GLP10-01-02; Interim Report 02 

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

March/April 2010 

3M 

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

Ground Water Samples Collected from Decatur. AL in March/April 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, Bldg 260-05-N-17 

Maplewood, MN 55144 

Project Identification 

GLPl 0-01-02-02 

Total Number of Pages 

57 

lACCREDITEDJ The testing reported herein meet the requirements of ANS/1S0/IEC17025:2005 "General Requirements for the 

Competence of Testing and Calibration Laboratories", In accordance with the A2LA Certificate #2052-01. 

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

Certificate #2052-01 

Page 1 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

This page has been reserved for specific country requirements. 

Page 2 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

GLP COMPLIANCE STATEMENT 

Report Title: Interim Report 02 Analysis of PFBS, PFHS, and PFOS in Ground Water Samples 

Collected at Decatur, AL in March/April 2010 

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

Perfluorobutane sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 SiteRelated Monitoring Program. 

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

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

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

system and no dosing of a test system. 

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

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

Gary Honensteih, Sponsor Representative Date 

\ 

QZkhkl^ 

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

Page 3 of 57 
GLP10-01-02; Interim Report 02 

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

iWarch/April 2010 

QUALITY ASSURANCE STATEMENT 

Report Title: Interim Report 02 Analysis of PFBS, PFHS, and PFOS in Ground Water Samples 

Collected at Decatur, AL in March/April 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 

3/3/10 

3/25/10 

6/3/10-6/4/10 

Phase 

Protocol 

In-Phase Audit - Bottle 

Order Prep 

Interim Report 02 

Data and Report 

Date Reported to 

Testing Facility 

•Management 

3/16/10 

4/5/10 

6/11/10 

Study Director 

3/16/10 

4/5/10 

6/11/10 

y 

(,-^"7^0 

QAU Represeirative Date 

Page 4 of 57 
GLP10-01-02; Interim Report 02 

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

iVIarch/April 2010 

TABLE OF CONTENTS 

GLP Compliance statement 3 

Quality Assurance Statement 4 

Table of Contents 5 

List of Tables 6 

1 Study Infomnation 8 

2 Summary 9 

3 Introduction 10 

4 Test & Control Substances 11 

5 Reference Substances 12 

6 Test System 14 

7 Method Summary 14 

7.1 Methods 14 

7.2 Sample Collection 14 

7.3 Sample Preparation 14 

7.4 Analysis 14 

8 Analytical Results 16 

8.1 Calibration 16 

8.2 System Suitability 16 

8.3 Limit of Quantitation (LOQ) 16 

8.4 Continuing Calibration 16 

8.5 Blanks 16 

8.6 Lab Control Spikes (LCSs) 17 

8.7 Analytical Method Uncertainty 19 

8.9 Field Matrix Spikes (FMS) 20 

9 Data Summary and Discussion 20 

Page 5 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

10 Conclusion 31 

11 Data/Sample Retention 31 

12 Attachments 31 

13 Signatures 32 

LIST OF TABLES 

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

March/April 2010) 10 

Table 2. Instmment Parameters 15 

Table 3. Liquid Chromatography Conditions 15 

Table 4. Mass Transitions 15 

Table 5. Limit of Quantitation (LOQ) 16 

Table 6. Laboratory Control Spike Recovery 18 

Table 6 continued. Laboratory Control Spike Recovery 19 

Table 7. Analytical Uncertainty 19 

Table8. GW203LQ1 Y10LF 21 

Table9. GW220RQ1 Y10LF 21 

Table 10. GW220LQ1 Y10 LF 22 

Table 11. GW222RQ1 Y10LF 22 

Table 12. GW227LQ1 Y10 LF 23 

Table 13. GW227RQ1 Y10 LF 23 

Table 14. GWGRS04Y10LF 24 

Table 15. GW310RQ1 Y10CP 25 

Table 16. GW312RQ1 Y10 CP 25 

Table 17. GW317LQ1 Y10CP 26 

Table 18. GW324LQ1 Y10CP 26 

Table 19. GW327RQ1 Y10CP 27 

Table 20. GW328LQ1 Y10CP 27 

Page 6 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

Table 21. GW328RQ1 Y10CP 28 

Table 22. GW 330LQ1 YI 0 CP 28 

Table23. GW330RQ1 Y10CP 28 

Table24. GW331SQ1 Y10CP 29 

Table 25. Trip Blank 29 

Table 26. Rinseate Blanks 30 

Page 7 of 57 
GLP10-01-02; Interim Report 02 

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

March/Aprii 2010 

Sponsor 

3M Company 

Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

Study Director 

Jaisimha Kesari, P.E., DEE 

Weston Solutions, Inc. 

Westchester, PA 19380 

Phone:(610)701-3761 

Fax:(610)701-7401 

j.kesari@westonsolutions.com 

Study Location 

Testing Facility 

3M EHS Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55106 

Study Personnel 

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

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

Susan Wolf, 3M Analyst 

Jonathan Steege; analyst 

Study Dates 

Study Initiation: March 8,2010 

Interim #2 Sample Collection: March 30,2010-April 14,2010 

Interim #2 Experimental Termination: May 26, 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 57 
GLP10-01-02; Interim Report 02 

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

Marcli/April2010 

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

representing 17 different sampling locations. A total of ninety-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 firom each 

sampling location. Samples also included low, mid and high field matrix spike (FMS) samples for each 

location, one trip blank containing Milli-QTM water and appropriate trip blank spikes, and five equipment 

rinseates. Two additional soil-equipment rinseates that were collected as part of project GLPl 0-01-02-

01 for analysis of PFBS, PFHS, and PFOS in soils collected from the fomner sludge incorporation area 

(FSIA) fields at the Decatur site in March/April 2010, were also included in this analysis. The 

equipment rinseate blanks did not have FMS samples prepared for detemriination of PFBS, PFHS or 

PFOS recovery. All groundwater samples for this project were logged under GLPl 0-01 -01 -02. 

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

personnel on April 15, 2010. The soil-equipment rinseate blanks were received with the FSIA soil 

shipment on April 01,2010. 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-10-01-02-02. Many of the groundwater samples required dilution to attain PFBS, PFHS, and 

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

required. The average measured PFBS, PFHS, and PFOS concentrations 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 groundwaters ranged over four orders of magnitude from 0.534 ng/mL to 

4470 ng/mL. The PFHS concentration results for all groundwaters ranged over four orders of 

magnitude from 0.691 ng/mL to 6190 ng/mL. The PFOS concentration results for all groundwaters 

ranged over three orders of magnitude from 2.44 ng/mL to 1750 ng/mL. 

Page 9 of 57 
GLP10-01-02; Interim Report 02 

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

IVIarch/April 2010 

Table 1. Summarized PFBS, PFHS, and PFOS Results (Decatur Groundwater, March/April 

2010). 

Sampling Location 

GW203LQ1 Y10 LF 

GW220RQ1 Y10 LF 

GW220LQ1 Y10 LF 

GW222RQ1 Y10 LF 

GW227LQ1 Y10 LF 

GW227RQ1 Y10 LF 

GWGRS04Q1 Y10 LF 

GW310RQ1 Y10 CP 

GW312RQ1 Y10 CP 

GW317LQ1 Y10 CP 

GW324LQ1 Y10 CP 

GW327RQ1 Y10 CP 

GW328LQ1 Y10 CP 

GW328RQ1 Y10 CP 

GW330LQ1 Y10 CP 

GW330RQ1 Y10 CP 

GW331SQ1 Y10 CP 

Trip Blank (Milli-QTM Water) 

Equipment Rinseate Blanks 1 to 5, 203L 

DAL DF05 SS07 2 0010 (soil equipment 

rinseate blank) 

DAL DFl 1 SS07 2 0010 (soil equipment 

rinseate blank) 

PFBS 

Avg. Conc. 

(ng/mL) ± RPD 

61.9 ±3.4% 

7.46 ± 3.5% 

11.1 ±13% 

129 ±3.9% 

342±4.1% 

23.8± 6.7% 

1930 ±13% 

386 ± 8.0% 

1220 ±0.0% 

0.534 ± 0.94% 

95.7 ± 2.8% 

75.8 ± 14% 

76.8 ±1.6% 

36.0 ±1.9% 

504 ± 6.0% 

4470 ± 2.5%<^' 

349 ±13% 

<0.0255 

<0.0255 

<0.0255 

<0.0255 

PFHS 

Avg. Conc. 

(ng/mL) ± RPD 

360 ± 0.83% 

32.0 ± 0.63% 

53.0 ± 4.9% 

845 ±1.3% 

63.7 ± 4.7% 

169 ±0.0% 

6190±9.0%<^> 

424 ± 5.4% 

946 ± 0.74% 

0.691 ± 0.72% 

101 ±5.6% 

154 ±2.6% 

25.9 ±1.2% 

67.7 ± 6.7% 

403 ±1.2% 

258 ± 5.0% 

426 ±13% 

<0.0258 

<0.0258 

<0.0258 

<0.0258 

PFOS 

Avg. Conc. 

(ng/mL) ± RPD 

852 ±1.1% 

46.0 ±12% 

63.6 ± 3.8% 

974 ± 4.7% 

287 ±13% 

956 ± 7.4% 

1400 ±16% 

760 ± 5.4% 

1750 ±4.6% 

2.44 ± 3.7% 

203 ±11% 

639 ±18% 

14.5 ± 0.69% 

146 ± 19% 

145 ± 14% 

759 ±1.1% 

922±21%<^' 

<0.510 

<0.510 

<0.510 

<0.510 

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

and PFOS 100% ±44%. 

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

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

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 

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

Page 10 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

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

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

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

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

aqueous soil-equipment rinseate samples collected as part of the PFBS, PFHS, and PFOS 

assessment in soils from former sludge incorporation area (FSIA) fields at the Decatur site in 

March/April 2010, were also analyzed. 

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

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

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

spike samples. Each empty container was mari<ed with a "fill to here" line to produce a final sample 

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

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

the field for sample collection. All sample bottles included the addition of O2-PFBS, ^®02-PFHS, and 

^^Cg-PFOS (intemal standards) at a nominal concentration of 1 ng/mL. All sample bottles also 

included the addition of ^^C4-PF0S (surrogate spike) at a nominal concentration of 0.1 ng/mL. 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, similar to soil sample bottles (see GLP10-01-

02 Interim Report 01 for details). 

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

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

Perfomnance 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 8-26 

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 

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 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

Reference Substance 

Chemical Name 

Chemical Fonnula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

1 TCR Number 

Physical Description 

Purity 

PFBS 

Perfluorobutane sulfonate 

C4F9SO3" 

Potassium Salt 

3M 

1/10/2017 

Frozen 

41-2600-8442-5 

TCR-121 

White Powder 

1 96.7% 

PFHS 

(linear) 

Perfluorohexane sulfonate 

C6F13SO3" 

Sodium Salt 

Wellington 

4/2/2013 

Frozen 

LPFHxSAMOS | 

TCR08^018 1 

Crystalline 

98% 1 

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 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

Reference Substance 

Chemical Name 

Chemical Formula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

1 TCR Number 

Physical Description 

1 Purity 

^^OrPFBS 1 

Labeled - Perfluorobutane 

sulfonate 

C4F9S[^^02]0' 

Ammonium Salt 

RTI Intemational 

3/9/2015 

Frozen 

11546-107-2 

TCR-1013 

Liquid 

99% 

"OrPFHS 

Labeled - Perfluorohexane 1 

sulfonate 

C6Fi3S[''02]^®0' 

Sodium Salt | 

Wellington 

7/24/2011 1 

Frozen 

MPFHXA0706 | 

TCR-1218 

Liquid 

98% 1 

Reference Substance 

Chemical Name 

Chemical Formula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

1 TCR Number 

Physical Description 

1 Purity 

"C^PFOS 

Perfluorooctane sulfonate 

^^C;^C4Fi7S03 

1 Sodium Salt 

Wellington 

1 8/18/2011 

Frozen 

1 MPFPS0808 

1 TCR08-0043 

Liquid 

1 98% 

"CtfJ»FOS 

Perfluorooctane sulfonate 

''C8F17SO3 

1 Sodium Salt 

Wellington 

1 6/17/2012 

Frozen 

1 M8PFOS0609 

1 TCR09-0049 

Liquid 

1 98% 

Page 13 of 57 
GLPl 0-01-02; Interim Report 02 

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

March/April 2010 

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

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

specific lot of test substance. 

Sample Description Key Code. 

string Numljer 

Example 

1 

2 

3 

4 

String Descriptor 

GW277L Ql Y10 LFO 

Sample Type 

Sample Location 

Well Level 

Sampling Date 

Sample Type 

Example 

GW= Ground Water 

Example: 227LLF 

R = Residum shallow water-bearing zone 

L = Bedrock water-bearing zone 

S = Epikarst middle water-bearing zone 

Q1Y10-1st Quarter, 2010 

0=primary sample 

1=duplicate sample 

LS = low spike 

MS = mid spike 

HS = high spike 

7.1 Methods 

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

"Detemiination of Perfluorinated Compounds In Water by High Perfonnance Liquid 

Chromatography/Mass Spectrometry Direct Injection Analysis". 

7.2 Sample Collection 

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

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

15, 2010 Samples were stored refi-igerated 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 1 mL sample with 9 mLs of Mill! Q water 

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

additional Milli Q water. 

7.4 Analysi s 

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

peri'omnance liquid chromatography/ tandem mass spectrometry (HPLC/MS/MS). Detailed instrument 

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

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

Page 14 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

Table 2. Instrument Parameters. 

Instrument Name 

Analytical Method Followed 

Analysis Date 

Liquid Chromatograph 

Guard column 

Analytical column 

Injection Volume 

Mass Spectrometer 

ion Source 

Electrode 

Polarlly 

Software 

ETS Ginger 

ETS-8-044.0 

5/17/2010 and 5/26/2010 

Agilent 1100 

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

Betasil C18 (2.1 mmX 100 mm), 5n 

2,5,or10tiL 

Applied Biosystems API 5000 

Tuttjo Spray 

Turbo ion electrode 

Negative 

Analyst 1.4.2 

Table 3. Liquid Cliromatography Conditions. 

step 

Number 

0 

1 

2 

3 

4 

5 

Total Time 

(min) 

0 

1.0 

11.0 

13.5 

14.0 

17.0 

Flow Rate 

(fdJmin) 

300 

300 

300 

300 

300 

300 

PercenM 

(2 mM ammonium acetate) 

97.0 

97.0 

5.0 

5.0 

97.0 

97.0 

PercentB 

(Methanol) 

3.0 

3.0 

95.0 

95.0 

3.0 

3.0 

Table 4. Mass Transitions. 

/inalyte 

PFBS 

PFHS 

PFOS 

Mass Transition 

Q1/Q3 

299/80 

299/99 

299/130 

399/80 

399/99 

399/130 

499/80 

499/99 

499/130 

Dwell time was 50 msec for each transition. 

The individual transitions were summed to 

produce a "total ion chromatogram" (TIC), 

w/hich was used for guantitation. 

Page 15 of 57 
GLPl 0-01-02; Interim Report 02 

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

March/April 2010 

8.1 Calibration 

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

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

Milli Q water. A total of thirteen spiked standards ranging from 0.025 ng/mL to 50 ng/mL (nominal) were 

analyzed. Low curve points were disabled for PFOS to meet method blank criteria. A quadratic, 1/x 

weighted, calibration curve of the peak area counts was used to fit the data for each analyte. The data 

were not forced through zero during the fitting process. Calculating the standard concentrations using 

the peak area confimned accuracy of each curve point. 

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

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

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

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

PFBS, PFHS, and PFOS were not used during instrument calibration. 

8.2 System Suitability 

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

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

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

met for PFBS, PFHS, and PFOS. 

8.3 Limit of Quantitation (LOQ) 

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

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

blanks. The nominal LOQ for all analytes can be found in Table 4. 

Table 5. Limit of Quantitation (LOQ). 

Analysis Date 

5/17/10 

5/26/10 

Dilution 

1 

10 

100 

200 

PFBS 

LOQ, ng/mL 

0.0255 

0.255 

2.55 

NA 

PFHS 

LOQ, ng/mL 

0.0258 

0.258 

2.58 

51.6 

PFOS 

LOQ, ng/mL 

0.510 

5.10 

51.0 

NA 

8.4 Continuing Calibration 

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

analyzed to confimri that the instalment response and the initial calibration curve were still in control. All 

CCVs met method criteria of 100% ± 25%. 

8.5 Blanl(s 

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 perfonnance and to determine the 

LOQ for each analyte 

Page 16 of 57 
GLP10-01-02; Interim Report 02 

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

iVIarcli/April 2010 

8.6 Lab Control Spiltes (LCSs) 

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

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

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

analyzed in the same manner as the samples. Due to the analytical reporting limit, the low set of linear 

PFOS LCS samples could not be quantitated. The method acceptance criteria, average of LCS at 

each level should be within 100% ± 20% with an RSD <20%, were met for the PFBS, PFHS, and linear 

PFOS LCS 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. Due to the analytical reporting limit, the low set of LCS could not be quantitated. The LCS at the 

mid level met method acceptance criteria, while the high level did not meet method acceptance criteria 

with an average recovery of 172%. An additonal set of mid, mid-high, and high-level LCS, prepared on 

a different date with other samples, were analyzed at the end of the analytical run to confirm the 

recovery of the high-level LCS. The analysis of these samples produced acceptable recoveries for the 

mid and mid-high LCS, with the average recovery of the high-level LCS at 130%. Based on the 

recovery of the second set of high-level LCS, it is the opinion of the laboratory that the recovery of the 

high-level LCS is due to a sample preparation error, and not the result of any significant analytical bias. 

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 + branched) LCS that did not meet method 

acceptance criteria. 

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

. yer^ . i-> Calculated Concentration , . „.. , 

LCS Percent Recovery = * 100% 

Spiice Concentration 

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

average LCS recovery 

Page 17 of 57 
GLP10-01-02; Interim Report 02 

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

IVIarcii/April 2010 

Table 6. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Lab ID 

LCS-100512-1 

LCS-100512-2 

LCS-100512-3 

Average ±%RSD 

LCS-100512-4 

LCS-100512-5 

LCS-100512-6 

Average ±%RSD 

LCS-100512-7 

LCS-100512-8 

LCS-100512-9 

Average ±%RSD 

PFBS 

Spiked 

Concentration 

(ng/mL) 

0.204 

0.204 

0.204 

Calculated 

Concentration 

(ng/mL) 

0.239 

0.227 

0.251 

%Recovery 

117 

111 

123 

117% ±5.1% 

5.10 

5.10 

5.10 

4.68 

5.42 

5.35 

91.7 

106 

105 

101% ±7.9% 

30.6 

30.6 

30.6 

30.2 

30.6 

29.3 

98.8 

99.9 

95.8 

98.2% ±2.2% 

PFHS 

Spiked 

Concentration 

(ng/mL) 

0.206 

0.206 

0.206 

Calculated 

Concentration 

(ng/mL) 

0.244 

0.242 

0.250 

VoRecovery 

118 

118 

121 

119% ±1.5% 

5.15 

5.15 

5.15 

4.77 

5.43 

5.44 

92.6 

105 

106 

101% ±7.4% 

30.9 

30.9 

30.9 

29.8 

29.1 

29.5 

96.4 

94.3 

95.5 

95.4% ±1.1% 

ETS-8-044.0 

Lab ID 

LCS-100512-1 

LCS-100512-2 

LCS-100512-3 

Average ±%RSD 

LCS-100512-4 

LCS-100512-5 

LCS-100512-6 

Average ±%RSD 

LCS-100512-7 

LCS-100512-8 

LCS-100512-9 

Average ±%RSD 

PFOS (linear) 

Spiked 

Concentration 

(ng/mL) 

0.204 

0.204 

0.204 

Calculated 

Concentration 

(ng/mL) 

<0.510 

<0.510 

<0.510 

%Recovery 

NC 

NC 

NC 

NA 

5.10 

5.10 

5.10 

4.90 

5.45 

5.55 

96.0 

107 

109 

104% ±6.7% 

30.6 

30.6 

30.6 

30.0 

30.2 

30.5 

97.9 

98.7 

99.8 

98.8% ±1.0% 

Lab ID 

LCS-100512-10 

LCS-100512-11 

LCS-100512-12 

Average ±%RSD 

LCS-100512-13 

LCS-100512-14 

LCS-100512-15 

Average ±%RSD 

LCS-100512-16 

LCS-100512-17 

LCS-100512-18 

Average ±%RSD 

PFOS (linear+branched) 

Spiked 

Concentration 

(ng/mL) 

0.200 

0.200 

0.200 

Calculated 

Concentration 

(ng/mL) 

<0.510 

<0.510 

<0.510 

VoRecovery 

NC 

NC 

NC 

NA 

5.00 

5.00 

5.00 

5.74 

5.85 

5.64 

115 

117 

113 

115% ±1.7% 

30.0 

30.0 

30.0 

51.7 

49.8 

53.4 

172 

166 

178 

172% ±3.5%'^' 

NC = Not Calculated; Concentration detected was less than ttie analytical LOQ. 

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

Page 18 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

Table 6 continued. Laboratory Control Spike Recovery. 

ETS-8-044.0; 

Prepared with non-study samples 

Lab ID 

LCS-100517-16 

LCS-100517-17 

LCS-100517-18 

Average ±%RSD 

LCS-100517-19 

LCS-100517-20 

LCS-100517-21 

Average ±%RSD 

LCS-100517-22 

LCS-100517-23 

LCS-100517-24 

Average ±%RSD 

PFOS (linear + branched) 

Spiked 

Concentration 

(ng/mL) 

5.00 

5.00 

5.00 

Calculated 

Concentration 

(ng/mL) 

4.99 

5.27 

5.11 

VoRecovery 

99.8 

105 

102 

102% ±2.6% 

15.0 

15.0 

15.0 

16.6 

16.9 

17.5 

111 

113 

116 

113% ±2.2% 

30.0 

30.0 

30.0 

37.4 

40.0 

39.9 

125 

133 

133 

130%±3.5%<'' 

NC = Not Calculated; Concentration detected was less than the analytical LOQ. 

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

8.7 Analytical Method Uncertainty 

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

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

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

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

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

method uncertainty values listed in Table 7. 

Table 7. Analytical Uncertainty. 

Analyte 

PFBS 

PFHS 

PFOS 

Standard Deviation 

10.5 

12.4 

21.9 

Method 

Uncertainty 

100%±21% 

100%±25% 

100%±44% 

Page 19 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

8.8 Field Matrix Spikes (FMS) 

Low, mid and high field matrix spikes were collected at each sampling point to verify that the analytical 

method is applicable to the collected matrix. Field matrix spikes were generated by adding a measured 

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

PFOS (linear) prior to shipping sample containers for sample collection. Field matrix spike recoveries 

within method acceptance criteria of 100±30% confinn that "unknown" components in the sample matrix 

do not significantly interfere with the extraction and analysis of the analytes of interest. Field matrix spike 

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

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

The nominal spike level for the low field matrix spike was 1.0 ng/mL, the mid field matrix spike was 100 

ng/mL, and the high field marix spike was 1000 ng/mL for all sampling locations. For some sampling 

locations, the high field matrix spike was not appropriate as compared to the sample concentration. No 

laboratory matrix spikes were prepared. Field matrix spike levels will be adjusted accordingly for the 

next sampling event. 

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

of ^^C4-PF0S was not analyzed. 

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

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

Spike Concentraton 

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

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

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

from those listed in the raw data. 

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

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

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

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

no adjustment was made to the analytical uncertainty for PFOS. 

Page 20 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

Table 8. GW 203LQ1 Y10 LF 

3MUMSID 

GLP10-01-02-02-051 

GLP10-01-02-02-052 

GLP10-01-02-02-053 

GLP10-01-02-02-054 

GLP10-01-02-02-055 

Average Concenb 

Description 

GW203LQ1 Y10 LFO 

GW203LQ1 Y10 LF1 

GW203LQiyi O LFLS 

GW203LQ1Y10 LFMS 

GW203LQ1 Y10 LFHS 

•ation (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

62.9 

60.8 

NA<^> 

NA<^> 

1220 

%Recovery 

NA 

NA 

NA<^> 

NA<^' 

114 

61.9 ng/mL ±3.4% 

PFHS 

Concentration 

(ng/mL) 

358 

361 

NA'^) 

NA'^' 

1370 

%Recovery 

NA 

NA 

NA<^> 

NA(^' 

103 

360 ng/mL ±0.83% 

PFOS 

Concentration 

(ng/mL) 

856 

847 

NA<^) 

NA<^> 

1700 

%Recovery 

NA 

NA 

NA'^' 

NA(^' 

85.7 

852 ng/mL ±1.1% 

NA = Not Applicable 

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

Table 9. GW 220RQ1 Y10 LF 

3M LIMS ID 

GLP10-01-02-02-080 

GLP10-01-02-02-081 

GLPl 0-01-02-02-082 

GLP10-01-02-02-083 

GLP10-01-02-02-084 

Average Concent 

Description 

GW220RQ1 Y10 LFO 

GW220RQ1Y10 LF1 

GW220RQ1Y10 LFLS 

GW220RQ1Y10 LFIVIS 

GW220RQ1Y10 LFHS 

'ation (ng/mL) ±%RPD 

PFBS 

Concentration 

(ng/mL) 

7.59 

7.33 

8.86 

122 

1180 

%Recovery 

NA 

NA 

NC 

112 

115 

7.46 ng/mL ±3.5% 

PFHS 

Concentration 

(ng/mL) 

31.9 

32.1 

32.9 

138 

1100 

%Recovery 

NA 

NA 

NC 

108 

109 

32.0 ng/mL ±0.63% 

PFOS 

Concentration 

(ng/mL) 

43.2 

48.8 

44.4 

131 

1010 

VoRecovery 

NA 

NA 

NC 

85.9 

97.4 

46.0 ng/mL ±12% 

NA = Not Applicable 

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

Page 21 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

Table 10. GW 220LQ1 Y10 LF 

3IVILIMSID 

GLP10-01-02-02-071 

GLP10-01-02-02-072 

GLPl 0-01-02-02-073 

GLP10-01-02-02-074 

GLP10-01-02-02-075 

Description 

GW220LQ1 Y10 LFO 

GW220LQ1 Y10 LF1 

GW220LQ1 Y10 LFLS 

GW220LQ1 Y10 LFMS 

GW220LQ1 Y10 LFHS 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

10.4 

11.8 

13.5 

129 

1140 

%Recovery 

NA 

NA 

NC 

116 

111 

11.1 ng/mL ± 13% 

PFHS 

Concentration 

(ng/mL) 

51.7 

54.3 

54.4 

155 

1070 

%Recovery 

NA 

NA 

NC 

104 

104 

53.0 ng/mL ±4.9% 

PFOS 

Concentration 

(ng/mL) 

64.8 

62.4 

65.8 

157 

919 

%Recovery 

NA 

NA 

NC 

94.3 

86.4 

63.6 ng/mL ±3.8% 

NA = Not Applicable 

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

Table 11. GW 222RQ1 Y10 LF 

3iVILIMSID 

GLP10-01-02-02-031 

GLP10-01-02-02-032 

GLPl 0-01-02-02-033 

GLP10-01-02-02-034 

GLPIO-OI-02-02-035 

Average Concent 

Description 

GW222RQ1 Y10 LFO 

GW222RQ1 Y10 LF1 

GW222RQ1Y10 LFLS 

GW222RQ1 Y10 LFMS 

GW222RQ1 Y10 LFHS 

•ation (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

131 

126 

NA'^' 

NA'^' 

1200 

%Recovery 

NA 

NA 

NA'^' 

NA<^' 

105 

129 ng/mL ±3.9% 

PFHS 

Concentration 

(ng/mL) 

839 

850 

NA'^' 

NA(^> 

1880 

%Recovery 

NA 

NA 

NA<^> 

NA<^> 

105 

845 ng/mL ±1.3% 

PFOS 

Concentration 

(ng/mL) 

951 

997 

NA'^' 

NA<^> 

2030 

%Recovery 

NA 

NA 

NA'^> 

NA'^> 

107 

974 ng/mL ±4.7% 

NA = Not Applicable 

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

Page 22 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

Table 12. GW 227LQ1 Y10 LF 

3IVILIMSID 

GLPl CM)1-02-02-085 

GLPl 0-01-02-02-086 

GLP10-01-02-02-087 

GLPl 0^1-02-02-088 

GLP10-01-02-02-089 

Average Concent 

Description 

GW227LQ1 Y10 LFO 

GW227LQ1 Y10 LF1 

GW227LQ1Y10 LFLS 

GW227LQ1Y10 LFMS 

GW227LQ1 Y10 LFHS 

ration (ng/mL) ±%RPD 

PFBS 

Concentration 

(ng/mL) 

349 

335 

NA<^> 

NA'^' 

1480 

%Recovery 

NA 

NA 

NA*^> 

NA'^> 

112 

342 ng/mL ±4.1% 

PFHS 

Concentration 

(ng/mL) 

65.2 

62.2 

NA<^' 

NA<^> 

1120 

%Recovery 

NA 

NA 

NA<^> 

NA<^> 

108 

63.7 ng/mL ±4.7% 

PFOS 

Concentration 

(ng/mL) 

305 

269 

NA'^' 

NA<^> 

1260 

%Recovery 

NA 

NA 

NA<^' 

NA<^' 

98.3 

287 ng/mL ±13% 

NA = Not Applicable 

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

Table 13. GW 227RQ1 Y10 LF 

3MLIIVISID 

GLPl 0-01-02-02-001 

GLP10-01-02-02-002 

GLP10-01-02-02-003 

GLP10-01-02-02-004 

GLP10-01-02-02-005 

Description 

GW227RQ1 Y10 LFO 

GW227RQ1 Y10 LF1 

GW227RQ1Y10 LFLS 

GW227RQ1Y10 LFMS 

GW227RQ1Y10 LFHS 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

23.0 

24.6 

NA<^' 

NA'^' 

1170 

%Recovery 

NA 

NA 

NA'^' 

NA'^' 

112 

23.8 ng/mL ± 6.7% 

PFHS 

Concentration 

(ng/mL) 

169 

169 

NA<^' 

NA<^' 

1210 

%Recovery 

NA 

NA 

NA<^> 

NA<^> 

106 

169 ng/mL ±0.0% 

PFOS 

Concentration 

(ng/mL) 

920 

991 

NA<^' 

NA<^> 

1950 

%Recovery 

NA 

NA 

NA<^' 

NA<^) 

100 

956 ng/mL ±7.4% 

NA = Not Applicable 

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

Page 23 of 57 
GLP10-01-02; Interim Report 02 

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

iVIarch/April 2010 

Table 14. GWGRS04Y10LF 

3IVILIIVISID 

GLP10-01-02-02-036 

GLP10-01-02-O2-037 

GLP10-01-02-02-038 

GLP10-01-02-02-039 

GLP10-01-02-02-040 

Average Concent 

Description 

GWGRS04Q1Y10 LFO 

GWGRS04Q1Y10 LF1 

GWGRS04Q1Y10 LFLS 

GWGRS04Q1Y10 LFMS 

GWGRS04Q1Y10 LFHS 

•ation (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

1800 

2050 

NA'^^' 

NA'^> 

2730 

%Recovery 

NA 

NA 

NA<^' 

NA<2> 

78.9 

1930 ng/mL ±13% 

PFHSf" 

Concentration 

(ng/mL) 

5810 

6360 

NA<2' 

NA<^' 

7140 

%Recovery 

NA 

NA 

NA<^' 

NA<=' 

NC 

6090 ng/mL ±9.0%*^' 

PFOS 

Concentration 

(ng/mL) 

1510 

1290 

NA<^' 

NA<2' 

2730 

%Recovery 

NA 

NA 

NA<^' 

NA<^' 

134^ 

1400 ng/mL ±16% 

NA = Not Applicable 

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

(1) PFHS reported from 5/26/10 analysis. 

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

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

(4) Field matrix spike did not meet method acceptance criteria of 100% ± 30%. Since the method analytical uncertainty for PFOS is 100% ± 44%, no adjustment was made to the analytical 

uncertainty. 

Page 24 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

Table 15. GW 310RQ1 Y10 CP 

3IVILIMSiD 

GLP10-01-02-02-026 

GLP10-01-02-02-027 

GLP10-01-02-02-028 

GLP10-01-02-02-029 

GLP10-01-O2-02-030 

Average Concent 

Description 

GW310RQ1 Y10 CPO 

GW310RQ1 Y10 CPI 

GW310RQ1 Y10 CPLS 

GW310RQ1 Y10 CPMS 

GW310RQ1Y10 CPHS 

•ation (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

401 

370 

NA<^) 

NA<^> 

1430 

%Recovery 

NA 

NA 

NA<^' 

NA<^' 

102 

386 ng/mL ±8.0% 

PFHS 

Concentiation 

(ng/mL) 

435 

412 

NA<^' 

NA<^' 

1410 

%Recovery 

NA 

NA 

NA<^' 

NA<^' 

100 

424 ng/mL ±5.4% 

PFOS 

Concentiation 

(ng/mL) 

780 

739 

NA'^> 

NA'^> 

1730 

%Recovery 

NA 

NA 

NA<^> 

NA<^> 

98.0 

760 ng/mL iS.4% 

NA = Not Applicable 

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

Table 16. GW 312RQ1 Y10 CP 

3MLIIVISID 

GLP10-01-02-O2-090 

GLP10-O1-02-02-091 

GLP10-01-02-02-092 

GLP10-01-02-02-093 

GLP10-01-02-02-094 

Average Concent 

Description 

GW312RQ1Y10 CPO 

GW312RQ1Y10 CPI 

GW312RQ1Y10 CPLS 

GW312RQ1Y10 CPMS 

GW312RQ1 Y10 CPHS 

•ation (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

1220 

1220 

NA<^> 

NA<^> 

2240 

VoRecovery 

NA 

NA 

NA<^' 

NA*^' 

100 

1220 ng/mL ±0.0% 

PFHS 

Concentration 

(ng/mL) 

949 

942 

NA'^> 

NA<^> 

1970 

VoRecovery 

NA 

NA 

NA<^> 

NA<^> 

104 

946 ng/mL ±0.74% 

PFOS 

Concentration 

(ng/mL) 

1710 

1790 

NA'^' 

NA<^> 

2800 

VoRecovery 

NA 

NA 

NA<^' 

NA<^' 

106 

1750 ng/mL ±4.6% 

NA = Not Applicable 

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

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

Page 25 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

Table 17. GW 317LQ1 Y10 CP 

3M LIMS ID 

GLP10-01-02-02-021 

GLP10-01-02-02-022 

GLP1(W)1-02-02-023 

GLP10-01-02-02-024 

GLP10-01-02-02-025 

Description 

GW317LQ1Y10 CPO 

GW317LQ1 Y10 CPI 

GW317LQ1Y10 CPLS 

GW317LQ1Y10 CPMS 

GW317LQ1Y10 CPHS 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

0.536 

0.531 

1.78 

116 

NA<^> 

VoRecovery 

NA 

NA 

122 

113 

NA'^' 

0.534 ng/mL ±0.94% 

PFHS 

Concentration 

(ng/mL) 

0.688 

0.693 

1.85 

102 

NA(^' 

VoRecovery 

NA 

NA 

118 

103 

NA<^' 

0.691 ng/mL ±0.72% 

PFOS 

Concentration 

(ng/mL) 

2.48 

2.39 

2.98 

76.2 

NA<^' 

VoRecovery 

NA 

NA 

NC 

74.5 

NA<^' 

2.44 ng/mL ±3.7% 

NA = Not /Applicable 

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

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

Table 18. GW 324LQ1 Y10 CP 

3M LIMS ID 

GLP10-01-02-02-006 

GLP10-01-02-02-007 

GLP10-01-02-02-008 

GLP10^1-02-02-009 

GLP10-O1-O2-02-010 

Average Concent 

Description 

GW324LQ1Y10 CPO 

GW324LQ1Y10 CPI 

GW324LQ1Y10 CPLS 

GW324LQ1Y10 CPMS 

GW324LQ1Y10 CPHS 

'ation (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

94.3 

97.0 

NA'^' 

NA<^' 

1170 

VoRecovery 

NA 

NA 

NA<^' 

NA<^> 

105 

95.7 ng/mL ±2.8% 

PFHS 

Concentration 

(ng/mL) 

98.3 

104 

NA'^' 

NA'^' 

1130 

VoRecovery 

NA 

NA 

NA<^> 

NA<^' 

105 

101 ng/mL ±5.6% 

PFOS 

Concentration 

(ng/mL) 

192 

214 

NA<^' 

NA<^' 

995 

VoRecovery 

NA 

NA 

NA<^) 

NAW 

80.0 

203ng/mL±11% 

NA = Not /Applicable 

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

Page 26 of 57 
GLP10-01-02; Interim Report 02 

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

IVIarch/April 2010 

Table 19. GW 327RQ1 Y10 CP 

3M LIMS ID 

GLP10-01-02-02-061 

GLP10-01-02-02-062 

GLP10-01-02-02-063 

GLP10-01-02-02-064 

GLP10-01-02-02-065 

Average Concent 

Description 

GW327RQ1 Y10 CPO 

GW327RQ1 Y10 CPI 

GW327RQ1 Y10 CPLS 

GW327RQ1 Y10 CPMS 

GW327RQ1 Y10 CPHS 

^tion (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

80.9 

70.6 

NA<^' 

NA<^> 

1270 

VoRecovery 

NA 

NA 

NA'^' 

NA<^> 

117 

75.8 ng/mL ±14% 

PFHS 

Concentration 

(ng/mL) 

156 

152 

NA<^' 

NA*^' 

1220 

VoRecovery 

NA 

NA 

NA<^' 

NA<^' 

109 

154 ng/mL ± 2.6% 

PFOS 

Concentration 

(ng/mL) 

695 

582 

NA<^> 

NA<^' 

1490 

VoRecovery 

NA 

NA 

NA<^' 

NA<^' 

86.0 

639 ng/mL ±18% 

NA= Not/Applicable 

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

Table 20. GW 328LQ1 Y10 CP 

3M LIMS ID 

GLPl 0-01-02-02-066 

GLPl 0-01-02-02-067 

GLPl 0-01-02-02-068 

GLP10-01-02-02-069 

GLP10-01-02-02-070 

Average Concent 

Description 

GW328LQ1 Y10 CPO 

GW328LQ1 Y10 CPI 

GW328LQ1 Y10 CPLS 

GW328LQ1Y10 CPMS 

GW328LQ1Y10 CPHS 

ration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

77.4 

76.2 

NA(^) 

NA<^' 

1190 

%Recovery 

NA 

NA 

NA'^> 

NA'^' 

109 

76.8 ng/mL ±1.6% 

PFHS 

Concentration 

(ng/mL) 

26.0 

25.7 

NA<^> 

NA<^' 

1070 

%Recovery 

NA 

NA 

NA'^> 

NA<^' 

106 

25.9 ng/mL ±1.2% 

PFOS 

Concentration 

(ng/mL) 

14.5 

14.4 

NA<^' 

NA'^' 

865 

VoRecovery 

NA 

NA 

NA(^> 

NA<^' 

85.9 

14.5 ng/mL ±0.69% 

NA= Not/Applicable 

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

Page 27 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

Table 21. GW 328RQ1 Y10 CP 

3M LIMS ID 

GLP1CW)1-02-02-056 

GLP1CW)1-02-02-057 

GLP10-01-02-02-058 

GLP10^1-02-02-059 

GLP10-01-02-02-060 

Average Concent 

Description 

GW328RQ1 Y10 CPO 

GW328RQ1 Y10 CPI 

GW328RQ1 Y10 CPLS 

GW328RQ1 Y10 CPMS 

GW328RQ1 Y10 CPHS 

ration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

35.6 

36.3 

NA<^' 

NA<^' 

1230 

VoRecovery 

NA 

NA 

NA<^> 

NA<^' 

117 

36.0 ng/mL ±1.9% 

PFHS 

Concentration 

(ng/mL) 

69.9 

65.4 

NA<^> 

NA<^' 

1120 

%Recovery 

NA 

NA 

NA*^' 

NA'^> 

107 

67.7 ng/mL ±6.7% 

PFOS 

Concentration 

(ng/mL) 

159 

132 

NA<^> 

NA<^' 

1110 

VoRecovery 

NA 

NA 

NA<^' 

NA<^' 

97.4 

146 ng/mL ±19% 

NA = Not /Applicable 

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

Table 22. GW 330LQ1 Y10 CP 

3M LIMS ID 

GLP10-01-02-02-016 

GLP10-01-02-02-017 

GLP10-01-02-02-018 

GLP10-01-02-02-019 

GLP10^1-02-02-020 

Average Concent 

Description 

GW330LQ1 Y10 CPO 

GW330LQ1 Y10 CPI 

GW330LQ1 Y10 CPLS 

GW330LQ1Y10 CPMS 

GW330LQ1Y10 CPHS 

•ation (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

519 

489 

NA<^' 

NA<^' 

1570 

VoRecovery 

NA 

NA 

NA<^* 

NA<^' 

105 

504ng/mL ± 6.0% 

PFHS 

Concentration 

(ng/mL) 

405 

400 

NA'^' 

NA'^' 

1460 

VoRecovery 

NA 

NA 

NA'^' 

NA'^' 

108 

403ng/mL±1.r/o 

PFOS 

Concentration 

(ng/mL) 

155 

135 

NA<^> 

NA<^> 

1100 

VoRecovery 

NA 

NA 

NA<^' 

NA<^> 

96.5 

145 ng/mL ±14% 

NA = Not /Applicable 

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

Table 23. GW 330RQ1 Y10 CP 

Page 28 of 57 
GLP10-01-02; Interim Report 02 

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

iVIarcii/April 2010 

3M LIMS ID 

GLP10-01-02-02-011 

GLP10-01-02-O2-012 

GLP10-01-02-02-013 

GLP10-01-02-02-014 

GLP10-01-02-02-015 

Average Concent 

Description 

GW330RQ1Y10 CPO 

GW330RQ1Y10 CPI 

GW330RQ1Y10 CPLS 

GW330RQ1Y10 CPMS 

GW330RQ1Y10 CPHS 

•ation (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

4520 

4410 

NA<^> 

NA<^> 

NA(^> 

VoRecovery 

NA 

NA 

NA<^' 

NA<^' 

NA<^> 

4470 ng/mL ±2.5%^^ 

PFHS 

Concentration 

(ng/mL) 

264 

251 

NA<^> 

NA<^> 

1310 

VoRecovery 

NA 

NA 

NA<^> 

NA<^' 

107 

258 ng/mL ±5.0% 

PFOS 

Concerttration 

(ng/mL) 

763 

755 

NA<^' 

NA'^' 

1710 

VoRecovery 

NA 

NA 

NA<^' 

NA<^' 

96.1 

759ng/mL±1.1% 

NA = Not /Applicable 

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

(2) Analyte concentration exceeded calibration range. Further dilution of the sample was not prepared as ttie spike level was not appropriate as compared to the sample concentration. 

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

Table 24. GW 331SQ1 Y10 CP 

3M LIMS ID 

GLPl 0-01-02-02-046 

GLPl 0-01-02-02-047 

GLP10-01-02-02-048 

GLP10-01-O2-02-049 

GLP10-01-02-02-050 

Average Concent 

Description 

GW331SQ1 Y10 CPO 

GW331SQ1 Y10 CPI 

GW331SQ1 Y10 CPLS 

GW331SQ1 Y10 CPMS 

GW331SQ1Y10 CPHS 

'ation (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

327 

371 

NA<^' 

NA<^> 

1480 

%Recovery 

NA 

NA 

NA'^' 

NA'^' 

111 

349 ng/mL ±13% 

PFHS 

Concentration 

(ng/mL) 

398 

454 

NA<^' 

NA<^' 

1450 

VoRecovery 

NA 

NA 

NA<^' 

NA<^' 

104 

426 ng/mL ± 13% 

PFOS 

Concentration 

(ng/mL) 

824 

1020 

NA<^> 

NA<^> 

1810 

VoRecovery 

NA 

NA 

NA<^> 

NA<^' 

89.7 

922 ng/mL ±21%^^ 

NA = Not /Applicable 

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

(2) The RPD did not meet method acceptance criteria of ^0% . 

Table 25. Trip Blank 

Page 29 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

3M LIMS ID 

GLP10-01-02-02-076 

GLP10-01-02-02-077 

GLP10-01-02-02-078 

GLP10-01-02-02-079 

Description 

Trip Blank Sample 

Trip Blank FMS Low 

Trip Blank FMS Mid 

Trip Blank FMS High 

PFBS 

Concentration 

(ng/mL) 

<0.0255 

1.28 

120 

1140 

VoRecovery 

NA 

125 

118 

112 

PFHS 

Concentration 

(ng/mL) 

<0.0258 

1.21 

112 

1070 

VoRecovery 

NA 

123 

114 

109 

PFOS 

Concentration 

(ng/mL) 

<0.510 

1.21 

98.2 

925 

VoRecovery 

NA 

122 

99.2 

93.4 

NA = Not /Applicable 

Table 26. Rinseate Blanks 

3MUMSID 

GLP10-01-02-02-041 

GLP10-01-02-02-O42 

GLP10-O1-02-02-O43 

GLP10-01-02-02-044 

GLP10-O1-02-02-O45 

GLP10-01-02-01-006 

GLP10-01-02-01-031 

Description 

Rinseate Blanki 203L 

Rinseate Blank2 203L 

Rinseate Blanks 203L 

Rinseate Blank4 203L 

Rinseate Blanks 203L 

DAL DF05 SS SS07 2 0010 

DALDF11SSSS07 2 0010 

PFBS 

Concentration 

(ng/mL) 

<0.0255 

<0.0255 

<0.0255 

<0.0255 

<0.0255 

<0.0255 

<0.0255 

VoRecovery 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

PFHS 

Concentration 

(ng/mL) 

<0.0258 

<0.0258 

<0.0258 

<0.0258 

<0.0258 

<0.0258 

<0.0258 

VoRecovery 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

PFOS 

Concentration 

(ng/mL) 

<0.510 

<0.510 

<0.510 

<0.510 

<0.510 

<0.510 

<0.510 

VoRecovery 

NA 

NA 

NA 

NA 

NA 

NA 

NA 

NA = Not Applicable 

30 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

Laboratory control spikes and field matrix spikes were used to detemnine the anaiytic^a! method 

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

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

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

to 3M Environmental Laboratory standard operating procedures. 

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

Attachment B: Representative Chromatograms and Calibration Curves 

Attachment C: Analytical Method 

Attachment D: Method Deviation 

Page 31 of 57 
GLP10-01-02; Interim Report 02 

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

i\/larcl^/April 2010 

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

^/?0/^<y/ 0 

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

-7. 

tet 10 

Gary Hoherifeteiri^ponsor Representative 

Study Din 

\UJi/ 

Date 

mo 

/ 7 Date Jaisimha Kesari, Study Director 

Page 32 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

Analytical Protocol: GLP10-01-02 

Amendment 2 

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. 2 

Amendment Date: 

March 24. 2010 

Performing Laboratory 

3M Environmental, Health, and Safety Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55144-1000 

Laboratory Project Identification 

GLPl 0-01-02 

Page i of 7 

Page 33 of 57 
GLP10-01-02; Interim Report 02 

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

iVIarch/April 2010 

Analytical Protocol: GLP10-01-02 

Amendment 2 

This amendment modifies the following portion of protocol: 

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

Decatur Phase 3 Site-Related Monitoring Program" 

PROTOCOL READS: 

No changes to the wording of the protocol are required. 

AUENDTOREAD: 

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

addresses and documents the addition of the General Project Outline (GPO) for the 

collection and analysis of groundwater samples from Decatur. AL. and conducted as 

part of the 3M Decatur Phase 3 Program for PFOS. PFHS and PFBS (GLP10-01-02). 

The anticipated sample collection will occur around the timeframe of March 26. 2010. 

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

Environmental Laboratory LIMS as project GLP10-01-01-02 and reported as interim 

report GLPl0-01-02-02. (reflecting study GLP10-01-02 and amendment -02). 

Reason: 

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

which describes the anticipate groundwater sample collection event to be conducted for 

the 3M Decatur, AL fecility. 

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

Page 2 of 7 

Page 34 of 57 
GLP10-01-02; Interim Report 02 

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

March/April 2010 

Analytical Protocol: GLP10-01-02 

Amendment 2 

Amendment Approval 

f^t % ) 

Gary Hohenstein, Sponsor Representative 

Cleston C. Lange, Principal Analytical Investigator 

Date 

j/z^/2.i>/^ 

Date 

^S~'/^-/M<'y^.^o 

William Reagen, EHS Opns Environmental Lab Management Date 

4S-

^ /bate 

Jaisimha Kesari P.E., DEE, Study Director 

Page 3 ot 7 

Page 35 of 57 
GLP10-01-02; Interim Report 02 

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

IMarch/April 2010 

Analytical Protocol: GLP10-01-02 

Amendment 2 

Environmental Health & Safety Operations, Environmental Laboratory 

General Project Outline 

To: Gary Hohenstein, 3M EHS&Opns 

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

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

Cliffton Jacoby, 3M EHS&Opns; Environmental Lab 

Jai Kesari, Weston Solutions 

Charies Young, Weston Solutions 

Tim Frinak, Weston Sdutions 

Date: March 24, 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 #2 - Decatur I** Quarter 

Groundwater Sampling 

1 General Project Information 

Contacts 

Lab Request Number 

Six Digit Department Number 

ProJQCt Schedulerrost Datvs 

3M Sponsor Representative 

Gary Hohenstein 

3M EHS OperatiorJS 

3IVI Buiiding 224-5W-03 

Saint Paul, MN 55144-1000 

Phone: (651) 737-3670 

Qahohenstein@mmm.conn 

3lia Environmental Laboratory Management 

William IC Reagen 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9739 

wlcreaQen@mmm.com 

Principal Analytical Investigator 

Cleston Lange 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9860 

ppi^nq^mmmcom 

Sampling Coordinator 

Timothy Frinak 

Weston Solutions 

Timolhv.frinakiaiwestonsolutions.com 

Phone: (334)-332-9123 

GLP1&41-02-02 

Dept #530711, Project #0022674449 

Sampling scheduled for ths wssk of March 29,2010 

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

Page 4 of 7 

Page 36 of 57 
GLPl 0-01-02; Interim Report 02 

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

March/April 2010 

Analytical Protocol: GLP10-01-02 

Amendment 2 

2 Background Information and Project ObJective(s) 

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

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

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

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

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

March 29, 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 GLPl 0-01-02-

02. 

3 Project Schedule 

Sample collection bottles will be prepared by 3M Environmental Laboratory for sampling the week of March 29, 

2010. Sample bottles will be shipped in coolers overnight to 3M Decatur for arrival on Friday, March 26,2010 to 

the attention of Keith Schmuck., 3M Cordova Environmental Engineer. Sample bottles should be stored 

refrigerated on-site until sample collection. 

Martin Smith \ Weston Trailer 

3M Decatur Plant 

1400 State Docks Road 

Decatur, Alabama 35601 

4 Test Parameters 

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

A total of seventeen sampling locations have been specified. Sampling location descriptions were not available 

at the time of sample bottle preparation. For each sampling kx:ation, a total of five sample bottles will be 

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

matrix spike). The liil to here" line on each 250 mL Nalgene bottle will be 20O mL Four sets of trip blanks 

consisting of reagent-grade water, a tow-level trip blank spike, mki-level field spike and a high-level trip blank 

spike will be prepared at the 3M Environmental Laboratory and sent to the sampling location with the other 

bottles. The low field matrix spike will be prepared at 1 ng/nnL, the mid field matrix spike at 100 ng/mL, and the 

high fiekl matrix spike at 1000 ng/mL. Five additional bottles will be prepared to be used hr the preparation of 

the equipment rinseate blanks. A toteil of 106 sample bottles will be prepared. 

All sample bottles will include the addition of ^*OrPFBS, ^^OrPFHS, and '^C«-PFOS, 1802.PFBS (intemal 

standards) at a nominal concentration of 1 ng/mL All sampte bottles will also include the addition of ^'C4-PF0S 

(sunnogate spike) at a nominal concentration of 0.1 ng/mL. 

5 Test Methods 

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

Compounds In Water by High Performance Liquid Chromatography/Mass Spe(*x3metry Direct Injection 

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

analytk^l accuracy of 100±30%. Field matrix spikes not yielding recoveries wi&iin 1001:30% will be addressed 

in the report and the final acctjracy statement may be adjusted accordingly. 

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

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

Chromatography/Mass Spectromefry". Method Ers-8-154 has been validated for PFOA and PFOS only; 
GLP10-01-02; Interim Report 02 

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

IVIarch/April 2010 

Analytical Protocol: GLP10-01-02 

Amendment 2 

however, specific quality control samples analyzed with the samples will be used to detennine overall method 

precision and accuracy. 

6 Reporting Requirements 

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

field matrix spikes. A single trip blank and three trip blank spikes will be reported for the sampling event as will 

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

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

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

detection limit. /Miy laboratory matrix spikes that may t>e prepared will also tie included in the final report 

7 Emai l Correspondence 

Attachment /K: Sampling Bottle Request 

Page 6 of 7 

Paffe 38 of 57 
GLP10-01-02; Interim Report 02 

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

IVIarch/April 2010 

Analytical Protocol: GLP10-01-02 

Amendment 2 

Bottle Request - GLPlO-01-01 / GLPlO-01-02 

QUO Decatur Groundwater Sampling 

02181.129.145.0001 

DATE REQUESTED: 17 March 2010 

No. of Samples Sample Tvpe Comment 

5 Groundwater Anticipate high VOC concentrations 

12 Groundwater Average Samples 

1 Rinseate Sample Will need HPLC water 

4 Trip Blanks Anticipate 1 per cooler 

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

BOTTLES REQUIRED BY 26 MARCH 2010 

Shipping Address: 

Martin Smith \ Weston Trailer 

3M Decatur Plant 

1400 State Docks Road 

Decatur, AL 35601 

256-552-6189 

Page 7 of 7 

Paffe 39 of 57 
"** Ginger AG01330509 

GLP10-01-02; Interim Report 02 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples from Decatur, AL^gg^j^j-g NameMarch/April 2010 

gl00517a.rdb 

r

Sampl* Nanw: -g100517a02r Sampte ID: "08 008-147-10" Fite: "g 100517a.wifT 

Paak Namo: 'ptbs' Mass(«s): -299.0/99.0 amu,299.0/80.0 amu,299.0/130.0 amiT 

Commant "5.0 ppb curva point in Mi i Q Watsi" Annotation:"" 

Saraple Indey; 27 

Satnple Type; 

Concentration: 

Calculated Conc: 

Acq. Date: 

Modified; 

RT Window: 

Expected RT: 

L'se Relative RT: 

ng/mL 

Height: 

Start T: 

End Tim. 

7975661 ci 

2I0OOOO, 

10.2 

10.7 

Z1a6 

2.0e6 

1.9a6 

1.ea6 

1.7a6 

1.6a6 

1.5a6 

1.4a6 

1.3a6 

1.2a6 

1.1 a6 

1.0a6 

9.085 

8.0a5 

7.0a5 

6.0a5 

5.0a5 

4.0B5 

3.0a5 

2.0a5 

I.OaS 

10.37 

I 

I

San^aNam8;"g100517a074' Sampte ID:'GLP1(M)1-02-02O01" Fite; •g100517a.wir 

Paak Nama: 'ptbs' Mass(as): "299.0/99.0 amu,299.0/80.0 amu,299.0/130.0 amu' 

Commant-GW227RQ1 Y10 LF0{dil1:100)' Annotation:-' 

1.05a5 

I.OOaS9.50a4-

9.00a4 

8.50a4 

8.00a4 

7.50a4 

7.00a4 

6.50a4 

e 6.00e4 

is- 5.50o4 

SS 

I 5.00a4 

4.50a4 

4.00a4 

3.50e4 

3.00a4 

Z50a4 

Z00a4 

1.50a4 

1.00e4 

5000.00-

0.00 

7 8 9 10 11 12 13 14 15 16 

Ttme. min 

Sample Type: 

Concentration: 

Calculated Conc 

Acq. Date: 

Acq. Time: 

Modified: 

RT Window: 

Expected RT: 

Unknown 

H/A 

< 0 

5/1B/2010 

!:;2:13 AM 

Yes 

30.0 

10.4 

I

Sampte Nanw: -fl100517a059" Sampta ID: 'Sotvent btaniC Fite: 'g1O0517a.wHr 

Paak Nama: 'ptbs" Mass<es): "299.0/99.0 amu.299.0/80.0 amu.299.0/130.0 amu* 

ComntanfMiniQWatarTNIOOISS" Annotation:" 

Sample Index: 59 

5000 

4800 

4600 

4400 

4200 

4000 

3800 

3600 

3400 

3200 

3000-

2800 

2600 

24O0 

2200 

2000 

1800-

1600 

1400-

1200 

1000-

800 

..•iJ|i-^.i^..,...L,...iii,lii I, I 11, ifUttp m 

I

Sanpte Nama: "g100517a168' Sampia ID: "LCS-100517-22- Fite: "g100517a.v*r 

Paak Nama: 'pfba' M8ss{es): -299.0^.0 amu,299.0/S0.0 amu,299.0/130.0 amiT 

Commant "30ppb LCS ECP Annotation: " 

Sample Index : 16B 

Sample Tvpe: 

Concentration : 

Calculate d Conc 

Acq . Date : 

Acq . Tirae: 

Modified : 

RT Window: 

Expecte d RT: 

L'nknown 

N/A 

23. 0 

5/13/201 0 

5:52:3 0 At 

Yes 

30.0 

10.4 

Height: 

Start ' 

End Tir 

Sample Type: 

Concentration : 

Calculate d Conc 

Acq. Date: 

Acq. Time: 

Modified : 

RT Window: 

Expected RT: 

Use Relativ e RT 

Int . Type: 

Retentio n Time: 

Area ; 

Height : 

QC 

0.00 

0.407 

5/19/201C 

12:15:4 1 

Yes 

30.0 

10.4 

No 

Manual 

10.4 

96364 CO 

183000. c 

ng/mL 

ng/mL 

PH 

ssc 

min 

min 

jnt s 

ps 

>-"l-8' 12.99,13.36 

^^^ *• ...^WlWWllV, M. S 

Dat a worke d u p b y STW 

Printin g Time : 3:24:0 4 PM 

Printing Date: Tuesday, June 29, 2010 

Page 1 of 3 

Page 40 of 57 
Ginge r AG01330509 

GLP10-01-02; Interim Report 02 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples from Decatur, ALj^ggults Name: gl00517a. rdb 

March/April 2010 

• Sampla Name:'g100517a027' Sampte ID: "08 006-147-10" FBo; "g100517a. 

I Paak Nama: "pths' Masa^ea): -399.0/99.0 amu,399.0/80.0 amu,399.Qyi30.0 amu" 

I Commant '5.0 ppb curva point in Mi l Q Watar" Annotation: 

Sample Index: 

Sample Type; 

Concentration: 

Calculated Conc: 

Acq. Date: 

Acq. Time: 

Modified: Yes 

RT Window: 30.0 

Expected RT: 11.8 

Use Relative RT: No 

106J1251 

2810000. 

11.5 

Sampte Nama: •g^0QSi^aQ5Sr Sampte ID: "Solvent l>lanIT Fite: "g100517a.wir 

Peak Nama: 'pfhs" Maat(ea): "399.0/99.0 amu.399.0/80.0 amu,399.0/130.0 amu" 

Comment 'Milli 0 Wtator TN10O153" 

Sample Index: 59 

1.20ft4' 

1.15a4 

1.1064 

1.05e4 

1.00a4 

9500.00 

9000.00 

s 8500.00 

8000.00 

7500.00 

7000.00 

§-6500.00 

'I'6000.00 

I 5500.00 

5000.00 

4500.00 

4000.00 

3500.00 

3000.00 

2500.00-

Sample Type: 

Concentratlo 

Calculated Conc 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algorithm 

Noise Percen aq 

Unicnown 

N/A 

0.00179 

5/18/2010 

1:22:13 AM 

No 

IntelliCua 

: 50 

Base. Sub. Window: 1.00 

P^ah-Split. Factor: 5 

Report Large 

Min. Peak He 

Min. Peak Wi 

t Peah: No 

th 

Smoothing Width 

RT Window: 

Ey.pected RT: 

Use Relative 

Int. Type: 

Retention Ti 

Area: 

Height: 

Start Time: 

End Time: 

RT 

e: 

: 0.00 

0.00 

0 

30.0 

11.6 

Ho 

Base To Ba 

11.6 

4 003 COU 

723. cp 

11.5 

11.7 

2000.00' 

1500.00 

500.00 

0.00 ^,.1, ,. II llf ,l,ti,lijl 

Sanpte Name: "glOOSnalSe" Sampte ID: "LCS-100517-2r Fite: '3100517a.wtfT 

Peak Name: "ptha* Maa8(ea): "399.0/99.0 aniu.399.0/80.0 amu.3gg.0/130.0 amiT 

Comment '30ppb LCS ECP Anrmtation: *" 

Sample Index: 158 

Sample Type: QC 

Concentration: 0.00 ng/mL 9.0e5 

Calculated Conc: 1.99 ng/mL 

Acq. Date: 5/19/2010 „-^e 

Acq. Time: 12:16:41 PM °-^° 

Modified: Yes 8.0*5 

RT Window: 30.0 sec 

-T: 11.6 min 7.5.5 

vo BT: Ho 

Manual 7.0e5 

Time: 11.6 min 

3998324 counts 6.5a5 

908000. cps 

11. 4 min -

11.5 min ®-°»5 

5.5e5 

I 5.0e5 

# 4.5e5 

I 

3.0e5 

2.5*5 

Z0»5 

1.5*5 

1.0*5 

5.0*4 

0.0 

I

Sampl* Name: 'g100517a074- Sampte ID: "GLPl OOI-02-02-001' Fite: -g100517a.Mr 

Peak Nama: "plhs" Ma8a(ea): "399.0/99.0 amu.399.0/80.0 annu.399.0/130.0 am f 

Commant"GW227RQ1 Y10 LFO{dai:100r Annotation:" 

Sample Index: 74 

Sample Type: 

Calculated Conc 

Acq. Date: 

Acq. Time: 

Modified: 

RT Window: 

Expected RT: 

Use Relative 

int. Type: 

Retention Ti 

Area: 

Height: 

Start Time: 

End Tim-: 

RT 

3 

Unknown 

N/A 

169. ng 

5/19/2010 

5:52:30 A M 

Yes 

30.0 sec 

11.6 min 

No 

Manual 

11.5 min 

82003 counts 

939000. cps 

11.3 min 

11 12 13 14 15 16 

Data worked up by STW 

Printin g Time: 3:24:0 4 PM 

Printin g Date : Tuesday, Jun e 29, 2010 

Page 2 of 3 

Page 41 of 57 
Ginge r AG01330509 

GLP10-01-02; Interim Report 02 

Analysisof PFBS, PFHS, and PFOS in GroundwaterSamplestrom Decatur, AL Result s Name- gl00517 a rd b 

March/April 2010 

1 • Sampl* Nanw: "91005178027" Sampte ID: "08 008.147-10" Fite:'g100517a.wir 

• Paak Nam*: 'pfoa' Mass<*B): '499.0/99.0 amu,499.0ra0.0 amu,499.0/130.0 amu" 

• Commant '5.0 ppb curve point in Mi i Q Watar" Annotation:" 

Sample Index : 27 

Sample Type: Standar d 

Concentration : 5.10 ng/mL 

Calculate d Conc: 5.09 ng/mL -J-f i 

Acq . Date : S/17/2010 ^^ ^ 

Acq . Time: 3:46:48 PM 2.3*6 

Modified : Yes 2.2*6 

RT Window: 30. 0 sec 

Expected RT: 12.4 ni n 2.1*6 

Uae Relativ e RT: No jOeB 

Int . Type: Manual 19*6 

Retentio n Time : 12.4 min 

Area : 9725685 count s 1.8*6-

Height : 2510000. cps 

Star t Time: 12. 1 min 1.7*6-

End Time: 12.7 min , g^g 

1.5*6 

1 1.3*6 

1 1.2*6 

- 1.1*6 

1.0*6 

9.0*5 

6.0*5 

7.0*5 

6.0*5-

5.0e5 

4.0e5-

3.0*5 

2.0*5' 

1.0*5 

"• ° i 2 3 4 5 "e 

• Sample Nanrw: 'g100517a074" Sampte ID: "GLPltM)1-02-02-001' Fite: 'gl00517a.v«r 

1 Paak Name: "ptoa' Mass(*»):'499.099.0 amu,499.0/80.0 amu.499.0/130.0 amu' 

• Comm*nt-6W227RQ1Y10 LFO{dK1:100r Annotation:-

Sample Index : 74 

Sample Type : Uriknown 

Concentration : N/A 

Calculate d Conc: 920. ng/mL 

Acq. Date: 5/18/2010 2.2e6' 

Acq. Tirae: 5:52:3 0 AM 2.1.6-

Modified : Yes ,- ^ 

RT Window: 30.0 sec ^'^ ^ 

Expected RT: 12.4 min 1 9e6 

Use Relativ e RT: No 

1.ee6 

Int . Type: Manual 

Retentio n Time : 12.4 min 1.7*6 

Araa : 17175744 count s 

Height : 2300000. cps 1.6*6-

Star t Time: 12.0 min 

End Time: 12.6 min 1.5*6-

1.4*6-

1 1.1*6 

- 1.0*6' 

9.0*5 • 

8.0*5-

7.0*5-

8.0*5-

5.0*5-

4.0*5-

3.0*5-

2.0*5-

1.0*5-

0.0- J • • • • • • • 1 . 1 • r 

1 2 3 4 5 6 

12-42 

I 

7 8 9 10 11 12 13 14 15 16 

Time, min 

1241 

12.2&,. 

1Z16 . 

h 

7 8 9 10 11 12 13 14 15 16 

• Sampte Name:'g100517a05? Sampte ID:'Sohent tilanir FBa:-g100517a.<Mr 

• Paak Nama;'pfos- Ma«a<es): "499.0199.0 amu,499.0ffi0.0amu,499.0/130.0 amu" 

• Commant "Mini 0WatefTN10«15 r Annotation: " 

Sample Index : S9 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Conc: 0.144 ng/mL 6500 

Acq. Date: 5/18/2010 

Acq. Time: 1:22:13 AM gQQModified : Yea 

RT Window: 30.0 sec 7500 

Expected RT: 12.4 min 

Use Relativ e RT: No y^j ^ 

Int . Type: Manual 

Area : 31467 count s 

Height : 8020. cps p-_-

Star t Time: 12.2 min ^°° ° 

End Time: 12.5 min 

5500 

5000 1 

>, 4500 

1 4000 

3500 

3000 

2500 

2000 

1500 

1000 

500 

,*,jJL-..L_L.li.i^*._iJL-. 1 j 

1 

h. uiuJHii 

J 

1 1 i .fl i l i 

1 lumW " \ 

IW ,]Jr r 1 

w^ iji f - " 1 

.i^jtmm \ \ mm^"' ^ V 

i 2 3 4 5 6 7 8 9 10 i'l 12 13 14 15 16 | 

• Sampte Name:'gl00517a168' Sampte ID: •LCS-100517-22' Fite:'g100517a.wir 

• Peak Name:'pfoa' Ma**(*»):-499.0ira9.0amu,499.0/80.0amu,499.0rt 30.0 amu" 

• Commant -30ppb LCS ECP Annotation: "' 

Sample Index : ISB 

Sample Type: QC 

Concentration : 30.0 nq/mL Rn»e 

Calculate d Conc: 37.4 ng/mL o.iw -

Acq. Date : 5/19/2010 

Acq. Time: 12il6:4 1 PM 7.5^5 

Modified : Yes 

RT Window: 30.0 sec 7.0*6 

Expected RT: 12.4 min 

Uae Relativ e BT: No 

Int . Type: Manual 

Retentio n Time: 12.4 min 60* 6 

Area : 53622417 count s 

Height : 6140000. cps 

Star t Time: 12.0 min 5.5*6 

End Time: 12.8 min 

5.0*6 

1 4.5*6 

Jf 

1 4.0*6 

1 

3.5*6 

a0a6 

Z5*6 

Z0*6 

1.5*6 

1.0*6 

5.0*5 

°'° i 2 3 4 1 

Time, min 

12.45 

12.32s. 

12.20 

1 11 

6 7 8 9 10 i'l 12 13 14 15 16 || 

^ Jm^m II 

Data worked up by STW 

Printin g Time: 3:24:0 5 

Printin g Date : Tuesday , 

Page 3 of 3 

PM 

June 29 , 2010 Page 42 of 57 
Ginge r AG01330509 

GLPlO-01-02; Interim Report 02 

Analysisof PFBS, PFHS.and PFOSinGroundwaterSamplesfrom Decatur, AL Results Name: gl00517a rdb 

March/April 2010 

g100517a.rdb (pfbs): "Quadratic" Regression ("1 Ix" weighting): y = -1.3e•^004 x'^2 + 1.71e•^006 x •^ 3.98e+003 (r = 0.9996) 

-T ' 1~ ~l 1 T" 

0 8 

"T ' r~ "T ' r^ 

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

Concentration, ng/mL 

Data worked up by STW 

Printing Time: 3:24:26 PM 

Printing Date: Tuesday, June 29, 2010 

Page 1 of 1 

Page 43 ot 57 
Ginge r AG01330509 

GLP10-01-02; Interim Report 02 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples from Decatur, AL Results Name: gl00517a. rdb 

March/April 2010 

Data worked up by STW 

Printin g Time: 3:24:4 5 PM 

Printin g Date : Tuesday , June 29, 2010 

Page 1 of 1 

Page 44 of 57 
»** Ginge r AG01330509 

GLPlO-01-02; Interim Report 02 

Analysisof PFBS, PFHS, and PFOS in Groundwater Samples from Decatur, AL Results Name- gl00517a rdb 

Marcti/April 2010 

Data worked up by STW 

Printin g Time: 3:25:0 7 PM 

Printin g Date : Tuesday , Jun e 29, 2010 

Page 1 of 1 

Page 45 of 57 
GLPlO-01-02; Interim Re9o9SiJiTi®nt "is y 'oB usGcl, If cufrent, for 14 day s fro m 06/29/2010 

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

March/April 2010 

Environmenfal Laboratory 

l\/letiiod 

Metiiod of Analysis for ttie Determination of Perfluorinated Compounds in Water 

by LC/MS/MS; Direct Injection Analysis 

Mettiod Number: ETS-8-044.0 

Adoption Date: Upon Signing 

Effective Date: Q ^ 1(2, f o "1 

Approved By: 

4^//^/o y 

William K. Reagen, Laboratory Manager Date 

ETS-8-044.0 Page 1 of 11 

Metiiod of Analysis for the Detenmination of Perfluorinated Conipounds in Water by LC/MS/MS; Direct 

Injection Analysis Page 46 of 57 
GLP10-01-02; Interim ReP)f?S^iJrnent may be used, if current, for 14 days from 06/29/2010 

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

March/April 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 "Detemnination 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 perfomnance-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 determined using field matrix spikes to verify that the method is applicable to 

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

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

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

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

accuracy for analytical results. 

3 Definitions 

3.1 Calibration Standard 

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

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

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

concentration. 

3.2 Laboratory Duplicate Sample (LDS, or Lab Dup) 

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

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

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

preservation, or storage procedures. 

3.3 Field Blank (FB)/Trip Blank 

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

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

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

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

ETS-8-044.0 Page 2 of 11 

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

Injection Analysis 

Page 47 of 57 
GLPlO-01-02; Interim R^of?S|Jrnent may be used, if current, for 14 days from 06/29/2010 

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

March/April 2010 

3.4 Field Duplicate Sample (FDS, Field Dup) 

A sample collected in duplicate at the same time fi-om 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 Sampie, FSCS) 

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

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

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

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

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

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

3.7 Laboratory Control Sample (LCS) 

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

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

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

exactly like a laboratory sample to 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 48 of 57 
GLP10-01-02; Interim R^oQQjJiTient "lay be used, if current, for 14 days from 06/29/2010 

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

IVlarcti/April 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 detemnine if test substances or other interferences are present in the laboratory 

environment, the reagents, or the apparatus. 

3.12 Sample 

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

material. 

3.13 Stock Standard Solution (SSS) 

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

compound. 

3.14 Surrogate 

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

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

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

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

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

quality control measure and is NOT required. 

3.15 Working Standard (WS) 

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

calibration standards and other required analyte solutions. 

4 Warnings and Cautions 

4.1 Health and Safety 

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

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

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

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

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

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

4.2 Cautions 

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

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

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

5 Interferences 

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

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

conditions of analysis by 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 49 of 57 
GLP10-01-02; Interim RePoR?i-"Tient may be used, if current, for 14 days from 06/29/2010 

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

March/April 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 pL connected to a tandem Mass Spectrometer 

(LC/MS/MS). I 

Analytical balance capable of reading to 0.0001 g 

A device to collect raw data for peak integration and quantitation 

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

Gas tight syringes, 25^1, 50|JL, lOOpL, 250IJL, 500pL, 1000|JL. 

1 mL plastic HPLC autovial. 

Disposable pipettes, polypropylene or glass as appropriate 

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

6.2 Chromatographi c System 

Guard Column: Prism RP, 4.6 mm x 50 mm, 5 |jm 

Analytical Column: Betasil CI8,4.6 mm x 100 mm, 5 pm 

Temperature: 10°C 

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

Mobile Phase (B): Methanol 

Gradient Program: 

Time (min) 

0.0 

0.5 

11.0 

13.5 

13.6 

17.0 

%A 

97 

97 

5 

5 

97 

97 

%B 

3 

3 

95 

95 

3 

3 

Flow Rate 

(mL/min) 

1.0 

1.0 

1.0 

1.0 

1.0 

1.0 

Injection Volume: 100 pL 

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

Run Time: ~ 17 minutes. 

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

provided that data quality objectives are met. 

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 50 of 57 
GLPlO-01-02; Interim ReQjffffi-'rnent may be used, if current, for 14 days from 06/29/2010 

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

March/April 2010 

6.3 MS/MS System 

6.3.1 Mode: Electrospray Negative bn, 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 information is intended as a guide, alternate instalments and equipment may be used. 

7 Reagents and Standards 

7.1 Chemicals 

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

Methanol - HPLC grade 

Ammonium Acetate -A.C.S. Reagent Grade 

7.2 Standards 

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

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

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

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

Products, Inc 

Perfluorooctanoic Acid (PFOA - C8 acid); 3M 

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

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

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

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

Perfluorobutanesulfonate (PFBS - C4 sulfonate); 3M 

Perfluorohexanesulfonate (PFHS - C6 sulfonate); 3M 

Perfluorooctanesulfonate (PFOS - C8 sulfonate); 3M 

ETS-8-044.0 Page 6 of 11 

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

Analysis 

Page 51 of 57 
GLPlO-01-02; Interim RePoffS"^ me nt msy be used, if current, for 14 days from 06/29/2010 

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

Marcli/April2010 

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 flask. Transfer to a 

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

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

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

,. X. r X molecular weight of anion 

salt correction factor = ^ 

moclecular weight of salt 

499 

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

538 

10 mg CsFiySOs K* with purity 90% = 8.35mg CsFuSOa" (10 mg*0.90*0.9275=8.35 mg) 

5 (jg/mL (5000 ng/mL) mixed working standard-^dd O.SmL each of the lOOpg/mL SSSs to a lOmL volumetric 

flask and bring up to volume with solvent. 

250 ng/mL mixed working standard—Add 1.25mL of the 5 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 52 of 57 
GLPlO-01-02; Interim RepoRSi^ment may be used, if current, for 14 days from 06/29/2010 

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

March/April 2010 

7.5 Calibration Standards 

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

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

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

than those listed below can be prepared as needed. 

Concentration 

of WS, ng/mL 

125 

125 

125 

125 

250 

250 

250 

250 

5000 

5000 

5000 

Volume Of WS,M L 

10 

15 

20 

30 

20 

50 

100 

200 

25 

50 

100 

Final Volume of 

Calibration Standard (mL 

of ASTM Type 1 Water, or 

other suitable water) 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

Final Concentration of 

Calibration Standard, ng/mL 

(ppb) in ASTM Type 1 Water, 

or other suitable water 

0.025 

0.0375 

0.050 

0.075 

0.100 

0.250 

0.500 

1.00 

2.50 

5.00 

10.0 

8 Sample Handling 

8.1 Water Sample Preparation 

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

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

sample aliquot, or filtered. 

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

prefen-ed over the use of glass autovials, to prevent the possibly of fiuorochemical 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 Analysi s - 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-detemnined 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 determination (r^) value for the calibration curve must be greater than or equal to 0.990. Each 

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

ETS-8-044.0 Page 8 of 11 

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

Analysis 

Page 53 of 57 
GLPlO-01-02; Interim R^offS^ment may be used, if current, for 14 days from 06/29/2010 

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

March/April 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, perform routine maintenance or prepare a new standard 

curve (if necessary) and reanalyze. 

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

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

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

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

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

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

curve should be further diluted and reanalyzed. 

10 Quality Control 

10.1 Data Quality Objectives 

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

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

the raw data and footnoted in the final report. 

10.2 Method Blanks 

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

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

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

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

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

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

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

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

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

10.3 Sample Replicates 

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

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

replicates excludes fleld 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 Detemiination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection 

Analysis 

Page 54 of 57 
GLPlO-01-02; Interim ReQjQSi'J'Tient may be used, if current, for 14 days from 06/29/2010 

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

March/April 2010 

10.6 Field Matrix Spikes / Lab Matrix Spikes 

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

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

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

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

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

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

11 Data Analysis and Calculations 

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

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

A I A. t .1, / IV (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. 

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

If criteria listed in this method perfomnance section are not met, maintenance may be perfomned 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 ^5% and a retention time RSD of ^ % 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 55 of 57 
GLPlO-01-02; Interim Repo(?Sil-iment may be used, if current, for 14 days from 06/29/2010 

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

March/April 2010 

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

standard) and the mass spectral response of unique ions. 

12.3 Sensitivity 

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

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

to Section 10 for additional details. 

12.4 Accurac y 

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

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

spikes and laboratory matrix spikes. 

12.5 Precision 

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

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

requirement for replicates excludes fleld blanks or rinse blanks. 

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

13 Pollution Prevention and Waste Management 

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

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

14 Records 

Each data package generated for a study must include all supporting infomiation 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, instmment acquisition 

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

15 Affected Documents 

None. 

16 Revisions 

Revision 

Number Summary of Changes 

ETS-8-044.0 Page 11 of 11 

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

Analysis 

Page 56 of 57 
GLPlO-01-02; Interim Report 02 

3M Confidential Analysis of PFBS, PFHS, and PFOS in Groundwater Samples from Decatur, AL 

iVIarch/April 2010 

RECORD OF DEVIATION/NONCONFORMANCE 

/. Identification 

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

GLP10-01-02-02 j100517a ETS-8-044.0 

Deviation type D SOP D Equipment Procedure 0 Method 

(Check one) D Protocol IZl GPO D Other. 

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

Method Requirements: 

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

2. Sample/Sample Duplicate RPD S20%. 

3. FMS recovery of 100% ± 30%. 

Actual procedure/process: 

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

(2) The RPD for PFOS for sampling location 331S was 21% . 

(3) The recovery of the FMS High sample for GRS04 for PFOS was 134%. 

///. Actions Talien 

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

Corrective Action (D Yes 0 No) Reference: 

Acceptability of the nonconfonning work: 

1) The branched PFOS when quantitated against calibration curve point prepared from linear 

PFOS have been quantitating around 15-20% higher. The set of 30 ppb branched LCS 

prepared with the samples produced recoveries -170%. The 5 ppb branched LCS recovery 

was within acceptance criteria, suggesting that the 30 ppb average recovery may be in error. 

Three replicates of branched LCS at 5 ppb, 15 ppb, and 30 ppb, prepared with non-study 

samples, were analyzed with the study samples to confirm the higher recovery. The results 

of the additional samples were within the field matrix spike acceptance criteria of 100%±30%. 

All LCS were used in the detennination of the analytical uncertainty. 

2) The RPD value for PFOS for sampling location 331S will be footnoted in the data tables. 

3) Since the method analytical uncertainty for PFOS is 100% ± 44%, no adjustment was made 

to the analytical uncertainty for PFOS on GRS04. 

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

EI Other: Deviations will be noted in final report. 

Project Lead/PAI Approval: Suja n Wolf H ^ Date: . 

Study Director (if GLP): KUXfyj-J / ^ D^^®-

Sponsor Approval (for GLP protocol deviations): NA Date: N, 

Technical Reviewer (optional): NA Date: NA 

W 

Laboratory Department Manager Approval: Date: 

c:/SoAo/rJ 

IV. Authorization to Resume Work 

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

Laboratory Department IVIanager Approval: NA Date: NA 

Deviation No. 

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

Attachment A ETS-4-008.7 Page 1 of 1 

Documentation of Deviations and Control of Nonconforming Testing Page 57 of 57