Solutions 

Tlmothv.frinak@westonsolutions.com 

PtK)ne:(334)-332-9123 

GLP10-01^2-17 

Dept #530711, Project #0022674449 

Sampling scheduled for the week of IVIarch 21,2011 

Alt verbal and written correspondence mil be directed to Gary Hohenstein. 

Page 4 of 7 

Page 42 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Analytical Pmtocol: GLP10-01-02 

Amendment 17 

2 Background information and Project Objective(s) 

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

samples collected from seventeen groundwater wells for Perfluorobutanesulfonate (PFBS), 

Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS). 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 

March 21, 2011. The 3M Environmental Laboratory will prepare the sample bottles vvith ail 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-

17. 

3 Project Schedule 

Sample collection bottles will be prepared by the 3M Environmental Laboratory. Sample bottles will be shipped 

in ccKDlers overnight to 3M Decatur for anrival by Friday, March 18,2011. 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 vwll be 0.025 ng/mL (ppb) for PFBS, PFHS, and PFOS. 

A total of seventeen sampling locations have been specified. For each sampling location, four sample bottles 

will be collected (sample, sample duplicate, low field matrix spike, and high field matrix spike). The "fill to here" 

line on each 250 mL Nalgene bottle will be 200 mL. Four sets of trip blank spikes consisting of reagent-grade 

water, as well as an additional bottle to be used for the preparation ofthe equipment rinseate blanks, will be 

prepared at the 3M Environmental Laboratory and sent to the sampling location with the other bottles. Results 

from GLP10-01-02-02 and GLP10-01-02-09 were used to determine the field matrix spike levels for GLP10-01-

01-17 listed in Table 1. 

Table 1. Sampling Locations and Field Matrix Spike levels. 

Well No. 

317L 

220R, 220L. 328L 

203L, 222R, 227L, 227R. 

1 310R.324L,327R.330L. 

3313, 335S 

GRS04. 312R. 330R 

328R 

Trip Blank Sets 

1 and 2 

Sample Level 

Low 

High 

Low 

High 

Low 

High 

Low 

High 

Low 

High 

Low 

Mid 

High 

Spike Cone. (ng/mL) 

1 

10 

10 

100 

100 

1000 

1000 

5000 

100 

500 

10 

100 

1000 

Page 5 of 7 

Page 43 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 2011 

Analytical Protocol: GLPlO-ul-02 

Amendment 17 

5 Test Methods 

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

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

Analysis". Due to previous data for these sampling locations (GLP 10-01-02-02 and GLP10-01-02-09), samples 

GLP10-01 -02-17 will most likely require dilution. Samples requiring dilution will be prepared in Milli-Q water 

prior to analysis by ETS-8-044.0. The data quality objectives for these studies are quantitative results for the 

target analytes with an anaiyticai acxajracy of 100±30%. Field matrix spikes not yielding recoveries within 

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

/^temately, samples may be analyzed by ETS 8-110.1 "Analysis of Fluorochemicals in Extracts Using HPLCElectrospray-Mass Spectrometry-Mass Spectrometry" as an analytical reference for the sample locations 

analyzed by direct on-column injection analysis of samples diluted with methanol as opposeci to Milli-0 water. 

Calibration curves used for both ETS-8-044.0 and ETS-8-110.1 will be constructed using the linear isomer of 

PFOS only, fi"om nominal concentrations of 0.02 ng/mL -100 ng/mL. Due to the expected cxjncentration of 

linear + branched PFOS in the samples, there may be the potential for analytical bias due to quantitating linear 

and branched isomers of PFOS against a predominately linear reference standard for PFOS at the higher end 

of the calibration curve. Laboratory cont-ol samples (LCS) of linear + branched PFOS will be prepared at three 

concentrations to evaluate the potential for analytical bias. LCS witti average recoveries greater than 

100%±30%may suggest analytical bias. If tiie recovery ofthe linear + branched LCS is greater than 

100%±30% it may be necessary to quantitate PFOS by processing the linear and branched isomers separately 

and summing the calculated concentrations togeWier to generate the final PFOS concentration. This may be 

done to help minimize any potential analytical bias due to quantitating linear and branched isomers of PFOS 

against a predominately linear reference standand for PFOS. 

6 Reporting Requirements 

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

matrix spikes. Trip blank sets will be reported for the sampling event as will any equipment blanks prepared in 

tiie field. Laboratory conti-ol spikes of reagent water prepared at the time of sample extraction will also be 

reported and used to evaluate the overall method accuracy and precision. Method blanks of reagent water 

prepared attiie time of sample extinction will be used to detennine the method detection limit. Any laboratory 

matrix spikes fliat may be prepared will also be included in the final report 

7 Email Correspondence 

Attachment A: Sampling Bottle Request 

Page 6 of 7 

Page 44 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Analytical Protocol: GLP10-01-02 

Amendment 17 

203L 

220R 

220L 

222R 

227R 

227L 

Total N 

NOTE: 

Decatur FC Sample Locations (Ql 2011) | 

Confirmed Samples 

310R 3355 

317L GRS04 

324L 

328R 

328L 

330R 

330L 

umber of Samples: 

Rinsate Samples: 

Trip Blanks 

Potential Samples (See Note) 

RW312R 

RW327R 

RW331S 

18 

1 Water Needed: Yes 

2 

Groundwater samples will be collected from the recovery wells if the system 

is operating at the time of the sampling event. 

We are expected to begin sampling activities the week of 21 March 

Page 7 of 7 

Page 45 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

ATTACHMENT B: REPRESENTATIVE SAMPLE CHROMATOGRAMS AND 

CALIBRATION CURVE(S) 

Page 46 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Ginger AG01330509 Results Name: gll0419b.rdb 

g110419b.rdb (PFOS): "Quadratic" Regression ("1 / x" weigtiting): y = -2.83e+003 x''2 + 8.4e+005 x + 4.54e+004 (r = 0.9999) 

45 50 55 

Concentration, ng/mL 

100 

Data printed by STW 

Printing Time: 9:50:05 AM 

Printing Date: Monday, July 18 

Page 1 of 1 

Page 47 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 2011 

Ginger AG01330509 Results Name: gll0419b.rdb 

g110419b.rdb (PFHS): "Quadratic" Regression ("1 / x" weighting): y = -1.79e+003 x''2 + 5.66e+005 x + 3.34e+003 (r = 0 

45 50 55 

Concentration, ng/mL 

60 65 70 75 80 85 90 95 100 

Data printe d by STW 

Printin g Time: 9:49:1 3 AH 

Printin g Date : Monday, Jul y 18, 2011 

Page 1 of 1 

Page 48 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

»» Ginger AG01330509 Results Name: gll0419b.rdb 

Data printed by STW 

Printing Time; 9:45:26 AM 

Page 1 of 1 

Page 49 of 98 
Ginger AG01330509 

GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 2011 

Results Name: gll0419b.rdb 

I

SamptaN<tnM:'g11(M19b016' Sampta ID:-10007-27-r Fle:-g110419b.wirr 

P«ak Name: TFBS* Mass(«s): "299.0/99.0 Bmu.299.0/SO.O amu* 

Comment: '1.0 nsTmL FC std In MH Q water* Annotation: 

Sanple Index: 16 

Sample Type; Standard 

Concentration: 1.00 ng/nL 

Calculated Cone: 0.993 ng/nl. 

Acq. Date: 4/19/2011 

Acq. Tine: S:01:04 PH 

Modified: 

Pioc . Algorithm: 

Hin. Peak Height 

Smoothing Width; 

RT Mlndow: 

expecte d RT; 

Use Relativ e BT: 

Retentio n Tine : 

l e s 

IntelliOua n 

0.00 cp 

0.00 st 

12.1 mi 

No 

Manual 

12.0 mi 

Area : 295559 count 

Height: 

End Time: 

69BO0. cps 

11.9 mi 

12.2 ai. 

y 12/43 .,1238 '^^JSx. 

12.5 13.0 -

) 1240 12B9 

2:2 ^ 13.73 14.03 

13.5 14.0 

1339 1388 

14.33 

14.5 

143S 

I S3mptoNan»:*g110419b03r 

I pMkNameiTf^S- MaM{M 

Sample ID 

•299.0/99. 

• Comment -2ppb LCS' Anr>ot3tkm: " 

Sample Index : 31 

Sample Type: QC 

Concentration : 2.00 

Calculate d Cone: 2.17 

Acq. Date : 4/19/201 

Acq. Tine : 9:30:32 

Modified: Ho 

ng/mL 

ng/mL 

. PM 

Proc . Algorithm: IntelliOua n - 10, 

Min. Peak Height: 0.00 

Min. Peak Width: 0.00 

Smoothing Width: 0 

RT Window: 30.0 

Expected RT: 12.1 

Use Relativ e RT: Ho 

Int . Type: Valle y 

Retentio n Tine : 11.9 

Area: 643311 c 

Height: 142000. 

Star t Time: 11.8 

End Time: 12.2 

c p s 

points 

n i n 

m i n 

c p s 

m i n 

n i n 

1>*s5' 

1.4^' 

1.3»5 

1.3e5' 

1.2e5-

1.265' 

1.1e5-

l.laSI.0e5-

9.5e4-

g.0e4-

83M8.0M7.5e4-

7.0MB.5e4-

6.0M5.5e4-

5XM4.5e4-

4Xte4-

3.S©4-

3.0M2.5»4-

2.0»4' 

1.S«4-

1.0e4-

5000.0-

0.0-

1D42 

I

Sample Name: 'gl 10419t>034' Sample ID: l-CS-l 10412-10' Fla: 'g1104igb.witr 

P«ak Name:'PFBS' Mass(«):'299XV99.0nnu,299.0/80.0amuConwrtent "^ipb LCS ECP Annotation: ** 

Sample Index: 34 

Sanpl e Type: 

Concentrati o 

Acq. Tine : 

Modified: 

Proc . Algori 

Min. peak He 

Kin. Peak wj 

ihn: 

igh t 

tr.h: 

Smoothing Width: 

RT Window: 

Expected RT: 

• a e Relativ e 

Int . Type: 

Retentio n Ti 

Area : 

Height: 

R T : 

QC 

0.00 

4/19/20 

10:24:2 

Ho 

Intelll ' 

0.00 

0.00 

0 

30.0 

12.1 

No 

Valle y 

11.9 

n g / n l . 

ng/mL 

1 

2020. c p s 

QA 

1800 

17O0 

1B0O 

1500 

1300 

5" ^'""^ 

I 900-

I

Sample Name: •g1104l9bO3r Sample ID: •LCS-110412-4' Filo: 'fll 104l9b.wir 

PMkName:-W^S' MO»»(M):-299^1/99.0 

Comment •20ppb LCS' Annotation: -

Sample Index : 37 

Sample Type: QC 

20. 0 ng/mL 

Calculate d Cone: 20.6 

Acq. Date : 4/19/20 1 

Acq. Tine : 11:16:15 

ng/mL 

1 

Modified: Yes 

Proc . Algorithm: IntelliQua n -

Min. Peak Height: 0.00 cps 

Min. Peak Width: 0.00 sec 

Smoothing width : 0 poin 

RT HindOH: 30.0 sec 

Expected RT: 12.1 min 

Use Relativ e RT: tlo 

Int . Type: Manual 

Retentio n Tine : 11.9 

Area : 5822139 c 

Height: 1270000. 

Star t Time: 11.9 

End Time: 12.4 

cp s 

nin 

Bin 

I QA 

5 

1.25«6^ 

1.20e6J 

I.ISeSJ 

i.ioeej 

1.05«6J 

LOOefij 

9.50»5J 

9.00e5H 

8.50<i5J 

8.00e5J 

7.50*5 j 

7.00e5J 

6.50e5J 

e.00»5J 

5.50*5 j 

5.00e5J 

4.50e5 

4.00*5 j 

3.50*5 j 

3.00e5'] 

2.50e5J 

2.00«5J 

1.50*5 J 

1.00*5J 

5.00*4-] 

Dat a printe d by STW 

Printin g Time : 9:43:2 1 AM 

Page 1 of 13 

Page 50 of 98 
Ginger AG01330509 

GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 2011 

Results Name: gll0419b.rdb 

I

Sampto Nama:'g11O419b045' SwiptolOiTCS-llcmZ-ir Fk:'g l ttMISb.wiT 

P«ak NBIIM: T f BS* Ma3S(«s): '2S9JVg9.0 aimt^9SJOieO.O amu* 

Coinmenf20ppbLCSECF- Annotalion:-

Sanple Index: 15 

Sample Type: 

Concentration : 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modi(led: 

Proc . Algorithm: 

Min. Peak Height 

Hin. Peak Width: 

Smoothing width ; 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type: 

Retentio n Tine : 

Height : 

QC 

O.OO 

0.229 

4/20/2O11 

l:41:5B AH 

No 

IntelliQua n 

0.00 c 

0.00 s 

30. 0 s 

12. 1 n 

Ho 

Valle y 

12.0 n 

9130 coun 

15100. cps 

1.1*4 

1.0*4 

9500.0 

9000.0 

B500.0 

% 8000.0 

& 7500.0 

I 7000.0-

~ 8500.0 

6000.O 

5500.0 

5000.0-

4500.0 

4000.0 

3500.0 

3000.0-

2500.0-

2000il1500.0-

1000.0-

500,0-

0.0- +*..^*^^^!L_^ ^ 

I Samp)eName:*g11O419b075- Sampl«ID:'GLP1041-02-17<O0g^ Rla:-'gll0419b.vnfr 

P«ak Name: TFaS" Mass(*s): '299.0^99.0 amu,299.0/80.0 amu' 

I Comment'GWSSORQIYIICPOtSOX)* Annolation:-

anple Index: 75 

3.0*6 

2.9*6 

2.8*6 

2.7*6 

2.6e6 

2.506-

2.4*6 

2.3*8 

2.2*6 

2.1*6-

2.0*6-

1.9*6 

1.8*6 

1.7*6-

1.6*6-

1.5*6-

1.4*8-

1.3*6-

1.2*6-

1.1*6-

1.0*6-

9.0*5-

&0*S7.0*5-

8.0*5-

5.0*5-

4.0*5-

3.0*5-

2.0*5-

11.0 11.5 12.0 12.5 13.0 13.5 14.0 14.5 

1091 1141 1190 1240 1289 1339 1388 1438 

Tim*, rrin 

TSii;,pl«Nam*:'g1104i9b061'" &i ^ D:-GLPIMI-OTIT:*)!- Fll*:'a11041*.wir 

I PaalcN3me:-PFBS- Mau<*9):-299JV99.0 amu.299.<VB0Jl amu' 

• Commwit Trip BJank 1 Sampla' AnootaBoo: -

Sample Index: 61 

Sanpl e Type: Onknovn 

Concentration : H/A 

Calculate d Cone: < 0 

Acq. Date : 4/20/2011 

Acq. Time: 6:29:25 AM 

Modified: Ho 

Proc . Algorithm: IntelliOua n - IQA 

Min. Peak Height: 0.00 cps 

Hin. Peak Width: 0.00 se c 

Smoothing width : 0 points 

RT Window: 30. 0 se c 

Expected RT: 12. 1 min 

U»e Relativ e RT: Ho 

Int . Type: Base To Base 

Area : 557 counts 

Height: 240. cps 

Star t Time: 11.9 min 

End Tine : 12.0 ni n 

950 

80 

es -

Sampl*Nams:-g11O419b089' Sampte ID:-GLPia-01-02-17-0ir Fil*: •fl110419b.wtr 

P*ak Name: 'FTBS- Ma«l*a): •299.0/99.0 amu.299.0/80.0 amu" 

Concentration : 

Calculate d Cone. 

Acq. Date: 

Acq. Tine : 

Modified: 

proc . Algorith n 

Min. Peak Heighi 

Min. Peak Width: 

RT Window: 

Expected RT: 

Ose Relativ e RT: 

Int . Type: 

Retentio n Tine : 

Area : IS 

Height : 

Star t Time: 

Unknown 

N/A 

2990. 

4/20/20 1 

10:41:14 

Yes 

Intelll Q 

: 0.0 0 

0 

30. 0 

No 

Manual 

12. 0 

L25849 

3080000. 

11.9 

• Comment'GW317LQ1 

Sanple Index: 89 

Sanple Type: Unknown 

Calculated Cone: 0.0272 

Acq. Date: 4/20/20: 

Acq. Tine: 2:53:1 

Modified: Ho 

Proc. Algorithm: Intell 

Min. Peak Height: 0.0' 

Min. Peak width: O.Oi 

Smoothing width: 0 

RT Mlndow: 30.0 

Expected RT: 12. 

Use Relative RT: Ho 

CP 0' Annotation:" 

12.84 13.11 13.48 ^13.88 14.15 14.SS^, 

11.0 11.5 12.0 12.5 13.0 13.5 14-0 14.5 

1091 1141 1190 1240 1289 1339 1388 1438 

TTm*. min 

2100 

2000 

1900 

1800 

1700 

1600 

1500 

1400 

1300 

1100 

1000 

900 

800 

700 

SOO 

500 

400 

300 

200 

100 

0 UtK! ^ im^ikmfiJ* W/ \ h 

Data printed by STW 

Printing Time: 9:43:21 AM 

Page 2 of 13 

1190 1240 1289 

Page 51 of 98 
Ginger AG01330509 

GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Results Name: gll0419b.rdb 

I

SamplBNama:'g110419b094- Sampla ID:'GLP10-01-02-17-021- RIe:'g110419b.Mr 

Peak Name: "PFes* M3ss(*s): -299Xif99.0 amu,299.0/80.0 amu" 

CommanfGWaiORQIYIICPOOOOX)' Anfwlatten:^ 

Sample Index: 94 

Sanple Type: Unknown 

Concentration: H/A 

Calculated Cone: 836. ng/nL 

Acq. Date: 4/20/2011 

Acq. Tine: 4:23:15 PM 

I

SampI* Nam*: 'g110419b1ir Sample ID: 'GLP10-01-02-

P*ak Nam*: -PFBS- Masft(as): "299.0^9.0 amu,299.0/80j 

Comment: 'GW 220R 01 Y11 LF 0 (SXf Annotaflon: -

Sample Index: 117 

Sanple Type: Unknot 

I

Sampla Nam*: •g110419b103- Sample D: •GLPKW31-02-17-025' Fil*:'gl10419b.wtfr 

P«al( Nam*: TFBS' Uassfas): -299.0/99.0 amu.299.0/80.0 amu' 

Comm«nt'GW227LQ1 Y11LF0(20X)' Annotalion:-

Sanple Index: 103 

Unknown 

H/A 

286- ng/nL 

4/20/2011 0^. 

7:04:56 PM "•'•^^ 

Sanple Type 

Concent rat: 

Calculated 

Acq. Date: 

Acq. Tine: 

Yes 

proc. Alg< thn: IntelliQuB 

Hin. Peak Height 

Hin. Peak Width: 

Expected RT: 

Use Belativt 

Int. Type: Manual 

Retention Tine: 12.0 nin 

Area: 4103922 counts 

Height: 848000. cps 

Cone N/A 

Modified: 

Proc. Algorithn: 

Min. Peak Height 

Min. Peek Width; 

Snoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Retention Tine: 

Area: 5 

Start Tina: 

End Tine: 

Yes 

IntelliQu 

: 0.00 

0.00 

0 

30.0 

12.1 

No 

Manual 

12.0 

10706 CO 

,09000. c 

11.3 

12.1 

I

SamploNama:-Bl10419b136' Sampte ID: •GLP1CW)1-02-17-O45" FMe:'fl110419b.wirr 

P*ak Mama: 'PFBS' Mau(*s): '299.0/99.0 amu,299JV80.0 amu' 

Comment "GW324LQ1Y11CP0(20X)' Arawtalion:-

Sanple Index: 136 

Sanple Type: Unknown 

Calculated Cone: 113. ng/nL 

Acq. Date: 4/21/2011 

Acq. Tine: 4:59:05 AH 

Proc. Algorithm: IntelliQuan - IQA 

Min. Peak Height: 0.00 cps 

Hin. Peak Width: 0.00 sec 

RT Window: 30.0 sec 

Expected HT; 12.1 min 

Use Relative RT: Ho 

Int. Type: Manual 

Area: 165239B counts 

Height: 339000. cps 

End Tine; 12.3 min 

1141 1190 1240 

Jjm*. min 

Data printe d by STW 

Printing Time: 9:43:21 AiM 

Page 3 of 13 

Page 52 of 98 
Ginger AG01330509 

GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 2011 

Results Name: gll0419b.rdb 

I

Sarr ^ Name: *g1104196150' Sampla ID: 'GLP1001-02-17-053' File: *g110419b.wHr 

Peak Nam*: -PFBS* Ma3s(e3): •299.0/911.0 amu.299.Qno.O amuConf«n*nt:'GW203LQ1Y11LF0{20X)' AnnotaUoo:" 

Sample Inde: 

Sample Type 

H/A 

Calculated Cone; 106. 

Acq. Date: 4/21/2011 

Acq, Tine: 9:11:16 AH 

ng/iaL 

Modified: 

Proc. Algor 

Min. Peak H. 

Min. Peak W» 

Snoothing W: 

RT Window: 

Expected RT 

Use Relative 

Int. Type: 

Retention Ti 

Height: 

Start Tine: 

Lhm; ; 

ight: 

dth: 

RT: 

Yes 

ntelllQuan 

0.00 

3 

30.0 

12.1 

Ho 

Manual 

12.0 

1555 949 

3000. 

11.e 

cp 

poi 

mi 

cps 

nl 

I

Sampte Name: 'g110419b178' Sampte ID: 'GLP1(KI1-<I2-

P*Bk Nam*: -Pf BS" Mass(*s): '299.0/99.0 amu,299.0/80. 

Comment*GW331SQ1 Y11CP0{50X)' Annotatton:" 

Sample Index: 17S 

Sample Type: Unknown 

Cone: 640. ng/ml. 

Sampte Name:'o11041«>164' San^te ID:'GLP1(M)1-0M7-06r 

Paak Nam*: "PFBS* Maudes): "299.0/99.0 amu,2»9JV80.0 amu' 

CommanC *GW 32BR Ql Y11 CP 0 (lOX)' Annotation: ~ 

Sanpl e Index : 164 

Sanple Type: 

Concentration: 

Calculated Cone: 

Acq. Date: 

Acq. Time: 

MOdllied: 

Proc. Algorithm: 

Hin. Peak Height 

Hin. Peak Width: 

Smoothing width: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

Unknown 

H/A 

4/21/2011 

1:23:19 PM 

Yes 

IntelliQua 

0.00 

0 p 

30.0 

Ho 

Manual 

12.1 I 

Sampte Name: •g110419bier Sampte ID:'GLP 10-01-02-17-073' Fil*: •fl110419b.wir 

P*ak Nam*: 'PFBS' Mass(*s): •299.(V99.0 amu.299.0/e0.0 amu' 

Comment'GW327RQ1Y11CP0{50X)' Annotation:" 

Sample Index: 167 

Sample Type: Unknown 

Conct 

Acq. Date: 

Acq. Tine; 

Modified: 

Proc. Algor 

Min. Peak H 

Smoothing K 

RT Window: 

Expected RT 

Use (talativ 

Retention T 

Area: 

Height: 

Start Tine: 

End Time: 

4/21/20 

5:35:25 PM 

Yes 

thm: IntelliQuan - IQA 

ight: 0.00 cps 

dth: 0.00 sec 

dth: 0 points 

30.0 sec 

12.1 min 

RT: No 

Manual 

ne: 12.1 

36B7404 

a33000. 

11.9 

12.* 

min 

cps 

min 

J 

6.0*5 

7.5*5 

7.0*5 

e.5e5 

6.0*5 

5.5*5 

5.0*5 

4.5*5 

4.0*5 

3.5*5 

3.0e5 

2.5*5 

2.0*5 

ng/raL 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algorithn: 

Hin. Peak Height 

Min. Peak width: 

Smoothing Width: 

RT Window: 

Use Relative RT: 

Int. Type: 

Retention Time: 

4/21/2011 

8:17:25 PM 

Ho 

IntelliQua 

: 0.00 

0.00 

30.0 

Ho 

Valley 

Area: 54542B cou 

Height: 

Start Tine: 

End Tine: 

113000. cp 

11.9 

12.3 

1.0*5 

5.0*4 

Data printed by STW 

Printing Time: 9:43:21 AM 

12.0 12.5 

1190 1240 

Page 4 of 13 

Page 53 of 98 
Ginger AG01330509 

GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Results Name: gll0419b.rdb 

I I I SanvteNama:*g1lO410b19r Sampte ID:'GLP1(M>1-02 

1 Peak Nam*: "PFBS* M8sa(es): "299.0/99.0 amu.299.0/80 

• Comment'GW312RQ1Y11 CPO(lOOX)' Annotatton: " 

Sample Index: 192 

Sample Type: Unknown 

Concentration : H/A 

Calculate d Cone: 1170. ng/mL 

Acq. Date : 4/21/201 1 7.0*5 

Acq. Tine : 9:47:23 PM 

Modified: Yea .5 ^ 

Proc . Algorithn : IntelliQua n - IQA 

Min. Peak Height: 0.0 0 cp s 

Min. Peak Width: 0.0 0 se c 

Snoothin g Width: 0 points O-"** 

RT Window: 30. 0 se c 

Expected RT: 12. 1 min 

Use Relativ e RT: Ho 5.5*5 

Int . Type: Manual 

Retentio n Tine : 12. 1 min 50- 5 

Area : 3376396 counts 

Height: 738000. cps 

1 4.0.5 

1 3.5*5 

3.0*5 

2.5*5 

2.0*5 

1.5*5 

1.0*5 

5.0*4 

• Peak Name: -PFHS* Mass(*s}: '399.cra9.0 amu.399.0/80 

• Comment •2ppb LCS" Anrwtalion:" 

Sample Index: 31 

Sample Type: QC 

Concentration : 2.00 ng/mL 

Calculate d Cone: 2.22 ng/mL 

Acq. Date : 4/19/201 1 3.0*5-

Acq. Time: 9:30:3 2 PM 

Modified: Bo 2.8*5 

Proc . Algorithm; IntelliQua n - IQA 

Hin. Peak Height: 0.0 0 cps 

Hin. Peak Width: 0.00 se c 2.6*5 

Snoothin g Width; 0 points 

RT Window: 30. 0 se c 

Expected RT: 13.2 min 2.4*5 

Int . Tipe : Valle y j , _, 

Retentio n Tine : 13. 1 ni n •"" " 

Area : 1253265 counts 

Height : 315000. cps , - , 

Star t Tine : 13.0 ni n ''""' ' 

End Tine : 13.4 min 

1.8*5 

1 '•"' 

1 1-4*5 

1.2*5-

1.0*5-

8.0*4-

6.0M4.0*4-

2.0*4-

17-07r Fa*:'g110419b.wtr 

Oamu" 

12 07 

1 1 

10.0 10.5 11.0 11.5 12. 1 0 12.5 13.0 

992 1042 1091 1141 1190 1240 1289 

• F*.:-8l10419b.*«r 

Oamu13 11 

I 

lij) 11.5 12.0 12.5 13.0 li s 14.0 

1091 1141 1190 1240 1289 1339 1388 

aia.n-5 

13.5 14.0 

1339 1388 

14.5 15.0 

1436 1488 

14.5 

1438 

153 

1537 

• Sampte NanM:'g110419t)016' Sampte 10:'10007-27-6* F0e:'g110419b.wir 

I P*akName:TFH5* Mass<*s): "399.0/99.0 amu,399.0/80.0 amu* 

• Comment'l.OngnnLFCstdinhliliOwatBr' Amotation:-

Sanpl e Index : 16 

Sanpl e Type: Standar d 

Concentration : 1.00 ng/nL 1.4e5T 

Calculate d Cone: 1.05 ng/nL j 

Acq. Date : 4/19/2011 1.4«>| 

Acq. Time: 5:01:04 PM ^2e5 ^ 

Hodified : Ho 1.3*5 

Proc . Algorithn : IntelliQua n - IQA 

Hin. Peak Height: 0.0 0 cps l-^eS 

Hin. Peak Width: 0.00 sec ,, , 

Smoothing Width: 0 points 

RT Window: 30. 0 sec 1.1,5 

Expected RT: 13.2 min 

Use Relativ e RT: Ho 1.1*5 

Int . Type: Valle y ^-^ ^ 

Retentio n Tine : 13.2 nin -, c-i 

Area : 597629 counts "-" ^ 

Height: 140000. cps go M 

Star t Tine : 13.0 nin 

End Tine : 13.4 min 83*4 

8.0*4 

J 7.5*4 

& 7.0*4 

1 6.5*4 

~ 6.0*4 

5.5*4 

5.0*4 

4.5*4 

4.0*4 

3.5*4 

3.0*4 

23*4 

2.0*4 

13*4 

1.0*4 

5000.0 

0.0 

11X1 113 

1091 1141 

• SampteHama:-a11O119b034' Sarrvte 10:ICS-110412-0* Fite:-ol10419b.wffl-

• Peak Nam*:-PFHS' Mas3(*s): *399.0/99.0 smu,399.0/80Jl amu-

• Comment •2ppb LCS ECP Annotation: -

Sanpl e Index; 34 

Sample Type: QC 

Concentration : 0.00 ng/nL 13»4-i 

Calculate d Cone: 0.120 ng/nL j 

Acq. Date : 4/19/2011 ^•*^ 1 

Acq. Tine : 10:24:2 3 PM ^^t^ l 

Hodified : Yas 13M 

Ptoc . Algorithn : IntelliQua n - IQA 

Hin. Peak Height: 0.0 0 cps ^-'** 

Min. Peak Width: 0.00 sec i.2e4 

Smoothing Width: 0 points 

RT Window: 30. 0 sec 1.2e4 

Expected RT: 13.2 min 

Use Relativ e RT: Mo ^'^ ^ 

Int . type : Hanual 

Retentio n Time: 13.1 min 1.0*4 

Heigtit: 14500. cps ^^00. 

r.rizi-^- li.i T. »«»•'> 

8500.0 

8000.0 

0 7500.0 

1 7000.0 

E 6500.00 

5500.0-

5000.0 

4500.0-

4000.0 

3500.0-

3000.0 

2500J}-

2000.0-

1500.0-

1000.0-

500.0-

11.0 113 

1091 1141 

12.0 

1190 

12.0 

1190 

123 

1240 

123 

1240 

13,17 

13.0 13.5 

1289 1339 

1 J 13J) 

1289 

—ms 

I^Cvf^t^ 

13.5 

1339 

14.0 

1388 

...tK. 

14.0 

1388 

14.5 15.0 15.5 

1438 1488 1537 

W^"Ww ^ 

143 15i) 15.5 

1438 1488 1537 

Data printed by STW 

Printin g Time : 9:43:2 1 AM 

Page 5 o£ 13 

Page 54 of 98 
Ginger AG01330509 

GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Results Name: gll0419b.rdb 

I

Sani(itoNani«:-g11041SbO3r Sani|itolD;\CS-110412'^- FHa;-gl 10419b.vritr 

PvafcNainaiTFHS- Man(n): *399.a«9.0 amu.399.0/80.0 amuCommant •20Mib LCS- Annoiatlwi:" 

Sample Index: 37 

Sample Type: 

Concentration: 

Calculated Cone 

Acq. Date; 

Acq. Tine; 

Proc. Algorithm 

Hin. Peak Heigh 

Hin. Peak Width 

Snoothing width 

Expected RT: 

Use Relative RT 

Int. Type; 

Retention Tina: 

Height: 

End Tine: 

QC 

20.0 

21.1 

4/19/20: 

11:18:15 

ng/mL 

ng/nL 

1 

PM 

IntelliQuan - IQA 

: O.OO 

O.OO 

0 

13.2 

No 

Manual 

13.1 

15e6S4 

2620000. 

13.6 

points 

min 

eps 

min 

2.6*(-] 

2.4*6-

2.2*6 

1.9*6 

1.8*1 -

I

Sampte Name: 's110419b045' Sampte Uy. -LCS-110412-13* File: *g110419b.wtr 

Paak Name: -PFHS' Man(es); *3S9.0/9gj> amu,399.0/80.0 amu* 

Comment'20ppb LCS ECP' AmoCatton:" 

Sample Index: 45 

Sample Type: 

Concentration: 

Acq. Date: 

Acq. Time: 

Hodified: 

Proc. Algorithm: 

Hin. Peak Height 

Hin. Peak Width: 

Snoothing width: 

RT Mlndow: 

Expected RT: 

Use Relative RT; 

Retention Time: 

Area; 6' 

Height; : 

Start Time: 

End Tine; 

QC 

0.00 ng/nL 

4/20/2011 

l;41:58 AM 

Ho 

IntelliQuan -

0.00 sec 

30.0 sec 

13.2 min 

13.1 min 

32000. cps 

12.9 min 

13.4 min 

TOA 

i 

1.2*5-

1.2*5-

1.0*5 

9.0* : 

83* : 

7.5*4-

7.0*4-

8.5»t6.0*4-

53*4-

5.0*4-

4.5*4: 

4.0*4: 

33e4: 

3.0*4: 

23*4: 

2.0*4: 

13*4: 

I

SampteName:'g110419bD75' Sampte ID:'GLP1041-02-17-009* Fite:'g110419b.wi(r 

Peak rtema: 'PFHS' M3»(ea}: -399.0/99.0 amu.399.OfB0.0 am ' 

Comment 'GW 330R 01 Y11 CP 0 (SOX)' Annotatton: -

Sanpl e Index: 75 

Sanpl e Type: Unknown 

123 13.0 13.5 14.0 143 15J) 

1240 1289 1339 1388 1438 1488 

TTm*. min 

I

Sampte Name: 'g110419bO6r Sampte ID: 'GLPi 04)1-02-17-001' 

Paak Nam*: -PFHS' Ma»«(*«): '399.099.0 amu,399.0/80.0 amu' 

Comment: Trip Blank 1 Sarnpte* ArYtotatton: ~ 

Sample Index: 61 

Sample Type: Unknown 

Concentration : H/A 

Calculate d Cone; < 0 

Acq, Date : 4/20/201 1 

Acq. Tine : 6:29:25 AM 

Proc. Algorithm; 

Hin. Peak Height 

Hin. Peak width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type; 

Retention Tine: 

Height: 

Start Tine: 

End Tine: 

Intelli 

O.OD 

0.00 

30.0 

13.2 

No 

Valley 

2277 

528. 

13.0 

13.2 

3uan -

min 

cps 

Bin 

min 

IQA 

5 

f 

257. 

Modified: 

Proc. Algorithn: 

Min. Peak Height 

Hin. Peak width: 

Smoothing Width: 

RT Window: 

Expected RT; 

Use Relative RT: 

Retention Tine: 

Ho 

IntelliQu 

: 0.00 

0.00 

30.0 

13.2 

Ho 

Valley 

13.2 

Area: 286BB43 co 

Height: 594000. Cf 

5.8*5-

5.6e5 

5>4*5-

5.2e5 

5.0*5-

4.8*5-

4.6*5' 

4/4*5-

4.2*5-

4.0*5-

34*5 

3.6*5 

3.4*5-

3.2ft5 

3.0*5-

23*5-

2.6a5 

2.4*5-

2.2*5-

2.0*5-

1.8*5-

1.6*5-

1.4*5-

1J2e5-

1.0*5-

8.0*4-

6.0*4-

4.0*4-

2.0*4-

13.0 13.5 

1289 1339 

TTm*. min 

Data printe d by STW 

Printing Time: 9:43:21 AM 

Page 6 of 13 

1240 1289 

Tlm*.mtn 

14.23 1430 14.7S..14.65 15.41 

1388 1438 1488 1537 

Page 55 of 98 
Ginger AG01330509 

GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Results Name: gll0419b.rdb 

I

SamptoNaffl«:'g11M19b089- SamftolD:'GLP1CM)1^)2-17.0ir ni«:-g11M19b.w 

P«ak Nat^a:-PFHS- Mas3(m):-399.0/99.0 aiTHi.399.0/80 J) aimr 

C«TMTwnfGW317LQ1 Y11CP0- Annolatlon: " 

Sample Index: 89 

Sample Type: 

Concentration: 

Calculated Cone: 

Acq. Date: 

Acq. Time: 

Modified; 

Ptoc. Algorithn: 

Min. peak Height 

Hin. Peak Width: 

Smoothing Width: 

R? Window: 

Expected RT; 

Use Relative RT: 

Int. Type: 

Retention Time: 

Height: 

Start Time: 

End Time; 

Unknown 

H/A 

0.121 ng/nL 

4/20/2011 

2:53:14 PM 

IntelliQuan - IQA 

0.00 cps 

0.00 aec 

0 pointa 

13.2 min 

Ho 

Hanual 

13.2 min 

71966 counts 

14000. cps 

13.0 min 

13.3 min 

1 

1.4*4 

1.4*4 

1.3*4 

1.3*4 

1.2*4 

1.2*4 

1.1*4 

1.1*4 

1.0*4 

9500.0 

9000.0 

8500.0 

8000.0 

7500.0 

7000.0 

6500.0 

6000.0 

5500.0 

5000.0 

4500.0 

4000.0 

3500.0 

3000.0-

2500.0 

2000.0-

1500.0 

1000.0 

500.0 

0.0 

11.0 

1091 

JKm^m.iry^J'f^ Z^^''*'^*''''^*^*:^****^' i^^p^t H»»»» ^A/^Y*^ 

13.0 13-5 14.0 14.5 15.0 15J 

1289 1339 1388 1438 1488 1537 

Time, min 

I

Sampte Name:-o11041«)094' Sampte ID:'6LP1(KI1-02-17-021' 

Paak Nam*:'PFHS' Mas3(*s):'309.0/99J) emu,399.0/&0.0 

Comment'GW310RQ1Y11 CPO(lOOX)* Annotation:" 

lanple Index: 94 

iample Type 

H/A 

4 6E. ng/n 

Acq. Date: 

Acq. Tine: 

Hodified: 

Proc. Algorithm: 

Min. Peak Height: 

Hin- peak Width: 

Snoothing Width: 

RT Window: 

Expected RT: 

4/20/2011 

4:23:15 PM 

Yes 

IntelliQuan 

0.00 c 

0-00 s 

0 po 

30.0 s 

13.2 m 

I Sampte Nam*:'g110419b1ir Sampte ID:'GLP 1W»1-02-17-033' Fite:'g110419b.wir 

Peak Nam*:-PFHS* Mass(*s):'399.0/99J) amu.3dd.0/80.0 amu' 

I Comment:'GW220RQ1Y11 LFO(5X)" " 

12.5 13.0 13-5 14.0 14.5 15J1 15.5 

1240 1289 1339 1386 1438 1488 1537 

Sampte Name!-g110419b103* San ^ ID: 'GLP1<M> 1-02-17-025' Flte: 'g110419b.wtr 

Paak Nam*: -pFHS' Mass(e«): -SgO-OM-O amu,399.0/80i) amu" 

C«»jment:'GW227LQ1Y11LF0 ~ 

Sample Index: 

Sample Type: 

Concentration; 

Calculated Cone: 

Proc. Algorithm: 

Min. Peak Height 

Min. Peak Width: 

Smoothing Width: 

Jse Relati\ 

Int. Type; 

Sample Index: 

Sanple Type: 

Concentration: 

Calculated Cone: 

Acq. Time: 

ModifiedProc. Algorithm: 

Min. Peak Height 

Min. Peak width; 

Smoothing Width: 

fit Window: 

Expected BT: 

Use Relative RT; 

Int. Typo: 

117 

Unknown 

M/A 

35.1 

4/20/2011 

11:17:23 PM 

Yes 

IntelliQuan 

0-00 c 

0.00 J 

30-0 a 

13.2 m 

Ho 

Hanual 

Area: 3888265 coun 

Height: 

Start Time: 

17000. cps 

12.9 m 

12B9 1339 1388 1438 

Data printed by STW 

Printing Time: 9:43:21 

""'^•'^ " 

Page 7 of 13 

12.5 13.0 13.5 14.0 14.5 15.0 15.5 

1240 1289 1339 1388 1438 1466 1537 

Tlm*),[pln 

AM 

Page 56 of 98 
*** Ginger AG01330509 

GLP10-01-02; Interim Report 17 

Analysis of PFBS. PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 2011 

Results Name: gll0419b.rdb 

I

Sampte Name: *g11041%136' Sampte ID: 'GLPI(Ml 1-02-17-045' Flte: -g1104l9b.' 

Peak Name: *PFHS' Maeefes): *399.Ck'99.0 amu.399.0/80.0 amu" 

Comm*nt:'GW324LQ1Y11CP0(20X}' Annotation: 

Sample Index; 136 

Sample Type: Unknown 

Concentration; H/A 

Calculated Cone: 114. ng/mL 

Acq. Date: 4/21/2011 

Acq. Tine: 4:59:05 AM 

6.0*5-

Proc- Algori 

Min. Peak Hi 

Smoothing M: 

RT Window: 

Expected RT 

Int. Type: 

Retention T: 

Area: 

Height: 

thn: intelliO 

ight: 0.00 

dth: O.OO 

dth: 0 

30-0 

13.2 

RT: No 

Valley 

3183545 c 

620000. 

5.5*5-

Sampte Name;-g110419b164- Sampte ID:'GLP10-01-02-17-061* Rte:'g110419b.wtrr 

Paak Nam*:'PFHS' Mass(*8):-399^199.0 anfxi.399.0ra0.0 amir 

Co«nm*nt:'GW32BRQ1 Y11 CP0{10X)' " • -

sanple Index: 164 

Sanple Type: Unknown 

Concentration: N/A 

Calculated Conc: G4.7 

Acq. Date: 4/21/201 

Acq. Tine: 

Modified: yes 

Proc. Algorithm: IntelliQuan 

Hin- Peak Height: 

Min. Peak width; 

Snoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT; 

Int. Type: Hanual 

Retention Tine: 13.2 

Area; 3592726 

Height: 721000-

Start Time: 13.0 

End Time: 13.6 

1141 1190 

I

SanipteNam*:-g110419b150' Sampte ID:•GLP1tM)1-02-17-053' Flte:'g110419b.wi(r 

Peak Name: "PFHS- M«s8(*i): •399.0^9.0 amo,399.0«0J) amu" 

Comment *GW203LQ1Y11 LFO (20Xr Annotation:" 

Sample Index: 150 

Sanple Type: Unknown 

H/A 

Calci 601, 

Acq. Date: 

Acq. Time: 

Hodified: 

Proc. Algorithm; 

Min- Peak Height 

Hin. Peak Width: 

Smoothing Width; 

RT Window: 

Use Relative RT; 

Int- Type: 

Retention Time: 

4/21/2011 

9:11:16 At 

Ho 

IntelliQu 

: 0.00 

0.00 

0 

30.0 

13.2 

tlo 

Valley 

13.2 

Area: 15403694 c 

Height: 3000000. 

ng/ti 

12.5 13.0 13.5 14.0 

1240 12B9 1339 1388 

Time, min 

I

Sampte Mame:'fl110419b178' Sampte ID: •GLP1OO1-02-17-069' Fite:'g1104l9b.wir 

Peak Name: -PFHS' Mass(*s}: '399.0/99.0 amu.399.0/80.0 

Commem:'GW331SQ1 Y11CP0{50X)' Annotation:-

Sample Index: 178 

sample Type: 

Concentration: 

Calculated Conc: 

Acq. Date: 

Acq. Time; 

Modified: 

Ptoc- Algorithn; 

Hin. Peak Height 

Min. Peak Width; 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time; 

Area: 34 

Height: 

Start Time; 

End Time: 

Unknown 

H/A 

314-

4/21/2011 

5:35:25 PM 

(lo 

IntelliQuan 

0.00 c 

0.00 a 

0 po 

30-0 B 

13.2 m 

Ho 

Valley 

13.2 n 

1623 coun 

96000. cps 

12.9 m 

13.6 m 

Data printed by STW 

Printing Tims: 9:43:21 AM 

Page 8 of 13 

Page 57 of 98 
Ginger AG01330509 

GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Results Name: gll0419b.rdb 

|llSampteName:'fl110419bia r Sampte ID: •GLP1.>^11-02-17-073' Flte:'fl110419b..rtr 

• Peak Name: •PF>1S- Mass(B»):-399.0/99.0 amu.399.0/80.0 amu" 

• Comment: *GW 327R Ql Y11 CP 0 (SOXT Annotation: " 

Sample Index: 187 

Sample Type: Unknown 

concentration : H/A 34-5-1 

Calculate d Conc; 169. ng/nL 

Acq- Date : 4/21/2011 

Acq. Time: 8:17:25 PM 3Je 5 

Hodified : Yes 

Ptoc . Algorithm; InteillQua n - IQA 3.0*5-

Hin. Peak Height: 0.00 cps 

Hin. Peak Width: 0-00 ae c 

1 Smoothing Width; 0 points 2.8*5-

RT Window: 30. 0 se c 

Expected RT: 13.2 ni n ,„ ^ 

Use Relativ e RT; Ho 2.6*5-

Int . Type: Hanual yAr^ 

Retentio n Tine : 13.3 min ^^ ^ 

Area: 1B9S4S7 counts 

Height: 345000. cp s 2 2B5 -

Star t Tine : 13.0 min 

2-0e5-

^ 1.8e5-

^ i i.6e5-

1.4e5-

1.2*5 

I 1.0*5 

8.0*4 

6.0*4 

4.0*4-

2.0*4-

11.0 11.5 12.0 12.5 

1091 1141 1190 1240 

• SampteNam*:-g11O4l9b0ifi- Sampte ID:'10007-27-8- Fie:-g1l04l9b.wir 

I P*akNam*:-PFOS- Ma«(e»):-499.W99.0amu,499.0fflO.Oamu.4&9.tf130.0amu-

• Comment-1.0 ngAnLFCMd In M» Q water" Annotatton: " 

Sample Index : 16 

1 Sample Type: Standar d 

Concentration : 1.00 ng/nL 

Calculate d Conc: 1.03 ng/mL 2.le5 

Acq. Date : 4/19/201 1 

Acq. Time: 5:01:04 PM 2-0e5 

Modified: Yes 1.9*5 

Proc . Rlgorithn : IntelliQua n - HQII 

Moise Percentage ; 50 -- ^ 

Base . Suli. Window: 1.00 min '•°° ' 

Peak-Split . Factor: 2 

Report Largest Peak: No ^-^ ^ 

Min. Peak Height : 0.00 cps 

Hin. Peak Width: 0.00 se c 1.6*5 

Snoothing Width: 0 points 

RT Window: 30.0 ae c 1.5^ 

Expected RT; 13.9 ni n 

Use Relativ e RT: Ho .^^ ^ 

Int- Type: Manual 

Retentio n Time: 13. 9 ni n 1-3*5 

Area; 904180 COunta 

Height: 21S000. cps 1.2*5 

Star t Time: 13.8 min _ 

End Tine : 14.2 ni n & y^ ^ 

1 1.0*5 

^ 9.0*4 

6.0*4 

7.0*4 

6.0*4 

5J>*4 

4J}*4 

3J)*4 

2J}e4 

1X«4 

11.5 12.0 12.5 13.0 

1141 1190 1240 1289 

1S7R 

13.19.., 1 

13.0 13. I 5 14.0 14.5 15.0 15.5 

1289 1339 1388 1438 1488 1537 

Tim*, min 

13.93 

\ 

13.5 14.0 14.5 15.0 15.5 16.0 

1339 1388 1438 1488 1537 1587 

• samrt*Nam*:'g110419b1C2- Sampte ID:-GLP1(K.1-02-17-07r Fie:-fl110419b.wir 

1 Peak Name:-PFHS- MaM{es};-399.0^9J> amu.399.0/B0.O amu* 

• Comment'GW312RQ1Y11CP0(100X)' Annotatkxi:"-

Sanpl e index : 192 

Sample Type; Unknown 

Concentration : H/A 

Calculate d Conc: 710. ng/nL 

Acq. Date : 4/21/201 1 

Acq. Time: 9:47:23 PM 7.0e5 

Modified: Ho 

Proc . Algorithm: IntelliQua n - IQA 6.5*5-

Kin. Peak Height: 0-00 cps 

Kin. Peak Width: 0.00 se c 

Smoothing width : 0 points gj^ J 

RT Window; 30-0 se c ^'^ ^ 

Expected RT: 13.2 min 

Use Relativ e BT: Ho ^^^ j 

Int . Type: Valle y 

Retentio n Time: 13.2 min 

Area ; 3932601 counts 5.0e5-

Height: 745000. cps 

Star t Time: 12.9 min 

End Tine ; 13.6 min 4.5*5-

^ 4.0*5^ 

t 

1 ^•^^-. 

3J)*5-

2.5*5-i 

2.0*5^ 

1.5*5-

1.0e5J 

5.0*4J 

11.0 11.5 12.0 12.5 

1091 1141 1190 1240 

1 Samfte Nam*:'91104196031' Sampte ID: TCS-110412-1- Flte;'o110419b.wi(r 

I Paak Nam*:-PFOS- Ma»(es):'499JV99.0amu,499.0/80.0Bmu,499.0/l30Jlamu' 

• Commert:'2ppb LCS" Annotatkyi:" 

Sanpl e Index: 31 

Sample Type: QC 

Concentration : 2.O0 ng/nL 

Calculate d Conc : 2.21 ng/nlL 4.4,5 

Acq. Date : 4/19/201 1 

Acq. Time: 9:30:32 PM ^^ ^ 

Modified: HO 5 

Proc . Algorithm: IntelliQua n - MOII '"•' 

Noise Percentage ; 50 

Base . Sub. window: 1.00 min •'••*=' 

Peak-Split . Factor: 2 

Report Largest Paak: No 3-W5 

Hin. Peak Height: 0.00 cps 

Hin. Peak width : 0.00 ae c 3.4e5 

Smoothing Width: 0 points 

RT Window; 30-0 se c 3.2e5 

Expected RT; 13.9 min 

Use Relativ e RT: Ho 3.0 ^ 

Int . Type: Valle y 2Je 5 

Retentio n Time; 13. 9 min '"" ^ 

Area : 1890855 counts _- _ 

Height : 452000. cps ^"" ^ 

Star t Time: 13.8 min , 

End Tine : 14.3 min g ^•**^ 

# 2.2e5 

S 2.0*5 

1.8*5 

1.6*5 

1.4*5 

1.2e5 

1.0e5 

8.0*4 

6.0*4 

4.0*4 

2.0*4 

11.5 12.0 12.5 13.0 13.5 

1141 1190 1240 1289 1339 

1.V?1 

[ 

13.0 13.5 14.0 

1289 1339 1388 

T1me.ntin 

13.88 

1 1 1 1 X14J) 14. - 5 15.0 

1388 1438 1488 

14.5 15.0 15.5 

1438 1488 1537 

15.5 16.0 

1537 1587 

Data printe d by STW 

Printing Time: 9:43:21 AM 

Page 9 of 13 

Page 58 of 98 
*** Ginger AG01330509 

GLP10-01-02; Interim Report 17 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Results Name: gll0419b.rdb 

I

SainptoNam«;'fl11041flM34- Sample ID: •t.CS-110412-10' Fto: "gl 10419b.w«r 

P«ak Name: TFOS' Massfes): '499.0/99.0 aniAK.OIW.O amu.499.0/130.0 amu* 

Comment.2pi*>l.CSECF* Annotation;-

Sanple Index: 34 

Sample Type: QC 

Concentration; 2.02 ng/nL 

Calculated Conc: 2.14 ng/mL 

Acq. Date: 4/19/2011 

Acq. Tine: 10:24:23 PH 

Modified: les 

Proc. Algorithm: IntelliQuan - MQI 

Base. Sub. Window: 1.00 min 

Peak-Split. Factor: 2 

Report Largest Peak: No 

Min. Peak Height: 0.00 cps 

Min. Peak Width: 0.00 sec 

Smoothing Width; 0 polr 

RT Window: 30.0 sec 

Use Relative RT; No 

Retention Time: 13.9 min 

Area: 1B325B6 counts 

Height: 299000. cps 

Start Time! 13.6 «in 

End Time: 14.2 min ^ 

& f 

1 

2.9e5 

2.8*5 

2.7*5 

2.6*5 

Z3*i2.0*5 

1.8*5 

1.5*5 

1.4*5 

1Ai5 

1.2*5 

1.1*5 

1J)e5 

9.0*1 

6.0e4 

7J)*4 

6.0*4 

5.0*4 

4JM 

3.0*4 

2.0»l 

1X*4 

13.5 14.0 14.5 15.0 15.5 16.0 

1339 1386 1438 1488 1537 1587 

Time, mfri 

I

Sampte Name:'g110419b03r SamptelD:TCS.ll0412-4' Flte:'gl10419b.wlfr 

P*ak Name: *PFOS* Mase{es}: '499.0/99.0 amu.499.0W).0 amu .499.0/130.0 amu' 

Comment '20ppb LCS* AnnotaSan: ** 

Sample Index: 37 

Sample Type: QC 

Concentration: 20.0 ng/nL 

Acq. Date: 4/19/2011 

Acq. Tine: 11:18:15 PH 

Proc. Algorithm: IntelliQuan - HQII 

Woise Percentage: 50 

Base. Sub. Window: 1.00 min 

Peak-Split. Factor: 2 

Report Largest Peak: Mo 

Min. Peak Height; 0.00 cps 

Min. Peak Width: 0.00 sec 

Smoothing Width; 0 poini 

Expected RT; 13.9 nin 

Use Relative RT; Ho 

Retention Tine: 13.9 min 

Area: 16914425 counts 

Height: 3740000. cps 

Start Time: 13.8 m m 

^ 

3.4*6 

3.2*6 

3.0*6 

2.8*6 

2/4*6 

2.2*6 

8.0*5-

6.0*5-

4.0*5-

2.0*5-

I

Sampte Name:-s1104l9t>045' Sampte ID: TCS-110412-13' Fie: 'gl 10419b.wir 

Peak Name: "PFOS' Mass(e3): '499.0/99.0 emu.499.0/S0.0 annu,499.0/l 30.0 

Comment '20ppb LCS ECP Annotation: ~ 

Sample Index: 45 

Concentration: 20.2 ng/raL 

Calculated Conc: 21.8 ng/iiiL 

Acq. Date: 4/20/2011 

Acq. Time: 1:41:58 AM 

Modified: Yes 

Proc. Algorithm: IntelliQuan - HQII 

Base. Sub. window: 1.00 min 

Peak-Split. Factor: 2 

Report Largest Peak: Ho 

Min. Peak Height: 0.00 cps 

Min. Paak Width; 0.00 sec 

Smoothing Width: 0 poii 

RT Window: 30.0 sec 

Expected RT: 13.3 Bin 

Use Relative RT; No 

Int. Type: Hanual 

Retention Tine: 13.9 min 

Area: 1701S165 counts 

Height: 2550000. cps 

Start Tine; 13.5 min 

End Tine: 14.3 min ^ 

2.3*6 

2.1*6 

1.8*6 

1.7e6 

1.6*6 

1.5*6 

1.2*6 

1.1*6 

1.0*6 

9.0*5 

6.0*5 

7.0*5 

6.0*5 

5.0*5 

4.0*5 

3.0*5 

2.0*5 

1.0*5 

ng/Ti 

I

Sampte Name: •8l10419b061' Sampte ID:'GLP1O-O1-O2-17-O0V File:-gl10419b.wifr 

Peak Nam*: 'PFOS' Mass(es): -499.0/99.0 amu ,499.0/80.0 amu ,499.0/130.0 amiT 

Comment Trip Blank 1 Sampte' Annolalion: 

Sample Index: 61 

Sample Type: Unknown 

Concentration : H/A 

Calculate d Conc: 0.0171 

Acq. Date ; 4/20/201 1 

Acq. Tine : 6:29:25 AM 

Peak-Split . Factor: 

Report Largest Feat 

Hin. Peak Height: 

Hin. Peak width : 

Smoothing Width: 

15.5 16X) 

1339 1388 1436 1438 1537 1587 

Data printed by STW 

Printing Time: 9:43:22 AM 

Page 10 of 13 

Page 59 of 98 
Ginger AG01330509 

GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 2011 

Results Name: gll0419b.rdb 

I

Sampte Name:'g110419b075- Sampte ID:'GLPUM11-02-17-009- Fite:-g110419b.wtr 

Peak Nane: -PFOS' *tass{ea): •499.0«9.0 amu,49fl.a«0.0 amu,499.0/130.0 

CommenL'GW330RQl Y11CP0(50Xr Annotation:" 

Sample Index; 7S 

Sanpl e Type: Unknown 

Concentration : H/A 

Calculate d Conc; 725 . ng/nL 

Acq. Date : 4/20/201 1 

Acq. Tine : 10:41:14 AH ''•^•^ 

Proc. Algorithm: Int 

Noise Percentage: 

Base. Sub. Window: 

Peak-Split. Factor: 

Report Largest Peak: 

Min. Peak Height: 

Min. Peak Width: 

Smoothing width; 

elllQu 

50 

1.0{ 

2 

No 

O.i 

an 

1 

0.00 

0 

RT Window: 30.0 

Expected RT: 

Use Relative RT: No 

Int. Type: Manual 

Area: 11625; 

.3.9 

37 c 

Height: 1600000. 

Start Time: 

End Time; 

.3.5 

14.3 

- MQII 

m 

a n 

1.4e6 

1.3e6 

1.1e6 

1.0e6 

9Xe5 

\ 

6.0*5-

5.0*5-

4.0*5 

3.0*5 

2.0e5 

1.0e5-

0.0 

I

Sanr^Name:'g11041Sb094' Sampte ID;'GLP1(M)1-02-17-021' FUe:*gna419b.wifr 

Peak Name: "PFOS' Irta3s{*a): '499.0/99.0 amu.499.0/B0. ~ 

Comment:'GW310RO1 YIICPO(IOOX)' Annotalfam:-

Sanpl e Index: 94 

Sample Type: Unknown 

13.0 13.5 14.0 14.5 15.0 15.5 16.0 

1289 1339 1388 1436 1488 1537 1567 

Time, min 

I

Sampte Nam*: 'g110419bOS9' San ^ ID: 'GLPI 0-01-02-17-01 r FVe: 'gl 10419b.wHr 

P*ak Nam*: "PFOS' M3ss(es}: '499.0/99^) amu.499.0/80.0 amu^9g.0/130.0 amu* 

Comment'GW317LQ1Y11 CPO" Amotatton:" 

Sanple Index: B9 

Sample Type; Unknown 

Concentration: H/A 

Calculated Conc: 0.222 ng/nL 

Acq. Date: 4/20/2011 

Acq. 2:53:14 

Modified: 

Proc. Algorithm: 

Noise Percentage: 

Base. Sub. Window 

Peak-Split. Facto 

Yes 

[ntelli 

r: 2 

Report Largest Peak: M 

Hin. Peak Height: 

Smoothing Width: 

RT Window: 

Use Relative RT: 

Int. Type: 

Area: 23 

Height; 

0 

0 

30.0 

13.9 

Ho 

Manual 

2083 

32300. 

^j^^^Mh'V.*^**/*''*^'*^ ^ ^^^^^'Vv-^vw^^JN.. , 

15.5 16.0 

1537 1587 

I SampteName:'g110419b103' Sanpte ID:'GLPI0-01-02-17-025' Flte:'g110419b.wiir 

Peak Name: -PFOS' Uassfea): '499.0/99.0 amu.49g.0/80.0 amu.499.0/130.0 amu* 

I Comment'GW227LO1Y11LF0(20XJ' • -

Acq. Date: 

Acq. Time; 

ModifiedProc. Algorithn: 

Noise Percentage: 

Base. Sub. window 

Peak-split. Facto 

/20/20n 

:23:15 PH 

Yes 

ntelliQua 

50 

1.00 

2 

Report Largest Peak: Ht> 

Min. Peak Height: 

Snoothing Width: 

RT Window: 

Use Relative RT: 

Int. Type: 

0.00 

0.00 

0 

30.0 

13.9 n 

Ho 

Hanual 

13.9 1 

Area; 7707027 cour 

Height: 9 3000. cpa 

Sample Index: 103 

Concentration: H/A 

Calculated conc: 365. 

Acq. Date: 4/20/2011 

Acq. Time: 7:04:56 PM 

Hodified: Yes 

Proc. Algorithn: IntelliQuan 

Noiae Percentage: 50 

Base. Sub. window: l.Oo 

Peak-Split. Factor: 2 

Report Largest Peak: No 

Hin. Peak Height: 0.00 

Smoothing Width: 0 

RT Window: 30.0 s 

Expected RT; 13.9 n 

Use Relative RT: Mo 

Int. Type: Hanual 

Retention Tine; 13.9 m 

Area: 1442969G cou 

Height: 2000000. cp 

nL 

MOII 

n 

c 

n 

Start Tine: 13.5 min 

End Time: 14.3 m S 

1.9*(' 

1.8*6 

1.6*6 

1.3*6 

1.1*6 

1.0*6 

9.0*5 

5.0*5-

4.0*5-

3.0*5-

2.0*5-

1Xe5 

13.0 13.5 14J) 14.5 15.0 15.5 16.0 

1289 1339 1388 1438 1488 1537 1587 

Data printed by STW 

Printing Time: 9:43:22 AM 

Page 11 of 13 

Page 60 of 98 
*** Ginger AG01330509 

GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 2011 

Results Name: gll0419b.rdb 

I

Sxtfike Name: -g110419b1ir Sampte ID: 'GLPICKi 1-02-17-033' Rte: -g110419b.wHr 

P«ak Nam*: "PFOS' h<3s$(es): '499.0/99.0 amu.499.0/B0.0 amu,499.0/130.0 amu' 

Comnr)*nt'GW220RQ1Y11lF0<5XJ' AnnotaSon:" 

Sample Index: 117 

Sample Type: Unknown 

Acq. Tine: 

Modified: 

Ptoc. Algorithm; 

Hois* Percentage: 

Peak-Split. Facto 

/20/2011 

1:17:23 PM 

Yes 

ntelliQuan 

r: 2 

Report Largest Peak: No 

Min. Peak Height: 

Min. Peak Width: 

Smoothing Width: 

KT Window: 

Use Relative RT: 

0.00 

0 

13.9 m 

No 

Manual 

13.9 n 

Area: 8523064 coun 

Height: 936000. cps 

Start Time: 13.5 ni 

I

SampteName:*g110419bl50' Sampte ID:'GLPIO^l-02-17-053' Rte;'g110419b.wtfr 

Peak Name: 'PFOS' Mass(es): '499.0/99.0 amu.499.0/BO.O amu.499.0/130.0 amu" 

Comment: •GW203LQ1Y11LFO(20X)' AnrwjteBon:-

Sample Index: 150 

13.0 13.5 14.0 14.5 15.0 15.5 16,0 

1289 1339 1388 1438 1488 1537 1587 

Tlm^-mln 

I

SampteName:'g110419b136- Sampte ID:'GLP10^)1-02-17-045' FSe:'g110419b.wlfr 

Paak Name: "PFOS* Uase(es); '499il/99.0 amu,4gg.0/80.0 nnu .499.0/130J) ami/ 

Comment'eW324LQ1Y11CP0(2OX)' Annotation:" 

Sample Index: 136 

Concentration; 

Acq. Tine: 

Modified: 

Proc. Algorithm: 

Noise Percentage 

Base. Sub. Windo 

a/A 

332. 

4/21/2011 

4:59:05 At 

Yes 

IntelliOu 

: 1.00 

Peak-Split. Factor: 2 

Report Largest Peak: No 

Min. Peak Height 

Min. Peak width: 

Snoothing Width; 

Bt Window: 

Expected BT; 

Use Relative RT; 

Retention Tine: 

0.0 

0.0 

0 

30.0 

13.9 

Ho 

Hanual 

13.9 

Area: 13209743 e 

Height: 

Start Time: 

680000. 

13.6 

Type: Unki 

Calculated Conc: • 

Acq. Date: 4/2: 

Modified: : 

proc. Algorithn: Inti 

Noise Percentage: 

Base. Sub. Window: 

Peak-Split. Factor: 

Report Largest Peak: 

Min. Peak Height: 

Hin. Peak Width: 

Smoothing Width: 

RT Window: 3{ 

Expected RT: 1 

Use Relative RT: [ 

Ini Type: 

Area: 32516909 

Height: 4010000. 

Start Tine: 13.6 

End Time; 14.4 

3.6*6 

3.6*6 

3.4*6 

3.2*6 

3.0*6 

2.6*6-

2.6*6 

2.4*6 

2.2*6-

^ 2.0*6 

I 1.6*6 

1.6*6-

1.4*6 

1.2*6-

1J)*6-

ej)e5 

6.0*5 

I

S3mpteName:'g110419b164' Sampte ID:'GLP10^)1-02-17-061' Flte:'o1104l9b.wtfr 

Peak Name: 'PFOS" Mass(es): '499.0/99.0 amu ,499.0/80.0. 

Comment*GW328RQ1Y11CPO{10X)- Annotatton: 

Sample Index; 164 

Sample Type: Unknown 

Concentration: 

Calculated Conc: 

Acq. Tif ,;23:1 

Modified: 

Proc. Algorithn: 

Noise Percentage: 

Base. Sub. Wlndoi 

Yes 

[ntelllQ 

: 1.0 

Peak-Split. Factor: 2 

Report Largest Pe 

Hin. Peak width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

ak: No 

0. 

0. 

0 

13.9 

Ho 

Manual 

Area: 17361911 

Height: 2 

Start Time: 

End Tine; 

.20000. 

13.6 

14,5 

Data printe d by STW 

Printing Time: 9:43:22 AM 

nja 13.5 14.0 14.5 15.0 15.5 16.0 

12S9 1339 1388 1438 1488 1537 1587 

12.0 MJ5 13.0 13.5 14.0 14.5 15.0 15J 16.0 

11S0 1240 1289 1339 1388 1438 1488 1537 1587 

Page 12 of 13 

Page 61 of 98 
Ginger AGO13305O9 

GLPI 0-01 -02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 2011 

Results Name: gll0419b.rdb 

• Peak Nam*:'PFOS' Mass(es):'499.0/99.0amu,49g.0/80.0amu.49g.0/130.0anwr 

• Comm*nt'GW327RQ1Y11CP0(50X)' AnnotaBon:-

Sample Index: 187 

I

Sampte Name:'g110419b178- Sampte ID: •GU»1O4)1-O2-17-06r Fite:'gll0419b.»«r 

Peak Name: 'PFOS' htas3<es): '499.0/99.0 amu.499.0/&0.0 amu,499.0/l 30.0 amtT 

Comment:'GW331SQl Y11CP0(50X)' Annotatton:" 

Sample Index: 17S 

Sample Type: Unknovn 

Concentration : H/A 

Calculate d Conc: 668. ng/nL 1.15e6' 

Acq. Date : 4/21/201 1 

Acq. Tine : 5:35:2 5 PM 1.10e6 

Modified; Yes i.05e6 

Proc. Algorithn: IntelliQuan - HQII 

1.00e6-

9.50*5-

9.00*5 

' 8.50*5-

8.00*5 

7.50*5 

7.00*5-

6.50*5-

^ 6.00*5-

I 5.50*5-

5.00e5-

4.50*5-

4.00*5-

3.50e5-

3.00*5-

2.50*5-

2.00e5-

1.50*5-

1.00*5-

5.00*4-

0.00-

Noise Percentage: 

Base. Sub. Window: 

Peak-Split. Factor 

Report Largest Pea 

Min. Peak Height: 

Min. Peak Width: 

Snoothing width; 

Expected BT: 

Use Relative RT; 

Int. Type: 

Retention Tine; 

S 

2 

30-0 

13. 

No 

Hanua 

Area; 10749465 

Height: 11 

Start Time: 

End Time: 

(0000 

13. 

14, 

11^ 

13.5 14.0 14.5 15.0 15.5 16.0 

1339 1388 1438 1488 1537 1587 

Tlme.nrin 

toName:'g11041Sb1Sr Sampte ID:'GLP1CKI1-O2-17-073' Fite:'g1104igb.wtr 

Sample Type; Unknown 

Concentration; H/A 

Calculated Cone: 591. ng/nL 

Acq. Date: 4/21/2011 

Acq. Tine: 8:17:25 PH 

Modified: Yes 

Proc. Mgorithn: IntelliOuan - HQII 

Noise Percentage: 50 

Base. Sub. Window: 1.00 min 

Peak-Split. Factor; 2 

Report Largest Peak; No 

Min. Peak Height: 0.00 cps 

Min. Peak Width: 0.00 sec 

Smoothing Width: 0 poin 

RT Window: 30.0 sec 

Expected RT: 13.9 min 

Use Relative RT; No 

Int. Type: Manual 

Retention Time: 14.0 nin 

Area: 9576141 counts 

Height; 986000. cps 

Start Tine; 13.6 nin 

End Time: 14.3 min ^ 

t 

9.5*5 

9.0*5 

83e5 

8.0e5 

7.5*5 

7JiB5 

6.5*5 

55*5 

5.0*5 

4.5*5 

4J)*5 

3.5*5 

3.0*5 

2.5*5 

2.0*5 

1.5*5 

11.5 12.0 12.5 13.0 13.5 14.0 14.5 • 15.0 15.5 16.0 

1141 1190 1240 1289 1339 1368 1438 1488 1537 1587 

time, min 

I Sampte Name:-g110419b19r Sampte 10; *GIP1041-02-17-O7r Flte:'g1l0419b.wtir 

Paak Name: "PFOS' Mass{*s): '499.0/99.0 emu.499.0/80.0 anmi,499.0/130.0 smu' 

I Comment:'GW312R01 Y11 CPO(100X)' " -

1.00*6 

9.50*5 

9.00e5 

6.50e5-

8.00*5-

7.50*5-

7.00*5-

6.50*5-

6.00*5 

. 5.50e5 

£ 5.00e5 

I 4.50*5-

4.00*5-

3.50*5-

3.00*5-

2.50*5 

2.00*5-

1.50e5-

I.OOeS5.0ae4: 

0.00-

sample Index: 92 

Sample Type; Unknown 

Calculated Conc: 

N/A 

iiao. 

Acq. Date: 4/21/20 

Acq. Tine: 9 

Hodified: 

Proc. Algorithm: I 

Noise percentage: 

Base. Sub. window; 

Peak-Split. Factor 

47:23 

Yes 

Ite m 

50 

2 

Report Largest Peak: N 

Hin. Peak Height: 

Min. Peak Width: 

Smoothing Width: 

Expected RT: 

Use Relative RT; 

Retention Tine: 

Area: 9579 

Height: 10 

Start Tine: 

End Time: 

0 

0 

30.0 

13.9 

No 

lanual 

14,0 

52 

0000. 

13,6 

14.3 

Data printed by STW 

Printin g Time: 9:43:22 AM 

"'*~'M" 

Page 13 of 13 

Page 62 of 98 
GLP10-01-02; Interim Report 17 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Ginger AG01330509 Results Name: gll0424b.rdb 

g110424b.rdb (PFOS): "Quadratic" Regression ("1 / x" weighting): y = -3.18e-f003 x''2 + 7.79e-^005 x -^ 1.27e-^004 (r = 0.9998) 

3.2e7 

3.0e7 

2.8e7 

2.6e7 

2.4e7 

18 20 22 24 26 28 

Concentration, ng/mL 

36 38 42 44 46 48 

Data printed by STW 

Printing Time: 9:55:49 AM 

Printing Date: Monday, July 18, 2011 

Page 1 o£ 1 

Page 63 of 98 
GLP10-01-02; Interim Report 17 

/Vnalysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Ginger AG01330509 Results Name: gll0424b.rdb 

1 • g110424b.rdb (PFHS): "Quadratic" Regression ("1/x" weighting): y = 

2.3e7-

2.2e7-

2.1e7-

2.0e7-

1.9e7-

1.8e7-

1.7e7-

1.6e7-

1.5e7-

1.4e7-

1.3e7 

§ ^-^^^ 

TM- 1.1e7-

"^ 1.0e7 

9.0e6 

S.Oee 

7.0e6-

6.0e6 

5.0e6 

4.0e6 

S.OeS 

2.0e6 

1.0e6 

0.0 

y ^ 

y ^ 

y ^ 

y ^ 

y ^ 

• y ^ 

• y 

y^ 

^ 

0 2 4 6 8 10 12 14 16 

-2.11e-f003 x'^2 * 5.47e•^005 x * 7.83e-f004 (r = 0.9962) 

^ ^ 

^ - ^ 

/ ^ 

^ y 

y " ^ • 

X 

18 20 22 24 26 28 30 32 34 

Concentration, ng/mL 

^ 

36 38 

^ 

^ 

40 

y ^ 

42 

^ 

44 

^ 

46 

^ ^ 

48 

• 

^ 

50 

Data printed by STW 

Printing Time: 9:55:13 AM 

Printing Date: Monday, July 18, 2011 

Page 1 of 1 

Page 64 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

Ginger AG01330509 Results Name; gll0424b.rdb 

• g110424b.rdb (PFBS): "Quadratic" Regression ("1 / x" weighting): y = 

1.3e7:( 

1.3e7-

1.3e7-

1.2e7-

1.2e7-

1.1e7-

1.1e7-

1.0e7-

9.5e6-

9.0e6-

8.5e6-

8.0e6-

7.5e6-

i 7.0e6-

°. 6.5e6-

5 6.0e6-

5.5e6-

5.0e6-

4.5e6-

4.0e6-

3.5e6-

3.0e6-

2.5e6^ 

2.0e6^ 

1.5e6-

1.0e6-

5.0e5: 

0.0-

y 

y ^ 

y ^ 

y ^ 

^«r 

y y 

y ^ 

j i i 

y^ 

y ^ 

I T 

0 2 4 6 8 10 12 14 16 

-959 x*2 -^ 3.12e-f005 x * 1.81e-f003 (r = 0.9999) 

y ^ 

y ^ 

y ^ 

y ^ 

y ^ 

y"" ^ 

• ^ 

18 20 22 24 26 28 30 32 

Concentration, ng/mL 

34 

^ 

36 38 40 42 

^ 

44 

^ 

^ 

46 48 

^ 

50 

Data printed by STW 

Printing Time; 9:54:29 AM 

Printing Date: Monday, July 18, 2011 

Page 1 of 1 

Page 65 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Ginger AG01330509 Results Name: gll0424b.rdb 

I

San^:teN«tie:'gl10424l)0lr Samph tO: •1O0O7-27-9' Fito:-g110424b.wifr~ 

PMk Nama: 'PFBS' Massfas): -299.0/99.0 •mu,299.0rtl0.0 amu* 

Commant '1.0 ngfrnL FC std in WB Q watar Annotatton: -

Sanpl e Inclex: 17 

7,5a4 

7.0»4-

6.5M6.0e4-

5.5*4-

5.0«4-

4.SM4.0a4-

3.5a4-

3.0a4-

sample Type: S 

Calc 

Modi 

lated 

Time; 

led: 

Algo 

Hoise Pete 

Base 

Peak 

Min. 

Sub. 

Split 

Conc: 

» 

ithm: I 

ntage: 

t Largest Pea 

Peak HeighC; 

Peak Hidth: 

Smoothing 

RT Kindow: 

idth: 

tandacd 

1.00 

1.03 

25/2011 

09:Se AH 

Yea 

celllQuan 

SO 

1.00 

2 

1:: No 

0.00 

0 

30.0 s 

AreaHeight: 

Stact Tine: 

End Time: 

321790 

75700. 

12.3 

2.5*4 

2.0*4-

9.77,9.85 10.26 11.37.., 11.57 11.a 

I

Sampte Nama: *g110424bO34* Sampte ID:-LCS-110422-4' Flo:'gl10424b.wir 

Paak Name:-PFBS- Massfat):-299.0/99.0 amu.299.Ck'80.0 amt/ 

Comment: *2ppb LCS* Annotatton: " 

Sanple Index: 31 

I

Sample Nama: *g1l0424b02r Sampte ID:-Msthod Blank- Fte:-gll0424b.wMr 

Paak Nama:-PFBS' Mass(*t): *299.Q/99.0 amu,299.Q/80.~ 

Commant TN11-0156 Mi l QWatar- AnnolBtion:-

Sanpl« Index: 27 

Concentre 

Calculatec 

Acg. Time 

Modified: 

Proc. Algo 

Noise Pete 

Base. Sub 

Feak-Spll' 

Report Lar 

Min. Peak 

Smoothing 

RT Kindoe: 

ion; 

Conc: 

rithra: 

Un 

4/ 

4: 

known 

H/A 

S/2011 

0:26 AM 

Ho 

IntelliQua 

Window: 

. Fact r: 

gest Peak 

Height 

dldth: 

Plldth: 

Expected RT: 

Use Relatl ve RT: 

50 

1.00 

2 

No 

0.00 

0 

0.0 

12.1 

Mo 

Base To Base 

I

Sampte Nama:-g110424b042- Sampte ID: *LCS-110422-13' Flte:'gl10424b.«rtr 

Paak Nama; 'PFBS' Mass(at): '299.0/99.0 amu,299.aWl.O amuComment *2ppb LCS ECP /kjmotatlon: ** 

Sampl e Index : 42 

Sampl e Type : 

Concentration ; 

Acq . Tine : 

Hodified : 

Proc . Algorithm : 

Nois e Percentage : 

Base . Sub . Hlndo u 

Peak-split . Fact o 

9c 

2.00 

1.91 

/25/2 0 

:16:26 

Yea 

ntell i 

50 

1. 

; 2 

Repor t Larges t Peak : H 

Min . Peak Height : 

Snoothin g (fidth : 

R T Windoii: 

Expecte d RT ; 

U se Relativ e RT : 

Int . Type : 

Retentio n Time : 

Area : 59 

0 

0 

30. 0 

12.1 

Manua l 

12.0 

346 

Star t Time : 

1.3*5 

1.2*5 

1.1 e5 

1.0*5 

9.0*4 

8.0*4 

7.0*4 

6.0*4 

5.0*4 

4.0*4 

3.0*4 

2.0M 

1.0*4 

10.86 11J7 

12.02 

11.78 L 12.42 12^' 13J7 13.64 14.15 14.46 

ConcenttBtlO 

Calculated C 

Acq. Time: 

Hodified: 

Ptoc. Algori 

Noise Percen 

Base. Sub. u 

Peak-Split. 

Report Large 

Hin. Peak He 

hn: 

ndo 

qht 

Hin. Peak Width; 

Smoothing Nl 

RT Window; 

Expected RT: 

Use Relative 

Int. Type: 

Area: 

Height: 

Start Time: 

KT: 

0.00 ng/mL 

0.0235 ng/oL 

4/25/2011 

S;40:02 AM 

Yes 

IntelliQuan - MQ 

50 

«: 1.00 min 

lak; Ho 

0.00 cps 

0.00 aec 

0 po 

30.0 sec 

12.1 min 

Ho 

Manual 

9146 counts 

2250. cpa 

11.9 min 

Data printed by STW 

Printing Time: 9:53:33 AM 

Printing Date: Monday, July 18, 

Page 1 of 6 

Page 66 of 98 
GLPI 0-01-02; Interim Report 17 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 2011 

Ginger AG01330509 Results Name: gll0424b.rdb 

|HSampl*Nam*;-g110424b045- ^mpl*lD:TCS-11042^7-

• Paak Nam*; TFaS* Mass(«): •299.0«9.0 amu,299.(VB0.0 

• Commani; •20ppb LCS" Annotatton: -

Sample Index; 45 

Sample Type: QC 

Concentration : 20.0 ng/mL 

Calculate d Conc: 19.6 ng/nL 1 9n-R 

Acq. Date : 4/25/2011 '"^" ^ 

Acq. Tine : 9;34:04AM 1.15.6 

Modified; No 1.10*6 

Proc . Algorithm; IntelliOua n - HQII 

Noise Peceentage : 50 '•'TMTM 

Base . Sub. window; 1.00 min 1.00*6 

Peak-Split . Factor: 2 

Report Largest Peak: No 9.50a5 

Hin. Peak Height : 0.00 cps 

Hin. Peak Width: 0.00 se c 9.VOab 

Smoothing width ; 0 points o 50e.iE 

RT Window: 30. 0 se e ' ^ 

Expected RT: 12.1 min 8.00*5 

Ose Relativ e RT; No 

7.50*5 

Int . Type; Valle y ^ f^. 

Retentio n Tine : 12.0 min , '•"" " 

Area; 573576B counts & 6 50*5 

Height: 1250000. cps >, 

Star t Time: 11.9 min • 6.00a5 

End Time; 12.5 .i n | ^^ ^ 

5.00B5 

4.50a5 

4.00*5 

3.50e5 

3.00*5 

2.50*5 

2.0085 

1.50*5 

1.00*5 

5.00*4 

0.00 

1 SarTvl«^rrw:'gl10424b05r Sampte ID:-GLP1(H)1-02-1 

I P*BkNam*:-R=BS- Ma$«(at);-299.0»9.0 amu.299.0«0.0 

• Comm«nt:'GW222RQ1Y11LF0(20X)' Aroiotation:-

Sanple Index: 57 

Sample Type: Unknown 

Concentration : N/A 3AlS-| 

Calculate d Conc: 96.2 ng/mL 

Acq. Date : 4/25/2011 , , _ 

Acq. Tine : 1:09:47 PM " 

Hodified : Yes 3.0*5 

Proc . Algorithm: IntelliOua n - KQII 

Noise Percentage : 50 , o^_ 

Base . Sub. Window: 1.00 min ^ ^ 

Peak-Split . Factor; 2 

Report Largest Peak: No 2.6*5 

Hin. Peak Height : 0.00 cps 

Hin. Peak width ; 0.00 se c 2.4«s 

Smoothing Width: 0 points 

RT Window: 30.0 se c 

Expected RT: 12.1 min 2.2*5 

Ose Relativ e RT: Ho 

2.0*5 

int . Type: Manual ^" ^ 

Retentio n Time; 12.1 min • 

Area: 1478981 counts & 1.8*5 

Height: 341000. cps >. 

Start Time: 11.9 min « . ^ , 

End Time: 12.3 min | " ^ 

1.4*5 

1.2*5 

1.0«5 

8.0*4 

6.0*4 

4J)*4 

ZOtA 

0,0 

Fi*:-9l10424b.wir 

amu10.00 10.59..10.74 11.2T..,11.41 1 

10.0 10.S 11.0 

992 1042 1091 

7-041- FN:-gl10424b.wifr 

amu10.69 

10.0 10.5 11.0 

992 1042 1091 

11.5 

1141 

11.43 

11.5 

1141 

12.01 

1 1 1 1 1 1 

• -88- ^ . 

12.0 

1190 

121» 

11.97^H 

12.0 

1190 

12.52 

^2£ 

1240 

12.68 

12.5 

1240 

12.9913.23 

13.0 

1289 

13.0 

1289 

' "^ 

13.50 

13.5 

1339 

13.5 

1339 

13.83 14.11 

14.0 

1388 

14.0 

1388 

-14.23 , 

14.5 

1438 

14.5 

1438 

• Samp4«Nania:'g110424bO48' Sampte ID:-LCS-110422-16' Fite:*g110424b.t«tfr 

• P»ak Name:-PFBS- MaM(*i}:'299.0/99.0 amu.299.0/80.0 amu" 

• Commant •20ppb LCS ECF* Annotatton: " 

Sample Index: 48 

Sampla Type: QC 

Concentration : 0.00 ng/mL 

Calculate d Conc: 0.229 ng/mL 

Acq. Date : 1/25/2011 1.5*4 

Acq. Tine ; 10:27:5 8 AH 

Hodified : Ho 1-4*' 

Proc . Algorithm: IntelliOua n - MQII 

Noise Percentage : 50 ^ ^MA 

Base . Sub. window: 1.00 min 

Peak-Split . Factor: 2 

Report Largest Peak: No 1.2*4 

Hin. Peak Height: 0.00 cps 

MIn. Peak Width: 0.00 se c 

Smoothing width ; 0 points 1.1*^ 

RT Window: 30. 0 Sec 

Expected RT: 12. 1 min .-_ . 

Use Relativ e RT; Ho '"" ^ 

Int . Type: Valle y 90OO.O 

Retentio n Time: 12.0 min „ 

Area : 73111 counts gHeight: 15800. cps >, 8000.0 

Star t Time: 11.8 min g 

End Time: 12.2 min | ^^ ^ 

6000.0 

5000.0 

4(H)0.0 

3000.0 

2000.0 

1000.0 

0.0 

10.0 10.5 

992 1042 

1 Sampte Name:-g110424bO17J Sampte ID: •10007-27-8' Flte:'gl10424b.wm^ 

• P«ak Nam*; 'PFHS' M8ss(*s): '399.0/99.0 amu,399.0/S0.0 amu' 

• Comment:'1.0 ng/mL FCstd In MM Q water" Annotatton;-

Sample Index: 17 

Sample Type: Standar d 

Concentration : 1.00 ng/nO. 1.6*5-1 

Calculate d Conc: 1.09 ng/nL 

Acq. Date : ^'"/^^ l 1.5*5 

Acq. Time; 1:09:56 AH I-JOJI 

Modified; Ho 1.4*5-^ 

Proc . Algorithm: IntelliQua n - IQA 

Hin. Peak Height: 0.00 cps 

Hin. Peak width : 0.00 se c 1-3*S 

Smoothing Width: 0 points 

BT Window: 30.0 se c . - _ 

Expected BT: 13.2 ni n ^^ ^ 

Use Relativ e RT: Ho 

1.1*5 

Int . Type: Valle y 

Betentio n Time: 13.3 ni n 

Area: 671033 counts 1-C^ 

ReLght; IGOOOO. cpa 

Star t Time: 13.2 ni n .(^ , 

'••'"- • ' " •' " J • 

- i 8.0*4 

1 7.0*4-

6.0*4-

5.0*4-

4J)e4' 

3.0*4 

2.0*4 

1XM 

11.0 11.5 

1091 1141 

11.0 11.5 

1091 1141 

12.0 12.5 

1190 1240 

12.0 

1190 

I WSJ« A t 

12.5 13.0 13.5 14.0 14.5 

1240 1289 1339 1388 1438 

Tknemin 1 

13.28 1 

'13.0 ' 

1289 

13.5 14.0 14.5 15.0 1S.S 

1339 1388 1438 1488 1537 

fflla 

Dat a printe d by STW 

Printing Time; 9:53:33 AM 

Printing Date: Monday, July 18 

Page 2 of 6 

Page 67 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

1st Quarter Sampling - 2011 

Ginger AG01330509 Results Name: gll0424b.rdb 

I SaniplsNaiT)e:*g11M24b02r Sampte ID:-MettMd Blank* Fi«:-g110424b.wttr 

I Pule Name;-PFHS- Mass[es):-399.0/99.0 amu.399.0/80.0 amu' 

I Comment:*TN11.01S6MaQWaie(' /VnnotatlMi:-

Sample TypeCalculated C 

Acq. Date: 

Acq. Tine: 

Modified: 

Proc. Algori 

Hin. Peak WJ 

Smoothing Mi 

Expected RT: 

Use Relative 

Retention Ti 

Height: 

Start Time: 

End Time: 

ight 

Hrh: 

kT; 

Unknown 

(J/fl 

< 0 

4/25/2011 

4:10:26 AM 

No 

IntelliQuar 

0.00 c 

0.00 

30.0 

13.2 0 

No 

Valley 

2569 cour 

645. cp 

13.1 B 

I

Sampte Nam*; "91104241)042- Sampte 1D;'T.CS-110422-13' Rte; •g110424b.wirr 

Peak Name; 'PFHS- Mass(*s); '399.0/99.0 amu,399.0/80X1 artiu' 

Comment: •2ppb LCS ECP Armotatton: -

Sample Index : 42 

Type: 

11.0 11.5 12.0 12.5 13.0 13.5 14.0 

1091 1141 1190 1240 1269 1339 1388 

Thn*. min 

I

Sampte Narr»:'g110424t)034- Sampte ID:-LCS-110422-4' Fll*:-g110424b.wtr 

P*ak Nama: 'PFHS' Mass{*s); -399.0/99.0 amu,399,0/80.0 amu' 

Commant •2ppb LCS' Annotation: ~ 

Sample Index: 34 

Sample Type: QC 

Calculated Conc; 

Acq. Date: ' 

Acq. Tine: I 

Modified; 

Proc. Algorithm: ] 

Min. Peak Height: 

Int . Type: 

Retention 1 

2.6*5-

2.5*5-

2.4*5-

2.3*5-

2.2*5-

2.1e5-

2.0e5-

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-

4.0*4-

3.0*4-

2.0*4-

1.0*4-

12.00 .,12.18 12.6912.95 13.46 13.7213.97 14.7K 1S.07^ 15.25 15.55 

1091 1141 

Concentration; 

Calculated Conc: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Hin. Peak Height 

Min. Peak Width: 

Smoothing Width: 

O.OO ng/raL 

4/25/2011 

8:40:02 AM 

1-es 

IntelliQuan - IQA 

0.00 cps 

0.00 sec 

0 points 

30.0 sec 

1.3*4 

1.3*4 

1.2*4 

1.2*4 

1.1*4 

1.1*4 

1.0*4 

I

Sampte Nam*: •g110424b045" Sampte ID: •LCS-110422-r Fil*:'g110424b.wir 

P*ak Nam*: 'WHS' Mass{*s); -399.0/99.0 amu,399 

Comment '20ppb LCS' Annotation:" 

sample Index : 45 

Sample Type; QC 

13.2 

59452 cc 

12900. ! 

7500.0-

8 7000.0 

^ 6500.0-

i 6000.0-

- 5500.0-

5000.0-

4500.0-

4000.0-

Concentration; 

Calculated Conc; 

Acq. Date: 

Acq. Time: 

Hodified: 

Proc. Algorithm: 

Min. Peak width: 

Smoothing Width: 

BT Mindow: 

Expected RT: 

Use Relative BT: 

Int. Type: 

Betention Time: 

Area: 90 

20.0 

17.6 

4/25/201 

9:34:04 

Yes 

IntelliQ 

0.00 

O.OO 

0 

13.2 

Ho 

Hanual 

13.2 

Height: 2110000. 

Start Time: 13.1 

ng mL 

ng/raL 

1 

AM 

sec 

poin 

rain 

min 

IQA 

& 

f 

^ 

2.1*6 

2.0*6 

1.9*6 

1.8*6 

1.7*6 

15o6 

1.4*6 

1.3*6 

1.2*6 

1.1*6 

1.0*6 

9.0*5 

Data printe d by STW 

Printing Time: 9:53:33 AM 

Printing Date: Monday, July 18, 2011 

Page 3 of 6 

Page 68 of 98 
GLPI 0-01-02; Interim Report 17 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 2011 

Ginger AG01330509 Results Name: gll0424b.rdb 

I SemfJeNema:-9l10424bO4S' Samt]telO;TCS.110422-ir Flle:-g110424b.wWPeak Name:-PFHS* hteaafaa):-399J}/99.0 

• Commem:-ZOcfti LCS ECP /Annotation:-

Sample Inde;.; 4S 

Sample Type: 

Calculated Conc: 

Acq. Dote: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Min. Peak HeighC: 

Min. Peak width; 

Smoothing Width: 

BT Window: 

Expected BT: 

Use Relative BT: 

int. Type: 

Retention Time: 

Area: 55 

Beight: 1 

Start rime: 

End Time: 

QC 

0.00 

O.BBO 

1/25/2011 

10:27;5B 

Yes 

ntelliOu 

0.00 

0.00 

0 

30.0 

13.2 

Mo 

Hanual 

13.2 

7000. c 

13.0 

13.1 

I

Sampte Name: -g11O424b0ir Sampte lO: '10007-27-6- Flte: 'g110424b.wlfr 

P*ok Nam*: 'PFOS" MaM{a9): -499.0/99.0 amu.499iV80.0 amu.499.0/130.0 amu" 

Commant: -1.0 nglmL FC std in MDIQ water* /Annotation: 

Sample Index: 17 

I

Sampte Name:'g110424bO57* Sampte ID:-GLP1(W)1-02-17-041' Fite:-g110424b.w1(r 

P*ak Name: "PFHS* Mas»(*«): "399.0/99.0 amu ,399. 

Comment *GW 222R 01 Y11 LF 0 (20X)' Annotation: 

Sample Index: 57 

Sample Type: 

Calculated Conc 

Acq. Time: 

Modified: 

Proc. Algorithn 

Min. Peak Heigh 

Min. Peak width 

Snoothing Width 

RT Window: 

Expected RT: 

Use Relative RT 

Int. Type: 

Betention Time: 

Unknown 

tl/A 

615. 

4/25/2011 

1:09:17 PM 

Yes 

IntelliQua 

0.00 

0.00 

0 PC 

30.0 

13.2 n 

Ho 

Manual 

13.3 It 

Area; 14905378 COL 

Height; 2790000. CF 

11.0 115 12.0 12.S 13.0 13.5 14.0 14.5 15.0 15.5 

Sampte Nam*: •g110424b027' Sampte ID:'Method Blank" Fls;*gll0424b.wWr 

Peak Nama: -PFOS" Massfas): -499.0/99.0 amu,499.0/8ao amu.499.0/130.0 annuCommentTnil-OlSeUilQWater Annotation:' 

Sample Index: 27 

Sanple Type: 

Concentration: 

Calculated Conc: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Hoiae Percentage 

Base. Sub. Wlndo 

Peak-Split. Fact 

Standard 

1.00 

0.959 

4/25/2011 

1:09:56 A 

No 

IntelliOu 

50 

-: 1.00 

Report Largest Peak: No 

Hin. Peak Height 

Hin. Peak Width: 

Smoothing Width; 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

0.0 

0 

30.0 

14.0 

Ho 

Valley 

Area: 756564 co 

Height; 

End Time: 

ng/raL 

ng/mL 

n - HQII 

min 

cps 

min 

82000. cps 

13.9 

min 

a 

S 

(7 

Data printed by STW 

Printing Time: 9:53:33 AM 

Printin g Date: Monday, July 18 

Page 4 of 6 

Page 69 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS. and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Ginger AG01330509 Results Name: gll0424b.rdb 

I

SampteNem*:-gil0424t)034' Sampte ID: TCS-110422-4' Fl*:'g110424ti.wt(r 

P*8k Name: •pFOS* Mass{*s): '499.0/99.0 amu^»9.0/S0.0 Bmu,499.0/130.0 

Comment: -2ppb LCS* AnnotaSon: ~ 

Sample Index: 

Sampla Type: QC 

Concentration: 

Calculated Conc: 

Acg. Date: 

Acq. Time: 

Hodified; 

Proc. Algorithm: 

Noise Percentage: 

Base. Sub. Window 

Peak-Split. Focto 

2.00 

1.75 

4/25/2011 

6:16:26 AH 

No 

IntelliQua 

50 

: 1.00 

r: 0 

Report Largest Paak: Ho 

Kin. Peak Height: 

Kin. Peak width: 

Smoothing width; 

RT Window: 

Expected RT: 

Use Relative RT: 

O.OO 

O.OD 

0 

30.0 

ng/mL 

ng/mL 

tl - MQ 

aec 

po 

14.0 min 

NO 

I

Sampte Name;'g110424t)04S' Sampte ID:'LCS-1ia422-r Fle:'gl10424b.wir 

Paak Nam*;-PFOS' Maaa{as): "499.0/99.0 omu.489.0/80.0 

Comm*nt; *20ppb LCS' /Vrnotation: — 

Sample Index: 15 

Sample Type: QC 

Concentration : 20.0 ng/mL 

Calculate d Conc: 20. 5 ng/nL 

Acq. Date : 4/25/2011 

Acq. Tine : 9:34:04 AH 

15.49s. 15.73^15^7 16^7... 

I

Sampte Nam*: -gl 104241)042- Sampte C: TCS-110422-13- Fa*: -gl 10424b.wtfP 

Peak Nama: "PFOS* U8ss(**}: -499.0/99.0 amu,499.0no.O amu.499.(V130J) anu* 

C^ommant: *2ppb LCS ECP /Annotation: ~ 

Sample Index: 

Sample Type: 

Concentration: 

Calculated Conc; 

Acq. Date: 

Acq. Time: 

Hodified: 

Proc. Algorithn: 

Noise Percentage: 

Base. Sub. Mlndow 

Peak-Split. Facto 

42 

QC 

2.02 

1.S4 

/25/2011 

:40:02 AH 

Yes 

ntelliOuar 

1.00 

: 0 

Report Largest Peak: No 

Hin. Peak Height: 

Kin. Peak width: 

Smoothing Width: 

Expected RT: 

Use Relative BT; 

Int. Type: 

Retention Time: 

Area; 143 

0.00 

0.00 

0 

14.0 n 

Ho 

Hanual 

13.9 It 

709 cour 

Height: 221000. cps 

Start Tina: 13.6 n 

I

Sampte Nam*:'gi 104241)048' Sampte ID: tCS-l 10422-16* Fite:'g1l0424b.wtr 

P*ak Nam*: -PFOS- Mas£(»s): '499.0/99.0 amu.499.0/80.0 amu,499.0/130.0 ami/ 

Comment: -20ppb LCS ECP Annotation: ~ 

13.0 13J UJO 14.S 15J) 15.5 16.0 16.5 

1289 1339 1388 1438 1488 1537 1587 

Ttn*. min 

Kodlfled: 

Proc. Algorithm: Inl 

Noise Percentage; 

Base. Sub. Window: 

Peak-Split. Factor; 

Report Largest Peak; 

Min. Peak Height: 

Min. Peak width: 

RT Window: : 

Expected RT: 

Use Relative RT: 

Yes 

elliQuan - MQII 

Height: 

Start TJ 

End TiiH 

Manual 

le: 13.9 

116TS095 c 

Sample Type: 

Calculated Conc: 

Acq. Date: 

Acq. Time: 

Proc. Algorithn: 

Noise Percentage: 

Base. Sub. Hindou 

Peak-Spltt. Facto 

QC 

20.2 

21.0 

/25/aOll 

0:27:56 

ntelliOu 

50 

1.0( 

: 0 

Report Largest Paak: No 

Hin. Peak Height: 

Hin. Peak Width: 

Smoothing Width: 

Expected RT: 

Use Relative RT; 

int. Type: 

Retention Time; 

0-C 

0 

14.0 

NO 

Manual 

Area: 14955959 c 

Height: 2 

Start Time: 

End Time: 

20OOO. 

13.6 

14.3 

ng/raL 

ng/mL 

AH 

an - HQII 

min 

) cps 

1 sec 

min 

cps 

min 

min 

S 

f 

2a*€-

2.1*6 

1.9*6 

1.8*6-

1.7*«-

1.6*(-

1.5*6-

1.4*6-

1.0*6 

9.0*5 

8.0*5 

7.0*5 

6.0*5-

5.0*5 

4.0*5 

3.0*5 

2.0*5 

1339 1388 

Tim*, mhi 

Data printed by STW 

Printing Time: 9:53:33 AM 

Printing Date: Monday, July 18 

Page 5 of 6 

Page 70 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS. PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 2011 

Results Name: gll0424b.rdb 

Page 6 of 6 

Page 71 of 98 

*** Ginger AG01330509 

I Sampte Nam*:'gl104241)05r Sampte ID:-GLP10-01-02.17-04r Fl*:'g110424b.wtir 

Sanqile Type; 

late d Cor 755. 

4/25/2011 

1:09:47 ! 

Noise 

Sub. ""•.ndow: 

Spli t 

Report Largest Peek: Nc 

Hin. Peak Height : 0. 

Hin. Peak width : 0. 

Snoothing Width: 0 

RT Window: 30. 0 

Expected RT: 

3XM23*8 

U s e ! RT: No 

8.0*5 

4.0eSData printed by STW 

Printing Time: 9:53:33 AM 

Printing Date: Monday, July 18, 
GLP10-01-02; Interim Report 17 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

*ETS-McCoy Results Name: mcll0512a.rdb 

mcl 10512a.rdb (PFHS): "Quadratic" Regression ("1 / x" weighting): y = 63.4 x''2 + 1.87e-^005 x + 787 (r = 0.9998) 

1.1 1.2 1.3 1.4 

Concentration, ng/mL 

2.5 

Data printed by STW 

Printing Time: 10:11:17 AM 

Printing Date: Monday, July 18 

Page 1 of 1 

Page 72 of 98 
GLPI 0-01-02; Interim Report 17 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

*ETS-McCoy Results Name: mcll0512a.rdb 

• mc110512a.rdb (PFBS): "Quadratic" Regression ("1 / x" weighting): y = -2.63e+003 x'^2 + 2.47e+005 x + 2.26e+003 (r = 0.9997) 

6.0e5-

5.5e5-

5.0e5-

4.5e5-

4.0e5-

3.5e5-

12 

c 

^- 3.0e5-

< 

2.5e5-

2.0e5-

1.5e5-

1.0e5-

5.0e4-

0.0-

/ ^ 

y ^ 

y ^ 

/ ^ 

y ^ 

/ ^ 

. /- ^ 

X^ 

X ^ 

y ^ 

^ 

0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 1.1 1.2 1.3 1.4 1.5 1.6 1.7 

Concentration, ng/mL 

1.8 1.9 

^ 

2.0 2.1 

^ 

2.2 

/ " 

1 

2.3 

1 

2.4 

/ • 

1 

2.5 

Data printed by STW 

Printing Time: 10:09:54 AM 

Printing Date: Monday, July 18, 2011 

Page 1 of 1 

Page 73 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS. and PFOS in Groundwater 

1st Quarter Sampling - 2011 

*ETS-McCoy Results Name: mcll0512a.rdb 

I

SHrplaNam*: "nncl 10512*013' Ssmpt* ID: '10007-51-06* PO*: -mc110512a.wtr 

P*ak Nam*: -pFeS* Ma3s(*9): -299.000/80.000 Da.299.0aU99.000 Da' 

Commant-0.25 r^)/mLFC std in Synth. Watw AmotaHon:'-

Saople Index: 13 

Sample Type: standard 

Concentration: 0.250 ng/mL 

Calculated Conc; O.250 ng/nL 

Acq. Date: 5/lZ/ZOl l 1. 

Acq. Time: 1:27:52 PH 

Hodified ; Ho 

Proc. Algoritlim: IntelliQuan - IQA II 

Hin. Feak Height: 0.00 cps 

Hin. Peak Width: 0.00 sec 

Smoothing Width: 0 points 

BT Window: 30.0 

> Relal 

1 RT; 

• RT: 

10.6 

Ho 

Valley 

10.6 

63874 c 

1.3*4 

1.2*4-

1.1*4-

1.0*4-

9000.0-

§ 8000.DI 7000.0-

6000.0-

6000.0-

4000.0-

3000J>-

2000.0-

1000.0-

0.0-lm^,HfilMiiilh4i>lfcDH 

8.5 

^kUti 

I

SampI* Nam*: *mc110S12a020- Sampt* ID; *11002-78' Fla; 'mc110512a.wtr 

P*Bk Nsm«: -PFBS- Mau(*a): "299.000^0.000 Da.2gdJX)0/99..000 Da' 

Commant: "Method blank' Annotalion:~ 

Sanple Index: 20 

Saople Type: Unknown 

Concentration; M/A 

Calculated Conc: < 0 

Acq. Date: 5/12/2011 

Acq. Tine: 3:52:15 PH 

I

Sampte Nam*;'mc110Sl2a02l' Sampta ID:'GLPia-01-02-154}l3' F3a^VncTlOS12a.w<r 

Paak Nama: 'PFBS' Manfas): -209J)0aB0.000 Da,299.000/99JX)0 Da* 

Commant *OAL SS SS15 RB' Annolatkyi: *" 

Sample Index: 21 

Sample Type 

Concenttati 

Calculated • 

Acq. Date: 

Acq. Tine: 

Kodified: 

Proc. Algor 

Min. Peak a 

Hin. Peak H 

ight 

HrhSmoothing Width: 

RT Window: 

Expected RT 

Use Relativ 

Int. Type: 

Retention T 

Area: 

Height: 

RT: 

Unknow 

H/A 

5/12/< 2 

4:11:5 

Ho 

Intell 

0.0 

0.0 

0 

30.0 

10. 

Ho 

Base r 

10. 

473 

6.04etO 

Star t Time: 

8.5 

I

Sample Nam*:'mc110512a02S' Sampl*ID:TCS-110509-1* FUa:*nKllOS12a.wirr 

Paak Nam*: 'PFBS' Mass(aa}: "299.000/80.000 Da.29S.0O0/99.O00 DaComment '0.2ppb LCS* Annolatlan: ~ 

Sample Index : 2B 

Sample Type: QC 

Concentration : 0.193 ng/nL 1.15*4-

Calculate d Conc: 0.185 ng/nL 

Acq. Date : 5/12/2011 1.10*4 

6:37:1 3 PM ^^ ^ 

,A II 1«> ^ 

9500.00 

9000.00-

8500.00-

8000.00-

7500.00-

7000.00-

6500.00 

^6000.00 

£ 5500.00 

~ 5000.00-

4500.00-

4000.00-

3500.00-

3000.00-

2500.00' 

2000.00' 

1400-

1300 

Proc. Algorithm: 

Hin. Peak Height 

Hin. Peak Width: 

Smoothing width; 

Expected RT: 

Use Relative RT; 

Retention Time: 

Height: 

Start Time: 

End Time; 

IntelliQuan -

0.00 

0 

30.0 

10.6 

Ho 

Base To 

10.7 

551 c 

.03e*00: 

10.7 

10.7 

poin 

Base 

min 

Din 

Bin 

IQA I 

5 

f 

Hodified: 

Proc. Algorithm 

Hin. Peak Heigh 

Hin. Peak width 

Smoothing Width 

RT Window: 

Expected RT: 

Ose Relative RT 

Int. Type: 

Retention Time: 

Height; 

Start Time: 

End Tine: 

Ho 

IntelliQ 

: 0.00 

0.00 

0 

30.0 

Ho 

Valley 

10.6 

47694 C 

1.13e*004 

10.S 

10.B 

Data printed by STW 

Printing Time: 10:12:53 AM 

Printin g Date: Monday, July 18, 2011 

9.0 9.5 10.0 10.5 11.0 11.5 12.0 12.5 13.0 

1500.00-

1000.00-

500.00 

0.00 .niiiiiiii>iiiiuii<4i)MiiWr... 

Page 1 of 3 

Tl"^.r'" 

Page 74 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS. and PFOS in Groundwater 

1st Quarter Sampling - 2011 

*ETS-McCoy Results Name: mcll0512a.rdb 

I

SampteNam*;'mc110512a034' SampI* ID: TCS-110509M' Flla:'mc110512a.wifr 

P*ak Nam*; "PFBS' Mies(*s): *299.000/80.000 Da.299.00O/9gj»O Da' 

Comm*m; '2ppb LCS' Annotatkm:" 

Sample Index: 34 

Sample Type: QC 

Concentration: 1.98 ng/nL 

Calculated Conc; 1.70 ng/mL 

Acq. Date: 5/12/2011 

Acq. Tine: B:40:S9 PM 

Hodified: No 

Proc. Algorithm: IntelliOuan - IQA II 

Hin. Peak width 

Smoothing Width 

RT Window: 

Expected RT: 

Use Relative RT 

Int. Type: 

Height: 

Start Time: 

End Time: 

r 9. 

0 00 

) 30.0 

No 

Valley 

10.6 

lee t 

SOe-tOO 

10.5 

10.9 

I

SampI* Nam*: 'mc110512a021* SampI* ID: "GLP 1(W 1-02-15-013* File: *me1105I2a.wiir 

P*ak Nam*:-PFHS' Mass(*»):'399.00W80.000 Da,399.000«9.000 Da' 

Comm*nt: ^A L SS SSI 5 KB' Aiviotafion:" 

Sample Index: 21 

Sample Type; Unknown 

Concentration: N/A 

Calculated Conc; < 0 

Acq. Date: 5/12/2011 

Acq. Time: 4:12:51 PM 

Modified; No 

Proc. Algorithm: IntelliQuan - IQA 11 

Min. Peak Height: 0.00 cps 

Hin. Peak Width: 0.00 sec 

Smoothing Width: 0 points 

RT Window: 30.0 sec 

Expected RT: 12.6 min 

Use Relative RT: No 

I

Sampl*Nam*:tncll05l2a013' Sampte ID: •10007-61-06" Fi|e:'mcll0512a.wtr 

Paak Nam*: 'PFHS' Ma93{*s): '399.000/80.000 Da,39g.000/99.000 Da' 

Commant "0.25 ngltnL FC std in Synth. Vifatar* Annotation; -

Concentratio 

Calculated C 

Acq. Date: 

Acq. Tine: 

Hodified: 

Proc. Algori 

Min. Peak He 

hn; 

qht: 

Min. Peak Width: 

Smoothing Wi 

RT Window: 

Expected RT: 

Use Relative 

Int. Type: 

th: 

RT: 

Retention Time: 

Area: 

Height: 

Start Time: 

End Time: 

' i 

0.250 

0.243 

5/12/201 

1:27:52 

Ho 

ng/roL 

PH 

[ntelliQuan - IQ 

0.00 

0 

30.0 

12.6 

Ho 

Valley 

12.6 

;ii3 c 

12.5 

12.7 

cps 

pointa 

Bin 

cps 

min 

nin 

Int . Type: 

Retentio n TJ 

Height: 

Star t Time: 

End Time: 

Base Vo Bast 

I

Sampte Mama; •me1105l2a020' Sampte ID: "11002-76' Fle:'mc110612a.«rtr 

P*ak Nam*: 'PFHS' Masa(*s): •399.000«0.000 Da.399.O0W99.OOO Da' 

Comm*nt 'Method blank* Annotatton: -

Sample Index: 20 

Sanple Type: Unknown 

Calculate d Conc: < 0 

Acq. Date : 5/12/201 1 

Acq. Time: 3:52:1 5 PM 

Proc. Algorithm: 

Min. Peak Height 

Min. Peak Width: 

RT Window: 

Eitpected RT; 

Use Relative RT: 

int. Type: 

Retention Time: 

Height: 

IntelliO 

O.OO 

0.00 

0 

30.0 

12.6 

Ho 

Base To 

12.7 

153 c 

.4 6e+002 

uan - IQA 

cps 

Base 

ounts 

cps 

Data printed by STW 

Printing Time: 10:12:53 AM 

Printin g Date; Monday, July 18, 2011 

Page 2 of 3 

Page 75 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

*ETS-McCoy Results Name: mcll0512a.rdb 

I

Sampte Nam*;'mcl 10512a028* Sampte ID: TCS-110509-1' Flte: "mcl 10512a.w<ir 

Paak Nam*; 'PFHS' Maaa(as): '399.000/80.000 Oa.399.00Q/99J»0 Da' 

Commant: '0.2ppt> LCS" AntMtatton: ** 

Sample Index : 28 

Sample Type: 

Concentration: 

Calculated Conc: 

Acq. Date: 

Acq. Tine: 

Modified: 

Proc. Algorithm: 

Min. Peak Width: 

Snoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time; 

Area: 

Height: 

Start Time: 

End Time: 

QC 

0.198 

0.201 

5/12/2011 

6:37:13 P 

Ho 

IntelliQu 

: 0.00 

0.00 

30.0 

12.6 

No 

Valley 

12.6 

38227 CO 

..O2a-tO04 

12.5 

12.7 

ng/mL 1.00*4 

9500.00-

9000.00-

8500.00-

8000.00-

7500.00-

7000.00-

6500.00-

6000.00-

§•5500.00-

• 5000.00-

^ 4500.00-

4000.00 

3500.00 

3000.00 

2500.00 

2000.00 

1500.00 

1000.00 

500.00 

0.00 I th iBil^liJllMlill^UUljWMill*! kmJmMi 

13J2 1385 ,4 ^ 14.74s. 

14.5 15.0 

Sampte Nam*:'^nc110512a034' Sample ID: TCS-IIOSOM* F)l*:*mc110512a.wtir 

Paak Nam*: *PFKS* I4ass(*s): '399.000/801)00 Da,39g.000/99.000 Da' 

Commant *2ppb LCS* Annotatton:" 

Sanple Type: OC 

Concentration: 1.98 ng/nL 

Calculated Conc: 1.74 ng/raL 

Acq. Date: 5/12/2011 

Acq. Time: 8:40:59 PM 

Modi 

RT W 

led: 

Algc 

Peak 

Peak 

nlng 

ndow 

rithn; 

Height 

Width: 

Expected RT: 

Use Relat 

Int. 

Betei 

Area 

Heig! 

Star 

End 1 

Type 

tion 

C; 

Tim 

ime: 

ve RT: 

Time: 

No 

IntelliQu 

0.00 

0.00 

0 

30.0 

12.6 

Ho 

Valley 

326059 CO 

• .51a-t004 

12.e 

Data printed by STW 

Printing Time: 10:12:53 AM 

Printin g Date: Monday, July 18, 

Page 3 of 3 

Page 76 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

*ETS-McCoy Results Name: mcll0514b.rdb 

mc110514b.rdb (PFOS): "Quadratic" Regression ("1 / x" weighting); y = 0.0025 x*2 -H.27 x -•• 0.0126 (r = 0.9999) 

35 

34 

12 14 

Analyte Conc. / IS Conc. 

Data printed by STW 

Printing Time: 10:15:01 AM 

Printing Date: Monday, July 18, 2011 

Page 1 of 1 

Page 77 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 2011 

*ETS-McCoy Results Name: mcll0514b.rdb 

I

Sampte Nam*:'mcl 10514b014- Swt^lD : *10007-61-09* Flte;'mc110514b. 

P*ak Nam*: *13C8PFOS^S(IS)' Matifas): '507.000/80.000 DaCommarrt: *2.5 nglmL FC ctd in Synth. Watat* Annotatton:" 

Sample Index : 11 

Sample Type: Standar d 

Concentration ; O.960 ng/mL 

Calculate d Conc 

Acq. Tin 

'15/201 : 

11:54 i 

Hodified : Ho 

Proc . Algorithm: Specify Paramet 

Noise Percentage : SO 

Base . Sub. Nindow: 1.00 min 

Peak-Split . Factor: 2 

Hin. Peak Height: 

Min. Peak Nldth : 

Smoothing Hidth : 

BT Window: 

0-00 

I

Sampte Nam*:'mcl 10514b023' Sampte ID:'GLP1CM}1-02-17-Oir FUe:-mc110514b. 

Paak NanM: '13C8PFOS-IS{IS)' Maas(«3); 'S07JXKI/80XOO DaComment: -GW 31 TL Ql Y11 CP 0- Annotation; ** 

Sample Index: 23 

SampteName:*me1l05l4t)021' Sampte ID:'11002-76' Fito:-mcll05l4b.««r 

P*Bk Nam*: '13C8PFOS-tS{(S)^ Uasa{*s): •«07.00(VBO.OOO Da' 

Commant "Method Mank* Anrwtalton: ** 

Sample Index: 21 

Sample Type; Unknown 

Concentration : 0.960 ng/mL 

Acq. Datr- t/.c,^«, S/lS/20 , 5-5»< : 

11:37;5: AH 

Proc. Algorithn: 

Base. Sub. Hindot 

Peak-Split. Facto 

Report Largest Pe 

Hin. Peak Height; 

MIn. Peak Width: 

Smoothing width: 

Expected RT; 

Use Relative RT: 

Int. Type: 

Betention Time: 

Specity 

SO 

r: 2 

k: Y« 

0 

0 

3 

30.0 

13.8 

Ho 

valley 

13.8 

Area: 232122 c 

Height: 5 

End Time: 

75et00 

13.7 

14.0 

paiame 

0 mi 

OO 9 

min 

cps 

min 

11.5 12.0 

SampteName:'mc110514t)029' SanfteID:*GLP 10-01-02-17-05r File:'mcl10514b.wtr 

P*akName:'13C«PFOS-IS(IS)' Mass{*s):-507.000/80.000 Da" 

CommenfGW 3261Q1Y11 CPO' " " ~ 

Sample Index: 29 

Type; Unknown 

0.955 ng/raL 

Sample Type: 

Calculated Con 

Acq. Date: 

Acq. Time; 

Unknown 

0.955 

= : M/A 

5/15/2011 

12:19:34 PM 

ll/A 

, Algorithm: Specif y i 

Sub. Wine 

Hois< 

Peak-Split . Factor : 

Repor t Larges t Peak ; 

Hin . Peak Height ; 

Min . Peak Hidth : 

Smoothin g Width : 

B T Window : 3( 

Expecte d RT : 1 

U s e Relativ e RT : I 

Int . Type : VaJ 

Acq . Date ; 5/15/201 1 

Acq. Time: 2:24 

Hodified: 1 

Proc. Algorithm: Spec 

Hoise Percentage: 

Peak-Split. Factor; 

Report Largest Peak; 

Hin. Peak Height: 

Hin. Peak width: 

Smoothing Width: 

BT Window; 30 

40 PM 

, fy Pa 

50 

2 

Yes 

0.00 

3 

0 s 

Data printed by STW 

Printing Time: 10:16:22 AM 

Printin g Date: Monday, July 18, 2011 

Page 1 of 4 

TTM" * 

Page 78 of 98 
GLP10-01-02: Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

*ETS-McCoy Results Name: mcll0514b.rdb 

• Sampte Nama: "mcl 10514t)03r S8mptelD:-VCS-110513-1* FU*;*mc110514b.wtfr 

I Paak Nama:'13C6PFOS-IS(IS)' Ma>a(*s):'507.000/80.000 Da* 

I Commant: *0J2p()b LCS ' Annolatton:" 

Sample Index : 37 

Sample Type; QC 

Concentration : 0.951 ng/nL 

Calculate d Conc: N/A 

Acq. Date: 

Acq. Time; 

Hodified: 

Proc. Algorithm; 

Noise Percentage 

5/15/20 

No 

Specify 

50 

Base. Sub. Window: 1. 

Peak-Split. Factor: 2 

Beport Largest Peak: t i 

Hin. Peak Height 

Hin. Peak width: 

Smoothing Width: 

BT Window: 

Expected RT: 

Use Relative BT: 

Int. Type; 

Betention Time: 

0 

0 

3 

30.0 

13.8 

No 

Valley 

13.8 

Area: 1893S3 c 

1 

PH 

Pa 

n 

on 00 

ou 

I SampteNam*:-YiicllO514bO40- SafH)lalD:TCS-110513-10* Flte:-mcl 10514b.w«r 

Calculated 

Acq. 

Acq. 

Modi 

Proc 

Peak 

Hfn. 

Smoo 

Date: 

Time; 

fled: 

Algo 

: Perc 

Sub. 

-Split 

Peak 

thing 

Conc: 

rithra; 

Windo 

5/ 

6; 

H/A 

5/20: 

4:04 

Yes 

specify 

Factor: 

leight 

[idth: 

Width: 

50 

1.1 

Y' 

0 

0 

3 

PH 

Pa 

n 

no 

I

Sampte Nam*:'mc110514b05r SaiTtialD:*LCS-ll0513-l3' Flte:'mc110514b.wtr 

Peak Nama:'13C8PFOS-<S(IS)- Mass{«s):'507.000/80.000 Da* 

Comment '2ppb LCS ECF* Annotation; ** 

.ample Index : 51 

0.951 

K/A 

5/15/2011 

::3S PM 

I

Sampte Name: 'mcl 105141)043' 

P»ak Nama: -13C8PFOS-IS{IS)' 

Comment:*2ppbLCS' Annotatton:' 

Sample Index: 43 

Sample Type: 

Calculated Conc: 

Acq. Time: 

Hodified: 

Koise Percentage: 

Base. Sub. window: 

Peak-Split. Factor 

Beport Largest peal 

Hin. Peak Height: 

Hin. Peak Hidth: 

Smoothing width: 

BT Window: 

Expected BT: 

Use Relative RT: 

Int . Type: ' 

Specify Parameters -

Calculated Conc; 

Acq. Date: 

Acq. Time: 

Hodified; 

Proc. Algorithm: 

Koise Percentage 

Base. Sub. windo 

Peak-Split. Fact 

Beport Largest P 

Hin. Peak Height 

Min. Peak Width: 

Smoothing Width: 

Expected BT: 

Use Relative RT: 

Retention Time: 

>1/A 

5/15/2011 

10:03:35 PH 

Yea 

Specify paramete 

50 

; 1.00 min 

r: 2 

ak: Yes 

0.00 sec 

30.0 sec 

13.8 min 

No 

Valley 

13.8 min 

Area: 230816 counts 

5.58^.004 cp» 

Data printed by STW 

Printin g Time: 10:16:22 AM 

Printin g Date: Monday, July 18, 2011 

Page 2 of 4 

Page 79 of 98 
GLPI 0-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 2011 

*ETS-McCoy Results Name: mcll0514b.rdb 

I

Sampte Name:'mcl I0514b0l4' Sampte ID; 

P*ak Nam*:'PFOS* Mass(*s): *499.00(VB0. 

Commant:-Uno'mL FC atd In Synth. Watai' 

SBD^ile Index: 14 

Standi 

•10007-S1-09* Fite:'mc110 

.000 Da,499.00(VM.OOO Da.4( 

Sample Type: 

Concentrat 

Calculatec 

ng/mL 

Acq. Time: >;11;54 

Hodified : No 

Proc . Algorithm: Specify Paramete : 

Koise Percentage : 50 

Base . Sub. window; 1.00 min 

Peak-Split . Factor: 2 

Beport Largest Peak: Yes 

Hin. Peak Height: 0.00 cps 

Min. Peak Width: 0.00 se c 

Smoothing width ; 3 po; 

1.4*5 

1.3*5 

1.3*5 

1.2*5 

1.2*5 

1.1*5 

1.1*5 

1.0*5 

9.5*4 

9.0*4 

8.5*4 

8.0*4 

7.5*1 

7.0*4 

6.5*4 

6.0*4 

5.5*4 

5.0*4 

4.5*4 

4.0*4 

3.5*4 

3.0*4 

2.5*4 

2J}*4 

1.5*4 

1X)«4 

5000.0 

0.0 

13 82 

k 

I

Sampte Nam*: 'mcl 10514b023' Sampte ID: 'C^Pl0-01-02-17-0ir File: *mcl 10514b.wtfr 

Paak Nam*: "PFOS* MaM(oa): '499.000/80.000 Da,499.00(V99.000 Da.499.000/130.000 Da' 

Comment:-GW 317LQ1Y11 CPO" Annolatton:-

Sample Index: 23 

I

Sampte Nama: *mc110514b021' S8mptelD:-11002-76* Fla:*mc110514b.wtfr 

Paak Nam*: -PFOS* Mass<*a): '499XXXVS0JX)0 Da,499.000/99.000 Oa.499.00a'130.000 Da' 

Commant: "Matltod Uar^ Annolatton; ~ 

Sample Index: 21 

Sample Type; Unknown 

Concentration; ll/A 

Calculated Conc; 0.00376 ng/mL 

Acq. Date; 5/15/2011 

Acq. Time: 11:37:51 AM 

750' 

:ed: Yes 

Proc. Algorithm: Specify Paramet* 

Hoise Percentage: 50 

Base. Sub. HindoM: 1.00 nin 

Peak-Split. Factor: 2 

Beport Largest Paak: Yas 

Hin. Peak Height: 0.00 cpi 

Hin. Peak Width: 0.00 se( 

Smoothing width: 3 pc 

RT Window: 30.0 sec 

Expected RT; 13.8 ni n 

Use Relativ e RT: Wo 

Int . Type: Manual 

- HQ II I 

Sample Type: 

Concentration: 

Calculated Conc: 

Acq. Time: 

Kodified: 

Proc. Algorithm; 

Hoise Percentage 

Base. Sub. Windo 

Peak-Split. Fact 

Beport Largest P 

Hin. Peak Height 

Kin. Peak Width: 

Snoothing Width: 

RT Window: 

Expected RT; 

Use Relative RT: 

Int. Type; 

Retention Time; 

Height: 

Start Time: 

End Time; 

Unknown 

H/A 

0.268 

5/15/201 

12:19:34 

Yes 

50 

<: 1. 0 

or; 2 

Eak: Ye 

0. 

3 

30.0 

13.8 

Ho 

Hanual 

13.8 

3174 c 

.30et004 

13.4 

13.9 

PH 

1 

10 

10 

m 

D) 

OF 

n 

I

SampteNama;'mcl10514b029' SarT¥telD:"GLP1^01-02-17-05r FUe:'mc110514b.viir 

P*ak Nam*: 'PFOS* Maaa(*s}: '499.000/80.000 Da.4d9.000/99.000 Da,499.000*130.000 Da' 

Commem:*GW32eLQl YllCPO' Annotatton; ** 

Sample Index : 29 

Sample Type; Unknoon 

Calculate d Conc: 1.42 ng/mL 

Acq. Date: 5/15/2011 3.4*4-

Acq. Time: 2:24:4 0 PM 

3.2*4 

2.8*4 

2.6*4 

2.4*4 

2.2*4 

2.0*4-

13*4-

Modified: 

Koise Percentage 

Base. Sub. Wlnde 

Peak-Split. Fac 

Yes 

Specify 

: 50 

Report Largest Peak: Y' 

Min. Peak Heigh 

MIn. Peak width 

Smoothing Width 

BT Window: 

Expected BT: 

Use Relative BT 

Area: 

Height; 

Start Tine: 

End Time; 

: 0. 

30.0 

13.8 

Ho 

Hanual 

56233 c 

3.57e*00-

13.2 

14.0 

) min 

)0 cps 

po 

min 

nin 

cps 

min 

1.2*4 

1.0*4' 

8000.0-

6000.0 

4000.0-

2000.0-

5.5 16.0 

0.0 

1Z.5 13.0 13.5 14.0 14.5 15.0 15.5 

Data printed by STW 

Printing Time: 10:16:22 AM 

Printing Date: Monday, July 18 

Page 3 of 4 

Page 80 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

*ETS-McCoy Results Name: mcll0514b.rdb 

I

SanvteNam*:*mcll0514b03r Sampte ID: TCS-110513-1' FUa:*mc110514b.<*tfr 

Paak Nam*: "PFOS* U3ss(*s): *499JKXVSO.00O Da.499.0O0/99.OO0 Da,49gX)00/130.000 Da' 

Comment: *0.2ppb LCS * Annotafion: ** 

Sample Index: 37 

Sanple Type: QC 

Concentration: 0.199 ng/mL 

Calculated Conc: 0.188 ng/mL 

Acq. Date: 5/15/2011 

Acq. Time: 5;11:30 PM 

Hodified; Ho 

Proc. Algoritlim: i 

Hoise Percentage: 

Base. Sub. Window; 1 

Peak-Split. Factor; 2 

Report Largest Peak: 

Min. Peak Height: i 

Kin. Peak Width: 

Smoothing Width: 

RT Window: 30.0 

Expected RT: 

Use Relative RT; No 

Int. Type; Valle; 

Retention Time: 13.1 

Area: 50012 

Height: 1.17e40( 

fy Parameter! 

3.8 

Mod I 

Proc 

Hois 

Base 

Peak 

MIn. 

Smoo 

iod: Y 

Algorithm: Spec 

Percentage: . 

Sub 

Spli 

Peak 

hlnq 

RT Window 

Window: 

gest Peak; 

Height: 

Width: 

30 

Expected BT: 1 

Use 

Int. 

Ftete 

Area 

)elat 

Type 

Height: 

Star Tiin 

End Time: 

ve RT: H 

Han 

Time; 1 

69754 

1.13e 

1 

Sampte Nam*:'mcl10514b040' SaiTfi*ID:1 

P*ak Nam*; 'PFOS' Mass(*s): *499.00a'8tl ~ 

Commont "Oippb LCS ECP Annolatton: -

Sanple Index: 40 

Sample Type: OC 

Concentration : 0.201 ng/mL 

Calculate d Conc: 0.19e ng/mL 

Acq. Bate : S/lS/2011 

Acq. Time: 6:14:04 PM 

1.10*4 

1.05*4-

1.00*4 

9500X0 

9000X0 

8500.00 

8000X0 

7500.00 

7000.00 

6500.00 

& 6000.00 

I 5500.00 

^ 5000.00 

4500.00 

4000.00 

3500.00 

3000.00-

2500.00-

2000.00 

1500.00-

1000.00 

500.00-

0.00 

I

SamrfaNam*:"mcl 105146043* San^lO:-LCS-110513-4' Fite:*mc11D514b.wir 

P*ak Nam*: -pFOS' M«K(«S); '499.000/80.000 Da ,499.000/99X00 Da.499.000/130.000 Da' 

Comm*nt:'2ppbLCS* Annotation;" 

Sample Index: 43 

Sample Type; QC 

Concentration: 1.99 ng/mL 

Calculated Conc: 2.22 ng/mL 

Acq. Date: 5/15/2011 

Acq. Time: 7:16:38 PM 

Kodified : Yes 

Proc . Algorithm; Specif y Parameters - HQ II I 

Hois e Percentage : 50 

Base . Sub. Window: 1.00 ni n 

Peak-Spilt . Factor: 2 

Report Largest Peak: Yes 

k Height: 0.00 cps 

Sampte Nam*:'mcll0514bO5r Sampte 10:1 

Paak Nam*: 'PFOS' Uass(*s): '499.000/80.01 

Comment *2ppb LCS ECF* Annotatton: "• 

Sample Index; 51 

2.0 5 n? 

5/15/2011 

10:03;3 5 PM 

Kin. Peak 

Smoothing Wlc 

RT Window: 

Expected RT; 

Use Relativ e 

Height; 

Star t ti l 

End Tina 

poll 

Hodified : 

Proc . Algocithm: 

Hoise Percentage . 

Base . Sub. Window 

Peak-Split . Fact o 

Beport Largest Fe 

Hin. Peak Height: 

Kin. Peak width ; 

Width: 

Specif y Paramel 

i: 1.00 mil 

638286 counts 

9.5*4 

9X*4-

8.5e4 

8.0*4 

7.5*4 

7.0*4 

8.5*4 

6.0*4 

5.5*4-

5.0*4-

43*4 

4Xe4 

3.5*4-

3.0*4-

2.5*4-

2.0*4-

1.5*4-

1Xe4-

5000.0-

OXData printe d by STW 

Printing Time: 10:16:22 AM 

Printing Date: Monday, July 18, 

Page 4 of 4 

13.0 13.5 14.0 14.5 15X 15.5 IfiX 

Ttm*. mlr| 

Page 81 of 98 
GLPI 0-01-02; Interim Report 17 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

*ETS-McCoy Results Name: mcll0517a.rdb 

Data printed by STW 

Printing Time: 10:18:27 AM 

Printing Date: Monday, July 18, 2011 

Page 1 of 1 

Page 82 of 98 
GLP10-01-02; Interim Report 17 

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

1 st Quarter Sampling - 2011 

*ETS-McCoy Results Name: mcll0517a.rdb 

I

San^toNamei-mcliOSITaOnS- Sampte ID:-nOOO?.??-!!* Fito:-mcl 1051T«..rf(r 

P«ak Naffl«: -PFOS* Ma»<M): '499X00/80.000 Da.499.aO<Vg9J)00 Oa.499X00/13OX00 Da* 

Cammant'lOngrmLFCcUkiMBQwator- Annotation: 

Sacple Index: 15 

saople Type; 

Concentration: 

Acq. Date: 

Acq. Time: 

Hodified: 

Proc. Algoritliiii 

Hin. Peak Heigh' 

Hin. Peak Width 

Smoothing Width 

RT Window: 

Use Relative RT 

Int. Type: 

Retention Tine: 

Standard 

10.0 

10.1 

5/n/201 

1:29:52 

No 

IntellK 

: 0.00 

0.00 

0 

30.0 

13.1 

No 

Base To 

13.7 

Area: 883112 c 

Height: 2.26e-f005 

ng/ml. 

PH 

uan - IC 

points 

sec 

min 

Base 

ain 

cps 

I

Sampte Name: *mc110517a02r San^ite ID: "GLPI 001.02-17-4)65' Flte: *nv;110S17a.wHr 

P*ak Nam*: "PFOS' Mass(*a): '499XO0/W.OOO Da.499.OOCV99XO0 Da.499JKKV 130.000 Da* 

Comm*nt:*GWGRS04Q1 Y11CP0(200x)- Annotation:** 

Sample Index: 22 

Sample Type: Unknown 

Concentration; H/A 

Calculated Conc: 3150. ng/mL 

Acq. Date: 5/17/2011 

• Conmant*MaOw 

Saople Type: 

Concentration: 

Acq. Date; 

Acq. Time; 

Hodified: 

Proc. Algorithn: 

Hin. Peak Height 

Hin. Peak width; 

Smoothing Width: 

RT Window: 

ratar TN11-0184 

21 

Unknown 

M/A 

< 0 

5/17/2011 

3:33:06 PM 

Ho 

IntelliQuan 

0.00 c 

0.00 s 

0 po 

30.0 s 

I

Sampte Nama: tnc110517a028' Sampte ID: *LCS-l105l7-r Fie:-mcllOSWa-wr 

Paak Nama: TFOS* Mass<**): -499.000ra0.000 Da,499X0W99X00 Da,499.000/130.000 DaComment "5ppb LCS- Annotation: *" 

Modified: 

Proc. Algorithm: 

Min. Peak Height: 

Min. Peak Width: 

Smoothing width: 

IntelliOuan - IQA I 

14*5 

1.3*5 

1.3*5 

1J*5 

1.2*5 

1.1*5 

1.1*5 

1.0*5 

9.5*4 

9X*4 

8.5*4 

8.0*4 

7.6*4 

7.0*4 

6.5*4 

6.0*4 

5.5*4 

5.0*4 

4.5*4 

4.0*4 

3.5*4 

3.0*4 

!.6*4 

2.0*4 

1.5*4 

1.0*4 

SOODX 

13.35 

J 

Sanple Index; 

Sample Type: 

Concentration: 

Calculated Conc; 

Acq. Date: 

Acq. Time: 

Hodified: 

Proc. Algorithm: 

Hin. Peak Height 

Hin. Peak Hidth: 

Smoothing width: 

RT Window: 

Use Relative RT: 

Int. Type: 

Retention Time; 

26 

OC 

5.82 

S/17/2011 

5:56:55 PM 

No 

IntelliQua 

0.00 

0.00 

0 p( 

13.7 

Ho 

Valley 

13.7 B 

Area: 507654 cou 

Height: .25etO0S c 

13X 13.5 14X 

Data printed by STW 

Printing Time: 10:20:21 AM 

Printing Date: Monday, July 18, 

Page 

Page 83 of 98 
GLPI 0-01-02; Interim Report 17 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 2011 

*ETS-McCoy Results Name: mcllOSna.rdb 

Data printed by STW 

Printing Time: 10:20:21 AM 

Printing Date: Monday, July 18, 2011 

Page 2 of 2 

Page 84 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

ATTACHMENT C: ANALYTICAL METHOD 

Page 85 of 98 
GLPI 0-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

3M Enviromneiilai Labofatoiy 

Method 

Method of Analysis for the 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 UI ^ f o 1 

Approved By: 

^/^j/c:^ 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 Page 86 of 98 
GLPI 0-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 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), PerfluoroundecanoicAcid (PFUnA), 

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

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

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

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

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

Performance Liquid Chromatography/Mass Spectrometry". 

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

defined QC elements are satisfied. 

Sample collection is not covered under this analytical procedure. 

2 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 detemnined 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% ofthe 

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 ofthe Working Standard (WS) into a predetermined 

amount of ASTM Type 1, 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 1, HPLC grade water, or other suitable water, placed in a sample container in the laboratory 

and treated as a sample in all respects, including exposure to sampling site conditions, storage, 

preservation and all analytical procedures. The purpose ofthe 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 87 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 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 ofthe 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 ofthe 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 ofthe sample analysis. 

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

An aliquot of ASTM Type 1, HPLC grade water, or other suitable water, to which known quantities of the 

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

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

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

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

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

3.7 Laboratory Control Sample (LCS) 

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

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

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 determine whether the sample 

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

sample matrix must be detemnined in a separate aliquot and the measured values in the LMS con^ected 

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

3.9 Laboratory Sample 

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

3.10 Limit of Quantitation (LOQ) 

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

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

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

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

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

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

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

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 88 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 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 quantify 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 fypically a target analyte with at least one atom 

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

control samples. Sun-ogate(s) are added to quantitatively evaluate the entire analytical procedure 

including sample collection, preparation, and analysis. Inclusion of a surrogate analyte is an optional 

qualify 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 toxicify 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 safefy glasses to prevent exposure to chemicals that might be present. 

The laboratory is responsible for maintaining a safe wori< environment and a current awareness of local 

regulations regarding the handling ofthe chemicals used in this method. A reference file of material safefy 

data sheets (MSDS) should be available to all personnel involved in these analyses. 

4.2 Cautions 

The analyst must be familiar with the laboratory equipment and potential hazards including, but not limited 

to, the use of solvents, pressurized gas and solvent lines, high voltage, and vacuum systems. Refer to the 

appropriate equipment procedure or operator manual for additional information and cautions. 

5 Interferences 

During sample preparation and analysis, major potential contaminant sources are reagents and 

glassware. All materials used in the analyses shall be demonstrated to be free from interferences under 

conditions of analysis by njnning 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 89 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

Parts and supplies that contain Teflon® should be avoided or minimized due to the possibilify of 

interference and/or contamination. These may include, but are not limited to: wash bottles. Teflon® lined 

caps, autovial caps, HPLC parts, etc. 

The use of disposable micropipettes or pipettes to aliquot standard solutions is recommended to make 

calibration standards and matrix spikes. 

6 Instrumentation, Supplies, and Equipment 

6.1 Instrumentation and Equipment 

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

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

(LC/MS/MS). I 

Analytical balance capable of reading to 0.0001 g 

A device to collect raw data for peak integration and quantitation 

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

Gas tight syringes, 25|JL, 50|JL, 100|JL, 250|JL, 500|JL, 1000|JL. 

1 mL plastic HPLC autovial. 

Disposable pipettes, polypropylene or glass as appropriate 

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

6.2 Chromatographic System 

Guard Column: Prism RP, 4.6 mm x 50 mm, 5 pm 

Analytical Column: Betasll CI 8,4.6 mm x 100 mm, 5 ^Jm 

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 |JL. 

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

RunTime: ~ 17minutes. 

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

provided that data qualify 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 90 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

6.3 MS/MS System 

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

Analyte 

PFBA 

PFPeA 

PFHA 

PFHpA 

PFOA 

PFNA 

PFDA 

PFUnA 

PFDoA 

PFBS 

PFHS 

PFOS 

Transition Monitored 

213^169 

263^219 

313 ^269 and 313 ^119 

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

413 ^ 369, 413 -^ 219 and 413 -^ 169 

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

513 ^ 469, 513 -» 219 and 513 -^ 269 

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

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

299 -^ 80 and 299 -> 99 

399 -^ 80 and 399 -> 99 

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

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

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

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

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

The previous information is intended as a guide, altemate instalments 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 

PerfluoroundecanoicAcid (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 

Page 91 of 98 

Analysis 
GLPI 0-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 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: Altemative volumes may be prepared as long as the ratios ofthe solvent to solute ratios are maintained. 

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

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

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

when diluting stock solutions to appropriate levels. 

100 \iglmL 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 sfandard operating 

procedure. An example of purify and salt con-ection is given below for PFOS. 

^. , ^ molecular weight of anion 

salt correction factor = 

moclecular weight of salt 

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

538 

10 mg CsFiySOsK* with purify90% = 8.35mg CsFiySOs"(10 mg*0.90*0.9275=8.35 mg) 

5 |jg/mL (5000 ng/mL) mixed working standard-^dd 0.5mL each ofthe 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 [jg/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 ofthe 5 jjg/mL-mixed wori<ing standard solution to a 25mL volumetric 

flask and bring up to volume with solvent. 

Storage Conditions—Store all SSSs and working standards in accordance with laboratory standard operating 

procedure or in a refrigerator at 4°±2°C for a maximum period of 6 months from the date of preparation. 

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 

Page 92 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

7.5 Calibration Standards 

Using the worthing standards described above, prepare calibration solutions in ASTM Type 1 water, HPLC water, or 

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

be adjusted to meet the data qualify 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 ASTM Type 1 Water, 

or other suitable water 

0.025 

0.0375 

0.050 

0.075 

0.100 

0.250 

0.500 

1.00 

2.50 

5.00 

10.0 

8 Sample Handling 

8.1 Water Sample Preparation 

This method is applicable to clean water samples. Samples containing heavy particulate may not be suitable for 

analysis by this method. Samples containing suspended particulate should be centrifuge prior to removing a 

sample aliquot, or filtered. 

Thoroughly mix sample before removing an aliquot and placing in a labeled plastic autovial. Plastic is 

preferred over the use of glass autovials, to prevent the possibly of fluorochemical sticking to the glass. 

Dilute sample, if necessary, with ASTM Type 1, HPLC water, or other suitable water. 

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

Prepare at least five method blanks. 

9 Sample Analysis - LC/MS/MS 

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

weighted 1/x or unweighted, or by quadratic fil (y = ax^ + bx + c), weighted Mx 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-determined acceptance criteria. Low-level curve 

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

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

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

ETS-8-044.0 Page 8 of 11 

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

Analysis 

Page 93 of 98 
GLPI 0-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 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 construct the calibration curve. 

If the calibration curve does not meet acceptance criteria, perform routine maintenance or prepare a new standard 

curve (if necessary) and reanalyze. 

Continuing calibration verifications (CCV) are analyzed to verify the accuracy ofthe calibration cun/e. Analyze a 

mid-range calibration standard, one ofthe same standards used to construct the calibration curve, at a minimum 

after every tenth sample, not including solvent blanks, with a minimum of one per sample set. Calibration 

verification injections must be within ±25% to be considered acceptable. The calibration curve and the last passing 

CCV will then bracket acceptable samples. Multiple CCV levels may be used. 

Samples containing analytes that are quantitated above the concentration ofthe highest standard in the 

curve should be further diluted and reanalyzed. 

10 Quality Control 

10.1 Data Quality Objectives 

This method and required qualify control samples is designed to generate data accurate to ±30% with a targeted 

LOQ of 0.025 ng/mL. Any deviations from the qualify 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 from 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 mn. 

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

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

the mean area counts ofthe method blanks exceed 50% ofthe LOQ standard, then the LOQ must be raised to the 

first standard level in the curve that meets criteria, or alternatively, the method blanks must be evaluated 

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

10.3 Sample Replicates 

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

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

replicates excludes field blanks. 

10.4 Surrogate Spikes 

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

10.5 Lab Control Sample 

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

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

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

The relative standard deviation ofthe 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 Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection 

Analysis 

Page 94 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 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% ofthe 

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

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

The targeted fortification levels should be at least 50% ofthe 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 ofthe sample and the field duplicate should be used to calculate the recovery. 

11 Data Analysis and Calculations 

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

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

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

Slope 

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

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

percent recovery. 

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

Analyte added (ng/mL) 

12 Method Performance 

Any method performance parameters that are not achieved must be considered in the evaluation ofthe 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 performed on the system and 

samples reanalyzed, or other actions taken as appropriate. Document all actions in the raw data. 

If data are to be reported when 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 Suitabilify standards are not a required component of this method. If required by protocol or by the 

technical manager, a minimum of three system suitebilify 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 suitabilify injections must 

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

12.2 Quantitation 

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

equal to 0.990. Each point in the curve must be within ±25% ofthe theoretical concentration with the exception of 

the LLOQ, which may be within ±30%. 

CCV Performance: The calibration standards that are interspersed throughout the analytical sequence are 

evaluated as continuing calibration verifications in addition to being part ofthe calibration curve. The accuracy of 

each curve point must be within 25% ofthe theoretical value (within 30% for lowest curve point). Samples that are 

bracketed by CCVs not meeting these criteria must be reanalyzed. 

ETS-8-044.0 Page 10 of 11 

Method of Analysis for the Detemnination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection 

Analysis 

Page 95 of 98 
GLPI 0-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1 st Quarter Sampling - 2011 

Demonstration of Specificity: Specificify 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 ofthe low-level calibration curve points. Refer 

to Section 10 for additional details. 

12.4 Accurac y 

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

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

spikes and laboratory matrix spikes. 

12.5 Precision 

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

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

requirement for replicates excludes field blanks or rinse blanks. 

Section 10 contains additional information 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 internal procedures. 

14 Records 

Each data package generated for a study must include all supporting information for reconstmction ofthe data. 

Information 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 (instmment batch records, instmment acquisition 

method, summary pages), instmment results files, chromatograms, calibration 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 Detemnination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection 

Analysis 

Page 96 of 98 
GLP10-01-02; Interim Report 17 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

1st Quarter Sampling - 2011 

ATTACHMENT D: DEVIATION(S) 

Page 97 of 98 
GLP10-01-02; Interim Report 17 

RECORD OF DEVIATION/NON(fW6Sii^f!&iSu"°'"°TM""^^^'^ 3uarter Sampling - 201^ 1 

/. Identification 

Study / Project No. 

GLP10-01-02-17 

Deviation type D SOP 

(Check one) D Protocol 

Date(s) of OccunTsnce: 

g11419b 

G Equipment Procedure 

D GPO 

Document Number 

ETS-8-044.0 

m Method 

D Other: 

//. Descriptio n (attach extra pages as needed) 

Method Requirements: 

1. RPD values S20% (section 10.3). 

2. FMS recovery within ±30% (section 10.6). 

Actual procedure/process: 

1. The following sampling locations had sample/sample duplicate RPOs outside method acceptance criteria; 

DAL GW 227R: PFBS (24%), PFHS (23%), PFOS (23%). DAL GW 312R: PFHS (26%) and PFOS (34%). 

and DAL GW 331S: PFBS (29%). 

2. The following sampling locations had FMS samples outside method acceptance criteria; DAL GW 203L HS 

for PFOS (138%), DAL GW 335S HS for PFBS (134%), DAL GW GRS04 HS for PFOS (<50%), and DAL 

GW 327R LS for PFHS (141%). 

IIL Actions Taken 

(such as amendment issued, SOP revision, etc.) 

Con-ective Action (D Yes IZI No) Referent: 

Acceptability of the nonconforming work: 

1. Sampling locations with RPD values outside method acceptance criteria will be flagged In the report. 

2. Sampling locations with FMS recoveries outside method acceptance criteria will be flagged In the report 

and the analytical uncertainty adjusted for PFOS for DAL GW 203L. PFBS for DAL GW 335S, and PFHS 

for DAL GW 327R. No PFOS results will be reported for DAL GW GRS04 since the recovery ofthe HS 

was <50%. 

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: 

Study Director (if GLP): 

Sponsor Approval (for GLP protocol deviations): NA 

Technical Reviev*/er (optional): NA 

Laboratory Department Manager Approval: 

Date: * > 

"7//f/// 

Date:^^^f( 

Date: NA 

Date: NA 

Date: . 

y//^//r 

IV. Authorization to Resume Work 

Where halting of worfc occurred, resumption of worfc must first be approved by Lalmratory Management 

Laboratory Department Manager Approval: NA Date: NA 

Deviation No, 

(assigned by Study Director or Team Leader at the end of study or prefect) 

ETS-4-008.7 Page 1 of 1 

Documentation of Deviations and Control of Nonconforming Testing Page 98 of 98