GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

3M 

GLP10-01-02: Interim Report 11 - Analysis of PFBS. PFHS. and PFOS in Ground Water 

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

in November 2010 

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 

Maplewood, MN 55144 

Project Identification 

GLP10-01-02-11 

Total Number of Pages 

104 

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

Competence of Testing and Calibration L^tMiatories", In accordance with the A2LA Certificate #2052.01. 

Testing that compiles with this Intemational Standard also operate in accordance with ISO 9001:2000. 

Testing Cert #2052.01 

Page 1 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Former Sludge Incorporation Area - November 2010 

This page has been reserved for specific country requirements. 

Page2of104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Former Sludge Incorporation Area - November 2010 

GLP COMPLIANCE STATEMENT 

Report Title: Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Ground Water Samples 

Collected at the Fonner Sludge Incorporation Area (FSIA) at Decatur, AL in November 2010 

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 detennined under GLPs. 

t^(( 

Gary Hol/enstein, Sponsor Representative Date 

Jaisimhaf^esari, P.E., DEE, Study Director Date 

Page 3 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

QUALITY ASSURANCE STATEMENT 

Report Title: Interim Report 11 Analysis of PFBS, PFHS, and PFOS in Ground Water Samples 

Collected at the Former Sludge Incorporation Area (FSIA) at Decatur, AL in November 2010 

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 

3/24/11-3/25/11 

Phase 

Data / Report 

Date Reported to 

Testing Facility 

Management 

4/25/11 

Study Director 

4/25/11 

^-/O' u 

QAU Representative Date 

Page 4 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Former Sludge Incorporation Area - November 2010 

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 Tests Control Substances 11 

5 Reference Substances 12 

6 Test System 13 

7 Method Summary 13 

7.1 Methods 13 

7.2 Sample Collection 13 

7.3 Sample Preparation 13 

7.4 Analysis 14 

8 Analytical Results 15 

8.1 Calibration 15 

8.2 System Suitability 15 

8.3 Limit of Quantitation (LOQ) 15 

8.4 Continuing Calibration 16 

8.5 Blanks 16 

8.6 Lab Control Spikes (LCSs) 16 

8.7 Analytical Method Uncertainty 21 

8.9 Field Matrix Spikes (FMS) 22 

Page 5 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

9 Data Summary and Discussion 23 

10 Conclusion 43 

11 Data/Sample Retention 43 

12 /attachments 43 

13 Signatures 44 

LIST OF TABLES 

Table 1. Summarized PFBS, PFHS, and PFOS Results (FSIA Groundwater, November 2010). .10 

Table 2. Sample Description Key Code 13 

Table 3. Instalment Parameters 14 

Table 4. Liquid Chromatography Conditions 14 

Table 5. Mass Transitions 15 

Table 6. Limit of Quantitation (LOQ) 16 

Table 7. Laboratory Control Spike Recovery 18 

Table 8. Analytical Uncertainty 22 

Table 9. Field Matrix Spike Levels 22 

Table 10. DAL GW130R 101105 24 

Table 11. DAL GW130L 101105 24 

Table 12. DAL GW130S 101105 25 

Table 13. DAL GW131R 101103 25 

Table 14. DAL GW131L 101103 26 

Table 15. DAL GW131S 101103 26 

Table 16. DAL GW132R 101102 27 

Table 17. DALGW132L101103 27 

Table 18. DAL GW132S 101102 28 

Table 19. DAL GW 133R 101102 28 

Table 20. DAL GW133L 101103 29 

Page 6 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 21. DAL GW133S 101103 29 

Table 22. DAL GW134R 101105 30 

Table 23. DALGW134L 101105 30 

Table 24. DAL GW134S 101105 31 

Table 25. DAL GW 135R 101105 31 

Table 26. DAL GW135L 101105 32 

Table 27. DAL GW135S 101105 33 

Table 28. DAL GW136L 101103 33 

Table 29. DAL GW136S 101103 34 

Table 30. DAL GW 137L 101109 34 

Table 31. DAL GW137S 101109 35 

Table 32. DAL GW138S 101110 36 

Table 33. DAL GW138L 101110 36 

Table33. DALGWCW26R 101110 37 

Table34. DALGWCW26L 101110 37 

Table35. DALGW 140R 101104 38 

Table36. DALGW 141R 101110 38 

Table37. DALGW 142R 101110 39 

Table38. DALGW 144R 101110 39 

Table 39. Trip Blank 40 

Table 40. Trip Blank 2 40 

Table 41. Trip Blank 3 41 

Table42. TripBlank4 41 

Table 43. Rinseate Blanks 42 

Table 44. GLP10-01-02-12 Soil Equipment Rinseate Blank 42 

Page 7 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Former Sludge Incorporation Area - November 2010 

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 

Maplewood, MN 55106 

Study Personnel 

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

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

Susan Wolf, 3M Analyst 

Chelsie Grochow, Analyst 

Study Dates 

Study Initiation: March 8,2010 

Interim 11 Experimental Termination: February 11,2011 

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 104 
GLP10-01-02: Interim Report 11 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Former Sludge Incorporation Area - November 2010 

\2--'fsWmi^ary.: " 1 1 •Ml,; 

The 3M Environmental Laboratory received ground water samples from wells located at the Fonner 

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

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

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

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

included at least two fleld matrix spike (FMS) samples for each location, four trip blank sets containing 

Milli-QTM water and appropriate trip blank spikes, and two equipment rinseate blanks. In addition, one 

soil equipment rinseate blank from GLP10-01-02-12 was analyzed. The equipment rinseate blanks did 

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

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

02-11 were received from Weston personnel on November 18, 2010. The soil equipment rinseate 

blank associated with GLP10-01-02-12 was received from Weston personnel on October 15,2010. All 

of the samples were prepared and analyzed for PFBS, PFHS, and PFOS following 3M Environmental 

Laboratory Method ETS-8-044.0 and conducted under 3M project GLP-10-01-02-011. Many of the 

ground water samples required dilution to attain PFBS, PFHS, and/or POPS concentrations within the 

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

PFBS, PFHS, and PFOS concentrations are summarized in Table 1. The equipment rinseate and the 

trip blank samples 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 ground water samples ranged from 0.0431 ng/mL to 81.2 

ng/mL. The PFHS concentration results for all ground water samples ranged from 0.0914 ng/mL to 

839 ng/mL. The PFOS concentration results for all ground water samples ranged from 0.315 ng/mL to 

1510 ng/mL. The analytical method uncertainties associated with the reported results are: PFBS + 

20%, PFHS + 22% and PFOS + 33%. For some samples, the method uncertainty was expanded for 

PFHS or PFOS. 

Page 9 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 1. Summarized PFBS, PFHS, and PFOS Results (FSIA Groundwater, November 2010). 

Sampling Location 

pALGW130R101105 

pALGW130S101105 

pALGW130L101105 

DAL GW131R 101103 

DAL GW131S 101103 

DAL GW131L 101103 

DAL GW132R 101102 

DALGW 1328 101102 

DALGW132L101103 

DAL GW133R 101102 

DALGW 1338 101103 

DALGW133L101103 

DAL GW134R 101105 

DALGW1348101105 

DALGW134L101105 

DAL GW135R 101105 

DALGW135S101105 

DALGW135L101105 

DALGW 1368 101103 

DALGW136L101103 

DALGW 1378 101109 

DAL GW137L 101109 

DALGW 1388 101110 

DALGW138L101110 

DAL GWCW26R 101110 

DAL GWCW26L 101110 

DAL GW140R 101104 

DAL GW141R 101110 

DAL GW142R 101110 

DAL GW144R 101110 

Trip Blanks (Milli-QTM Water) 

GLP10-01-02-11 Equipment rinseate blanks 

GLP10-01-02-12 Soil Equipment rinseate blank 

PFBS 

Avg. Cone. 

(ng/mL) ± RPD 

16.6 ±6.6% 

3.50 ±11% 

1.77 ±40% 

81.2 ±4.2% 

0.785 ± 3.2% 

3.35 ±4.5% 

8.03 ± 3.5% 

25.9 ± 2.3% 

8.89 ± 3.8% 

4.61 ± 7.6% 

14.0 ±0.0% 

7.65 ±1.7% 

56.2 ±13% 

0.143 ±42% 

11.9 ±3.4% 

81.0 ±2.7% 

0.799 ±1.1% 

5.73 ± 3.8% 

2.55 ± 2.0% 

2,53 ±7,9% 

0,102 ±4.9% 

0,0823 ± 2,6% 

4,69 ± 2,3% 

0.0473 ± 5,3% 

8.27 ±3,1% 

12,9 ±5,4% 

1,63 ±2.5% 

0.0431 ± 6,0% 

1.68 ±1.2% 

1.95 ±3.6% 

<0.0250 

<0,0250 

<0,0250 

PFHS 

Avg. Cone. 

(ng/mL) ± RPD 

128 ±0.0% 

31.3 ±0.32% 

14,4 ± 3.5% 

413 ±0,73% 

4,63 ±6,3% 

20,7 ± 4,8% 

52.8 ± 5.9% 

205 ±1,5% 

77,2 ±1,2% 

31.1 ±6.4% 

91.5 ±1.1% 

53.4 ± 2.4% 

503 ± 9,4% 

1.71 ±6,5%'^' 

112 ±0.0% 

839 ±1,9% 

6.25 ± 3.2% 

35.9 ± 2.5% 

16.5 ±5,5% 

16,2 ±8,0% 

0.0914 ±6.1% 

0.199 ±3.4% 

23.5 ±4.7% 

0.144 ±0.70% 

63,1 ±4.3% 

92,9 ± 5.8% 

17,2 ±0,0% 

0.258 ±12% 

9,98 ± 0.40% 

8,57 ±5.1% 

<0.0250 

<0.0250 

<0.0250 

PFOS 

Avg. Cone. 

(ng/mL) ± RPD 

583 ± 2,4% 

117 ±3,4% 

82.7 ± 5.9% 

1510 ±2.6% 

5.55 ± 5.6% 

34,3 ± 5,0% 

295 ±1.7% 

633 ±12% 

293 ± 5.5% 

60.8 ±6,1% 

224 ± 3,6% 

204 ±1,5% 

1420 ±15% 

11.4 ±1.8% 

579 ± 2.6% 

892 ± 2,6% 

4.88 ± 5.3% 

22,6 ±12% 

87.1 ±3.7% 

79.2 ± 8.8% 

0,315 ±33%*^'^' 

0.893 ± 3,6% 

245 ± 5,7% 

0.581 ±0.17% 

451 ± 2.0% 

848 ± 9.4% 

136 ±6.6% 

4.23 ±12% 

108 ±6.5% 

NR<^' 

<0,250 

<0.250 

<0.250 

The analytical method uncertainties associated with the reported results are: PFBS ± 20%, PFHS ± 22%, and PFOS ± 33%. 

(1) The analytical uncertainty has been adjusted for PFHS based on FMS recovery for: DAL GW 134S to ± 35%. 

(2) The analytical uncertainty has been adjusted for PFOS based on FMS recovery for DAL GW 137S to ± 41 %. See discussion 

in section 9 of the report. 

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

(4) NR = Not Reported; Matrix spike recovery was <50%, See section 9 of the report for additional Infomnatlon, 

Page 10 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Former Sludge Incorporation Area - November 2010 

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 

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

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

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

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

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

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

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

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

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

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

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

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

The aqueous equipment rinseate samples were collected in plain bottles without mari<ings or 

fortifications. 

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

Laboratory method ETS-8-044.0 "Detemnination of Perfiuorinated 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, the trip blanks, aqueous equipment rinseate blanks, and aqueous soil-equipment rinseate 

blank samples. Tables 10-44 summarize the individual sample results and the associated field matrix 

spike recoveries. All results for the quality control samples prepared and analyzed with the samples 

are reported and discussed elsewhere in this report 

4 Tiesf & 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 104 
5 Reference Substances 

GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Former Sludge Incorporation Area - November 2010 

Reference Substance 

Chemical Name 

Chemical Fonnula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFBS 

(piredominantly 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 

LPFHX8AM08 

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 

CgFiySOa 

Potassium Salt 

CAS # 2795-39-3 

Wellington 

10/18/2013 

Frozen 

LPFOSKBM06 

TCR08-0001 

Crystalline 

98% 

PFOS 

(linear + branched) 

Perfluorooctane sulfonate 

CsFiySOs' 

Potassium Salt 

CAS # 2795-39-3 

3M 

12/14/2016 

Frozen 

171 

TCR-696 

White Powder 

86.4% 

Page 12 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

6 Test System 

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 worid" samples, not dosed with a 

specific lot of test substance. 

Table 2. Sample Description Key Code. 

String Number 

Example 

1 

2 

3 

4 

5 

String Descriptor 

DAL GW135LDB 101105 

Sampling Location 

Sample Type 

Sampling Point 

Well Level 

Sampling Date 

Sample Type 

Example 

DAL = Decatur, AL 

GW= Groundwater 

Example: 135 

R = Residum shallow water-bearing zone 

L = Bedrock water-bearing zone 

S = Epikarst middle water-bearing zone 

101105 = November 5, 2011 

0=primary sample 

DB=duplicate sample 

LS = low spike 

MS = mid spike 

HS = high spike 

7 Method Summar y 

7.1 Methods 

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

"Detemriination of Perfiuorinated Compounds In Water by High Perfonnance 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 associated with GLP10-01-02-11 were returned to the 

laboratory at ambient conditions on November 18, 2010. The equipment rinseate blank associated with 

GLP10-01 -02-12 was returned to the laboratory at ambient conditions on October 15,2010. 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 each cooler of sample collection bottles. 

7.3 Sample Preparation 

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

analysis. 

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

(dilution 1:10). Most sampling locations were diluted 1:100 by further diluting the 1:10 dilution with 

additional Milli Q water. 

Page 13 of 104 
GLP10-01-02: Interim Report 11 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Former Sludge Incorporation Area - November 2010 

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. 

All samples were inifially prepared on 12/30/10. Due to the large number of samples requiring analysis, 

along with network communication en'ors that were experienced during the analysis, the samples were 

broken up into three analytical runs. The LCS samples prepared with the samples on 12/30/10 were reanalyzed with each analytical batch analyzed on ETS Buster from 1/7/11 -1/4/11. 

Table 3. Instrument Parameters. 

Instrument Name 

Analytical Method Followed 

Analysis Date 

Liquid Chromatograph 

Guard column 

Analytical column 

Injection Volume 

Mass Spectrometer 

ion Source 

Electrode 

Polarity 

Software 

ETS Buster 

ETS-8-044,0 

1/7/11,1/10/11, and 1/14/11 -PFBS, 

PFHS, and PFOS 

Agilent 1100 

Prism RP (2,1 mm X 50 mm), 5 n 

Betasil C18 (2,1 mm X 100 mm), 5u 

2or10nL 

Applied Blosystems AP\ 4000 

Turtjo Spray 

Turtjo ion electrode 

Negative 

/Analyst 1.4,2 

ETS Ginger 

ETS-8-044.0 

2/11/11-PFBSand PFOS 

Agilent 1100 

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

Betasil CIS (2.1 rrirn X 100 mm), 5n 

5or10^L 

Applied Blosystems API 5000 

Turt)0 Spray 

Turbo Ion electrode 

Negative 

Analyst 1.4.2 

Table 4. Liquid Chromatography Conditions. 

step 

Number 

0 

1 

2 

3 

4 

5 

Total Time 

(min) 

0 

2.0 

14.5 

15.5 

16.5 

20.0 

Flow Rate 

(fdJmin) 

Percent A 

(2 mM ammonium acetate) 

ETS-8-044.0 Analyzed on ETS Buster 

300 

300 

300 

300 

300 

300 

97.0 

97.0 

5,0 

5,0 

97.0 

97.0 

PercentB 

(MethanoO 

3.0 

3.0 

95,0 

95.0 

3.0 

3.0 

ETS-8-044.0 Analyzed on ETS Ginger 

0 

1 

2 

3 

4 

5 

0 

2.0 

11.0 

14.5 

14,5 

17,0 

300 

300 

300 

300 

300 

300 

97.0 

97.0 

5,0 

5,0 

97.0 

97,0 

3.0 

3.0 

95,0 

95,0 

3.0 

3.0 

Page 14 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 5. Mass Transitions. 

Analyte 

PFBS 

PFHS 

PFOS 

Mass Transition 

Q1/Q3 

299/80 

299/99 

399m 

399/99 

499/80 

499/99 

499/130 

Reference Material 

Structure 

Linear 

Linear 

Linear 

Dwell time was 50 msec for each transition. The individual transitions 

were summed to produce a "total ion chromatogram" (TIC), which was 

used for quantitation. 

8 Analytical Results 

8.1 Calibration 

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

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

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

analyzed. Low or high curve points may have been disabled to meet method 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 forced through zero during the fitting process. Calculating the standard concentrations using 

the peak area confinned accuracy of each curve point. 

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

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

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

8.2 System Suitability 

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

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

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

met for PFBS, PFHS, and PFOS. 

8.3 Limit of Quantitation (LOQ) 

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

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

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

Page 15 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 6. Limit of Quantitation (LOQ). 

Analysis Date 

1/7/11 and 1/10/11 

Analysis 

1/14/11 Analysis 

2/11/11 Analysis 

2/28/11 Analysis 

Dilution 

1 

5 

10 

100 

50 

100 

1 

10 

100 

10 

PFBS 

LOQ, ng/mL 

0,0250 

0.125 

0,250 

2,50 

1.25 

2.50 

0,0250 

0,250 

2,50 

NA 

PFHS 

LOQ, ng/mL 

0.0250 

0.125 

0.250 

2.50 

1.25 

2.50 

0.0250 

0.250 

2,50 

NA 

PFOS 

LOQ, ng/mL 

0.250 

1.25 

2.50 

25.0 

12.5 

25.0 

0,0300 

0.300 

3,00 

0.250 

NA = Not Applicable 

8.4 Continuing Calibration 

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

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

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

8.5 Blanks 

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

Method blank results were reviewed and used to evaluate method peri'onnance and to determine the 

LOQ for each analyte 

8.6 Lab Control Spikes (LCSs) 

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

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

produce the desired concentration. The spiked water samples were then prepared and analyzed in the 

same manner as the samples. The method acceptance criteria, average of LCS at each level should be 

within 100% ± 20% with an RSD 520%AII samples were initially prepared on 12/30/10. Due to the 

large number of samples requiring analysis, along with networi< communication errors that were 

experienced during the analysis, the samples were broken up into three analytical runs. The LCS 

samples prepared with the samples on 12/30/10 were re-analyzed with each analytical batch analyzed 

on ETS Buster fi-om 1/7/11 -1/4/11. 

1/7/11 Analysis: Due to an autosampler error, the third replicate of the low set of LCS samples did not 

inject. The average recovery for the low set of LCS for PFBS was 122% and for PFHS 123%. All other 

LCS analyzed in this run met method acceptance criteria. 

1/10/11 Analysis: The low set of LCS samples for PFHS had an average recovery of 122%. All other 

LCS analyzed in this run met method acceptacne criteria. 

1/14/11 Analysis: All three sets of LCS method acceptance criteria for PFBS, PFHS, and PFOS. 

2/11/11 Analysis: All three sets of LCS method acceptance criteria for PFBS, PFHS, and PFOS. 

As the reference material 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 

Page 16 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

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

for analytical bias. 

1/7/11 Analysis: The low and mid sets of linear and branched PFOS LCS met method acceptance 

criteria, while the average recovery of the high set of LCS samples was 123%. 

1/10/11 Analysis: The low and mid sets of linear and branched PFOS LCS met method acceptance 

criteria while the high set had an average recovery of 121%. 

1/14/11 Analysis: All three sets of linear and branched PFOS LCS met method acceptance criteria. 

2/11/11 Analysis: The low and mid sets of linear and branched PFOS LCS met method acceptance 

criteria while the high set had an average recovery of 133%. 

The recovery of the high sets of linear and branched PFOS suggest possible analytical bias when 

samples containting both linear and branched isomers of PFOS are quantitated against a calibration 

curve constnjcted of primarily linear PFOS. Therefore, the analytical method uncertainty for this study 

has been adjusted based on the highest average recovery of the linear and branched PFOS LCS 

samples to ± 33%. 

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

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

LCS Percent Recovery = * 100% 

Spike Concentration 

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

average LCS recovery 

Page 17 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 7. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Analyzed 1/7/11 

Lab ID 

LCS-101230-1 

LCS-101230-2 

LCS-101230-3 

Average ±%RSD 

LCS-101230-4 

LCS-101230-5 

LC8-101230-6 

Average ±%RSD 

LC8-101230-7 

LC8-101230-8 

LC8-101230-9 

Average ±%RSD 

PFBS 

Spiked 

Concentration 

(ng/mL) 

0.497 

0.497 

NA'^' 

Calculated 

Concentration 

(ng/mL) 

0.631 

0.580 

NA<^> 

'/oRecovery 

127 

117 

NA<=^' 

122±5.8%<^' 

4.97 

4.97 

4.97 

6,01 

5,86 

5,87 

121 

118 

118 

119% ±1.5 % 

29.9 

29.9 

29.9 

30,6 

29,8 

29,9 

102 

99,6 

100 

101 % ±1.3 % 

PFHS 

Spiked 

Concentration 

(ng/mL) 

0.498 

0,498 

NA<=' 

Calculated 

Concentration 

(ng/mL) 

0,631 

0,595 

NA<^' 

%Recovery 

127 

119 

NA'^' 

123% ±4.6%'^ ' 

4.98 

4.98 

4.98 

5.94 

5.83 

5.86 

119 

117 

118 

118% ±0.85 % 

29.9 

29.9 

29.9 

30.7 

29.6 

30.5 

103 

99,0 

102 

101 % ±2.1 % 

ETS-8-044.0 

Analyzed 1/7/11 

L ab ID 

LCS-101230-1 

LC8-101230-2 

LC8-101230-3 

Average ± %RSD 

LCS-101230-4 

LCS-101230-5 

LCS-101230-6 

Average ± %RSD 

LC8-101230-7 

LCS-101230-8 

LC8-101230-9 

Average ± %RSD 

PFOS (linear) 

Spike d 

Concentration 

(ng/mL) 

0.497 

0.497 

NA<2' 

Calculated 

Concentration 

(ng/mL) 

0,524 

0,507 

NA<^* 

%Recovery 

105 

102 

NA<^' 

104% ±2.0 % 

4.97 

4,97 

4,97 

5.81 

5.78 

5.81 

117 

116 

117 

117% ±0.49 % 

29,9 

29.9 

29,9 

31.2 

31.7 

31,3 

104 

106 

105 

105% ±1.0 % 

Lab ID 

LCS-101230-10 

LCS-101230-11 

LCS-101230-12 

Average ± %RSD 

LCS-101230-13 

LCS-101230-14 

LCS-101230-15 

Average ±%RSD 

LC8-101230-16 

LCS-101230-17 

LCS-101230-18 

Average ±%RSD 

PFOS (linear + branched) 

Spiked 

Concentration 

(ng/mL) 

0,492 

0,492 

NA'^' 

Calculated 

Concentration 

(ng/mL) 

0,539 

0,498 

NA<^' 

XRecovery 

110 

101 

NA<=' 

106% ±6.0 % 

4,93 

4,93 

4,93 

6.10 

5.87 

5,77 

124 

119 

117 

120% ±3.0 % 

29.6 

29.6 

29.6 

36,4 

35,7 

37,3 

123 

121 

126 

123% ±2.0%'^' 

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

(2) NA = Not applicable: LCS was not injected due to an autosampler error. 

Page 18 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 7 continued. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Analyzed 1/10/11 

Lab ID 

LC8-101230-1 

LCS-101230-2 

LCS-101230-3 

Average ± %RSD 

LCS-101230-4 

LC8-101230-5 

LC8-101230-6 

Average ± %RSD 

LCS-101230-7 

LCS-101230-8 

LC8-101230-9 

Average ±%RSD 

PFBS 

Spiked 

Concentration 

(ng/mL) 

0.497 

0.497 

0,497 

Calculated 

Concentration 

(ng/mL) 

0.620 

0.578 

0.578 

VoRecovery 

125 

116 

116 

119 ±4.4% 

4,97 

4,97 

4,97 

5.93 

5.77 

5.72 

119 

116 

115 

117% ±1.8% 

29,9 

29.9 

29.9 

30.4 

29,3 

29,2 

102 

98,0 

97,8 

99.3% ±2.4% 

PFHS 

Spiked 

Concentration 

(ng/mL) 

0,498 

0.498 

0.498 

Calculated 

Concentration 

(ng/mL) 

0.627 

0,586 

0,602 

VoRecovery 

126 

118 

121 

122% ±3.3%'^' 

4,98 

4,98 

4,98 

6,15 

5,97 

5.86 

123 

120 

118 

120% ±2.1% 

29,9 

29.9 

29.9 

30.8 

30.1 

29.8 

103 

101 

99,6 

101% ±1.7% 

ETS-8-044,0 

Analyzed 1/10/11 

Lab ID 

LCS-101230-1 

LCS-101230-2 

LC8-101230-3 

Average ± %RSD 

LCS-101230-4 

LCS-101230-5 

LCS-101230-6 

Average ± %RSD 

LCS-101230-7 

LCS-101230-8 

LC8-101230-9 

Average ± %RSD 

PFOS (linear) 

Spiked 

Concentration 

(ng/mL) 

0.497 

0.497 

0.497 

Calculated 

Concentration 

(ng/mL) 

0.536 

0.532 

0,512 

'/oRecovery 

108 

107 

103 

106% ±2.5% 

4.97 

4,97 

4,97 

5.92 

5.84 

5.87 

119 

118 

118 

118% ±0.49% 

29.9 

29.9 

29.9 

30.6 

30.7 

30.3 

102 

103 

101 

102% ±0.98% 

Lab ID 

LCS-101230-10 

LC8-101230-11 

LCS-101230-12 

Average ± %RSD 

LCS-101230-13 

LC8-101230-14 

LCS-101230-15 

Average ± %RSD 

LCS-101230-16 

LC8-101230-17 

LC8-101230-18 

Average ± %RSD 

PFOS (linear + branched) 

Spiked 

Concentration 

(ng/mL) 

0,492 

0,492 

0,492 

Calculated 

Concentration 

(ng/mL) 

0.559 

0.509 

0.551 

VoRecovery 

114 

103 

112 

110% ±5.3% 

4.93 

4.93 

4.93 

5.97 

5.69 

5,65 

121 

115 

115 

117% ±3.0% 

29,6 

29,6 

29.6 

35,2 

36,0 

35.9 

119 

122 

121 

121% ±1.3%'^' 

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

(2) NA = Not applicable; LCS was not Injected due to an autosampler error. 

Page 19 of 104 
GLP10-01-02: Interim Report 11 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 7 continued. Laboratory Control Spike Recovery. 

ETS-8-044,0 

Analyzed 1/14/11 

Lab ID 

LC8-101230-1 

LCS-101230-2 

LC8-101230-3 

Average ± %RSD 

LC8-101230-4 

LC8-101230-5 

LCS-101230-6 

Average ±%RSD 

LCS-101230-7 

LC8-101230-8 

LCS-101230-9 

Average ±%RSD 

PFBS 

Spiked 

Concentration 

(ng/mL) 

0.497 

0,497 

0,497 

Calculated 

Concentration 

(ng/mL) 

0.612 

0,589 

0,590 

VoRecovery 

123 

119 

119 

120 ±1.9% 

4.97 

4.97 

4.97 

5.99 

5,73 

5,78 

121 

115 

116 

117% ±2.7% 

29.9 

29.9 

29.9 

30,4 

30,1 

29,9 

102 

101 

99,9 

101% ±1.0% 

PFHS 

Spiked 

Concentration 

(ng/mL) 

0,498 

0,498 

0,498 

Calculated 

Concentration 

(ng/mL) 

0.602 

0,589 

0,589 

VoRecovery 

121 

118 

118 

119% ±1.5% 

4.98 

4.98 

4.98 

6,03 

5,82 

5,81 

121 

117 

117 

118% ±2.0% 

29.9 

29.9 

29.9 

31,0 

30,5 

30.5 

104 

102 

102 

103% ±1.1% 

ETS-8-044.0 

Analyzed 1/14/11 

Lab ID 

LCS-101230-1 

LCS-101230-2 

LCS-101230-3 

Average ± %RSD 

LCS-101230-4 

LC8-101230-5 

LC8-101230-6 

Average ± %RSD 

LC8-101230-7 

LCS-101230-8 

LCS-101230-9 

Average ± %RSD 

PFOS (linear) 

Spiked 

Concentration 

(ng/mL) 

0,497 

0,497 

0.497 

Calculated 

Concentration 

(ng/mL) 

0.523 

0.517 

0.504 

VoRecovery 

105 

104 

101 

103% ±2.0% 

4.97 

4.97 

4.97 

5.87 

5.66 

5.72 

118 

114 

115 

116% ±1.8% 

29.9 

29.9 

29.9 

31,2 

31,6 

30,7 

104 

106 

103 

104% ±1.5% 

Lab ID 

LCS-101230-10 

LCS-101230-11 

LC8-101230-12 

Average ± %RSD 

LC8-101230-13 

LCS-101230-14 

LCS-101230-15 

Average ± %RSD 

LCS-101230-16 

LCS-101230-17 

LCS-101230-18 

Average ± %RSD 

PFOS (linear + branched) 

Spiked 

Concentration 

(ng/mL) 

0.492 

0.492 

0.492 

Calculated 

Concentration 

(ng/mL) 

0.522 

0,472 

0,527 

VoRecovery 

106 

96,0 

107 

103% ±5.9% 

4.93 

4,93 

4,93 

6.03 

5,69 

5.65 

122 

115 

115 

117% ±3.4% 

29,6 

29.6 

29.6 

34.6 

36.0 

36.1 

117 

122 

122 

120% ±2.4% 

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

(2) NA = Not applicable; LCS was not injected due to an autosampler error. 

Page 20 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 7 continued. Laboratory Control Spike Recovery. 

ETS-8-044,0 

Analyzed 2/11/11 

Lab ID 

LCS-110210-1 

LCS-110210-2 

LCS-110210-3 

Average ±%RSD 

LCS-110210-4 

LC8-110210-5 

LCS-110210-6 

Average ±%RSD 

LCS-110210-7 

LCS-110210-8 

LCS-110210-9 

Average ± %RSD 

PFBS 

Spiked 

Concentration 

(ng/mL) 

0,498 

0,498 

0,498 

Calculated 

Concentration 

(ng/mL) 

0,563 

0,542 

0,581 

VoRecovery 

113 

109 

117 

113 ±3.5% 

4,98 

4,98 

4,98 

5,37 

5,52 

5.58 

108 

111 

112 

110% ±1.9% 

29,9 

29,9 

29,9 

29,8 

31,1 

32,0 

100 

104 

107 

104% ±3.6% 

PFHS 

Spiked 

Concentration 

(ng/mL) 

0,498 

0,498 

0,498 

Calculated 

Concentration 

(ng/mL) 

0,603 

0,594 

0.599 

VoRecovery 

121 

119 

120 

120% ±0.83% 

4,98 

4,98 

4,98 

5.61 

5,36 

5,96 

113 

108 

120 

114% ±5.3% 

29,9 

29,9 

29,9 

30.7 

30,8 

32.7 

103 

103 

109 

105% ±3.3% 

ETS-8-044,0 

Analyzed 2/11/11 

Lab ID 

LCS-110210-1 

LC8-110210-2 

LCS-110210-3 

Average ± %RSD 

LCS-110210-4 

LC8-110210-5 

LC8-110210-6 

Average ±%RSD 

LC8-110210-7 

LCS-110210-8 

LCS-110210-9 

Average ±%RSD 

PFOS (linear) 

Spiked 

Concentration 

(ng/mL) 

0,498 

0.498 

0.498 

Calculated 

Concentration 

(ng/mL) 

0,650 

0,587 

0,540 

VoRecovery 

130 

118 

108 

119% ±9.3% 

4.98 

4.98 

4,98 

5,43 

4.93 

5,86 

109 

99,1 

118 

109% ±8.7% 

29,9 

29,9 

29,9 

30,8 

30.7 

32.4 

103 

103 

108 

105% ±2.8% 

Lab ID 

LCS-110210-10 

LC8-110210-11 

LC8-110210-12 

Average ±%RSD 

LCS-110210-13 

LCS-110210-14 

LCS-110210-15 

Average ±%RSD 

LCS-110210-16 

LCS-110210-17 

LC8-110210-18 

Average ± %RSD 

PFOS (linear + branched) 

Spiked 

Concentration 

(ng/mL) 

0.502 

0.502 

0.502 

Calculated 

Concentration 

(ng/mL) 

0,539 

0,585 

0,541 

VoRecovery 

107 

117 

108 

111% ±5.0% 

5.04 

5.04 

5,04 

6,15 

5,38 

5,44 

122 

107 

108 

112% ±7.5% 

30,2 

30,2 

30.2 

40.7 

40.4 

39.6 

135 

134 

131 

133% ± 1.6% <^' 

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

(2) NA = Not applicable; LCS was not injected due to an autosampler error. 

Page 21 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

8.7 Analytical Method Uncertainty 

Analytical uncertainty is based on historical QC data that is control charted and used to evaluate 

method accuracy and precision. The method uncertainty is calculated following ETS-12-012.2. The 

standard deviation is calculated for the set of accuracy results (in %) obtained for the QC samples. The 

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

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

method uncertainty values listed in Table 8. The analytical method uncertainty for PFOS when 

calculated following the above described procedure was found to be ± ^8%. However, due to potential 

analytical bias that was observed when quantitating LCS samples containing linear and branched 

isomers of PFOS, the analytical for PFOS has been expanded to ± 33%. 

Table 8. Analytical Uncertainty. 

Analyte 

PFBS 

PFHS 

PFOS 

Standard Deviation 

10.9 

11.0 

9.07 

Method Uncertainty 

±20% 

±22% 

±33%'" 

(1) See section 8.6 of the report for a discussion of the assigning of the analytical method uncertainty for PFOS, 

8.8 Field Matrix Spikes (FMS) 

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

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

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

by the laboratory with PFBS (linear), PFHS (linear), and PFOS (linear) prior to shipping sample 

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

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

extraction and analysis of the analytes of interest. Field matrix spike concentrations must be 50%) of the 

sample concentration to be considered an appropriate field spike. Field matrix spikes are presented in 

section 9 of this report. 

Table 9. Field IVIatrix Spike Levels. 

Sampling Location 

136R, 137R, 137s, 137L, 138L 

130L, 131L, 132L, 133R, 134S, 134L, 

136S 

130R, 130S, 131S, 132R, 132S, 133S, 

133L, 135S, 135L , 136L, 138S , 138R 

131R, 134R, 135R 

Trip Blank 

Spike Level 

Low 

Mid 

High 

Low 

Mid 

High 

Low 

Mid 

High 

Low 

High 

Low 

Mid 

Mid-High 

High 

PFBS, ng/mL 

0.0972 

0.972 

9.72 

0.972 

9,72 

97,2 

9,72 

97,2 

972 

97.2 

972 

0.972 

9.72 

97.2 

972 

PFHS, ng/mL 

0.0961 

0,961 

9,61 

0,961 

9,61 

96,1 

9.61 

96.1 

961 

96,1 

961 

0,961 

9,61 

96.1 

961 

PFOS, ng/mL 

0.0978 

0.978 

9.78 

0,978 

9,78 

97,8 

9,78 

97.8 

978 

97.8 

978 

0,978 

9,78 

97.8 

978 

Page 22 of 104 
GLP10-01-02: Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

(Sample Concentration of FMS - Average Concentration: Field Sample & Field Sample Dup.) ^, „„„, FMS Recovery = -^^ :- ^-^* 100% Spike Concentraton 

8.9 Laboratory Matrix Spikes (LMS) 

The mid FMS sample for DAL GW 144R analyzed on 1/10/11 did not meet method acceptance criteria 

for PFOS with a recovery of 28.7%). The high FMS sample analyzed on 1/10/11 exceeded the 

instrument calibration range. Further dilution of the high FMS sample was not performed since the high 

FMS sample (spike level 978 ng/mL) was not appropriate as compared to the observed sample 

concentration. The sample set was reanalyzed on 2/28/11 along with a 50 ng/mL laboratory matrix 

spike. Laboratory matrix spike recoveries within method acceptance criteria of 100±30% confinn that 

"unknown" components in the sample matrix do not significantly interfere with the extraction and analysis 

of the analytes of interest. See section 9 for a discussion of the PFOS results. 

9 Data Summary and Discussion 

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

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

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

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

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

quantitative ranges. 

DAL GW 134S - The recovery of the low FMS sample for PFHS was 135%). The mid and high FMS 

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

compared to the sample concentration, the analytical uncertainty has been adjusted for PFHS to 100% 

± 35%. 

DAL GW 137S - The recovery of the mid FMS sample for PFOS was 58.8%), while the recovery of the 

high FMS was 59.4%i. Since the mid spike was the most appropriate spike level as compared to the 

sample concentration, the analytical uncertainty has been adjusted for PFOS to 100%) ± 41%. 

DAL GW144R-The sample set was diluted 1:10 and analyzed on 1/10/11. The recovery of the mid 

FMS sample for PFOS was 28.7%). The high FMS sample exceeded the instrument calibration range. 

Further dilution of the high FMS sample was not performed since the high FMS sample (spike level 978 

ng/mL) was not appropriate as compared to the sample concentration. The sample set was re-diluted 

and analyzed on 2/28/11 along with a 49.8 ng/mL laboratory matrix spike. The recovery of the mid 

FMS sample was 33.4%), and the recovery of the LMS sample was 294%. Since the recovery of both 

matrix spike samples was <50%), no PFOS results will be reported for DAL GW 144R. 

Page 23 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 10. DAL GW 130R 101105 

3M LIMS ID 

GLP10-01-02-11-001 

GLP10-01-02-11-002 

GLP10-01-02-11-003 

GLP10-01-02-11-004 

GLP10-01-02-11-005 

Average Concent 

Description 

DAL GW130R 0 101105 

DALGW130RDB101105 

DAL GW130RLS 101105 

DAL GW130R MS 101105 

DAL GW130RHS 101105 

ration (ng/mL) + VoRPD 

PFBS 

Concentration 

(ng/mL) 

16.0 

17.1 

28.0 

122 

998 

VoRecovery 

NA 

NA 

118 

108 

101 

16.6 ng/mL ±6.6% 

PFHS 

Concentration 

(ng/mL) 

128 

128 

140 

232 

1120 

VoRecovery 

NA 

NA 

NC 

108 

103 

128 ng/mL ±0.0% 

PFOS 

Concentration 

(ng/mL) 

590 

576 

606 

626 

1490 

VoRecovery 

NA 

NA 

NC 

NC 

92.7 

583 ng/mL ±2.4% 

NA = Not /Applicable 

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

PFBS, PFHS, and PFOS were analyzed on 1/10/11 with a 1:10 dilution. 

Table 11. DAL GW 1 SOL 10il05 

3M LIMS ID 

GLP10-01-02-11-011 

GLP10-01-02-11-012 

GLP10-01-02-11-013 

GLP10-01-02-11-014 

GLP10-01-02-11-015 

Description 

DAL GW130L 0 101105 

DAL GW130LDB 101105 

DALGW130LLS101105 

DAL GW130L MS 101105 

DALGW130LHS101105 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

1.80 

1.73 

2.91 

13.0 

107 

VoRecovery 

NA 

NA 

118 

116 

108 

1.77 ng/mL ±4.0% 

PFHS 

Concentration 

(ng/mL) 

14.1 

14.6 

15.9 

25.3 

119 

%Recovery 

NA 

NA 

NC 

114 

109 

14.4 ng/mL ±3.5% 

PFOS 

Concentration 

(ng/mL) 

85.1 

80.2 

82.1 

84.5 

182 

VoRecovery 

NA 

NA 

NC 

NC 

102 

82.7 ng/mL ±5.9% 

NA = Not Applicable 

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

PFBS, PFHS, and PFOS were analyzed on 1/7/11 with a 1:10 dilution. 

Page 24 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 12. DALGW 1 SOS 101105 

3M LIMS ID 

GLP10-01-02-11-006 

GLP10-01-02-11-007 

GLP10-01-02-11-008 

GLP10-01-02-11-009 

GLP10-01-02-11-010 

Description 

DALGW 1308 0 101105 

DALGW 1308 DB 101105 

DALGW 1308 LS 101105 

DALGW 1308 MS 101105 

DALGW 1308 HS 101105 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

3.30 

3.70 

13.9 

109 

1020 

VoRecovery 

NA 

NA 

107 

109 

105 

3.50 ng/mL ±11% 

PFHS 

Concentration 

(ng/mL) 

31.3 

31.2 

41.8 

134 

1060 

VoRecovery 

NA 

NA 

NC 

107 

107 

31.3 ng/mL ±0.32% 

PFOS 

Concentration 

(ng/mL) 

119 

115 

127 

203 

1070 

VoRecovery 

NA 

NA 

NC 

87.9 

97.4 

117 ng/mL ±3.4% 

NA = Not Applicable 

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

PFBS, PFHS, and PFOS were analyzed on 1/10/11 with a 1:100 dilution. 

Table IS. DALGW 131R 101103 

3M LIMS ID 

GLP10-01-02-11-017 

GLP10-01-02-11-018 

GLP10-01-02-11-019 

GLP10-01-02-11-020 

Description 

DAL GW131R 0 101103 

DALGW131RDB 101103 

DAL GW131RLS 101103 

DAL GW131RHS 101103 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

82.9 

79.5 

184 

1120 

VoRecovery 

NA 

NA 

NC 

107 

81.2 ng/mL ±4.2% 

PFHS 

Concentration 

(ng/mL) 

411 

414 

512 

1440 

VoRecovery 

NA 

NA 

NC 

107 

413 ng/mL ±0.73% 

PFOS 

Concentration 

(ng/mL) 

1490 

1530 

1610 

2700 

VoRecovery 

NA 

NA 

NC 

122 

7570 ng/mL ±Z6% 

NA = Not /Applicable 

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

PFBS, PFHS, and PFOS were analyzed on 1/14/11 with a 1:100 dilution. 

Page 25 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 14. DAL GW 131L10110S 

3M LIMS ID 

GLP10-01-02-11-026 

GLP10-01-02-11-027 

GLP10-01-02-11-028 

GLP 10-01-02-11-029 

GLP10-01-02-11-030 

Description 

DAL GW131L 0 101103 

DALGW131LDB 101103 

DAL GW131LL8 101103 

DAL GW131L MS 101103 

DALGW131LHS 101103 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

3.42 

3.27 

4.57 

14.7 

109 

VoRecovery 

NA 

NA 

NC 

117 

109 

3.35 ng/mL ±4.5% 

PFHS 

Concentration 

(ng/mL) 

20.2 

21.2 

21.6 

32.8 

127 

VoRecovery 

NA 

NA 

NC 

NC 

111 

20.7 ng/mL ±4.8% 

PFOS 

Concentration 

(ng/mL) 

33.4 

35.1 

33.7 

43.0 

128 

VoRecovery 

NA 

NA 

NC 

NC 

95.9 

34.3 ng/mL ±5.0% 

tvIA = Not Applicable 

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

PFBS, PFHS, and PFOS were analyzed on 1/7/11 with a 1:10 dilution. 

Table 15. DALGW ISIS 101103 

3M LIMS ID 

GLP10-01-02-11-021 

GLP10-01-02-11-022 

GLP10-01-02-11-023 

GLP10-01-02-11-024 

GLP 10-01-02-11-025 

Description 

DAL GW131S 0 101103 

DALGW131SDB 101103 

DALGW131SL8 101103 

DALGW1318 MS 101103 

DALGW 1318 HS 101103 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

0.772 

0.797 

1.98 

12.6 

112 

VoRecovery 

NA 

NA 

123 

122 

114 

0.785 ng/mL ±3.2% 

PFHS 

Concentration 

(ng/mL) 

4.77 

4.48 

6.06 

16.3 

112 

VoRecovery 

NA 

NA 

NC 

121 

112 

4.63 ng/mL ±6.3% 

PFOS 

Concentration 

(ng/mL) 

5.39 

5.70 

5.73 

14.5 

101 

VoRecovery 

NA 

NA 

NC 

91.6 

97.6 

5.55 ng/mL ±5.6% 

NA = Not Applicable 

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

PFBS, PFHS, and PFOS were analyzed on 1/7/11 with a 1:10 dilution. 

Page 26 of 104 
GLP10-01-02; Interim Report 11 

/\nalysis of PFBS, PFHS, and PFOS In Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 16. DAL GW 1S2R101102 

3MUMSID 

GLP10-01-02-11-031 

GLP10-01-02-11-032 

GLP10-01-02-11-033 

GLP10-01-02-11-034 

GLP10-01-02-11-035 

Average Concent 

Description 

DAL GW132R 0 101102 

DAL GW132RDB 101102 

DALGW132RL8 101102 

DAL GW132R MS 101102 

DAL GW132RHS 101102 

•ation (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

8.17 

7.89 

19.3 

116 

1060 

VoRecovery 

NA 

NA 

116 

111 

108 

8.03 ng/mL ±3.5% 

PFHS 

Concentration 

(ng/mL) 

54.3 

51.2 

65.4 

161 

1130 

%Recovery 

NA 

NA 

NC 

113 

112 

5Z8 ng/mL ±5.9% 

PFOS 

Concentration 

(ng/mL) 

297 

292 

306 

397 

1270 

VoRecovery 

NA 

NA 

NC 

NC 

99.7 

295 ng/mL ±1.7% 

NA = Not Applicable 

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

PFBS, PFHS, and PFOS were analyzed on 1/14/11 with a 1:100 dilution. 

Table 17. DALGW1S2L101103 

3MUMSID 

GLP10-01-02-11-041 

GLP10-O1-O2-11-042 

GLP10-01-02-11-043 

GLP10-01-02-11-044 

GLP10-01-02-11-045 

Average Concent 

Description 

DAL GW132L 0101103 

DAL GW132LDB 101103 

DAL GW132LL8 101103 

DAL GW132L MS 101103 

DALGW132LHS101103 

'ation (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

9.06 

8.72 

19.5 

114 

1060 

VoRecovery 

NA 

NA 

109 

108 

108 

8.89 ng/mL ±3.8% 

PFHS 

Concentration 

(ng/mL) 

76.7 

77.6 

85.4 

177 

1140 

VoRecovery 

NA 

NA 

NC 

104 

111 

77.2 ng/mL ±1.2% 

PFOS 

Concentration 

(ng/mL) 

285 

301 

367 

489 

1400 

VoRecovery 

NA 

NA 

NC 

NC 

113 

293 ng/mL ±5.5% 

NA= Not Applicable 

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

PFBS, PFHS, and PFOS were analyzed on 1/7/11 with a 1:10 dilution. 

Page 27 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 18. DAL GW132S 101102 

3M LIMS ID 

GLP10-01-02-11-036 

GLP10-01-O2-11-037 

GLP10-01-02-11-038 

GLP10-01-02-11-039 

GLP10-01-02-11-040 

Average Concent 

Description 

DALGW 1328 0101102 

DAL GW 1328 DB 101102 

DALGW 1328 LS 101102 

DALGW 1328 MS 101102 

DAL GW 1328 HS 101102 

ration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

26.2 

25.6 

37.3 

129 

1040 

VoRecovery 

NA 

NA 

NC 

106 

104 

25.9 ng/mL ±2.3% 

PFHS 

Concentration 

(ng/mL) 

203 

206 

209 

300 

1220 

VoRecovery 

NA 

NA 

NC 

NC 

106 

205 ng/mL ±1.5% 

PFOS 

Concentration 

(ng/mL) 

593 

672 

584 

612 

1570 

VoRecovery 

NA 

NA 

NC 

NC 

95.9 

633 ng/mL ±12% 

NA = Not Applicable 

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

PFBS, PFHS, and PFOS were analyzed on 1/14/11 with a 1:100 dilution. 

Table 19. DALGW 133R 101102 

3MUMSID 

GLP10-01-02-11-046 

GLP10-01-02-11-047 

GLP10-01-02-11-048 

GLP10-01-02-11-049 

GLP10-01-02-11-050 

Average Concent 

Description 

DAL GW133R 0101102 

DALGW133RDB101102 

DAL GW133RL8 101102 

DALGW133RMS101102 

DAL GW133RHS 101102 

ration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

4.78 

4.43 

5.35 

15.3 

106 

VoRecovery 

NA 

NA 

NC 

110 

104 

4.67 ng/mL ± 7.6% 

PFHS 

Concentration 

(ng/mL) 

32.1 

30.1 

30.4 

41.3 

132 

VoRecovery 

NA 

NA 

NC 

NC 

105 

37.7 ng/mL ± 6.4% 

PFOS 

Concentration 

(ng/mL) 

62.6 

58.9 

60.5 

68.5 

161 

VoRecovery 

NA 

NA 

NC 

NC 

103 

60.8 ng/mL ± 6.1% 

NA = Not Applicable 

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

PFBS, PFHS, and PFOS were analyzed on 1/10/11 with a 1:10 dilution. 

Page 28 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 20. DAL GW 1 SSL 10110S 

3M LIMS ID 

GLP10-01-02-11-056 

GLP10-01-02-11-057 

GLP10-01-02-11-058 

GLP10-01-02-11-059 

GLP10-01-02-11-060 

Average Concent 

Description 

DAL GW133L 0101103 

DAL GW133LDB 101103 

DALGW133LL8101103 

DAL GW133L MS 101103 

DAL GW133LHS 101103 

•ation (ng/mL) ± VoRPD 

PFBS 

Concerttration 

(ng/mL) 

771 

7.58 

18.3 

114 

984 

VoRecovery 

NA 

NA 

110 

109 

100 

7.65 ng/mL ±1.r/o 

PFHS 

Concentration 

(ng/mL) 

54.0 

52.7 

63.7 

154 

1060 

VoRecovery 

NA 

NA 

NC 

105 

105 

53.4 ng/mL ±2.4% 

PFOS 

Concentration 

(ng/mL) 

205 

202 

198 

283 

1210 

VoRecovery 

NA 

NA 

NC 

NC 

103 

204 ng/mL ±1.5% 

NA=NotApplicat)le 

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

PFBS, PFHS, and PFOS were analyzed on 1/10/11 with a 1:10 dilution. 

Table 21. DAL GW1SSS 101103 

3M LIMS ID 

GLP10-01-02-11-051 

GLP10-01-02-11-052 

GLP10-01-02-11-053 

GLP10-01-02-11-054 

GLP10-01-02-11-055 

Average Concent 

Description 

DALGW 1338 0101103 

DALGW 1338 DB 101103 

DAL GW133SLS 101103 

DALGW 1338 MS 101103 

DALGW 1338 HS 101103 

ration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

140 

14.0 

25.1 

117 

966 

VoRecovery 

NA 

NA 

114 

106 

97.9 

14.0 ng/mL ±0.0% 

PFHS 

Concentration 

(ng/mL) 

92.0 

91.0 

104 

192 

1050 

VoRecovery 

NA 

NA 

NC 

105 

99.7 

91.5 ng/mL ±1.1% 

PFOS 

Concentration 

(ng/mL) 

228 

220 

235 

330 

1200 

VoRecovery 

NA 

NA 

NC 

NC 

99.8 

224 ng/mL ±3.6% 

NA = Not Applicable 

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

PFBS, PFHS, and PFOS were analyzed on 1/10/11 with a 1:10 dilution. 

Page 29 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 22. DAL GW 134R 101105 

3M LIMS ID 

GLP10-01-02-11-061 

GLP10-01-02-11-062 

GLP10-01-02-11-063 

GLP10-01-02-11-064 

Description 

DAL GW134R 0101105 

DAL GW134RDB 101105 

DAL GW134RLS 101105 

DALGW134RHS101105 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

59.9 

52.5 

162 

1050 

%Recoveiy 

NA 

NA 

109 

102 

56.2 ng/mL ±73% 

PFHS 

Concentration 

(ng/mL) 

526 

479 

590 

1450 

VoRecovery 

NA 

NA 

NC 

98.6 

503 ng/mL ±9.4% 

PFOS 

Concentration 

(ng/mL) 

1530 

1310 

1430 

2310 

VoRecovery 

NA 

NA 

NC 

91.0 

1420 ng/mL ±15% 

NA = Not Applicatsle 

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

PFBS, PFHS, and PFOS were analyzed on 1/14/11 with a 1:100 dilution. 

Table 23. DALGW 1S4L 101105 

3M LIMS ID 

GLP10-01-02-11-070 

GLP10-01-02-11-071 

GLP10-01-02-11-072 

GLP10-01-02-11-073 

GLP10-01-02-11-074 

Average Concent 

Description 

DAL GW134L 0101105 

DAL GW134LDB 101105 

DALGW134LL8101105 

DALGW134LMS101105 

DAL GW134LHS 101105 

ration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

11.7 

12.1 

22.3 

110 

NA<'' 

%Recovery 

NA 

NA 

107 

101 

NA<^' 

77.9 na/m/.± 3.4% 

PFHS 

Concentration 

(ng/mL) 

112 

112 

120 

203 

NA<^' 

%Recovery 

NA 

NA 

NC 

94.7 

NA'^> 

772 ng/mL ±0.0% 

PFOS 

Concentration 

(ng/mL) 

571 

586 

617 

646 

1640 

VoRecovery 

NA 

NA 

NC 

NC 

109 

579 ng/mL ±2.6% 

NA = Not Applicatile 

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

PFBS and PFHS were analyzed on 1/10/11 with a 1:10 dilution. PFOS was analyzed on 1/14/11 with a 1:50 dilution. 

(1) A dilution of the sample was not prepared as ttie spike level was not appropriate as compared to the sample concentrations. 

Page 30 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 24. DALGW 134S 101105 

3M LIMS ID 

GLP10-01-02-11-065 

GLP10^1-02-11-066 

GLP10-01-02-11-067 

GLP10-01-02-11-068 

GLP10-01-02-11-069 

Average Concent 

Description 

DALGW 1348 0101105 

DALGW134SDB101105 

DALGW 1348 LS 101105 

DALGW 1348 MS 101105 

DALGW 1348 HS 101105 

ration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

0.146 

0.140 

1.27 

11.6 

102 

VoRecovery 

NA 

NA 

116 

118 

105 

0.143 ng/mL ±4.r/o 

PFHS 

Concentration 

(ng/mL) 

1.76 

1.65 

3.00 

13.2 

104 

VoRecovery 

NA 

NA 

135'^' 

120 

106 

7.77 ng/mL ±6.5%'^ 

PFOS 

Concentration 

(ng/mL) 

11.3 

11.5 

10.2 

22.4 

119 

VoRecovery 

NA 

NA 

NC 

112 

110 

77.4 ng/mL ± 1.8% 

NA= Not Applicable 

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

PFBS, PFHS and PFOS were analyzed on 1/7/11 with a 1:5 dilution. 

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

(2) The analytical uncertainty has been adjusted to ± 35%. 

Table 25. DALGW 135R 101105 

3M LIMS ID 

GLP10-01-02-11-075 

GLP10-01-02-11-076 

GLP10-01-02-11-077 

GLP10-01-02-11-078 

Description 

DAL GW135R 0101105 

DAL GW135RDB 101105 

DAL GW135RLS 101105 

DAL GW135RH8 101105 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concerttration 

(ng/mL) 

82.1 

79.9 

195 

1150 

VoRecovery 

NA 

NA 

117 

110 

81.0 ng/mL ±2.7% 

PFHS 

Concentration 

(ng/mL) 

847 

831 

914 

1900 

VoRecovery 

NA 

NA 

NC 

110 

839 ng/mL ±1.9% 

PFOS 

Concentration 

(ng/mL) 

903 

880 

955 

1890 

VoRecovery 

NA 

NA 

NC 

102 

892 ng/mL ±2.6% 

NA= Not Applicable 

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

PFBS, PFHS, and PFOS were analyzed on 1/14/11 with a 1:100 dilution. 

Page 31 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table26. DALGW 1S5L 101105 

3M LIMS ID 

GLP10-01-02-11-084 

GLP10-01-02-11-085 

GLP10-01-02-11-086 

GLP10-01-02-11-087 

GLP10-01-02-11-088 

Average Concent 

Description 

DAL GW135L 0101105 

DAL GW135LDB 101105 

DALGW135LL8 101105 

DALGW135LM8101105 

DALGW135LHS 101105 

ratfon (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

5.84 

5.62 

16.5 

120 

1060 

VoRecovery 

NA 

NA 

111 

118 

108 

5.73 ng/mL ±3.8% 

PFHS 

Concentration 

(ng/mL) 

35.4 

36.3 

48.0 

150 

1090 

VoRecovery 

NA 

NA 

NC 

119 

110 

35.9 ng/mL ±2.5% 

PFOS 

Concentration 

(ng/mL) 

23.9 

21.3 

39.8 

134 

1030 

VoRecovery 

NA 

NA 

NC 

114 

103 

22.6nfi/mL±72% 

NA=NotApplicat)le 

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

PFBS and PFHS were analyzed on 1/14/11 with a 1:100 dilution. PFOS was analyzed on 2/11/11 with a 1:10 dilution. 

Page 32 of 104 
GLP10-01-02; Interim Report 11 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 27. DAL GW135S 101105 

3M LIMS ID 

GLP10-01-02-11-079 

GLP10-01-02-11-080 

GLP10-01-02-11-081 

GLP10-01-02-11-082 

GLP10-01-02-11-083 

Description 

DALGW 1358 0101105 

DALGW135SDB101105 

DALGW1358LS 101105 

DALGW 1358 MS 101105 

DALGW135SHS 101105 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

0.794 

0.803 

1.94 

11.4 

NA<^' 

VoRecovery 

NA 

NA 

117 

109 

NA'^' 

0.799 ng/mL ±1.1% 

PFHS 

Concentration 

(ng/mL) 

6.35 

6.15 

7.26 

16.8 

NATM 

VoRecovery 

NA 

NA 

105 

110 

NATM 

6.25 ng/mL ±3.r/o 

PFOS 

Concentration 

(ng/mL) 

5.01 

475 

5.59 

148 

NATM 

VoRecovery 

NA 

NA 

NC 

101 

NATM 

4.88 ng/mL ±5.3% 

NA = Not Applicable 

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

PFBS, PFHS and PFOS were analyzed on 1/7/11 without dilution. 

(1) A dilution of the sample was not prepared as the spike level was not appropriate as compared to the sample concentrations. 

Table 28. DAL GW 136L 10110S 

3M LIMS ID 

GLP10-01-02-11-094 

GLP10-01-02-11-095 

GLP10-01-02-11-096 

GLP10-01-02-11-097 

GLP10-01-02-11-098 

Description 

DAL GW136L 0101103 

DAL GW136LDB 101103 

DAL GW136LL8 101103 

DALGW136LMS101103 

DALGW136LHS 101103 

Average Concerttration (ng/mL) ± %RPD 

PFBS 

Concentration 

(n^mL) 

2.43 

2.63 

13.5 

103 

976 

VoRecovery 

NA 

NA 

113 

103 

100 

2.53 ng/mL ±7.9% 

PFHS 

Concentration 

(ng/mL) 

15.5 

16.8 

27.2 

117 

1020 

VoRecovery 

NA 

NA 

115 

105 

104 

16.2 ng/mL ±8.0% 

PFOS 

Concentration 

(ng/mL) 

75.7 

82.7 

91.9 

171 

1110 

VoRecovery 

NA 

NA 

NC 

93.9 

105 

79.2 ng/mL ±8.8% 

NA = Not Applicable 

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

PFBS, PFHS and PFOS were analyzed on 1/10/11 witha 1:10dilution. 

Page 33 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 29. DAL GW 1S6S 101103 

3M LIMS ID 

GLP10-01-02-11-089 

GLP10-01-02-11-090 

GLP10-01-02-11-091 

GLP10-01-02-11-092 

GLP10-01-02-11-093 

Average Concent 

Description 

DALGW 1368 0101103 

DAL GW 1368 DB 101103 

DALGW1368LS 101103 

DALGW 1368 MS 101103 

DALGW136SHS101103 

ration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

2.52 

2.57 

3.66 

13.5 

101 

VoRecovery 

NA 

NA 

NC 

113 

101 

2.55 ng/mL ±2.0% 

PFHS 

Concentration 

(ng/mL) 

16.0 

16.9 

177 

27.1 

114 

VoRecovery 

NA 

NA 

NC 

111 

102 

16.5 ng/mL ±5.5% 

PFOS 

Concentration 

(ng/mL) 

85.5 

88.7 

87.2 

94.6 

180 

VoRecovery 

NA 

NA 

NC 

NC 

95.0 

87.1 ng/mL ±3.7% 

NA = Not Applicable 

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

PFBS, PFHS and PFOS were analyzed on 1/10/11 with a 1:10 dilution. 

Table 30. DAL GW137L 101109 

3M LIMS ID 

GLP10-01-02-11-104 

GLP10-01-02-11-105 

GLP10-01-02-11-106 

GLP10-01-02-11-107 

GLP10-01-02-11-108 

Description 

DAL GW137L 0101109 

DALGW137LDB101109 

DAL GW137LL8 101109 

DAL GW137L MS 101109 

DALGW137LH8 101109 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

0.0812 

0.0833 

0.190 

1.22 

10.7 

VoRecovery 

NA 

NA 

111 

117 

109 

0.0823 ng/mL ±2.6% 

PFHS 

Concentration 

(ng/mL) 

0.117 

0.121 

0.240 

1.25 

10.8 

VoRecovery 

NA 

NA 

126 

118 

111 

0.199 ng/mL ±3.4% 

PFOS 

Concentration 

(ng/mL) 

0.877 

0.909 

0.948 

1.79 

10.0 

VoRecovery 

NA 

NA 

NC 

91.7 

93.1 

0.893 ng/mL ±3.6% 

NA= Not Applicable 

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

PFBS, PFHS and PFOS were analyzed on 1/7/11 without dilution. 

Page 34 of 104 
GLP10-01-02; Interim Report 11 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table31. DALGW 1S7S 101109 

3M LIMS ID 

GLP10-01-02-11-099 

GLP10-01-02-11-100 

GLP10-01-02-11-101 

GLP10-01-02-11-102 

GLP10-01-02-11-103 

Description 

DAL GW137S 0101109 

DALGW137SDB 101109 

DALGW 1378 LS 101109 

DALGW 1378 MS 101109 

DALGW 1378 HS 101109 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

0.0990 

0.104 

0.206 

1.21 

10.6 

VoRecovery 

NA 

NA 

108 

114 

108 

0.102 ng/mL ±4.9% 

PFHS 

Concentration 

(ng/mL) 

0.0886 

0.0942 

0.201 

1.15 

10.4 

VoRecovery 

NA 

NA 

114 

110 

107 

0.0974 ng/mL± 6.7% 

PFOSf^ 

Concentration 

(ng/mL) 

0.367 

0.263 

0.328 

0.890 

6.12 

VoRecovery 

NA 

NA 

NC 

58.8TM 

59.4TM 

0.315 ng/mL ± 33%'^^' 

NA = Not Applicable 

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

PFBS, PFHS and PFOS were analyzed on 1/7/11 without dilution. 

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

(2) The analytical uncertainty for PFOS has been adjusted for FMS recovery to ± 41 %. 

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

Page 35 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table32. DALGW 138S 101110 

3M LIMS ID 

GLP10-01-02-11-109 

GLP10-01-02-11-110 

GLP10-01-02-11-111 

GLP10-01-O2-11-112 

GLP10-01-02-11-113 

Average Concent 

Description 

DALGW 1388 0101110 

DAL GW 1388 DB 101110 

DAL GW 1388 LS 101110 

DALGW 1388 MS 101110 

DAL GW 1388 HS 101110 

ration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

4.74 

4.63 

16.2 

99.8 

949 

VoRecovery 

NA 

NA 

118 

97.9 

97.2 

4.69 ng/mL ±2.3% 

PFHS 

Concentration 

(ng/mL) 

24.0 

22.9 

35.4 

119 

991 

VoRecovery 

NA 

NA 

NC 

99.4 

101 

23.5 ng/mL ±4.r/o 

PFOS 

Concentration 

(ng/mL) 

252 

238 

256 

307 

1210 

VoRecovery 

NA 

NA 

NC 

NC 

98.7 

245 ng/mL ±5.7% 

NA = Not /Applicable 

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

PFBS, PFHS and PFOS were analyzed on 1/10/11 with a 1:50 dilution. 

Table33. DALGW 138L 101110 

3M LIMS ID 

GLP10-01-02-11-114 

GLP10-01-02-11-115 

GLP10-01-02-11-116 

GLP10-01-02-11-117 

GLP10-01-02-11-118 

Average Concent 

Description 

DAL GW138L 0101110 

DAL GW138LDB 101110 

DALGW138LLS 101110 

DAL GW138L MS 101110 

DALGW138LH8 101110 

ration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

0.0460 

0.0485 

0.157 

1.16 

10.8 

VoRecovery 

NA 

NA 

113 

114 

111 

0.0473 ng/mL ±5.3% 

PFHS 

Concentration 

(ng/mL) 

0.143 

0.144 

0.259 

1.28 

10.9 

VoRecovery 

NA 

NA 

120 

118 

112 

0.144 ng/mL± 0.70% 

PFOS 

Concerttration 

(ng/mL) 

0.581 

0.580 

0.684 

1.29 

8.42 

VoRecovery 

NA 

NA 

NC 

72.5 

80.2 

0.581 ng/mL ±0.17% 

NA = Not Applicable 

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

PFBS, PFHS and PFOS were analyzed on 1/7/11 without dilution. 

Page 36 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table S3. DAL GW CW26R 101110 

3M LIMS ID 

GLP10-01-02-11-119 

GLP10-01-02-11-120 

GLP10-01-02-11-121 

GLP10-01-02-11-122 

GLP10-01-02-11-123 

Description 

DAL GWCW26R0 101110 

DAL GWCW26RDB 101110 

DAL GW CW26R LS 101110 

DAL GWCW26R MS 101110 

DAL GWCW26RH8 101110 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

8.14 

8.40 

19.2 

105 

NATM 

VoRecovery 

NA 

NA 

112 

100 

NATM 

8.27 ng/mL ±3.1% 

PFHS 

Concentration 

(ng/mL) 

61.7 

64.4 

73.9 

155 

NATM 

VoRecovery 

NA 

NA 

NC 

95.7 

NATM 

63.7 ng/mL± 4.3% 

PFOS 

Concentration 

(ng/mL) 

455 

446 

439 

526 

1470 

VoRecovery 

NA 

NA 

NC 

NC 

104 

451 ng/mL ±2.0% 

NA = Not Applicable 

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

PFBS and PFHS were analyzed on 1/10/11 with a 1:10 dilution. PFOS were analyzed on 1/14/11 with a 1:50 dilution. 

(1) A dilution of the sample was not prepared as tfie spike level was not appropriate as compared to the sample concentration. 

Table 34. DAL GW CW26L 101110 

3M LIMS ID 

GLP10-01-02-11-124 

GLP10-01-02-11-125 

GLP10-01-02-11-126 

GLP10-01-02-11-127 

GLP10-01-02-11-128 

Description 

DAL GWCW26L 0101110 

DALGWCW26LDB 101110 

DAL GWCW26LL8 101110 

DAL GW CW26L MS 101110 

DAL GWCW26LHS 101110 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

13.2 

12.5 

23.3 

107 

NATM 

VoRecovery 

NA 

NA 

108 

96.9 

NATM 

12.9 ng/mL ±5.4% 

PFHS 

Concentration 

(ng/mL) 

95.6 

90.2 

102 

183 

NATM 

VoRecovery 

NA 

NA 

NC 

93.8 

NATM 

92.9 ng/mL± 5.8% 

PFOS 

Concerttration 

(ng/mL) 

888 

808 

896 

855 

1840 

VoRecovery 

NA 

NA 

NC 

NC 

101 

848 ng/mL ±9ji% 

NA = Not Applicable 

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

PFBS and PFHS were analyzed on 1/10/11 with a 1:10 dilution. PFOS were analyzed on 1/14/11 with a 1:50 dilution. 

(1) A dilution of the sample was not prepared as the spike level was not appropriate as compared to ttie sample concentration. 

Page 37 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Ajrea - November 2010 

Table 35. DAL GW 140R101104 

3M LIMS ID 

GLP10-01-02-11-129 

GLP10-01-02-11-130 

GLP10-01-02-11-131 

GLP10-01-02-11-132 

GLP10-01-02-11-133 

Description 

DAL GW140R 0101104 

DALGW140RDB 101104 

DALGW140RLS101104 

DALGW140RMS101104 

DAL GW140RHS 101104 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

1.65 

1.61 

11.9 

96.4 

NATM 

VoRecovery 

NA 

NA 

106 

97.5 

NATM 

1.63 ng/mL ±2.5% 

PFHS 

Concentration 

(ng/mL) 

17.2 

17.2 

27.2 

115 

NATM 

VoRecovery 

NA 

NA 

104 

102 

NATM 

17.2 ng/mL± 0.0% 

PFOS 

Concentration 

(ng/mL) 

140 

131 

139 

229 

NATM 

VoRecovery 

NA 

NA 

NC 

95.6 

NATM 

136 ng/mL ±6.6% 

NA = Not Applicable 

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

(1) A dilution of the sample was not prepared as the spike level was not appropriate as compared to the sample concentration. 

Table 36. DAL GW 141R 101110 

3M LIMS ID 

GLP10-01-02-11-134 

GLP10-01-02-11-135 

GLP10-01-02-11-136 

GLP10-01-02-11-137 

GLP10-01-02-11-138 

Description 

DAL GW141R0 101110 

DAL GW141RDB 101110 

DALGW 141 RLS 101110 

DAL GW141R MS 101110 

DAL GW141RHS 101110 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

0.0444 

0.0418 

10.1 

96.7 

977 

VoRecovery 

NA 

NA 

103 

99.4 

101 

0.0431 ng/mL ±6.0% 

PFHS 

Concentration 

(ng/mL) 

0.273 

0.243 

10.4 

96.2 

NATM 

VoRecovery 

NA 

NA 

106 

99.8 

NATM 

0.258 ng»nL± 72% 

PFOS 

Concentration 

(ng/ml^ 

4.48 

3.97 

11.4 

81.2 

NATM 

VoRecovery 

NA 

NA 

73.4 

78.7 

NATM 

4.23 ng/mL ±ir/o 

NA = Not Applicable 

PFHS and PFOS were analyzed on 1/10/11 with a 1:10 dilution. PFBS was analyzed on 2/11/11. The sample, sample duplicate and LS were analyzed without a dilution, the MS with a 1:10 

dilution, and the HS with a 1:50 dilution. 

(1) A dilution of the sample was not prepared as the spike level was not appropriate as compared to the sample concentrations. 

Page 38 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 37. DAL GW 142R 101110 

3M LIMS ID 

GLP10-01-02-11-139 

GLP10-01-02-11-140 

GLP10-01-02-11-141 

GLP10-01-02-11-142 

GLP10-01-02-11-143 

Description 

DAL GW142R 0101110 

DAL GW142RDB 101110 

DAL GW142RL8 101110 

DAL GW142R MS 101110 

DAL GW142RHS 101110 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

1.69 

1.67 

11.9 

98.0 

NATM 

VoRecovery 

NA 

NA 

105 

99.1 

NATM 

7.68 ng'mL± 7.2% 

PFHS 

Concentration 

(ng/mL) 

10.0 

9.96 

19.8 

108 

NATM 

VoRecovery 

NA 

NA 

102 

102 

NATM 

9.98 ng/mL ±0.40% 

PFOS 

Concentration 

(ng/mL) 

111 

104 

118 

200 

NATM 

VoRecovery 

NA 

NA 

NC 

94.6 

NATM 

108 ng/mL ±6.5% 

NA = Not Applicable 

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

PFBS, PFHS and PFOS were analyzed on 1/10/11 with a 1:10 dilution. 

(1) A dilution of the sample was not prepared as ttie spike level was not appropriate as compared to the sample concentrations. 

Table 38. DAL GW 144R 101110 

3M LIMS ID 

GLP10-01-02-11-144 

GLP10-01-02-11-145 

GLP10-01-02-11-146 

GLP10-01-02-11-147 

GLP10-01-02-11-148 

Description 

DAL GW144R 0101110 

DAL GW144RDB 101110 

DALGW144RLS 101110 

DAL GW144R MS 101110 

DALGW144RH8 101110 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

1.98 

1.91 

11.6 

98.5 

NATM 

VoRecovery 

NA 

NA 

99.3 

99.3 

NATM 

1.95 ng/mL ±3.6% 

PFHS 

Concentration 

(ng/mL) 

8.79 

8.35 

17.9 

103 

NATM 

VoRecovery 

NA 

NA 

97.1 

98.3 

NATM 

8.57 ng/mL ±5.1% 

PFOS 

Concentration 

(ng/mL) VoRecovery 

Not Reported 

Not Reported'^ 

NA = Not Applicable 

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

PFBS, PFHS and PFOS were analyzed on 1/10/11 with a 1:10 dilution. 

(1) A dilution of the sample was not prepared as the spike level was not appropriate as compared to the sample concentrations. 

(2) Not Reported; The matrix spike samples prepared and analyzed for this sampling location for PFOS had recoveries <50%. 

Page 39 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 39. Trip Blank 

3M LIMS ID 

GLP10-01-02-11-150 

GLP10-01-02-11-151 

GLP10-01-O2-11-152 

GLP10-01-02-11-153 

GLP10-01-02-11-154 

Description 

TRIP BLANK 1 0 

TRIP BLANK 1 LS 

TRIP BLANK 1 MS 

TRIP BLANK 1 MHS 

TRIP BLANK 1 HS 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

1.12 

10.6 

98.6 

1050 

VoRecovery 

NA 

115 

109 

101 

108 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

1.10 

10.5 

101 

1050 

VoRecovery 

NA 

114 

109 

105 

109 

PFOS 

Concentration 

(ng/mL) 

<0.250 

1.04 

10.3 

104 

930 

VoRecovery 

NA 

106 

105 

106 

95.1 

NA = Not /Applicable 

Table 40. Trip Blank 2 

3M LIMS ID 

GLP10-01-02-11-155 

GLP10-01-02-11-156 

GLP10^1-02-11-157 

GLP10-01-02-11-158 

GLP10-01-02-11-159 

Description 

TRIP BLANK 2 0 

TRIP BLANK 2 LS 

TRIP BLANK 2 MS 

TRIP BLANK 2 MHS 

TRIP BLANK 2 HS 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

1.12 

10.8 

97.1 

1040 

VoRecovery 

NA 

115 

111 

100 

107 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

1.09 

10.8 

99.3 

1040 

VoRecovery 

NA 

113 

112 

103 

108 

PFOS 

Concentration 

(ng/mL) 

<0.250 

1.01 

10.7 

105 

952 

VoRecovery 

NA 

103 

109 

107 

97.3 

NA = Not Applicat)le 

Page 40 of 104 
GLP10-01-02; Interim Report 11 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 41. Trip Blank 3 

3M LIMS ID 

GLP10-01-02-11-160 

GLP10-01-02-11-161 

GLP10-01-02-11-162 

GLP10-01-02-11-163 

GLP10-01-02-11-164 

Description 

TRIP BLANK 3 0 

TRIP BLANK 3 LS 

TRIP BLANK 3 MS 

TRIPBU\NK3MHS 

TRIP BLANK 3 HS 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

1.11 

10.3 

99.2 

1030 

VoRecovery 

NA 

114 

106 

102 

106 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

1.08 

10.4 

101 

1040 

VoRecovery 

NA 

112 

108 

105 

108 

PFOS 

Concentration 

(ng/mL) 

<0.250 

1.03 

9.96 

105 

925 

VoRecovery 

NA 

105 

102 

107 

94.6 

NA = Not Applicable 

Table 42. Trip Blank 4 

3M LIMS ID 

GLP10-01-02-11-165 

GLP10-01-02-11-166 

GLP10-01-02-11-167 

GLP10-01-02-11-168 

GLP10-01-02-11-169 

Description 

TRIP BLANK 4 0 

TRIP BLANK 4 LS 

TRIP BLANK 4 MS 

TRIP BLANK 4 MHS 

TRIPBL^NK4H8 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

1.10 

10.7 

99.5 

1020 

%Recovery 

NA 

113 

110 

102 

105 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

1.09 

10.6 

101 

1020 

%Recovery 

NA 

113 

110 

105 

106 

PFOS 

Concentration 

(ng/mL) 

<0.250 

0.983 

10.2 

103 

909 

VoRecovery 

NA 

101 

104 

105 

92.9 

NA = Not Applicable 

Page 41 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 43. Rinseate Blanks 

3M LIMS ID 

GLP10-01-02-11-016 

GLP10-01-02-11-149 

Description 

DAL GW130LRB 101105 

DAL GW144RRB 101110 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

VoRecovery 

NA 

NA 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

VoRecovery 

NA 

NA 

PFOS 

Concentration 

(ng/mL) 

<0.250 

<0.250 

VoRecovery 

NA 

NA 

NA= Not/Applicable 

Table 44. GLP10-01-02-12 Soil Equipment Rinseate Blank 

3M LIMS ID 

GLP10-01-02-12-009 

Description 

DAL SS 607R RB 0040 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

VoRecovery 

NA 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

VoRecovery 

NA 

PFOS 

Concerttration 

(ng/mL) 

<0.250 

VoRecovery 

NA 

NA = Not /Applicable 

Page 42 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

10 Conclusion;. •••. 

Laboratory control spikes and field matrix spilces were used to determine the analytic^al metliod 

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

3I\/I Environmental Laboratory method ETS-8-044.0 described herein. 

11 Data/Sample Retention 

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

to SM Environmental Laboratory standard operating procedures. 

12 Attachment s 

Attachment A: Protocol Amendment 11 (General Project Outline) 

Attachment B: Representative Chromatograms and Calibration Curves 

Attachment C: Analytical Method 

Attachment D: Method Deviation 

Page 43 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

13 Signatures 

^/io/2ai) 

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

/^A^ y ^/ / 

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

ra 

9: 

If 

Gary Hohenstain, Sponsor Representative 

Olhd, 

Date 

Jaisimha Kesari, Study Director ' Date 

Page 44 of 104 
GLP10-01-02; interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

ATTACHMENT A: PROTOCOL AMENDMENT 

Page 45 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge incorporation Area - November 2010 

Analytical Protocol: GLP10-01-02 

Amendment 11 

Study Title 

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

Perfluorobutane sulfonate (PFBS) In Groundwater, Sol! and Sediment for the 3M 

Decatur Phase 3 Site-Related Monitoring Program 

PROTOCOL AMENDMENT NO. 11 

Amendment Date: 

October 20, 2010 

Performing Laboratory 

3M Environmental, Health, and Safety Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55144-1000 

Laboratory Project Identification 

GLP10-01-02 

Sampling Event 

Former Sludge Incorporation Area (FSIA) Groundwater 

Page 1 of 7 

Page 46 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Former Sludge Incorporation Area - November 2010 

Analyticai Protocol: GLP10-01-02 

Amendment 11 

This amendment modifies the following portion of protocol: 

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

Decatur Phase 3 Site-Related Monitoring Program" 

PROTOCOL READS: 

No changes to the wording of the protocol are required. 

AMEND TO READ: 

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

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

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

(GLP10-01-02). The anticipated sample collection will occur around the timeframe of October 25, 2010. 

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

LIMS as project GLP10-01-02-11 and reported as interim report GLP10-01-02-11, (reflecting study 

GLP10-01-02 and amendment-11). 

Reason: 

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

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

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

Page 2 of 7 

Page 47 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Analytical Protocol: GLP10-01-02 

Amendment 11 

Amendment Approval 

/ 

^% ljW%m^k 

iO L, 

id 

Gary Hohenstein, Sponsor Representative Date 

Cleston C. Lange, Principal Analyticai Investigator I D6te 

o/ cjcr'^o/o 

William Reagecd EHS Opns Environmental Lab Management Date 

Jaisimha Kesari P.E., DEE, Study Director 

Page 3 of 7 

Page 48 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Analytical Protocol: GLP10-01-02 

Amendment 11 

Environmental Health & Safety Operations, Environmental Laboratory 

General Project Outline 

To: Gary Hohenstein, 3M EHS&Opns 

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

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

Cliffton Jacoby, 3M EHS&Opns; Environmental Lab 

Jai Kesari, Weston Solutions 

Charles Young, Weston Solutions 

Tim Frinak, Weston Solutions 

Date: October 20,2010 

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 11 - Former Sludge 

Incorporation Area (FSIA) Groundwater 

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(a)mmm.com 

3M Environmental Laboratory Management 

William K. Reagen 

SIVI EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9739 

wkreaqenOmmm.com 

Principal Analytical Investigator 

Cleston Lange 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9860 

cclanqeOmmm.com 

Sampling Coordinator 

Timothy Frinak 

Weston Solutions 

Timothv.frinakOwestonsolutions.com 

Phone: (334)-332-9123 

GLP10-01-02-11 

Dept #530711, Project #0022674449 

Sampling scheduled for the week of October 25, 2010 

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

Page 4 of 7 

Page 49 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Analytical Protocol: GLP10-01-02 

Amendment 11 

2 Background Information and Project Objective(s) 

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

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

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

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

Laboratory Practice Standards 40 CFR 792. 

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

October 25, 2010. The 3M Environmental Laboratory will prepare the sample bottles with all required 

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

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

01-02-11. 

3 Project Schedule 

Sample collection bottles will be prepared by 3M Environmental Laboratory for sampling the week of June 21, 

2010. Sample bottles will be shipped in coolers overnight to 3M Decatur for arrival on Friday, June 18,2010. 

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

Martin Smith \ Weston Trailer 

3M Decatur Plant 

1400 State Docks Road 

Decatur, Alabama 35601 

4 Test Parameters 

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

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

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

con-esponding field spike levels. The "fill to here" line on each 250 mL Nalgene bottle will be 200 mL. Four sets 

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

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

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

of the equipment rinseate blanks. A total of 189 sample bottles will be prepared. 

Page 5 of 7 

Page 50 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Analytical Protocol: GLP10-01-02 

Amendment 11 

Table 1. Sampling Locations and Field Matrix Spike levels. 

Well No. 

136R, 137R,137S,137L, 138L 

130L, 131L, 131S, 133R, 134S, 

1358,1368 

130R,130S,132R, 132L, 132S, 

133S, 133L, 134L, 135L, 136L, 

138S, 138R, CW26R, CW26L, 

140R, 141R, 142R, 143, and 144R 

131R, 134R, 135R 

Trip Blank Set 1,2, 3, and 4 

Sample Level 

Low 

Mid 

High 

Low 

Mid 

High 

Low 

Mid 

High 

Low 

High 

Low 

Mid 

Mid-High 

High 

Spike Cone. (ng/mL) 

0.1 

1.0 

10 

1 

10 

100 

10 

100 

1000 

100 

1000 

1 

10 

100 

1000 

5 Test Methods 

Samples will be prepared and analyzed by LC/MS/MS follov\flng ETS-8-044.0 "Detennination of Perfiuorinated 

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

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

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

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

previously collected samples from the FSIA (GLP10-01-02-07), most sampling locations will require dilution with 

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

Altemately, samples may be analyzed by ETS 8-154.3 "Determination of Perfiuorinated Acids, Alcohols, 

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

Chromatography/Mass Spectrometry". 

6 Reporting Requirements 

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

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

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

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

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

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

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

the final report. 

7 Email Correspondence 

Attachment A: Sampling Bottle Request 

Page 6 of 7 

Page 51 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Analytical Protocol: GLP10-01-02 

Amendment 11 

Attachment A 

Bottle Request 

Decatur Groundwater Sampling 

On-site FSIA Wells 

02181.129.145.0004 

DATE REQUESTED: 18 October 2010 DATE REQUIRED: 25 October 2010 

This request addresses the bottle requirements for the following wells: 

130R 

130S 

130L 

131R 

131S 

131L 

132R 

132S 

132L 

133R 

133S 

133L 

134R 

134S 

134L 

135R 

135S 

135L 

136R 

136S 

136L 

137R 

137S 

137L 

138R 

138S 

138L 

CW26R 

CW26L 

NOR 

141R 

142R 

143R 

144R 

Total Wells: 34 

Sample Summary 

No. of Samples 

34 

2 

4 

Sample Type 

Groundwater 

Rinseate Sample 

Trip Blanks 

Comment 

Will need HPLC water 

Anticipate 1 per cooler 

Note: Some of the wells have limited volume so the smaller the volume requirements the better. 

SHIPPING INFORMATION 

Please ship to the following address: 

Martin Smith \ Weston Field Office 

3M Decatur Plant 

1400 State Docks Road 

Decatur, AL 35601 

256-552-6189 

Page 7 of 7 

Page 52 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

ATTACHMENT B: REPRESENTATIVE SAMPLE CHROMATOGRAMS AND 

CALIBRATION CURVE 

Page 53 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Buster J2930203 Batch Name: bll0107a.dab 

• 

m 

c 

8 

CO 

< 

b110107a.rdb (PFBS): "Quadratic" Regression ("1 / x" weigliting): y = -7.8e+003 x'2 + 1.03e+006 x + 5.1e+003 (r = 0.9997) 

4.8e7-

4.6e7-

4.4e7-

4.2e7-

4.0e7-

3.8e7-

3.6e7-

3.4e7-

3.2e7-

3.0e7-

2.8e7-

2.6e7 

2.4e7-

2.2e7 

2.0e7-

1.8e7-

1.6e7-

1.4e7-

1.2e7-

1.0e7-

8.0e6 

6.0e6-

4.0e6-

2.0e6-

0.0^ 

/ ' ' 

/ A / / 

/ 

/ 

/ / / / / 

• / / 

/ 

0 5 10 15 20 25 30 35 40 

^.. ^ ' " " 

45 50 55 60 65 

Concentration, ng/mL 

-.-. 

70 

O 

—-___ 

75 80 

"•''•--, „ 

85 

^^•^ ^ 

90 95 

^ 

X 

100 

Printing Time: 3:12:03 PM 

Printing Date: Tuesday, February 01, 2011 

Page 1 of 1 

Page 54 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Buster J2930203 Batch Name: bll0107a.dab 

b110107a.rdb (PFHS): "Quadratic" Regression {"1 / x" weighting): y = -7.09e+003 x"2 + 9.06e+005 x + 4.64e+003 (r = 0.9997) 

4.16/ 

4.0e7 -

3.8e7-

3.6e7-

3.4e7-

3.2e7-

3.0e7 -

2.8e7-

2.6e7-

2.4e7-

2.2e7-

2.0e7-

1.8e7-

1.6e7-

1.4e7-

1.2e7 

1.0e7-

8.0e6-

6.0e6-

4.0e6 -

2.0e6-

0.0-

P 

/ 

/ 

/ 

/ 

/ / 

/ 

/ 

/ 

, / 

X ' 

y 

/ 

,--''' 

^^••"' ^ 

^ '^ ' 

O 

-—.,^,. 

""•"--- ^ \ _ 

^^-.^ 

v_/ 

'^ 

-v. 

10 15 20 25 30 35 40 45 50 55 

Concentration, ng/mL 

60 65 70 75 80 85 90 95 100 

Printing Time: 3:12:25 ?K 

Printing Date: Tuesday, February 01, 2011 

Page 1 of 1 

Page 55 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Buster J2930203 Batch Name: bll01073.dab 

b110107a.rdb (PFOS): "Quadratic" Regression ("1 / x" weighting): y = -6.1e+003 x''2 + 8.64e+005 x + 2.98e+004 (r = 0.9999) 

4.2e7 

4.0e7 

3.8e7 

3.6e7 

3.4e7 

3.2e7-

3.0e7 

2.8e7 

2.6e7 

2.4e7 

2.2e7 

2.0e7 

1.8e7 

1.6e7 

1.4e7 

1.2e7 

1.0e7-

8.0e6-

6.0e6-

4.0e6-

2.0e6 

0.0 / 

O 

/ 

10 15 20 25 30 35 40 45 50 55 

Concentration, ng/mL 

60 65 70 75 80 85 90 95 100 

Print inq Time : 3 : 1.? : 51 ?K 

Printing Date: Tuesday, February 01, 2011 

Page 1 of 1 

Page 56 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS. PFHS. and PFOS in Groundwater 

Fonner Sludge Incorporation Area - November 2010 

Blister J293C203 

I

Sampto Name: -i)11O1O7a0l6' SamplB IDr tlB00«-194^* 

Pvnk Name: "PFBS- Messfas}: •299.0/99.0 aTM.299J3('80.0 a 

CofimBnl; '1.0 nglni. FC »Id it MS Q Watai' Aniotalion' -

2.4e5 

2ABS 

2JB 5 

2J«S 

Z2eS 

2.2eS 

2.ieS 

2.1«5 

2J0t&-

2.0eS 

1.9eS1.9»S1.8«5-

1.8»i5-

1.roS1.7oS1.6«S 

1.& 

1.4eS 

1.46S 

1.34S 

1-3eS 

1^«S 

1.2eS 

1.1«S 

I.IoS 

1.0«5 

9.5e4 

^.OM 

a.te4 

8-0e4 

7.Se4 

&.SM 

5.0M 

4.SM' 

4.0e4 

3.5*1 • 

3.0e4 

2.&M 

2.ae4' 

1.5^ 

1.0e4-

5000 J> 

0.0 A<J&£ ^ 

I

SampteNafn«:-b1tOia7a0a8' Sauipte 10:'Solver:! Kank (AAiO^O Element)' Fie: tj-llOIOZal.w 

Peak Name: "PFBS* Ma*s(es}: •299.a'9S.0 «niu.299.a'80.0 amu" 

Comment tm-. Q Water TN11JXKJB" Anno-ation: -

Ki.-i. r#»k HDight: 

Printing Titne: 2:56:41 PM 

Printing Date: Tuesday, March 

Page 1 of 4 

10 12 

Ttrnq. min 

2 9 , 

Page 57 Of 104 
Buster J2930203 

GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

I

Sampte Name: T>nO1O7«034' Sample ID: 1.05-101230-4" 

PMk Name: TFBS" Maa*(es): •2M.0«9.0 amu,299.0iB0,a aj 

Cotrment: "Spf* LCS* Armotaltor' ~ 

Conctri.-ati 

1.20*6 

I.I896 

I.i6e6 

I.14e6 

1.12e6 

1.10o«-

V0S«6 

t.06ee 

I.04e6 

1.D2e6 

1-00c6-

9.B0«5 

3.60B5 

9.<0e5 

9.20e5 

9.00e5 

g.eoe5 

8.60e5 

B.40e5 

8.20e5-

B.00e5 

7.8065 

7.60e5 

7.40e5 

7.20e5 

VOOeS6.S0a5 

6.eaeS' 

6.40e5 

; t20BS' 

6.00«5-

5.fiOe5 

5.60e&-

5.40«5-

5,20eS 

S.MteS4.80«5' 

4.e0eS 

4.40eS4.20ea 

4.00e5 

3,60o5 

3.60e5 

3.40o5 

3.30B5 

3-00e5 

2.S0e6 

2.G0aS 

2.40e5 

2.20^ 

2.00«5 

I.BOeS 

VSOeS 

V40«S 

1.20eS 

l.OCteS' 

S.OOM 

e.00e4 

4.00*1 

2.00e4 

O.tX)' 

t-Spllt. Faozor 

(

Sample Name: "b • 1O107aO92- Sampto ID: ••GLPIiMli-02-! 

Peak Nanw: TFBS' MaM[es): '299.&-9S.0 Bniu.299.!V80.0 ar 

Comment: "DAL GW 134S 0 lOl ^05" Annotation: " 

Sansl c Type : Ur.V.-.own 

Ccncer.i rat ioi : !i.'.« 6400 

«3rtiii(ic: N o 8000 

7600 

C- .-r.j 

^po-r.:: '''XW 

J.in 7200 

i;.= '000 

i^'-t'! 6800 

^ i n 6600 

$400 

6200 

6000 

5800 

seco 

S400 

5200 

SOOO 

4600 

•(600-

. 4«0. 

- 4000 

3300 

3600 

3400-

3200 

KX»-

2S0Q' 

2fi00 

2400-

2200-

2000-

MOO 

1200 

1000 

li.llU4..Jt4^.i; 

Printing Time: 2:56:41 PM 

Princing Date: Tuesday, March 29, 

Page 2 of 4 

Page 58 of 104 
Buster J2930203 

GLP10-01-02; Interim Report 11 

Analysis of PFBS. PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

I

SampteName:T>11O1O7a016" Sampte ID-"08008-194-8' File:-b110107a1.witr 

P«ak Naire: -PFHS' Massfea): -39S.Q'-99.0 amu.3S9.0,'80.0 ama' 

Con-jnent: "1.0 ng/mL FC std in MMi Q Wstai' Annotasor ~ I

Sample Name: "bl 10107a008' Sample ff): 'Stdvent Blank (tMQ eiemeni)- Fla: "bl I01Q7a1.wir 

Peak Name: -PFMS" Mas8(es): -SSS.O'-Sg.O amy.399.0m0.0 amu" 

Comment: tm-. Q Water TNI 1-OOOS" Annotation: *• 

2.3eS 

2.3e5: 

2.1 eS 

2.1e5 

2.0e5 

1.7e5-

I.SeS 

I.ift5 

l.ieS 

1.0e5 

9.5e4' 

&.0e4 

B.5e4 

7.0*4 

6.5o4 

fi.0o4-

5.Se4 

S.OoA4.5*4-

4.0e4-

3.5B4-

3.0e4 

2.5e4-

2.0e4-

1.5e4-

1.0e4-

5000.0-

0.0- • ..-A.. 

1 JlJIii 

16 18 20 

Printing Time: 2:56:41 PM 

Printing Date: Tuesday, March 

Page 3 of 4 

Page 59 of 104 
Buster J2930203 

GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

tor.ti 

•.tjt-: 

5 

1 

36P7 : 

1.1 &• 

[

Sample Name:-b110iO7aO34- Sampto ID: T-CS-lOIZStM- Fie:1)noi07a1.wt(r 

Peakt(ama:TFHS- MaM(e»):-399.0^.0 amu,3e9.(V80^ attw* 

Cotrmenl: "Sppti LCS' AnnoCalkxi-" 

1.14e6 

1.l2e6 

1.IDe6 

1.0ee6 

1.06e6 

I.04a6 

1.02a6 

1.00e6 

9.60eS 

3.60e5 

9.40e5 

9.20e5 

9.00e5 

e.80e5 

e.60e5 

e.40e5 

a.2ae5 

a.00e5 

7.60e5 

7.60e5-

7.40e5-

7.!0e5 

r.OOeS 

&B0ft5 

S.60e5 

S.40eS 

5.20a5 

. S.0OeS 

• S.eOe5 

5.60e5 

S.40eS' 

SJOeS 

5.00e5-

4.S0«5 

4,60e5 

4.40eS' 

4.20e5' 

4.00e5' 

3.80c4-

3.60e5' 

3.4aeS 

3.2005-

3.00*5 

3.80^ 

2.60e5 

2.40e5 

2.20e5 

2.00e5-

1.80e5' 

I.60e5-

1.40«SLlOeS1.00e5-

e.oo»4-

6.00e4-

4.0064 • 

2.00e4-

0.00-

I

SamplaName:'bilO107aO9r Sampteffl:-GLPlfrOl-02-i1-065- F9et)I10107ai.wi(P 

Peak Name: "PFHS- MaMfes): •399.0-^.0 amu.399.0/80.0 amo* 

CommenfDALG\V;34S0101l05- AmtOaSon:-

6.5e4 

6.4e4 

6.3e4 

6.2fr4 

6.1M 

6.0e4 

5.9*4 

5.864 

5.7*4 

5.6»4 

5.5»4 

5,4e4 

5.3*4 

5.2*4 

5.ie4 

5,0e4 

4.9*4 

4.Be4 

4.7e4 

4.Se« 

4.5*4 

4.4e4 

4Jfl4 

4.2M 

4.lei 

4.Ce4 

3.9*4 

3.ae4 

3,7e4 

3.6*4 

3.5e4 

3.4*4 

3.3*4 

3.2*4 

3.1*4 

3.0*4 

2.9e4 

2.9*4 

2.7*4 

2.6*4 

2.5*4 

2.4e4 

2.3*4 

2.2e* 

2.1 e4 

2.0*4 

i.9e4 

i.8e4 

i.7*a 

1.S*4 

t.5e4 

t.4e4 

1JJ*4 

1.2*4 

1.1*4 

1J}»4 

9000.0 

8000.0 

70OC.0 

6000.0 

5000.0 

4000.0 

3000.0 

2000.0 

1000.0 

0.0 

14 IB 

1 

1 1 Ji*i.ii^r— • 

i| 

A i 

1*1—J.—, 16 18 20 

Printing Tine: 2:56:41 PM 

Printing Date: Tuesday, March 2 9, 

Page 4 of 4 

Page 60 of 104 
5te r J293020 3 

GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS. and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

• Sample Nam*:'bt 10107<t0l6- Sampi* ID: XS0Ofl-l94-8- FBe: -b1101U7a1.wrfr 

I Peakrtamo:-PFOS- Massieil:-':e9.C«9.0amu.499,0«OJ)aTXj.499.0.'I30.0amir 

I ComTienl:'1.0n9fniLFCs;iJ>--)MAQWate[' An:>olat>on-' 

Sjr-ple In^CK- 1 li 

Printing Time; 2:53:15 PM 

Printing Date: Tuesday, March 

Page 1 of 3 

Page 61 of 104 
Buster J2930203 

GLP10-01-02; interim Report 11 

Analysis of PFBS, PFHS. and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

I Sample Name; •bl10IO7a034- Sample 10: XCS-10123IM- Fae:-b1iO107a1.w 

I Peak Naire; -PFOS- Massiet): "JSa.OraS.O amu.499.0«0.0 amu.499.3.'130.0 ami 

I Corrmeni: •5ppb LCS' AnnotaUon' " 

1.14e6-

1.12e6-

1.10e«' 

1.0606 

i.oeo6' 

1.04«6 

1.02e6 

1.00*6 

I

Sample Name: •b110107a04r Sample ff):T.CS-!0i23O-i3- Fde. •b110107al.*ir 

Peak Name: TFOS' MassCes): '499IV99.0 amu,499.0)80.0 aim;.499.0/130.0 amu' 

Comment: 'Sppb LCS ECF" Annotation."" 

Enpect'^c RT : 

9.60eS 

9.40e5 

9.20e5-

9.00e5 

e.80aS 

B.e0e5 

8.40*5 

a.20c5 

aooos 

7.80e5 

r.COeS 

7.40*5 

7.20e5 

7.00*5 

3.B0e5 

6.60*5' 

5,40eS• 

6.20*5' 

S 6.00*5-

^ S.80e5-

I 5.G0eS' 

S.40e5-

5.20c5-

S.OOr.6-

4,80eS-

<.60e5' 

4.40*5 

4.20e5' 

4,00e5-

3.80*5 

3.60eS3.40*5' 

3.20e5' 

3.00e5' 

3.40eS 

2.20r6 

2.00*5 

I.80e5 

I.60e5 

V40e5 

1.20*5 

1.00*5 

a.00e* 

6.00*4 

4.00M 

2.00*4 

0.00 '!!=]L 

Printing Time: 2:58:15 PM 

Printing Date: Tuesday, March 

Page 2 of 3 

Page 62 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS. and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Buster J2930203 

I

Sample Name: *bll0107a092' Sample ID: •GW'0-OA.Ql-i 

Peak Name: *PFOS* Mass(e£): '^lES.CJSSi} amu.499.0/80.0 ai 

Cofrmeot:XAl GW 13^5 0101105' Annoaflon;" 

.k-ipU t 

I. ?«ah • 

2.2*5 

2.2e5 

2.1*5 

2.1e5 

2.0*5 

2.0e5 

i.9e5 

1.9e5 

1-8e5 

13e5 

1-7e5 

1.7*5 

1-6*5 

1.6*5 

1.5*5 

l.SeS 

1,465 

1.4e5 

13e5 

13*5 

1J?e5 

1.205 

1.1*5 

1.1*5 

1.0*5 

9.5*4 

9,0*4 

aie 4 

EOeA 

7.5*4 

7.0*4 

65*4 

6.0e4 

5.5*4 

5.0*4 

45*4 

4.0*4 

3.5e4 

3.0*4 

2.5e4 

2.0*4 

1.5*4 

1.0*4 

5000,0 

n n 

15.16 

15,0K 

V-*-- . . 

Printing Time: 2:53:15 PM 

Printing Date: Tuesday, March 

Page 5 of 

Page 63 Of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Fomrier Sludge Incorporation Area - November 2010 

Buster J2930203 Batch Name: bllOllOa.dab 

b1101 lOa.rdb (PFHS): "Quadratic" Regression ("1 / x" weighting); y = -7.03e-^003 x'^2 + 9.02e•^005 x •^ 6e-^003 (r = 0.9995) 

< 

4.0e7-

3,8e7-

3.6e7 -

3,4e7-

3,2e7-

3,0e7-

2,8e7' 

2.6e7-

2,4e7 -

2.2e7-

2.0e7-

1.8e7-

1.6e7-

1.4e7-

1,2e7-

1.0e7-

8.0e6-

6,0e6 -

4,0e6-

2.0e6-

0,0-

/ 

/ 

P 

/ 

/ jd 

/ 

/ 

/ / 

/ 

/ 

^ 

/ 

/ 

/ 

,„ 

,-''' 

y ' 

y 

/ • 

,^'' 

^y' ' 

.-•'— 

o 

_^ 

"'•'"-\. , 

v_/ 

\ ^ 

10 15 20 25 30 35 40 45 50 55 

Concentration, ng/mL 

60 65 70 75 80 85 90 95 100 

Printinq Time: 3:32:17 PM 

Printing D-3te: Tuesday, February 01, 2011 

Page 1 of 1 

Page 64 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Buster J2930203 Batch Name: bHOHOa,dab 

bl 10110a,rdb (PFBS): "Quadratic" Regression ("1 / x" weighting): y = -8.15e-^003 x*2 -^ 1.05e+006 x + 4,4e•^003 (r = 0.9996) 

4.8e7-

4.6e7-

4.4e7 -

4.2e7-

4.0e7-

3.8e7-

3.6e7-

3.4e7-

3,2e7-

3.0e7-

2.8e7-

2,6e7-

2.4e7-

2.2e7 -

2,0e7-

1.8e7-

1.6e7-

1,4e7-

1.2e7-

1.0e7-

8,0e6-

6,0e6 -

4.0e6 -

2,0e6 -

0,0-

/ 

•-

/ 

/ 

/ 

/ 

/ 

/ 

/ 

/ 

/ 

y ' 

y ' 

y 

y 

/ 

,y'' ' 

y ^ 

^,^' 

.••-—" 

o 

•—•-—. -

~'-^ 

^'-

^-v^ 

""^N 

v.^ 

\ ^ 

10 15 20 25 30 35 40 45 50 55 

Concentration, ng/mL 

60 65 70 75 80 85 90 95 100 

Prin 

Prin 

:ing Time: 3:31:56 PM 

ling Date: Tuesday, February 01, 2011 

Page 1 of 1 

Page 65 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Fonner Sludge Incorporation Area - November 2010 

Buster J2930203 Batch Name: bllOllOa.dab 

b110110a,rdb (PFOS): "Quadratic" Regression ("1 / x" weighting): y = -6,12e-^003 x'^2 -f 8.81e-^005 x + 1.98e•^004 (r = 0,9999) 

4,je / 

4.2e7-

4.0e7-

3.8e7-

3.6e7-

3.4e7-

3.2e7-

3.0e7-

2,8e7-

2,6e7-

2,4e7 -

2.2e7-

2.0e7-

1.8e7-

1,6e7-

1,487-

1.2e7-

1.0e7-

8.0e6-

6.0e6-

4,0e6-

2.0e6-

0.0-

/ • / 

/ 

/ 

/ 

/ 

/ 

/ 

/ 

y 

y 

y 

^ y ' 

, x ' 

y 

,.,-•••''' 

o 

"'~~---.„ ^ 

K j 

""•^•^ ^ 

"--, 

0 5 10 15 20 25 30 35 40 45 50 55 

Concentration. ng/mL 

60 65 70 75 80 85 90 95 100 

printing Time: 3;32:'!5 ?K 

Printing Date: Tuesday. February 01, 2011 

Page 1 of 1 

Page 66 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

i',ister J2930203 

I

SampteName:1,110il0aOi6' Satr^e 10--OSOOS-ISW F««:-b1t0110a-*«r 

PMk Nflir*:-PFBS- Massjes): •299,tM93.0 arrw.2a9.0«0.0 ajwjCommanI: *1.0 ngmi FC s!d n US O Wala,- Annotation " 

q . Dlti : 

L. ?vp.-: b 

/IJ.' / 

"'"": 

js.:' 

"Ir-

^ 4 

•jua.T -

:t; 

'"'. 

:',: 

Mwl l 

2.5*5 

2.5*5 

2.4*5 

2.4*5 

2J*S 

2.3*5 

2Ji*5 

2.2*5 

2.1*5 

2.1*5 

2-0*5 

2.0*6 

1.9*5 

1.9*5 

1.3*5-

1.8*5 

1.7*5 

Printi 

Print: 

ng Time: 3:C3:21 

ng Date: Tuesday, t-Jarch 2 3 

Sample Name: •bllOllOaOOr Sample tD: "Solxer-t Blanii JfAIlO Elemeni)- F»e:-b110110a.*nr 

Peak Name: 'PFeS' M3s*(esL •299.a'99.0 amu.299.0iW).0 amu" 

Comment 'MSt Q Water TNI 1-O308" Annotation:" 

Page ] of 

Page 67 Of 104 
Buste r J293020 3 

GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

w 

F *-

Peal 

hin< 

rr!<-h 

:nri 

c^ejL 

H•ig^ 

w^d-.^ 

B Tt 

?.;« 

I

Sample Nam*:-bllonOaOW Sample ID: TCS-101230-4' FBa: •bllOHOa.wr 

Peak Name: Tf=BS- Mass(es): '299.0n%.l3 amu,295.0*80.0 amu' 

CofT-menl: "SpplJ LCS' AnnoCalion-" 

1.24*6-

i.22«6 

1.20*6 

1.18e6 

1.1C*6 

1.14*6-

1.12B6 

i.iOeSi.oacfl1.06*6 

1.04*6-

1.02o6-

1.00*6-

9.e0e5 

9.60*5 

9.4De5' 

9.20*5-

9.00*5 

6.80*5-

8.60c5' 

S.40«5 

8.20*5-

9.00*5 

7.80*5-

7.6Qe5-

7,40e5 

7.20*5 

7.00*6 

3.80*5 

6.60e5 

; e.40oS 

o.20e5 

e.OOeS 

5.60*5 

S.eOaS 

5.40*5 

5,20e5 

5.00*5 

4.e0o5 

4.60*5 

4.40*5 

4.20*5' 

4.00e6 

3.60*5 

3.60*5 

3.40*5-

3.20*5-

3.00*5 

2.60*5-

2-60c6-

2.40*5 

2.20e5' 

2.00*6 

1.80*5-

1.60e5 

1.40*5 • 

1.20o5-

1.00*5-

a.00*4 

6.00*4 

4.00*4 

2.00*4-

0.00-

[ Sampl*ltome:t)110110a05r Sample ID:'GLP1O^)1-02-;i-O46' FSe-bllOilOa.wWr 

Peak Name; *PFeS' MaM(es): •299.0.'9S.O amu.299.0'80.0 

I CommenL'DAl. GW133R0 101102(dil 1:10)* Annotation:" 

:xpic',«a F.T.-

l6 18 20 

Printing Time: 3:03:21 PM 

Printing Date: Tuesday, March 2 9, 2 011 

Page 2 of 

Page 68 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Blister J2930203 

Sample Name:-bl 101108016- Sample ID'-08008-194-6' Fie: ti1iai10a.wi(r 

I

Peak Name: -pFHS" Mass{o»); •399.Q'9g.0 a-no.3S9.(y80il amu' 

Con-.inenl:'1.0r.9'mLFC«Id<--iM:SQkr;alar Annolatior-~ 

2.4e5 

2.3«5 

2.3a6 

2Je 5 

2.2*5 

2.1*5 

2.1*5 

2.0*5 

2.0*5 

Heigl;; : 

1.9*5-

1.ea5-

1.8e5 

1.7e5-

i.7e5 

1.6eS 

1.So5-

13e5-

15*5 

I.OeS 

9.5*4 

9,0*4 

8.5*4 

8.0*4 

7.5*4 

7,0*4 

6.5*4 

6,0*4 

5.5*4 

5^4 -

4.5*4-

4,0*4 

3.5*4 

3.0*4' 

2.5*4 • 

2.0*4 

13*4 

1.0*4 

5000X 

0.0-

,>A. 

I

Sample Nam*:-bl 101 lOaOOr Sample IO:'Sotrart Blank (MiniOEterrent)' Fle:*b11011i: 

Peak Name: 'PFHS' htessfei): •339.0''S9.0 amo,399.0/80i) amuCommenr -Ptsa Q Wrter TN11-0008" Annotation: -

iK-Jpat . Fac: 

I/I3,',-:JI /% -

N-

:.5C =-.!.-, 

O.CG .ips 

o"'^ "H i 

I.. : .i. , 

^'\^ i .-n 

zs 

1 

S 

2650 

2500 

2550 

2500 

2450 

2400 

2350 

2300 

2250 

2200 

2150 

2100 

2050 

20G0 

1950 

1900 

1850 

1800-

1750 

1700 

1650 

1SO0 

1550-

1500 

1460 

1400-

1350 

13C0 

1250-

1200-

1150-

1100-

1050-

1000 

Printing Time: 3:03:21 PM 

Printing Date: Tuesday, March 

Page 3 of 4 

Page 69 of 104 
GLP10-01-02: Interim Report 11 

Analysis of PFBS. PFHS. and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Suster J29302C3 

I

Sample Name: "bilOl 10JI034' Sample ID: XCS-10i23(M' FSe: "bllOHOa.Wifr 

Peak Name: -pFHS" tWass!**): "399.(^99.0 a?wi,3S9.a'80.0 amu" 

Corrmeni: "Sppb LCS" AnnoCalion- -

Jjcpi e In-ifx: 34 

ier-F'le !•,•?-: v^ 

:aici::iM«'i Co-c : H.M nrj'nL 

\=q. D.-it,t: 1/11,'?011 1,16*6 

1.14*6 

= r^r'"AliOtitV.r.: In.9Lii::uan - Hull ^-'^ ^ 

PEsk-JFllt. ?tc--ot: - 1,08o6-

^in . Peak i!«i=h;: C-.CC :p i 1.06e6-

li.i . i.*i>. Via-..-.: j.CC S4C 

3xot.;hit.^ •-i.jLh: •) pyii-;s 1.04«6' 

J!* S(lal.lv * ?.?t :ir. ^^^ ^ 

i:iTi. t-ypc: ''^^t'' ; 9.e0e5-

'.c^^.-. 5^64'-i; t-oi-niJ 9.60*5 

Star-.. lixf : l':-l J.i.i 9.40*5-

9.20*5 • 

g.OOeS 

S.S0*5 

8.60e5 

8.40e5-

8.20*5 

8.00*5-

7.80e5 

7.60e5-

7.40e5-

?.20c5 

/.00e5-

6.80*5 

3.60*5 

6.40*5 

« 6.20e5 

>. 6.00*5 

S S.80e5 

~ 5.60*5 

5.40e5 

5.20*5 

5.00*5 

4.80*5 

4.60*5 

4.40eS 

4.20*5 

4.00e5 

3-80e5 

3.60*5 

3.40e5 

3.20*5 

3.00e5 

2.80*5 

2.60*5 

2.40*5 

2.20*5 

2.00*5 

i.eoes 

1.60*5 

i.40eS1.20*5 

I.OOeS 

8.00*4 

5.00e4 

4.00*4 

2.00*4 

0.00-

FHe:"b110110».w!(r 

I Commwrt:"OALewi33K010l102(dal:10r Annotation:"' 

5.7*5 

5.6*5 

5-Se5 

5.4*5 

5.3*5 

6.2*5 

5.1*5 

S.Ce5 

4,9e5 

4,8*5 

4.7*5 

4,6*5 

4.5*5 

4.4*5 

4.3*6 

4.2*5 

4.1*5 

4,G«S 

3.9*5 

3.6*5 

3.7*5 

3.6*5 

3.5e5 

3.4*5 

3.3*5 

3.295 

3.1*5 

3.0*5 

2.8*5 

2.ee5 

2.7*5 

2.6*5 

2.5*5 

2.4eb 

2.3*5 

2.2*5 

2-1*5 

2.0*5 

1.9*5 

1.Be5 

1.7e5 

1.6e5 

1.Sc5 

1.4*5 

1.3«5 

1Je5 

1.1*5 

1.Ce5 

9,Ct>4 

8,0*4 

-.0** 

6.0*4 

5.0*4 

4,0e4 

3.Ce4 

2.0e4 

1.0*4 

0.0 

14 

14.03.., 

18 

1 

_ 1 -._ _ L12 14 1 . 6 18_ 20 

Printing Tine: 3:03:21 PM 

Printing Date: Tuesday, March 29, 20 

Page 4 cf 4 

Page 70 of 104 
Buster J2930203 

GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

I

Sample Name: "SI lOIIOaOie" SampI* ID' *D80O8-i94-8-

P«ak Kama: -pFOS' Masses): "'99.IV99J) 3mu.499.0/80J) a' 

Cofrm*nl:-1.0nflPiH. FCsaJiaMJIiQWalBf- An--vaallor--"" 

2.2e5 

2.2e6 

2.1e5 

2-1*5 

2.0a5 

2.0*5 

1.9*5 

1.9*6 

1-8«5' 

1.ae5 

1.7*5 

1.6e5' 

1-6e5 

1.5*5 

13*5' 

1-4e5 

1.4e5 

9.5*4-

9.0*4 

65*4 

8.0e4 

7.5*4 

T.OM 

6.5*4-

6-0*4-

5.5*4 

5.0*4 

4.5*4-

4 0fi4 

3.5*4 

3.0*4-

2.5*4-

ZXteA1.5*4-

1.0*4-

5000.0-

0.0 J&fV* 

I

Sample Nam*: "bl 101 lOaOOa" Sample 10: 'SolWM BUn< [MiH^ EiorP*nt)- Fie: til 10110a.*ir 

Peak Nam*: •PFOS" Mas»(*S): •499JJ.'99,0 amu.49S.aB0.0 amo.499.0/130.0 am*." 

Comment: "MS: Q Water TNI 1-<KI08- Anno!3lkxi:" 

Exoftc'.ea F.T: 

PetB.-.iion ria--

Printing Time: 3:04:17 PM 

Printing Date: Tuesday, March 

1.9*4 

1.6*4 

1.8*4 

1.7*4 

1.7e4 

1.6*4 

1.5*4 

l - ^ 

1.5*4 

1.4*4 

1.4e4 

1.3*1 

1.3*4 

1^*4 

l,2n4 

1.1*4 

1.1*4 

1.0*4 

§ 

? 9500,0 

» ^ 9000.0 

asoco 

80O0.O 

7500.0 

7000.0 

6S0C.0 

6000.0 

5500.0 

5OOC.0 

4500.0 

4000.0 

3500.0 

300C.0 

250C.O 

2000.0 

1500 0 

100C.0 

500.0 

0.0 

i 1 . :i i ,. 1 ,, _ _^^i 

., .1 ^ 1-1.-1^^ i...-1-. . *tj y I 

; * ^ ,- , , . Lj. .1 J_ . Jl i •.. 

< V I JJfci^^,itn*>, .^IIMM 

,1 

.-i^MiivJit 

1 

k^ • "nrf^ii.uu , 10 12 16 16 20 

Page 1 of 3 

Page 71 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS. PFHS. and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

[Sampte Name: "bl 10110a034- Sample ID: TCS-10123fr4" 

Peak Kama: -PFOS" Masstesl: "499.0/991) amo,493 OfflO.0 ai 

t Cw"nen!:-Sppb LCS" Annotation-•" 

1.16*6' 

1.14*6-

1.12*6 

1.10*6 

i.0Se6' 

1.06*6-

1.<>**6 

1.02*6 

1,00*6 

9.80e5' 

3.60*5 

9.40*5 

9.20*5-

9.00e5-

8.80*5 

8.60*5 

8.40*5-

8.20*5-

8.00*5 

7.80eS 

7,60*5-

7.40e5-

7.20*5-

7.00*5 

6.60*5-

6.60*5-

6.40*5-

I 6.20e5 

^ 6.00*5-

I 5.60*5-

5.60c5-

5.40*5 

5.20*6-

5.00*5-

4,80e5-

4.60*5-

4.40*5-

4.20e5-

4,00*5-

3,80*5-

160*5 

3.40*5-

3.20*5-

3.00*5-

2.SOe5' 

2.60e5-

2.40*5-

2.20e5-

2.00e5 

1.80c*-

1.60e5-

I.40e5-

I.20e5-

1.00c6-

8.00*4-

6.00*4-

4.00M2.00*4 • 

0.00-

I

SampleName:"b'!l0110a04r Sample !D: 105-101230-13- Fil*:-b110110a.wi(r 

Peak Name: "PFOS- M3U(*3): "499.0.'S9.0 amu.49S.Q(SO.O amu.499.0/130.' 

Comm*ni: *5ppb LCS FCP Anooiatioo:" 

12 14 16 16 20 

Printing Time: 3:04:17 PM 

Printing Date: Tuesday, March 29, 

Page 2 of 3 

Page 72 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Fonner Sludge Incorporation Area - November 2010 

Buster J29302C3 

Princinq Time: 3:04:17 PM 

Printing Date: Tuesday, t-jarch 29, 

Page 3 of 3 

Page 73 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Buster J2930203 Batch Name: bllOll'ia .dab 

bllOl 14a,rdb (PFHS); "Quadratic" Regression ("1 /x" weighting): y = -6,64e-^003 x'^2 -i- 8.6e-t-005 x + 3.29e-^003 (r = 0.9997) 

i2 

c 3 

8 

a 

< 

4.0e7-

3.8e7-

3.6e7-

3.4e7-

3.2e7-

3.0e7-

2.8e7-

2.6e7-

2,4e7-

2.2e7 -

2,0e7 -

1,8e7-

1.6e7-

1.4e7-

1.2e7-

1.0e7-

a.OeS6.0e6-

4.0e6-

2.0e6-

0.0- / 

/ 

P 

/ 

/ / 

/ 

/ 

/ 

/ / 

^y"^ 

^ y ' 

y ' 

y 

y ^ 

y 

..---'" 

-•--"" 

'"\. . 

O 

^ 

^\.,^ 

'\ 

\ 

10 15 20 25 30 35 40 45 50 55 

Concentration, ng/mL 

60 65 70 75 80 85 90 95 100 

Printing Time: 9:06:13 AM 

Printing Date: Wednesday, February 02, 2011 

Page 1 of 1 

Page 74 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Fonner Sludge Incorporation Area - November 2010 

Buster J2930203 Batch Name: bllOll'Sa.dab 

b110114a.rdb (PFBS): "Quadratic" Regression ("1 / x" weighting): y = -7,54e-^003 x'^2 + 9,96e•^005 x + 5.76e-^003 (r = 0.9996) 

t,/e / 

4,6e7 -

4.4e7-

4.2e7-

4.0e7-

3.8e7-

3.6e7 -

3.487 -

3.2e7-

3,0e7-

2,8e7-

2.6e7-

2.4e7-

2.2e7-

2.0e7-

1.8e7-

1.6e7-

1.4e7-

1.2e7-

1.0e7-

8.0e6-

6.0e6-

4.0e6 • 

2.0e6-

0.0-

/ 

/ 

/ 

/ 

• 

/ 

/ / 

/ 

/ 

y 

/ 

/ / 

y'' ' 

^ y 

/ / 

.* 

-•' ' 

.,---''' 

o 

''"•-,- , 

•^- , 

o 

""^^^ 

X 

10 15 20 25 30 35 40 45 50 55 

Concentration, ng/mL 

60 65 70 75 80 85 90 95 100 

'.-rin-

?rin 

ling Time: 9:05:51 AM 

.ing Date: Wednesday, February 02, 2011 

Page 1 of 1 

Page 75 Of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Fornier Sludge Incorporation Area - November 2010 

Buster J2930203 Batch Naine: bllOll'Sa.dab 

bl 10114a.rdb (PFOS): "Quadratic" Regression ("1 / x" weighting): y = -5.57e-^003 x*2 + 8.19e-^005 x + 5.51e-^004 (r = 1,0000) 

*2 

8 

CO 

< 

4.0e7 

3.8e7 

3,6e7 

3.4e7-

3,2e7-

3.0e7-

2.8e7~ 

2.6e7-

2.4e7-

2.2e7-

2.0e7 -

1.867-

1.6e7-

1.4e7-

1.2e7-

1.0e7-

8.0e6 -

e.OeS4.0e6-

2.0e6-

0.0-

/ 

9 

/ 

/ 

/ 

/ 

/ 

/ 

/ 

/ / 

„.-

X 

y 

y 

y 

,,-«'' ' 

.,.^'' 

,.'"'' 

o 

"" 

o 

••---... ^ 

" " • 

10 15 20 25 30 35 40 45 50 55 

Concentration, ng/mL 

60 65 70 75 80 85 90 95 100 

Printing Time: 9:06:33 AK 

Printing Date: Wednesday, February 02, 2011 

Page 1 of 1 

Page 76 of 104 
Buster J2930203 

GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

I

Sample Nam*: ti l 10114a016- Sample ID: "08008-194-6' 

Peak Narr^e: "Pf BS- Mass(Bsl: -299.0/99.0 amu,299.0/SO,0 

Corrment: -1.0 og/mL FC std i-i MS Q WaWr" Annotation-"" 

23tS 

23*5 

2.2*5 

2.2*5 

2.1*5 

2.1*5 

2.0e5 

2.0*5 

1.9e5 

? 

1" 

1.7*5 

1.7*5 

1.6*5 

1.6eS 

1.5*5 

1.5*5 

1.4*5 

1/4*5 

1.3e5 

1.3eS 

1J!e5 

1.2*5 

1.0*5 

9.5*4-

9.0*4 

8.5e4 

e.0e4 

7.5*4-

7.0*4-

6.5*4-

6.0e4' 

5.5*4-

5i>e4 

4.5*4-

4J}e4-

3.5*4 

3.0*4 

2.5*4-

2.0*4 

13*4 

IJM -

5000.0-

0.0- U i ^ 

I

SamptaNaina:liliai14a0a8- Sample ID.'Sotver^tBlamt {MdlKD E)e[r.*nt}' Fl*:-b110114a.<wr 

Peak Name: "PFBS" Masses): •299.0.'9S.O aniii.299-0W.0 amu' 

Comment "M3t: Q Wa!e' TNI 1-0008" Annoialion: 

Printing Tine: 3:Cb:C3 PM 

Pri.nting Date: Tuesday, March 

Page 1 of 

25, 

Page 77 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Fonner Sludge Incorporation Area - November 2010 

ii.-5ter J293020 3 

SampteName:-bll0114a05r Sample iO;-Gt.PHWll.02-: 

Peak Nanw:-PFBS- Maaa(es):-299.a'9e.0 ainu.299.0'SO.O «r 

Comfnenl:-DALGW-.34L010110S{(tlT10r Areiolallon'-

Printing Time: 

Printing Date: 

3:06:03 PM 

Tuesday, March 

..... .-: ..^IfSu^.^.j^^l'^i.fi^.^.^.^jM^ Vii,rt,iftiiPage 2 of 4 

Page 78 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Fornier Sludge incorporation Area - November 2010 

Buster J2930203 

IT Sample Name: "blIOIMBOIS" Sample ID: -0800«-194.«" 

Peak hame: "PFHS' Mass;«»): •399.a'99,0 a.'nu,3fi9.C«0.0. 

ConTnanl: *1.0 ngfirL FC eld in M:S Q Watar" An-iotallon- I

Sample Name: "bl 101 MaOOS' Sample ID: 'Solvert Blani^ {MUS^Q Elerr«nt)' Fie: "b110114a.Mfr 

Peak Name: "PFHS" MaM(*s]: -399.o;99.0 amu.399.0/80.0 amu* 

Comn>*ni:"Min:QWBt*rTN11-0008' Annotation:" 

y.od.ii^t : 

Fro: . Aioarithn : 

.V=ise Ferc-nr.,gB 

Ki^- r« k UBign-, 

ill^.t't' xtd^V 

Rl i>i.r.do.ff-ap^c'.*.•'. r:T : 

Peten-aor: rln-a: 

K*i(ihL: 

Frd Tint ; 

11:^1 

NO 

inufi 

:;: 

3 D . 

No 

6ds« 

1< 

: ; 5 *;i 

9 0 

o.c-cc.c-e 

J .= rtC 

m i 

. 2 pii n 

. 2 Bi n 

.•nL 

^ 

ll'.r. J 

3300 

3250 

3200 

3150 

3100 

3050 

3000 

2950 

2900 

2850 

2B00 

2750 

2700 

2S50 

2600 

2550 

2500 

2450 

2400 

2350 

2300 

22S0 

2200 

2150 

2100 

2050 

2000 

1950 

1900 

1650 

1800 

1750 

1700 

iiao 

Printing Time: 3:06:03 PM 

Printing Date: Tuesday, Marc:n 

Page 3 of 4 

29, 2011 

Page 79 of 104 
Buster J2930203 

GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

I

Sample Name: "bllO! 14a034' Sample ID' T.CS-1012JO^- Fte: "bllOIUa.wr 

Peak Name: "Pf HS" M3s»(e»): "399.0.'99.0 3.110,399,0/80.0 amu" 

Cofrnient: "Sppb LCS" Annotation-" 

i:2» : >S ^M 

1.14e6 

1.12*6 

1.10*6 

1.08e6 

1.06e6 

1.04*6 

1.02e«' 

i.00e€ 

9.80*5 

g.GOeS 

9.40*5 

9.20*5 

9.00*5 

e.80e5 

B.60e5' 

e.40e5 

8.20*5 

6.00*5 

7.60*5 

7.60*6 

7.40*5 

f.20*5 

7.00*5 

S.80a5 

3.60*5 • 

5.40e5 

6.20e5 

• d.oOeS-

- S.80eS5.60*5 

5.-<0e5-

5.20e5 

5.00*5 

4.S0eS' 

4.60e5 

4.40*5 

4.20*5 

4.00*5 

3.80e5 

3.60*5 

3,40*5-

3.20*5 

3.00*5-

2.S0e5' 

2.60*5-

2.40*5-

2.20*5-

2.00*5 

1.80*5 

i.eoes 

1.40*5-

1.20*5-

1.00*5-

8.00*4-

6.00*4-

4.00*»-

2.00*4-

0.00-

[

Sample Name; "bl I0ll4a0sr Sample !D: "GLPI0-01-02-1 

Peak Name: "PFHS" Mais{e»): "399.0''S9.0 amu.399.0/8D.O 

CWnmenI: "DAI. GW 134L 0 101105 (da I -lOf Annotallor- ^ 

^ne : 

- c : 

.^ic = rlt.ho : 

.'iiiti. ••.-indo 

p-it . Fac-

«sk. fl»iri.i' 

'.r.q Hldch: 

is'.iv e RT: 

ri.Tie: 

<:3J:,; ? A4 

V,., 

IiisL^lliWua,-- -

'JO 

a^; [ly 

O-CC 

0 

i«.Z .,r. 

ajs e To Bif.s 

K . Z Bin 

.S7t-i5 5 cp^ 

13. i .nio 

• 3 

'o-- -

3.8e5 

3.7*5 

3.6*5 

3.5eS 

3.4*5 

3.3*5 

3.2aS 

3.ie5 

a.OeS 

2.9e5 

2Je 5 

2.7e5 

2.6e5 

2.5e5 

Printing Time: 3:06:03 PM 

Printing Date: Tuesday, March 29, 

Page 4 o f A 

Page 80 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Ete r J293020 3 

I

Sample Name: ^110114a0l6" Sample 10: -08008-194-8-

Peak Name: -PFOS' MasM**); '469.0/99.0 amu.499.0/80.0 w 

Conmenl: "1.0 ng/ml. FC sld in Mffi Q Water' AmotaUoP' " 

2.2*5-

2.1*5 

2.1e5-

2.0*5-

2.0*5 

1.9*5 

1.9eS 

1.8*5 

1.8*5 

1.7*5 

1.7*5 

1.6*5 

1.6eS 

1.5e5 

15e5 

1.4*5 

1.4*5-

1Je5 

1.3*5-

1.2e5-

1.2e5 

1.1*5-

1.1*5-

1.0*5 

9.5*4-

9.0*4-

8.5*4 

8.0*4 

7.5*4-

7.0*4 

6.5*4-

6.0*4-

5.5*4-

5.0*4 

4.5*4-

4.0*4-

35*4-

3.0*4-

23*4 

2.0*4 

1.5*4 

1.0*4 

5000.0 

0.0-

Printinq Time; 3:06:58 PM 

Printing Date: Tuesday, March 

(

Sample Name: "bllO! 14a00a' Sample 10: "Solvent man^t {MiltiO Elerr.enl)' FUe: "bl I0114a.>vrfr 

Peak Kama: "PFOS" Mass(e3j: "499i>''g9.0 amu.49S.0iS0.0 amu.499.0/130.0 amu" 

Comment: "MJl Q Water TN11 -0008" Annotation: ~ 

3J©4 

32e4 

3.2*4 

3.ie4 

3.1*4 

3.0*4 

3.0*4 

2.9*4 

2-9*4 

2-ee4 

2.8*4 

2.7*4 

2,7e4 

2.6*4 

2.5*4 

2.Se4 

2i64 

2.4*4 

2.4*« 

2.3*4 

2.3*4 

2i* 4 

2.2*4 

2.1*4 

2.1*4 

2.0*4 

2.0*4 

1.9*4 

1.9*4 

1.6*4 

1.8*4 

!.7*4 

I.7e4 

t.6*4 

1.6*4 

1.5*4 

i.Se4 

1.4*4 

1.4*4 

1.304 

13*4 

1.2*4 

1Je4 

1.1*4 

1.1*4 

1.0*4 

950C.0 

9000.0 

8500.0 

8000.0 

7500.0 

7000.0 

6S0C.0 

600C.O 

550C.0 

500C.0 

4500.0 

4000.0 

35O0.O 

3000,0 

:soc.o 

2000.0 

1500.0 

lOOCO 

50C.0 

0.0 ...^.....U . ^ , ^.^.....^.^^ ^ ....^L,U,t»I.^^M" * 

15 24 

j j 

4, 

T* **fty*t*>t*i<d*i..... 

16 18 20 

Page 1 of J 

Page 81 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS. PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

3ii5te r J293020 3 

I

Sample Name: "bl 10114a034" Sample ID: •LCS-101230-*" 

Peak Kame; TTOS" Massies), "499,W99.0 amu.493,0«0.0 ai 

Comment: "Sppb LCS" Annoialion-" 

Conctr.^iaticr.; * . 5" .-1.,,'nl, 1.12*6 

1.10*6 

1.08*6 

1.06*e 

1,04*6 

I.02e6 

1.00*6 

••* 9.80*5 

9.60*5 

9.40*5 

9.20*5 

9.00*5 • 

8.80*5 • 

B,60e5 

S.40«5 

8.20*5 

BOOcS 

7.60e5 

7.60*5 

7.40e5 

7.20*5 

7.00*5 

G.C0e5 

6.60eS 

3.40*5 

6.20*5 

6.00*5 

§- 5.80*5 

I" 5,60e5 

£ 5,40*5-

5.20e5-

5.00e5 

4.80*5 

4.80*5' 

4.40*5-

4,?0e5 

4.00e5 

3.eOe5-

3.60*5 

3.40«S 

3.20e5 

3.00*5 

2.eae5 

2.60*5 

2.40*5 

2.20*5 

2.00*5 

1.80*5 

1.60B5' 

1.40*6 

1.20*5 

1,00*5 

8.00e4 

8.00*4 

4.00^ 

2.00*4 

0.00 

I SamBteName:'bl10114aO4r Sample ID: "LCS-10i230-ir Fil*:"b1I0n4a.w«r 

15.0&.^ 

Printing Time: 

Printina Date: 

:0t;:58 PM 

uesday, March 

Page 2 of 3 

Page 82 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundw/ater 

Former Sludge Incorporation Area - November 2010 

Buster J2930203 

Printing Tine: 

Printina Date: 

3:06:5 8 PM 

Tuesday , Marc:n 29 , 2011 

Page 3 cf 3 

Page 83 of 104 
Ginger AG01330509 

GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Results Name: gll0211a.rdb 

g11021 la.rdb (PFBS): "Quadratic" Regression ("1 / x" weighting): y = -3.35e-*-003 x'*2 + 6.88e-^005 x + 3.41e•^003 (r = 0.9997) 

2.7e7-

2.6e7-

2.5e7-

2.4e7-

2.3e7-

2.2e7-

2.1e7-

2.0e7 

1.9e7 

1.8e7-

1.7e7-

1.6e7-

1.5e7-

1.4e7-

1.3e7-

1.2e7n 

1.1e7 

1.0e7-

9.0e6-

8.0e6-

7.0e6-

6.0e6-

5.0e6-

4.0e6-

3.0e6-

2.0e6-

i.oee0.0- ^ • ^ 

y 

9^ / 

y 

y 

y 

y 

y 

y 

y 

y 

y 

y 

,y 

/ 

y ' 

y 

y 

' " 

y 

y ' 

y ^ 

y ' 

,,, 

, y 

^ y 

y"' ' 

y " 

y d 

y ' ^ 

X 

,.'-' 

.,.'''' 

y ' 

,..--'" 

.^ 

...--'-"'" 

....-'' 

^-"" 

_..• • 

10 12 14 16 18 20 22 24 26 28 

Concentration, ng/mU 

30 32 34 36 38 40 42 44 46 48 50 

Prir 

Prir 

tin g Tine: 3:16:33 PM 

ting Date: Tuesday, Marc:n 29, 20 

Page 1 of 1 

Page 84 of 104 
Ginger AG01330509 

GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundw/ater 

Former Sludge Incorporation Area - November 2010 

Results Name: gll0211a.rdb 

• g11021 la.rdb (PFOS): "Quadratic" Regression ("1 / x" weighting): y = -1.24e•^004 x'^2 + 1.76e-t-006 x + 8.61e-f003 (r = 0.9998) 

5.9e7 i 

5.8e7-

5.6e7-

5.4e7-

5.2e7 -

5.0e7-

4.8e7-

4.6e7 -

4.4e7-

4.2e7 -

4.0e7-

3.8e7 

3.6e7-

3.4e7 -

3.2e7-

1 3.0e7-

8 

CO- 2.8e7 

< 2.6e7 

2.4e7-

2.2e7 

2.0e7-

1.8e7 

1.6e7-

1.4e7 

1.2e7-

1.0e7-

8.0e6 

e.OeS4.0e6-

2.0e6-

0.0-

..-'' 

.,-''' 

,^' 

y ' ^ 

,•' ' 

y 

y 

y 

y 

y'^ 

y 

y 

y 

y 

y 

/ < 

y 

y 

y 

/ 

/ 

/ 

m' 

• 

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 

Concentration, ng/mL 

34 36 

,y' ' 

38 

.^--""' 

40 

.,--" 

42 

„...-' 

44 

,..--''" 

46 48 

_^.m 

50 

Printing Time: 3:16:58 PM 

Printing Date: Tuesday, t-Iarc:n 29, 20 

Page 1 of 1 

Page 85 of 104 
Ginger AG0i330509 

GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Results Name: gll0211a.rdb 

I

Sample Name:'gllO211a0i9- SampI* ID: •10007-27-e' Fll«:"g1102t1a.witr 

Peak Name: T f BS" Massfes): •299.0«9.0 amu,29S.QfB0,0 amu" 

Cofnm*nt: 1J3 ng/ml. FC sld in hl:lf Q water" Annotation- ' 

:Ur.p;e Ir.fjer.-

% 

1.6*5 

1.6*5 

1.5*5 

1.Se5 

1.4*5 

1.4e5 

1.3*5 

1,3e5 

U « 5 

1.2*5 

l.leS 

1.1*5 

1.0eS 

95*4 

9.0e4 

8.5»4 

8.0*4 

7.5*4 

7.0*4 

65*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 

2.0*4 

1.5*4 

1.0*4 

SDOO.O 

0.0 

10 

- It .- ,-.. - -.-. .-..- ^-. 

59 

k. ,--,_ 

Pri.nting Time: 3:14:55 PM 

Printing Date: T-jesday, March 29, 2011 

5 6 7 8 9 10 11 12 13 14 15 16 

^ rBn*.ipfn^ _ II I 

I Samplo Name:-91102113011' Sample ID:"Solvert Blani<" Fiki:"g110211a.*ifr 

Peak Name: "PFBS' Hassles): •299.0«9.0amu.299.0i80.0amuI Comment'Ml^QWEdeiTNII-OOSr Annotation:-

i««k HBigh; 

Page 1 of 2 

Page 86 of 104 
Ginger AGOi330509 

GLP10-01-02; Interim Reportll 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Results Name: gll0211a.rdb 

I SampleName:-Bl10211a032' SamptelD:1.CS-110210-4" FUe:'gl 1021 la.wifT 

Peak Name: T>FBS- Mas4<as); "299.0/99.0 Bmu.299.0i80.0 amu" 

I Conrnenl: "Sppb LCS' Annotation-" 

SampI* Name; "gnoaiialOS* SaniplolO:"GLP1<W)l-02-! 1-134' Fte--g110211a.w!fr 

Peak Name: TrBS' Mass(«t}: '299.a-9S.0 aniu.299.a'80.0 amu" 

Comm*nf DAl,CW'!41R0 101110" AnnolaUon:-

5 6 7 8 9 10 11 12 13 14 15 16 17 

^/itL 

Li.-. 

1 

7400 

7200 

7000 

6BO0 

6500 

6400 

6200 

5000 

5800 

5600 

5400 

5200 

5000 

4800 

4600 

4400 

4200 

4000 

3800 

3600 

3400 

3»0 

3000 

2S00 

2600 

34O0 

2200 

2000 

1900 

1600 

1400 

1200 

1000 

BOO 

600 

400 

200 

0 

i \ k. *.4- •i..L,. -,-iJ -u.^ J ^ ^•^^ 

j t h 

'J^y'' ^»^>%,^^m^\ 

15 16 17 

Printing Tine: 3:14:55 PM 

Printing Date: Tuesday, March 29, 

Page 2 of 2 

Page 87 of 104 
Ginge r AGO 

GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Results Name: gll0211a.rdb 

(

SamploNanw g 0211aO 9 Sample ID:-10007-27-8" RIe;-g110211a.vntr 

PaakNan-e PFOS Masses) a99C/990amu.499.0/80.0amu.499.0/13D.Oamt 

Con-„ien C ng,TU F s d MISQ wale,- AnnotatJor' ~ 

4.2*5 

4.1eS 

4i)65 

3.965 

3.ae5 

3.7e5 

3.6*5 

3.5e5 

3.4*6 

3.3*5 

3.2*5 

3.1*5 

3.0*5 

2.9*5 

2.6*5 

2.7*5 

2.6*5 

2.5*5 

2.4*5 

2.3*5 

2.2*5 

2.1e5 

2.0*5 

1.9*5 

1.6*5 

1.7*5 

1.6e5 

1.Se5 

1.4*5 

1.3*5 

U e S 

1.1*5-

1.0*5-

SJ>s4 

6.0*4 

7.0*4 

6.0*4 

5.0*4 

4.0*4 

3.0*4' 

2.0*4-

1.0*4-

no 

12 

, 

39 

L^>- V : 

12 13 14 15 

(

Sample Name: "gl 1021 laOII" Sample ID:'Solvent Kank" File: "011021 la.wirT 

Peak Name; "PFOS' Mass{esj: •499.0<'99.0 amo.49S.Q/e0.0 amo.499.0/130.0 amL" 

Comment; "Mifl: Q Water TNI l-005r Annotation: "• 

Eziiio'.ed RI: 

54O0 

5200 

5000 

48DD 

4600 

4400 

4200 

4000 

3800 

3800 

34O0 

3200-

3000 

2800 

2600 

1200 

1C00 

i 

It 

^.4ik4 i ii^...,aijXtfi4-*U>,.ifl^,>^ji.uiti^Jta^JvJi^ 

i/ 

2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 

Printing Time: 3:15:57 PM 

Printing Date: Tuesday, t-5arc.h 29, 2011 

Page 1 of 3 

Page 88 of 104 
Ginger AG01330509 

GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Results Name: gll0211a.rdb 

I

Sampt* Name: "9110211*032" Sa*npl* ID: \CS-110210-4" 

Peak N«re: "PFOS' Ua»»(*»»: '-isg.twgjj 8rw.499.0«O.D a^ 

CoRvnenI: *Sf>pt> LCS" Anniatation: " 

*ir.i.ie iRripx: 32 

ar'E.le T-,-?-; : UC 

oncc-r.v:»tic.:i: * . 96 n^/nl, 2.2e6 

aiculotB'i Co-c: 5.43 aj/aL 

-q . Dit.!.- 2/l?.'iO: i „^ , 

.:.!. TiiiE; *:l<:i? - ».!1 

edified : No 2.1e6 

f=c . Aliciir..^.n: Inv«iii5iia n - Mui I 

o n e .i-ei-.-^.-itrtSe: 5u 2.1e6 

•,is.j. Sub. Wir.dow: i-eP ni.-i 

•in. ?«ak:ieich; : O.CC -pa 

;in. p»i»L Widtf-.; O.CC sa c 2.0*6 

.ROoit-.ir>g siidTL^,: J poii-zs 

•xp.it'^o'RT: 1?.4 sVSi '^'^^ 

13* Ruiatlve ?.T: Mo 

1.9*6 

!it.. Type; Villiiy 

-lar.tlar. Tlne^ ^ i:.4^^^s.ir, , g ^ 

eigfi;: i:CO-30-3. cc» 

i-arv Ti.T*: i:.? ii:i 1-8*6 

1.7*6-

1.7oe 

1.6*6-

1.6e6 

1.4*6 

1.4*6 

lJe 6 

1J*6 

1.2*6-

1.2*6 

1.1*6 

1.1*6 

1.0*6 

9.5*5-

9.0e5 

6.5*5 

6.5*5 

6.0*5 

55e5 

S.OeS 

45e5-

4.0*5 

33*5 

3.0*5 

2,5*5 

2.0*5 

15*5 

1.0*5 

S.0e4 

10 11 12 13 

I SampleName:"gn0211»04r SamplelD:XCS-110210-i3' FS*:-fll102l1a.ynfr 

Printing Tine: 3:15:57 PM 

Printing Date: Tuesday, t-Jarch 25, 2011 

Page 2 cf 3 

Page 89 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

Results Name: gll0211a.rdb 

Page 3 of 3 

Page 90 of 104 

Ginger AG0i330509 

I SampleNam«;-gH0211a096- SarM" ID:-GLPiO4)1-02-11-0W Flte;-g1102!la.w«-

5.1*5 

5.0*5 

4.9*5 

4.SeS 

4.7*5 

4£e5 

45e5 

4.4e5 

4.3e5 

4.2*5 

4.1*5 

4.0*5 

3.9*5 

3.8*5 

3.7*5 

3.6*5 

.1.5*5 

3.4*5 

3.3eS 

3.2*5 

3.1*5 

3.0e5 

2.9e5 

2.8*5 

2.7*5 

2.6*5 

2.5*5 

2.4*5 

2.3*5 

2.3*5 

2.1*5 

2.0*5 

1.9e5 

1.6*5 

1.7e5 

1.6eS 

1.5eS 

1.4e5 

1.3e5 

1.2a5 

1.1o5 

lOeS 

9.0e4 

8.0*4 

7.0*4 

6.0*4 

5.0*4 

4.0*4 

3.0*4 

2.0*4 

1.0*4 

12.17.. 

Printin g Time: 3:15:58 PM 

Printin g Date: Tuesday, March 29, 2011 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

ATTACHMENT C: ANALYTICAL METHOD 

Page 91 of 104 
GLP10-01-02;Jnterim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

3M Enviranmental Laboraloiy 

Method 

Method of Analysis for the Determination of Perfiuorinated Compounds in Water 

by LC/MS/MS; Direct Injection Analysis 

Method Number: ETS-8-044.0 

Adoption Date: Upon Signing 

Effective Date: Q ^1( 1 ( o "1 

Approved By: 

^//j/a y 

William K. Reagen, Laboratory Manager Date 

ETS-8-044.0 Page 1 of 11 

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

Injection Analysis Page 92 of 104 
GLP10-01-02: Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

1 Scope and Application 

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

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

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

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

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

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

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

Perfiuorinated 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 perfomnance-based method. Method accuracy is detennined for each sample set using multiple 

laboratory control spikes at multiple concentrations. This method also requires that the precision and 

accuracy for each sample be detennined using field matrix spikes to verify that the method is applicable to 

each sample matrix. Sample results for spikes outside of 70% to 130%, may be flagged as such (with 

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

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

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

accuracy for analytical results. 

3 Definitions 

3.1 Calibration Standard 

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

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

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

concentration. 

3.2 Laboratory Duplicate Sample (LDS, or Lab Dup) 

A laboratory duplicate sample is a separate aliquot of a sample taken in the analytical laboratory that is 

analyzed separately with identical procedures. Analysis of LDSs compared to that of the first aliquot give 

a measure of the precision associated with laboratory procedures, but not with sample collection, 

preservation, or storage procedures. 

3.3 Field Blank (FB)/Trip Blank 

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

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

preservation and all analytical procedures. The purpose of the FB is to detemnine 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 Perfiuorinated Compounds in Water by LC/MS/MS; Direct 

Injection Analysis 

Page 93 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

3.4 Field Duplicate Sample (FDS, Field Dup) 

A sample collected in duplicate at the same time from the same location as the sample. The FDS is 

handled under identical circumstances and treated exactly the same throughout field and laboratory 

procedures. Analysis of the FDS compared to that of the first sample gives a measure of the precision 

associated with sample collection, preservation and storage, as well as with laboratory procedures. 

3.5 Field Matrix Spike (FMS) 

A sample to which known quantities of the target analytes are added to the sample bottle in the laboratory 

before the bottles are sent to the field for collection of aqueous samples. A known, specific volume of 

sample must be added to the sample container without rinsing. This may be accomplished by making a 

"fill to this level" line on the outside of the sample container. The FMS should be spiked between 

approximately 50% and 10 times the expected analyte concentration in the sample. If the expected range 

of analyte concentrations is unknown, multiple spikes at varying levels may be prepared to increase the 

likelihood that a spike at an appropriate level is made. The FMS is analyzed to ascertain if any matrix 

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

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

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

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

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

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

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

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

3.7 Laboratory Control Sample (LCS) 

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

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

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

exactly like a laboratory sample to detemiine 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 detemnine whether the sample 

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

sample matrix must be detennined in a separate aliquot and the measured values in the LMS corrected 

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

3.9 Laboratory Sample 

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

3.10 Limit of Quantitation (LOQ) 

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

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

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

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

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

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

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

ETS-8-044.0 Page 3 of 11 

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Injection Analysis 

Page 94 of 104 
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Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

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 detemiine if test substances or other interferences are present in the laboratory 

environment, the reagents, or the apparatus. 

3.12 Sample 

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

material. 

3.13 Stock Standard Solution (SSS) 

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

compound. 

3.14 Surrogate 

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

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

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

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

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

quality control measure and is NOT required. 

3.15 Working Standard (WS) 

A solution of several analytes prepared in the laboratory from SSSs and diluted as needed to prepare 

calibration standards and other required analyte solutions. 

4 Warnings and Cautions 

4.1 Health and Safety 

The acute and chronic toxicity of the standards for this method have not been precisely determined; 

however, each should be treated as a potential health hazard. The analyst should wear gloves, a lab 

coat, and safety glasses to prevent exposure to chemicals that might be present. 

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

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

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

4.2 Cautions 

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

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

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

5 Interferences 

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

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

conditions of analysis by running method blanks. 

ETS-8-044.0 Page 4 of 11 

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

Injection Analysis 

Page 95 of 104 
GLP10-01-02; Interim Report 11 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

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

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

caps, autovial caps, HPLC parts, etc. 

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

calibration standards and matrix spikes. 

6 Instrumentation, Supplies, and Equipment 

6.1 Instrumentation and Equipment 

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

variable volume injector capable of injecting 5-100 pL 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, 25pL, 50pL, lOOpL, 250pL, 500|JL, lOOOpL. 

1 mL plastic HPLC autovial. 

Disposable pipettes, polypropylene or glass as appropriate 

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

6.2 Chromatographic System 

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

Analytical Column: Betasil CI 8, 4.6 mm x 100 mm, 5 pm 

Temperature: 10°C 

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

Mobile Phase (B): Methanol 

Gradient Program: 

Time (min) 

0.0 

0.5 

11.0 

13.5 

13.6 

17.0 

%A 

97 

97 

5 

5 

97 

97 

%B 

3 

3 

95 

95 

3 

3 

Flow Rate 

(mL/min) 

1.0 

1.0 

1.0 

1.0 

1.0 

1.0 

Injection Volume: 100 pL. 

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

Run Time: ~ 17 minutes. 

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

provided that data quality objectives are met. 

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Injection Analysis 

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Analysis of PFBS, PFHS, and PFOS in Groundwater 

Fornier Sludge Incorporation Area - November 2010 

6.3 MS/MS System 

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

Analyte 

PFBA 

PFPeA 

PFHA 

PFHpA 

PFOA 

PFNA 

PFDA 

PFUnA 

PFDoA 

PFBS 

PFHS 

PFOS 

Transition Monitored 

213^169 

263^219 

313 ^269 and 313 ^119 

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

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

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

513 -^ 469, 513 ^ 219 and 513 ^ 269 

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

613 -» 569, 613 ^ 169 and 613 ^ 319 

299 -> 80 and 299 -> 99 

399 -^ 80 and 399 -> 99 

499 -» 80, 499 -^ 99 and 499 -> 130 

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

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

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

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

The previous infonnation is intended as a guide, alternate 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 

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

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

Perfluorobutanesulfonate (PFBS - C4 sulfonate); 3M 

Perfluorohexanesulfonate (PFHS - C6 sulfonate); 3M 

Perfluorooctanesulfonate (PFOS - C8 sulfonate); 3M 

ETS-8-044.0 Page 6 of 11 

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

Analysis 

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Former Sludge Incorporation Area - November 2010 

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

used. 

7.3 Reagent Preparation 

2 mM Ammonium acetate solution (Analysis)—Weigh 0.3 g of Ammonium acetate and dissolve in 2.0 L of reagent 

water. 

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

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

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

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

when diluting stock solutions to appropriate levels. 

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

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

125mL LDPE bottle or other suitable container. Prepare a separate solution for each analyte. Expiration dates 

and storage conditions of stock solutions should be assigned in accordance with laboratory standard operating 

procedure. An example of purity and salt correction is given below for PFOS. 

,. , , molecular weight of anion 

salt correction factor = 

moclecular weight of salt 

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

538 

10 mg CaFiySOa'K* with purity 90% = 8.35mg CsFiySOa" (10 mg*0.90*0.9275=8.35 mg) 

5 pg/mL (5000 ng/mL) mixed working standard—Add 0.5mL each of the 10Opg/mL SSSs to a 10mL volumetric 

flask and bring up to volume with solvent. 

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

volumetric flask and bring up to volume with solvent. 

125 ng/mL mixed standard—Add 625pL of the 5 pg/mL-mixed worthing standard solution to a 25mL volumetric 

flask and bring up to volume with solvent. 

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

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

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Former Sludge Incorporation Area - November 2010 

7.5 Calibration Standards 

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

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

be adjusted to meet the data quality objectives addressed in the general project outline. Calibration levels other 

than those listed below can be prepared as needed. 

Concentration 

of WS, ng/mL 

125 

125 

125 

125 

250 

250 

250 

250 

5000 

5000 

5000 

Volume of WS,ftL 

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 I, HPLC water, or other suitable water. 

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

Prepare at least five method blanks. 

9 Sample Analysis - LC/MS/MS 

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

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

software. The calibration curves may include but should not be forced through zero. The mathematical method 

used to calculate the calibration curve should be applied consistently throughout a study. Any change should be 

thoroughly documented in the raw data. 

High and/or low points may be excluded from the calibration curves to provide a better fit over the range 

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

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

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

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

ETS-8-044.0 Page 8 of 11 

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Analysis 

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Former Sludge Incorporation Area - November 2010 

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 constmcl the calibration curve. 

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

curve (if necessary) and reanalyze. 

Continuing calibration verifications (CCV) are analyzed to verify the accuracy of the calibration curve. Analyze a 

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

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

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

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

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

curve should be further diluted and reanalyzed. 

10 Quality Control 

10.1 Data Quality Objectives 

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

LOQ of 0.025 ng/mL. Any deviations from the quality control measures spelled out below will be documented in 

the raw data and footnoted in the final report. 

10.2 Method Blanks 

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

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

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

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

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

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

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

first standard level in the curve that meets criteria, or 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 

Surrogate spikes are not required but may be used on project specific requirements. 

10.5 Lab Control Sample 

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

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

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

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

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

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

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Former Sludge Incorporation Area - November 2010 

10.6 Field Matrix Spikes / Lab Matrix Spikes 

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

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

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

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

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

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

11 Data Analysis and Calculations 

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

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

. ,^ , ., , ,, (Peak Area-Intercept) ^.^ 

Analyte found (ng/mL) = -^ ^-^ x DF 

Slope 

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

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

percent recovery. 

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

Analyte added (ng/mL) 

12 Method Performance 

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

Nonconfomiance 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 perfonnance section are not met, maintenance may be perfomied on the system and 

samples reanalyzed, or other actions taken as appropriate. Document all actions in the raw data. 

If data are to be reported when perfonnance criteria have not been met, the data must be footnoted on tables and 

discussed in the text of the report. 

12.1 System Suitability 

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

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

run prior to the calibration curve. Typically these samples are at a concentration near the mid level of the 

calibration curve and are repeated injections from one autosampler vial. The system suitability injections must 

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

12.2 Quantitation 

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

equal to 0.990. Each point in the curve must be within ±25% of the theoretical concentration with the exception of 

the LLOQ, which may be within ±30%. 

CCV Performance: The calibration standards that are interspersed throughout the analytical sequence are 

evaluated as continuing calibration verifications in addition to being part of the calibration curve. The accuracy of 

each curve point must be within 25% of the theoretical value (within 30% for lowest curve point). Samples that are 

bracketed by CCVs not meeting these criteria must be reanalyzed. 

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Former Sludge Incorporation Area - November 2010 

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

standard) and the mass spectral response of unique ions. 

12.3 Sensitivity 

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

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

to Section 10 for additional details. 

12.4 Accurac y 

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

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

spikes and laboratory matrix spikes. 

12.5 Precision 

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

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

requirement for replicates excludes field blanks or rinse blanks. 

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

13 Pollution Prevention and Waste Management 

Waste generated when perfomiing 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 infonnation for reconstruction of the data. 

Infonnation for the data package must include, but is not limited to the following items: study or project number, 

sample and standard prep sheets/records, instmment run log (instalment batch records, instalment acquisition 

method, summary pages), instrument 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 

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i'.H 

ATTACHMENT D: DEVIATION 

Page 103 of 104 
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Analysis of PFBS, PFHS, and PFOS in Groundwater 

Former Sludge Incorporation Area - November 2010 

RECORD OF DEVIATION/NONCONFORMANCE 

/. Identification 

study / Project No. 

GLP10-01-02-11 

Date(s) of Occurrence: 

1/7/11 -2/11/11 

Document Number: 

ETS-8-044.0 

Deviation type 0 SOP D Equipment Procedure 0 Method 

(Check one) D Protocol D GPO D Other: 

//. Descriptio n (attach extra pages as needed) 

lyiethqd Requirernen^^^^ 

(1) LCS average recovery of 100% ± 20%. 

(2) Sample/Sample Duplicate RPD <20%. 

(3) Field matrix spike recovery of 100% ± 30%. 

Actual procedure/proces^^^ 

(1) 1/7/11; the average recovery for the low set of LCS for PFBS was 123% and for PFHS 123%. The 

average recovery of the high set of ECF LCS samples for PFOS was 123%. 

1/10/11; the low set of LCS samples for PFHS had an average recovery of 122%. The average 

recovery of the high set of ECF LCS samples for PFOS was 121%. 

2/11/11; the high set of ECF LCS for PFOS had an average recovery of 133%. 

(2) PFOS RPD value for DAL GW 137S was 33%. 

(3) PFOS FMS recovery; DAL GW 137S (59.4%) and DAL GW 144R (28.7%). PFHS FMS recovery; DAL 

GW134S(135%). 

III. Actions Taken 

(such as amendment issued, SOP revision, etc.) 

Corrective Action (D Yes 0 No) Reference: 

Acceptability of the nonconforming work: 

1) In general, the ECF LCSs for PFOS have been running 15-20% higher when quantitated using linear 

PFOS. All LCS were used in the determination of method uncertainty. The detennination of the 

method uncertainty by ETS-12-012.2 was ± 18%. However, due to potential analytical bias that was 

observed when quantitating LCS samples containing linear and branched isomers of PFOS, the 

analytical for PFOS for this study has been expanded to ± 33%. 

2) Sampling locations with RPD values S20% will be footnoted in the data tables. 

3) Analytical uncertainties for DAL GW 137S and DAL GW 134S will be adjusted accordingly. Sampling 

location DAL GW 144R - PFOS results will not be reported. Samples were re-dlluted and a LMS 

samples was prepared. Recoveries for the LMS sample for PFOS were still ~30% for the re-analysis. 

Actions: D Halting of Work D Client Notification D Work Recall D Withholding of Report 

0 Other: Deviations will be noted in finaPreport. 

Project Lead/PAI Approval: Susari Wolf ( 

Study Director (if GLP): 

Sponsor Approval (for GLP protocol deviations): NA 

Technical Reviewer (optional): NA i Date: NA 

Laboratory Department Manager Approval: Date: 

IV. Authorization to Resume Work 

Wliere halting ofworl< occurred, resumption ofworl< must first be approved by Laboratory Management 

Laboratory Department Manager Approval: NA ! Date: NA 

Deviation No. 

(assigned by Study Director or Team Leader at tlie end of study or project) 

ETS-4-008.7 Page 1 of 1 

Documentation of Deviations and Control of Nonconfomiing Testing ^^^^ ^ ^ °^ ^°'*