GLP10-01-02; Interim Report 07 

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

June/July 2010 

GLP10-01-02: Interim Report 07 - Analysis of PFBS. PFHS. and PFOS in Ground Water 

Samples Collected at the Former Sludge Incorporation Area (FSIA) located 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 

GLP10-01-02-07 

Total Number of Pages 

68 

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

^ y ^ ^T ^ Competence of Testing and Calibration Laboratories", In accordance with the A2LA Certificate #2052.01. 

lACC'^^l^l^i^Pi Testing that complies with this Intematlonal Standard also operate In accordance with ISO 9001:2000. 

Certificate #2052.01 

Page 1 of 68 
GLP10-01-02; Interim Report 07 

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 36 

Page 2 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

GLP COMPLIANCE STATEMENT 

Report Title: Interim Report 07 Analysis of PFBS, PFHS, and PFOS in Ground Water Samples 

Collected at the Former Sludge Incorporation Area (FSIA) at 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 detennined under GLPs. 

/i6 

Gary Hol/enalein, Sponsor Representative Date 

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

Page 3 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

QUALITY ASSURANCE STATEMENT 

Report Title: Interim Report 07 Analysis of PFBS, PFHS, and PFOS in Ground Water Samples 

Collected at the Fonner Sludge Incorporation Area (FSIA) at 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 

10/1,10/4, and 10/5/10 

Phase 

Interim Report 07 

Data and Report 

Date Reported to 

Testing Facility 

Management 

10/11/10 

Study Director 

10/11/10 

h /o-;i'^'^ 6 

QAU RepresCTitative Date 

Page 4 of 68 
GLP10-01-02; Interim Report 07 

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 Infonnation 8 

2 Summary 9 

3 Introduction 11 

4 Test & Control Substances 11 

5 Reference Substances 12 

6 Test System 13 

7 Method Summary 13 

7.1 Methods 13 

7.2 Sample Collection 13 

7.3 Sample Preparation 13 

7.4 Analysis 13 

8 Analytical Results 14 

8.1 Calibration 14 

8.2 System Suitability 15 

8.3 Limit of Quantitation (LOQ) 15 

8.4 Continuing Calibration 15 

8.5 Blanks 15 

8.6 Lab Control Spikes (LCSs) 16 

8.7 Analytical Method Uncertainty 18 

8.9 Field Matrix Spikes (FMS) 19 

9 Data Summary and Discussion 19 

Page 5 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

10 Conclusion 35 

11 Data/Sample Retention 35 

12 /attachments 35 

13 Signatures 36 

LIST OF TABLES 

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

Table 2. Sample Description Key Code 13 

Table 3. Instalment Parameters 14 

Table4. Liquid Chromatography Conditions 14 

Table 5. Mass Transitions 14 

Tables. Limit of Quantitation (LOQ) 15 

Table 7. Laboratory Control Spike Recovery 17 

Tables. Analytical Uncertainty 19 

Table 9. Field Matrix Spike Levels 19 

Table 10. DAL 130R 02 Y10 SF 21 

Table 11. DAL130LQ2 Y10SF 22 

Table 12. DAL 130S 02 Y10 SF 23 

Table 13. DAL 131R 02 Y10 SF 23 

Table 14. DAL 131L 02 Y10 SF 24 

Table 15. DAL 131S 02 Y10 SF 24 

Table 16. DAL 132R 02 Y10 SF 25 

Table 17. DAL 132L 02 Y10 SF 25 

Table 18. DAL 132S 02 Y10 SF 26 

Table 19. DAL 133R 02 Y10 SF 26 

Table 20. DAL 133L 02 Y10 SF 27 

Table 21. DAL133SQ2 Y10SF 27 

Page 6 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 22. DAL 134R 02 Y10 SF 28 

Table 23. DAL 134L 02 Y10 SF 28 

Table 24. DAL 134S 02 Y10 SF 29 

Table 25. DAL 135R 02 Y10 SF 29 

Table 26. DAL 135L02 Y10SF 30 

Table 27. DAL 135S Q2 Y10 SF 30 

Table 28. DAL 136L 02 Y10 SF 31 

Table 29. DAL 136S 02 Y10 SF 31 

Table 30. DAL 137L Q2 Y10 SF 32 

Table 30. DAL 137S 02 Y10 SF 32 

Table 32. DAL 138SQ2 Y10SF 33 

Table 33. DAL138LQ2 Y10SF 33 

Table 34. Trip Blank 34 

Table 35. Rinseate Blanks 34 

Page 7 of 68 
GLP10-01-02; Interim Report 07 

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 Operafions 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

Study Director 

Jaisimha Kesari, P.E., DEE 

Weston Solutions, Inc. 

Westchester, PA 19380 

Phone:(610)701-3761 

Fax:(610)701-7401 

j.kesari@westonsolutions.com 

Study Location 

Testing Facility 

3M EHS Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55106 

Study Personnel 

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

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

Susan Wolf, 3M Analyst 

Jonathan Steege; analyst 

Study Dates 

Study Initiation: March 8, 2010 

Interim 07 Experimental Tennination: September 17, 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 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

2 Summar y 

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

Sludge Incorporation Area (FSIA) in Decatur, AL, representing twenty-four different sampling locations. 

A total of one hundred twenty-four sample bottles were received at the 3M Environmental Laboratory 

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

(PFBS), and included duplicate groundwater samples from each sampling location. 

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

containing Milli-QTM 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 ground water samples, trip blank and two equipment rinseate blanks were 

collected on June 30, July 1 and July 2,2010, and received from Weston personnel on July 6,2010. 

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

Environmental Laboratory Method ETS-8-044.0 and conducted under 3M project GLP-10-01-02-07. 

Many of the ground water samples required dilution to attain PFBS, PFHS, and/or POFS 

concentrations within the range of the curve, in some instances up to 100-fold dilution were required. 

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

equipment rinseates and the trip blank were below the lower limit of quantitation (LLOQ), indicating 

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

concentration results for all ground waters ranged over three orders of magnitude from 0.0463 ng/mL to 

75.1 ng/mL. The PFHS concentration results for all ground waters ranged over three orders of 

magnitude from <0.103 ng/mL to 754 ng/mL. The PFOS concentration results for all ground waters 

ranged over four orders of magnitude from 0.427 ng/mL to 1720 ng/mL. 

Page 9 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 1. Summarized PFBS, PFHS, and PFOS Results (FSIA Groundwater, June/July 2010). 

Sampling Location 

DAL 130RQ2Y10SF 100701 

DAL 130LQ2Y10SF 100701 

DAL 130SQ2Y10SF 100701 

DAL 131RQ2Y10SF 100701 

DAL 131LQ2Y10SF 100630 

DAL 131SQ2Y10SF 100630 

DAL 132RQ2Y10SF 100701 

DAL 132LQ2Y10SF 100701 

DAL 132SQ2Y10SF 100701 

DAL 133RQ2Y10SF 100701 

DAL 133LQ2Y10SF 100702 

DAL 133SQ2Y10SF 100701 

DAL 134RQ2Y10SF 100702 

DAL 134LQ2Y10SF 100702 

DAL 134SQ2Y10SF 100702 

DAL 135RQ2Y10SF 100702 

DAL 135LQ2Y10SF 100702 

DAL 135SQ2Y10SF 100702 

DAL 136LQ2Y10SF 100630 

DAL 136SQ2Y10SF 100630 

DAL 137LQ2Y10SF 100701 

DAL 137SQ2Y10SF 100701 

DAL 138SQ2Y10SF 100630 

DAL 138LQ2Y10SF 100630 

Trip Blank (Milli-QTM Water) 

Equipment Rinseate Blanks, 137L and 131R 

PFBS 

Avg. Cone. 

(ng/mL) ± RPD 

16.6 ±1.2% 

1.53 ±2.0% 

3.57 ± 2.0% 

75.1 ±0.53% 

2.94 ± 6,8% 

1.06 ±0,95% 

7.64 ±1.0% 

10,0 ±5,2% 

32.6 ± 4,9% 

7,70 ±2,1% 

6,75 ±1,9% 

12,7 ±0.79% 

59.1 ±1.7% 

12.8 ±0.78% 

0,0938 ±13% 

83,0 ± 0,48% 

6,36 ± 0,63% 

0,735 ± 3,5% 

2,91 ± 3,8% 

3,49 ±1,1% 

0,0847 ± 16% 

0,119 ±7,6% 

5,72 ± 3,3% 

0,0463 ± 27% '^' 

<0,0306 

<0,0306 

PFHS 

Avg. Cone. 

(ng/mL) ± RPD 

119 ±0,0% 

13.0 ±2.0% 

12,1 ±16% 

345 ±1,2% 

19,3 ±3,6% 

5,49 ±1.5% 

36,0 ±1,9% 

78.2 ± 3,7% 

211 ± 0,0% 

45,6 ±1,1% 

39,4 ± 0,76% 

77,1 ±4,2% 

441 ± 2.3% 

106 ±1,9% 

1.33 ±6,0% 

754 ±1.9% 

37,9 ± 8,4% 

5,88 ± 5,4% 

11,7 ±2.6% 

19,3 ±1.0% 

<0,103 

<0,103 

16.9 ±1,8% 

<0,103 

<0,103 

<0.103 

PFOS 

Avg. Cone. 

(ng/mL) ± RPD 

532 ± 8.5% 

74,4 ± 2,3% <^' 

72,1 ±0,69% 

1720 ±1,4% 

33,6 ±1,6% 

8,25 ± 3,9% 

263 ± 0.76% 

240 ±2,1%'^''^ 

861 ± 0.58% 

77,5 ± 9,2% 

144 ± 7.6% 

228 ± 5,4% 

1180 ±2,3% 

491 ± 2,7% <^' 

12,6 ±7,2% 

1040 ±1.8% 

55,4 ± 9,9% 

7,16 ±8,1% 

89,7 ± 4,4% 

106 ±6.0% 

0,734 ±14% 

0,427 ± 3,7%'^' 

216 ± 0,42% 

0,791 ± 3,7% 

<0,102 

<0,102 

The analytical method uncertainties associated with the reported results are as follows: PFBS 100% ± 19%, PFHS 100% ± 20%, 

and PFOS 100% ±37%, 

(1) The analytical uncertainty has Iseen adjusted for PFOS based on FMS recovery for: DAL 1 SOL to 100% ± 45% and D/\L 

137S to 100% ± 38%, See discussion in section 9 of the report. 

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

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

Page 10 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

3 Introduction 

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

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

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

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

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

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

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

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

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

containers for each sampling locafion 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. See section 8.8 of the report for field matrix spike levels. The aqueous 

equipment rinseate samples were collected in plain bottles without mari<ings or fortifications. 

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

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

Perfonnance Liquid Chromatography/Mass Spectrometry Direct Injection Analysis". 

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

collected, and for the trip blanks and aqueous soil-equipment rinseate samples. Tables 10-33 

summarize the individual sample results and the associated FMS recoveries. All results for the quality 

control samples prepared and analyzed with the samples are reported and discussed elsewhere in this 

report 

4 Test & Control Substances 

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

was purely analytical in nature. 

Page 11 of 68 
5 Reference Substances 

GLP10-01-02; Interim Report 07 

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

June/July 2010 

Reference Substance 

Chemical Name 

Chemical Fonnula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFBS 

(predominantly linear) 

Perfluorobutane sulfonate 

C4F9S03' 

Potassium Salt 

3M 

1/10/2017 

Frozen 

41-2600-8442-5 

TCR-121 

White Powder 

96,7% 

PFHS 

(linear) 

Perfluorohexane sulfonate 

CeFiaSOs 

Sodium Salt 

Wellington 

4/2/2013 

Frozen 

LPFHxSAMOS 

TCR08-0018 

Crystalline 

98% 

Reference Substance 

Chemical Name 

Chemical Formula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFOS 

(linear) 

Perfluorooctane sulfonate 

C8F17SO3" 

Potassium Salt 

CAS #2795-39-3 

Wellington 

10/18/2013 

Frozen 

LPFOSKBM06 

TCR08-0001 

Crystalline 

98% 

PFOS 

(linear + 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 £ 
GLP10-01-02; Interim Report 07 

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 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 Numtier 

Example 

1 

2 

3 

4 

String Descriptor 

DAL 131S Q2Y10 SFO 

Sampling Location 

Sampling Point 

Well Level 

Sampling Date 

Sample Type 

Example 

DAL = Decatur, AL 

Example: 131S 

R = Residum shallow water-bearing zone 

L = Bedmck water-tiearing zone 

S = Epikarst middle water-bearing zone 

Q2Y10 - 2nd Quarter, 2010 

0=primary sample 

1=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 

"Detennination of Perfluorinated Compounds In Water by High Perfonnance Liquid 

Chromatography/Mass Spectrometry Direct Injection Analysis". 

~TM , 

7.2 Sample Collection 

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

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

6, 2010 Samples were stored refrigerated at the laboratory after receipt. A set of laboratory prepared 

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

7.3 Sample Preparation 

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

analysis. 

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

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

additional Milli 0 water. 

7.4 Analysis 

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

perfonnance 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 13 of 68 
GLP10-01-02; Interim Report 07 

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 

ETS OIlie 

ETS-8-044,0 

7/15/2010 

Agilent 1100 

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

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

2or10tiL 

/Applied Biosystems API 4000 

Turtxj Spray 

Turtjo ion electrode 

Negative 

/Analyst 1,4,2 

ETS Mary Ann 

ETS-8-044,0 

9/17/10 

Agilent 1100 

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

Betasil CI 8 (2,1 mm X 100 mm), 5n 

SorlOuL 

/\pplied Biosystems API 5000 

Turtjo Spray 

Turbo ion electrode 

Negative 

Analyst 1.4.2 

Table 4. Liquid Chromatography Conditions. 

step 

Numtter 

0 

1 

2 

3 

4 

5 

Total Time 

(min) 

0 

1.0 

14.5 

15.5 

16.5 

20.0 

Flow Rate 

(fdJmin) 

300 

300 

300 

300 

300 

300 

Percent A 

(2 mM ammonium acetate) 

90,0 

90,0 

10,0 

10,0 

90,0 

90,0 

PercentB 

(Methanol) 

10.0 

10,0 

90,0 

90,0 

10.0 

10,0 

Table 5. Mass Transitions. 

Analyte 

PFBS 

PFHS 

PFOS 

Mass Transition 

Q1/Q3 

299/80 

299/99 

399/80 

399/99 

399/130 

499/80 

499/99 

499/130 

Dwell time was 125 or 50 msec for each 

transition. The individual transitions were 

summed to produce a "total ion chromatogram" 

(TIC), which was used for quantitation. 

8 Analytical Results 

8.1 Calibration 

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

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

Page 14 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Milli 0 water. A total of fifteen spiked standards ranging from 0.025 ng/mL to 100 ng/mL (nominal) were 

prepared, however, the 9/17/10 analysis did not contain the two highest curve points. Low or high curve 

points may have been disabled to meet method criteria. A quadratic, 1/x weighted, calibration curve of 

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

during the fitting process. Calculating the standard concentrations using the peak area confirmed 

accuracy of each curve point. 

7/15/10 Analysis for PFOS; The calibration curve was constructed using the linear isomer of PFOS only. 

Since the samples were expected to contain both linear and branched isomers of PFOS, LCS and 

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 PFO.S for both the 

7/15/10 and 9/17/10 analysis. 

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% relafive 

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

met for PFBS, PFHS, and PFOS for both the 7/15/10 and 9/17/10 analysis. 

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 LOO for all analytes can be found in Table 6. 

Table 6. Limit of Quantitation (LOQ). 

Analysis Date 

7/15/10 

9/17/10 

Dilution 

1 

10 

100 

1 

PFBS 

LOQ, ng/mL 

0.0306 

0,306 

3,06 

0.0255 

PFHS 

LOQ, ng/mL 

0.103 

1,03 

10,3 

0,0258 

PFOS 

LOQ, ng/mL 

0.102 

1.02 

10.2 

0.510 

8.4 Continuing Calibration 

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

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

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

7/15/10 Analysis; Twenty-one CCVs were analyzed during the course of the run with three CCVs not 

meeting method acceptance criteria with recoveries of 70.8%, 73.6%, and 73.3% for PFHS. Reported 

samples bracketed by these CCVs include: 132S, 134R, 135S, and 135L. 

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 perfomnance'and to detemnine the 

LOO for each analyte 

Page 15 of 68 
GLP10-0i-02; Interim Report 07 

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

June/July 2010 

8.6 Lab Control Spikes (LCSs) 

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

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

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

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

within 100% ± 20% with an RSD <20% Acceptance criteria was met for the PFBS, PFHS, and linear 

PFOS for LCS samples analyzed on 7/15/10. Acceptance criteria was not met for the low set of linear 

PFOS LCS analyzed on 9/17/10 with an average recovery of 191 %. The mid and high sets of linear 

PFOS LCS met method acceptance criteria, as did all three sets of LCS for PFBS and PFHS. The 

9/17/10 analysis included a number of samples that contained PFOS concentrations greater than the 

calibration range. It is believed that the high recovery for the low set of LCS is due to analyte carry-over 

as the low set of LCS were analyzed immediately after these samples. 

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

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

PFOS (linear + branched) were prepared at three concentrations to evaluate the potential for analytical 

bias. The LCS analyzed on 7/15/10 at the low and mid levels met method acceptance criteria, while the 

high level did not meet method acceptance criteria with an average recovery of 122%. The LCS 

analyzed on 9/17/10 at the mid and high levels met method acceptance criteria, while the low level did 

not meet method acceptance criteria with an average recovery of 125%. All PFOS (linear + branched) 

LCS were used in the determination of the analytical uncertainty. A method deviation is filed with the 

raw data for PFOS (linear and linear + branched) LCS that did not meet method acceptance criteria. 

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

1 /^or, . o Calculated Concentration ..-_., 

LCS Percent Recovery = 100% 

Spil<e Concentration 

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

average LCS recovery 

Page 16 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 7. Laboratory Control Spike Recovery. 

ETS-8-044,0 

Analyzed 7/15/10 

Lab ID 

LCS-100707-1 

LCS-100707-2 

LCS-100707-3 

Average ±%RSD 

LCS-100707-4 

LCS-100707-5 

LCS-100707-6 

Average ±%RSD 

LCS-100707-7 

LCS-100707-8 

LCS-100707-9 

Average ±%RSD 

PFBS 

Spiked 

Concentration 

(ng/mL) 

0,510 

0,510 

0,510 

Calculated 

Concentration 

(ng/mL) 

0.506 

0,534 

0,530 

YoRecovery 

99,3 

105 

104 

103 ±3.0% 

5.10 

5.10 

5,10 

5,13 

4,90 

5,23 

101 

96,1 

103 

100% ±3.5% 

30,6 

30,6 

30,6 

28,4 

27,9 

28,6 

92,7 

91,0 

93.6 

92.4% ±1.4% 

PFHS 

Spiked 

Concentration 

(ng/mL) 

0,515 

0,515 

0,515 

Calculated 

Concentration 

(ng/mL) 

0.463 

0.455 

0.480 

YoRecovery 

89,8 

88,3 

93,2 

90.4% ±2.8% 

5.15 

5.15 

5,15 

5,64 

5,59 

5,73 

110 

108 

111 

110% ±1.4% 

30,9 

30.9 

30,9 

30,7 

29,9 

30,4 

99.3 

96,7 

98.3 

98.1% ±1.3% 

ETS-8-044,0 

Analyzed 7/15/10 

Lab ID 

LCS-100707-1 

LCS-100707-2 

LCS-100707-3 

Average ±%RSD 

LCS-100707-4 

LCS-100707-5 

LCS-100707-6 

Average ±%RSD 

LCS-100707-7 

LCS-100707-8 

LCS-100707-9 

Average ± %RSD 

PFOS (linear) 

Spiked 

Concentration 

(ng/mL) 

0,510 

0,510 

0,510 

Calculated 

Concentration 

(ng/mL) 

0,480 

0,447 

0,470 

YoRecovery 

94,1 

87,6 

92,2 

91.3% ±3.6% 

5.10 

5.10 

5.10 

5,48 

5,43 

5,46 

107 

106 

107 

107% ±0.46% 

30,6 

30,6 

30,6 

30,1 

30,6 

30,7 

98,4 

100 

100 

99.6% ±1.1% 

Lab ID 

LCS-100707-10 

LCS-100707-11 

LCS-100707-12 

Average ±%RSD 

LCS-100707-13 

LCS-100707-14 

LCS-100707-15 

Average ±%RSD 

LCS-100707-16 

LCS-100707-17 

LCS-100707-18 

Average ±%RSD 

PFOS (linear + branched) 

Spiked 

Concentration 

(ng/mL) 

0,500 

0.500 

0.500 

Calculated 

Concentration 

(ng/mL) 

0,493 

0,431 

0.419 

YoRecovery 

98,6 

86,2 

83,8 

89.5% ±8.9% 

5,00 

5,00 

5,00 

5.84 

5.67 

5.83 

117 

113 

117 

116% ±1.7% 

30,0 

30,0 

30,0 

37,8 

36,0 

36,3 

126 

120 

121 

122% ±2.6%"' 

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

Page 17 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 7 continued. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Analyzed 9/17/10 

Lab ID 

LCS-100916-1 

LCS-100916-2 

LCS-100916-3 

Average ±%RSD 

LCS-100916-4 

LCS-100916-5 

LCS-100916-6 

Average ±%RSD 

LCS-100916-7 

LCS-100916-8 

LCS-100916-9 

Average ±%RSD 

PFBS 

Spiked 

Concentration 

(ng/mL) 

0,510 

0,510 

0,510 

Calculated 

Concentration 

(ng/mL) 

0.474 

0.583 

0.592 

YoRecovery 

93,0 

114 

116 

108% ±12% 

5,10 

5.10 

5.10 

5.07 

5.98 

6.14 

99,4 

117 

120 

112% ±9.9% 

15.3 

15.3 

15.3 

16,9 

16,1 

16,7 

110 

105 

109 

108% ±2.4% 

PFHS 

Spiked 

Concentration 

(ng/mL) 

0,515 

0,515 

0,515 

Calculated 

Concentration 

(ng/mL) 

0.461 

0.565 

0.563 

YoRecovery 

89,5 

110 

109 

103% ±11% 

5,15 

5.15 

5,15 

4.66 

5.50 

5.54 

90,5 

107 

108 

102% ±9.7% 

15.5 

15,5 

15,5 

15.7 

15.8 

15,3 

101 

102 

98.6 

101% ±1.7% 

ETS-8-044,0 

Analyzed 9/17/10 

Lab ID 

LCS-100916-1 

LCS-100916-2 

LCS-100916-3 

Average ±%RSD 

LCS-100916-4 

LCS-100916-5 

LCS-100916-6 

Average ±%RSD 

LCS-100916-7 

LCS-100916-8 

LCS-100916-9 

Average ±%RSO 

PFOS (linear) 

Spiked 

Concentration 

(ng/mL) 

0,510 

0,510 

0,510 

Calculated 

Concentration 

(ng/mL) 

1.10 

1.01 

0.821 

YoRecovery 

216 

197 

161 

191% ±15%'^-^ 

5,10 

5,10 

5,10 

4,32 

4,93 

5,18 

84.7 

96.8 

102 

94.5% ±9.4% 

15,3 

15,3 

15,3 

14.0 

14.7 

13.6 

91.3 

96.1 

88.9 

92.1% ±4.0% 

Lab ID 

LCS-100916-10 

LCS-100916-11 

LCS-100916-12 

Average ±%RSD 

LCS-100916-13 

LCS-100916-14 

LCS-100916-15 

Average ±%RSD 

LCS-100916-16 

LCS-100916-17 

LCS-100916-18 

Average ±%RSD 

PFOS (linear + branched) 

Spiked 

Concentration 

(ng/mL) 

0,500 

0,500 

0.500 

Calculated 

Concentration 

(ng/mL) 

0,678 

0,669 

0,527 

%Recovery 

136 

134 

105 

125% ±14%''' 

5,00 

5,00 

5,00 

4,87 

4,97 

4.84 

97,4 

99,4 

96,8 

97.9% ±1.4% 

15,0 

15,0 

15,0 

14,9 

15,2 

15,0 

99,5 

102 

100 

101% ±1.3% 

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

(2) The high recovery is most lilcely due to carry over, which is liicely due to samples analyzed prior to LCS samples which had 

PFOS concentrations exceeding the calibration range, 

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 OC samples. The 

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

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

method uncertainty values listed in Table 8. 

Page 18 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 8. Analytical Uncertainty. 

Analyte 

PFBS 

PFHS 

PFOS 

Standard Deviation 

9.39 

9.76 

18.6 

Method 

Uncertainty 

100%±19% 

100%±20% 

100%±37% 

8.8 Field Matrix Spikes (FMS) 

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

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

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

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

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

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

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

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

section 9 of this report. 

Table 9. Field Matrix Spike Levels. 

Sampling Location 

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

130L, 131L, 132U 133R, 134S, 134U 136S'^' 

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

135S, 135L<^\ 136U 138S '^', 138R 

131R, 134R, 135R 

Trip Blank 

Spike Level 

Low 

Mid 

High 

Low 

Mid 

High 

Low 

Mid 

High 

Low 

High 

Low 

Mid 

Mid-High 

High 

PFBS, ng/mL 

0.102 

1.02 

10.2 

1.02 

10,2 

102 

10,2 

102 

1020 

102 

1020 

1,02 

10.2 

102 

1020 

PFHS, ng/mL 

0.103 

1.03 

10.3 

1.03 

10.3 

103 

10,3 

103 

1030 

103 

1030 

1,03 

10,3 

103 

1030 

PFOS, ng/mL 

0.102 

1,02 

10.2 

1,02 

10,2 

102 

10,2 

102 

1020 

102 

1020 

1,02 

10,2 

102 

1020 

(1) One of the spiked bottles in this sampling set was overfilled by more than 10%, The field matrix spilce true value has been 

adjusted accordingly. 

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

Spike Concentraton 

00% 

9 Data Summar y and Discussion 

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

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

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

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

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

quantitative ranges. 

Page 19 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

DAL 1 SOL - The recovery of the high FMS sample for PFOS was 54.8%. The mid spike was not 

calculated since the detected concentration was lOx higher than the expected concentration. The 

analytical uncertainty has been adjusted for PFOS based on the recovery of the high FMS to 100% ± 

45%. 

DAL 132L - The high FMS spike level at 102 ng/mL was not an appropriate spike level to sufficiently 

evaluate PFOS recovery. 

DAL 134L - The high FMS spike level at 102 ng/mL was not an appropriate spike level to sufficiently 

evaluate PFOS recovery. 

DAL 135L - The recovery of the mid FMS sample for PFOS was 68.2%. The high FMS sample did 

meet method acceptance criteria with a recovery of 91.1%. The mid spike was the most appropriate 

spike level as compared to the sample concentration, however, no adjustment will be made to the 

analytical uncertainty as the method uncertainty for PFOS is 100% ± 37%. 

DAL 136L - The recovery of the mid FMS sample for PFOS was 65.6%. The high FMS sample did 

meet method acceptance criteria with a recovery of 79.4%. The mid spike was the most appropriate 

spike level as compared to the sample concentration, however, no adjustment will be made to the 

analytical uncertainty as the method uncertainty for PFOS is 100% ± 37%. 

DAL 137L - The recovery of the low FMS sample for PFHS was 149%. The mid and high FMS 

samples did meet method acceptance criteria with recoveries of 119% and 103%, respectively. The 

samples contain trace PFHS below the method LOQ of 0.103 ng/mL, which most likely accounts for the 

high recovery of the low FMS sample (spike level 0.103 ng/mL). Since the mid FMS met method 

acceptance criteria, and was an appropriate spike level as compared to the sample concentration, no 

adjustment will be made to the analytical uncertainty. 

DAL 137S - The recovery of the low FMS sample for PFHS was 186%. The mid and high FMS 

samples did meet method acceptance criteria with recoveries of 123% and 108%, respectively. The 

samples contain PFHS just below the method LOO of 0.103 ng/mL, which most likely accounts for the 

high recovery of the low FMS sample (spike level 0.103 ng/mL). Since the mid FMS met method 

acceptance criteria, and was an appropriate spike level as compared to the sample concentration, no 

adjustment will be made to the analytical uncertainty. The recovery of the mid FMS sample for PFOS 

was 61.5%. The high FMS sample did meet method acceptance criteria with a recovery of 83.9%. 

Since the mid spike was the most appropriate spike level as compared to the sample concentration, the 

analytical uncertainty has been adjusted for PFOS to 100% ± 38%. 

DAL 1 SSL - The recovery of the low FMS sample for PFHS was 203%. The mid and high FMS 

samples did meet method acceptance criteria with recoveries of 124% and 101%, respectively. The 

samples contain PFHS just below the method LOQ of 0.103 ng/mL, which most likely accounts for the 

high recovery of the low FMS sample (spike level 0.103 ng/mL). Since the mid FMS met method 

acceptance criteria, and was an appropriate spike level as compared to the sample concentration, no 

adjustment will be made to the analytical uncertainty. 

Page 20 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 10. DAL 130R Q2 Y10 SF (Sampled 7/1/10) 

3MUMSID 

GLP10-01-02-07-001 

GLP10-01-02-07-002 

GLP10-01-02-07-003 

GLP10-01-02-07-004 

GLP10-01-02-07-005 

Description 

DAL130RQ2Y10 SFO 

DAL130RQ2Y10 SF 1 

DAL130RQ2Y10 SF LS 

DAL130RQ2Y10 SF MS 

DAL130RQ2Y10 SF HS 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

16.5 

16.7 

27.4 

NA<^' 

NA<^> 

YoRecovery 

NA 

NA 

106 

NA<^' 

NA*^' 

16.6 ng/mL ±1.2Yo 

PFHS 

Concentration 

(ng/mL) 

119 

119 

130 

218 

979 

YoRecovery 

NA 

NA 

NC 

96.1 

83.5 

119 ng/mL tO.OYo 

PFOS 

Concentration 

(ng/mL) 

554 

509 

498 

598 

1350 

YoRecovery 

NA 

NA 

NC 

NC 

79.9 

532 ng/mL ±8.5Yo 

NA = Not Applicable 

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

PFHS and PFOS were analyzed on 7/15/10 with a 1:100 dilution. PFBS was analyzed on 9/17/10 without dilution. 

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

Page 21 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 11. DAL 1S0L Q2 Y10 SF (Sampled 7/1/10) 

3M LIMS ID 

GLP10-01-02-07-011 

GLP10-01-02-07-012 

GLP10-01-02-07-013 

GLP10-01-02-07-014 

GLP 10-01-02-07-015 

Average Concenti 

Description 

DAL130LQ2Y10 SFO 

DAL130LQ2Y10 SF 1 

DAL130LQ2Y10 SF LS 

DAL130LQ2Y10 SF MS 

DAL130LQ2Y10 SF HS 

ration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

1,51 

1.54 

2.61 

463 

130 

YoRecovery 

NA 

NA 

106 

NA'^' 

126 

1.53 ng/mL ±2.0Yo 

PFHS 

Concentration 

(ng/mL) 

12.9 

13.1 

14.1 

432 

134 

%Recovery 

NA 

NA 

NC 

NA(^' 

117 

13.0 ng/mL ±1.5Yo 

PFOS 

Concentration 

(ng/mL) 

75.2 

73.5 

75.2 

476 

130 

XRecovery 

NA 

NA 

NC 

NA<^' 

54.8'^' 

74.4 ng/mL ±2.3Yo'^> 

NA = Not Applicable 

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

PFBS, PFHS, and PFOS were analyzed on 7/15/10 with a 1:10 dilution. 

(1) Suspect the sample bottle was prepared in correc^tly. The MS concentration detected is not consistent with the spike level (nominal concentration of 10 ng/mL). 

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

(3) The analytical uncertainty for PFOS has been adjusted for FMS recovery to 100% ± 45%. 

Page 22 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 12. DAL 1S0S Q2 Y10 SF (Sampled 7/1/10) 

3M LIMS ID 

GLP10-01-02-07-006 

GLP10-01-02-07-007 

GLP10-01-02-07-008 

GLP10-01-02-07-009 

GLP10-01-02-07-010 

Average Concent 

Description 

DAL130SQ2Y10 SFO 

DAL130SQ2Y10 SF 1 

DAL130SQ2Y10 SF LS 

DAL130SQ2Y10 SF MS 

DAL130SQ2Y10 SF HS 

Tition (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

3.53 

3.60 

14.0 

NA'^' 

NA'^' 

YoRecovery 

NA 

NA 

102 

NA<^' 

NA<^' 

3.57 ng/mL ±2.(y'/o 

PFHS 

Concentration 

(ng/mL) 

11.1 

13.0 

22.9 

113 

924 

YoRecovery 

NA 

NA 

105 

98.0 

88.5 

12.1 ng/mL ± 16Yo 

PFOS 

Concentration 

(ng/mL) 

72.3 

71.8 

84.5 

152 

937 

YoRecovery 

NA 

NA 

NC 

78.2 

84.8 

72.1 ng/mL ±0.69Yo 

NA = Not /Applicable 

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

PFHS and PFOS were analyzed on 7/15/10 with a 1:100 diluton. PFBS was analyzed on 9/17/10 without dilution. 

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

Table 13. DAL 131R Q2 Y10 SF (Sampled 7/1/10) 

3MUMSID 

GLP10-01-02-07-016 

GLP10-01-02-07-017 

GLP10-01-02-07-018 

GLP10-01-02-07-019 

Description 

DAL131RQ2Y10 SFO 

DAL131RQ2Y10 SF 1 

DAL131RQ2Y10 SF LS 

DAL131RQ2Y10 SF HS 

Average Concentration (ng/mL) t YoRPD 

PFBS 

Concentration 

(ng/mL) 

74.9 

75.3 

179 

NA<^> 

YoRecovery 

NA 

NA 

102 

NA<^' 

75.1 ng/mL ±0.53Yo 

PFHS 

Concentration 

(ng/mL) 

343 

347 

447 

1160 

YoRecovery 

NA 

NA 

NC 

79.1 

345 ng/mL ±1.2Yo 

PFOS 

Concentration 

(ng/mL) 

1710 

1730 

1820 

2430 

YoRecovery 

NA 

NA 

NC 

69.8 

1720 ng/mL ±1.4Yo 

NA = Not /Applicable 

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

PFHS and PFOS were analyzed on 7/15/10 with a 1 ;100 dilution. PFBS was analyzed on 9/17/10 without dilution. 

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

Page 23 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 14. DAL 1S1L 02 Y10 SF (Sampled 6/30/10) 

3M LIMS ID 

GLP10-01-02-07-025 

GLP10-01-02-07-026 

GLP10-01-02-07-027 

GLP10-01-02-07-028 

GLP 10-01-02-07-029 

Description 

DAL131LQ2Y10 SFO 

DAL131LQ2Y10 SF 1 

DAL131LQ2Y10 SF LS 

DAL131LQ2Y10 SF MS 

DAL131LQ2Y10 SF HS 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

2.84 

3.04 

4.18 

13.2 

88.4 

YoRecovery 

NA 

NA 

NC 

101 

83.8 

2.94 ng/mL ±6.8% 

PFHS 

Concentration 

(ng/mL) 

18.9 

19.6 

20.7 

30.2 

104 

YoRecovery 

NA 

NA 

NC 

106 

82.3 

19.3 ng/mL ±3.6Yo 

PFOS 

Concentration 

(ng/mL) 

33.9 

33.4 

34.9 

43.9 

112 

YoRecovery 

NA 

NA 

NC 

NC 

76.9 

33.6 ng/mL ±1.6Yo 

NA = Not Applicable 

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

PFBS, PFHS, and PFOS were analyzed on 7/15/10 with a 1:10 dilution. 

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

Table 15. DAL ISIS Q2 Y10 SF (Sampled 6/S0/10) 

3M LIMS ID 

GLP10-01-02-07-020 

GLP10-01-02-07-021 

GLP10-01-02-07-022 

GLP10-01-02-07-023 

GLP10-01-02-07-024 

Average Concenti 

Description 

DAL131SQ2Y10 SFO 

DAL131SQ2Y10 SF 1 

DAL131SQ2Y10 SF LS 

DAL131SQ2Y10 SF MS 

DAL131SQ2Y10 SF HS 

•atfon (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

1.06 

1.05 

11.0 

NA<^' 

NA'^> 

YoRecovery 

NA 

NA 

97.5 

NA<^' 

NA<^' 

1.06 ng/mL ±0.95Yo 

PFHS 

Concentration 

(ng/mL) 

5.53 

5.45 

14.3 

NA<^' 

NA<^' 

YoRecovery 

NA 

NA 

85.5 

NA<^> 

NA<^' 

5.49 ng/mL ±1.5Yo 

PFOS 

Concerrtration 

(ng/mL) 

8.41 

8.09 

18.2 

NA(^> 

NA*^' 

YoRecovery 

NA 

NA 

97.5 

NA<^' 

NA'^' 

8.25 ng/mL ±3.9Yo 

NA = Not Applicable 

PFBS, PFHS, and PFOS were analyzed on 9/17/10 without dilution. 

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

Page 24 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 16. DAL 1S2R Q2 Y10 SF (Sampled 7/1/10) 

3M LIMS ID 

GLP 10-01-02-07-030 

GLP10-01-02-07-031 

GLP10-01-02-07-032 

GLP 10-01-02-07-033 

GLP10-01-02-07-034 

Description 

DAL132RQ2Y10 SFO 

DAL132RQ2Y10 SF 1 

DAL132RQ2Y10 SF LS 

DAL132RQ2Y10 SF MS 

DAL132RQ2Y10 SF HS 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

7,60 

7.68 

17.5 

NA<^' 

NA'^' 

YoRecovery 

NA 

NA 

96.7 

NA<^> 

NA<^' 

7.64 ng/mL ±1.0Yo 

PFHSf^> 

Concentration 

(ng/mL) 

36.3 

35.6 

44.8 

133 

865 

YoRecovery 

NA 

NA 

NC 

94.2 

80.5 

36.0 ng/mL ±1.9Yo 

PFOS 

Concentration 

(ng/mL) 

262 

264 

274 

333 

1070 

YoRecovery 

NA 

NA 

NC 

NC 

79.3 

263 ng/mL ±0.76Yo 

NA= Not Applicable 

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

PFHS and PFOS were analyzed on 7/15/10 with a 1:100 dilution. PFBS was analyzed on 9/17/10 without dilution. 

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

Table 17. DAL 132L Q2 Y10 SF (Sampled 7/1/10) 

3M LIMS ID 

GLP 10-01-02-07-040 

GLP 10-01-02-07-041 

GLP10-01-02-07-042 

GLP10-01-02-07-043 

GLP 10-01-02-07-044 

Description 

DAL132LQ2Y10 SFO 

DAL132LQ2Y10 SF 1 

DAL132LQ2Y10 SF LS 

DAL132LQ2Y10 SF MS 

DAL132LQ2Y10 SF HS 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

10.3 

9.78 

11.2 

18.9 

102 

YoRecovery 

NA 

NA 

NC 

86.9 

90.2 

10.0 ng/mL ±5.2Yo 

PFHS 

Concentration 

(ng/mL) 

76.7 

79.6 

79.7 

84.9 

177 

YoRecovery 

NA 

NA 

NC 

NC 

96.0 

78.2 ng/mL ±3.r/o 

PFOS 

Concentration 

(ng/mL) 

238 

243 

257 

270 

379 

YoRecovery 

NA 

NA 

NC 

NC 

NC 

240 ng/mL tZIYo'^ ' 

NA = Not Applicable 

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

PFBS, PFHS, and PFOS were analyzed on 7/15/10 with a 1:10 dilution. 

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

Page 25 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 18. DAL 1S2S Q2 Y10 SF (Sampled 7/1/10) 

3MUIVISID 

GLP10-01-02-07-035 

GLP10-01-02-07-036 

GLP10-01-02-07-037 

GLP10-01-02-07-038 

GLP10-01-02-07-039 

Average Concenti 

Description 

DAL132SQ2Y10 SFO 

DAL132SQ2Y10 SF 1 

DAL132SQ2Y10 SF LS 

DAL132SQ2Y10 SF MS 

DAL132SQ2Y10 SF HS 

-atfon (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

31.8 

33.4 

44.8 

135 

NA*^' 

YoRecovery 

NA 

NA 

NC 

100 

NA'^' 

32.6ng/mL±4.9Yo 

PFHS 

Concentration 

(ng/mL) 

211 

211 

213 

287 

1100 

YoRecovery 

NA 

NA 

NC 

NC 

86.3 

211 ng/mL ±0.0Yo 

PFOS 

Concentration 

(ng/mL) 

863 

858 

825 

873 

1660 

YoRecovery 

NA 

NA 

NC 

NC 

77.9 

861 ng/mL ±0.58Yo 

NA= Not Applicable 

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

PFHS and PFOS were analyzed on 7/15/10 with a 1:100 dilution. PFBS was analyzed on 9/17/10 without dilution. 

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

Table 19. DAL 1SSR Q2 Y10 SF (Sampled 7/1/10) 

3MUMSID 

GLP10-01-02-07-045 

GLP10-01-02-07-046 

GLP 10-01-02-07-047 

GLP10-01-02-07-048 

GLP10-01-02-07-049 

Description 

DAL133RQ2Y10 SFO 

DAL133RQ2Y10 SF 1 

DAL133RQ2Y10 SF LS 

DAL133RQ2Y10 SF MS 

DAL133RQ2Y10 SF HS 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

7.78 

7.62 

8.87 

18.2 

NA<^' 

YoRecovery 

NA 

NA 

NC 

103 

NA'^' 

7.70ng/mL±2.1Yo 

PFHS 

Concentration 

(ng/mL) 

45.8 

45.3 

44.6 

52.9 

128 

YoRecovery 

NA 

NA 

NC 

NC 

80.0 

45.6 ng/mL ± 1.1 Yo 

PFOS 

Concentration 

(ng/mL) 

73.9 

81.0 

71.0 

84.2 

160 

YoRecovery 

NA 

NA 

NC 

NC 

80.9 

77.5 ng/mL ±9.2Yo 

NA= Not Applicable 

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

PFHS and PFOS were analyzed on 7/15/10 with a 1:10 dilution. PFBS was analyzed on 9/17/10 without dilution. 

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

Page 26 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 20. DAL 133L Q2 Y10 SF (Sampled 7/2/10) 

3M LIMS ID 

GLP 10-01-02-07-055 

GLP10-01-02-07-056 

GLP10-01-02-07-057 

GLP10-01-02-07-058 

GLP10-01-02-07-059 

Average Concenti 

Description 

DAL132LQ2Y10 SFO 

DAL132LQ2Y10 SF 1 

DAL132LQ2Y10 SF LS 

DAL132LQ2Y10 SF MS 

DAL132LQ2Y10 SF HS 

•ation (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

6.81 

6.68 

16.7 

NA'^' 

NA<^' 

YoRecovery 

NA 

NA 

97.6 

NA<^' 

NA'^' 

6.75 ng/mL ±1.9Yo 

PFHS 

Concentration 

(ng/mL) 

39.5 

39.2 

48.3 

145 

914 

YoRecovery 

NA 

NA 

NC 

103 

84.9 

39.4 ng/mL ±0.76Yo 

PFOS 

Concentration 

(ng/mL) 

139 

149 

161 

274 

1030 

YoRecovery 

NA 

NA 

NC 

128 

86.8 

144 ng/mL ± 7.6% 

NA= Not Applicable 

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

PFHS and PFOS were analyzed on 7/15/10 with a 1:50 dilution. PFBS was analyzed on 9/17/10 without dilution. 

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

Table 21. DAL 1SSS 02 Y10 SF (Sampled 7/1/10) 

3M LIMS ID 

GLP10-01-02-07-050 

GLP10-01-02-07-051 

GLP10-01-02-07-052 

GLP10-01-02-07-053 

GLP10-01-02-07-054 

Description 

DAL133SQ2Y10 SFO 

DAL133SQ2Y10 SF 1 

DAL133SQ2Y10 SF LS 

DAL133SQ2Y10 SF MS 

DAL133SQ2Y10 SF HS 

Average Concerrtration (ng/mL) ± YoRPD 

PFBS 

Concerrtration 

(ng/mL) 

12.6 

12.7 

21.8 

NA<^> 

NA<^> 

YoRecovery 

NA 

NA 

89.7 

NA'^' 

NA'^' 

12.7 ng/mL ±0.79Yo 

PFHS 

Concentration 

(ng/mL) 

75.5 

78.7 

89.5 

173 

990 

YoRecovery 

NA 

NA 

NC 

93.1 

88.6 

77.1 ng/mL ±4.2Yo 

PFOS 

Concentration 

(ng/mL) 

221 

234 

230 

337 

1180 

YoRecovery 

NA 

NA 

NC 

107 

93.2 

228 ng/mL ±5.4Yo 

NA = Not /Applicable 

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

PFHS and PFOS were analyzed on 7/15/10 with a 1:50 dilution. PFBS was analyzed on 9/17/10 without dilution. 

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

Page 27 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 22. DAL 134R Q2 Y10 SF (Sampled 7/2/10) 

3M LIMS ID 

GLP10-01-02-07-060 

GLP10-01-02-07-061 

GLP10-01-02-07-062 

GLP10-01-02-07-063 

Description 

DAL134RQ2Y10 SFO 

DAL134RQ2Y10 SF 1 

DAL134RQ2Y10 SF LS 

DAL134RQ2Y10 SF HS 

Average Concentration (ng/mL) + YoRPD 

PFBS 

Concentration 

(ng/mL) 

58.6 

59.6 

157 

NA<^' 

YoRecovery 

NA 

NA 

96.0 

NA<^' 

59.1 ng/mL ± I.V/o 

PFHS 

Concentration 

(ng/mL) 

436 

446 

521 

1270 

YoRecovery 

NA 

NA 

NC 

80.5 

441 ng/mL ±2.3Yo 

PFOS 

Concentration 

(ng/mL) 

1170 

1190 

1140 

1900 

YoRecovery 

NA 

NA 

NC 

70.3 

1180ng/mL±2.3Yo 

NA = Not Applicable 

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

PFHS and PFOS were analyzed on 7/15/10 vwth a 1:100 dilution. PFBS was analyzed on 9/17/10 without dilution. 

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

Table 23. DAL 134L Q2 Y10 SF (Sampled 7/2/10) 

3M LIMS ID 

GLP10-01-02-07-075 

GLP10-01-02-07-076 

GLP10-01-02-07-077 

GLP10-01-02-07-078 

GLP10-01-02-07-079 

Description 

DAL134LQ2Y10 SFO 

DAL134LQ2Y10 SF 1 

DAL134LQ2Y10 SF LS 

DAL134LQ2Y10 SF MS 

DAL134LQ2Y10 SF HS 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

12.7 

12.8 

13.8 

22.5 

NA(^> 

YoRecovery 

NA 

NA 

NC 

95.6 

NA<^' 

12.8 ng/mL ±0.78Yo 

PFHS 

Concentration 

(ng/mL) 

107 

105 

107 

112 

184 

YoRecovery 

NA 

NA 

NC 

NC 

75.7 

106 ng/mL ±1.9Yo 

PFOS 

Concerrtration 

(ng/mL) 

484 

497 

503 

470 

535 

YoRecovery 

NA 

NA 

NC 

NC 

NC 

491 ng/mL ±2.^/0^^ 

NA = Not Applicable 

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

PFHS and PFOS were analyzed on 7/15/10 with a 1:10 dilution. PFBS was analyzed on 9/17/10 without dilution. 

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

(2) Sampling location did not have an appropriate FMS spike level to sufliciently evaluate PFOS recovery. 

Page 28 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 24. DAL 134S Q2 Y10 SF (Sampled 7/2/10) 

3M LIMS ID 

GLP10-01-02-07-070 

GLP10-01-02-07-071 

GLP10-01-02-07-072 

GLP10-01-02-07-073 

GLP 10-01-02-07-074 

Description 

DAL134SQ2Y10 SFO 

DAL134SQ2Y10 SF 1 

DAL134SQ2Y10 SF LS 

DAL134SQ2Y10 SF MS 

DAL134SQ2Y10 SF HS 

Average Concerrtration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

0,100 

0,0876 

1,21 

10.9 

87.8 

YoRecovery 

NA 

NA 

109 

106 

86.0 

0.0938 ng/mL ±13Yo 

PFHS 

Concentration 

(ng/mL) 

1.37 

1.29 

2.43 

12.7 

91.4 

YoRecovery 

NA 

NA 

107 

110 

87.4 

1.33 ng/mL ±6.0Yo 

PFOS 

Concentration 

(ng/mL) 

13.1 

12.2 

13.1 

23.4 

101 

YoRecovery 

NA 

NA 

NC 

106 

86.3 

12.6 ng/mL ± 7.2Yo 

NA= Not Applicable 

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

PFBS, PFHS and PFOS were analyzed on 7/15/10 with a 1:5 dilution. 

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

Table 25. DAL 1S5R Q2 Y10 SF (Sampled 7/2/10) 

3M LIMS ID 

GLP10-01-02-07-064 

GLP10-01-02-07-065 

GLP10-01-02-07-066 

GLP10-01-02-07-067 

Description 

DAL135RQ2Y10 SFO 

DAL135RQ2Y10 SF 1 

DAL135RQ2Y10 SF LS 

DAL135RQ2Y10 SF HS 

Average Concerrtration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

82.8 

83.2 

185 

NA<^' 

YoRecovery 

NA 

NA 

100 

NA<^' 

83.0 ng/mL ±0.48Yo 

PFHS 

Concentration 

(ng/mL) 

761 

747 

853 

1610 

YoRecovery 

NA 

NA 

NC 

83.1 

754 ng/mL ±1.9Yo 

PFOS 

Concentration 

(ng/mL)^ 

1030 

1050 

1190 

1890 

YoRecovery 

NA 

NA 

NC 

83.2 

1040 ng/mL ±1.8Yo 

NA = Not Applicable 

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

PFHS and PFOS were analyzed on 7/15/10 with a 1:100 dilution. PFBS was analyzed on 9/17/10 without dilution. 

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

Page 29 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 26. DAL 1S5L Q2 Y10 SF (Sampled 7/2/10) 

3M LIMS ID 

GLP10-01-02-07-085 

GLP10-01-02-07-086 

GLP10-01-02-07-087 

GLP10-01-02-07-088 

GLP10-01-02-07-089 

Description 

DAL135LQ2Y10 SFO 

DAL135LQ2Y10 SF 1 

DAL135LQ2Y10 SF LS 

DAL135LQ2Y10 SF MS 

DAL135LQ2Y10 SF HS 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

6.38 

6.34 

15.6 

NA'^' 

NA'^' 

YoRecovery 

NA 

NA 

90.6 

NA'^' 

NA<^' 

6.36 ng/mL ±0.63Yo 

PFHS 

Concentration 

(ng/mL) 

36.3 

39.5 

49.6 

132 

922 

YoRecovery 

NA 

NA 

NC 

103 

85.8 

37.9 ng/mL ±8.4Yo 

PFOS 

Concentration 

(ng/mL) 

52.6 

58.1 

62.2 

117 

985 

YoRecovery 

NA 

NA 

NC 

68.2 <^' 

91.1 

55.4 ng/mL ±9.9Yo 

NA = Not Applicable 

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

PFHS and PFOS were analyzed on 7/15/10 v«ith a 1:100 dilution. PFBS was analyzed on 9/17/10 without dilution. 

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

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

Table 27. DAL 1S5S Q2 Y10 SF (Sampled 7/2/10) 

3M LIMS ID 

GLP10-01-02-07-080 

GLP10-01-02-07-081 

GLP10-01-02-07-082 

GLP10-01-02-07-083 

GLP 10-01-02-07-084 

Description 

DAL135SQ2Y10 SFO 

DAL135SQ2Y10 SF 1 

DAL135SQ2Y10 SF LS 

DAL135SQ2Y10 SF MS 

DAL135SQ2Y10 SF HS 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concerrtration 

(ng/mL) 

0.748 

0.722 

11.0 

NA'^' 

NA<^' 

YoRecovery 

NA 

NA 

101 

NA'^' 

NA'^' 

0.735 ng/mL ±3.5Yo 

PFHS 

Concentration 

(ng/mL) 

5.72 

6.04 

15.2 

NA'^> 

NA'^' 

%Recovery 

NA 

NA 

90.5 

NA<^> 

NA'^' 

5.88 ng/mL ±5.4Yo 

PFOS 

Concentration 

(ng/mL) 

6.87 

7.45 

16.5 

NA<^' 

NA(^> 

YoRecovery 

NA 

NA 

91.6 

NA(^' 

NA<^' 

7.16 ng/mL ±8.1Yo 

NA = Not Applicable 

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

PFBS, PFHS and PFOS were analyzed on 9/17/10 without dilution. 

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

Page 30 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 28. DAL 1S6LQ2Y10 SF (6/30/10) 

3M LIMS ID 

GLP10-01-02-07-095 

GLP10-01-02-07-096 

GLP10-01-02-07-097 

GLP10-01-02-07-098 

GLP10-01-02-07-099 

Description 

DAL136LQ2Y10 SFO 

DAL136LQ2Y10 SF 1 

DAL136LQ2Y10 SF LS 

DAL136LQ2Y10 SF MS 

DAL136LQ2Y10 SF HS 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

2.96 

2.85 

13.7 

NA<^' 

NA<^> 

YoRecovery 

NA 

NA 

106 

NA'^> 

NA'^' 

2.91 ng/mL ±3.8Yo 

PFHS 

Concentration 

(ng/mL) 

11.8 

11.5 

20.7 

108 

856 

YoRecovery 

NA 

NA 

87.9 

93.5 

82.0 

11.7 ng/mL ±2.6Yo 

PFOS 

Concentration 

(ng/mL) 

87.7 

91.6 

93.8 

157 

899 

YoRecovery 

NA 

NA 

NC 

65.6 '^> 

79.4 

89.7 ng/mL ±4.4Yo 

HA. = Not /Vpplicable 

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

PFHS and PFOS were analyzed on 7/15/10 with a 1:50 dilution. PFBS was analyzed on 9/17/10 without dilution. 

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

(2) The field matrix spike did not meet method acceptance criteria. 

Table 29. DAL 1S6S Q2 Y10 SF (Sampled 6/S0/10) 

3M LIMS ID 

GLP10-01-02-07-090 

GLP10-01-02-07-091 

GLP10-01-02-07-092 

GLP10-01-02-07-093 

GLP10-01-02-07-094 

Description 

DAL136SQ2Y10 SFO 

DAL136SQ2Y10 SF 1 

DAL136SQ2Y10 SF LS 

DAL136SQ2Y10 SF MS 

DAL136SQ2Y10 SF HS 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

3.47 

3.51 

4.78 

14.1 

NA<^' 

YoRecovery 

NA 

NA 

NC 

104 

NA'^' 

3.49 ng/mL ±1.1Yo 

PFHS 

Concentration 

(ng/mL) 

19.2 

19.4 

20.0 

29.1 

98.8 

YoRecovery 

NA 

NA 

NC 

95.1 

85.7 

19.3 ng/mL ±1.0Yo 

PFOS 

Concerrtration 

(ng/mL) 

103 

109 

110 

110 

183 

YoRecovery 

NA 

NA 

NC 

NC 

83.9 

106 ng/mL ±6.0Yo 

NA = Not Applicable 

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

PFHS and PFOS were analyzed on 7/15/10 with a 1:10 dilution. PFBS was analyzed on 9/17/10 without dilution. 

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

Page 31 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 30. DAL 137L Q2 Y10 SF (Sampled 7/1/10) 

3M LIMS ID 

GLP10-01-02-07-105 

GLP10-01-02-07-106 

GLP10-01-02-07-107 

GLP10-01-02-07-108 

GLP10-01-02-07-109 

Description 

DAL137LQ2Y10 SFO 

DAL137LQ2Y10 SF 1 

DAL137LQ2Y10 SF LS 

DAL137LQ2Y10 SF MS 

DAL137LQ2Y10 SF HS 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

0.0914 

0.0780 

0.203 

1.21 

10.6 

YoRecovery 

NA 

NA 

116 

110 

103 

0.0847 ng/mL ±16% 

PFHS 

Concerrtration 

(ng/mL) 

<0.103 

<0.103 

0.153 

1.23 

10.6 

YoRecovery 

NA 

NA 

149 <^> 

119 

103 

<0.103 ng/mL 

PFOS 

Concerrtration 

(ng/mL) 

0.684 

0.784 

0.886 

1.85 

10.6 

YoRecovery 

NA 

NA 

NC 

109 

96.5 

0.734 ng/mL±14Yo 

NA = Not /Applicable 

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

PFBS, PFHS and PFOS were analyzed on 7/15/10 without dilution. 

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

Table 31. DAL 1S7S Q2 Y10 SF (Sampled 7/1/10) 

3M LIMS ID 

GLP10-01-02-07-100 

GLP10-01-02-07-101 

GLP10-01-02-07-102 

GLP10-01-02-07-103 

GLP10-01-02-07-104 

Description 

DAL137SQ2Y10 SFO 

DAL137SQ2Y10 SF 1 

DAL137SQ2Y10 SF LS 

DAL137SQ2Y10 SF MS 

DAL137SQ2Y10 SF HS 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

0.123 

0.114 

0.232 

1.38 

11.6 

YoRecovery 

NA 

NA 

111 

124 

113 

0.119 ng/mL ±7.6Yo 

PFHS 

Concentration 

(ng/mL) 

<0.103 

<0.103 

0.192 

1.27 

11.1 

YoRecovery 

NA 

NA 

186 <^' 

123 

108 

<0.103 ng/mL 

PFOS 

Concerrtration 

(ng/mL) 

0.435 

0.419 

0.562 

1.05 

8.99. 

YoRecovery 

NA 

NA 

NC 

61.5'^> 

83.9 

0.427 ng/mL ±3.7Yo^ 

NA = Not /Applicable 

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

PFBS, PFHS and PFOS were analyzed on 7/15/10 without dilution. 

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

(2) The analytical uncertainty for PFOS has been adjusted for FMS recovery to 100% ± 38%. 

Page 32 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 32. DAL 138S Q2 Y10 SF (Sampled 6/30/10) 

3M LIMS ID 

GLP10-01-02-07-110 

GLP10-01-02-07-111 

GLP10-01-02-07-112 

GLP10-01-02-07-113 

GLP10-01-02-07-114 

Average Concent 

Description 

DAL138SQ2Y10 SFO 

DAL138SQ2Y10 SF 1 

DAL138SQ2Y10 SF LS 

DAL138SQ2Y10 SF MS 

DAL138SQ2Y10 SF HS 

ratfon (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

5.81 

5.62 

15.5 

NA<^' 

NA<^' 

YoRecovery 

NA 

NA 

106 

NA<^' 

NA<^' 

5.72 ng/mL ±3.3Yo 

PFHS 

Concentration 

(rig/mL) 

17.0 

16.7 

27.8 

116 

888 

YoRecovery 

NA 

NA 

NC 

96.3 

84.6 

16.9 ng/mL ±1.8Yo 

PFOS 

Concentration 

(ng/mL) 

216 

217 

240 

319 

1091 

YoRecovery 

NA 

NA 

NC 

NC 

85.7 

216 ng/mL ±0.42Yo 

NA = Not Applicable 

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

PFHS and PFOS were analyzed on 7/15/10 with a 1:50 dilution. PFBS was analyzed on 9/17/10 without dilution. 

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

Table 33. DAL 138L Q2 Y10 SF (Sampled 6/30/10) 

3M LIMS ID 

GLP10-01-02-07-115 

GLP10-01-02-07-116 

GLP10-01-02-07-117 

GLP10-01-02-07-118 

GLP10-01-02-07-119 

Description 

DAL138LQ2Y10 SFO 

DAL138LQ2Y10 SF 1 

DAL138LQ2Y10 SF LS 

DAL138LQ2Y10 SF MS 

DAL138LQ2Y10 SF HS 

Average Concentration (ng/mL) ± YoRPD 

PFBS 

Concentration 

(ng/mL) 

0.0525 

0.0401 

0.153 

1.19 

11.2 

YoRecovery 

NA 

NA 

105 

112 

109 

0.0463 ng/mL ±2r/o'^^ 

PFHS 

Concentration 

(ng/mL) 

<0.103 

<0.103 

0.209 

1.28 

10.4 

%Recovery 

NA 

NA 

203'^' 

124 

101 

<0.103 ng/mL 

PFOS 

Concentration 

(ng/mL) 

0.805 

0.776 

0.805 

1.66 

9.71 

YoRecovery 

NA 

NA 

NC 

85.1 

87.5 

0.791 ng/mL ±3.7Yo 

NA=NotApplicat)le 

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

PFBS, PFHS and PFOS were analyzed on 7/15/10 without dilution. 

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

(2) The field matrix spike did not meet method acceptance criteria. 

Page 33 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Table 34. Trip Blank 

3M LIMS ID 

GLP10-01-02-07-124 

GLP10-01-02-07-120 

GLP10-01-02-07-121 

GLP10-01-02-07-122 

GLP10-01-02-07-123 

Description 

Trip Blank Sample 

Trip Blank LS 

Trip Blank MS 

Trip Blank MHS 

Trip Blank HS 

PFBS 

Concentration 

(ng/mL) 

<0.0306 

1.35 

12.7 

117 

1170 

YoRecovery 

NA 

132 <^' 

125 

115 

115 

PFHS 

Concentration 

(ng/mL) 

<0.103 

1.22 

11.4 

108 

1090 

YoRecovery 

NA 

118 

111 

105 

106 

PFOS 

Concentration 

(ng/mL) 

<0.510 

1.19 

11.6 

114 

900 

YoRecovery 

NA 

117 

114 

112 

88.2 

NA= NotApplicatJe 

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

Table 35. Rinseate Blanks 

3M LIMS ID 

GLP10-01-02-07-068 

GLP10-01-02-07-069 

Description 

DAL137LQ2Y10SFRB 

DAL131RQ2Y10SFRB 

PFBS 

Concentration 

(ng/mL) 

<0.0306 

<0.0306 

PFHS 

Concerrtration 

(ng/mL) 

<0.103 

<0.103 

PFOS 

Concentration 

(ng/mL) 

<0.102 

<0.102 

Page 34 of 68 
GLP10-01-02; Interim Report 07 

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 analytic:al method 

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

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

11 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 Attachment s 

Attachment A: Protocol Amendment #2 (General Project Outline) 

Attachment B: Representative Chromatograms and Calibration Curves 

Attachment C: Analytical Method 

Attachment D: Method Deviation 

Page 35 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

13 Signatures 

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

D'/ocr^-o/o 

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

(( 

'Id 

Gary Hohenstein, Sponsor Representative Date 

mm 

Jaisimha P^sari, Study Director Jate 

Page 36 of 68 
GLP10-01 -02; Interim Report 07 

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

Attachment A June/July 2010 , , . ,. , . .,, „^ „ „ ^ «« 

Analytical Protocol: GLP10-01-02 

Amendment 07 

Study Title 

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

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

Decatur Phase 3 Site-Related Monitoring Program 

PROTOCOL AMENDMENT NO. 07 

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 

Former Sludge Incorporation Area (FSIA) Groundwater 

Page 1 of 9 

Page 37 of 68 
GLP10-01-02; Interim Report 07 

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

Attachment A 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, pttfcedurai blank, and at variable known con(»ntrations in calibration standards, and 

quantified to evaluate surrogate recoveries. 

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

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

surrogate. 

A statrfe Isotope-labeled intemal standard, [(^®02)-PFHS] will be added at a fixed concentration to each sample, 

LMS, LCS, procedural blank and calitH-ation standard for aiding quantitation of PFHS. 

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

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

AMEND TO READ: 

A stable isotope-labeled sun-c^ate [(1,2,3,4-"C4)-PFOS] may also be added at a fixed level to each sample, 

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

evaluate surrogate recoveries. 

A stable isotope-labeled intemal standard, {(1,2,3,4,5,6,7,8-"C8)-PFOSj may be added at a fixed oDncentration 

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

surrogate. 

A stable isotope-labeled intemal standard, [(^*02)-PFHS] may 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 interna! standand, [(^*02H'FBS] may be added at a fixed concenti^tion to each sample, 

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

The use of intemal standards and sun'ogate are only appropriate for those sampling locations witii 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 the sampling points of interest, ttie data will be reviewed to 

detennine if the use of intemal standards and surrogate is appropriate for the current sampling event 

Page 2 of 9 

Page 38 of 68 
GLP10-01-02; Interim Report 07 

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

Attachment A June/July 2010 

Analytical Protocol: GLP10-01-02 

Amendment 07 

PRoreKOL READS: 

No changes to the wording of the protocol are required. 

AMEND TO READ: 

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

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

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

(GLP1O-01-02). The anticipated sample collection will occur around the timeframe of June 21,2010. The 

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

as project GLP10-01-01-07 and reported as interim report GLP10-01-02-02, (reflecting study GLP10-01-

07 and amendment -07). 

/Reason: 

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

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

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

Page 3 of 9 

Page 39 of 68 
Attachment A 

GLP10-01-02; Interim Report 07 

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

June/July 2010 

Analytical Protocol: GLP10-01-02 

Amendment 07 

Amendment Approval 

^ . (€/ 

YJ 

Gary Hohenstein, SponsorRepresentative Date 

W/'77^^/ ^ 

Cleston C. Lange, Principal /^alytical Investigator Date 

/>Jt^^A^/0 

William Reagen, EHSpprts Environmental Lab Management 

Jaisimha KesarilEEfljEE, Study Director 

Date 

I I Date 

Page 4 of 9 

Page 40 of 68 
Attachment A 

GLP10-01-02; Interim Report 07 

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

June/July 2010 

AnalyUcal Protocol: GLP10-01-02 

Amendment 07 

Environmental Health & Safety Operations, Environmental Laboratory 

General Project Outline 

To: Gary Hohenstein, 3M EHS&Opns 

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

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

Cliffton Jacoby, 3M EHS&Opns; Environmentel Lab 

Jai Kesari, Weston Solutions 

Charles 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 07 - Fonner Sludge 

Incorporation Area (FSIA) Groundwater 

1 General Project Information 

Contacts 

Lab Request Number 

Six Digit Department Numi>er 

Project Schedule/Test Dates 

3M Sponsor Representative 

Gary Hohenstein 

3M EH 3 Operations 

3M Building 224-5W-03 

Saint Paul. MN 55144-1000 

Phone:(651)737-3570 

oahohenstein(a!mmm.com 

3IM Environmental Laboratory Management 

William K. Reagen 

3M EHS Opns, Environmental Laboratory 

260-5N.17 

651 733-9739 

wkreaflSD.i3>ri^mm.con3 

Principal Analytical Investigator 

Cleston Lange 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9860 

cclanqe(a!mmm.com 

Sampling Coordinator 

Timothy Frinak 

Weston Solutions 

Timothv.frinakffiwestonsolutions.com 

Phone: (334)-332-9123 

GLP10-01-02-07 

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 5 of 9 

Page 41 of 68 
GLP10-01-02; Interim Report 07 

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

Attachment A June/July 2010 

Analytical Protocol: GLP10-01-02 

Amendment 07 

2 Background Information and Project Objective(s) 

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

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

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

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

Laboratory Practice Standards 40 CFR 792. 

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

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

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

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

07. 

3 Project Schedule 

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

2010. Sample bottles will be shipped in coolers overnight to 3M Decaturfor amval on FrWay, June 18,2010. 

Sample bottles should be stored refligerated on-site unfil 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-seven sampling locations have been specified. For each sampling location, a sample, sample 

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

corresponding field sipike levels. The "fill to here" line on each 250 mL Nalgene bottie will be 200 mL. Three 

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

field spike, and a high-level tiip blank spike will be prepared at the 3M Environmentel Laboratory and sent to the 

sampling location with tiie otiier botties. Two additiianal botties will be prepared to be used for tiie preparation 

of the equipment rinseate blanks. A total of 145 sample botties will be pnepaned. 

Page 6 of 9 

Page 42 of 68 
Attachment A 

GLP10-01-02; Interim Report 07 

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

June/July 2010 Analytical Protocol: GLP10-01-02 

Amendment 07 

Table 1. Sampling Locations and Field Matrix Spike levels. 

Well No. 

136R. 137R. 137S, 137L. 

138L 

130L. 131L, 132L, 133R. 

134S, 134L, 136S 

130R.1303,131S,132R, 

132S, 133S, 133L, 135S. 

135L, 136L. 138S. 138R 

131R. 134R, 135R 

TnpBlankSet 1,2, and3 

Sample Level 

Low 

Mid 

High 

Low 

Mid 

Hiflh 

Low 

Mid 

High 

Low 

High 

Low 

Mid 

Mid-High 

High 

Spike Cone. (ng/mL) 

0.1 

1.0 

10 

1 

10 

100 

10 

100 

1000 

100 

1000 

1 

10 

100 

1000 

5 Test Methods 

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

Compounds In Water by High Perfonnance Liquid Chromat(^raphy/Mass Specbx)metry Direct Injection 

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

analytical accuracy of 100+30%, Field matrix spikes not yielding recoveries witiiin 100+30% will be addressed 

in ttie report and the 1inat accuracy statement may be adjusted accordingly. 

Alternately, samples may be analyzed by ETS 8-1 &4.3 "Detennination of Perfluorinated Acids, Alcohols, 

Amides, and SuJfonafes In Water By Solid Phase ExtracAon arid High Performance Liquid 

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

however, specific quality control samples analyzed witii ttie samples will be used to detennine overall metiiod 

predsion and accuracy. 

6 Reporting Requirements 

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

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

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

preparation will also be reported and used to evaluate tiie overall metiiod accuracy and precision. Metiiod 

blanks of reagent water prepared at ttie tirne of sample preparation will be used to detemnine ttie metiiod 

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

higher tiian expected analyte concenttations, a laboratory matiix spike may be prepared and vwll be included in 

the final report 

7 Email Correspondence 

AttadimentA: Sampling Bottie Request 

Page 7 of 9 

Page 43 of 68 
Attachment A 

GLP10-01-02; Interim Report 07 

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

June/July2010 . , . , „ , , ^ . ...^^ ^^ „ „ 

Analytical Protocol: GLP10-01-02 

Amendment 07 

Project Duration: 21 June through 2 July 2010 Date Required: 18-Jun-lO 

Ship Containers to: 

Weston Solutions, Inc. Field 

Office 

3M Decatur Plant 

1400 State Docks Road 

Decatur, Al 35S01 

256-552-6189 

Attn: Martin Smith 

Sample Media 

Groundwater 

Sample Container Requirements 

Samples 

27 

Duplicate 

Samples 

na 

Rinsate Blank 

Sets 

2 

Trip Blank Sets 

See Note 1 

Note 1: One trip blank will be required for each shipping container returned to the laboratory. It should be 

noted that ice will be required for shipments of soil / sediment samples which may result in an increase in 

the number of shipping containers (and trip blanks) required. 

Note 2: Rinsate Blank Sets should be accompanied witii an appropriate volume of water to accomplish the 

sampling. The volume should account for spillage during the rinsing process. 

Note 3: Please note that any bottle sets not used due to unique field conditions will be isolated and returned 

to the laboratory labeled for disposal. 

Page 8 of 9 

Page 44 of 68 
Attachment A 

GLP10-01-02; Interim Report 07 

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

June/July 2010 ^^^^^^ ^ ^^^^^ ^ GLP10-01-Q2 

Amendment 07 

Wells Included in This Sampling 

Event: 

Well No. 

130R 

13DS 

130L 

131R 

I31S 

131L 

132R 

1323 

132L 

133R 

133S 

133L 

134R 

134S 

134L 

135R 

135S 

135L 

136R 

136S 

136L 

137R 

137S 

1371 

138R 

1385 

138L 

Page 9 of 9 

Page 45 of 68 
'Ollie : U00110402 

Attachment B 

GLP10-01-02; Interim Report 07 

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

June/July 2010 

o100715b.rdb (PFBS): "Quadratic" Regression ("1 / x" weighting): y = -3.18e+003 x'^2 + 4.79e+005 x + 6.13e-H003 (r = 0.9997) 

2.7e7 

2.6e7 

2.5e7-] 

2.4e7 

2.3e7-

2.2e7-

2.1e7-

2.0e7 

1.9e7 

1.8e7 

1.7e7 

1.6e7-

1.5e7-

1.4e7 

1.3e7 

1.2e7 

1.1e7-

1.0e7-

9.0e6-

8.0e6 

7.0e6 

6.0e6-

5.0e6-

4.0e6-

3.0e6 

2.0e6 

1.0e6 

0.0-] 

O 

o 

/ 

X 

0 5 10 15 20 25 30 35 40 45 50 55 60 

Concentration, ng/mL 

65 70 75 80 85 90 95 100 

*Data wock-up performed by STW 

Page 1 of 1 

Printing Time: 8:40:48 AM 

Printing Date: Monday, October 25, 2010 

Page 46 of 68 
*011ie : U00110402 

Attachment B 

GLP10-01-02; Interim Report 07 

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

June/July 2010 

o100715b.rdb (PFHS): "Quadratic" Regression ("1 / x" weighting): y = -2.96e+003 x'^2 + 5.97e+005 x + 6.69e+004 (r = 0.9993) 

to 

c 

8 

OS 

1 

o.oei 

3.4e7-

3.2e7-

3.0e7-

2.8e7-

2.6e7-

2.4e7-

2.2e7-

2.0e7n 

1.8e7-

1.6e7-

1.4e7-

1.2e7-

1.0e7-

8.0e6-

6.0e6-

4.0e6-

2.0e6-

0.0-

/ 

/ 

/ 

/ 

/ 

/ 

X 

^ 

-^ 

' • 

•^_ „ .^--- ' 

o 

10 15 20 25 30 35 40 45 50 55 60 

Concentration, ng/mL 

65 70 75 80 85 90 95 100 

*Datd work-up performed by STW 

Page 1 of 1 

Printing Time: 8:41:08 AM 

Printing Date: Monday, October 25, 2010 

Page 47 of 68 
*011ie : U00110402 

Attachment B 

GLP10-01-02; Interim Report 07 

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

June/July 2010 

^^. 

0100715b PFOS linear.rdb (PFOS): "Quadratic" Regression ("1 / x" weighting): y = -2.28e+003 x'^2 + 4.74e+005 x + 5.33e+004 (r = 0.9996) 

2.8e7 

2.7e7 

2.6e7 

2.5e7 

2.4e7 

2.3e7 

2.2e7-] 

2.1e7 

2.0e7-

1.9e7-

1.8e7-

1.7e7 

1.6e7-j 

1.5e7 

1.4e7 

1.3e7H 

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 

O 

0 5 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: 8:37:45 AM 

Printing Date: Monday, October 25, 

Page 48 of 68 
*011ie : U00110402 

Attachment B 

GLP10-01-02; Interim Report 07 

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

June/July 2010 

T

San^b Narr>e: "ol00715b023- Sampte ID: "08 008-147-10" Fito: "o100715b.wir 

Peak Name: "PFBS' Macs(es): '298.9)98.9 amu,298.9/79.9 amu" 

Comment "5.0 ppb curve point in MiBI Q Vhia f Anrwtalion: " 

Sair.pl.i IiiJoj; : 2.' 

3an:j;le Typa: Stinkar d 

Cuncentraciun : f-. It) nq/mL 

•Talcuiaced Cone: 5.34 ng/mL 

Acq. DiZe: 7/15/2:' 

Acq. Tir 03 PM 

3.7e5-

3.6aS 

3.5e5 

3.4«5-

3.3e5 

3.2e5 

3.1e5 

3.0e5 

2.9e5-

2.ea5 

Z7e5 

Z6a5-

Z5e5 

Z4e5 

2.3e5' 

2.2e5 

Z1e5 

. 2-0e5 

e 1.9e5-

I 1,8e5 

1.7e5 

1.6eS 

1.5e5 

1.4*5 

1.3a5 

1.2e5 

l.leS 

1.0e5 

9.0e4 

S.0»4 

7.0e4 

6.0e4-

5.0»4 

4.0»4' 

3.0e4 

2.0e4 

1.0e4 

0.0 

1.9e5 

1.8«5 

S 

S 1.6e5 

1.5e5 

1.4«5 

n.leS 

1.0e5 

9.0*4 

8.0e4 

7.0e4 

6.0e4 

S.0e4 

4.0*4 

3.0*4 

Z0»4 

1.0e4 

*Data work-up performed by STW 

Page 1 of 4 

Printing Time: 8:40:17 AM 

Printing Date: Monday, October 25, 2010 

Page 49 of 68 
*011ie : U00110402 

Attachment B 

GLP10-01-02; Interim Report 07 

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

June/July 2010 

I

SariM* Nam*: *ol00715b060" SampI* ID: "Sotvent Blank (MBHQ Etement)" File: "o100715b.wir 

Peak Name: "PFBS" Ma««(*»): -298.9«8.9 amu,298.9^.9 amu" 

Comment'TN10-0237" Annotation:" 

2750-

2700 

2650 

2600-

2550 

2500 

2450 

2400 

2350 

2300 

2250 

2200-

2150 

2100 

2050 

2000 

! Riilati' 

.. Type: 

cps 

i rain 

tnln 

1950-

1900 

1850-

1800 

1750-

1700 

1650-

1600-

1550-

1500-

1450-

1400-

1350-

1300-

1250 

1200-

1150-

1100-

1050-

jijMi 

I

Sampte Nam*: "o100715b09r Sampte ID: •GLP10-01-01-07-070' Fil*: "olDOTISb.vi, 

Peak Name: "PFBS" Mass{es): "298.9/98.9 amu,298.9/79.9 amu' 

Comment" DAL134SQ2Y10SF0' Annotation:" 

Sample Inda^: S3 

Sample Type: Unknown 

.-Splii 

apor Larne; 

Hin. Peak Height: 

Min. Peak Width: 

jDiOQthing Width: 

Expaccad BT: 

Use Relative RT: 

I n t Typei 

2600 

2550 

2500 

2450 

2400 

2350 

2300 

2250 

2200-

2150 

2100 

2050 

2000 

1950 

1900 

1850 

1800 

1750 

1700 

1500 

1450 

1400 

1350 

1300 

1250 

1200 

1150 

1100 

1050 

1000 

950 

900 

B50-

Jto^ Mail, 

*Data work-up performed by STW 

Page 2 of 4 

Pri 

Pri 

nting Time: 8:40:18 AM 

nting Date: Monday, October 25, 2010 

Page 50 of 68 
*011ie: U00110402 

Attachment B 

GLP10-01-02; Interinn Report 07 

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

June/July 2010 

riG/tiL 

S.5 1 ng/mL 

7/lE/ZOl O 

Expe-ta d RT: 14.C m 

.T: No 

Bas e To Bas' 

: 14. 1 m 

liioZi i ciiun 

13. 9 ra 

14. 3 m 

5.7*5 

5.6*5 

5.5*5 

5,4*5 

5.3*5 

5.2*5 

5.1*5 

5.0*5 

4.9e5 

4.8*5 

4.7*5 

4.6*5 

4.5*5 

4.4*5 

4.3*5 

4.2e5 

4.1e5 

4.0e5 

3.9eS 

3.ee5 

3.7e5 

3.6e5 

3.5eS 

3.4e5 

3.3e5 

3.2e5 

3.1*5 

3.0*5 

2.9eS 

2.8*5 

2.7*5 

2.6*5 

2.5*5 

2.4*5 

2.3*5 

2.2*5 

i1* 5 

ZOeS 

1.9*5 

1.8*5 

1.7*5-

1.6*5 

1.5*5 

1.4*5 

1.3*5 

1.2*5. 

1.1*5 

1.0e5 

9.0*4 

8.0*4-

7.0*4-

6.0*4-

5.0*4-

4.0*4-

3.0*4-

2.0*4-

1.0*4-

0.0-

19.07 

7/16/201 0 

2:22:3 1 

tie 

Intflll i 

5.D 

: 1 

a k : ^ 

0 

0 

AM 

Qua 

00 

0 

. 0 0 

. 0 0 

Int . Type : 

Ratentio n Tirae: 

Area : 3 

Height : 

Star t Tin,^ : 

End TiroG: 

Base T 

30837B 

F,.^5611 

13. 

H . 

Sample Nam*: "o100715b037" Sampte ID: "LCS-100707-5" 

P*ak Name: "PFHS" Masc{e«): "398.9/98.9 amu,398.9/80.0 

Comment "5ppb LCS" Annotation: *" 

Sampl e Type : OC 

5.3B 5 

5.2B 5 

5.1 e 5 

S.OeS 

4.9*5 

4.8e5 

4.7*5 

4.6*5 

4.5*5 

4.4*5 

4.3*5 

4.2*5 

4.1*5 

4.0*5 

3.9*5 

3.8*5 

3.7*5 

3.6e5 

3.5*5 

3.4*5 

3.3*5 

3J* 5 

3.1*5-

3.0*5-

Z9*S 

2.8*5 

2.7*5-

2.6*5 

2.5*5 

2.4*5 

^3* 5 

2.2*5 

2.1*5-

Z0B5 -

1.9e5 

1.8e5 

1.7*5 

1.6e5 

I.SeS 

1.4*5 

1.3e5 

1.2e5 

1.1e5 

1.0e5 

9.0*4 

8.0*4 

7.0*4 

6.0*4 

5.0*4 

4.0*4-

3.0*4 

2.0*4 

1.0*4 

File:"o100715b.wir 

amu,398.9/129.9 amu' 

0.0 

-y^ . 

*Data work-up performed by STW 

Page 3 of 4 

Pri 

Pri 

nting Time: 8:40:18 AM 

nting Date: Monday, October 25, 2010 

Page 51 of 68 
*01iie : U00110402 

Attachment B 

GLP10-01-02; Interim Report 07 

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

June/July 2010 

r

San ^ Nama:*o100715b060' Sampte ID: "Solvent 81anlc(MiI[iQ Elam*nt)' Fite:-o100715b.Mifr 

Peak Name: -PFHS" Mass(es): "398.9/98.9 amu.398.9/80.0 amu.39S.9/129.9 amu" 

Convnent "TN10-0237" Annotation:" 

SaffipU InisK : 60 

San.pl* Type: UnKnown 

Acq. ViKB: 

ftcq. Time; 

Hodified: 

Ptoc. ftlgorithm: 

Ncis« PercTflntH'je 

Bas«. jub. Kinds 

P2st:-Split. Fact 

Rapcrr Largest P 

Min. Peak Heiglit 

Hin. Peat Vlidtli: 

:;pi";thin<] Width: 

RT Window: 

Exp«;-.t9d RT: 

Use BsUtive RT: 

Int. Type: 

Ratention Time: 

A.'.'s: 

7/16/2010 

2:11:04 PH 

No 

IntsliiQua 

: SO 

v: 1.00 

or: 5 

eak: Ho 

: 0.00 

0.00 

3 

30.0 

14.0 

No 

Base To Ba 

H . O 

4736 cou 

r

Sampte Nan«: "ol00715b09r Sampte ID; "GLP10-01-01-07-070' File: "0100715b.vi«r 

Peak Name: "PFHS" Mass<es): "398.9/98.9 amu.398.9/80.0 amu,398.9/129.9 amu' 

Comment "DAL 134SQ2Y10 SFO- AnnotatJon:"-

Saiaple Typa: Unknown 

C-jncnntiation : N/A 

Calculata d Core : 1.37 nq/r,L 

Acq. Pate : 7/17/2010 

Acq. Time: 1:45: 11 AM 

Modified: 

Proc. Alaorithn,: ] 

Noise Percentage: 

Base. Jub. Window: 

Peak-Split. Factor 

Report Larnast Pea 

Min. Peak Height: 

Min. Peak Width; 

Smoothiri'] Width: 

RT Window: 

Expected RT: 

Use Relativd BT! 

Int. Type: B 

Retention Tittie: 

Ho 

ntelliQ'jan - MQII 

?0 

1.00 min 

(: No 

0.00 cps 

0-00 sec 

3 p:.in 

30.0 sec 

14.0 rain 

No 

ase T= Base 

14.0 isin 

Area: 230553 counts 

H-tight: 

Start Time: 

End Tina: 

32769 cps 

13.6 rain 

14.2 rain 

3.3*4 

3.2*4 

3.1*4 

3.0*4 

Z9e4 

2.8*4 

Z7*4 

2.6*4 

2.5*4 

2.4*4 

2.3*4 

2.2e4 

2.1*4 

2.0*4 

1.9*4 

1.8*4 

1.7e4 

V.6e4 

1.5*4 

1.4*4 

1.3*4 

1.2e4 

1.1B4 

1.0e4 

9000.0 

8000.0 

7000.0 

6000.0 

5000.0 

4000.0 

3000.0 

2000.0 

1000.0 

n o 

13 

13.76v^ 

^_M--v ^ 

.97 

16.6f 

\ J ^ 

19.18 

i 

18.B6J 

f 

I8.59J 

18.36.^1 

18.08.-/ 

^ 

12 14 16 18 

*Data work-up performed by STW 

Page 4 of 4 

Printin g Time: 8:40:1 8 AM 

Printin g Date : Monday, Octobe r 25, 2010 

Page 52 of 68 
*011ie : U00110402 

Attachment B 

GLP10-01-02; Interim Report 07 

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

June/July 2010 

Sample Nam*:-01007151)023" Sampla ID: t)B 008-147-10- Fito:-o100715b.wr 

• Peak Nama:-PFOS- Mass(a8):-499.1Sa.9amu.499.1/79.9arnu.499.1/130.0arT«j' 

a Carranant: -5.0 ppb curva paint in Mini Q Watar- Annotalion: 

SampU InJa>:: 2 i 

*Data work-up performed by STW 

Page 1 of 3 

Printing Time: 8:36:45 AM 

Printing Date: Monday, October 25, 2010 

Page 53 of 68 
*011ie: U00110402 

Attachment B 

GLP10-01-02; Interim Report 07 

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

June/July 2010 

I SaiTiptoName:"ol00715M5(r Sample ID: "LCS-100707-14- Fito: •ol00715b.wfr 

I Peak Name: "PFOS- Massfes):'499.1^98.9 a j,499.1^79.9amu.499.1/13O.0amir 

I Camment "Sppb LCS ECF' Annotation: " 

Sample Index: 50 

Sampi« Type: OC 

Ccncenttatioii: 5.00 ng/al 

Calculated Cone: 3.70 ng/n.L 

Acq, r^te : 7/16/2010 

Acq. Time: 5:56:00 WI 

Modified: 

RT Window: 

Expected RT: 

Use Relative 

Int. Type: 

Retention Ti 

Area: 

Height: 

Start Time: 

End Time: 

Yf-s 

30.000 

1?.395 

RT: No 

Manual 

la: 15.J 

n752S0 

JJ8il5.l} 

15.3 

15.f 

3.2e5 

3.1 e5 

3.0e5 

2.9B5 

2.ee5 

2.7e5 

2.6e5 

2.5e5 

2.4e5 

2.3e5 

2.2B5 

2.1e5 

2.0e5 

1.9eS 

1.8e5 

1.7e5 

1.6e5 

1.5e5 

1.4e5 

1.3e5 

1.2e5 

l.leS 

1.0e5 

9.0e4 

8.0e4 

7.0e4 

6.0e4 

5.0e4 

4.0e4 

3.0e4' 

2.0e4 

1.0e4 

i ; 

15.12... 

.35 

I

San ^ Name: -o100715b060" Sample ID: "Solvent Blank (MiOiQ Elementr File: -o10071Sb.wtr 

Peak Name: "PFOS* Mass(es): '499.1/98.9 amu.499.1/79.9 amu.499.1/130.0 afTuT 

Comment *TN1tM237" Annotation:"" 

Hodified: 

RT Kindov: 

Expected RT: 

Use Relative RT 

Int. Type: 

Retention Tirae: 

;;rea: 

H-ight: 

Start Time: 

Yes 

30.000 

15.353 

th: 

Manual 

Ib.t 

42201 

?319.9&0 

15.3 

*DaCa work-up performed by STW 

Page 2 of 3 

Printing Time: 8:36:45 AM 

Printing Date: Monday, October 25, 2010 

Page 54 of 68 
GLP10-01-02; Interim Report 07 

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

June/July 2010 

Printing Time: 8:36:45 AM 

Printing Date: Monday, October 25, 2010 

Page 55 of 68 

*011ie : U00110402 

Attachment B 

San^le Name: "ol00715b093- Sampte ID: -GLP1[>01-01-07-070r File: "o100715b.wir 

•

Peak Name: -PFOS' Mass(es): -499.1/98.9 amu.499.1/79.9 amu.499.V130.0 amu" 

Comment 'DM . 134S 0 2 YIO SF 0" Annotation: ~ 

Samplfl 

impla Typo: 

RT WindO! 

Expected 

Use RflU 

Unl-.i 

N/A 1.16eS 

1.14e5 

1.12a5 

1.10e5-

1.08e5-

1.06e5 

1.04e5 

1.02e5 

I.OOeS 

9.80e4 

9.60e4 

S.40e4 

9.20e4 

9.00e4 

8.80D4 

8.60e4 

8.40e4 

S.20e4 

8.00e4 

7.S0e4 

7.60e4 

7.40e4 

7.20e4 

7.00e4 

6.80e4 

6.60*4-

6.40»4 

6.20e4 

8- 6.00»4< 

'i 5.80e4 

-I 5.60e4 

5.40e4 

5J20e4-

5.00O4 

4.80e4 

4.60e4 

4.40e4 

4.20e4 

4.00e4 

3.80e4 

3.60e4 

3.40e4 

3.20e4 

3.00e4 

2.60e4 

2.60e4 

2.40e4 

2.20e4 

2.00e4 

1.B0e4 

1.60*4 

1.40e4 

1.20e4 

LOO M 

8000.00 

6000.00 

4000.00 

2000.00 

0.00 

*Data work-up performed by STW 

Page 3 of 3 
•Ollie: U00110402 

Attachment B 

GLP10-01-02; Interim Report 07 

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

June/July 2010 

IT Sanvle Name: "o100715b050" Sample ID: "LCS-100707-14" FUe: -o100715b.'Mfr 

Peak Name: 'PFOS* Massfes): '499.1/98.9 amu,499.1/79.9 amu.499.1/130.0 emu* 

Comment '5ppb LCS ECF" Annotation: ~ 

50 

Sample Type: OC 

Concentration: i.OO r.-j/nL 

Calculated Cone: 1.91 ng/mL 

Acq. rate : 7/16/2010 

Acq. Time: 5:56:00 AM 

180216 cO'Ji 

lJ2e9S.475 

H.9 r 

Hodi f 

RT Wi 

E^pe^ 

Usa R 

Int. 

Reten 

Area: 

Heigt 

i e 

nd 

t e 

*1 

TV 

t : 

^ 

f 

3.2e5 

3.1 eS 

3.0eS 

2.9e5 

2.8e5 

2.7eS 

2.6e5 

2.5e5 

2.4e5 

2.3e5 

2.2e5 

2.1*5 

2.0e5 

1.9e5 

1.8«S 

1.7e5 

1.6e5 

1.5e5 

1.4e5 

1.3e5 

1.2e5 

l.leS 

I.OeS 

9.0*4 

8.0e4 

7.064 

6.064 

5.0«4 

4.0e4 

3.0*4 

2.0*4 

1,0e4 

15 

15.12.^ 

14.93.. 

35 

Sample Name: "o100715b09r Sample ID: •GLP1(W]1-01-07-O70' File:"o100715b.wiff' 

Peak Name: 'PFOS* Massfes): '499.1/98.9 amu.499.1/79.9 anui,499.1/13D.0 amu" 

Comment 'DAL 134S 0 2 Y10 SF 0" Annotalion:" 

Sample 

Sample Typo: Unkr 

N/A 

Hodirifd: 

RT Window 

Exparted 

Uaa Relat 

Int. Type 

Retention 

J53HS count s 

102609.7SB cps 

l.lSeS 

1.14«5-

1.12e5 

1.10e5-

1,08e5 

1.06e5 

1.04*5 

1.02e5 

1.00*5 

9.80*4 

9.60*4 

9.40e4 

9.20*4 

9.00*4 

8.80e4 

8.6064-

8.40*4 

8.2064 

e.00e4 

7.8064 

7.60e4 

7.40*4 

7.20*4 

7.00*4 

6.80*4 

6.60*4 

6.40*4 

6.20*4 

& 6.00*4 

^ 5.80*4 

I 5.60e4 

5.40*4 

5.20*4 

5.00*4 

4.80*4 

4.60*4 

4.40e4-

4.20*4 

4.00*4 

3.80*4 

3.60*4 

3.40*4 

3.20*4 

3.00*4 

2.80*4 

Z60*4 

2.40*4 

2.20*4 

2.00*4 

1.80*4 

1.60*4-

1.40*4 

1.20*4 

1.00*4-

8000.00 

6000.00 

4000.00 

2000.00 

0.00 

*Data work-up performed by STW 

Page 1 of 1 

Printing Time: 8:38:56 AM 

Printing Date: Monday, October 25, 2 010 

Page 56 of 68 
DocKBiii(ft*0ifjiPo;!rjfitfewnKgi$3ii.o5f current, for 14 days from 10/25/2010 

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

Attachment C June/July 2010 

3M Emronmenfal L^iorafioiy 

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 (^^f^ ^ ^ j 

Approved By: 

^/-j/ a •> 

William K. Reagen, Laboratory Manager Date 

ETS-8-044.0 Page 1 of 11 

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

Injection Analysis Page 57 of 68 
Doci®:im«K.i!)ioQ;!rjm'grtniE®rMl,oW current, for 14 days from 10/25/2010 

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

Attachment C 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 "Determination of 

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

Performance Liquid Chromatography/Mass Spectrometry". 

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

defined QC elements are satisfied. 

Sample collection is not covered under this analytical procedure. 

2 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 performance-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 detemnined using field matrix spikes to verify that the method is applicable to 

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

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

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

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

accuracy for analytical results. 

3 Definitions 

3.1 Calibration Standard 

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

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

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

concentration. 

3.2 Laboratory Duplicate Sample (LDS, or Lab Dup) 

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

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

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

preservation, or storage procedures. 

3.3 Field Blank (FB)/Trip Blank 

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

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

preservation and all analytical procedures. The purpose of the FB is to determine 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 58 of 68 
Doc«EC)P3!(«tj-ra2ijMbcmiE®i«:'ct.oM'current, for 14 days from 10/25/2010 

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

Attachment C 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 determine whether the method is in control. LCSs should be prepared 

each day samples are extracted. 

3.8 Laboratory Matrix Spike (LMS) 

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

in the laboratory. The LMS is analyzed exactly like a laboratory sample to detennine 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 59 of 68 
Doci®mwt)-H}3"j«fesnifi??!|fcii,olf current, for 14 days from 10/26/2010 

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

Attachment C 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 nonnally 

found in the sample(s). A sunogate 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 deteimined; 

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 work environment and a current awareness of local 

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

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

4.2 Cautions 

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

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

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

5 Interferences 

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

glassware. All materials used in the analyses shall be demonstrated to be free from intert^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 60 of 68 
Attachment 0 

)oci«ra:wi!)iR03MMWmKi!rToM,o'?f current, for 14 days from 10/25/2010 

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

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

(LC/MS/MS). I 

Analytical balance capable of reading to 0.0001 g 

A device to collect raw data for peak integration and quantitation 

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

Gas tight syringes, 25pL, 50pL, 100(JL, 250|JL, 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 flt, 1/x weighted. 

Run Time: ~ 17 minutes. 

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

provided that data quality objectives are met. 

ETS-8-044.0 Page 5 of 11 

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

Injection Analysis 

Page 61 of 68 
Attachment 0 

Docmsmmbwzi'pkmmimy!^ 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, altemate instalments and equipment may be used. 

7 Reagents and Standards 

7.1 Chemicals 

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

Methanol - HPLC grade 

Ammonium Acetate -A.C.S. Reagent Grade 

7.2 Standards 

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

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

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

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

Products, Inc 

Perfluorooctanoic Acid (PFOA - C8 acid); 3M 

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

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

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

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

Perfluorobutanesulfonate (PFBS - C4 sulfonate); 3M 

Perfluorohexanesulfonate (PFHS - C6 sulfonate); 3M 

Perfluorooctanesulfonate (PFOS - C8 sulfonate); 3M 

ETS-8-044.0 Page 6 of 11 

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

Analysis 

Page 62 of 68 
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Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

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

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

^. , ^ molecular weight of anion 

salt correction factor = 

moclecular weight of salt 

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

538 

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

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

fiask and bring up to volume with solvent. 

250 ng/mL mixed woricing 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 worthing 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 63 of 68 
Attachment C 

DocL(SB:vRst5if)iqo3'jhtteirmiBi8^#ioW current, for 14 days from 10/25/2010 

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 worthing standards may 

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

than those listed below can be prepared as needed. 

Concentration 

of WS, ng/mL 

125 

125 

125 

125 

250 

250 

250 

250 

5000 

5000 

5000 

Volume of WS, fd. 

10 

15 

20 

30 

20 

50 

100 

200 

25 

50 

100 

Final Volume of 

Calibration Standard (mL 

of ASTM Type 1 Water, or 

other suitable water) 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

Final Concentration of 

Calibration Standard, ng/mL 

(ppb) in ASTIVI Type 1 Water, 

or other suitable water 

0,025 

0.0375 

0.050 

0.075 

0.100 

0.250 

0.500 

1.00 

2.50 

5.00 

10.0 

8 Sample Handling 

8.1 Water Sample Preparation 

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

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

sample aliquot, or filtered. 

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

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 fli (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 

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

Attachment C 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 cun/e. Analyze a 

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

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

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

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

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

curve should be further diluted and reanalyzed. 

10 Quality Control 

10.1 Data Quality Objectives 

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

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

the raw data and footnoted in the final report. 

10.2 Method Blanks 

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

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

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

CCV samples, and at the end of the analytical 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 

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

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

10.3 Sample Replicates 

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

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

replicates excludes field blanks. 

10.4 Surrogate Spikes 

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

10.5 Lab Control Sample 

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

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

targeted LOQ and high lab control spikes should be prepared at concentrations near the mid-point 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 65 of 68 
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Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

Attachment C June/July 2010 

10.6 Field Matrix Spikes / Lab Matrix Spikes 

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

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

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

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

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

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

11 Data Analysis and Calculations 

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

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

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

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

Slope 

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

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

percent recovery. 

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

Analyte added (ng/mL) 

12 Method Performance 

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

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 performed on the system and 

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

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

discussed in the text of the report. 

12.1 System Suitability 

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

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

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

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

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

12.2 Quantitation 

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

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

the LLOQ, which may be within ±30%. 

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

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

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

bracketed by CCVs not meeting these criteria must be reanalyzed. 

ETS-8-044.0 Page 10 of 11 

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

Analysis 

Page 66 of 68 
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Analysis of PFBS, PFHS, and PFOS in Water Samples from Decatur, AL 

Attachment C 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 speciflc 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 performing this method will be disposed of appropriately. The original samples will be 

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

14 Records 

Each data package generated for a study must include all supporting infonnation for reconstmction 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, instrument acquisition 

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

15 Affected Documents 

None. 

16 Revisions 

Revision 

Number Summarv of Changes 

ETS-8-044.0 Page 11 of 11 

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

Analysis 

Page 67 of 68 
SMcffM^ntial 

GLP10-01-02; Interim Report 07 

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

June/July 2010 

RECORD OF DEVIATION/NONCONFORMANCE 

/. Identification 

Study / Project No. 

GLP10-01-02-07 

Date(s) of Occurrence: 

0100715b and ml 00917a 

Document Number: 

ETS-8-044.0 

Deviation type D SOP D Equipment Procedure 13 Method 

(Ciieclf one) D Protocol B GPO D Other: 

//. Description (attach extra pages as needed) 

M9^h9AB'^'^\''^JPTf}^D^^l 

(1) CCV recovery within 100% ± 25%. 

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

(3) Sample/Sample Duplicate RPD S20%. 

(4) FMS recovery of 100% ± 30%. 

Actual procedure/process: 

(1) 

(2) 

(3) 

(4) 

Twenty-one CCVs were analyzed during the course of the run with three CCVs not meeting method 

acceptance criteria with recoveries of 70.8%, 73.6%, and 73.3% for PFHS (o100715b). 

LGS average recovery for the high set of linear and branched PFOS was 122% (s100715b). LCS 

average recovery for the low set of linear PFOS was 121% and 125% for the low set of linear and 

branched PFOS (m100917a). 

The RPD value for PFBS for 138L was 27%. 

The following locations did not have an appropriate FMS level for PFOS: DAL 132L and DAL 134L. The 

following FMS level did not meet method acceptance criteria: the high FMS for PFOS on DAL 130L 

(54.8%), the mid FMS for PFOS DAL 135L (68.2%), the mid FMS for PFOS on DAL 136L (65.6%), the 

low FMS for PFHS on DAL 137S (149%), the low FMS for PFHS on DAL 137S (186%), the mid FMS for 

PFOS on DAL 137S (61.5%), and the low FMS for PFHS on DAL 138L (203%). 

///. Actions Taken 

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

Corrective Action (D Yes 0 No) Reference: 

Acceptability of the nonconforming work: 

1) 

2) 

3) 

4) 

Reported samples bracketed by the three CCVs for PFHS that did not meet method acceptance criteria 

(132S, 134R, 135S, and 135L) will be noted in the final report. 

The 9/17/10 analysis included a number of samples that contained PFOS concentrations greater than 

the calibration range. It is believed that the high recovery for the low set of LCS is due to analyte carryover as the low set of LCS were analyzed immediately these samples. 

The RPD value for PFBS for 138L with a value >20% will be footnoted in the data tables. 

Sampling locations without an appropriate spike level for PFOS will be footnoted in the final report (DAL 

132L and DAL 134L). Sampling locations DAL 135L and 136L had FMS recoveries for PFOS that did 

not meet method acceptance criteria (68.2% and 65.6%), however, since the method analytical 

uncertainty for PFOS is 100% ± 37%, no adjustment was made to the analytical uncertainty. Sampling 

locations DAL 137L, DAL 137S, and DAL 138L had high recoveries for the low FMS for PFHS, however, 

the samples contained PFHS just below the method LOQ of 0.103 ng/mL, which most likely accounts for 

the high recovery of the low FMS samples. The mid and high FMS levels for these sampling locations 

met method acceptance criteria. For sampling locations DAL 130L and DAL 137S, the analytical 

unc^rtairity will be adj^u^^^ on the recovery of the most appropriate spike level. 

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

0 Other: Deviations will be noted in fiopi report. 

Project Lead/PAI Approval: 

Study Director (FGLP)^ 

Sponsor Approval (for GLP^rotocol deviations): NA Date: NA 

Technical Reviewer (optional): NA ! Date: NA 

Laboratory Department Manager Approval: 1 Date: 

IV. Authorization to Resume Work 

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

Laboratory Department Manager Approval: NA Date: NA 

Deviation No. 

Attachment A 

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

ETS-4-008.7 Page 1 of 1 

Documentation of Deviations and Control of Nonconforming Testinc, ^^^^ ^® °^ ^^