GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

3M 

GLP10-01-02: Interim Report 06 - Analysis of PFBS. PFHS. and PFOS in 

Groundwater/Surface Water Samples Collected as Part of the Avenue A Investigation Area 

in Decatur. AL in June/July 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 

GLP10-01-02-06 

Total Number of Pages 

67 

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

Competence of Testing and Calibration i.^boratories", in accordance with the A2iA. Certificate #2052.01. 

Testing that compiies with this intematlonal Standard also operate in accordance with ISO 9001:2000. 

Certificate #2052.01 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

This page has been reserved for specific country requirements. 

Page 2 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

GLP COMPLIANCE STATEMENT 

Report Title: Interim Report 06 Analysis of PFBS, PFHS, and PFOS in Groundwater/Surface Water 

Samples Collected as Part of the Avenue A Investigation Area in Decatur, AL in June/July 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 SiteRelated Monitoring Program. 

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

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

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

system and no dosing of a test system. 

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

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

Gary Hohenstein, Sponsor Representative Date 

(( 

% 

OkkUi 

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

Page 3 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

QUALITY ASSURANCE STATEMENT 

Report Title: Interim Report 06 Analysis of PFBS, PFHS, and PFOS in Groundwater/Surface Water 

Samples Collected as Part of the Avenue A Investigation Area in Decatur, AL in June/July 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 SiteRelated 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 

9/23, 9/24, 9/27, and 

9/28/10 

Phase 

Data and Interim Report 

Date Reported to 

Testing Facility 

Management 

10/12/10 

Study Director 

10/12/10 

H^r^^f /d-2^-/0 

Date 

Page 4 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

TABLE OF CONTENTS 

GLP Compliance statement 3 

Quality Assurance Statement 4 

Table of Contents 5 

List of Tables 6 

1 Study Infomnation 8 

2 Summary 9 

3 Introduction 11 

4 Test & Control Substances 12 

5 Reference Substances 12 

6 Test System 14 

7 Method Summary 14 

7.1 Methods 14 

7.2 Sample Collection 14 

7.3 Sample Preparation 14 

7.4 Analysis 14 

8 Analytical Results 16 

8.1 Calibration 16 

8.2 System Suitability 16 

8.3 Limit of Quantitation (LOQ) 16 

8.4 Continuing Calibration 17 

8.5 Blanks 17 

8.6 Lab Control Spikes (LCSs) 17 

8.7 Analytical Method Uncertainty 19 

8.9 Field Matrix Spikes (FMS) 20 

9 Data Summary and Discussion 21 

Page 5 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

10 Conclusion 37 

11 Data/Sample Retention 37 

12 Attachments 37 

13 Signatures 38 

LIST OF TABLES 

Table 1. Summarized PFBS, PFHS, and PFOS Results (Avenue A Investigation, June/July 2010). 10 

Table 2. Sample Description Key Code 14 

Table 3. Instalment Parameters. 15 

Table 4. Liquid Chromatography Conditions 15 

Table 5. Mass Transitions 15 

Table 6. Limit of Quantitation (LOQ) 16 

Table 7. Laboratory Control Spike Recovery 18 

Table 8. Analytical Uncertainty 20 

Table 9. DALSWSW01 100623 22 

Table 10. DAL SWSW02 100622 22 

Table 11. DAL SWSW03 100622 23 

Table 12. DAL SWSW04 100622 23 

Table 13. DAL SWSW05 100622 24 

Table 14. DAL SWSW06 100622 24 

Table 15. DAL SWSW07 100622 25 

Table 16. DAL SWSW08 100623 25 

Table 17. DAL SWSW09 100623 26 

Table 18. DAL SWSW10 100623 26 

Table 19. DALSWSW11 100623 27 

Table 20. DAL SWSW12 100623 28 

Table 21. DALGWGP01 100709 28 

Page 6 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 22. DAL GWGP02 100709 29 

Table 23. DAL GW GP03 100709 29 

Table 24. DAL GWGP04 100709 30 

Table 25. DAL GW GP05 100709 31 

Table 26. DAL GWGP07 100709 31 

Table 27. DAL GWGP08 100709 32 

Table 28. DAL GW GP09 100709 32 

Table 29. DAL GWGP10 100709 33 

Table 30. DALGWGP11 100708 33 

Table 31. DAL GWGP12 100708 34 

Table 32. DAL GW216R 100716 34 

Table 33. Trip Blank 35 

Table 34. Rinseate Blanks 36 

Page 7 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 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(gwestonsolutions.com 

Study Location 

Testing Facility 

3M EHS Operations 

3M Environmental Laboratory. 

Building 260-5N-17 

Maplewood, MN 55106 

Study Personnel 

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

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

Susan Wolf, 3M Analyst 

Jonathan Steege; analyst 

Study Dates 

Study Initiation: March 8, 2010 

Interim Report 06 Experimental Termination: September 10, 2010 

Interim Report Completion: Date of Interim Report Signing 

Location of Archives 

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

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

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

Page 8 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

2 Summar y 

The 3M Environmental Laboratory received groundwater and surface water samples collected as part 

of the Avenue A Investigation area in Decatur, AL, representing twenty-four different sampling 

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

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

perfluorobutane sulfonate (PFBS), and included duplicate water samples from each sampling location. 

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

containing Milli-Q'^" water and appropriate trip blank spikes, and two equipment rinseates. The 

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

PFOS recovery. 

The surface water samples, one set of trip blanks and equipment rinseate blanks were received from 

Weston personnel on June 25,2010. The groundwater samples and one set of trip blanks were 

received on July 13, 2010. The groundwater samples from location 216R and one set of trip blanks 

were received on July 22, 2010. All water samples for this project were logged under GLP10-01 -01-06. 

In addition, soil-equipment rinseate blanks from GLP10-01-02-03 (Wetlands Edge Environment Center 

-WEEC Swamp), GLP10-01-02-05 (Avenue A Investigation - Soils), and GLP10-01-02-08 (Phase 3 

Offsite Soil) are also reported herein. 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 -02-06. 

Most of the water 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 was required. The average measured 

PFBS, PFHS, and PFOS concentrations are summarized in Table 1 The equipment rinseates and trip 

blanks were below the lower limit of quantitation (LLOQ) collected with the water samples for GLP10-

01-02-06, indicating adequate control of sample contamination during shipping and sample collections. 

The soil-equipment rinseate blanks from GLP10-01-02-03, GLP10-01-02-05, and GLP10-01-02-08 

were below the LLOQ with the exception of one soil-equipment rinseate blank collected under GLP10-

01-02-03 which had a detected concentration just above the LLOQ. The PFBS concentration results 

for all groundwater and surface water samples ranged over three orders of magnitude from 0.764 

ng/mL to 279 ng/mL. The PFHS concentration results for all groundwater and surface water sample 

ranged over three orders of magnitude from 3.68 ng/mL to 1130 ng/mL. The PFOS concentration 

results for all groundwater and surface water samples ranged over two orders of magnitude from 17.5 

ng/mL to 1780 ng/mL 

Page 9 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 1. Summarized PFBS, PFHS, and PFOS Results (Avenue A Investigation, June/July 

2010). 

Sampling Location 

DALSWSW01 100623 

DAL SWSW02 100622 

DAL SWSW03 100622 

DAL SWSW04 100622 

DAL SWSW05 100622 

DAL SWSW06 100622 

DAL SWSW07 100622 

DAL SWSW08 100623 

DAL SWSW09 100623 

DAL SWSW10100623 

DALSWSW11 100623 

DAL SWSW12 100623 

DALGWGP01 100709 

DAL GWGP02 100709 

DAL GWGP03 100709 

DAL GWGP04 100709 

DAL GWGP05 100709 

DAL GWGP07 100709 

DAL GWGP08 100709 

DAL GWGP09 100709 

DAL GWGP10 100709 

DALGWGP11 100708 

DAL GWGP12 100708 

DAL GW216R 100712 

PFBS 

Avg. Cone. 

(ng/mL) ± RPD 

15.0 ±4.0% 

7.68 ±5.1% 

9.57 ±1.2% 

13.7 ±5.8% 

20.9 ±1.9% 

17.4 ±4.6% 

10.8 ±0.0% 

40.7 ± 4.2% 

279 ±2.5% 

22.5 ± 4.4% 

102 ±3.0% 

0,764 ± 2.4% 

5.02 ± 0.20% 

21.1 ±13% 

66.4 ± 0.45% 

19.1 ±0.0% 

30.0 ± 0.0% 

20.7 ± 3.9% 

6.36 ±1.1% 

20.7 ±1.9% 

447 ±2.5% 

67.0 ±3.1% 

2.59 ± 58% '^' 

10.6 ±1.9% 

PFHS 

Avg. Cone. 

(ng/mL) ± RPD 

120 ±1.7% 

52.0 ±0.19% 

, 72.2 ±2.1% 

86.5 ± 2.0% 

102 ±3.9% 

77.5 ± 0.77% 

47.9 ±1.0% 

166 ± 3.6% 

643 ± 9.0% 

233 ± 2.6% 

1130 ±0.89% 

3,68 ± 0,54% 

7,63 ± 3,7% 

11,2 ±13% 

413 ±0,24%'^' 

85,8 ± 8,6% 

158 ±5,7% 

171 ±2,9% 

70,2 ± 7,8% 

36.0 ±13% 

420 ± 3,3% 

330 ±1,8% 

11,2±44%<^' 

30,5 ± 3,0% 

PFOS 

Avg. Cone. 

(ng/mL) ± RPD 

248 ± 4,0% 

213 ±7,7% 

197 ±1,1% 

192 ±2.2% 

392 ± 3,6% 

228 ±1,1% 

129 ±2,2% 

266 ±1,9% 

382 ±2,1% 

389 ±1.0% 

850 ± 3.2% 

104 ±2,0% 

26,2 ± 5,3% 

17,5 ±20% 

373 ±17%'^' 

152 ±30%'^' 

382 ±18% 

1780 ±4,5% 

1420 ±4,9% 

95,5 ± 33% '^' 

127 ±31%*^' 

660 ±6,1% 

48,8 ± 67% '^' 

119 ±9,2% 

The analytical method uncertainties associated with the reported results are as follows: PFBS 100% ± 21%, PFHS 100% 

and PFOS 100% ±41%, 

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

(2) The RPD did not meet method acceptance criteria of £20%, 

(3) Sample GLP10-01-02-03-009 (DAL-SD-WESB4-RB) PFOS result was 0,260 ng/ml. 

± 23%, 

Page 10 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 1 continued. Summarized PFBS, PFHS, and PFOS Results (Avenue A Investigation, 

June/July 2010). 

Sampling Location 

Trip Blank and (Milll-QTM Water) 

Equipment rinseate blanks 

GLP10-01-01-03 

Soil-Equipment rinseate blanks 

GLP10-01-01-05 

Soil-Equipment rinseate blanks 

GLP10-01-01-08 

Soil-Equipment rinseate blanks 

PFBS 

Avg. Cone. 

(ng/mL) ± RPD 

<0.0255 

<0,0255 

<0,0255 

<0,0255 

<0,0255 

PFHS 

Avg. Cone. 

(ng/mL) ± RPD 

<0,103 

<0,103 

<0.103 

<0.103 

<0.103 

PFOS 

Avg. Cone. 

(ng/mL) ± RPD 

<0,255 

<0,255 

<0,255''' 

<0.255 

<0,255 

The analytical method uncertainties associated with the reported results are as follows: PFBS 100% ± 21%, PFHS 100% ± 25%, 

and PFOS 100% ±44%, 

(1) The RPD did not meet method acceptance criteria of £20%, 

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

(3) Sample GLP10-01 -02-03-009 (DAL-SD-WESB4-RB) PFOS result was 0,260 ng/mL, 

3 Introduction 

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

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

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

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

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

conducted to analyze ground water and surface water samples collected as part of the Avenue A 

Investigation in Decatur, AL for PFBS, PFHS, and PFOS in an effort to characterize on-site 

groundwater conditions. In addition, three aqueous soil-equipment rinseate samples from GLP10-01-

01-03 (Wetlands Edge Environment Center-WEEC Swamp), six soil-equipment rinseate samples 

from GLP10-01-01-05 (Avenue A Investigation - Soils), and one soil-equipment rinseate sample from 

GLP10-01-01-08 (Phase 3 Offsite Soil) are also reported herein. 

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 three 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 O2-PFBS, ^^Oa-PFHS, and 

^^Cs-PFOS (internal standards) at a nominal concentration of 1 ng/mL. However, due to the levels of 

PFBS, PFHS, and PFOS detected in the samples, the use of internal standards was not used for 

quantitation. See section 8.8 of the report for field matrix spike levels. The aqueous equipment 

rinseate samples were collected in plain bottles without markings or fortifications. 

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

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

Performance Liquid Chromatography/Mass Spectrometry Direct Injecfion Analysis". 

Page 11 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

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

collected, trip blanks, groundwater-equipment rinseate samples, and aqueous soil-equipment rinseate 

samples. Tables 9-34 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 

.»r;«-

4 'i'Cesf & ContmliSubstanceS'V' ' 

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

was purely analytical in nature. 

5 • Reference'Substances .. . 

Chemical Name 

Chemical Formula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFBS 

(predominantly linear) 

Perfluorobutane sulfonate 

C4F9SO3" 

Potassium Salt 

3M 

1/10/2017 

Frozen 

41-2600-8442-5 

TCR-121 

White Powder 

96.7% 

PFHS 

(linear) 

Perfluorohexane sulfonate 

CsFiaSOs 

Sodium Salt 

Wellington 

4/2/2013 

Frozen 

LPFHxSAMOS 

TCR08-0018 

Crystalline 

98% 

Reference Substance 

Chemical Name 

Chemical Formula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFOS 

(linear) 

Perfluorooctane sulfonate 

CsFiySOs 

Potassium Salt 

CAS #2795-39-3 

Wellington 

10/18/2013 

Frozen 

LPFOSKBM06 

TCR08-0001 

Crystalline 

98% 

PFOS 

(linear + branched) 

Perfluorooctane sulfonate 

C8F17SO3 

Potassium Salt 

CAS # 2795-39-3 

3M 

12/14/2016 

Frozen 

171 

TCR-696 

White Powder 

86.4% 

Page 12 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Reference Substance 

Chemical Name 

Chemical Formula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

"O2-PFBS 

Labeled - Perfluorobutane 

sulfonate 

C4F9S[^^02]0-

Ammonium Salt 

RTI International 

3/9/2015 

Frozen 

11546-107-2 

TCR-1013 

Liquid 

99% 

"OrPFHS 

Labeled - Perfluorohexane 

sulfonate 

CeFiaSt^'Oal^'O" 

Sodium Salt 

Wellington 

7/24/2011 

Frozen 

MPFHXA0706 

TCR-1218 

Liquid 

98% 

Reference Substance 

Chemical Name 

Chemical Formula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

"Cg-PFOS 

Perfluorooctane sulfonate 

CsFiy SO3 

Sodium Salt 

Wellington 

6/17/2012 

Frozen 

M8PFOS0609 

TCR09-0049 

Liquid 

98% 

Page 13 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

6 Test System 

The test system for this study are surface water and ground water samples collected from wells located 

in Decatur, AL by Weston Solutions, Inc. personnel. Samples for this study are "real worid" samples, 

not dosed with a specific lot of test substance. 

Table 2. Sample Description Key Code. 

string Numbier 

Example 

1 

2 

4 

String Descriptor 

DAL SWSW07 0100622 

Sample Type 

Sample Location 

Sampling Date 

Sample Type 

Example 

SW=Surfyce Water 

Example: SVV07 

100622-June 22, 2010 

0=piimary sample 

DB=duplicate sample 

LS = low spike 

MS = mid spike 

HS = high spike 

7 Method Summar y 

7.1 Methods 

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

"Determination of Perfluorinated Compounds In Water by High Performance Liquid 

Chromatography/Mass Spectrometry Direct Injection Analysis". 

,TM , 

7.2 Sample Collection 

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

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

June 25, July 13, and July 22, 2010. Samples were stored refrigerated at the laboratory after receipt. 

One set of laboratory prepared Trip Blank and Trip Blank field matrix spikes were returned with each 

batch of sample collection bottles. 

7.3 Sample Preparation 

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

analysis. 

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

(dilution 1:10). A few sampling locations were diluted 1:20 by diluting 0.5mL of sample with 9.5 mLs of 

Hi Q water. 

7.4 Analysis 

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

perfomiance 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. 

Page 14 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 3. Instrument Parameters. 

Instrument Name 

Analytical Method Followed 

Analysis Date 

Liquid Chromatograph 

Guard column 

Analytical column 

Injection Volume 

iVIass Spectrometer 

ion Source 

Electrode 

Polarity 

Software 

ETSStan 

ETS-8-044.0 

8/04/2010 

Agilent 1100 

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

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

10 nL 

Applied Biosystems API 4000 

Turiw Spray 

Turto ion electrode 

Negative 

Analyst 1,4,2 

bIbMaryAnn 

ETS-8-044,0 

9/10/10 

Agilent 1100 

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

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

2or10nL 

Applied Biosystems API 5000 

TurtDO Spray 

TurtDo ion electrode 

Negative 

Analyst 1,4,2 

Table 4. Liquid Chromatography Conditions. 

step 

Number 

Total Time 

(min) 

Flow Rate 

(fdJmin) 

Percent A 

(2 irM ammonium acetate) 

PercentB 

(Methanol) 

8/4/10 Analysis 

0 

1 

2 

3 

4 

5 

0 

1.0 

11,0 

13,5 

14,0 

17.0 

300 

300 

300 

300 

300 

300 

80,0 

80,0 

10,0 

10.0 

80,0 

80,0 

20,0 

20,0 

90,0 

90.0 

20,0 

20,0 

9/10/10 Analysis 

0 

1 

2 

3 

4 

5 

0 

2,0 

14,5 

15,5 

16,5 

20,0 

300 

300 

300 

300 

300 

300 

90,0 

90,0 

5,0 

5,0 

90,0 

90,0 

10,0 

10.0 

95,0 

95,0 

10,0 

10,0 

Table 5. Mass Transitions. 

Analyte 

PFBS 

PFHS 

PFOS 

Mass Transition 

Q1/Q3 

299/80 

299/99 

399/80 

399/99 

499/80 

499/99 

499/130 

Dwell time was 50 or 125 msec for each 

transition. The individual transitions were 

summed to produce a "total ion chromatogram" 

(TIC), which was used for quantitation. 

Page 15 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

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 flfeen spiked standards ranging firam 0.025 ng/mL to 100 ng/mL (nominal) were 

analyzed. Low and/or high curve points were disabled as needed to meet calibration acceptance 

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

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

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

PFOS: The calibration curve was constmcted using the linear isomer of PFOS only. Since the samples 

were expected to contain both linear and branched isomers of PFOS, LCS and GLP10-01-02-06 

samples were quantitated by processing the PFOS linear and branched isomers separately and 

summing the calculated concentrations together to generate the final PFOS concentration. This was 

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. 

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. 

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. 

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. 

8.3 Limit of Quantitation (LOQ) 

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

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

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

Table 6. Limit of Quantitation (LOQ). 

Analysis Date 

8/4/10 

9/10/10 

Dilution 

1 

10 

20 

1 

200 

PFBS 

LOQ, ng/mL 

0.0255 

0.255 

0.510 

0.0306 

NA 

PFHS 

LOQ, ng/mL 

0.103 

1.03 

2.06 

0,103 

NA 

PFOS 

LOQ, ng/mL 

0,255 

2.55 

5,10 

NA 

20,4 

Page 16 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

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%. 

8.5 Blanks 

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

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

LOQ for each analyte 

8.6 Lab Control Spikes (LCSs) 

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

preparation set. LCSs were prepared by spiking known amounts of the analyte into 40 mL of Milli Q 

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

analyzed in the same manner as the samples. The method acceptance criteria states that the average 

of LCS at each level should be within 100% ± 20% with an RSD 220%. 

8/4/10 Analysis: Method acceptance criteria was met for the PFBS, PFHS, and the mid and high set of 

linear PFOS LCS samples. The low set of linear PFOS LCS had an average recovery of 121 %. 

9/10/10 Analysis: Method acceptance criteria was met for all three levels of LCS for PFBS. The mid 

and high LCS met method acceptance criteria for PFHS and PFOS. The average recovery for the low 

set of LCS for PFHS was 73.5% and not calculated for PFOS as the detected values were <LOQ. 

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 and branched) were prepared at three concentrations to evaluate the potential for 

analytical bias. 

8/4/10 Analysis: The low, mid, and high set of LCS (linear + branched ) did not meet method 

acceptance criteria with an average recovery of 166%, 128%, and 141 %, respectively. 

9/10/10 Analysis: The mid set of LCS (linear + branched), met method acceptance criteria, while the low 

set (57.4%) and high set (123%), did not meet method acceptance criteria. 

Based on the recovery of the linear and branched PFOA LCS, it is the opinion of the laboratory that the 

recovery discrepency of the linear and branched isomers of PFOA indicates an analytical bias. Because 

of this bias, the method uncertainty will be adjusted to 100% ± 41 %, based on the highest recovery of 

the linear and branched LCS, at the spike level most appropriate as compared to the on-column 

concentrations of PFOS detected in the samples. In this case, the 30 ppb LCS (linear + branched) 

analyzed on 8/4/10 with an average recovery of 141%. 

A method deviation addressing the LCS recoveries is included in the raw data package. 

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

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

LCS Percent Recovery = * 100% 

Spike Concentration 

LCS% RSD = ^'^"^^'•'^ ^^^'^''° " ^^ ^ ^^P"^^^^ '100% 

average LCS recovery 

Page 17 of 67 
GLP10-01-02; interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 7. Laboratory Control Splice Recovery. 

ETS-8-044,0 

Analyzed 8/4/10 

Lab ID 

LCS-100726-1 

LCS-100726-2 

LCS-100726-3 

Average ±%RSD 

LCS-100726-4 

LCS-100726-5 

LCS-100726-6 

Average ±%RSD 

LCS-100726-7 

LCS-100726-8 

LCS-100726-9 

Average ±%RSD 

PFBS 

Spiked 

Concentration 

(ng/mL) 

0,510 

0,510 

0,510 

Calculated 

Concentration 

(ng/mL) 

0.558 

0.593 

0.572 

YoRecovery 

110 

116 

112 

113% ±2.7% 

5.10 

5.10 

5.10 

4.59 

5.64 

5,64 

90,0 

111 

111 

104% ±12% 

30.6 

30.6 

30.6 

32.1 

32.9 

32,4 

105 

107 

106 

106% ±0.94% 

PFHS 

Spiked 

Concentration 

(ng/mL) 

0,515 

0,515 

0,515 

Calculated 

Concentration 

(ng/mL) 

0.513 

0.613 

0.531 

YoRecovery 

100 

119 

103 

107% ±9.7% 

5,15 

5.15 

5.15 

4.70 

5.63 

5,84 

91.2 

109 

113 

104% ±11% 

30.9 

30.9 

30.9 

32,6 

33,4 

33.4 

106 

108 

108 

107% ±1.1% 

ETS-8-044.0 

Analyzed 8/4/10 

Lab ID 

LCS-100726-1 

LCS-100726-2 

LCS-100726-3 

Average ±%RSD 

LCS-100726^ 

LCS-100726-5 

LCS-100726-6 

Average ±%RSD 

LCS-100726-7 

LCS-100726-8 

LCS-100726-9 

Average ± %RSD 

PFOS (linear) 

Spiked 

Concentration 

(ng/mL) 

0,510 

0,510 

0,510 

Calculated 

Concentration 

(ng/mL) 

0.590 

0,652 

0,613 

YoRecovery 

116 

128 

120 

121% ±5.1%TM 

5.10 

5,10 

5.10 

4,67 

5,70 

5,81 

91,6 

112 

114 

106% ±12% 

30,6 

30,6 

30,6 

34.5 

34.9 

34,9 

113 

114 

114 

114% ±0.66% 

Lab ID 

LCS-100726-10 

LCS-100726-11 

LCS-100726-12 

Average ±%RSD 

LCS-100726-13 

LCS-100726-14 

LCS-100726-15 

Average ±%RSD 

LCS-100726-16 

LCS-100726-17 

LCS-100726-18 

Average ±%RSD 

PFOS (linear + branched) 

Spiked 

Concentration 

(ng/mL) 

0,500 

0,500 

0,500 

Calculated 

Concentration 

(ng/mL) 

0.844 

0,829 

0,817 

YoRecovery 

169 

166 

163 

166% ±1.6%TM 

5,00 

5.00 

5,00 

6,28 

6,49 

6,38 

126 

130 

128 

128% ±1.6%TM 

30,0 

30,0 

30,0 

42,2 

41,9 

43,1 

141 

140 

144 

141% ±1.5%TM 

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

Page 18 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 7 continued. Laboratory Control Spil<e Recovery. 

ETS-8-044,0 

Analyzed 9/10/10 

Lab ID 

LCS-100910-1 

LCS-100910-2 

LCS-100910-3 

Average ±%RSD 

LCS-100910-4 

LCS-100910-5 

LCS-100910-6 

Average ±%RSD 

LCS-100910-7 

LCS-100910-8 

LCS-100910-9 

Average ±%RSD 

PFBS 

Spiked 

Concentration 

(ng/mL) 

0,204 

0,204 

0,204 

Calculated 

Concentration 

(ng/mL) 

0,185 

0,231 

0,245 

YoRecovery 

90.7 

113 

120 

108% ±14% 

5,10 

5,10 

5,10 

5,17 

5,79 

5,43 

101 

113 

106 

107% ±5.7% 

15.3 

15.3 

15.3 

14,8 

17.3 

17.1 

96,9 

113 

111 

107% ±8.2% 

PFHS 

Spiked 

Concentration 

(ng/mL) 

0,206 

0,206 

0,206 

Calculated 

Concentration 

(ng/mL) 

<0,103 

0.144 

0,159 

YoRecovery 

NA 

69,8 

77,1 

73.5% ±7.0%TM 

5.15 

5,15 

5,15 

5,20 

5,77 

5.45 

101 

112 

106 

106% ±5.2% 

15,5 

15,5 

15,5 

14.9 

16.6 

16.7 

96,1 

107 

108 

104% ±6.4% 

ETS-8-044,0 

Analyzed 9/10/10 

Lab ID 

LCS-100910-1 

LCS-100910-2 

LCS-100910-3 

Average ±%RSD 

LCS-100910-4 

LCS-100910-5 

LCS-100910-6 

Average ±%RSD 

LCS-100910-7 

LCS-100910-8 

LCS-100910-9 

Average ±%RSD 

PFOS (linear) 

Spiked 

Concentration 

(ng/mL) 

0,204 

0,204 

0,204 

Calculated 

Concentration 

(ng/mL) 

<0.102 

<0.102 

<0.102 

YoRecovery 

NA 

NA 

NA 

NA 

5.10 

5.10 

5.10 

4.44 

4.97 

4.65 

87.1 

97,5 

91,1 

91.9% ±5.7% 

15.3 

15.3 

15,3 

13.7 

15.5 

16.2 

89,5 

101 

106 

98.8% ±8.6% 

Lab ID 

LCS-100910-10 

LCS-100910-11 

LCS-100910-12 

Average ±%RSD 

LCS-100910-13 

LCS-100910-14 

LCS-100910-15 

Average ±%RSD 

LCS-100910-16 

LCS-100910-17 

LCS-100910-18 

Average ±%RSD 

PFOS (linear + branched) 

Spiked 

Concentration 

(ng/mL) 

0,495 

0.495 

0,495 

Calculated 

Concentration 

(ng/mL) 

0.302 

0.278 

0,273 

YoRecovery 

60,9 

56,2 

55,2 

57.4% ± 5.3% '^' 

4.95 

4,95 

4,95 

4,92 

5,02 

5,81 

99,3 

101 

117 

106% ±9.2% 

14,8 

14,8 

14,8 

17,8 

18,3 

18,3 

120 

124 

124 

123% ±1.9%TM 

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

8.7 Analytical Method Uncertainty 

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

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

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

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

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

method uncertainty values listed in Table 7 for PFBS and PFHS. For PFOS, the analytical uncertainty 

Page 19 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

was determined based on the quality control data generated with the project samples (Table 6) and 

was used to evaluate method accuracy and precision. Due to the analytical high bias observed during 

the quantitation of the linear + branched PFOS against a calibration curve constmcted from the 

analysis of calibration standards containing linear PFOS only, an analytical uncertainty of 41 % is 

applied to all PFOS sample results for this project. 

Table 8. Analytical Uncertainty. 

Analyte 

PFBS 

PFHS 

PFOS 

Standard Deviation 

10.6 

11.6 

NA<^> 

Method 

Uncertainty 

100%±21% 

100%±23% 

100%±41% 

(1) NA = Not Applicable, See section 8,6 of the report for a discussion on the assigning of the method uncertainty for PFOS, 

8.8 Field Matrix Spikes (FMS) 

Low, mid and high 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% confimn 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.. 

The nominal spike level for the low field matrix spike was 1.0 ng/mL, the mid field matrix spike was 10 

ng/mL, and the high field marix spike was 100 ng/mL for all sampling locations. For some sampling 

locations, the high field matrix spike was not appropriate as compared to the sample concentration. 

Field matrix spike levels will be adjusted accordingly for the next sampling event. 

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

FMS Recovery = -^^ 2 £: :: £Li. • i oo% 

Spike Concentraton 

8.9 Laboratory Matrix Spikes (LMS) 

Samples were analyzed under project GLP10-01-01-06 for PFOA. Results from that analysis found 

that the high FMS level was not sufficient for several of the surface water sampling locations for PFOA. 

Since it was presumed that the levels of PFOS in these samples would be similar to the PFOA results, 

laboratory matrix spikes were prepared for GLP10-01-01-06 were analyzed instead of the FMS 

samples prepared with the sample set. Laboratory matrix spike were prepared and analyzed for the 

following sample locations: 

200ppb LMS: DAL SW SW01, DAL SW SW04, DAL SW SW05, and DAL SW SW08, 

400ppb LMS; DAL SW SW10 and DAL SW SW11, 

500ppb LMS; DAL SW SW09, and 

1500ppb LMS; DAL GW GP07 and DAL GW GP08 

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

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

analysis. 

Page 20 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

.„„ „ (LMS Sample Conc^entration - Average Concentration: Sample & Sample Pup,)«..pno/ 

LMS Spike Concentraton 

9 Data SummaiyXanB'Disci^^ 

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

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

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

from those listed in the raw data. 

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

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

GW GRS04Q1 - The recovery of the high FMS sample for PFOS was 134%. This was the only 

appropriate field matrix spike level for PFOS. Since the method analytical uncertainty is 100% ± 44%, 

no adjustment was made to the analytical uncertainty for PFOS. 

Page 21 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Tables. DALSWSW01 100623 

3M LIMS ID 

GLP10-01-02-06-035 

GLP10-01-02-06-036 

GLP10-01-02-06-037 

GLP10-01-02-06-038 

GLP10-01-02-06-039 

GLP10-01-02-06-036 LMS 

Description 

DALSWSW01 0 100623 

DALSWSW01 DB 100623 

DALSWSW01 LS 100623 

DAL SW SW01 MS 100623 

DALSWSW01 HS 100623 

DAL SW SW01 DB - 200ppb LMS 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

15.3 

14.7 

NA'" 

NA'" 

NA'" 

246 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

113 

15.0 ng/mL ±4.0Yo 

PFHS 

Concentration 

(ng/mL) 

119 

121 

NA'" 

NA'" 

NA'" 

345 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

109 

120 ng/mL ±1.r/o 

PFOS 

Concentration 

(ng/mL) 

243 

253 

NA'" 

NA'" 

NA'" 

505 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

126 

248 ng/mL ±4.0Yo 

NA = Not Applicable 

(1) Ttie sample was not analyzed. 

Table 10. DAL SW SW02 100622 

3M LIMS ID 

GLP10-01-02-06-030 

GLP10-01-02-06-031 

GLP10-01-02-06-032 

GLP10-01-02-06-033 

GLP10-01-02-06-034 

Description 

DAL SWSW02 0 100622 

DAL SW SW02 DB 100622 

DAL SWSW02LS 100622 

DAL SW SW02 LS 100622 

DAL SW SW02 HS 100622 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

7.48 

7.87 

NA'" 

NA'" 

119 

YoRecovery 

NA 

NA 

NA'" 

NA<" 

109 

7.68 ng/mL tS.IYo 

PFHS 

Concentration 

(ng/mL) 

51.9 

52.0 

NA<" 

NA<" 

161 

YoRecovery 

NA 

NA 

NA<" 

NA<" 

106 

52.0 ng/mL ±0.19Yo 

PFOS 

Concentration 

(ng/mL) 

221 

205 

NA'" 

NA'" 

307 

YoRecovery 

NA 

NA 

NA<" 

NA<" 

92.4 

213 ng/mL ±7.7Yo 

NA = Not Applicable 

(1) Ttie sample was not analyzed. 

Page 22 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 11. DAL SW SW03 100622 

3M LIMS ID 

GLP10-01-02-06-021 

GLP10-01-02-06-022 

GLP10-01-02-06-023 

GLP10-01-02-06-024 

GLP10-01-02-06-025 

Description 

DAL SWSW03 0 100622 

DAL SWSW03DB 100622 

DAL SWSW03LS 100622 

DAL SW SW03 MS 100622 

DAL SWSW03HS 100622 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

9.51 

9.62 

NA'" 

NA'" 

120 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

108 

9.57 ng/mL ±1.2% 

PFHS 

Concentration 

(ng/mL) 

71.4 

72.9 

NA'" 

NA<" 

184 

YoRecovery 

NA 

NA 

NA<" 

NA<" 

109 

72.2 ng/mL ±2.1Yo 

PFOS 

Concentration 

(ng/mL) 

196 

198 

NA<" 

NA<" 

278 

YoRecovery 

NA 

NA 

NA<" 

NA<" 

80.1 

197 ng/mL ±1.1Yo 

NA= Not Applicable 

(1) Ttie sample was not analyzed. 

Table 12. DAL SW SW04 100622 

3M LIMS ID 

GLP10-01-02-06-016 

GLP10-01-02-06-017 

GLP10-01-02-06-018 

GLP10-01-02-06-019 

GLP10-01-02-06-020 

GLP10-01-02-06-017; LMS 

Average Concen 

Description 

DAL SWSW04 0 100622 

DAL SW SW04 DB 100622 

DAL SW SW04 LS 100622 

DAL SWSW04 MS 100622 

DAL SWSW04HS 100622 

DAL SW SW04 DB - 200ppb LMS 

ti^on (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

14.1 

13.3 

NA'" 

NA'" 

NA'" 

230 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

106 

13.7 ng/mL ±5.8Yo 

PFHS 

Concentration 

(ng/mL) 

87.3 

85.6 

NA'" 

NA'" 

NA'" 

320 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

113 

86.5 ng/mL ±2.0% 

PFOS 

Concentration 

(ng/mL) 

190 

194 

NA'" 

NA'" 

NA'" 

413 

%Recovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

108 

192 ng/mL ±2.r/o 

NA = Not Applicable 

(1) TTie sample was not analyzed. 

Page 23 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 13. DAL SWSW05 100622 

3M LIMS ID 

GLP10-01-02-06-011 

GLP10-01-02-06-012 

GLP10-01-02-06-013 

GLP10-01-02-06-014 

GLP 10-01-02-06-015 

GLP10-01-02-06-012; LMS 

Average Concen 

Description 

DAL SWSW05 0 100622 

DAL SW SW05 DB 100622 

DAL SWSW05LS 100622 

DAL SWSW05 MS 100622 

DAL SW SW05 HS 100622 

DAL SW SW05 DB - 200ppb LMS 

tration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

21.1 

20.7 

NA'" 

NA'" 

NA'" 

247 

%Recovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

111 

20.9 ng/mL ±1.9Yo 

PFHS 

Concentration 

(ng/mL) 

104 

100 

NA'" 

NA'" 

NA'" 

327 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

109 

102 ng/mL ±3.9Yo 

PFOS 

Concentration 

(ng/mL) 

399 

385 

NA<" 

NA<" 

NA<" 

615 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

109 

392 ng/mL ±3.6Yo 

NA = Not Applicatile 

(1) The sample was not analyzed. 

Table 14. DAL SW SW06 100622 

3MUMSID 

GLP10-01-02-06-006 

GLP10-01-02-06-007 

GLP10-01-02-06-008 

GLP 10-01-02-06-009 

GLP 10-01-02-06-010 

Average Concent 

Description 

DAL SWSW06 0 100622 

DAL SWSW06DB 100622 

DAL SWSW06LS 100622 

DAL SWSW06 MS 100622 

DAL SW SW06 HS 100622 

ration (ng/mL) ± YoRPD 

PFBS 

(ng/mL) 

17.8 

17.0 

NA'" 

NA'" 

131 

YoRecovery 

NA 

NA 

NA<" 

NA<" 

111 

17.4 ng/mL ±4.6Yo 

PFHS 

Concentration 

(ng/mL) 

77.8 

77.2 

NA'" 

NA'" 

190 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

109 

77.5 ng/mL ±0.77Yo 

PFOS 

Concentiation 

(ng/mL) 

229 

227 

NA<" 

NA'" 

325 

YoRecovery 

NA 

NA 

NA<" 

NA<" 

95.3 

228 ng/mL ±1.1Yo 

NA = Not Applicable 

(1) The sample was not analyzed. 

Page 24 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 15. DAL SWSW07 100622 

3M LIMS ID 

GLP10-01-02-06-001 

GLP10-01-02-06-002 

GLP10-01-02-06-003 

GLP10-01-02-06-004 

GLP10-01-02-06-005 

Average Concent 

Description 

DAL SWSW06 0 100622 

DAL SWSW06DB 100622 

DAL SW SW06 LS 100622 

DAL SWSW06 MS 100622 

DAL SWSW06HS 100622 

ration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

10.8 

10.8 

NA<" 

NA<" 

129 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

116 

10.8 ng/mL ±0.0Yo 

PFHSf^^ 

Concentration 

(ng/mL) 

47.6 

48.1 

NA' " 

NA' " 

174 

YoRecovery 

NA 

NA 

NA<" 

NA<" 

122 

47.9 ng/mL ±1.0Yo 

PFOS 

Concentration 

(ng/mL) 

128 

131 

NA' " 

NA' " 

222 

YoRecovery 

NA 

NA 

NA'" 

NA' " 

90.8 

129ng/mL±2.2yo 

NA = Not Applicable 

(1) Ttie sample was not analyzed. 

Table 16. DAL SW SWOB 100623 

3M LIMS ID 

GLP10-01-02-06-045 

GLP10-01-02-06-046 

GLP10-01-02-06-047 

GLP10-01-02-06-048 

GLP10-01-02-06-049 

GLP10-01-02-06-046; LMS 

Description 

DAL SWSW08 0 100623 

DAL SWSW08DB 100623 

DAL SWSW08LS 100623 

DAL SW SW08 MS 100623 

DAL SWSW08HS 100623 

DAL SW SW08 DB - 200ppb LMS 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

39.8 

41.5 

NA<" 

NA'" 

NA' " 

264 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

109 

40.7 ng/mL ±4.2% 

PFHS 

Concentration 

(ng/mL) 

169 

163 

NA' " 

NA' " 

NA' " 

392 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

110 

166 ng/mL ±3.6Yo 

PFOS 

Concentration 

(ng/mL) 

268 

263 

NA'" 

NA'" 

NA'" 

504 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

117 

266 ng/mL ±1.9Yo 

NA= Not Applicable 

(1) The sample was not analyzed. 

Page 25 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 17. DAL SWSW09 100623 

3M LIMS ID 

GLP10-01-02-06-050 

GLP10-01-02-06-051 

GLP10-01-02-06-052 

GLP10-01-02-06-053 

GLP10-01-02-06-054 

GLP10-01-02-06-051;LMS 

Average Concer 

Description 

DAL SWSW09 0 100623 

DAL SWSW09DB 100623 

DAL SWSW09LS 100623 

DAL SW SW09 MS 100623 

DAL SWSW09HS 100623 

DAL SW SW09 DB - 500ppb LMS 

rtration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

275 

282 

NA'" 

NA'" 

NA'" 

808 

YoRecovery 

NA 

NA 

NA<" 

NA<" 

NA'" 

104 

279 ng/mL ±2.5Yo 

PFHS 

Concentration 

(ng/mL) 

672 

614 

NA'" 

NA'" 

NA'" 

1200 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

108 

643 ng/mL ±9.0% 

PFOS 

Concentration 

(ng/mL) 

386 

378 

NA<" 

NA<" 

NA<" 

960 

%Recovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

113 

382 ng/mL ±2.1% 

NA = Not Applicable 

(1) The sample was not analyzed. 

Table 18. DAL SWSW10 100623 

3M LIMS ID 

GLP 10-01-02-06-060 

GLP10-01-02-06-061 

GLP10-01-02-06-062 

GLP10-01-02-06-063 

GLP10-01-02-06-064 

GLP10-01-02-06-061;LMS 

Average Concer 

Description 

DAL SWSW10 0 100623 

DAL SWSW10DB 100623 

DAL SW SW10 LS 100623 

DAL SWSW10 MS 100623 

DAL SWSW10HS 100623 

DAL SW SW10 DB - 400ppb LMS 

rtration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

23.0 

22.0 

NA'" 

NA'" 

NA'" 

420 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

97.4 

22.5 ng/mL ±4.4% 

PFHS 

Concentration 

(ng/mL) 

236 

230 

NA'" 

NA'" 

NA'" 

661 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

104 

233 ng/mL ±2.6% 

PFOS 

Concentration 

(ng/mL) 

387 

391 

NA'" 

NA<" 

NA'" 

805 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA<" 

102 

389 ng/mL ±1.0% 

NA = Not Applicable 

(1) The sample was not analyzed. 

Page 26 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 19. DAL SWSW11 100623 

3M LIMS ID 

GLP10-01-02-06-055 

GLP10-01-02-06-056 

GLP10-01-02-06-057 

GLP10-01-02-06-058 

GLP10-01-02-06-059 

GLP10-01-02-06-056; LMS 

Description 

DALSWSW11 0 100623 

DALSWSW11 DB 100623 

DALSWSW11 LS 100623 

DALSWSW11 MS 100623 

DAL SW SW11 HS 100623 

DALSWSW11 DB -500ppbLMS 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

103 

100 

NA'" 

NA'" 

NA'" 

641 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

106 

102 ng/mL ±3.0% 

PFHS 

Concentration 

(ng/mL) 

1120 

1130 

NA<" 

NA'" 

NA<" 

1830 

-

YoRecovery 

NA 

NA 

NA<" 

NA'" 

NA'" 

NO 

1130ng/mL±0.89Yo^^ 

PFOS 

Concentration 

(ng/mL) 

863 

836 

NA'" 

NA'" 

NA<" 

1400 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

108 

850 ng/mL ±3.2% 

NA= Not Applicable 

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

(1) The sample was not analyzed. 

(2) Sampling location did not have an appropriate field matrix spike level. 

Page 27 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 20. DAL SW SW12 100623 

3M LIMS ID 

GLP10-01-02-06-040 

GLP10-01-02-06-041 

GLP10-01-02-06-042 

GLP10-01-02-06-043 

GLP10-01-02-06-044 

Average Conceirt 

Description 

DAL SWSW12 0 100623 

DAL SWSW12DB 100623 

DAL SW SW12 LS 100623 

DAL SWSW12 MS 100623 

DAL SWSW12HS 100623 

ration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

0.773 

0.755 

NA<" 

12.4 

114 

YoRecovery 

NA 

NA 

NA'" 

114 

111 

0.764 ng/mL ±2.4% 

PFHS 

Concentration 

(ng/mL) 

3.69 

3,67 

NA'" 

15.3 

113 

YoRecovery 

NA 

NA 

NA<" 

113 

106 

3.68 ng/mL ±0.54% 

PFOS 

Concentration 

(ng/mL) 

103 

105 

NA'" 

118 

168 

YoRecovery 

NA 

NA 

NA<" 

NC 

63.5'^' 

104 ng/mL ±2.0Yo 

NA = Not Applicable 

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

(1) The sample was not analyzed. 

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

Table 21. DAL GWGP01 100709 

3M LIMS ID 

GLP10-01-02-06-070 

GLP10-01-02-06-071 

GLP10-01-02-06-072 

GLP10-01-02-06-073 

GLP10-01-02-06-074 

Average Concent 

Description 

DALGWGP01 0 1007009 

DALGWGP01 DB 100709 

DALGWGP01 LS 100709 

DALGWGP01 MS 100709 

DALGWGP01 HS 100709 

ration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

5.01 

5.02 

6.60 

17.1 

123 

5.02 ng/m 

YoRecovery 

NA 

NA 

NC 

118 

116 

L±0.20Yo 

PFHS 

Concentration 

(ng/mL) 

7.49 

7.22 

9.33 

19.5 

121 

YoRecovery 

NA 

NA 

NC 

118 

110 

7.36 ng/mL ±3.7Yo 

PFOS 

Concentration 

(ng/mL) 

26.9 

25.5 

NA<" 

NA'" 

115 

YoRecovery 

NA 

NA 

NA<" 

NA<" 

87.3 

26.2 ng/mL ±5.3% 

NA= Not Applicable 

(1) The sample was not analyzed. 

Page 28 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 22. DAL GW GP02 100709 

3M LIMS ID 

GLP10-01-02-06-075 

GLP10-01-02-06-076 

GLP10-01-02-06-077 

GLP10-01-02-06-078 

GLP10-01-02-06-079 

Description 

DAL GWGP02 0 1007009 

DAL GWGP02DB 100709 

DAL GWGP02LS 100709 

DAL GW GP02 MS 100709 

DAL GWGP02HS 100709 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

19.7 

22.4 

NA<" 

NA<" 

134 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

. Il l 

21.1 ng/mL ± 13%, 

PFHS 

Concentration 

(ng/mL) 

10.4 

11.9 

NA'" 

NA'" 

127 

YoRecovery 

NA 

NA 

NA'" 

NA<" 

112 

11.2 ng/mL ±13% 

PFOS 

Concentration 

(ng/mL) 

15.7 

19.3 

NA'" 

NA'" 

87.6 

YoRecovery 

NA 

NA 

NA'" 

NA<" 

68.7'^' 

17.5 ng/mL ±20% 

NA= Not Applicable 

(1) The sample was not analyzed. 

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

Table 23. DAL GWGP03 100709 

3M LIMS ID 

GLP10-01-02-06-080 

GLP10-01-02-06-081 

GLP10-01-02-06-082 

GLP10-01-02-06-083 

GLP 10-01-02-06-084 

Description 

DAL GWGP03 0 1007009 

DAL GWGP03DB 100709 

DAL GW GP03 LS 100709 

DAL GW GP03 MS 100709 

DALGWGP03HS 100709 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

66.2 

66.5 

NA'" 

NA<" 

180 

YoRecovery 

NA 

NA 

NA'" 

NA<" 

111 

66.4 ng/mL ±0.45% 

PFHS 

Concerrtration 

(ng/mL) 

413 

412 

NA'" 

NA'" 

571 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NC 

413 ng/mL ±0.24%'^ 

PFOS 

Concerrtration 

(ng/mL) 

341 

405 

NA<" 

NA<" 

678 

YoRecovery 

NA 

NA 

NA'" 

NA<" 

NC 

373 ng/mL ±17%'^ 

NA = Not Applicable 

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

(1) The sample was not analyzed. 

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

Page 29 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples firom Decatur, AL 

June/July 2010 

Table 24. DAL GW GP04 100709 

3M LIMS ID 

GLP10-01-02-06-085 

GLP10-01-02-06-086 

GLP10-01-02-06-087 

GLP10-01-02-06-088 

GLP10-01-02-06-089 

Description 

DAL GW GP04 0 1007009 

DAL GWGP04DB 100709 

DAL GW GP04 LS 100709 

DAL GWGP04 MS 100709 

DAL GWGP04HS 100709 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concerrtration 

(ng/mL) 

19.1 

19.1 

NA'" 

NA'" 

136 

YoRecovery 

NA 

NA 

NA<" 

NA<" 

115 

19.1 ng/mL ±0.0% 

PFHS 

Concentration 

(ng/mL) 

89.5 

82.1 

NA'" 

NA'" 

232 

%Recovery 

NA 

NA 

NA'" 

NA<" 

142(2) 

85.8 ng/mL ±8.6%''' 

PFOS 

Concentration 

(ng/mL) 

175 

130 

NA<" 

NA<" 

296 

YoRecovery 

NA 

NA 

NA'" 

NA<" 

141 '^' 

152ng/mL±30Yo''-^ 

NA= Not Applicable 

(1) The sample was not analyzed. 

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

(3) The analytical unceitainty has been adjusted for field matrix spike recovety to 100% ± 42% for PFHS and 100% ± 41 % for PFOS. 

(4) The sample/sample duplicate RPD did not meet method acceptance criteria of <20%. 

Page 30 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 25. DAL GW GP05 100709 

3M LIMS ID 

GLP10-01-02-06-090 

GLP10-01-02-06-091 

GLP10-01-02-06-092 

GLP10-01-02-06-093 

GLP10-01-02-06-094 

Description 

DAL GWGP05 0 1007009 

DAL GWGP05DB 100709 

DAL GWGP05LS 100709 

DAL GWGP05 MS 100709 

DAL GWGP05HS 100709 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(rig/mL) 

30.0 

30.0 

NA'" 

NA'" 

141 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

109 

30.0 ng/mL ±0.0% 

PFHS 

Concentration 

(ng/mL) 

162 

153 

NA'" 

NA'" 

280 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

119 

158 ng/mL ±5.r/o 

PFOS 

Concerrtration 

(ng/mL) 

416 

347 

NA<" 

NA<" 

515 

YoRecovery 

NA 

NA 

NA<" 

NA<" 

NC 

382ng/mL±18Yo'^ 

NA= Not Applicable 

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

(1) The sample was not analyzed. 

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

Table 26. DAL GW GP07 100709 

3MUMSID 

GLP 10-01-02-06-095 

GLP10-01-02-06-096 

GLP10-01-02-06-097 

GLP10-01-02-06-098 

GLP10-01-02-06-099 

GLP10-01-02-06-095 LMS 

Average Concent 

Description 

DAL GWGP07 0 1007009 

DALGWGP07DB 100709 

DAL GWGP07LS 100709 

DAL GWGP07 MS 100709 

DAL GW GP07 HS 100709 

DAL GWGP07 0; 1500ppb LMS 

'ration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

20.3 

21.1 

NA'" 

NA'" 

137 

NA'" 

YoRecovery 

NA 

NA 

NA<" 

NA'" 

114 

NA'" 

20.7 ng/mL ±3.9% 

PFHS 

Concentration 

(ng/mL) 

173 

168 

NA<" 

NA<" 

298 

NA<" 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

124 

NA'" 

171 ng/mL ± 2.9% 

PFOS 

Concentration 

(ng/mL) 

MAO 

1820 

NA'" 

NA'" 

NA'" 

3660 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA'" 

123 

1780 ng/mL ±4.5% 

NA = Not Applicable 

(1) The sample was not analyzed. 

Page 31 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 27. DAL GW GP08 100709 

3M LIMS ID 

GLP10-01-02-06-100 

GLP10-01-02-06-101 

GLP10-01-02-06-102 

GLP10-01-02-06-103 

GLP10-01-02-06-104 

GLP10-01-02-06-100LMS 

Average Concent 

Description 

DAL GW GP08 0 1007009 

DAL GWGP08DB 100709 

DAL GWGP08LS 100709 

DAL GWGP08 MS 100709 

DAL GWGP08HS 100709 

DAL GWGP08 0; ISOOppb LMS 

tation (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

6.39 

6.32 

NA'" 

NA'" 

118 

NA<" 

YoRecovery 

NA 

NA 

NA<" 

NA'" 

109 

NA'" 

6.36 ng/mL ±1.1% 

PFHS 

Concerrtration 

(ng/mL) 

67.4 

72.9 

NA'" 

NA'" 

173 

NA<" 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

99.9 

NA'" 

70.2 ng/mL ±7.8% 

PFOS 

Concentration 

(ng/mL) 

1380 

1450 

NA'" 

NA'" 

NA'" 

3210 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NA<" 

117 

1420 ng/mL ±4.9% 

NA = Not Applicable 

(1) The sample was not analyzed. 

Table 28. DAL GW GP09 100709 

3M LIMS ID 

GLP10-01-02-06-105 

GLP10-01-02-06-106 

GLP10-01-02-06-107 

GLP10-01-02-06-108 

GLP10-01-02-06-109 

Description 

DAL GWGP09 0 1007009 

DAL GWGP09DB 100709 

DAL GWGP09 LS 100709 

DAL GW GP09 MS 100709 

DAL GWGP09HS 100709 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

20.9 

20.5 

NA<" 

NA'" 

128 

YoRecovery 

NA 

NA 

NA<" 

NA<" 

105 

20.7 ng/mL ±1.9% 

PFHS 

Concentration 

(ng/mL) 

33.7 

38.3 

NA'" 

NA<" 

147 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

108 

36.0 ng/mL ±13Yo 

PFOS 

Concentration 

(ng/mL) 

79.9 

111 

NA'" 

NA<" 

188 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

90.6 

95.5 ng/mL ± 33%'^ 

NA = Not Applicable 

(1) The sample was not analyzed. 

(2) The sample/sample duplicate RPD did not meet method acceptance criteria of <20%. 

Page 32 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 29. DAL GW GP10 100709 

3M LIMS ID 

GLP10-01-02-06-110 

GLP10-01-02-06-111 

GLP10-01-02-06-112 

GLP10-01-02-06-113 

GLP10-01-02-06-114 

Description 

DAL GWGP10 01007009 

DAL GWGP10DB 100709 

DAL GWGP10LS 100709 

DAL GWGP10 MS 100709 

DAL GWGP10HS 100709 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concerrtration 

(ng/mL) 

441 

452 

NA'" 

NA'" 

541 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NC 

447 ng/mL ±2.5Yo'^ 

PFHS 

Concerrtration 

(ng/mL) 

A l l 

413 

NA<" 

NA<" 

532 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NC 

420ng/mL±3.3Yo^ 

PFOS 

Concentration 

(ng/mL) 

146 

107 

NA'" 

NA<" 

200 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

72.1 

127 ng/mL ± 31%'' ' 

NA = Not Applicable 

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

(1) The sample was not analyzed. 

(2) Sampling location did not have an appropriate field matrix spike level for PFS or PFHS. 

(3) The sample/sample duplicate RPD did not meet method acceptance criteria of <20%. 

Table 30. DAL GWGP11 100708 

3M LIMS ID 

GLP10-01-02-06-115 

GLP10-01-02-06-116 

GLP10-01-02-06-117 

GLP10-01-02-06-118 

GLP10-01-02-06-119 

Description 

DALGWGP11 0 1007008 

DALGWGP11 DB 100708 

DALGWGP11 LS 100708 

DALGWGP11 MS 100708 

DALGWGP11 HS 100708 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

65.9 

68.0 

NA<" 

NA<" 

181 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

112 

67.0 ng/mL ±3.1% 

PFHS 

Concentration 

(ng/mL) 

327 

333 

NA'" 

NA<" 

486 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NC 

330 ng/mL ± 1.8% (^ 

PFOS 

Concentration 

(ng/mL) 

640 

680 

NA'" 

NA'" 

1076 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

NC 

660 ng/mL ±6.1%'^ 

NA = Not Applicable 

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

(1) The sample was not analyzed. 

(2) Sampling location did not have an appropriate field matrix spike level for PFS or PFHS. 

Page 33 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 31. DAL GWGP12 100708 

3M LIMS ID 

GLP10-01-02-06-120 

GLP10-01-02-06-121 

GLP10-01-02-06-122 

GLP10-01-02-06-123 

GLP10-01-02-06-124 

Description 

DAL GWGP12 0 1007008 

DALGWGP12DB 100708 

DALGWGP12LS 100708 

DAL GW GP12 MS 100708 

DALGWGP12HS 100708 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

1.84 

3.33 

3.92 

14.4 

117 

YoRecovery 

NA 

NA 

NC 

116 

112 

2.59 ng/mL ±58%'^ 

PFHS 

Concentration 

(ng/mL) 

8.78 

13.7 

13.8 

24.4 

126 

YoRecovery 

NA 

NA 

NC 

128 

111 

11.2 ng/mL ±44%'^ 

PFOS 

Concentration 

(ng/mL) 

32.4 

65.1 

NA'" 

NA'" 

148 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

96.9 

48.8ng/mL±67Yo'^ 

NA = Not Applicable 

(1) The sample was not analyzed. 

(2) The sample/sample duplicate RPD did not meet method acceptance criteria of s20%. 

Table 32. DAL GW 216R 100716 

3M LIMS ID 

GLP10-01-02-06-130 

GLP10-01-02-06-131 

GLP10-01-02-06-132 

GLP10-01-02-06-133 

GLP10-01-02-06-134 

Average Concent 

Description 

DAL GW216R 0 1007016 

DALGW216RDB 100716 

DAL GW216RLS 100716 

DAL GW216R MS 100716 

DALGW216RHS 100716 

"ration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

10.5 

10.7 

NA<" 

NA<" 

118 

YoRecovery 

NA 

NA 

NA<" 

NA<" 

105 

10.6ng/mL±1.9% 

PFHS 

Concentration 

(ng/mL) 

30.9 

30.0 

NA'" 

NA'" 

141 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

107 

30.5 ng/mL ±3.0% 

PFOS 

Concentration 

(ng/mL) 

114 

125 

NA'" 

NA'" 

192 

YoRecovery 

NA 

NA 

NA'" 

NA'" 

71.6 

119 ng/mL ±9.Z'/o 

NA = Not Applicable 

(1) The sample was not analyzed. 

Page 34 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 33. Trip Blank 

3M LIMS ID 

GLP10-01-02-06-026 

GLP10-01-02-06-027 

GLP10-01-02-06^28 

GLP10-01-02-06-029 

GLP10-01-02-06-066 

GLP10-01-02-06-067 

GLP10-01-02-06-068 

GLP10^1-02-06-069 

GLP10-01-02-06-125 

GLP10-01-02-06-126 

GLP10-01-02-06-127 

GLP1(W)1-02-06-128( 

Description 

DAL SWTRIP1 0100622 

DAL SWTRIP1LS 100622 

DALSWTRIP1 MS 100622 

DAL SWTRIP1HS 100622 

DALGWTRIP1 0100708 

DALGWTR1P1LS 100708 

DALGWTRIP1 MS 100708 

DAL GWTRIP1HS 100708 

DAL GWTRIP2 0100716 

DAL GWTRIP2LS100716 

DAL GWTRIP2 MS 100716 

DAL GWTRIP2HS100716 

PFBS 

Concentration 

(ng/mL) 

<0.0255 

1.21 

11.4 

120 

<0.102 

1.21 

11.9 

121 

<0.102 

1.16 

11.4 

112 

YoRecovery 

NA 

119 

112 

118 

NA 

119 

117 

119 

NA 

114 

112 

110 

PFHS 

Concentration 

(ng/mL) 

<0.103 

1.19 

11.6 

119 

<0.258 

1.15 

11.6 

119 

<0.258 

1.12 

11.7 

115 

YoRecovery 

NA 

116 

113 

116 

NA 

112 

113 

116 

NA 

109 

114 

112 

PFOS 

Concerrtration 

(ng/mL) 

<0.255 

1.22 

10.9 

101 

<0.255 

1.13 

10.6 

102 

<0.255 

1.22 

10.9 

102 

YoRecovery 

NA 

120 

107 

99.0 

NA 

111 

104 

100 

NA 

120 

107 

100 

NA = Not Applicable 

Page 35 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Table 34. Rinseate Blanks 

3M LIMS ID 

GLP10-01-01-06-065 

GLP10-01-01-06-129 

GLP10-01-01-03-009 

GLP10-01-01-03-015 

GLP10-01-01-03-021 

GLP10^1-01-05-008 

GLP10-01-01-05-020 

GLP1001-01-05-053 

GLP10-01-01-05O86 

GLP10-01-01-05-100 

GLP10-01-01-05-110 

GLP10-01-01-08O10 

Description 

DAL SWSW1 ORB 100623 

DALGW216RRB 100716 

DAL-SD-WESB4-R&O000 

DAL-SD-WESC4-RB-0000 

DAL-SS-WEU01-RB-0000 

DAL SDSD03RB 100625 

DAL SDSD08RB100625 

DAL SSSS06 RBI 00707 

DAL SSGP06RB 100709 

DAL SSGP09RB 100708 

DAL SSGP11 RBI 00708 

DAL-SS-OSS08-RB-0010 

PFBS 

Concentration 

(ng/mL) 

<0.0255 

<0.0255 

<0.0255 

<0.0255 

<0.0255 

<0.0255 

<0.0255 

<0.0255 

<0.0255 

<0.0255 

<0.0255 

<0.0255 

YoRecovery 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

PFHS 

Concentration 

(ng/mL) 

<0.103 

<0.103 

<0.103 

<0.103 

<0.103 

<0.103 

<0.103 

<0.103 

<0.103 

<0.103 

<0.103 

<0.103 

YoRecovery 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

PFOS 

Concentration 

(ng/mL) 

<0.255 

<0.255 

0.260 

<0.255 

<0.255 

<0.255 

<0.255 

<0.255 

<0.255 

<0.255 

<0.255 

<0.255 

YoRecovery 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

NA = Not Applicable 

Page 36 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

10 Conclusion 

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

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

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

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 Attachments 

Attachment A: Protocol Amendment 06 (General Project Outline) 

Attachment B: Representative Chromatograms and Calibration Curves 

Attachment C: Analytical Method 

Attachment D: Method Deviation 

Page 37 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

13 Signatures 

I^jzq-Itd/O 

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

2 f a>/s>^/o 

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

fl^H^i 

(I 

/O 

Gary Hohenstein, Sponsor Representative 

l^A^ . 

Date 

Jaisimha Kesari, Study Director I ' Date 

Page 38 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 ^^^^^^^ ^ ^^^^^^^ ^ GLP10-01.02 

Amendment 06 

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 Progrann 

PROTOCOL AMENDMENT NO. 06 

Amendment Date: 

June 16, 2010 

Performing Laboratory 

3M Environmental, Health, and Safety Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55144-1000 

Laboratory Project identification 

GLP10-01-02 

Sampling Event 

Avenue A Investigation - Surface Water and Groundwater 

Page 1 of 6 

Page 39 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 . . .. . ^ . ^ , ^^ ^ ^^ „ „ 

Analytical Protocol: GLP10-01-02 

^ Amendment 07 

This amendment modifies the following portion of protocol: 

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

Decatur Phase 3 Site-Related Monitoring Program" 

PROTOCOL READS: 

Section 9.2.1: A stable isotope-labeled surrogate [(1,2.3,4-"C4)-PFOS] will also be added at a fixed level to 

each sample, LMS, LCS, procedural blank, and at variable kncsvn concentrations in calibration standards, and 

quantified to evaluate surrc^ate recoveries. 

A steible isotope-labeled iritemal standard, [(1,2,3,4,5,6,7,8-^^C8)-PFOS] will be added at a fixed concentration to 

each sample, LMS, LCS, procedural blank and calibration standard for aiding quantitation of PFOS and the 

sunnogate. 

A stable isotope-labeled internal standard, [(^^OzH'FHS] will be added at a fixed concentration to each sample, 

LMS, LCS, procedural blank and calibration standard for aiding quantitation of PFHS. 

A stable isotope-labeled internal standard, [(^®02)-PFBS] will be added at a fixed (X)ncentratipn to each sample, 

LMS, LCS, procedural blank and calibration standard for aiding quantitation of PFBS 

AMEND TO READ: 

A stable isotope-labeled surrogate t(1,2,3,4-''^C4)-PFOS] may also be added at a fixed level to each sample, 

LMS, LCS, procedural blank, and at variable known concentrations in calibration standards, and quantified to 

evaluate surrogate recoveries. 

A stable isotope-labeled internal standard, [(1,2.3,4,5,6,7,8-"C8)-PFOS] may be added at a fixed concentration 

to each sample, LMS, LCS. procedural blank and calibration standarcl for aiding quantitation of PFOS and the 

surrogate. 

A stable isotope-labeled intemal standard, [('®02)-PFHS] may be added at a fixed concentration to eac^ 

sample, LMS, LCS, procedural blank and calibration standard for aiding quantitation of PFHS. 

A stable isotope-labeled intemal standard, [{^®02)-PFBS] may be added at a fixed concentration to each sample, 

LMS, LCS, procedural blank and calibration standard for aiding quantitation of PFBS. 

The use of intemal standards and sun-cjgate are only appropriate for those sampling locations with PFBA, 

PFHS. and PFOS concentrations in the low ppb range. Prior to each sampling event, if previously obtained 

PFBS, PFHS, and PFOS data is available for tiie sampling points of interest, the data will be reviewed to 

determine if tiie use of intemal standards and surrogate is appropriate for the cunant sampling event 

Page 2 of 9 

Page 40 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 ^^^^^.^^ ^ p^^^^^^^_. Q^^Q^^.^ ^ 

Amendment 06 

Amendment Approval 

^fd^jWPui^ 

Gary Hohenstein, sponsor Representative Date 

I •7-/2^^ ^ 

Cleston C. Lange, Principal Analytical investigator Date 

/yJ^^^-^/o 

William Reagen, EHSipjpns Environrtiehtal Lab Management 

[QMM/ 

Date 

mk 

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

Page 3 of 6 

Page 41 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/Julv2010 

Analytical Protocol: GLP10-01-02 

Amendment 06 

Environmental Health & Safety Operations, Environmental Laboratory 

General Project Outline 

To: Gary Hohenstein, 3M EHS&Opns 

From: Susan Wotf. 3M EHS&Opns; Environmental Lab 

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

Cliffton Jacoby, 3M EHS&Opns; Environmental Lab 

Jai Kesari, Weston Solutions 

Charies Young, Weston Solutions 

Tim Frinak. Weston Solutions 

Date: June 16,2010 

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 06 - Avenue A Investigation 

1 General Project Information 

Contacts 

Lab Request Number 

Six Digit Department Number 

Project SchedulefTest Dates 

3M Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

SainfPaul.MN 55144-1000 

Phone:(651)737-3570 

flahPtiepstein@mfTim.cpiH 

3M Environmental Laboratory Management 

William K. Reagen 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9739 

wi<reaaen(a>mmm.com 

Principal Analytical Investigator 

Cleston Lange 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9860 

cclanaeffimmm.com 

Sampling Coordinator 

Timothy Frinak 

Weston Solutions 

Timothv.frinakSiwestonsolutions.com 

Phone: (334)-332-9123 

GLP10-01-02^6 

Dept #530711, Project #0022674449 

Sampling scheduled for the week of June 21,2010 

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

Page 4 of 6 

Page 42 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Analytical Protocol: GLP10-01-02 

Amendment 06 

2 Background Information and Project Objective(s) 

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

groundwater samples collected from twenty-five sampling locations for Perfluorobutanesulfonate (PFBS), 

Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfdnate (PFOS) as part of the Avenue A 

Investigation. Analyses will be conducted under the GLP requirements of EPA TSCA Good Laboratory 

Practice Standards 40 CFR 792. 

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

21,2010. The 3M Environmental Laboratory will prepare the sample bottles with all required spikes to 

ensure that resulte 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-

06. 

3 Project Schedule 

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

2010. Sample botUes will be shipped in coolers overnight to 3M Decaturfor arrival on Friday, June 18,2010. 

Sample botttes 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 twenty-five sampling locations have been specified. Sampling location descriptions were not available 

at the time of sample botUe preparation. For each sampling location, a total of five sample botfles will be 

collected (sample, sample duplicate, low-level field matrix spike, mid-level field matiix spike, and high-level field 

matrix spike).The "fill to here" line on each 2K] mL Nalgene botUe will be 200 mL Three sets of trip blanks 

consisting of reagent-grade water, a low-level trip blank spike* mid-level field spike, and a high-level ti-ip blank 

spike will be prepared at tiie 3M Environmental Laboratory and serit to tiie sampling location witii the other 

botOes. The low field matiix spike will be prepared at 1 hg/mL, the mid field matiix spike at 10 ng/mL, and tiie 

high field matiix spike at 100 ng/mL. Five additional botUes will be prepared to be used for tiie preparation of 

the equipment rinseate blanks. A total of 142 sample botties will be prepared. 

Page 5 of 6 

Page 43 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

Analytical Protocol: GLP10-01-02 

Amendment 06 

Test Methods 

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

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

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

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

in tiie report and tiie final accuracy statement may be adjusted accordingly. 

Alternately, samples may be analyzed by ETS 8-154.3 "Detennination of Perfluorinated Acids, Alcohols, 

AmkJes, and Sulfonates In Water By Solid Phase Extraction and High Perfoimance Liquid 

Chromatography/Mass Spedrometiy". Metiiod ETS-8-154 has been validated for PFOA and PFOS only; 

however, specific quality control samples analyzed witii the samples will be used to detennineoverall method 

precision and accuracy. 

6 Reporting Requirement 

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

field matrix spikes. Trip blank and trip blank spikes will be reported for tiie sampling event as will any 

equipment/rinseate blanks prepared in tiie field. Laboratory conti-ol spikes of reagent water prepared at ttie time 

of sample extraction will also be reported and used to evaluate tiie overall method accuracy and precision. 

Metiiod blanks of reagent water prepared at the time of sample extinction will be used to detennine tiie method 

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

higher tiian expected analyte concenti^ations, a laboratory matrix spike rtiay be prepared and will be included in 

tiie final report. 

Page 6 of 6 

Page 44 of 67 
•Scan API4000 V1660305 

GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

s100804a.rdb (PFBS): "Quadratic" Regression ("1 / x" weighting): y = -2.22e+003 x'^2 + 5.52e+005 x + 2.94e+003 (r = 0.9999) 

3.6e7 

3.4e7 

3.2e7 

3.0e7 

2.8e7H 

2.6e7 

2.4e7-

2.2e7-

2.0e7- / 

1.8e7 

(0 

2 1.6e7 

< 

1.4e7 

1.2e7 

1.0e7 

8.0e6 

6.0e6 

4.0e6 

2.0e6 

0.0 

/ 

O 

/ 

/ 

10 15 20 25 30 35 40 45 50 55 60 

Concentration, ng/mL 

65 70 75 80 85 90 95 100 

*Data work-up performed by STW 

Page 1 of 1 

Printing Time: 1:16:02 PM 

Printing Date: Friday, October 22, 2010 

Page 45 of 67 
»Stan API4000 V1660305 

GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

• s100804a.rdb (PFHS): "Quadratic" Regression ("1 / x" weighting): y = -1.49e+003 x'^2 + 3.98e+005 x + 2.74e+004 (r = 0.9998) 

2.6e7-

2.5e7-

2.4e7-

2.3e7-

2.2e7-

2.1e7-

2.0e7-

1.9e7-

1.8e7-

1.7e7 

1.6e7-

1.5e7-

« 1.4e7 -

8 •'•3e7-

S 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-

^^'"" " 

^^" " 

^ 

^" ^ 

/-^ ' 

^ y ^ 

y ' 

y i 

y ^ 

• / 

/ 

/ 

/ 

p' 

/ 

__.J»-

^ - '" 

0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 

Concentration, ng/mL 

*Data work-up performed by STW 

Page 1 of 1 

Printing Time: 1:16:22 PM 

Printing Date: Friday, October 22, 2010 

Page 46 of 67 
•Stan flPI4000 V1660305 

GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

s100804a PFOS linear.rdb (pfos): "Quadratic" Regression ("1 / x" weighting): y = -479 x*2 + 1.63e+005 x + -1.06e+004 (r = 0.9997) 

20 25 30 35 40 45 50 55 60 

Concentration, ng/mL 

65 70 75 80 85 90 95 100 

•Data work-up performed by STW 

Page 1 of 1 

Printing Time: 1:18:38 PM 

Printing Date: Friday, October 22, 2010 

Page 47 of 67 
***Stan API4000 V1660305 

GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

I

Sample Narrw: ••100804a026" Sampl« ID: "08 00&-147-09- Fito: "«1008(Ma.wir 

Peak Name: "PFBS" Uass(es): -298.9/79.8 amu.298.9/99.0 amu' 

Comment: -2.5 ppb curve point in Milli 0 Water' Annotation: 

Sample Index : 25 

nrj/isL 

Sample Type: 

Concentrati o 

Calculate d C 

acq . r^te : 

Acq. Tiino: 

McdiEied i 

RT Windo«: 

Experta d RT: 

Use ftdUtiv« RT 

Standard 

2-5.S 

2.53 

e/J/2010 

e:l«:3 J 

Yes 

3P.0 

IP. l 

NL-. 

I

Sampla Name: -a10O8O4a043" Sample ID: "LCS-100726-6" File: "•100804a.wir 

Peak Name: -PFBS- Maw(e«): "298.9/79.8 

Comment "Sppb LCS' Annotation: *" 

ample Index : 43 

ample Typa: OC 

'jncBnttation : 5. 10 n-j/mL 

Calc u 

«cq . 

ncq . 

Modi 

RT Ki 

Exp«r 

l a 

Pa 

Ti 

i e 

nd 

c« 

H-iqht : 

Star t Ti. 

End Tim« 

*Data work-up performed by STW 

Page 1 of 4 

Printing Time: 

Printing Date: 

1:15:16 PM 

Friday, Oct ober 22, 2010 

Page 48 of 67 
^**Stan API4000 V1660305 

GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS. and PFOS in Water Samples from Decatur, AL 

June/July 2010 

I SarrvleNama;-s100804a06r Sample ID:'Solvent blanlT 

I Peak Name: 'PFBS ' Ma»(e9)i *298.9/79.8 amu,: 

I Comment"MiIIiQWilBrTNlCW27r Annotafion: 

Sampl e InJez : 61 

San,pU Type : UriKnovn 

Ccnc«nirdtion : N/A 

Calculate d Cone : 0.0011 1 ng/mL 

Acq. m« : e/5/201C 

Acq. Time : f: J3:3 6 AM 

Hin . Pea t wi d 

Jno.!thin g Wid 

RT Window: 

Exparta d RT: 

I

Sample Name: "s100804a07r Sampte ID: "GLP10-01-01-06-021" File: 's i 00804a.wifT 

Peak Name: "PFBS" Ma««(ea): "298.9/79.8 a mu ,298.9/99.0 amu' 

Comment "DAL SWSV«3 0 100622 (1;10 DU.)" 

• Type: 

Calci 

H/A 

9.5 1 q/fuL 

Acq. rate : 8/5/201 0 

Acq. Tim*;: 2:Z4:< J 

Modified : re s 

RT Window: 30. 0 

Experts d RT: 10. 1 

USB Relativ e BT: Ni; 

Int . Type : Manual 

Retentio n Time : 10. 1 

Area : 5257J 5 c 

9.?iqht : •).07^-00 4 

Star t Tine : 9.57 1 

End Timft: 10.30 0 

^ PM 

s e c 

min 

c p s 

min 

B.8e4 

S.6e4 

e.4e4 

S.2e4' 

8.0e4 

7.8*4 

7.6e4. 

7.4*4 • 

7.2*4 

7.0e4 

6.8*4 

*Data work-up performed by STW 

Page 2 of 4 

Printing Time: 1:15:16 PM 

Printing Date: Friday, October 22, 2010 

Page 49 of 67 
*^**Stan API4000 V1660305 

GLP10-01-02; Interim Report 06 

Analysis of PFBS. PFHS, and PFOS in Water Samples from Decatur. AL 

June/July 2010 

• Samph Name: ''s10D804a026' Sample ID: 'C 

I Peak Name:'PFHS" Mass(es):'399.0/79.8 an; 

I Comment "2.5 ppb curve point in Mill O Water" 

Sample Index : 25 

Sample Type: Standard 

Concentration : i.LS n-j/mL 

Calculate d Cone: 2.53 ntj/mL 

008-147-09- Rta: •«1008O4a.wir 

I.399.W99.0 amu' 

Annotation:"" 

Acq. rate : 

Acq. Time: 

Modified: 

PrDC. Algori 

Noise Parrel 

Base. Sub. K 

Psak-Split. 

Report Large 

Min. Peak He 

Min. Peak wi 

aracwthing Wi 

BT Window: 

Expected RT: 

Use Rdlativa 

Int. Type: 

Retention Ti 

Area: 

Height: 

Start Time: 

End Tirao: 

:hm: 

:a'je: 

Tacto 

St Pe 

ight: 

dth: 

dth: 

RT: 

9/1/2010 

e;l?:3J PM 

Yes 

:ntBlliOua 

95 

l.OC 

r: i 

ak; No 

0.00 

0.00 

3C.0 

12.7 

No 

Base To Ba 

12.7 

1025721 ecu 

i .OJe-OCS 

12.590 

12.92'! 

2.0eS 

2.0*5 

1.9e5 

1.9eS 

1.8*5 

^ 1.8*5. 

1.7*5 

1.7*5 

1.6*5 

1.6*5 

1.5*5 

1.5*5 

1.4*5 

1.4*5 

1.3*5 

1.3*5 

1JZe5 

1.2*5 

1.1*5 

I 1.1*5 

" 1.0*5 I 

9.5e4 

9.0e4 

8.5e4 

8.0e4 

7.5*4-

7.0e4-

6.Se4-

6.0e4-

S.Se4-

S.0e4-

4.5e4-

4.0e4-

3.5*4-

3.0*4; 

2.5*4-

2.0*4: 

1.5*4-

1.0*4-

5000.0: 

0.0; 

I

Sample Name:'s100804a043' Sample ID:-LCS-10072e-«-

Peak Name: "PFHS" Mas«(es): "399.0/79.8 smu.399.a99.0 

Comment '5ppb LCS" Annotation: — 

Sample Index : 43 

s 

c 

c 

A 

A 

M 

P 

N. 

B 

mpl e Type : QC 

ML-KntratioTi: 5,1 5 n'j 

iculata d Cone : 5.5 4 nq 

q . Pate : 8/5/20l a 

q . Time : 2:20:0 7 AH 

dified : Yes 

o c . Al()orithn, : IntelliQua n -

i s e P-.rcentag« : 55 

3 8 . Jub . Window: 1.00 m 

ml. 

rt.L 

HQ 

Expec-tttd BT: 

Use Relativ e 

Int . Type : 

Retentio n Ti 

Area : 

H-.igl.t: 

Star t Tir,e : 

End Time : 

12. 7 

RT: No 

Bas e To 

, e : 12. 7 

2:'00800 c 

4.6ee*00 S 

12.56 0 

12.93 9 

•^Data work-up performed by STW 

Page 3 of 4 

Pri 

Pri 

nting Time: 1:15:16 PM 

nting Date: Friday, October 22, 2010 

Page 50 of 67 
^*Stan API4000 V1660305 

GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

• Sarr^ile Name: "s100804a061* Saniple ID: "Solvent blank" File: "si00804a.wiiir 

I Peak Name: "PFHS" Mass(es}: "399.0/79.8 armi,399.0/99.0 amu" 

I Comment "Milli Q Water TNI 0-0272" Annotation: ~ 

,n,ple Type; Unki 

Calculate d Cone: 

Acq. Pate; 6/ 

Acq. Time: 

Modi tied : 

Proc. Alcforithm : I n 

Nuise Pecceiitage: 

Base. Sub. Window: 

P-ak-Split . Factor: 

Report Larges t Peak 

Min . Peak Heit|lit : 

Min . Peak Width : 

3m<...;thing Width : 

RT Hindo-rf: 

Exp«ctad RT: 

Uie Relativ e RT: 

Int . Type: 7 

Retentio n Time: 

Area : 105 

Height : 2.0 

V 0 

/2010 

3:36 AH 

No 

elUQu a 

;,o 

1.00 

4 

No 

0.0 0 

0.00 

0.0 

12-7 

No 

alle y 

12.7 

5e-00:< 

4800 

4700 

4600 

4500 

4400 

4300 

4200 

4100 

4000 

3900 

3600 

3700-

3600 

3500 

3400 

3300 

3200 

3100 

3000 

2900 

2500-

2400 

2300 

2200 

2100 

2000 

1900 

1600 

1701-

1600 

1500-

1400 

1300 

1200 

1100-

•* "-V-' ^ 

I

Sample Name: "«100804a077" Sample ID; •GLPl{W)1-01-0&02r File: "s 100804a.(MtT 

Peak Name: "PFHS" Mass(es): -399,0/79.8 amu,399.ora9.0 amu" 

Comment 'DAL SWSWD30 100622 (1:10 Oil.)" Annotation: 

Percentage: 

:plit . Facto 

Larges t Pe 

'eak Height : 

'eak Width : 

ling Width : 

• e d RT: 

elliQua i 

SO 

1,00 

*Data work-up performed by STW 

Page 4 of 4 

Printing Time: 1:15:16 PM 

Printing Date: Friday, October 22, 2010 

Page 51 of 67 
"**Stan API4000 V1660305 

GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur. AL 

June/July 2010 

r

SaiTvih Name: -s10D804a02r Sample ID: 

Peak Name: 'pfos* Mass(es); "498.9/99.2 

Comment: "2.5 ppb curve point in MiRi Q Water" Annotation: 

Sample InJey.: 26 

Sample Typa: .standard 

008-147-09" Fita: "sl00804a.»rir 

,438.9/130.0 amu,498.9/80.0 amu" 

Calculate d Cone: 

Acq. Pate : 

Acq. Time: 

Mcditied : 

RT Window: 

Expected RT: 

Use Relativ e 

Int . Type: 

Retentio n T i 

Area : 

Height : 

Star t Time: 

End Time: 

RT: 

e: 

2.5? 

2.39 

B/J/2010 

Yes 

30.0 

lA. b 

Manual 

14.3 

7&ai2 c 

e.OTatOOJ 

iJ.19 8 

1J.501 

ng/raL 

PH 

sec 

mm 

min 

ffiin 

8.0*4 

7.8e4 

7.6M 

7.4e4 

7.2e4 

7.0e4 

6.e<»4 

6,2e4 

6.0e4 

5.8e4 

5.6e4 

5.4e4 

5.2*4 

5.0e4 

4.8e4 

4.6M 

4.4e4 

. 4.2*4 

4.0*4 

3.8*4 

3.6*4 

3.4*4 

3.2*4 

3.0*4 

2.8*4 

Z6* 4 

2.4*4-

2.2*4-

2.0*4 

1.6*4 

1.6*4-

1.4*4-

1.2*4-

1.0*4-

8000.0-

6000.0-

4000.0-

3000.0-

0.0-

:yU:is 

C'jncontration : 

Calcutata d Cone 

Acq. rate : 

Acq. Time: 

Modified : 

RT Window: 

ExpoctHd RT: 

Uss Relativ e 

Inc . Type: 

Retentio n T i 

Area : 

Height : 

BT 

e, 

5 

5 

e/5 / 

2:20 

30 

1 

1 

22343 

l.SSe 

e l ng/n,L 

010 

07 AH 

.5 

a l 

.: 

005 

:" 

cps 

(

Sample Nam*: "8100804*043" Sample ID: tCS- l 00726-6* File: "si 00804a. wifT 

Peak Name: 'pfos" Ma««(*»): '498.9«9.2 amu,498.9n 30.0 am 

Comment" ^p b LC S' Annotation:"" 

1.9*5 

1.9*5 

1.8*5 

1.8e5 

1.7*5 

1.7*5 

1.6*5 

1.6*5 

1.5*5 

1.5*5 

1.4*5 

1.4*5 

1.3*5 

1.3*5-

1.2*5 

1.2*5 

1.1*5 

1.1*5-

1.0*5 

9.5*4 

9.0*4 

8.5*4 

8.0*4 

7.5*4 

7.0*4 

6.5*4 

6.0*4 

5.5*4 

5.0*4 

4.5*4 

4.0*4-

3.Se4 

3-0*4 

2.5*4 

Z0e4-

1.5*4 

1.0*4 

5000.0 

0.0 

*Data work-up performed by STW 

Page 1 of 3 

Printing Time: 1:18:15 PM 

Printing Date: Friday, October 22, 2010 

Page 52 of 67 
"Stan API4000 V1660305 

GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

• Sampta Nanne: •»100804a055' Sample ID: 'LCS-100726-15" Fil*: -«100804a.iMr 

I P«ak Name: "pfos' Ma$s<»s): "498.9/99.2 amu.498.9/130.0 amu,498.9/80.0 amt/ 

• Comment "5ppb LCS ECF" Annotation: " 

Sample Indez ; bt 

Sample Type: QC 

Concentratiuri: 5.00 nrj/ial 

Calculated Cone: J.15 ng/mL 

Acq. P^te: e/S/2010 1.3e5 

Acq. Time: 

Modified: 

RT Win-do-,j: 

Expected R-

;:35:44 AM 

RT: 

Int . Type: Manual 

Retentio n Time; 14.3 min 

Area : 659917 count s 

Height : 1.35e+005 cps 

End Til 

IJ.19S 

11.532 

c 6.5*4 

Sample Nam*: "s100e04a061" SamF^a ID: ~Solv*nt btank" Fit*: "•100804a.>Mr 

P*ak Name: "pfos' Mass(«s]: '498.9/99.2 annu,498.9/130.0 amu.498.9/80.0 amu' 

Comment 'Milli Q Water TN10^)272" Annotation: 

Sample lnde.\: 61 

Sample TiTe : Unknown 

Onc^ntcation : N/A 

Calculate d Cone: 0.076 

Acq. Pate: 5/b/2Q 

Acq. Tipe : 1:43:3 ' 

Hoditied : Yes 

RT Window: 30.0 

Expected RT: 14. : 

U3« Relativ e RT: tfi. 

3.38e*0P2 cps 

*Data work-up performed by STW 

Page 2 of 3 

inting Time: 1:18:15 PM 

inting Date: Friday, October 22, 2010 

Page 53 of 67 
•Stan API4000 V1660305 

GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS. and PFOS in Water Samples from Decatur, AL 

June/July 2010 

I

San^te Name: •s1O08O4a07r Sample ID: "GLP1(M1-01-06-021" File:*»100804a,wifr 

Peak Nam*: 'pfos' Mass(es): '498.9/99.2 amu,49e.9/130.0 amu,4S8.9A0.0 amuCorrmont "DAL SWSVW3 0 100622 (1:10 Dl f Annotation: -

Sample Tvpe: 

Calculate d C 

Acq. Pate ; 

A^q. Time : 

Modified : 

RT Window: 

Exp«rte d RT: 

Use Relativ e 

Int . Type ; 

Retentio n Ti 

Area : 

Height : 

Star t Time : 

End Time : 

>nc 

RT 

.., 

1 

101 . ng/mL 

6/5/201 0 

2:2J:< 4 PM 

Yes 

30. 0 sa c 

14. 5 min 

Manual 

H . 3 min 

523J 3 counts 

3.2?e'O0 5 cp s 

IJ.ie S (Sin 

1J.50 7 min 

3.2*5 

3.1*5 

3.0*5 

2.9*5-

2.8*5 

*Data work-up performed by STW 

Page 3 of 3 

Printin g Time: 1:18:15 PM 

Printing Date: Friday, October 22, 2010 

Page 54 of 67 
***Sta n API4000 V1660305 

GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

I

SampI* Name: -«100804a055" Sample ID: "LCS-100726-15" Fife: "s100e04a.wir 

Peak Name: 'pfos' Mass(es): '498.9/99.2 amu.498.9/130.0 amu.498.9/80.0 amu" 

Comment "5ppb LCS ECF" Annotation: "" 

Sample IndeK: 55 

San.plfl Type: C^~ 

Calculate d Cone ; 2.2 3 ng/mL 

Acq . P»ca : 8/5/201 0 

Acq. Til 4 1 AM 

Modified : 

RT Window: 

Exp«rte d RT: 

Use Rslativt , 

Int . Type : 

Retentio n Ti 

Heigfit : 

Star t Tine : 

End Time : 

RT: 

n e : 

y 

30 

1 

K 

M.in 

I 

.iO e 

1 3 -

I J . 

1.3*5 

1.3*5 

1.2*5 

1.2*5 

1.1*5 

1.1*5 

1.0*5 

9.5*4 

9.0*4 

6.5*4 

8.0*4 

7.5*4 

7.0e4 

6.5*4 

6.0*4 

5.5*4 

5.0*4 

4.5*4 

4.0e4 

3.5*4 

3.0*4 

Z5*4 

2.0*4 

1.5*4 

1.0*4 

5000.0 

14 

14.07.. 

30 

I

SampI* Nam*: "sl00e04aa77- SampI* ID: "GLP1&O1-01-06-021- Fil0:'s1OO8O4a.wifr 

Peak Nanv: "pfos" Mass(es): "498.9/99.2 amu,438.9/130.0 amu,498.9/80.0 

Commant "DAL SWSVW3 0 100622 {1:10 DB.)" Annotation: 

SanipL 

Sample Type Unhnow; 

N/A 

^cq . rsta : 

Acq. Tiwe : 

ModiEiert: 

RT Window: 

ExpertHri RT: 

9/5/2010 

2:2<:44 PH 

YPS 

30.0 

1^.5 

H-iqht : 

Star t 1 

^nd Tir 

*Data work-up performed by STW 

Page 1 of 1 

Printing Time: 1:21:51 PM 

Printing Date: Friday, October 22, 2010 

Page 55 of 67 
DocQm'Brtiro3ai|it&& iMj56«!Q6f current, for 14 days from 10/25/2010 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

3M Eiffidronmenfal laixNBlory 

Method 

Method of Analysis for the Determination of Perfluorinated Compounds in Water 

by LC/MS/MS; Direct Injection Analysis 

Method Number: ETS-8-044.0 

Adoption Date: Upon Signing 

Effective Date: Q U I n [ o "1 

Approved By: 

^ ^//^/ o • > 

William K. Reagen, Laboratory Manager Date 

ETS-8-044.0 Paget of 11 

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

Injection Analysis Page 56 of 67 
DocQ(:Ra=iiitrai|it<'m8:i s«lsBft]oef current, for 14 days from 10/25/2010 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

1 Scope and Application 

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

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

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

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

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

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

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

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

Perfonnance Liquid Chromatography/Mass Spectrometry". 

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

defined QC elements are satisfied. 

Sample collection is not covered under this analytical procedure. 

2 IVIethod Summar y 

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

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

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

This is a perfonnance-based method. Method accuracy is determined 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 detennine the statement of 

accuracy for analytical results. 

3 Definitions 

3.1 Calibration Standard 

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

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

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

concentration. 

3.2 Laboratory Duplicate Sample (LDS, or Lab Dup) 

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

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

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

preservation, or storage procedures. 

3.3 Field Blank (FB)/Trip Blank 

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

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

preservation and all analytical procedures. The purpose of the FB is to detennine if test substances or 

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

ETS-8-044.0 Page 2 of 11 

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

Injection Analysis 

Page 57 of 67 
DocGmf!*rtifei^ijitteiK€patsloef current, for 14 days from 10/25/2010 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 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 detennine 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 detemnine whether the sample 

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

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

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

3.9 Laboratory Sample 

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

3.10 Limit of Quantitation (LOQ) 

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

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

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

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

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

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

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

ETS-8-044.0 Page 3 of 11 

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

Injection Analysis 

Page 58 of 67 
Docamsgpliwtawtfe sc-aftloif current, for 14 days from 10/25/2010 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 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 detennine if test substances or other interferences are present in the laboratory 

environment, the reagents, or the apparatus. 

3.12 Sample 

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

material. 

3.13 Stock Standard Solution (SSS) 

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

compound. 

3.14 Surrogate 

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

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

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

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

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

quality control measure and is NOT required. 

3.15 Working Standard (WS) 

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

calibration standards and other required analyte solutions. 

4 Warnings and Cautions 

4.1 Health and Safety 

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

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

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

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

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

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

4.2 Cautions 

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

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

appropriate equipment procedure or operator manual for additional infomnation 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 interf'erences under 

conditions of analysis by running method blanks. 

ETS-8-044.0 Page 4 of 11 

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

Injection Analysis 

Page 59 of 67 
DocGica«SRlif0»|itfee«|3seloef current, for 14 days from 10/26/2010 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 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 perfomiance liquid chromatograph capable of pumping up to two solvents and equipped with a 

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

(LC/MS/MS). I 

Analytical balance capable of reading to 0.0001 g 

A device to collect raw data for peak integration and quantitation 

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

Gas tight syringes, 25pL, 50pL, lOOpL, 250pL, 500pL, lOOOpL. 

1 mL plastic HPLC autovial. 

Disposable pipettes, polypropylene or glass as appropriate 

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

6.2 Chromatographic System 

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

Analytical Column: Betasil 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. 

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

provided that data quality objectives are met. 

ETS-8-044.0 Page 5 of 11 

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

Injection Analysis 

Page 60 of 67 
DocQmsKli«eai|itlf» gipsaloef current, for 14 days from 10/25/2010 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

6.3 MS/MS System 

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

Analyte 

PFBA 

PFPeA 

PFHA 

PFHpA 

PFOA 

PFNA 

PFDA 

PFUnA 

PFDoA 

PFBS 

PFHS 

PFOS 

Transition Monitored 

213^169 

263-^219 

313 ^269 and 313-> 119 

363 ^ 319, 363 ^ 169 and 363 ^ 119 

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

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

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

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

613 ^ 569, 613 -» 169 and 613 -> 319 

299 -^ 80 and 299 -» 99 

399 -^ 80 and 399 -^ 99 

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

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

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

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

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

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

7 Reagents and Standards 

7.1 Chemicals 

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

Methanol - HPLC grade 

Ammonium Acetate -A.C.S. Reagent Grade 

7.2 Standards 

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

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

Perfluorohexanoic Acid (PFHA-C6 acid); Oakwood Products, Inc 

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

Products, Inc 

Perfluorooctanoic Acid (PFOA - C8 acid); 3M 

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

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

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

Perfluorododecanoic Acid (PFDoA-C12 acid); Oakwood Products, Inc 

Perfluorobutanesulfonate (PFBS - C4 sulfonate); 3M 

Perfluorohexanesulfonate (PFHS - C6 sulfonate); 3M 

Perfluorooctanesulfonate (PFOS - C8 sulfonate); 3M 

ETS-8-044.0 Page 6 of 11 

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

Analysis 

Page 61 of 67 
DocGtcRCOFdiKraatfitte H6i»i»]o6f current, for 14 days from 10/25/2010 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

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

used. 

7.3 Reagent Preparation 

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

water. 

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

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

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

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

when diluting stock solutions to appropriate levels. 

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

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

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

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

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

,^ ^- z X molecular weight of anion 

salt correction factor = = 

moclecular weight of salt 

499 PFOS (K^^ )salt correction factor = ^3fi = 0.9275 

538 

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

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

flask and bring up to volume with solvent. 

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

volumetric flask and bring up to volume with solvent. 

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

flask and bring up to volume with solvent. 

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

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

ETS-8-044.0 Page 7 of 11 

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

Analysis 

Page 62 of 67 
Doc'3OT<JXKlittBaijiteteigiia«!G«.f'tioef current, for 14 days from 10/26/2010 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 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 wori<ing standards may 

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

than those listed below can be prepared as needed. 

Concentration 

of WS, ng/mL 

125 

125 

125 

125 

250 

250 

250 

250 

5000 

5000 

5000 

Volume of WS.fd. 

10 

15 

20 

30 

20 

50 

100 

200 

25 

50 

100 

Final Volume of 

Calibration Standard (mi 

of ASTM Type 1 Water, or 

other suitable water) 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

Final Concentration of 

Calibration Standard, ng/mL 

(ppb) in ASTM Type 1 Water, 

or other suitable water 

0.025 

0.0375 

0.050 

0.075 

0.100 

0.250 

0.500 

1,00 

2.50 

5.00 

10.0 

8 Sample Handling 

8.1 Water Sample Preparation 

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

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

sample aliquot, or filtered. 

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

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

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

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

Prepare at least five method blanks. 

9 Sample Analysis - LC/MS/MS 

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

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

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

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

thoroughly documented in the raw data. 

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

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

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

The coefficient of 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 

Page 63 of 67 
DocQmffi^iiiK^i|it&ft g^^olpef current, for 14 days from 10/25/2010 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 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 constmct the calibration curve. 

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

curve (if necessary) and reanalyze. 

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

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

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

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

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

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

curve should be further diluted and reanalyzed. 

10 Quality Control 

10.1 Data Quality Objectives 

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

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

the raw data and footnoted in the final report. 

10.2 Method Blanks 

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

Method blanks may be injected multiple times, but no more than 3 injections should be removed 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 alternatively, the method blanks must be evaluated 

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

10.3 Sample Replicates 

Samples duplicates are collected in the field. The 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 

Sunnogate 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 Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection 

Analysis 

Page 64 of 67 
DocQicR®?di-Rffiaijit&8i8ffp«.i5i0ef current, for 14 days from 10/26/2010 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 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 , ^ r J / , , V (Peak Area - Intercept) ^..^ 

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

Slope 

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

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

percent recovery. 

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

Analyte added (ng/mL) 

12 Method Performance 

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

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

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

samples reanalyzed, or other actions taken as appropriate. Document all actions in ttie 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 <5% and a retention time RSD of S2% to be compliant. 

12.2 Quantitation 

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

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

the LLOQ, which may be within ±30%. 

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

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

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

bracketed by CCVs not meeting these criteria must be reanalyzed. 

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 

Page 65 of 67 
DocQi:R'aRtiwi«Mte!i» ia«^Mloef current, for 14 days from 10/25/2010 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

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

standard) and the mass spectral response of unique ions. 

12.3 Sensitivity 

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

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

to Section 10 for additional details. 

12.4 Accurac y 

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

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

spikes and laboratory matrix spikes. 

12.5 Precision 

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

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

requirement for replicates excludes field blanks or rinse blanks. 

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

13 Pollution Prevention and Waste Management 

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

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

14 Records 

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

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

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

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

15 Affected Documents 

None. 

16 Revisions 

Revision 

Number 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 66 of 67 
GLP10-01-02; Interim Report 06 

Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

June/July 2010 

/. Identification 

Study / Project No. 

GLP10-01-02-06 

Deviation type 

(Ctiecl< one) 

a 

D 

Date(s) of Occurrence: 

s100804aand miq0910a _ 

SOP D Equipment Procedure 

Protocol 0 GPO 

Document Number: 

ETS-8-044.0 

0 

D 

Method 

Other: 

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

Method Requirements: 

T. LCS average recovery of 100% ±20%/ 

2. Sample/Sample Duplicate RPD s20%. 

3. LMS/FMS recovery of 100% ± 30%. 

Actual procedure/process: 

(1) LCS average recovery for linear and branched PFOS was >120% (s100804a). LCS average recovery 

for the low set of LCS for PFHS, and the low and high set of linear and branched PFOS was outside 

acceptance criteria (mIOOQIOa). 

(2) The RPD for PFOS for sampling location GP04 was 30%, GP09 PFOS RPD was 33%, GP10 PFOS 

RPD was 31%, GP12 RPD for PFBS, PFHS, and PFOS was >50%. 

(3) The recovery of the high FMS sample for SW12 for PFOS was 63.5%. The recovery of the high FMS 

sample for GP02 for PFOS was 68.7%. The recovery of the high FMS sample for GP04 for PFOS was 

141%. 

///, Actions Taken 

(sue!) as amendment issued, SOP revision, etc.) 

Corrective Action (D Yes 0 No) Reference: 

Acceptability of the nonconforming work: 

1) The linear + branched PFOS LCS when quantitated against a calibration curve prepared from linear 

PFOS have been quantitating around 15-30% higher. By quantitating the linear and branched isomers 

of PFOS separately, against a linear PFOS curve, and summing the resulting concentrations, appears to 

help reduce the recovery of the linear + branched PFOS high LCS at 30ppb 8%. A slight increase was 

seen in the recovery of the low and mid linear + branched PFOS LCS, and an 18% decrease in the 

recovery of low set of linear PFOS LCS. The method analytical uncertainty was assigned based on the 

average recovery of the high set of linear + branched PFOS LCS (141%), since the sample on-column 

concentrations most closely matched the 30 ppb LCS. LCS average recoveries outside method 

acceptance criteria will be footnoted in the final report. 

2) The RPD value for sampling locations with RPD values >20% will be footnoted in the data tables. 

3) Since the method analytical uncertainty for PFOS is 100% ± 41%, no adjustment was made to the 

analytical uncertainty for PFOS on SW12, GP02, and GP04. 

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

0 Other: Deviations will be noted in final report 

Project Lead/PAI Approval: S/Jsan Wolf 

Study Director (if GLP) 

Sponsor Approval (for GL^ protocol deviations): NA 

Technical Reviewer (optional): NA 

Laboratory Department Manager Approval: 

/^/a</ / 

Date: NA 

Date: 

IV. Authorization to Resume Work 

Where iialting of worl< occurred, resumption of worl< must first be approved by Laboratory Management 

Laboratory Department Manager Approval: NA Date: NA 

Deviation No. 

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

Page 67 of 67