GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

3M 

GLP10-01-02: Interim Report 09 - Analysis of PFBS. PFHS. and PFOS in 

Ground Water Samples Collected from Decatur. AL in September 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 

GLP10-01-02-09 

Total Number of Pages 

83 

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

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

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

Certificate #2052.01 

Page 1 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

This page has been reserved for specific country requirements. 

Page 2 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

GLP COMPLIANCE STATEMENT 

Report Title: Interim Report 09 Analysis of PFBS, PFHS, and PFOS in Ground Water Samples 

Collected from Decatur, AL in September, 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. 

^ / 2=1, 7i\ 

Gary Hohenstein)Bponsor Representative 

Page 3 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

QUALITY ASSURANCE STATEMENT 

Report Title: Interim Report 09 Analysis of PFBS, PFHS, and PFOS in Ground Water Samples 

Collected from Decatur, AL in September 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 

3/2/11-3/4/11 

Phase 

Data / Report 

Date Reported to 

Testing Facility 

IVIanagement 

3/21/11 

Study Director 

3/21/11 

C^>^V^ / /(xr^-i^^eJZ/i I-^-

QAU Repre^ntative Date 

Page 4 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 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 10 

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 20 

8.9 Field Matrix Spikes (FMS) 21 

9 Data Summary and Discussion 22 

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GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

10 Conclusion 33 

11 Data/Sample Retention 33 

12 Attachments 33 

13 Signatures 34 

LIST OF TABLES 

Table 1. Summarized PFBS, PFHS, and PFOS Results (Decatur Groundwater, September 2010). .10 

Sample Description Key Code 13 

Table 2. Instrument Parameters 14 

Table 3. Liquid Chromatography Conditions 14 

Table 4. Mass Transitions 15 

Table 5. Limit of Quantitation (LOQ) 16 

Table 6. Laboratory Control Spike Recovery 18 

Table 6 continued. Laboratory Control Spike Recovery 19 

Table 6 continued. Laboratory Control Spike Recovery 20 

Table 7. Analytical Uncertainty 21 

Table 8. Field Matrix Spikes 21 

Table 9. DAL GW203L 100929 23 

Table 10. DAL GW220R 100930 23 

Table 11. DAL GW220L 100930 24 

Table 12. DAL GW222R 100929 24 

Table 13. DAL GW227R 100924 25 

Table 14. DAL GW227L 100924 25 

Table 15. DAL GWGRS04 100930 26 

Table 16. DAL GW 31 OR 100924 26 

Table 17. DAL GW 312R 100930 27 

Table 18. DAL GW 317L 100924 27 

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GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Table 19. DAL GW324L 100929 28 

Table 20. DAL GW 327R 100930 28 

Table 21. DAL GW 328R 100928 29 

Table 22. DAL GW328L 100928 29 

Table 23. DAL GW 330R 100923 30 

Table 24. DAL GW330L 100923 30 

Table 25. DAL GW 331S 100930 31 

Table 26. Trip Blank 1 31 

Table 26. Trip Blank 2 32 

Table 27. Rinseate Blank 32 

Page 7 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 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 

Jonathan Steege; analyst 

Study Dates 

Study Initiation: March 8, 2010 

Interim 09 Sample Collection: September 23 - 30,2010 

Interim 09 Experimental Termination: March 16,2011 

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 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

2 Summar y 

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

representing 17 different sampling locations. A total of seventy-seven sample bottles were received at 

the 3M Environmental Laboratory for perfluorooctane sulfonate (PFOS), perfluorohexane sulfonate 

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

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

blanks containing Milli-QTM water and appropriate trip blank spikes, and one equipment rinseate blank. 

The equipment rinseate blanks did not have FMS samples prepared for determination of PFBS, PFHS 

or PFOS recovery. All groundwater samples for this project were logged under GLP10-01 -02-09. 

The groundwater samples, trip and equipment rinseate blanks were received from Weston personnel 

on October 1, 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-

01-02-09. Many of the groundwater samples required dilution to attain PFBS, PFHS, and PFOS 

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

The average measured PFBS, PFHS, and PFOS concentrations are summarized in Table 1. 

Equipment rinseate and the trip blanks were below the lower limit of quantitation (LLOQ), indicating 

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

concentration results for all groundwaters ranged over four orders of magnitude from 0.324 ng/mL to 

2780 ng/mL. The PFHS concentration results for all groundwaters ranged over four orders of 

magnitude from 0.237 ng/mL to 7630 ng/mL. The PFOS concentration results for all groundwaters 

ranged over four orders of magnitude from <0.500 ng/mL to 5060 ng/mL. 

Page 9 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Table 1. Summarized PFBS, PFHS, and PFOS Results (Decatur Groundwater, September 

2010). 

Sampling Location 

DAL GW203L 100929 

DAL GW220R 100930 

DAL GW220L 100930 

DAL GW222R 100929 

DAL GW227R 100924 

DAL GW227L 100924 

DAL GWGRS04 100930 

DAL GW310R 100924 

DAL GW 312R 100930 

DAL GW 317L 100924 

DAL GW324L 100929 

DAL GW327R 100930 

DAL GW328R 100928 

DAL GW328L 100928 

DAL GW330R 100923 

DAL GW330L 100923 

DAL GW 331S 100930 

Trip Blank (Milli-QTM Water) 

DAL GW220R RB 100930 (rinseate blank) 

PFBS 

Avg. Cone. 

(ng/mL) ± RPD 

70.6 ±1.4 

10.0 ±1.8 

7.85 ± 3.6 

126 ±2.4 

16.7 ±4.2 

376 ± 0.53 

2410 ±3.7 

451 ±1.3 

1420 ±0.71 

0.324 '^' 

89.3 ± 0.45 

126 ±1.6 

31.8 ±0.31 

63.1 ±3.0 

2780 ± 2.2 

636 ± 5.2 

925 ± 0.54 

<0.250 

<0.250 

PFHS 

Avg. Cone. 

(ng/mL) ± RPD 

481 ±6.2 

48.7 ± 0.62 

41.9 ±5.7 

872 ± 0.0 

97.5 ±11 

255 ± 0.39 

7630 ±4.1 

453 ±3.1 

842 ±1.8 

0.237 ± 0.42 

110±8.2 

229 ±1.7 

68.0 ± 5.0 

23.6 ±8.9 

330 ± 0.61 

476 ± 9.2 *^' 

611 ±0.0 

<0.100 

<0.100 

PFOS 

Avg. Cone. 

(ng/mL) ± RPD 

836 ± 2.8 

70.2 ±10 

64.6 ± 4.3 

1230 ±4.9 

852 ± 4.5 

5060 ±10'^' 

1370 ±8.8 

895 ±15 

1510 ±5.3 

<0.500 

257 ± 5.8 

675 ± 0.74 

168 ±3.6 

0.686 ± 11 

802 ± 0.25 

172 ±24'*' 

1180±1.7 

<0.999 

<0.999 

The analytical method uncertainties associated with the reported results are as follows: PFBS 100% ± 19%, PFHS 100% ± 26%, 

and PFOS 100% ±33%. 

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

(2) A sample/sample duplicate RPD could not be calculated since one sample replicate had a result of BLOQ, 

(3) The analytical uncertainty for PFHS has been expanded to ± 35% based on FMS recovery. 

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

3 Introduction 

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

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

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

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

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

Page 10 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

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

PFBS, PFHS, and PFOS in an effort to characterize on-site groundwater conditions. 

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

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

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

samples. Each empty container was 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. All sample bottles included the addition of ^^Oa-PFBS, ^^Oa-PFHS, and "CgPFOS (intemal standards) at a nominal concentration of 1 ng/mL. All sample bottles also included the 

addition of ^'C4-PF0S (sun^ogate spike) at a nominal concentration of 0.1 ng/mL. See section 8.8 of 

the report for field matrix spike levels. 

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

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

Perforniance Liquid Chromatography/Mass Spectrometry Direct Injection Analysis". 

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

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

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

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

4 Test & Control Substances 

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

was purely analytical in nature. 

Page 11 of 83 
5 Reference Substances 

GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Reference Substance 

Chemical Name 

Chemical Formula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFBS 

(predominantly linear) 

Perfluorobutane sulfonate 

C4F9S03' 

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 

LPFHxSAM08 

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 

CaFiySOs 

Potassium Salt 

CAS #2795-39-3 

Wellington 

10/18/2013 

Frozen 

LPFOSKBM06 

TCR08-0001 

Crystalline 

98% 

PFOS 

Perfluorooctane sulfonate 

C8F17SO3" 

Potassium Salt 

CAS # 2795-39-3 

3M 

12/14/2016 

Frozen 

171 

TCR-696 

White Powder 

86.4% 

Page 12 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 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. 

Sample Description Key Code. 

String Number 

Example 

1 

2 

3 

4 

S 

String Descriptor 

DAL GW203L 0100929 

Sample Location 

Sample Type 

Well ID 

Well Level 

Sampling Date 

Sample Type 

Example 

DAL = Decatur, AL 

GW= Ground Water 

Example: 203 

R = Residum shallow water-bearing zone 

L = Bedrock water-bearing zone 

S = Epikarst middle water-bearing zone 

100929 = September 29,2010 

0=primary sample 

1=duplicate sample 

LS = low spike 

MS = mid spike 

HS = high spike 

RB = rinseate blank 

7 Mettiod Summary 

7.1 Methods 

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

"Detennination of Perfluorinated Compounds In Water by High Perfomiance Liquid 

Chromatography/Mass Spectrometry Direct Injection Analysis". 

7.2 Sample Collection 

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

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

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

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

7.3 Sample Preparation 

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

analysis. 

Samples that required dilution were prepared as follows: 

1:10 dilutions were prepared by diluting 1 mL sample with 9 mL of laboratory reagent water, 

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

1:50 dilutions were prepared by diluting 0.2mL sample with 9.8mL of laboratory reagent water, 

1:100 dilutions were prepared by diluting 0.1 mL sample with 9.9mL of laboratory reagent water, and 

1:500 dilutions were prepared by removing 2mL of the 1:100 dilutions and further diluting it with 8mL of 

laboratory reagent water. 

Page 13 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

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

7.4 Analysi s 

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. 

Table 2. Instrument Parameters. 

Instrument Name 

Analytical Method Followed 

Analysis Date 

Liquid Chromatograph 

Guard column 

Analytical column 

Injection Volume 

Mass Spectrometer 

Ion Source 

Electrode 

Polarity 

Software 

ETS Buster 

ETS-8-044.0 

10/25/10,11/8/10, and 3/15/11 

Agilent 1100 

10/25/10; Betasll 018 (2.1 mm X 100 mm), 5 n 

11/8/10; Prism RP (2.1 mm X 50 mm), 5 u 

Betasll C18 (2.1 mm X 100 mm), 5n 

5,2, or 1 nL 

Applied Biosystems API 4000 

Turtro Spray 

Turtx) ion electrode 

Negative 

Analyst 1.4.2 

ETS Ginger 

ETS-8-044.0 

2/11/11 

Agilent 1100 

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

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

2or10ML 

Applied Biosystems API 5000 

TurtDO Spray 

Turbo ion electrode 

Negative 

Analyst 1.4.2 

Table 3. Liquid Chromatography Conditions. 

step 

Number 

Total Time 

(min) 

Flow Rate 

(/jL/min) 

Percent A 

(2 mM ammonium acetate) 

PercentB 

(Methanol) 

ETS-8-044.0 Analysis 10/25110 and 11/8/10 

0 

1 

2 

3 

4 

5 

0 

2.0 

14.5 

15.5 

16.5 

20.0 

300 

300 

300 

300 

300 

300 

97.0 

97.0 

5.0 

5.0 

97.0 

97.0 

3.0 

3.0 

95.0 

95.0 

3.0 

3.0 

ETS-8-044.0/Analysis 2/11/11 and3/1S/11 

0 

1 

2 

3 

4 

5 

0 

2.0 

11.0 

14.0 

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 83 
Table 4. Mass Transitions. 

GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Analyte 

PFBS 

PFHS 

PFOS 

Reference Material 

Structure 

Linear 

Linear 

Linear 

Mass Transition 

Q1/Q3 

299/80 

299/99 

299/130 

399/80 

399/99 

399/130 

499/80 

499/99 

499/130 

Dwell time was 50 msec (2/11/11 and 3/15/11 analysis) or 75 msec 

(10/25/10and 11/8/10 analysis) 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 

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

to meet accuracy or method blank criteria. A quadratic, 1/x weighted, calibration curve of the peak area 

counts was used to fit the data for each analyte. The data were not forced through zero during the fitting 

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

point. 

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

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

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

analytical batch. 

Due to the concentration of PFBS, PFHS, and PFOS detected in the samples, isotopically-labeled 

PFBS, PFHS, and PFOS were not used during instrument calibration. In addition, due to the number of 

samples requiring dilution, the "C4-PFOS sun-ogate was not analyzed. 

8.2 System Suitability 

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

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

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

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

8.3 Limit of Quantitation (LOQ) 

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

Page 15 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

Table 5. Limit of Quantitation (LOQ). 

Analysis Date 

10/25/10 

11/8/10 

2/11/11 

3/15/11 

Dilution 

1 

10 

20 

50 

100 

1 

50 

100 

500 

1 

PFBS 

LOQ, ng/mL 

0.250 

2.50 

5.00 

12.5 

25.0 

0.250 

NA 

2.50 

12.5 

NA 

PFHS 

LOQ, ng/mL 

0.100 

1.00 

2.00 

5.00 

10.0 

0.100 

NA 

NA 

12.5 

NA 

PFOS 

LOQ, ng/mL 

0.999 

9.99 

20.0 

50.0 

99.9 

0.500 

25.0 

NA 

15.0 

0.0500 

NA = Not /Applicable; analytical results at the spedfied dilution were not reported from the run. 

8.4 Continuing Calibration 

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

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

CCVs met method criteria of 100% ± 25% with the following exceptions: 

10/25/10 Analysis: Founrteen CCVs were anayzed during the course of the oin. Two CCVs for PFBS 

were outside method acceptance crteria. One CCV for PFBS had a recovery of 137% and bracketed 

samples DAL GW 310R, DAL GW 312R, DAL GW 317L, and DAL GW 324L. A second CCV for PFBS 

had a recovery 130% and bracketed samples DAL GW 330L, DAI GW 331S, and the Trip Blank 

samples. Two CCVs for PFOS had recoveries of 128% and 127% and bracketed samples DAL GW 

222R, DAL GW 227L, and DAL GW GRS04. 

8.5 Blanks 

Three types of blanks were prepared and analyzed with the samples: method blanks, field/trip blanks, 

and equipment blanks. Method blank results were reviewed and used to evaluate method perfonnance 

and to determine the LOQ for each analyte 

8.6 Lab Control Spikes (LCSs) 

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

preparation set. LCSs were prepared by spiking known amounts of the analyte into 10 mL of Milli Q 

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

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

100% ± 20% with an RSD <20%. 

10/25/10 Analysis: Two levels of LCS were prepared and met method acceptance criteria for PFBS, 

PFHS, and linear PFOS. 

11/8/10 Analysis: Two levels of LCS were prepared and met method acceptance criteria for PFBS, 

PFHS, and linear PFOS. 

2/11/11 Analysis: Three levels of LCS were prepared and met method acceptance crtieria for PFBS, 

PFHS, and PFOS. 

3/15/11 Analysis: Two levels of LCS were prepared and met method acceptance criteria for PFOS. 

Page 16 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

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

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

PFOS (linear + branched) were prepared to evaluate the potential for analytical bias. 

10/25/10 Analysis: Two levels of linear and branched PFOS LCS were prepared and met method 

acceptance criteria. 

11/8/10 Analysis: Two levels of linear and branched PFOS LCS were prepared with the high set of LCS 

having an average recovery of 129%. 

2/11/11 Analysis: Three levels of linear and branched PFOS LCS were prepared with the high set of 

LCS having an average recovery of 133%. 

3/15/11 Analysis: Two levels of linear and branched PFOS LCS were prepared and met method 

acceptance criteria. 

The average recovery of the high set of linear and branched PFOS LCS at 129% and 133% suggests a 

slight bias when quantitating branched isomers of PFOS against a calibration curve of linear PFOS. 

Therefore, the method uncertainty for this study has been set of ± 33%, based on the highest average 

recovery of the linear and branched LCS samples. 

A method deviation is filed with the raw data for PFOS (linear + branched) LCS that did not meet method 

acceptance criteria. 

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

I oo r, . n, Calculated Concentration . . „„„, 

LCS Percent Recovery = * 100% 

Spike Concentration 

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

average LCS recovery 

Page 17 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Table 6. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Analyzed 10/25/10 

Lab ID 

LCS-101020-1 

LCS-101020-2 

LCS-101020-3 

Average ±%RSD 

LCS-101020-4 

LCS-101020-5 

LCS-101020-6 

Average ±%RSD 

PFBS 

Spiked 

Concentration 

(ng/mL) 

2.00 

2.00 

2.00 

Calculated 

Concentration 

(ng/mL) 

1.86 

1.98 

1.98 

%Recovery 

93.2 

98.9 

99.1 

97.1% ±3.5% 

20.0 

20.0 

20.0 

17.4 

19.6 

19.1 

86.8 

97.8 

95.5 

93.4% ±6.2% 

PFHS 

Spiked 

Concentration 

2.00 

2.00 

2.00 

Calculated 

Concentration 

(ng/mL) 

1.89 

1.98 

1.97 

%Recovery 

94.6 

99.2 

98.4 

97.4% ±2.5% 

20.0 

20.0 

20.0 

17.3 

19.5 

18.7 

86.4 

97.6 

93.5 

92.5% ±6.1% 

ETS-8-044.0 

Analyzed 10/25/10 

Lab ID 

LCS-101020-1 

LCS-101020-2 

LCS-101020-3 

Average ±%RSD 

LCS-101020-4 

LCS-101020-5 

LCS-101020-6 

Average ±%RSD 

PFOS (linear) 

Spiked 

Concentration 

(ng/mL) 

2.00 

2,00 

2.00 

Calculated 

Concentration 

(ng/mL) 

1.70 

1.79 

1.79 

VoRecovery 

85.2 

89.7 

89.5 

88.1% ±2.9% 

20.0 

20.0 

20.0 

17.0 

19.3 

18.6 

84.9 

96,5 

92.8 

91.4% ±6.5% 

Lab ID 

LCS-101020-7 

LCS-101020-8 

LCS-101020-9 

Average ± %RSD 

LCS-101020-10 

LCS-101020-11 

LCS-101020-12 

Average ± %RSD 

PFOS (linear+branched) 

Spiked 

Concentration 

(ng/mL) 

1,98 

1,98 

1,98 

Calculated 

Concentration 

(ng/mL) 

1,91 

1.89 

1,91 

%Recovery 

96,7 

95,6 

96,4 

96.2% ±0.59% 

19.8 

19,8 

19,8 

21,5 

21,5 

21,6 

108 

108 

109 

108% ±0.53% 

ETS-8-044,0 

Analyzed 11/8/10 

Lab ID 

LCS-101105-1 

LCS-101105-2 

LCS-101105-3 

Average ±%RSD 

LCS-101105-4 

LCS-101105-5 

LCS-101105-6 

Average ±%RSD 

PFBS 

Spiked 

Concentration 

(ng/mL) 

2,00 

2,00 

2,00 

Calculated 

Concentration 

(ng/mL) 

2,44 

2.36 

2.29 

VoRecovery 

122 

118 

115 

118% ±3.0% 

20,0 

20.0 

20.0 

24,3 

23,8 

22,5 

121 

119 

113 

118% ±3.5% 

PFHS 

Spiked 

Concentration 

(ng/mL) 

2,00 

2,00 

2,00 

Calculated 

Concentration 

(ng/mL) 

2,47 

2,37 

2,28 

VoRecovery 

124 

118 

114 

119% ±4.2% 

20.0 

20,0 

20.0 

24,00 

24.00 

23,00 

120 

120 

115 

118% ±2.4% 

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

Page 18 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

Table 6 continued. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Analyzed 11/8/10 

Lab ID 

LCS-101105-1 

LCS-101105-2 

LCS-101105-3 

Average ±%RSD 

LCS-101105-4 

LCS-101105-5 

LCS-101105-6 

Average ±%RSD 

Spiked 

Concentration 

(ng/mL) 

2,00 

2,00 

2,00 

PFOS (lineal) 

Calculated 

Concentration 

(ng/mL) 

2,30 

2,23 

2,17 

VoRecovery 

115 

111 

108 

111% ±3.2% 

20,0 

20,0 

20.0 

23,7 

24,6 

23.1 

119 

123 

115 

119% ±3.4% 

Lab ID 

LCS-101105-7 

LCS-101105-8 

LCS-101105-9 

Average ± %RSD 

LCS-101105-10 

LCS-101105-11 

LCS-101105-12 

Average ± %RSD 

PFOS (linear+branched) 

Spiked 

Concentration 

(ng/mL) 

1.98 

1,98 

1,98 

Calculated 

Concentration 

(ng/mL) 

2,14 

2,58 

2,18 

VoRecovery 

108 

130 

110 

116% ±10% 

19,8 

19,8 

19,8 

24,3 

27,2 

24.9 

123 

138 

126 

129% ±6.2%''' 

ETS-8-044,0 

Analyzed 2/11/11 

Lab ID 

LCS-110210-1 

LCS-110210-2 

LCS-110210-3 

Average ±%RSD 

LCS-110210-4 

LCS-110210-5 

LCS-110210-6 

Average ±%RSD 

LCS-110210-7 

LCS-110210-8 

LCS-110210-9 

Average ±%RSD 

Spiked 

Concentration 

(ng/mL) 

0,498 

0,498 

0,498 

PFBS 

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 

99,5 

104 

107 

104% ±3.6% 

Spiked 

Concentration 

(ng/mL) 

0,498 

0,498 

0,498 

PFHS 

Calculated 

Concentration 

(ng/mL) 

0,603 

0,594 

0,599 

%Recoveiy 

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% 

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

Page 19 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

Table 6 continued. Laboratory Control Spike Recovery. 

ETS-8-044,0 

Analyzed 2/11/11 

Lab ID 

-CS-110210-1 

.CS-110210-2 

LCS-110210-3 

Average ±%RSD 

LCS-110210-4 

LCS-110210-5 

LCS-110210-6 

Average ±%RSD 

LCS-110210-7 

LCS-110210-8 

LCS-110210-9 

Average ±%RSD 

Spiked 

Concentration 

(ng/mL) 

0,498 

0,498 

0,498 

PFOS (lineal) 

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 

LCS-110210-11 

LCS-110210-12 

Average ±%RSD 

LCS-110210-13 

LCS-110210-14 

LCS-110210-15 

Average ±%RSD 

LCS-110210-16 

LCS-110210-17 

LCS-110210-18 

Average ± %RSD 

PFOS 

Spiked 

Concentration 

(ng/mL) 

0,502 

0,502 

0,502 

' (linear •*• branched) 

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%'" 

ETS-8-044,0 

Analyzed 3/15/11 

Lab ID 

LCS-110315-1 

LCS-110315-2 

.CS-110315-3 

Average ±%RSD 

LCS-110315-4 

LCS-110315-5 

LCS-110315-6 

Average ±%RSD 

Spiked 

Concentration 

(ng/mL) 

0.498 

0.498 

0.498 

PFOS (linear) 

Calculated 

Concentration 

(ng/mL) 

0,456 

0,497 

0,463 

VoRecovery 

91,5 

99,9 

93.0 

94.8% ±4.7% 

4.98 

4,98 

4,98 

4,35 

5,05 

5,04 

87.3 

101 

101 

96.4% ±8.2% 

Lab ID 

LCS-110315-7 

LCS-110315-8 

LCS-110315-9 

Average ±%RSD 

LCS-110315-10 

LCS-110315-11 

LCS-110315-12 

Average ±%RSD 

PFOS 

Spiked 

Concentration 

(ng/mL) 

0,502 

0,502 

0,502 

(linear* branched) 

Calculated 

Concentration 

(ng/mL) 

0,427 

0,456 

0,429 

VoRecovery 

85,1 

90,9 

85,5 

87.2% ± 3.7% 

5,04 

5,04 

5.04 

5,02 

4,90 

5,12 

99,6 

97.2 

102 

99.6% ±2.4% 

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

8.7 Analytical IVIethod 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. The method uncertainty for PFOS by ETS-12-012-2 was found to be ± 

27% however, since one of the high sets of linear and branched LCS for PFOS had an average 

recovery of 133%, the analytical uncertainty assigned to this study for PFOS will be ± 33%. 

Page 20 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Table 7. Analytical Uncertainty. 

Analyte 

PFBS 

PFHS 

PFOS 

standard Deviation 

9.52 

13.2 

NA 

Method Uncertainty 

±19% 

±26% 

±33%"' 

(1) Analytical uncertainty for PFOS was based on batch QC prepared with the study samples. 

8.8 Field Matrix Spikes (FMS) 

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

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

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

prior to shipping sample containers for sample collection. Field matrix spike recoveries within method 

acceptance criteria of 100±30% confinn that "unknown" components in the sample matrix do not 

significantly interfere with the extraction and analysis of the analytes of interest. Field matrix spike 

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

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

Table 8. Field Matrix Spikes. 

Sampling Location 

317L 

220R, 220L, 328L '^' 

203L, 222R, 227L, 227R, 310R, 324L, 

327R, 330L'^331S 

GRS04, 312R, 330R 

328R"' 

Trip Blank Sets 1-4 

Spike Level 

Low FMS 

High FMS 

Low FMS 

High FMS 

Low FMS 

High FMS 

Low FMS 

High FMS 

Low FMS 

High FMS 

Low FMS 

Mid FMS 

High FMS 

PFBS 

(ng/mL) 

1,00 

10,0 

10,0 

100 

100 

1000 

1000 

5000 

100 

500 

10.0 

100 

1000 

PFHS 

(ng/mL) 

1,00 

10.0 

10,0 

100 

100 

1000 

1000 

5000 

100 

500 

10.0 

100 

1000 

PFOS 

(ng/mL) 

1.00 

10,0 

10,0 

100 

100 

1000 

1000 

5000 

100 

500 

10,0 

100 

1000 

(1) Sample bottles were overtilled by more than 10% for DAL GW328R HS (221 mL), DAL GW 328L LS (224 mL), DAL 

GW 330L LS (221 mL), and DAL GW 330L HS (224 mL), The FMS spike concentration has been adjusted accordingly. 

Due to the high concentration of PFBS, PFHS, and PFOS detected in the samples, the sun-ogate spike 

of ^^C4-PF0S was not analyzed. 

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

FMS Recovery = .^^ J-^' 

Spike Concentraton 

100% 

8.9 Lab Matrix Spikes (LMS) 

Sampling location DAL GW GRS04 100930 high spike at 5000 ng/mL produced recoveries <50% when 

initially ananyzed on 10/25/10. A laboratory matrix spike at 5000 ng/mL was prepared and analyzed on 

2/11/11. The lab matrix spike result is presented in section 9 of this report. 

Page 21 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

\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 blank. Results and average values are rounded to 

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

from those listed in the raw data. 

Field matrix spike recoveries meeting the method acceptance criteria of ± 30%, demonstrate that the 

method was appropriate for the given matrix and their respective quantitative ranges. 

DAL GW 330L100923 - The recovery of the high FMS sample for PFHS was 135%. This was the 

only appropriate field matrix spike level for PFHS. The method uncertainty has been adjusted for 

PFHS to ± 35%. 

DAL GW GRS04100923 -The recovery of the high FMS sample for PFBS, PFHS, and PFOS were 

<50%. A LMS at 5000ppb was prepared on the sample with acceptable recoveries for PFBS, PFHS, 

and PFOS. 

DAL GW 328L100928 - The recovery of the high FMS sample for PFOS was 69.0%, while the 

recovery of the low FMS was 102%. Since the low FMS was the more appropriate spike level as 

compared to the sample concentration, no adjustment was made to the analytical uncertainty. 

Page 22 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Tables. DAL GW203L 100929 

3M LIMS ID 

GLP10-01-02-09-001 

GLP10-01-02-09-002 

GLP10-01-02-09-003 

GLP10-01-02-09-004 

Description 

DAL GW203L 0 100929 

DAL GW203LDB 100929 

DAL GW203LLS 100929 

DAL GW203LHS 100929 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

70,1 

71.1 

175 

1000 

VoRecovery 

NA 

NA 

104 

92.9 

70.6 ng/mL ±1.4% 

PFHS 

Concentration 

(ng/mL) 

466 

496 

643 

1700 

%Recovery 

NA 

NA 

NC 

122 

481 ng/mL ±6.2% 

PFOS 

Concentration 

(ng/mL) 

824 

847 

907 

1930 

VoRecovery 

NA 

NA 

NC 

109 

836 ng/mL ±2.8% 

NA = Not Applicable 

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

Samples diluted 20x and analyzed 10/25/10 and 11/8/10. 

Table 10. DAL GW220R 100930 

3MUMSID 

GLP10-01-02-09-005 

GLP10-01-02-09-006 

GLP10-01-02-09-007 

GLP10-01-02-09-008 

Description 

DAL GW220R 0100930 

DAL GW220R DB 100930 

DAL GW220RLS 100930 

DAL GW220RHS 100930 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

9.92 

10.1 

20.1 

112 

VoRecovery 

NA 

NA 

101 

102 

10.0 ng/mL ±1.8% 

PFHS 

Concentration 

(ng/mL) 

48,5 

48.8 

59.3 

150 

VoRecovery 

NA 

NA 

NC 

101 

48.7 ng/mL ±0.62% 

PFOS 

Concentration 

(ng/mL) 

73.8 

66.5 

81.1 

152 

VoRecovery 

NA 

NA 

NC 

81.9 

70.2 ng/mL ±10% 

NA = Not Applicatde 

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

Samples diluted lOx and analyzed 10/25/10. 

Page 23 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Table 11. DAL GW 220L 100930 

3IVIUMSID 

GLP10-01-02-09-009 

GLP10-01-02-09-010 

GLP10-01-02-09-011 

GLP10-01-02-09-012 

Description 

DAL GW220L 0 100930 

DAL GW220LDB 100930 

DAL GW220LLS 100930 

DAL GW220LHS 100930 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

7.99 

7.71 

20.8 

112 

VoRecovery 

NA 

NA 

130 

104 

7.85 ng/mL ±3.6% 

PFHS 

Concerrtration 

(ng/mL) 

40.7 

43.1 

55.4 

150 

VoRecovery 

NA 

NA 

NC 

108 

41.9 ng/mL ±5.7% 

PFOS 

Concentration 

(ng/mL) 

63.2 

66.0 

80.8 

152 

VoRecovery 

NA 

NA 

NC 

87.4 

64.6 ng/mL ±4.3% 

NA= Not Applicable 

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

Samples diluted 20x and analyzed 10/25/10. 

Table 12. DAL GW222R 100929 

3IVILIIVISID 

GLP10-01-02-09-013 

GLP10-01-02-09-014 

GLP10-01-02-09-015 

GLP10-01-02-09-016 

Description 

DAL GW222R 0100929 

DAL GW222RDB 100929 

DAL GW222RLS 100929 

DAL GW222R HS 100929 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

124 

127 

238 

1200 

VoRecovery 

NA 

NA 

113 

107 

126 ng/mL ±2.4% 

PFHS 

Concentration 

(ng/mL) 

872 

872 

996 

2010 

VoRecovery 

NA 

NA 

NC 

114 

872 ng/mL ±0.0% 

PFOS 

Concentration 

(ng/mL) 

1200 

1260 

1220 

2310 

VoRecovery 

NA 

NA 

NC 

108 

1230 ng/mL ±4.9% 

NA = Not /Applicable 

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

Samples diluted 50x and analyzed 10/25/10. 

Page 24 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

Table 13. DAL GW227R 100924 

3MUMSID 

GLP10-01-02-09-017 

GLP10-01-02-09-018 

GLP10-01-02-09-019 

GLP10-01-02-09-020 

Description 

DAL GW227R 0100924 

DAL GW227RDB 100924 

DAL GW227RLS 100924 

DAL GW227RHS 100924 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

16.3 

17.0 

117 

1030 

VoRecovery 

NA 

NA 

100 

101 

16.7 ng/mL ±4.2% 

PFHS 

Concentration 

(ng/mL) 

103 

91.9 

185 

1190 

VoRecovery 

NA 

NA 

87.6 

109 

97.5 ng/mL ±11% 

PFOS 

Concentration 

(ng/mL) 

871 

833 

801 

2050 

VoRecovery 

NA 

NA 

NC 

120 

852 ng/mL ±4.5% 

NA = Not Applicable 

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

Samples diluted 50x and analyzed 10/25/10. 

Table 14. DAL GW227L 100924 

3M LIMS ID 

GLP10-01-02-09-021 

GLP10-01-02-09-022 

GLP10-01-02-09-023 

GLP10-01-02-09-024 

Description 

DAL GW227L 0100924 

DAL GW227LDB 100924 

DAL GW227LLS 100924 

DAL GW227LHS 100924 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mtj 

377 

375 

474 

1270 

VoRecovery 

NA 

NA 

NC 

89.4 

376 ng/mL ±0.53% 

PFHS 

Concentration 

(ng/mL) 

254 

255 

364 

1260 

VoRecovery 

NA 

NA 

NC 

101 

255 ng/mL ±0.39% 

PFOS 

Concentration 

(ng/mL) 

4790 

5320 

5680 

6860 

%Recovery 

NA 

NA 

NC 

NC 

5060 ng/mL ±10%"' 

NA = Not Applicable 

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

Samples diluted 20x for PFBS and PFHS, and lOOx for PFOS and analyzed on 10/25/10. 

(1) Sampling location did not have an appropriate field matrix spike level for PFOS. 

Page 25 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

Table 15. DAL GWGRS04 100930 

3M LIMS ID 

GLP10-01-02-09-025 

GLP10-01-02-09-026 

GLP10-01-02-09-027 

GLP10-01-02-09-028 

GLP10-01-02-09025; 5000ppb LMS 

Description 

DAL GW GRS04 0 100930 

DAL GW GRS04 DB 100930 

DAL GW GRS04 LS 100930 

DAL GW GRS04 HS 100930 

DAL GWGRS04 0100930 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

2360 

2450 

NA'^' 

4450 

7690 

VoRecovery 

NA 

NA 

NA<^> 

40.9 <^> 

106 

2410 ng/mL ±3.7% 

PFHS 

Concentration 

(ng/mL) 

7780 

7470 

NA<^> 

9440 

13300 

VoRecovery 

NA 

NA 

NA<^' 

36.3 '^' 

114 

7630 ng/mL ±4.1% 

PFOS 

Concentration 

(ng/mL) 

1310 

1430 

NA<^' 

2410 

5740 

VoRecovery 

NA 

NA 

NA'^> 

20.8 '^' 

87.4 

1370 ng/mL ±8.8% 

NA = Not Applicable 

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

Samples diluted 500x and analyzed on 2/11/11. 

(1) The LS sample was not diluted as the HS was the more appropriate spike for PFBA and PFHS. 

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

Table 16. DAL GW 31 OR 100924 

3MUMSID 

GLP10-01-02-09-029 

GLP10-01-02-09-030 

GLP10-01-02-09-031 

GLP10-01-02-09-032 

Description 

DAL GW310R 0100924 

DAL GW 31 OR DB 100924 

DAL GW 31 OR LS 100924 

DAL GW310RHS 100924 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

448 

454 

563 

1440 

VoRecovery 

NA 

NA 

NC 

98.9 

451 ng/mL ± 1.3% 

PFHS 

Concentration 

(ng/mL) 

460 

446 

563 

1460 

VoRecovery 

NA 

NA 

NC 

101 

453 ng/mL ±3.1% 

PFOS 

Concentration 

(ng/mL) 

961 

829 

863 

1920 

VoRecovery 

NA 

NA 

NC 

103 

895 ng/mL ±15% 

NA = Not Applicable 

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

Samples diluted lOOx and analyzed 10/25/10. 

Page 26 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Table 17. DAL GW 312R 100930 

3M LIMS ID 

GLP10-01-02-09-033 

GLP10-01-02-09-034 

GLP10-01-02-09-035 

GLP10-01-02-09-036 

Description 

DAL GW312R 0100930 

DAL GW312RDB 100930 

DAL GW312RLS 100930 

DAL GW312RHS 100930 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

1420 

1410 

2460 

6280 

VoRecovery 

NA 

NA 

105 

97.3 

1420ng/mL ±0.71% 

PFHS 

Concentration 

(ng/mL) 

834 

849 

1920 

6170 

VoRecovery 

NA 

NA 

108 

107 

842 ng/mL ±1.8% 

PFOS 

Concentration 

(ng/mL) 

1470 

1550 

2370 

6740 

VoRecovery 

NA 

NA 

86.0 

105 

1510 ng/mL ±5.3% 

NA = Not Applicable 

Samples diluted lOOx and analyzed 10/25/10. 

Table 18. DAL GW 317L 100924 

3M LIMS ID 

GLP10-01-02-09-037 

GLP10-01-02-09-038 

GLP10-01-02-09-039 

GLP10-01-02-09-040 

Description 

DAL GW317L 0100924 

DAL GW317LDB 100924 

DAL GW317LLS 100924 

DAL GW 317LHS 100924 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

<0.250 

0.324 

1.20 

9.76 

VoRecovery 

NA 

NA 

87.6 

94.4 

0.324 ng/mL^* 

PFHS 

Concentration 

(ng/mL) 

0.236 

0.237 

1.22 

9.93 

VoRecovery 

NA 

NA 

98.4 

96.9 

0.237 ng/mL ±0.4rAo 

PFOS 

Concentration 

(ng/mL) 

<0.500 

<0.500 

1.20 

8.52 

VoRecovery 

NA 

NA 

120 

85,2 

< 0.500 ng/mL 

NA = Not Applicable 

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

Samples were analyzed 11/8/10. 

(1) A sample/sample duplicate RPD could not be calculated since one sample replicate had a result of BLOQ. 

Page 27 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Table 19. DAL GW 324L 100929 

3M LIMS ID 

GLP10-01-02-09-041 

GLP10-01-02-09-042 

GLP10-01-02-09-043 

GLP 10-01-02-09-044 

Description 

DAL GW324L 0100929 

DAL GW324LDB 100929 

DAL GW324LLS 100929 

DAL GW324LHS 100929 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

89.1 

89.5 

186 

978 

VoRecovery 

NA 

NA 

96.7 

88.9 

89.3 ng/mL ±0.45% 

PFHS 

Concentration 

(ng/mL) 

105 

114 

216 

1140 

VoRecovery 

NA 

NA 

107 

103 

110 ng/mL ±8.2% 

PFOS 

Concentration 

(ng/mL) 

249 

264 

359 

1280 

VoRecovery 

NA 

NA 

NC 

102 

257 ng/mL ±5.8% 

NA= Not Applicable 

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

Samples diluted 20x and analyzed 10/25/10. 

Table 20. DAL GW327R 100930 

3M LIMS ID 

GLP10-01-02-09-045 

GLP10-01-02-09-046 

GLP10-01-02-09-047 

GLP10-01-02-09-048 

Description 

DAL GW327R 0100930 

DAL GW327R DB 100930 

DALGW327RLS 100930 

DALGW327RHS 100930 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

125 

127 

235 

1110 

VoRecovery 

NA 

NA 

109 

98.4 

126 ng/mL ± 1.6% 

PFHS 

Concentration 

(ng/mL) 

227 

231 

337 

1340 

VoRecovery 

NA 

NA 

NC 

111 

229 ng/mL ±1.rAo 

PFOS 

Concentration 

Jng/mL) 

672 

677 

761 

1930 

VoRecovery 

NA 

NA 

NC 

126 

675 ng/mL ±0.74% 

NA = Not Applicable 

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

Samples diluted 50x and analyzed 10/25/10. 

Page 28 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Table 21. DAL GW328R 100928 

3M LIMS ID 

GLP10-01-02-09-049 

GLP10-01-02-09-050 

GLP10-01-02-09-051 

GLP10-01-02-09-052 

Description 

DAL GW328R 0100928 

DAL GW328RDB 100928 

DAL GW328RLS 100928 

DAL GW328RHS 100928 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

31.8 

31.7 

137 

491 

VoRecovery 

NA 

NA 

105 

101 

31.8 ng/mL ±0.31% 

PFHS 

Concentration 

(ng/mL) 

66.3 

69.7 

183 

561 

VoRecovery 

NA 

NA 

115 

109 

68.0 ng/mL ±5.0% 

PFOS 

Concentration 

(ng/mL) 

171 

165 

261 

632 

VoRecovery 

NA 

NA 

93.0 

102 

168ng/mL±3.6Vo 

NA = Not Applicable 

Samples diluted 20x and analyzed on 10/25/10. 

Table 22. DAL GW328L 100928 

3M LIMS ID 

GLP10-01-02-09-053 

GLP10-01-02-09-054 

GLP10-01-02-09-055 

GLP10-01-02-09-056 

Description 

DAL GW328L 0100928 

DAL GW328LDB 100928 

DAL GW328LLS 100928 

DAL GW328LHS 100928 

Average Concentration (ng/mL) ± %RPD 

PFBS^> 

Concentration 

(ng/mL) 

62.1 

64.0 

72.6 

167 

VoRecovery 

NA 

NA 

NC 

104 

63.1 ng/mL ±3.0% 

PFHSf' 

Concentration 

(ng/mL) 

22.5 

24.6 

32.3 

131 

VoRecovery 

NA 

NA 

NC 

107 

23.6 ng/mL ±8.9% 

PFOS^ 

Concentration 

(ng/mL) 

0.722 

0.649 

9.83 

69.7 

VoRecovery 

NA 

NA 

102 

69.0 <^' 

0.686 ng/mL ± 11% 

NA = Not Applicable 

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

(1) Samples diluted 20x and analyzed on 10/25/10 for PFBS and PFHS. 

(2) Samples analyzed on 3/15/11 for PFOS, 

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

Page 29 of 83 
GLP10-01-02; Interim Report 09 

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

Quarteriy Groundwater Sampling - Sept 2010 

Table 23. DAL GW330R 100923 

3M LIMS ID 

GLP10-01-02-09-057 

GLP10-01-02-09-058 

GLP10-01-02-09-059 

GLP10-01-02-09-060 

Description 

DAL GW330R 0100923 

DAL GW330RDB 100923 

DALGW330RLS 100923 

DAL GW330R HS 100923 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

2810 

2750 

3750 

7610 

VoRecovery 

NA 

NA 

NC 

96.6 

2780 ng/mL ±2.2% 

PFHS 

Concentration 

(ng/mL) 

331 

329 

1380 

NA'^' 

VoRecovery 

NA 

NA 

105 

NA<^' 

330 ng/mL ±0.61% 

PFOS 

Concentration 

(ng/mL) 

803 

801 

1780 

NA<^' 

VoRecovery 

NA 

NA 

97.8 

NA<^) 

802 ng/mL ±0.25% 

NA = Not Applicable 

Samples were diluted 50x for PFHS and PFOS, and lOOx for PFBS and analyzed on 10/25/10. 

(1) Sample concentration exceeded calibration range. A further dilution was not prepared as the LS sample was the more appropriate spike level for PFHS and PFOS. 

Table 24. DAL GW330L 100923 

3M LIMS ID 

GLP10-01-02-09-061 

GLP10-01-02-09-062 

GLP10-01-02-09-063 

GLP10-01-02-09-064 

Description 

DAL GW330L 0100923 

DAL GW330LDB 100923 

DAL GW330LLS 100923 

DAL GW330LHS 100923 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

619 

652 

677 

1510 

VoRecovery 

NA 

NA 

NC 

97,8 

636 ng/mL ±5.2% 

PFHS 

Concentration 

(ng/mL) 

498 

454 

560 

1680 

VoRecovery 

NA 

NA 

NC 

135'^' 

476 ng/mL ±9.2%'^ 

PFOS 

Concentration 

(ng/mL) 

192 

151 

248 

1270 

VoRecovery 

NA 

NA 

84.5 

123 

172 ng/mL ±24%'^' 

NA = Not /Applicable 

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

Samples diluted 20x and analyzed on 10/25/10. 

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

(2) The analytical uncertainly has been adjusted for FMS recovery for PFHS to ± 35%. 

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

Page 30 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Table 25. DAL GW 331S 100930 

3M LIMS ID 

GLP10-01-02-09-065 

GLP10-01-02-09-066 

GLP10-01-02-09-067 

GLP10-01-02-09-068 

Description 

DAL GW331S 0100930 

DAL GW331SDB 100930 

DAL GW331SLS 100930 

DAL GW331SHS 100930 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

927 

922 

1070 

1990 

VoRecovery 

NA 

NA 

NC 

107 

925 ng/mL ±0.54% 

PFHS 

Concentration 

(ng/mL) 

611 

611 

788 

1770 

VoRecovery 

NA 

NA 

NC 

116 

611 ng/mL ±0.0% 

PFOS 

Concentration 

(ng/mL) 

1170 

1190 

1670 

2390 

VoRecovery 

NA 

NA 

NC 

121 

1180 ng/mL ±1.7% 

NA = Not Applicable 

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

Samples diluted 50x and analyzed on 10/25/10 

Table 26. Trip Blank 1 

3M LIMS ID 

GLP10-01-02-09-069 

GLP10-01-02-09-070 

GLP10-01-02-09-071 

GLP10-01-02-09-072 

Description 

Trip Blank 1 Sample 

Trip Blank 1 FMS Low 

Trip Blank 1 FMS Mid 

Trip Blank 1 FMS High 

PFBS 

Concentration 

(ng/mL) 

<0.250 

10.7 

108 

1100 

VoRecovery 

NA 

107 

108 

110 

PFHS 

Concentration 

(ng/mL) 

<0.100 

11.4 

114 

1160 

VoRecovery 

NA 

114 

114 

116 

PFOS 

Concentration 

(ng/mL) 

<0.999 

11.4 

102 

1080 

VoRecovery 

NA 

114 

102 

108 

NA= Not Applicable 

FMS Mid diluted lOx, FMS High diluted 50x, and analyzed on 10/25/10. 

Page 31 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Table 26. Trip Blank 2 

3M LIMS ID 

GLP10-01-02-09-073 

GLP10-01-02-09-074 

GLP10-01-02-09-075 

GLP10-01-02-09-076 

Description 

Trip Blank 2 Sample 

Trip Blank 2 FMS Low 

Trip Blank 2 FMS Mid 

Trip Blank 2 FMS High 

PFBS 

Concentration 

(ng/mL) 

<0.250 

10.8 

108 

1100 

VoRecovery 

NA 

108 

108 

110 

PFHS 

Concentration 

(ng/mL) 

<0.100 

11.4 

115 

1190 

%Recovery 

NA 

114 

115 

119 

PFOS 

Concentration 

(ng/mL) 

<0.999 

11.0 

99.6 

1090 

VoRecovery 

NA 

110 

99.6 

109 

NA = Not Applicable 

FMS Mid diluted lOx, FMS High diluted 50x, and analyzed on 10/25/10. 

Table 27. Rinseate Blank 

3M LIMS ID 

GLP 10-01-02-09-077 

Description 

DAL GW220RRB 100930 

PFBS 

Concentration 

(ng/mL) 

<0.250 

VoRecovery 

NA 

PFHS 

Concentration 

(ng/mL) 

<0.100 

VoRecovery 

NA 

PFOS 

Concentration 

(ng/mL) 

<0.999 

%Recovery 

NA 

NA = Not Applicable 

Sample was analyzed on 10/25/10 

Page 32 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

10 Conclusion 

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

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

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

11 Data/Sample Retention 

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

to 3M Environmental Laboratory standard operating procedures. 

12 Attacfiments 

Attachment A: Protocol Amendment 09 (General Project Outline) 

Attachment B: Representative Chromatograms and Calibration Curves 

Attachment C: Analytical Method 

Attachment D: Method Deviation 

Page 33 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

13^^Signatures 

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

j?j-Ai^;^e>i7::^jorA/ 

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

3. / ^ t 

11 

Gary Hohensteun, Sponsor Representative 

fJilAU/ 

Date 

Jaisimha Kesari, Study Director I I Date 

Page 34 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

ATTACHMENT A: PROTOCOL AMENDMENT 

Page 35 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Analytical Protocol: GLP10-01-02 

Amendment 9 

Study Title 

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

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

Decatur Phase 3 Site-Related Monitoring Program 

PROTOCOL AMENDMENT NO. 9 

Amendment Date: 

September 13, 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 

Page 1 of 7 

Page 36 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Analytical Protocol: GLP1Q-01-02 

Amendment 9 

This amendment modifies the foilowing 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 (GPQ) 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 September 20. 

2010. The groundwater samples for this sampling event will be entered into the 3M 

Environmental Laboratory LIMS as project GLP10-01-01-09 and reported as interim 

report GLP10-01-02-09, (reflecting study GLP10-01-02 and amendment -09). 

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 37 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Analytical Protocol: GLP10-01-02 

Amendment 9 

Amendment Approval 

Uf i^%^^fi y^/0 

Gary Hohenstein, Sponsor Representative Date 

Cleston C. Lange, Principal Analytical Investigator 

V/5/Z«f/2 . > 

Date 

P ^ S^/'^o/O 

William Reaoen, EHS Opns Environmental Lab Management Date 

mm 

Jaisimha^<esari P.E., DEE, Study Director Date 

Page 3 of 7 

Page 38 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Analytical Protocol: GLP10-01-02 

Amendment 9 

Environmental Health & Safety Operations, Environmental Laboratory 

General Project Outline 

To: Gary Hohenstein, SM EHS&Opns 

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

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

Clifflon Jacoby, 3M EHS&Opns; Environmental Lab 

Cleston Lange, 3M EHS&Opns; Environmental Lab 

Jai Kesari, Weston Solutions 

Charies Young, Weston Solutions 

Tim Frinak, Weston Solutions 

Date; September 13,2010 

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 09 - Decatur 3"^ Quarter Groundwater Sampling 

1 General Project Information 

Contacts 

Lab Request Number 

Six Digit Department Number 

Project Schedule/Test Dates 

3M Sponsor Representative 

Gary Hohenstein 

SM EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

aahohensteinSJmmm.com 

3M Environmental Laboratory IVIanagement 

William K. Reagen 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9739 

wkreaaenOmmm.com 

Principal Analytical investigator 

Cleston Lange 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9860 

cclanae(a)mmm,com 

Sampling Coordinator 

Timothy Frinak 

Weston Solutions 

Timothv.frinak(5!westonsolutions.com 

Phone; (334)-332-9123 

GLP10-01-02-09 

Dept #530711. Project #0022674449 

Sampling scheduled for the week of September 20, 2010 

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

Page 4 of 7 

Page 39 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Analytical Protocol: GLP10-01-02 

Amendment 9 

2 Background Information and Project Objective(s) 

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

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

Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS). Analyses will be conducted 

under the GLP requirements of EPA TSCA Good Laboratory Practice Standards 40 CFR 792. 

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

September 20, 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-

01-02-09. 

3 Project Schedule 

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

20,2010. Sample bottles will be shipped in coolers ovemight to 3M Decatur for amVal by Friday, September 

17,2010. 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 seventeen sampling locations have been specified. For each sampling location, four sample bottJes 

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

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

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

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

from GLP10-01-02-02 were used to detemiine the field matrix spike levels for GLP10-01-01-09 listed in Table 1. 

A total of 85 sample bottles will be prepared. 

Table 1. Sampling Locations and Field Matrix Spike levels. 

Well No. 

317L 

220R, 220L, 328L 

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

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

331S 

GRS04, 312R, 330R 

328R 

Trip Blank Sets 

1,2, 3, and 4 

Sample Level 

Low 

High 

Low 

High 

Low 

High 

Low 

High 

Low 

High 

Low 

Mid 

High 

Spike Cone. (ng/mL) 

1 

10 

10 

100 

100 

1000 

1000 

5000 

100 

500 

10 

100 

1000 

Page 5 of 7 

Page 40 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Analytical Protocol: GLP10-01-02 

Amendment 9 

5 Test Methods 

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

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

Analysis". Due to previous data for these sampling locations (GLP10-01-01-02) samples will most likely require 

dilution. Samples requiring dilution will be prepared in Milli-Q water prior to analysis by ETS-8-044.0. The data 

quality objectives for these studies are quantitative results for the target analytes with an 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. 

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

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

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

PFOS only, from nominal concentrations of 0.02 ng/mL -100 ng/mL. Due to the expected concentration of 

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

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

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

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

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

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

and summing the calculated concentrations together to generate the final PFOS concentraton. This may be 

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

against a predominately linear reference standard for PFOS. 

6 Reporting Requirements 

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

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

the field. Laboratory control spikes of reagent water prepared at the time of sample extraction will also be 

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

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

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

7 Email Correspondence 

Attachment A: Sampling Bottle Request 

Page 6 of 7 

Page 41 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Analytical Protocol: GLP10-01-02 

Amendment 9 

LABORATORY REQUEST FOR SAIVIPLE COI^AINERS 

SITE 

PROJECT; 

PROJEa NO. 

SHIPPING ADDRESS 

SHIPMENT REQUIRED BY: 

PROJECT CONTACT; 

CONTACT NUMBER; 

EMAIL; 

Confidential Client, Decatur, Alabama 

3RD QUARTER GROUNDWATER SAMPLING 

02181.129.145.0003 

Martin Smith - WESTON TRAILER 

3M DECATUR PUNT 

1400 STATE DOCKS ROAD 

DECATUR, AL 35601 

256-552-6189 

20-Sep-lO 

TIM FRINAK 

OFFICE: 334-466-5653; CELL 334-332-9123 

t.frinak(S)we5tonsolutions.com 

Samples 

17 

1 

4 

Sample Type 

Groundwater 

GW Duplicate 

Field Blanks 

Rinsate 

Samples 

Trip Blanks 

Parameter 

FCs 

FCs 

FCs 

Lab H20 

Required 

Yes 

Containers 

COCs Required 

USDA Permit 625 and Ubels Required 

MS/MSDs Selected by Lab 

Preserv. 

VES 

No 

YES 

COMMENTS: 

Please pack to prevent breakage. 

Please provide the laboratory Project Number for reference on the COC. 

One trip blank will be used per cooler shipped. Un-used trip blanks will be returned 

to 

the laboratory for disposal. 

203L 

220R 

220L 

222R 

227R 

227L 

6RS04 

310R 

RW312R 

317L 

3241 

RW327R 

WELL LIST 

328R 

328L 

330R 

330L 

RW331S 

Page 7 of 7 

Page 42 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

ATTACHIVIENT B: SAIVIPLE CHROMATOGRAIVIS AND CALIBRATION CURVE 

Page 43 of 83 
Buster J2930203 

GLP10-01-02; Interim Report 09 

Bat^pa|ym?f ?ffl%2'5Et^§t?"d PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

I Sample Name: •b101025b02r Sampja ID: -06008-194-10- File: -b101025b.v^ 

Peak Name: 'PFBS* liAass<es): -299.0/99.0 «mu,299.0AO.O anuJI Comment "5.0 ng/mL FC ltd in MU Q \AibtBr' Anrwtation; ~ 

.-. I^anual 

I Time: 12.S 

1930264 COI 

3.736+005 

Sample Name: -blO'tD25b034' Sample ID: ' 

I Peak Name: *PFBS- Massfea): *299.0/99.0 *i 

I Comment *20ppb LCS" Annotation:" 

Acq. Date: 

Acq. Time: 

Modified: 

RT Window: 

Expacced RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

10/26/ 

3:27:2 

Ves 

30.0 

12. 

No 

Manua 

12. 

Area: 62BS119 

Heiqhl:: 

Start Time: 

End Time: 

.19a-*0 

12. 

13. 

1.15e6-

1.10e6-

1.05e6-

I.OOeS 

9.50e5 

S.OOeS 

B.50e5 

8.00e5 

7.50e5 

7.00e5 

i 6.50eS 

j ^ 6.00e5 

I 5.50e5 

5.00e5 

4.50e5 

4.00*5 

3.50e5 

3.00e5 

2.50eS 

2.00e5 

1.50e5 

I.OOeS 

5.00e4 

0.00 

I

Sample Name: "^010256045- Sample ID: •LCS-101D2O-10r File: -b101025b.wfr 

Peak Name: 'PFBS* MasB<ei): *299.0/99.0 amu,299.0«0.0 amuComment "20ppb LCS ECF* Annotation: ~ 

Sample Index : Ab 

rvpe 

0.00 ng/mL 

0.219 ng/mL 

10/26/2010 

7:19:04 AH 

Heiglit : 

Star t T i 

End Time 

2.1 »4 

2.0e4 

1.9»4 

1.8e4 

1.7e4' 

1.6e4 

1.Se4' 

1.4 ^ 

1.3e4 

1.2e4-

1.1e4' 

1.0e4 

9000.0 

SOOO.O 

7000.0 

6000.0-

5000.0 

4000.0 

3000.0-

2000.0 

1000.0 

0.0 

I

Sample Name: -b101025b04?' Sample ID: ' 

Peak Name: -PFBS" Ma««(o«): -299.0»9.0 «i 

Comment -Method Blank* Annotation: ~ 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: - 0 

Acq. Date : 10/25/2010 

Ftte: "bl01025b.wifr 

RT Kit 

E.-pscced i 

l'3S Relat i 

Int. Type^ 

Retention 

Area: 

Height: 

'eak Heigtii 

'eak Widtll 

ling Widtrfi 

chm: IntelliCu; 

...AyiAv*Utol»Mtt»4*j4_... 

16 18 12 14 16 18 

Printing Time: 1:32:42 PM 

Printing Date: Tuesday, February 08, 

Page 1 of 6 

Page 44 of 83 
*** Buster J2930203 

GLP10-01-02; Interim Report 09 

Bat^R3!ym?f ?m^?§HcSi?"d PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

[

Sample Name: 'b101025b050" Sample ID: 

Peak Name: "PFBS' Mass{es): -299.0/99.0 

Comment 'DAL GW 203L 0 100929 (20X)* 

Sample Type: 

Concentration : 

Calculate d Cone: 

Acq. Time: 

Hsdified : 

RT V/indow: 

Expected RT: 

Use Relativ e RT: 

N/A 

70.1 ng/mL 

10/2e/2010 

9:0<:13 AM 

•GLP1&O1-O2-09-O0r 

amu, 299.0/80.0 amu' 

Annotation:"" 

Z5e5-

Z4e5 

2.3e5-

2.2e5 

2.1 e5 • 

2.0e5 

1.9«5 

1.8«5-

1.7e5 

1.6e5 

1.Se5-

1.4«5 

1.3«5 

1.2e5 

1.1«5 

I.OeS9.0e4 

8.0e4 

7.0e4 

6.De4-

5.De4-

4.0e4 

3.0e4 

^Oe4 

1.0o4 

Ftte: t l 01025b.wir 

0.0 l ^ s 

Sample T 

Calculat 

Acq. Dat 

Acq. Tim 

Modified 

RT KindoExpected 

Use Rela 

tion: 

d n 

RT: 

i v e 

n c ! 

KT: 

Unknown 

H/A 

115. 

10/26/2010 

4:;5:55 PM 

Y«s 

30.0 

12.6 

No 

I

Sample Name: 'b101025bO71' Sample ID: "GLP10^)1-02-09^)1 r Fite:"b101025b.wir 

Peak Name; "PFBS- Mass(ea); -299.0ra9.0 amu,299.0/80.0 amu' 

Comment* DALGW222R0100929{50X)- Annotation: " 

Sample Index: 71 

1.7e5 

1.6e5 

1.5e5 

1.4e5-

1.3e5 

1Ji«5 

1.1 eS 

1.0e5 

9.0»4-

B.0e4-

7.0e4 

6.0e4 

5.0e4 

4.0»4-

3.0e4 

Z0e4 

1.0e4-

0.0 JL. ^ 

I

Sample Name: -b101025b128- Sample 10: 'GLP1CM)1-02-0»O49-

Peak Name; -pFBS" Ma»«(B»): -299.0/99.0amu,299.0/80.0 amu" 

ConvTwnf DALGW328R0100S28{20X)- AnnotoSon: ~ 

Sample Index : 129 

Sample Type: 

File:-b101025b.wfr [Sample Name: "b101025b02r Sample ID: •08008-194-10' File: "b101025b.wir 

Peak Name: "PFHS- Mass{as}: -399.Qra9.0 amu,399.0/80.0 amu" 

Comment -5.0 ng/mL FC ttd in MM Q Wbter" Anrwtation: " 

tio. 

Modified: 

RT Window: 

Expected RT 

Use Relativ. 

N/A 

Heiijht: 

Start Ti 

End Tim? 

1.20e5 

1.15e5 

1.1 Oe5 

I.OSeSI.OOeS 

9.50e4 

9.00e4 

8.50e4 

6.0De4 

7.50e4 

7.00*4 

§- 6.S0e4 

^ 6.00e4 

I 5.50e4 

5.00e4 

4.50e4-

4.00e4 

3.50e4 

3.00e4 

Z50e4 

Z00e4 

1.50e4 

1.00e4 

5000.00 

0.00 

Sample Type: Standard 

Concentration: S.OO 

Calculated C 

Acq. Date: 

Acq. Tims: 

Modified: 

Proc. Algcri 

Min. Peak He 

Min. Psak wi 

Smoottiino Hi 

RT Window: 

E.".pactsd RT: 

I'se Relative 

Int- Type: 

Retention Ti 

Area: 

Height: 

Start Time: 

End Time: 

nc: S.o;-

10/25/2010 

10:5<:06 PH 

No 

hm: IntelliQ'jan 

ght: D.00 c 

ttl! 0.00 3 

•th: 0 po 

30.0 = 

H. 2 tn 

RT: No 

Valley 

tie: IJ. l m 

1655551 coun 

J.SSe.OOS c 

H.O a 

H . i m 

ID 12 

Time min 

Printing Time: 1:32:42 PM 

Printing Date: Tuesday, February 08, 2011 

Page 2 of 6 

Page 45 of 83 
*** Buster J2930203 

GLPIO-01-02; Interim Report 09 

Bat^Ra|ym?f effi%2'5§t^^^k?"d PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

Sampl e Tvpe : 

Concentration : 

Calculate d Cone : 

Acq. Date : 

Acq. Time : 

Modified : 

Proc . Algorithm : 

Min . Pea k Height : 

Min . Peak Width ! 

Smoothin g width : 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Tiisa : 

Area : 53< 

Height : 1 

QC 

20. 0 

17. 3 

10/2e/201 0 

3:27:2 7 AM 

Na 

IntelliQu a 

0.0 0 

0.0 0 

0 p 

30. 0 

14. 2 

No 

Valle y 

14. 1 

12*0 cou 

.ISetOOS 

I

Sampte Name: •b101025b034- Sampta ID: 'LCS-101020-4" Ftte: *b 101025b.wiff" 

Peak Name: 'PFHS' llAass(«s}: "399.0/99.0 amu.3g9.0/80.0 amijComment "20ppb LCS" Anrutation: ~ 

1.15e6-

I.IOeSI.OSeSI.OOeS9.50e5-

9.00e5-

8.50e5 

a.OOeS 

7.50e5-

7.00e5 

6.50e5-

6.00e5 

5.50e5 

S.OOeS 

4.50e5 

4.00e5-

3.50eS3.00e5 

2.S0e5 

ZOOeS 

1.50e5 

I.OOeS 

5.00e4 

0.00 

r

Sample Name: "b101025b045" Sample ID: "LCS-1D1020-10- File: -b101025b.vrtfr 

Peak Nanne: "PFHS- Masa(es): "399.0/99.0 amu.399.0/80.0 emu" 

Comment -20ppb LCS EOF" Annotation: " 

Sample Index : 45 

QC 

nq/raL 

Sampl e Type : 

Concentrati o 

Calculate d C 

Acq. Date : 

Acq, Time : 

llJdifiad : 

RT Window: 

Expncte d RT: 

Use Relativ e 

one : 

RT! 

OC 

0.0 0 

1.1 1 

10/26/201 0 

7:19:0 4 AM 

Yes 

30. 0 

14. 2 

No 

1 

|-

7.0e4 

6.5e4 

6.0e4 

5.5e4 

5.0»4 

4.5e4 

4.0e4 

3.5e4 

3.0e4 

Z5e4 

ZDe4 

1.5e4 

1.0o4 

SOOO.O 

DO 

14.12 

1 

Iu, 

A A . „ .<<^, 

•

Sample Name: "b101O2SbO49- Sannpte ID: "RO V*tor TN1CW311" File: "b 101025b.witT 

Peak Name: "PFHS' Uass(es): "399.0/99.0 amu,399.0/80.0 amiT 

Convnent 'Method Blank* Annotation: " 

Sample Index : 4 9 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: < 0 * 

Acq. Date : 10/26/201C 

Accj. Tima: 9:43:14 AM 

Proc . Alqoc i 

Min . Pea k He 

Min. Pea k Wi 

.hm: 

q h t 

•1th: 

Pmoothin g VJidth: 

RT Window: 

E.xpected RT: 

Uss Relativ e 

Int . Type : 

Retentio n Ti 

Area : 

Height : 

Star t Titne : 

End Time : 

KT: 

IntelliS u 

0.0 0 

0.0 0 

0 

30. 0 

14. 2 

No 

Valle y 

14. 1 

1365 CO 

;.70e+00 2 

14. 1 

14. 2 

an -

c p s 

poi n 

min 

unts 

c p s 

min 

min 

lOA 

3 

& 3000 

f 

1 2500 

Ki.lf...LU . I f -• ^. J. ..ft-^.J.a^... J4fa-^ -p '-"l-ll ^if 

I

Sampla Name: "b101025b050" Sample ID: "GLP1CK)1-02-0*O0r File: •b101025b.wir 

Peak Name: 'PFHS- M««»(o«): "399.0/99.0 amu,399.0/80.0 amu' 

Comment "DAL GW 203L 0100929 (20X)- Annotation: -

Sample Index : 50 

Saniple Type: Unknown 

Concentration : tl/A 

Calculate d Cone: 4Se. nq/n 

Acq. Date : 10/2S/2010 

Heiijlit: 

Star t T 

End Ti m 

Manual 

,e: 14.1 

70T4380 :• 

1.20e6 

1.15e6 

i.ioee 

1.05e6 

1.00eS 

9.50o5 

9.00eS 

6.50e5 

8.00e5 

7.50e5 

7.00e5 

6.50e5 

6.00e5 

5.50e5 

5.00*5 

4.50e5 

4.00e5 

3.50e5 

3.00o5 

2.50e5 

ZOOeS 

1.S0e5 

LOOeS 

5.00e4 

141 3 

14.00 . 

16.48 

10 12 14 16 

Time, min 

Printing Time: 1:32:43 PM 

Printing Date: Tuesday, February 08, 

Page 3 of 6 

Page 46 of 83 
•*• Buster J2930203 

GLPIO-01-02; Interim Report 09 

Bat^Ra!ym?f ?m%2'5EH<&#"d PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

[

Sampto Name:'b101O2SbO71- Sampta ID: •GLP1tW)1-02-<»«ir FJte: •b10102Sb,*rtr 

Peak Name: "PFHS" MaM<ec}: "399.0/99.0 aiTUJ.399.0/aO.O amiT 

Comment "DAL GW222R0100929 (50Xr Annolation:" 

Sample Type: 

Concentration : 

Calculate d Cone: 

Acq. Date : 

Acq. Tine : 

Modified : 

RT Windou: 

Expected RT: 

Use Relativ e RT: 

Int . Type: 

Retentio n Time: 

Unknown 

N/A 

ao7. 

10/26/2010 

J:25:5 5 PH 

Ves 

30. 0 

14.2 

No 

Manual 

!4. 1 

5an ^ Name: -b101025b128" Sample ID: 'GLPICHJI-02-09049^ File: -b10102Sb.\Mr 

Peak Name: "PFHS* Mau(es): "399.0/99.0 amu.399.0/SO.O amu* 

Comment 'DAL GW328R 0 100928 {20X)- Annotation; " 

Sample In< 

I'nki 

N/A 2.0eS 

1.ge5 

1.8e5 

1.7e5 

1.6e5 

1.5«5 

1.4e5 

1.3e5 

1.2e5-

l.leS 

1.0eS 

9.0e4 

8.004 

7.0e4 

6.0e4 

5.0e4 

4.0e4 

3.0e4 

Z0e4 

1.0e4 

14.10 

, ,../V,.. 

16 18 

I

Sample Name: ^10102^)021" Sample ID: "06008-194-10* Fde: "b10102Sb.>Mr 

Peak Name: "PFOS" Mass(ea): '499.0/99.0 amu.499.CV80.0 amu.499.0/130.0 amt/* 

Convnent "5.0 ng/mL FC sU in MS Q V^ter' /Annotation: 

Sampl e Index : 21 

Sampl e Type : Standar d 

Concentration : 5,0 0 nq/mL 

Calculate d Cone : 4,9 0 nq/(nL 

Acq. Date : 10/25/201 0 

Acq. Time : 10:54:0 6 FH 

Sample Name:-b1O102SbO34- San^ta ID:'LCS-101020-4" Fle:-b101025b.wir 

Peak Name: TFOS" kAass(es}: "499.0/99.0 ai 

Comment *20ppb LCS" Annotation: -" 

Sample Index : 34 

u,499.Dn30.0amir 

Nois e Perce n 

Ba.-e. S'jb. W 

Peak-split . 

Raport Larg e 

Min . Peak He 

Min . Peak Wi 

Jraoothin g Wi 

RT Window: 

Expecte d RT: 

Use Relativ e 

Int . Type : 

Retentio n Ti 

Area : 

Height : 

End Time : 

indow 

"act o 

st Pe 

ight : 

dtii : 

dtli : 

RT: 

50 

l.OO 

c: 1 

k: No 

0.0 0 

0.0 0 

0 

30. 0 

15. 1 

No 

Valle y 

15. 0 

1420B22 cou 

3 31etO0 5 

14. 9 

15. 3 

Acq. Date : 10/2S/201 0 

Acq . Tima : 3:27:2 7 AK 

Modified : Ho 

Proc . Algcrithm : Int a 11 iO'Jan -

Nois e Percentage : 50 

Base . Sub . Window: 1.00 m 

Peak-Split . Factor : 1 

Report Largest Peak : No 

MOII 

n 

Hin . Pea t Height : 0.0 0 cp s 

I4in. Peak width : 0.0 0 

RT Window: 50. 0 se c 

Expecte d RT: 15. 1 min 

Uae Relativ e RT; No 

Int . Type : Valle y 

Area : 4£3679 a counts 

Height : 1.05e+00 6 cp s 

End Time : 15.: ' min 

e c 

p o m 

J 

a 

I.OOeS 

9.50e5 

9.00«5 

8.50e5 

7.00e5 

S.50e5 

5.00e5 

4.50e5 

4.00e5 

3.50e5 

3.00e5 

Z50e 5 

2.00<.5 

1.50e5 

I.OOeS 

5.00e4 

0.00 

12 14 16 

Printing Time: 1:32:43 PM 

Printing Date: Tuesday, February 08, 2011 

Page 4 of 6 

Page 47 of 83 
Buste r J2930203 

GLP10-01-02; Interim Report 09 

Bat^3|ym?f ?ffi%2'5gH§band PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

I

Sample Name: "b101025b045- Sample ID: •LCS-101020-10- Filo: -b1D1025b.wir 

Peak Name: 'PFOS' Ma«s(es): '499.0/99.0 amu,499.0/80.0 amu,499.0/130.0 amu' 

Comment '20ppb LCS ECF" Annotation: " 

.•'ample Index: 45 

Sample Type: yC 

Concentration: IS. 6 ng/mL 

Calculated Cone: 21.5 ng/mL 

Acq. Date: 10/2€/2010 

Acq. Til 

Modified 

RT Windoi 

Expected 

Uss Rela! 

Height: 

Start T 

End Tim. 

7:1S:04 AM 

8.0eS 

7.SeS 

7.0eS 

6.5e5 

6.0e5 

5.5e5 

5.0e5 

4.S«5-

4.0e5 

3.Se5 

3.0e5^ 

2.5e5-

2.0e5 

I

Sampte Name: "b1O1025bO49- Sample ID: "RO Water TN1(H)3ir File: •b101025b.vwr 

Peak Name: 'PFOS' Mass{as): '499.0/99.0 anui,499.W80.0 amu.499.0/130.0 amu" 

Comment "Method Blank" Annotation: ~ 

Sample Inde.»c: 49 

Sample Type: Unknown 

Concentration: N/A 

Calculated Cone: -. 0 

Acq. Date: 10/26/2010 

Acq. Time: e:4J:14 AM 

1700 

Modified: 

Proc. Algcri 

Nx-:jise Percen 

hm: In 

age: 

Base. Sub. Window: 

P^ak-Split. 

R^purt Large 

Min. Peak He 

Hin. Peak Wi 

Smoothing Wi 

RT Window: 

E-pected RT: 

Use Relative 

Int. Type: 

Retention Ti 

Area: 

Height: 

Start Time: 

End Time: 

Factor: 

;t Peak 

ght: 

ith: 

ith: 

RT: 

V 

ne: 

92 

1.7 

No 

telliQua 

50 

1.00 

1 

Nc 

0.0 

0.0 

15.1 

No 

alley 

15.0 

4 0 CO 

5e.O03 

15.0 

15.1 

" 

m 

m 

n 

" 

m 

HQII 

n 

c p s 

n 

^ 

3 

c p s 

luin 

p o m 

t 

a 

IDUU 

1500-

1400-

1300 

1200-

1100 

1000-

900-

I

Sample Name: "b101025bOSO' Sample ID: 'GLP1C>O1'D2-O&O01- File: 'b101025b.Mifr 

Peak Nama: "PFOS" Mass(es): "499.0/99.0 amu,499.0/80.0 amu,499.0/130.0 amu" 

Comment-DAL GW203L 0100929 (20X)" Annotation:-

• Type : 

.e: 15.0 

10222554 Zl 

1.25et006 

1.25e6 

1.20e6 

1.15e6 

1.1 OeS 

1.05e6 

1.00e6 

9.50e5 

9.00e5 

8.50e5: 

aooes 

7.50e5 

g^ 7.00e5 

^ 6.50e5 

I 6.00e5 

- 5.50e5 

5.00e5 

4.50e5 

4.00e5 

3.50e5 

3.00e5 

ZSOeS 

ZOOaS 

I.SOaS 

1.00*5 

5.00e4 

0.00 

I

Sample Name: "bl01025b07r Sample ID: "GLP1OO1-02«»01T File: "b101025b.wir 

Peak Name: 'PFOS' MaM{es): '499.0/99.0 amu,499.0/80.0 amu,499.0/130.0 amu" 

Comment 'DAL GW222R 0 100929 (50X)' Annotation: " 

Sample Index: 71 

Sample Type: I'nknown 

Concentration: N/A 

Calculated Cone: 1130. ng/mL 

Acq. Date: 10/26/2010 

Acq. Tima: 4:25:55 PM 

Modified: Yes 

RT Window: 30.0 sec 

Expected RT: 15.1 min 

Int. Type: Manual 

Retention Time: 15.0 

Area: 6016061 co^ 

Height: 7.JPevOOS 

7.0e5 

6.5e5 

6.0e5 

5.5e5 

5.0e5 

4.5e5 

4.0*5 

3.5e5 

3.0e5 

Z5e5 

Z0e5 

1.5e5 

I.OeS5.0e4 

0 0 

15.02 

14.87^ 

, , , , I , , , 

Printing Time: 1:32:43 PM 

Printing Date: Tuesday, February 08, 2011 

Page 5 of 6 

Page 48 of 83 
GLP10-01-02; Interim Report 09 

Buster J2930203 Bat^P^lym?^ ?f(ft%2'5§H§i?nd PFOS in Groundwater 

Quarterly Groundwater sampling - Sept 2010 

r

Sample Name: 'b101025b128" Sample ID: 'GLPl(W)1-02-0&O49' File: •b101025b.'Mfr 

Peak Name: 'PFOS' llAass(es}: '499.0/99.0 amu,499.0^0.0 amu.4g9.0/130.0 amu" 

Comment -DAL GW 328R 0 100928 (20Xr Annotation: 

Sample Index : 129 

Sample Tvpe: Unknown 

Concentration: N/A 

Calculated Cone: 171. ng/mL 

Acq. Date: 10/27/2010 

Acq. Time: 12:25:42 PM 

Modified: Yes 

RT Window: 30.0 sec 

Expected RT: 15.1 min 

Use Relative RT: Ko 

Int. Type: Manual 

Retention Time: 15.0 min 

Area: 2419539 counts 

Heiijht: 2.79e*005 cps 

End Time: 15.2 min 

i 

! • 

1 

Z7e5-

Z6e5-

2.5e5-

Z4e5-

2.3e5-

Z2oS2.1 eS 

Z0e5-

1.9e5 

1.8e5-

1.7e5-

1.6e5 

I.SeS1.4e5-

1.3e5-

1.2e5 

l.laS 

I.OeS 

9.0e4' 

8.0e4-

7.0e4 

6.0e4-

5.0e4-

4.0e4-

3.0e4 

2.0e4 

1.0e4 

Printing Time: 1:32:44 PM 

Printing Date: Tuesday, February 08, 

Page 6 of 6 

2011 

Page 49 of 83 
Buster J2930203 

GLP10-01-02; Interim Report 09 

Bat'&RalymPf ?m%2?§H§i^"d PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

b101025b.rdb (PFBS): "Quadratic" Regression ("1 /x" weigliting): y = -1.43e+003 x*2 + 3.85e+005 x + 2.51e+004 (r = 0.9995) 

2.5e7-

2.4e7-

2.3e7-

2.2e7-

2.187-

2.0e7-

1.9e7-

1.8e7-

1.7e7-

1.6e7-

1.5e7-

1.4e7-

1.3e7-

1.2e7-

1.1e7-

1.0e7-

9.0e6-

8.0e6-

7.0e6-

6.0e6-

5.0e6-

4.0e6-

3.0e6-

2.0e6-

1.0e6-

0.0-

m. 

/ / 

/ 

/ 

/ ' 

•.-' 

/ ' 

y 

X 

^ y ^ 

y 

/' 

,/'' ' 

'•'' ' 

/ ' 

,,.--'''''• 

^''' 

,^''' 

^.yy -

._ 

.y-' ' 

^..yy^ ' 

_ y ^ • 

,^-^ ' 

" ^ 

^ ^ 

_,,.^-^"' ' 

• 

--" ^ 

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 Ti 

Printing Da 

me: 1:33:02 PM 

te: Tuesday, February 08, 2011 

Page 1 of 1 

Page 50 of 83 
Buster J2930203 

GLP10-01-02; Interim Report 09 

Bat^P^lym?* ?m%2?§H4#"d PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

b101025b.rdb (PFHS): "Quadratic" Regression ("1 / x" weighting): y = -1.36e+003 x'^2 + 3.35e+005 x + 9.93e+003 (r = 0.9997) 

2.1e7 

2.0e7-

1.9e7-

1.8e7-

1.7e7 

1.6e7 

1.5e7 

1.4e7 

1.3e7 

1.2e7 

1.1e7 

1.0e7 

9.0e6-

S.OeS7.0e6 

6.0e6 

5.0e6-| 

4.0e6 

3.0e6 

2.0e6 

1.0e6 

0.0 

10 15 20 25 30 35 40 45 50 55 60 80 85 90 95 100 

Concentration, ng/mL 

65 70 75 

Printing Time: 1:33:18 PM 

Printing Date: Tuesday, February 08, 2011 

Page 1 of 1 

Page 51 of 83 
"* Buster J2930203 

GLPIO-01-02; Interim Report 09 

Bat^Ra!ym?f em^^lEHa^and PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

b101025b.rdb (PFOS): "Quadratic" Regression ("1 / x" weighting): y = -1.03e+003 x'^2 + 2.89e+005 x + 3.08e+004 (r = 0.9997) 

1.9e7 

1.8e7 

1.7e7 

1.6e7^ 

1.5e7 

1.4e7H 

1.3e7 

1.2e7 

1.1e7 

1.0e7 

g 9.0e6 

8.0e6-

7.0e6-

6.0e6-

5.0e6 

4.0e6 

3.0e6-

2.0e6-

1.0e6 

0.0 

y 

/ 

• , / 

/ 

/ 

, ^ 

10 15 20 25 30 35 40 45 50 55 60 

Concentration, ng/mL 

65 70 75 80 85 90 95 100 

Printing Time: 1:33:33 PM 

Printing Date: Tuesday, February 08, 2011 

Page 1 of 1 

Page 52 of 83 
Buster J2930203 

GLP10-01-02; Interim Report 09 

Bat^Ra|ym?f ^fM-olsEt^cat^nd PI'OS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

I Sample Name:'b101108b026' Sample ID: 

I Pealc Name: "PFSS" Masses): "299.0/99.0 

• Comment "2.5 nflftnL FC sld in Mill Q Water" 

Sample Index : 26 

Sample Type; Standard 

Concentration : 2.SO ng/mL 

Calculate d Ccnc: 2.60 nq/n L 

Acq. Date : 11/9/2010 

Acq. Time: 10:15:16 PM 

Min. Peak Hidt h 

Fraoothin g Viidth 

RT Window: 

Expecte d RT: 

Use Relativ e RT 

Int . Type : 

Retentio n Time : 

Area : 1 

Height : 

Star t Time : 

End Tim^ : 

9 

2 

0.0 0 

0 

30. 0 

12. 5 

No 

Valle y 

12. 6 

.033 c 

71e+00 5 

12. 5 

12. 5 

"08008-194-9" File: "b101108b.wir 

rui,299.0/8O.0 amu' 

/Annotation:" 

2.7*5 

2.6eS 

2.5e5 

2.4a5 

2.3e5 

2.2e5 

2.1e5 

2.0eS 

1.9e5 

I.BeS 

1.7e5 

1.6e5 

1.5e5 

1.4e5 

1.3a5' 

1.2o5 

l.leS 

1.0e5 

9.0e4 

8.0e4 

7.De4 

6.0e4 

5.0e4 

4.0e4 

3.0e4 

2.0e4 

1.0e4 

•

Sample Name: 'blOl 108b033- Sample ID: 'RO Watar TN10-03ir File: 'blOHOSb.wiT 

Pealc Name: "PFBS- Mass(es): *299.0/99.0 amu.299.W80.0 amu" 

Comment -Method Blanl^ Annotation:" 

Sample Index : 32 

Sample Type: Unknovn 

Concentration : 

Acq. Date : 

Acq . Time : 

ModiEiad : 

Proc . Algorithm : 

Hin . Paak Haighi 

Smoothin g Width : 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

int . Type : 

Retentio n Time : 

Heigtit : 

Star t Time : 

End Time : 

M/A 

11/9/201 0 

12:^2:3 5 AM 

No 

Int^lliQua n - IQA 

: O.DO cp s 

0 point s 

30. 0 se c 

12. 6 min • 

Ho 

Valle y 

llSi O counts 

3.52e»00 3 cp s 

12. 5 min 

12.-J min i 

. : 

3400 

2800 

2600 

2400 

2200 

2000 

1600 

1400 

1200 

1000 

(

Sample Name: -b101108b036" Sample ID: " 

Peali Name: 'PFBS* Uass(es): "299.0/99.0 ai 

Comment "2ppb LCS' Annotation: "• 

Sample Index : 36 

Sampl e Tvpe : 

Concsntcation : 

Calculate d Cone : 

Acq. Date : 

Acq. Time : 

Modified : 

Proc . Algorithm : 

Min- Peak Heigh t 

Min. Pea k Hidth : 

Smoothin g wi.ith : 

RT Window: 

E.tpecta d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time : 

gc 

2.0 0 

2.3 5 

ll/9/20l ( 

ng/mL 

ng/mL 

1:4 5:44 AH 

No 

IntelliO u 

0.0 0 

0.0 0 

0 

30. 0 

12. S 

No 

Valle y 

12. 6 

Area : 1094142 co 

Height : 2 

Star t Time : 

End Time : 

.52e+0OS 

12. 5 

12. 9 

an - I S 

c p s 

point s 

s e c 

min 

unts 

min 

min 

2.5e5 

2.4eS 

2.3e5 

2.2e5 

2.1 eS 

2.0e5 

I.SeS 

I.eeS 

1.7e5 

1.6e5 

1.5e5 

1.4e5 

1.3e5 

1.2eS 

l.leS 

1.0e5 

9.0e4 

8.0e4 

7.0e4 

6.0e4 

S.0e4 

4.0tt4 

3.0e4 

2.0e4 

1.0e4 

0.0 

I

Sampte Name:-b101108bO4r Sample ID: "LCS-101020-7* File: "blOIIOSb.wiffPeak Name: "PFBS" Mass(es): "299.0/99.0 amu.299.0/80.0 amu" 

Comment *^p b LCS ECF" Annotation: "" 

Sampl e Index : A I 

Sampl e Type : QC 

Concentration : 0.0 0 ng/mL 

Calculate d Cone : •' 0 

Acq. Date : 11/9/201 0 

Acq. Time : 4 :13:1 4 AM 

Modifi i Ho 

Proc . Algcrithm : 

Min . Peak Heigh t 

Hin . Pea k Width : 

Sisoothin g Width : 

RT window: 

E^:pect9d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time : 

Area : 

Height : 

Intell i 

: 0.0 0 

0.0 0 

0 

30.1.1 

12. 6 

No 

Valle \ 

12. 6 

1J55 9 

;.99e*0 0 

Data printed by STW 

Printing Time: 12:29:11 PM 

Printing Date: Tuesday, March 22, 2011 

Page 1 of 4 

Page 53 of 83 
Buste r J2930203 

GLP10-01-02; Interim Report 09 

Bat^Ra!y|fe?f ?f(ft?-o'8EHc?^#nd PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

I

Sample Name: -b101108b070' Sampte ID:"GLP10O1-02-0&<l3r File: -blOIIOBb.wir 

Peak Name: 'PFBS' MasK(es): -299.0/99.0 amu,299.0/80.0 anuT 

Commont"DALGW317L0100924' /Annotation: " 

ample Index : 70 

ample Type; 

N/A 

Calculated Cone: 0.0392 ng/mL 

Acq. Date: 11/9/2010 

Acq. Time: 1:41:51 PH 

Algorithm: Intellit'uan - : 

eak Height: 0.00 cps 

eaK Width: 0.00 sec 

1.4c 

RT Window: 

Expected RT: 

Use Relative RT 

Int. Type: 

Retention Time: 

Area: 

Height: 

Start Time: 

End Time: 

30.0 

12.5 

No 

Valley 

12.6 

61322 c 

1.39e+004 

12.5 

12.7 

I" 7000.0 

6000.0-

5000.0 

8.66 iL 

...It •» ,i. eA^a h >Jtjlli Ih < 111 J I ftiwl 

I

Sample Name; "bl01108b026" Sample ID: "08008.194-9" File: "b101108b.wiir 

Peak Name: "PFHS" Mass(as): "399.0/99.0 amu,399.0/80.0 amu" 

Comment "2.5 ng/mL FC std in Milli Q Water" 

ample Index : 26 

ample Type: Standar d 

Concentration 

Calculated Co 

Acq. Daca: 

Acq. Time: 

Kodified: 

Proc. Algocit 

Hin. Peak Hei 

Hin. Peak Wic 

m : 

q h t 

t h : 

Smoothing Width; 

RT Window: 

Expected RT: 

2.50 

2.56 

ll/q/20 ! 

10:15:19 

Ho 

ng/mL 

ng/mL 

i 

PM 

Intelli0.jan - IQ 

0.00 

0.00 

0 

30.0 

14.2 

c p s 

points 

min 

Area: 

Height: 

Stsrt Time: 

End Time: 

10:?9310 

2.52 = 

1 

I 

Sample Index : 

Sample Tvpe: 

Concentration : 

Calculate d Cone 

Acq. Date : 

Acq. Tima: 

33 

Unknown 

N/A 

< 0 

ll/S/201 0 

12:42:35 AH 

Modified: Ko 

Proc. Algorithm: IntelllOuan - IQA 

Min. Peak Height; 0.00 cps 

Min, Peak Width: 0.00 sec 

Smoothing Width: 0 points 

RT Window; 30.0 sec 

E.tpected RT: 14.2 ntin 

Use Relative RT: No 

I

Sample Name: "b101108b033' Sample ID: "RO WatsrTN1(M)3ir File; "blOllOab.wifr 

Peak Name: "PFHS" Massfes): "399.0/99.O amu,399.0/80.0 amu" 

Comment "Method Blanl^ Annotation: ** 

3400 

3200 

3000-

2800 

2600 

2400-

2200-

2000 

1800-

1600-

1400 

1200 

1000 

800 

I Sample Name: "blOl 108b03r Sampta ID: 'LCS-101020-2" File: "blOllDSb.wir 

Peak Name: 'PFHS" Mass{es); "399.0/99.0 amu.399.a/80.0 amu" 

I Comment "2ppb LCS" Annotation; "* 

Int. Type: 

Retention 

Area: 

Height: 

Start Tim. 

End Time: 

Valley 

5J5& counts 

1.266*003 cps 

14.2 min 

Sample Type: 

Concenrratioi 

Calculated Co 

Acq. Datrt: 

Acq. TifUflJ 

QC 

2.00 ng/mL 

2.37 ng/mL 

11/9/2010 

1:45:44 ftM 

Smoothing width: 

RT Kindo-J: 

Expected RT: 

iiiL,i..jii|tai,mt<ii 

2.3e5 

2.2e5 

2.1 e5 

Z0e5 

1.9e5 

I.BeS 

1.7eS 

I.eeS 

I.SeS' 

1.4eS 

1.3eS 

1.2e5 

l.leS 

l.OeS 

9.0e4 

8.0e4-

7.0e4 

6.0e4 

S.0e4 

4.0e4 

3.0e4 

Z0e4 

1.0e4 

GO 

14 33 

i 16.30.^;,,^16,S018.45 

12 14 16 IS 20 

Data printe d by STW 

Printin g Time: 12:29:1 2 PM 

Printin g Date : Tuesday, March 22, 2011 

Page 2 of 4 

Page 54 of 83 
-* Buster J2930203 

GLP10-01-02; Interim Report 09 

Bat^Ra|ym?f ?ffl?'o'8§H<Si?"d PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

•

Sample Name: 'b10l108b04r Sample ID: 'LCS-101020-7" File: -blOIIOBb.wir 

Peak Name: "PFHS" Masses): "399.0/99.0 amu,399.0/80.0 amu" 

Comment -2ppb LCS ECF" Annotition: ~ 

Sample Type 

Concentrati< 

QC 

0.0 0 

0,10 0 

11/9/201 0 

4:13:1 4 AM 

thm: IntelliQua i 

• Sampla Name;-'b1011O8bO70" Sample ID:'GLPiabl-02-09O37" File;"b101108b.wifr 

I Peak Name: "PFHS" Mass(es); "399.0/99.0 amu.399.0/80.0 amiT 

• Comment-DALGW317L0100924" Annotation:-

Sample Index : 70 

RT Wir 

Expeci 

eak Height; 

eak Width: 

ing Width: 

Valley 

49765 c 

1.00e4 

9500.00 

gooo.w 

8500.00 

8000.00 

7500.00 

7000.00 

6500.00 

6000.00-

". 5500.00 

I 5000.00 

" 4500.00 

4000.00 

3500.00-

3000.00 

2500. W 

2000.00-

1500.00 

1000.00 

500.00 

0.00' ] . . ,_ 1 - L-Y " .. ....f^*fa-ji..*.-J[fi ^ 

Sampl e Type : 

Concentration ; 

Calculate d Cone : 

Ac4 . Date : 

Acq. Time : 

Modified : 

Proc . Algcrithm : 

Hin . Peak Heigh t 

Hin . Pea k Width : 

Smoothin g Width : 

RT Window; 

Expecte d RT: 

Use Relativ e RT: 

I'nknovn 

H/A 

0.23 6 ng 

U/9/201 0 

1:41:5 1 PM 

No 

IntelliQ'ia n -

: 0.0 0 cp s 

0.0 0 se c 

0 poin t 

30. 0 se c 

14. 2 min 

Ho 

Int . Type : Vaile y 

Retentio n Time : 14. 3 min 

Area : 103937 counts 

H-iight : 2.37ei00 4 cp s 

Star t Time : 14. 0 min 

End Time : 

mL 

IQA 

1 

1 

Z3e 4 

2.2e4 

Zle 4 

2.0e4 

1.9e4 

1.8e4 

1.7e4 

1.6e4 

1.5e4 

1.4e4 

1.3e4 

1.2e4 

1.1 e4 

1.0»4 

9000.0 

8000.0 

7000.0 

6000.0 

50OO.0 

4000.0 

3000.0 

20OO.0 

1000.0 

I SampleNan>e:-bl01106b026' 

Peak Name:-PFOS- Mass<efi): 

I Comment -2.5 nglM. FC std in h 

Concentrati o 

Calculate d C 

Acq. Date ; 

Acq . Time : 

Modified : 

Proc . Algor i 

Nsis e Perce n 

Ba:-e . Sub . W 

: 2.5 0 

n c : 2.5 1 

ll/a/201 0 

nc)/mL 

ng/mL 

10:15:i e PH 

No 

hm: IntelliQ u 

age : SO 

ndow: 1,00 

Peak-Split . Factor : 1 

Report targ e 

Min . Peak He 

t Peak : Nc 

n - MQ 

min 

ght : 0.0 0 cp s 

Min . Peak Width : 0.0 0 se c 

Smoothin g Width : 0 

RT Window: 

Expecte d RT: 

Use Relativ e 

Int . Type : 

Retentio n Ti 

Area ; 

Height : 

?tar t Time : 

End Time : 

30. 0 

15-4 

RT: Ho 

Valle y 

e : 15. 4 

963382 CO 

2.516+00 5 

15. 3 

15. S 

po 

s e c 

min 

min 

n ts 

c p s 

min 

Sample ID: -08006-194-a^ 

-499.0/99.0 anw.499.Q/80.0 ai 

na Q Water" /Vmotation:"" 

iSeSZ4e5-

Z3e5 

Z2e5 

Z1e5-

2.0e5-

1.9o5-

1.ae5-

1.7e5-

I.SeS1.5e5-

1.4e5 

1.3e5 

1.2«5-

l.leSl.OeS 

9.0e4 

S.0e4' 

7.0e4 

6.0e4 

5.De4 

4.064 

3.0»4 

Z0»4 

1.0e4' 

0.0 

I

Sample Name;-b10110SbO33" Sampte 10: "ROWMerTNICHQir Fiie:"bl01108b.wir 

Peak Name: 'PFOS" Massfes): "499.0/99.0 amu.499.(V80.0 amu.499.(V130.0 amiT 

Comment "Metiyid BtanlT Annotation: *" 

Sample Index : 33 

Sample Type: I'nknown 

Concentration : N/A 

Calculate d Cone: 0.0125 ng/mL 

Acq. Date : 11/9/2010 

R^poi t Larges t Pe; 

Pea k Height : 

Hin . Pea k Width : 

Smoothin g width : 

RT Window; 

Expecte d RT: 

Use Relati - RT: 

21531 =ai 

4 . S6e*00 3 

15. 2 

15. 5 

14 16 18 

Data printed by STW 

Printing Time: 12:29:12 PM 

Printing Date: Tuesday, March 22, 

Page 3 of 4 

2011 Page 55 of 83 
Buster J2930203 

GLPIO-01-02; Interim Report 09 

Bat'^Ra!ym?f ?m?'olgt^c&t?"d PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

I

San ^ Name: "b101108b03r Sample ID: 'LCS-101020-r 

Peak Name: 'PFOS" Macs(as}: "499.099.0 amu,499.0/80.0 a: 

Comment "2ppb LCS" Annotation:" 

Sampl e Type : QC 

ellitua i 

BO 

1,00 

Peak-Split . Facto r 

Repor t Largest Pea 

Hin , Peak Height : 

Hin . Pea k Hidth : 

Smoothin g Hidth : 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time : 

Area ; S51 

Height ; 2 . 

Star t Time : 

End Time : 

1 

.: Ho 

0 . 

0 . 

0 

30. 0 

15. 4 

No 

'alle y 

15. 4 

73 c 

4e+00 5 

15, 2 

15. 6 

2,2*5 

Z1e 5 

ZOeS 

1.9e5 

1.8e5 

1.7e5 

1.6e5 

1.5e5 

1.4e5 

1.3e5 

1.2e5 

1.1.5 

I.OeS 

9.0e4 

S.0e4 

7.0e4-

6.0*4 

5.0e4 

4.0e4 

3.0e4 

Z0e 4 

1.0*4 

153 5 

15.2 U iil ^ 18.45 

•

Sample Name: -b101108b04r Sample ID: -LCS-101020-r File: -blOIIOSb.wrtT 

Peak Name: 'PFOS- Man<as}: -499.0/99.0 amu,499.0/80.0 amu,499.Qn 30.0 amu' 

Comment -2ppb LCS ECF" Annotation; ~ 

Sample Index : 43 

Sample Type: QC 

Calculate d Cone 

Acq. Date : 

Acq. Time : 

Modified : 

BT Windo-.v: 

Expecte d RT: 

Use Relativ e RT 

Int . Type ; 

1.58 ng/mL 

2.1 4 ng/mL 

11/9/201 0 

4:13:1 4 AM 

Yes 

30. 0 se c 

15. 4 min 

No 

Manua l 

15, 3 min 

Area : S30S69 counts 

Height : 1.42e'-00 5 cp s 

Star t Time : 

End Time ; 

14. 5 min 

15. 5 tnin 

& 

t 

1 

1.4*5 

1.3eS 

1.2e5 

1.1*5 

1.0*5 

9.0e4 

S.0e4 

7.0e4 

6.0e4 

5.0e4 

4.0e4 

3.0*4 

I

Sample Name: -b1O1lO6bO70' Sample ID; -GLP1(H)1-02-0»<l37- File; "blOIIOBb.wir 

Peak Nama: "PFOS" Mats(es): '499.0/99.O amu.499.(V80.0 amu,499.0/130.0 amu" 

Comment "D/U.GW317L 0 100924" /Annotation: " 

Z7e4 

ZSe4 

Z5e4 

Z4e4 

2.3e4 

Z2e4 

Z1e4 

Z0e4 

1.9e4 

1.8e4 

1.7e4 

1.6e4-

1.5*4 

Sampl e Type : 

Concentration : 

Calculate d Con 

Acq. Date : 

Acci. Time ; 

Modified : 

RT Window: 

Expecte d RT: 

Un known 

K/A 

: : 0.41 5 

11/9/2 0 

1:41:5 1 

Yea 

30, 0 

15. 4 

0 

PI1 

1.4*4 

1.3e4 

1.2e4 

1.1e4 

1.0e4-

9000.0 

8000.0 

7000.0-

6000.0-

5000.0 

4000.0 

3000.0 

2000.0 

1000.0-

0.0 LJK^ 

10 12 14 16 18 20 

Data printed by STW 

Printing Time: 12:29:13 PM 

Printing Date: Tuesday, March 22, 2011 

Page 4 o f 4 

Page 56 of 83 
Buster J2930203 

GLPIO-01-02; Interim Report 09 

Bat^R^lyiJ^pf ffftq,^§H^^j^nd PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

• blOl 108b.rdb (PFBS): "Quadratic" Regression ("1 /x " weighting); y = -2.33e-H003 x'^2 -i- 4.57e-H005 x + 2.06e-^004 (r = 0.9998) 

1.7e7 

1.7e7-

1.6e7-

1.5e7-

1.4e7-

1.3e7-

1.2e7-

1.1e7-

1.0e7-

i 9.0e6-

8 

S 8.0e6-

70e6-

6.0e6-

5.0e6-

4.0e6-

3.0e6-

2.0e6-

1.0e6-

0.0-

,-''' 

---' 

//'" ' 

y 

, / 

X 

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

Concentration, ng/mL 

.--^' 

^ y y 

34 36 

^^- ^ 

38 

/-^'• ' 

40 

y ^ ' 

42 44 

,/-' " 

46 

, 

48 

,-'•'••' 

50 

Data printe 

Printing Ti 

Printing Da 

d by STW 

me: 12:26:25 PM 

te: Tuesday, March 22, 2011 

Page 1 of 1 

Page 57 of 83 
**• Buster J2930203 

GLPIO-01-02; Interim Report 09 

Bat^R^lyiJ^pf ffftq,olg§HS^^and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

• blOllOSb.rdb (PFHS): "Quadratic" Regression ("1 /x " weighting): y = -2.12e-H003 x'^2 + 4.05e-K005 x + 8.31e-K003 (r = 0.9997) 

1.5e7-

1.4e7-

1.3e7-

1.2e7-

1.1e7-

1.0e7-

9.0e6-

c 8.0e6-

8 

2 7.0e6-

< 

6.0e6-

5.0e6-

4.0e6-

3.0e6-

2.0e6-

1.0e6-

0.0-

•,/-'"' 

X'" 

y ^ 

X / " -

y 

y 

/ 

> 

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 

Concentration, ng/mL 

f - 7 '•• 

36 

yy- ^ 

38 

,_--

40 

y-^'' ' 

- > 1 

42 

^,..-'' 

44 

,^'-"' 

46 

^ 

7 

48 

y - ^ 

•^—I — 

50 

Data printed by STW 

Printing Time: 12:26:46 PM 

Printing Date: Tuesday, March 22, 2011 

Page 1 of 1 

Page 58 of 83 
Buster J2930203 

GLPIO-01-02; Interim Report 09 

Bat^Ra|ym?f ef(ft?.ol8iH&ba"d PI'OS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

• bl01 lOSb.rdb (PFOS): "Quadratic" Regression ("1 /x " weighting): y = -1.83e-H003 x'^2 + 3.84e-H005 x + 1.66e-^004 (r = 0.9997) 

1.5e7 

1.4e7-

1.3e7-

1.2e7-

1.1e7-

1.0e7-

9.0e6-

42 8.0e6-

c 

8 

CD 7.0e6-

< 

6.0e6-

5.0e6-

4.0e6-

3.0e6-

2.0e6-

1.0e6-

0.0-

y^ 

/ ' / 

•/-'"'' 

,/'' 

y 

y 

y 

y ' 

y ^ 

x' 

y 

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 

Concentration, ng/mL 

y ' ' 

1 

36 

.•••-'•' ' 

38 

y ' ^ 

40 

. - -

1 

42 

' ^ 

"• 1 1 

44 

1 

46 

y48 

,.-•# • 

50 

Data printed by STW 

Printing Time: 12:27:05 PM 

Printing Date: Tuesday, March 22, 2011 

Page 1 of 1 

Page 59 of 83 
Ginger AG01330509 

GLPIO-01-02; Interim Report 09 

Res^Pfl'^StfFa^.i^fi<aS..md PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

I

Sample Name: 'g110211a022- Sample ID: '10007-27-11' File; 'g110211a.wir 

Peak Name; 'PFBS" MaM<ea): "299.0/99.0 amu.299.0/80.0 amtT 

Comment *10 ng/mL FC std in MiS Q water' Anrwbtion; 

Sample Index : 22 

Sample Type: Standar d 

Concentration : 10.0 nq/nL 

Calculate d Cone: 9.75 ng/mL 

Acq. Date : i/12/201 1 

Acq. Time: ixlAib A MA 

Sampte Nanne: -9110211 a026" Sampte ID: 'Solvant BtanlT 

Peak Name:-PFBS* Ma»«(e«):'299.0ra9.0amu.299.CV80.0 

Comment 'Millt Q \AMer TNII-OOSr /Annotation: " 

Sample Index: 29 

Sample Type: I'nknown 

Concentration: H/A 

Calculated Cone: -. 0 

Acq. Date: 2/12/2011 

Acq, Time: ^:02:51 AM 

Modified: 

RT Window: 

Expected RT: 

use Relative 

int . Type: 

Retention Ti 

Area: 

Haight: 

Start Time: 

End Time: 

RT 

i 

Ve. 

3 0 . 

10 

No 

llanu 

10 

97397 

1J20CI0 

10 

n 

6 

1 

a 

s 

J 

Modified: 

Proc. Alg^-rithm: 

Noise Percentage: 

Base. Sub. Hindoo 

PeaK-Split. Facto 

No 

nt^lliQuan 

SO 

1.00 

: 2 

Raport Largest Paak: No 

Hin. Peak Haight: 

Hin. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

I'se Relative RT: 

Int. Type; 

Retention Time: 

Area: 

Height: 

Start Time: 

End Time: 

0.00 

0.00 

- HQII 

min 

c p s 

poin 

?0.0 3ec 

10.6 m 

Mo 

valley 

10.6 m 

e03 =oun 

US. cp:: 

10.S m 

10.7 m 

n 

" 

" 

s 

s. 

600 

I

Sample Name: 'g110211aO3r Sample ID; 'LCS-11021&«- File; 'gl10211a.«wfr 

Peak Name; -pFBS" Uass<es): "299.0/99.0 amu,299.0:180.0 amu" 

Comment 'Sppb LCS" Annotation; ~ 

Sample Index: 33 

Sample Type: gC 

Ccncentrat 

Calculated 

Acq. Date; 

Acq. Time: 

Modified: 

RT Window: 

Expected RI 

o n : 

Cone 

4.9B ng/mL 

: 5.52 ng/mL 

2/12/2011 

6:32:57 AH 

Ye3 

30.0 sec 

10.S rain 

Hcig.'-.r; 

Start Timi 

End Tim-: 

s 

f 

8.0e5 

7.5e5 

7.De5 

e.SeS 

e.0eS 

5.5e5 

5.0e5 

4.5e5 

4.0e5 

2.0e5 

1.5e5 

I.OeS 

5.0e4-

Sampto Name; "g110211a042- Sample ID; "LCS-110210-14" File; 'gl102na.wifr 

Peak Name; 'PFBS- Mass(es); -299.CV99.0 amu.299.0m0.0 amuComment "Sppb LCS ECF" Annotation: " 

Sample Index: 42 

Sample Type: QC 

0.00 ng/mL 

0.0578 ng/mL 

Acq, Date: 2/12/2011 

Acq. Tima: 9:14:59 AM 

Data printed by STW 

Printing Time: 12:33:41 PM 

Printing Date: Tuesday, March 22, 2011 

Page 1 of 4 

Page 60 of 83 
** Ginge r AG01330509 

GLPIO-01-02; Interim Report 09 

Res^P?&'%SAPF^?'cgf (['aS.M' P^OS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

• Sampte Name: •fl110211a114" Sampte ID; •GLP1(M)1.02-09-025' FBe: •gl10211a.wir 

1 Peak Name:-PFBS' Has«{es): *299.0«9.0 amu,299.0O0.0 amu" 

• Comment'DALGWGRS040100930{diIl;500r Annotation; " 

Sample Indaj; : 114 

Sample Type: Unknown 

Concenrrjtion : N/A 

Calculate d Cone; 2360. ng/mL fiSeSAcq. Dat« : 2/13/201 1 

Acq. Tima: 6:52:^3 AH 

Modified : Yes ®-°»^ 

Proc . Algorithm : IntelliCua n - MGII 

Nsise Percentage : 50 

Bare . Sub. Windcw: 1.00 min 5.5e5-

PeaK-Split , Factor: 3 

Report Latyea t Peak; Ho 

Min . Peak Height : 0-00 cps 5,0e5 

Min . Peak Width : 0.00 sec 

Smoothing Kidth : 3 point s 

RT Window: 30.0 sec 4.Se5 

Expected RT: 10,S min 

Use Relativ e RT: No 

4.0e5 

Int . Type: Base To Bsse 

Retentio n Time: 10.S min -

AL-ea: 3172747 count s & 

Height : 670000. -p s ^ •'•^=* 

Star t Time: 10.2 min ^ 

End Time: 11.3 n,in s 

£ lOeS 

ZSeS 

2.0eS 

1.5e5 

1.0e5 

5.0e4 

1 2 3 4 5 

• Sampte Name: "Bl102na02r Sample ID; "Solvent Blank' File; "g11021 la.wiT 

1 Peak Name; "PFHS" Mass(e*):-399.Qre9.0amu,399.0raO.OamLr 

• Comment'MilBQWatsrTNU-OOSr Annotation;-

Sample Index : 29 

Sample Type: Vnkno-Jn 

Cancentration : N/A 

Calculate d Cone: < 0 *•'"" 

Acq. Data : 2/12/201 1 

Acq. Time: 5:02:5 1 AM ^°° ° 

Modified : No 3800 

Proc . Algorithm ; IntelliQua n - MQIl 

Noise Percentage : 50 3600 

Ba.-e. Sub, Window: 1.00 min 

Peak-Split . Factor: 2 ^00 -

Repott Larges t Peak: H-; 

Min . Peak Height : 0.00 cps 3200-

Min . Peak Hidth : 0.00 sac 

Smootliing Width : 3 point s 3000 

RT Window: 30.0 seer. 

Expected RT: 11.7 min 2800 

Uss Relativ e RT: No 

2600 

Int . Type: Valle y 

Retentio n Time: 11.7 min . 2400 

Area : 1539 count s fr 

Haight : 332. cps ^ 2200 

Star t Time: 11.5 min "B 

Erid Time: 11.B min | 2000 

1800 

1600 

1400 

1200 

1000 

aoo 

600 

400 

200 

**iJw1 - ..... J A . ^ -i... - .M 

1 2 3 4 5 

10.59 

1D.4sJ 

, '^ i 7 8 9 10 

Time, min 

,. i l 

S 7 8 9 10 

11 12 13 14 15 16 17 

j 

l l 

y WF iM A i i\m 

. r^ lyjr Mf\*^ 

/ f 1 f i 

W ^ V J 

11 12 13 14 15 16 17 

• Sampte Name:-Bll0211a02r Sanpte ID: "10007-27-11" Fito; "g110211a.wrtr 

I Peak Name: "PFHS" Wa»«(e*); "399.0ra9.0 amu.399.Qreo.O amu" 

Sample Index : 22 

Sample Type: Standard 

Concentration : 10.0 ng/mL 

Calculate d Cone: 9.83 ng/mL -_ -

Acq. Date: 2/12/201 1 ^'^' ^ 

Acq. Time: 3:14:5J AM 2.4a6-

Hodified : Uo 2.3e6-

Proc- Algorithm : IntelliQua n - MQII _, . 

Noise Percentage : 50 ^-^ ^ 

Base. Sub. Window: 1.00 min 21e6-

P-!ak-3plic . Factor: 2 

R^p^rt Larges t PeaK: N= Z0e6 

Hin . Peak Height : 0.00 cps 

Hin . Peak Width : 0.00 sec ^3t>S 

Smoothing Width : 3 point s l.Se6' 

RT Window: 30.0 sec 

E.-pected RT: 11.7 min 1.7e6-

Use Relativ e BT: No 

Int . Type: Valle y i_5e6. 

Retentio n Time: 11.7 min . 

Area: 11327735 count s g" 1.4e6' 

Height : 2600000. cps * ,, ^ 

Star t Time: 11.5 min 9 ^-^ ^ 

End Time: 12.2 min J 1.2e6' 

1.1e6 

1.0e6 

9.0eS 

B.0e5 

7.0e5 

6.0e5 

5.0o5 

4.0e5 

3.0e5 

2.0e5 

I.OeS 

°' ° 1 2 3 4 5 

1 Sampte Name:-a110211a03r Sampte ID; "LCS-11021t^ File: "g110211a.v.ir 

I Peak Name: "PFHS" Mass<es); "399.0/99.0 amu.399.0/80.0 amu" 

Sample Index : 33 

Sample Type: OC 

Concentration : 4.9S ng/mL 

Calculate d Cone: 5.36 ng/mL 

Acq. Date : 2/12/201 1 1.4e6 

Acq. Tima: 6:32:57 AM 

Hodified : No 1.3e6-

Proc. Algorithm ; IntelliQuar . - HQII 

Noise Percentage : 50 

Base. Sub. Window: 1.00 min 1.2e6 

Peak-Split . Factor: 2 

Report Larges t Peak: No 

Min , Peak Haight ; 0.00 cp.^ 1.1e6 

Hin . Peak Width : 0.00 sec 

Smootliiny WiJtli : 3 point s 

RT Window: 30.0 sec l-OeS 

Expected RT: 11.7 min 

Use Relativ e RT: No 

9.0eS 

Int . Type; Valle y 

Retentio n Time : 11.7 min « 

Area: 6389201 count s g" S.OeS 

Height : H70000 . cps ^ 

Star t Time: 11.5 rain a 

End Time: 12.2 min | '-O^^ 

6.0e5 

S.0e5 

4.0e5 

3.0e5 

ZOeS 

I.OeS 

1 2 3 4 5 

11 68 

k. 

6 7 8 9 10 11 12 13 14 

Time min 

lie s 

.L 

6 7 8 9 10 11 12 13 14 

1S 16 17 

15 16 17 

Data printe d by STW 

Printin g Time: 12:33:4 2 PM 

Printin g Date : Tuesday , March 22, 

Page 2 of 4 

2011 Page 61 of 83 
Ginge r AG01330509 

GLPIO-01-02; Interim Report 09 

Res^P?&'S^S!iPF^?.cg!i^aS..M^ PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

Peak 

Kepo 

Min . 

Min . 

Smoo 

RT W 

Expe 

-spl i 

r t La 

Peak 

Peak 

hin g 

ste d 

t.,e 

VJ 

Fac 

.•3t 

Iqh 

d t h 

Width 

RT 

I Sample Name; "gl102l1a042- Sampte ID;'LCS-110210-14" Fae:-g110211a.<Mr 

Peak Name; "PFHS" Mass(es); '399.0/99.0 amu,399.0/80.0 amiT 

I Convnent "Sppb LCS £C P Annotation;"" 

ao»4 

7.5e4' 

7.0e4 

6.5e4 

6.0e4 

S.Se4 

5.0e4 

4.5M 

4.0»4-

3.5e4 

3.0e4 

2.5e4 

2.0»4 

1.Se4-

1.0e4-

5000.0-

Height : 

Star t Tin 

End Time ; 

0.0 

I

Sampte Name; "g110211a114- Sampte ID; "GLPl(W)1-02-09O25" Fito; 'g110211a.wtr 

Peak Name; 'PFHS* Man(es): '39g.0i«9.0 amu,399.(V80.0 amu' 

Comment 'D/U. GW GRSD4 0 100930 (da 1:500)- /Annotation: ~ 

ampl< 114 

Sample Type: I'nknovn 

Concentration: N/A 

Calculated Cone: 7780. i 

Acq. Data: 2/13/2011 

Ac(j. Time: 6:52:43 AM 

Moditi. Ye: 

P^aK-Split . Fac 

Repor t Largest 

Hin . Peak Heigh 

Hin . Pea k Width 

Smootiiinij Widtll 

RT Kindov : 

Expecte d RT: 

Use Relativ e RT 

int . Type : 

Retentio n Time : 

o r : 4 

•eak : No 

: 0.0 0 

0.0 0 

3 

?0. 0 

11. 7 

No 

va11e y 

11. 7 

Area : 1715668 3 co 

Height : 

Star t Time : 

End Tima ; 

2S30000 . c 

11. 4 

1C. 3 

I

Sampte Name; 'fl110211a022" Sampte ID: '10007-27-11' Fito: 'fl11021 la.wiT 

Peak Name: "PFOS" Uass(es}; '499.0/99.0 amu.499.0/60.0 amu.499.0/130.0 amu' 

Conwnent "10 ngAnL FC std in MilH Q water Annotation: ~ 

Sampl e Inde x 

p i e Standar d 

10. 0 

5.72 

2/12/201 1 

I

Sampte Name: "g110211a028" Sampte ID: "Solvent Blank- Fite: "g110211a.wfr 

Peak Name: 'PFOS* Uassfes}: "499.0/99.0 anuJ.499.D/80.0 amu.4g9.D/130.0 amiT 

Comment"MafiOV\ibterTN11-0052' /^notation: ' 

Sample Index : 29 

g/mL 

Repor t Largest Peak 

Min . Peak Height ; 

Min . Peak Width : 

Smoothin g Width : 

RT Window: 

Expecte d RT: 

U30 Relativ e RT: 

Int . Typt : \ 

Retentio n Time : 

Area : 159-12 

: H 

0 

3 

30. 0 

12. 4 

No 

alle y 

12. 4 

906 

Height : 3710000 . 

Star t Time : 

End Time : 

12, 3 

12. 5 

3.6e6-

3.4aG 

3.2e6 

3.0e6 

2.8a6 

Z6eGZ4e6 -

Z2B 6 

Z0e 6 

1.8e6 

1.6e6 

1.4e6' 

1.2e6 

I.OeS 

S.0e5 

6.0e5 

4.0e5 

ZOeS 

0.0 

Samp 

Cone 

Cal c 

Acq. 

Acq. 

Hodi 

RT W 

Expe 

e Type: 

nttation : 

late d Con 

Date : 

Time: 

ied : 

ndov: 

.-ted RT: 

Unknown 

N/A 

c; O.OOBOS 

2/12/201 1 

5; 02;5 1 AM 

Vea 

30.0 

12.4 

15 i e 17 9 10 n 12 13 14 15 IB 17 

Data printe d by STW 

Printin g Time: 12:33:4 2 PM 

Printin g Date : Tuesday, March 22, 

Page 3 of 4 

2011 Page 62 of 83 
Ginge r AG01330509 

GLPIO-01-02; Interim Report 09 

Res^P?l^%S|PF^'(^f tfaS.'M^ PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

Calculate d Cone : 

Acq. Date : i 

Acq. Time : 6 

Modified : 

Proc . Algorithm : I 

Nois e Percentage : 

Ba.-^e. Sub . Windcw: 

Peak-Split . Facto r 

Report Latyes t Pea 

Min . Peak Height : 

Min, Peak Width : 

Smoothin g Viidth : 

RT Window: 

E.'<pected RT: 

4.9 3 

12/2 0 

32:5 7 

No 

tell i 

50 

1, 

2 

: H 

0 

1 

30. 0 

12. 4 

I

Sample Nante: 'g110211a03r Sampte ID: "LCS-110210-5" 

Peak Name: 'PFOS' Uass(es}; "499.0/99.0 amu,49g.Q/80.0 ai 

Comment "Sppb LCS" Annotatten: ~ 

1.ge6 

1.8e6 

1.7e6 

1.6e6 

1.Se6 

1.4e6 

1.3e6 

1.2e6 

1.1e6 

1.0e6 

9.0e5 

8.0e5 

7.0e5 

6.0e5 

5.0e5 

4.0e5 

3.0e5 

Z0e 5 

I.OeS 

0.0 

I

Sampte Name: "g110211a042" Sampte ID: "LCS-110210-14" Fite; "g110211a.wir 

Peak Mame; 'PFOS* Mass(e$): "499.0/99.0 amu,499.0/80.0 amu,499.0/130.0 amu" 

Comment 'Sppb LCS ECP Annotation; " 

Sample Inde:i : 42 

Sample Type : 

5.04 

Calculate d C 

Acq. Date : 

Acq. Time : 

Modified : 

RT Window: 

Expecte d RT: 

Use Relativ e 

Int . Type : 

Retentio n Ti 

Area : 

Hsight : 

nc 

RT 

5 .1 

1 

5.3 e 

^/13/2 0 

'^;14:5 9 

Ves 

30. 0 

12. 4 

No 

Manua l 

1--.A 

•532 

20 0 00 . 

ng/mL 

1.4e6 

1.3e6-

1.2e6 

1.1e6 

1.0e6 

g.OeS 

B.OsS 

T.OeS 

SOeS 

SOeS 

4.0e5 

3.0eS 

ZOeS 

I.OeS 

0.0 

10 11 12 13 14 15 16 17 

I

Sampte Name; "g110211a114* Sampte ID: •GLP1[W)1-02-O9-O2S" 

Peak Nanrw: 'PFOS* Mass(es); "499.0/99.0 amu,499.0/80.0 amu,4S 

Comment "DAL GW GRS04 0 100930 (dil 1 :S00)" /Annotation: *" 

culate d C 

. Date : 

. Time : 

ified : 

Window: 

ecte d RT: 

ReUtiv e 

. Type : 

ght : 

Time : 

:>nc: 1310 . 

2/13/2 0 

E:52:4 3 

Yes 

30. 0 

12. 4 

RT: No 

Hanua l 

n e ; 12. 2 

4527137 < 

522000 . 

13. 0 

12. 8 

ng/mL 

1 

AH 

min 

C f 3 

s. 

S.OeS 

4.8e5 

4.6eS 

4.4e5 

4.2e5 

4.0eS 

3.8e5 

3.665 

3.4eS 

3.2e5 

3.0e5 

2.Se5 

2.6e5 

2.4eS 

2.2e5 

ZOeS 

1.8eS 

1.6e5 

1.4e5 

1.2e5 

I.OeS 

8.0e4 

6.0e4 

11 12 13 14 15 16 17 

Data printe d by STW 

Printing Time: 12:33:42 PM 

Printing Date: Tuesday, March 22, 

Page 4 of 4 

2011 Page 63 of 83 
Ginge r AG01330509 

GLPIO-01-02; Interim Report 09 

Res^??lm«iPF^§.j2f t'aS.M' ^^^ ^ '" Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

Data printed by STW 

Printing Time: 12:30:59 PM 

Printing Date: Tuesday, March 22, 2011 

Page 1 of 1 

Page 64 of 83 
Ginge r AG01330509 

GLP10-01-02; Interim Report 09 

Res^5'?&'^S|PFa^.(^f ^aS.M" PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

• g110211a.rdb (PFHS); "Quadratic" Regression ("1 /x " weighting); y = -8.76e+003 x'^2 + 1.24e+006 x + 4.17e+003 (r = 0.9995) 

4.2e7 J 

4.0e7-

3.8e7-

3.6e7-

3.4e7-

3.2e7-

3.0e7-

2.8e7-

2.6e7-

2.4e7-

^ 2.2e7-

° 2.087-

(IS 

< 1.8e7-

1.6e7-

1.487-

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 y 

/ 

/ 

/ y 

/ 

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 

Concentration, ng/mL 

^ 

36 

^y-^ " 

38 

^-•^''' ^ 

40 

^y.-" " 

42 

^ --

1 

44 

^.-""^ 

46 48 

•. 

50 

Data printed by STW 

Printing Time: 12:31:17 PM 

Printing Date: Tuesday, March 22, 2011 

Page 1 of 1 

Page 65 of 83 
Ginge r AG01330509 

GLPIO-01-02; Interim Report 09 

Res^P?&'^SAPF^?.j2!^aS.,md pro s in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

g11021 la.rdb (PFOS); "Quadratic" Regression ("1 /x" weighting): y = -1.24e+004 x'^2 + 1.76e+006 x + 8.61e+003 (r = 0.9998) 

5.9e7 

5.5e7-

5.0e7 

4.5e7 

4.0e7 

3.5e7 

5 3.0e7 o u 

ra" 

0) 

2.5e7-

2.0e7 

1.5e7 

1.0e7-

5.0e6-

0.0 

y 

y 

X / 

y 

8 10 12 14 16 18 20 22 24 26 28 30 32 34 36 38 40 42 44 46 48 50 

Concentration, ng/mL 

Data printed by STW 

Printing Time: 12:31:34 PM 

Printing Date: Tuesday, March 22, 2011 

Page 1 of 1 

Page 66 of 83 
Buster J2930203 

GLP10-01-02; Interim Report 09 

Bat^Ra!ym?f ?fmi?^Hc&i?"d PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

• Sample Name;-bUOSlSaOIS" Sampte ID:'10007-27-6' Fite:'bl 1031 Sa.wiT 

• Peak Name; "PFOS" Mass(es):'499.0/130.0amu,499.0/99.0amu,4g9.oraO.Oamu" 

5araple Index : 19 

Sample Type: Standard 

Concentration : 0.250 ng/mL 

Calculate d Cone: 0.250 ng/mL ,3- 4 

Acq. Date: 3/15/201 1 

Acq. Time: 9:45:5 5 PH 1.3e4 

Modified : No '"^• ^ 

Proc . Algorithm : IntelliQua n - lOA i,2e4 

Min . P«ak Height : 0.00 cps 

Hin . Peak Width : 0.00 sec l-l^ ^ 

Smoothing WiOth: 3 point s , . ^ 

RT Window: 30.0 sec '" ^ 

Expected RT: 12.5 min 1.0e4 

use ReUtiv e RT: No ^ ^ 

Int . Type: Valle y 9000.O 

Retentio n Time: 12.5 min 

Area : 43514 count s 8500.0 

Height : ''''r. T '? ' 8000.0 

Star t Timo: 12,B mm 

End Tim^ : ll'.C min • 7500.0 

• 6500.0 

1 6000.0 

5500.0 

5000.0 

4500.0 

4000.0 

3500.0 

3000.0 

2500.0 

2000.0 

1500.0 

1000.0 

500.0 

0.0 •—<—'—1—•—1—•—1—•—1 

1 2 3 4 5 

1 Sampte Name: "b110315a04r SamptelD;-LCS-110315-2- Fite: "b110315a.wir 

I Peak Name: "PFOS" Mass(es); "499.0/130.0 amu.499.0/99.0 annu,499.0/80.0 amu" 

• Comment "O.Sppb LCS" Annotabon; -

Sample Index : 33 

Sample Type: QC 

Concentration : 0.A99 ng/mL 3 8-4 

Calculate d Cone: 0.-197 ng/mL 

Acq. Data : :'/l£/201 1 

Acq. Time; 2:47:34 AM 2.6e4-

HoJiriad : Yes 

RT Window: 30.0 sec 

Expected RT: 12.5 min i-le^ -

Use Relativ e ST: No 

I„t . Typ. , H.„ua l "•' • 

Retantio n Time: 12.8 min 

Area : 99870 count s 

Hei.jht ! 2.a0e-t004 cps 2.De4-

Star t Time: 12.7 min 

Et.d Time: 12.9 min 

1.8e4-

re,,. 

u 

i ? 

B 1.4a4-

1 1.2e4-

1.0o4-

6000.0 

6000.0 

4000.0' 

2000.0 

1 2 3 4 5 

6.10 7.278.3K8.74 

6 7 8 9 

Time min 

6 7 8 9 

_ = = ^s,m= 

12.92 

1^58. 

1 

L ^13.06 

10 11 12 13 14 15 16 17 

12 79 

12.47.^ 

^12.95 

10.38 12.3^ ^ ^„. , -13.75 ^15.09 16.57 

10 11 12 13 14 15 16 17 

• Sampte Name:-b110315a034" Sampte ID;'Sojvent UanlT Fite; •bl10315a.Mfr 

• Peak Name: "PFOS- Maw(ea);'499.0/130.0amu,499.0«9.0amu,499.0ffi0.0amu' 

.'>ample Inde.t: 30 

Sample Type: I'nknovn 

Concentration : N/A 2100-

CalcuUte d Cone: 0.00B05 ng/mL 

Acq. Date : 3/16/201 1 2000-

Acq. Time; 12:22:5' ' AM 

1900-

Moditiad : Vea 

RT Kindo-.v: 30.0 s«c 1800-

Expected BT: 12.9 min 

I'ss Relativ e RT: No ^jaoInt . Type: Manual -gTM. 

Retentio n Time: 12.9 min ^**" 

Area : 222 count s -g-- . 

Height ; ;.7Oe'0O2 cps 

Star t Time: 12.9 min 

End Time: 12.9 min ^^ ^ 

1300 

1200 

^ 1100 Intensi) 1 

9 0 0 

8 0 0 

7 0 0 

6 0 0 

5 0 0 

4 0 0 

3 0 0 

2 0 0 

1 0 0 

1 2 3 4 5 

• San:)pteName:"bl10315a04g- Satnpte 10:'LCS-110315-6" Fite; "b110315a.wir 

1 Peak Name: "PFOS" Mass(as): "499.0/130.0 anuJ.499.(V99.0 «mu,499.0/80.0am>r 

Sample Index : 45 

Sample Type: QC 

Concentration : 0.502 ng/mL 1.9e4-' 

Calculate d Cone: 0,456 ng/mL 

Acq. Date: 3/16/201 1 ,0 ^ 

Acq. Time: 4:54:1 9 AM "" ^ 

modified : Ye , I-?** 

RT Window: 30.0 sec 

Expected RT: 12.9 min 1.6e4 

Use Relativ e RT: No 

1.5e4 

Int . Type: Manual 

Retentio n Time: 12.9 min . ^ . 

Area : 91510 count s ^'^ ^ 

Hsiglit : l.STsrOO^ cp3 

Star t Time: 12.8 min 1-3»4 

End Time: 13.0 min 

1.2e4 

1.1e4 

". 1.0e4 

1 9000.0 

8000.0 

7000.0 

6000.0 

5000.0 

4000.0 

3000.0 

2000.0 

1000.0 

1 2 3 4 5 

. iiil.iiiiht.k ItaJil 

6 7 8 9 10 

Time, min 

1260 

1 1 

l ^ 

^13.09 

1 

l l 1 

11 i .. itlbiiiLi liUll JJ 

11 12 13 14 15 16 l'7| 

12 91 

"•" 1 

t 

k 

J^'^.J^..^ ^ 

6 7 8 9 I'O i'l 12 13 14 15 16 iV] 

— 1 

Data printed by STW 

Printing Time: 12:35:59 PM 

Printing Date: Tuesday, March 22, 2011 

Page 1 of 2 

Page 67 of 83 
'** Buster J2930203 

GLP10-01-02; Interim Report 09 

Bat^P^lym?^ ?fmi'5lt^c|i?"d PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

I Sare^ple Name;'bl10315a035" Sampte ID: "GLP10-01-02-09-053" Fite: "bUOSlSa.vvifr 

I Peak Name: "PFOS' Man(es): "499.0/130.0 amu,499.0/99.0 amu.49g.0/80.0 amu" 

I Comment"DALGW328L0100928' /Wwtation;-

N/A 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Min. Peak Height 

Hin. Peak Width: 

Smoothing width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

Area; 1 

Height: 

Start Time; 

End Tima: 

;'/16/2011 

12:41:02 

No 

IntelliQu 

: 0.00 

0.00 

3 

30.0 

12.9 

No 

Valley 

12.B 

45506 CO 

1.94e-f004 

12.7 

13.0 

2.Cte4 

1.9e4 

1.8e4' 

1.7e4 

1.6e4 

1.5M 

1.4e4 

1.3e4 

1.2e4 

1.1e4 

1.0e4 

9000.0 

8000.0-

7000.0-

6000.0-

5000.0 

4000.0 

3000.0 

2000.0 

1000.0-

0.0 L 

/ ^mn/t,., n 

9 10 11 12 13 14 15 18 17 

Data printed by STW 

Printing Time: 12:36:59 PM 

Printing Date: Tuesday, March 22, 2011 

Page 2 of 2 

Page 68 of 83 
Buster J2930203 

6LP10-01-02; Interim Report 09 

Bat^R^lyiJ^^pf gf^,,l=|HSj^and PFOS in Groundwater 

Quarteriy Groundwater Sampling - Sept 2010 

bl lOSISa.rdb (PFOS): "Quadratic" Regression ("1 / x" weighting); y = -885 x*2 + 2.04e•^005 x + -1.42e-H003 (r = 0.9996) 

4.6e6-

4.4e6-

4.2e6-

4.0e6-

3.8e6-

3.6e6-

3.4e6-

3.2e6-

3.0e6-

2.8e6-

2.6e6-

2.4e6-

2.2e6-

2.0e6-

1.8e6-

1.6e6 

1.4e6-

1.2e6-

1.0e6-

S.OeSe.OeS4.0e5-

2.0e5-

0.0- ^ * 

X"" 

,,•--" 

y'"' 

y ' 

y 

y 

y ' ' 

y ^ 

y ' ' 

yii ' 

y 

y 

y " " 

y " 

y ' 

y ' ' 

y ' ' 

y'-' ' 

y'' ' 

y ' 

y 

y'' ' 

. y 

,/•-"" " 

y 

y ' 

0-

0 1 10 11 12 13 14 

Concentration, ng/mL 

15 16 17 18 19 20 21 22 23 24 25 

Data printed by STW 

Printing Time: 12:35:33 PM 

Printing Date: Tuesday, March 22, 2011 

Page 1 of 1 

Page 69 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

ATTACHMENT C: ANALYTICAL METHOD 

Page 70 of 83 
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Analysis of PFBS, PFHS, and PFOS In Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

3M Environmental Laboratoiy 

Mettiod 

Mettiod of Analysis for the Determination of Perfluorinated Compounds in Water 

by LC/MS/MS; Direct Injection Analysis 

Method Number: ETS-8-044.0 

Adoption Date: Upon Signing 

Effective Date: Q U I n f o '1 

Approved By: 

^y^/ a •> 

William K. Reagen, Laboratory Manager Date 

ETS-8-044.0 Page 1 of 11 

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

Injection Analysis Page 71 of 83 
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Analysis of PFBS, PFHS, and PFOS In Groundwater 

Quarterly Groundwater Sampling - Sept 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), Perfiuoroundecanoic Acid (PFUnA), 

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

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

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

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

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

Performance Liquid Chromatography/Mass Spectrometry". 

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

defined QC elements are satisfied. 

Sample collection is not covered under this analytical procedure. 

2 Method Summar y 

Clean aqueous samples are analyzed by direct injection using LC/MS/MS. Samples containing heavy 

particulate may not be suitable for analysis by this method. Samples containing suspended particulate 

should be centrifuge prior to removing a sample aliquot, or filtered. 

This is a perfonnance-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 determine the statement of 

accuracy for analytical results. 

3 Definitions 

3.1 Calibration Standard 

A solution prepared by spiking a known volume of the Wori<ing 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 determine if test substances or 

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

ETS-8-044.0 Page 2 of 11 

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

Injection Analysis 

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Analysis of PFBS, PFHS, and PFOS In Groundwater 

Quarteriy Groundwater Sampling - Sept 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 determine if the method is in control and 

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

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

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

3.7 Laboratory Control Sample (LCS) 

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

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

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

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

each day samples are extracted. 

3.8 Laboratory Matrix Spike (LMS) 

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

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

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

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

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

3.9 Laboratory Sample 

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

3.10 Limit of Quantitation (LOQ) 

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

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

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

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

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

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

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

ETS-8-044.0 Page 3 of 11 

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

Injection Analysis 

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Quarterly Groundwater Sampling - Sept 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 determine if test substances or other interferences are present in the laboratory 

environment, the reagents, or the apparatus. 

3.12 Sample 

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

material. 

3.13 Stock Standard Solution (SSS) 

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

compound. 

3.14 Surrogate 

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

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

containing an isotopically-labeled substitution. If used, surrogate(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 cun-ent awareness of local 

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

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

4.2 Cautions 

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

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

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

5 Interferences 

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

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

conditions of analysis by mnning method blanks. 

ETS-8-044.0 Page 4 of 11 

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

Injection Analysis 

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Quarteriy Groundwater Sampling - Sept 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 \3L connected to a tandem Mass Spectrometer 

(LC/MS/MS). I 

Analytical balance capable of reading to 0.0001 g 

A device to collect raw data for peak integration and quantitation 

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

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

1 mL plastic HPLC autovial. 

Disposable pipettes, polypropylene or glass as appropriate 

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

6.2 Chromatographi c System 

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

Analytical Column: Betasil C18,4.6 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. 

RunTime: ~ 17minutes. f 

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

provided that data quality objectives are met. 

ETS-8-044.0 Page 5 of 11 

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

Injection Analysis 

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Quarterly Groundwater Sampling - Sept 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, altemate instruments 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 

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

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

Perfluorobutanesulfonate (PFBS - C4 sulfonate); 3M 

Perfluorohexanesulfonate (PFHS - C6 sulfonate); 3M 

Perfluorooctanesulfonate (PFOS - C8 sulfonate); 3M 

ETS-8-044.0 Page 6 of 11 

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

Analysis 

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Quarterly Groundwater Sampling - Sept 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: Altemative volumes may be prepared as long as the ratios of the solvent to solute ratios are maintained. 

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

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

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

when diluting stock solutions to appropriate levels. 

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

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

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

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

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

^. , ^ molecular weight of anion 

salt correction factor = = 

moclecular weight of salt 

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

538 

10mg CsFiySOsK*with purity 90% = 8.35mg C8F17SO3"(10 mg*0.90*0.9275=8.35 mg) 

5 Mg/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 wori<ing standards in accordance with laboratory standard operating 

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

ETS-8-044.0 Page 7 of 11 

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

Analysis 

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Quarterly Groundwater Sampling - Sept 2010 

7.5 Calibration Standards 

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

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

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

than those listed below can be prepared as needed. 

Concentration 

of WS, ng/mL 

125 

125 

125 

125 

250 

250 

250 

250 

5000 

5000 

5000 

Volume of WS.fd. 

10 

15 

20 

30 

20 

50 

100 

200 

25 

50 

100 

Final Volume of 

Calibration Standard (mL 

of ASTM Type 1 Water, or 

other suitable water) 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

Final Concentration of 

Calibration Standard, ng/mL 

(ppb) in ASTIVI Type 1 Water, 

or other suitable water 

0.025 

0.0375 

0.050 

0.075 

0.100 

0.250 

0.500 

1.00 

2.50 

5.00 

10.0 

8 Sample Handling 

8.1 Water Sample Preparation 

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

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

sample aliquot, or filtered. 

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

prefen-ed over the use of glass autovials, to prevent the possibly of 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-determined acceptance criteria. Low-level curve 

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

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

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

ETS-8-044.0 Page 8 of 11 

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

Analysis 

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Quarterly Groundwater Sampling - Sept 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 construct the calibration curve. 

If the calibration curve does not meet acceptance criteria, perfomi 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 constmct 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 mn. 

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

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

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

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

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

10.3 Sample Replicates 

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

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

ETS-8-044.0 Page 9 of 11 

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

Analysis 

Page 79 of 83 
Document may be^iM^^i^amtifrnhpcsso^iA days from 03/22/2011 

Analysis of PFBS, PFHS, and PFOS In Groundwater 

Quarterly Groundwater Sampling - Sept 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: 

A ,1 r .J, , l^ (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 performance parameters that are not achieved must be considered in the evaluation of the data. 

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

If criteria listed in this method performance section are not met, maintenance may be performed on the system and 

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

If data are to be reported when 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 

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

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

have area counts with an RSD of S5% and a retention time RSD of ^2% to be compliant. 

12.2 Quantitation 

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

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

the LLOQ, which may be within ±30%. 

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

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

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

bracketed by CCVs not meeting these criteria must be reanalyzed. 

ETS-8-044.0 Page 10 of 11 

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

Analysis 

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Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 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 information regarding the required accuracy of laboratory control spikes, field matrix 

spikes and laboratory matrix spikes. 

12.5 Precision 

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

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

requirement for replicates excludes field blanks or rinse blanks. 

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

13 Pollution Prevention and Waste Management 

Waste generated when performing this method will be disposed of appropriately. The original samples will be 

archived at the 3M Environmental Laboratory in accordance with internal procedures. 

14 Records 

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

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

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

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

15 Affected Documents 

None. 

16 Revisions 

Revision 

Number Summarv of Changes 

ETS-8-044.0 Page 11 of 11 

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

Analysis 

Page 81 of 83 
GLP10-01-02; Interim Report 09 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Quarterly Groundwater Sampling - Sept 2010 

ATTACHMENT D: DEVIATION(S) 

Page 82 of 83 
GLPIO-01-02; interim Report 09 

3M Confidential Analysis of PFBS, PFHS, and PFOS in Groundwater 

__ _^ „ . Quarterly Groundwater Sampling-Sept 2010 

RECORD OF DEVIATION/NONCONFORMANCE 

/. identification 

Study / Project No. Date(s) of Occurrence: Document Number: 

GLP10-01-02-09 Sequence b101108a,g110211a, and b110315a ETS-8-044.0 

Deviation type D SOP D Equipment Procedure IZI Method 

(Checl< one) D Protocol E GPO D Other: 

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

Method Requirements: 

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

(2) Sample/Sanfiple Duplicate RPD s20%. 

(3) FMS recovery of 100% ± 30%. 

Actual procedure/process: 

(1) LCS average recovery for the high set of linear and branched PFOS was 129% (bl 01108a). LCS 

average recovery for the high set of linear and branched PFOS was 133% (g11021 la). 

(2) The RPD value for PFOS for DAL GW 330L was 24%. 

(3) Sampling location DAL GW 227L did not have an appropriate FMS level for PFOS. The recovery of the 

HS for PFHS for DAL GW 330L was 135%. The recovery of the HS for PFBA, PFHS, and PFOS for 

DAL GW GRS04 were <50%. The recovery of the HS for PFOS for DAL GW 328L was 69.0% 

III. Actions Taken 

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

Corrective Action (D Yes 0 No) Reference: 

Acceptability of the nonconforming work: 

1) The linear and branched LCS had been running 5-15% higher when quantitated against a calibration 

curve comprised of primarily linear PFOS. All LCS were used in the determination of method 

uncertainty. 

2) The RPD value for PFOS for DAL GW 330L with a value >20% will be footnoted in the data tables. 

3) Sampling location DAL GW 227L will be footnoted in the report as not having an appropriate spike level 

for PFOS. The analytical uncertainty for sampling location DAL GW 330L will be adjusted accordingly. 

A 5000ppb LMS was prepared on sampling location DAL GW GRS04 and met method acceptance 

criteria. Sampling location DAL GW 328L LS met method acceptance criteria and was the more 

appropriate spike level. No adjustment will be made to the analytical uncertainty. 

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

0 Other: Deviations will be npted in final report. 

Project Lead/PAI Approval: , „ 14-.^ \ , Date: , , 

study Director (if GLP): ^ Q I i . , :L> Date:' >j| >7» i 

Sponsor Approval (for GLP protocol deviations): NA Date: NA / ' 

Technical Reviewer (optional): NA Date: NA 

Laboratory Department Manager Approval: Date: 

IV. Authorization to Riesume Work 

Where halting of work occurred, resumption ot work must lirst be approved by Laboratory Management 

Laboratory Department Manager Approval: NA Date: NA 

Deviation No. 

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

Attachment A ETS-4-008.7 Page 1 of 1 

Documentation of Deviations and Control of Nonconforming Testing Page 83 of 83