GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

3M 

GLP10-01-02. Interim Report 10: Analysis of PFBS. PFHS. and PFOS in Groundwater 

Samples Collected at Off-Site Wells located in Decatur. AL in October 2010 

Study Title 

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

Perfluorobutane sulfonate (PFBS) In Groundwater, Soil and Sediment for the 3M Decatur Phase 3 

Site-Related Monitoring Program 

Data Requirement 

EPA TSCA Good Laboratory Practice Standards 40 CFR Part 792 

Study Director 

Jaisimha Kesari P.E., DEE 

Weston Solutions, Inc. 

1400 Weston Way 

Westchester, PA 19380 

Phone: 610-701-3761 

Author 

Susan Wolf 

3M Environmental Laboratory 

Interim Report Completion Date 

Date of signing 

Performing Laboratory 

3M Environmental Health and Safety Operations 

Environmental Laboratory 

3M Center, Bidg 260-05-N-17 

Maplewood, MN 55144 

Project Identification 

GLP10-01-02-10 

Total Number of Pages 

57 

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

Requirements for the Competence of Testing and Calibration Laboratories", in accordance with 

the A2LA Certificate #2052.01. Testing that complies with this International Standard also 

operate in accordance with ISO 9001:2000. 

Certificate #2052.01 

Page 1 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

This page has been reserved for specific country requirements. 

Page 2 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS In Groundwater from Decatur, AL 

October 2010 

GLP CoiviPLiANCE STATEMENT 

Report Title: GLP10-01-02, Interim Report 10. Analysis of PFBS, PFHS, and PFOS in Groundwater 

Samples Collected at Off-Site Wells located in Decatur, AL in October 2010 

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

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

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

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

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

system and no dosing of a test system. 

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

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

Gary Hohenstein; Sponsor Representative Date 

OM^ . 'L 

Jaisimha K^ari, P.E., DEE, Study Director ' Date 

Page 3 of 57 
GLP10-01-02; Interim Report 10 

Analysis of PFBS, PFHS, and PFOS in Grundwater from Decatur, AL 

October 2010 

QUALITY ASSURANCE STATEMENT 

Report Title: GLP10-01-02, Interim Report 10. Analysis of PFBS, PFHS, and PFOS in Groundwater 

Samples Collected at the Off-Site Wells located in Decatur, AL in October 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 report and the accompanying data were audited by the 3M Environmental Laboratory Quality 

Assurance Unit (QAU), as indicated below. The findings were reported to the principal investigator 

(P.I.), laboratory management and study director. 

Inspection Dates 

12/2/10-12/3/10 

Phase 

Data and Interim Report 

Date Reported to 

Testing Facility 

Management 

12/23/10 

Study Director 

12/23/10 

QAU Represrfitative 

^ . ^^ej ^ /-^'f l 

Date 

Page 4 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

TABLE OF CONTENTS 

GLP Compliance statement 3 

Quality Assurance Statement 4 

Table of Contents 5 

List of Tables 6 

1 Study Information 8 

2 Summary 9 

3 Introduction 10 

4 Test & Control Substances 10 

5 Reference Substances 11 

6 Test System 13 

7 Method Summary 13 

7.1 Methods 13 

7.2 Sample Collection 13 

7.3 Sample Preparation 13 

7.4 Analysis 13 

8 Analytical Results 14 

8.1 Calibration 14 

8.2 System Suitability 15 

8.3 Limit of Quantitation (LOQ) 15 

8.4 Continuing Calibration 15 

8.5 Blanks 15 

8.6 Lab Control Spikes (LCSs) 15 

8.7 Analytical Method Uncertainty 17 

8.8 Field Matrix Spikes (FMS) 17 

Page 5 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

9 Data Summary and Discussion 17 

10 Conclusion 26 

11 Data/Sample Retention 26 

12 Attachments 26 

13 Signatures 27 

LIST OF TABLES 

Table 1. Summarized PFBS, PFHS, and PFOS Results (Off-Site Groundwater, Decatur, AL, 

October 2010) 9 

Table 2. Instalment Parameters 14 

Table 3. Liquid Chromatography Conditions 14 

Table 4. Mass Transitions 14 

Table 5. Limit of Quantitation (LOQ) 15 

Table 6. Laboratory Control Spike Recovery 16 

Table 7. Analytical Uncertainty 17 

Table 8. Field Matrix Spike Levels 17 

Table 9. DALGW602L101029 18 

Table 10. DAL GW602S 101029 18 

Table 11. DALGW603L101029 19 

Table 12. DAL GW603S 101028 19 

Table 13. DAL GW604L 101029 20 

Table 14. DAL GW604S 101029 .> 20 

Table 15. DAL GW605R 101029 21 

Table 16. DAL GW605L101029 21 

Table 17. DAL GW607R 101028 22 

Table 18. DAL GW607L 101028 22 

Table 19. DAL GW609R 101027 23 

Table 20. DALGW609L101027 23 

Page 6 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

Table21. DALGW61 IR 101027 24 

Table22. DALGW611L 101027 24 

Table 23. Trip Blank 25 

Table 24. DAL GW 602S RB 101029 25 

Page 7 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS In Groundwater from Decatur, AL 

October 2010 

1 Study.Information ••#*. yf-:- -' " ••' ''^'^ 

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 

Chelsie Grochow; Analyst 

Study Dates 

Study Initiation: March 8, 2010 

Interim Report 10 Experimental Termination: November 09, 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 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

2 Summary 

The 3M Environmental Laboratory received groundwater samples from wells located at Off-Site Wells 

located in Decatur, AL, representing fourteen different sampling locations. A total of forty-five sample 

bottles were received at the 3M Environmental Laboratory for perfluorooctane sulfonate (PFOS), 

perfluorohexane sulfonate (PFHS) and perfluorobutane sulfonate (PFBS) analysis, and included 

duplicate groundwater samples from each sampling location. Samples also included one field matrix 

spike (FMS) samples for each location, one trip blank containing Milli-QTM water, a trip blank spike, and 

one equipment rinseate sample. The equipment rinseate blank did not have FMS samples prepared 

for determination of PFBS, PFHS, and PFOS recovery. The groundwater samples, trip blank and one 

equipment rinseate blank were received from Weston personnel on October 29,2010 and November 

4, 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-10-01-02-10. 

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

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

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

concentration results for all ground waters ranged from 0.0615 ng/mL to 0.480 ng/mL. The PFHS 

concentration results for all ground waters ranged from 0.0396 ng/mL to 0.622 ng/mL. The PFOS 

concentration results for all ground waters ranged from 0.0.0404 ng/mL to 2.41 ng/mL. The method 

uncertainty for PFBS is 100% ± 16%, PFHS 100% ± 16%, and PFOS 100% ± 21%. 

Table 1. Summarized PFOA Results (Off-Site Groundwater, Decatur, AL, October 2010) 

Sample ID 

DAL GW602L 101029 

DAL GW602S 101029 

DALGW603L101029 

DAL GW603S 101028 

DAL GW604L 101029 

DAL GW604S 101029 

DAL GW605R 101029 

DALGW605L101029 

DAL GW607R 101028 

DAL GW607L 101028 

DALGW609L101027 

DAL GW609R 101027 

DAL GW61 IR 101027 

DAL GW61 IL 101027 

Trip Blank (Milli-QTM Water) 

Equipment rinseate blanks 

Avg. PFBS 

Concentration 

(nq/mL) ± RPD 

0.0813 ±0.49% 

0.239 ±12% 

0.112 ±19% 

0.158 ±7.6% 

0.279 ±17% 

0.303 ±14% 

0.119 ±23% [a] 

0.406 ± 0.49% 

0.0870 ±0.12% 

0.0615 ±2.8% 

0.259 ±8.9% 

0.480 ± 14% 

0.191 ±6.3% 

0.317 ±1.3% 

< 0.0250 

< 0.0250 

Avg. PFHS 

Concentration 

(ng/mL) ± RPD 

0.291 ±27% [a] 

0.127 ±6.3% 

0.109 ±14% 

0.122 ±3.3% 

0.215 ±14% 

0.224 ±8.5% 

0.0661 ± 3.2% 

0.622 ±23% [a] 

0.0707 ±13% 

0.0823 ± 38% [al 

0.477 ±1.0% 

0.154 ±37% [a] 

0.0396 ± 32% [a] 

0.167 ±0.60% 

< 0.0250 

< 0.0250 

Avg. PFOS 

Concentration 

(ng/mL) ± RPD 

0.744 ±8.6% 

0.710 ±17% 

0.102 ±5.2% 

0.220 ±6.8% 

1.46 ±3.4% 

0.472 ± 8.9% 

0.0403 [b] 

0.522 ±2.5% 

0.0611 ±4.6% 

0.0920 ±8.2% 

2.41 ± 5.0% [c] 

0.164 ±39% [a] 

0.580 ±7.2% 

0.933 ±5.1% 

< 0.0400 

< 0.0400 

N/A; not applicable 

[a] The sample/sample duplicate RPD was ^0% . 

[b] A RPD could not be calculated as one of the sample replicates was <LOQ. 

[c] Sampling location did not have an appropriate FMS spike level to sufficiently evaluate PFOS 

recovery. 

Page 9 of 57 
GLP10-01-02; Interim Report 10 

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

October 2010 

3 Introduction 

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

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

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

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

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

conducted to analyze ground water samples collected from off-site wells located in Decatur, AL for 

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

The 3M Environmental Laboratory prepared sample bottles (250 mL high-density polyethylene) which 

were shipped to Decatur, AL Weston personnel prior to field sampling. Sample bottle sets for each 

groundwater sampling location included a field sample, field sample duplicate, and a field spike sample. 

Each empty container for groundwater samplings was marked 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, PFHS, and PFOS prior to being sent to the field for 

sample collection. All sample bottles also included the addition of internal standards ^^02-PFBS, ^^02-

PFHS, and ^^C4-PF0S at a nominal concentration of 1 ng/mL. All sample bottles also included the 

addition of surrogate spike "C4-PFOS at a nominal concentration of 0.1 ng/mL. See section 8.8 of the 

report for field matrix spike levels. 

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

Laboratory method ETS-8-044.0 "Determination of Perfluorinated Compounds in Water by High 

Performance Liquid Chromatography/Mass Spectrometry Direct Injection Analysis". 

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

groundwater samples collected, the trip blank, and equipment rinseate samples. Tables 9-24 

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

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

report. 

4 Test & Control Substances 

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

was purely analytical in nature. 

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

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

5 Reference Substances 

The analytical reference substances used for this study are listed below. 

Reference Substance 

Chemical Name 

Chemical Formula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFBS 

(predominantly linear) 

Perfluorobutane sulfonate 

C4F9S03' 

Potassium Salt 

3M 

1/10/2017 

Frozen 

41-2600-8442-5 

TCR-121 

White Powder 

96.7% 

PFHS 

(linear) 

Perfluorohexane sulfonate 

C6F13SO3" 

Sodium Salt 

Wellington 

4/2/2013 

Frozen 

LPFHxSAM08 

TCR08-0018 

Crystalline 

98% 

Reference Substance 

Chemical Name 

Chemical Fomiula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFOS 

(linear) 

Perfluorooctane sulfonate 

CfiFiySOs 

Potassium Salt 

CAS #2795-39-3 

Wellington 

10/18/2013 

Frozen 

LPFOSKBM06 

TCR08-0001 

Crystalline 

98% 

PFOS 

(linear + branched) 

Perfluorooctane sulfonate 

CeFiySOa' 

Potassium Salt 

CAS #2795-39-3 

3M 

12/14/2016 

Frozen 

171 

TCR-696 

White Powder 

86.4% 

Page 11 of 57 
GLP10-01 -02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

Reference Substance 

Chemical Name 

Chemical Formula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

"OjrPFBS 

Labeled - Perfluorobutane 

sulfonate 

C4F9S[''02]0" 

Ammonium Salt 

RTI International 

3/9/2015 

Frozen 

11546-107-2 

TCR-1022,TCR-1028and 

TCR-1033 

Liquid 

99% 

"Oj-PFHS 

Labeled - Perfluorohexane 

sulfonate 

CeFisSrOzj^'QSodium Salt 

Wellington 

04/29/2013 

Frozen 

MPFC-C-0410 

TCR10-0037 

Liquid 

NA'^' 

Reference Substance 

Chemical Name 

Chemical Fomriula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

"C,-PFOS 

Perfluorooctane sulfonate 

CsFiy SO3 

Sodium Salt 

Wellington 

04/29/2013 

Frozen 

MPFC-C-0410 

TCR10-0037 

Liquid 

NA<^> 

(1) Compound is part of a custom mixture of mass-latieled perfluorinated compounds at a concentration of 5.0 pg/mL. 

Page 12 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

6 Test System 

There was not a test system for this study in the classic sense of a GLP study. This study was 

conducted for analysis of ground water samples collected from wells located in Decatur, AL by Weston 

Solutions, Inc. personnel. Samples for this study are "real worid" environmental samples. 

Sample Description Key Code. 

String Number 

Example 

1 

2 

3 

4 

5 

6 

String Descriptor 

DAL GW602S 0101029 

Sample Location 

Sample Type 

Well ID 

Well Level 

Sampling Date 

Sample Type 

Example 

DAL= Decatur, Alabama 

GW= Groundwater 

Example: 602 

R = Residum shallow water-bearing zone 

L = Bedrock water-bearing zine 

S - Epikarst middle water-bearing zone 

101029-October 29,2010 

0=primaiy sample 

DB=duplicate sample 

LS = low spike 

RB = Rinseate Blank 

7 Method Summar y 

7.1 Methods 

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

"Detennination of Perfluorinated Compounds In Water by High Perfomnance 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 returned to the laboratory at ambient conditions on 

October 29, 2010 and November 4, 2010. Samples were stored refrigerated at the laboratory after 

receipt. A set of laboratory prepared Trip Blank and Trip Blank field matrix spike samples 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. 

7.4 Analysi s 

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

perfonnance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). Detailed instmment 

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 in 

Table 2, Table 3 and Table 4. 

Page 13 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

Table 2. Instrument Parameters. 

instrument Name 

Analytical IVIethod Followed 

Analysis Date 

Liquid Chromatograph 

Guard column 

Analytical column 

Injection Volume 

Mass Spectrometer 

Ion Source 

Electrode 

Polarity 

Software 

ETS Ginger 

ETS-8-044.0 

11/08/10 

Agilent 1200 

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

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

25 uL 

Applied Biosystems API 5000 

Turbo Spray 

Turbo Ion electi-ode 

Negative 

Analyst 1.4.2 

Table 3. Liquid Chromatography Conditions. 

step 

Number 

0 

1 

2 

3 

4 

5 

Total Time 

(min) 

0 

1.0 

13.0 

15.0 

15.5 

17.0 

Flow Rate 

(fiUmin) 

750 

750 

750 

750 

750 

750 

PercentA 

(2 mM ammonium acetate) 

97.0 

97.0 

5.0 

5.0 

97.0 

97.0 

PercentS 

(MethanoO 

3.0 

3.0 

95.0 

95.0 

3.0 

3.0 

Table 4. Mass Transitions. 

Analyte 

PFBS 

PFHS 

PFOS 

fC^PFOS surrogate 

Mass Transition 

Q1/Q3 

299/80 

299/99 

399/99 

399/80 

499/99 

499/80 

499/130 

503/80 

Intemal Standard 

t'OgjPFBS 

f'OglPFHS 

t'CJPFOS 

["CslPFOS 

Mass Transition 

Q1/Q3 

303/84 

403/84 

507/80 

507/80 

Dwell time was 50 msec for each transition. The individual transitions were summed to produce a "total ion chromatogram" 

(TIC), which was used for quantitation. 

'SK^'Analytical Results 

8.1 Calibration 

Samples were analyzed against a stable isotope matrix-matched intemal standard calibration curve. 

Calibration standards were prepared by spiking known amounts of the stock solution containing the 

target analytes into laboratory prepared synthetic groundwater containing calcium and magnesium. A 

Page 14 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

total of eleven spiked standards ranging from 0.025 ng/mL to 10 ng/mL (nominal) analyzed. The 0.025 

ng/mL curve point was disabled for PFOS to meet accuracy criteria. A quadratic, 1/x weighted, 

calibration curve of the peak area counts was used to fit the data for each analyte. The data were not 

forced through zero during the fitting process. Calculating the standard concentrations using the peak 

area confinned accuracy of each curve point. 

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

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

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

8.2 System Suitability 

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

demonstrate overall system suitability. All analytes met the acceptance criteria of less than or equal to 

5% relative standard deviation (RSD) for peak ratio and retention time criteria of less than or equal to 2% 

RSD was met for PFBS and PFOS. The area ratio for PFHS was 5.9%. A method deviation is filed with 

the raw data. 

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 5. 

Table 5. Limit of Quantitation (LOQ). 

Analysis Date 

11/08/10 

PFBS 

LOQ, ng/mL 

0.0250 

PFHS 

LOQ, ng/mL 

0.0250 

PFOS 

LOQ, ng/mL 

0.0400 

8.4 Continuing Calibration 

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

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

CCVs met method criteria of 100% ± 25%. 

8.5 Blanks 

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

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

perfonnance to detennine the LOQ for each analyte. Trip blanks reflect the shipping and sample 

collection conditons the sample bottles and samples experience. Equipment rinseate blanks are 

aqueous samples that reflect the efficiency of equipment cleaning in the field between different sample 

collections and are proof of no cross contamination of samples from the equipment. 

8.6 Lab Control Spikes (LCSs) 

Lab control spikes were prepared and analyzed in triplicate at two levels. LCSs were prepared by 

spiking known amounts of the target analytes into 10 mL of laboratory prepared synthetic groundwater 

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

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

100% ± 20% with an RSD <20%, were met for PFBS, PFHS, and linear PFOS. 

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

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

and branched PFOS were prepared at two concentrations to evaluate the potential for analytical bias. 

The linear and branched LCS at both levels did not meet method acceptance criteria with average 

Page 15 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

recoveries of 126% and 122%, respectively. All LCS results were used in the detennination of method 

analytical uncertainty in section 8.7. 

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

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

LCS Percent Recovery = * 100% 

Spike Concentration 

LCS% RSD -• 

standard deviation LCS replicates . 

average LCS recovery 

100% 

Table 6. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Analyzed 11/08/10 

Lab ID 

LCS-101105-1 

LCS-101105-2 

LCS-101105-3 

Average ±%RSD 

LCS-101105-4 

LCS-101105-5 

LCS-101105-6 

Average ±%RSD 

PFBS 

Spiked 

Concentration 

(ng/mL) 

0.198 

0.198 

0.198 

Calculated 

Concentration 

(ng/mL) 

0.200 

0.200 

0.215 

VoRecovery 

101 

101 

109 

104% ±4.5% 

1.98 

1.98 

.1.98 

2.03 

1.82 

2.05 

103 

92.2 

104 

100% ±6.6% 

PFHS 

Spiked 

Concentration 

(ng/mL) 

0A98 

0.198 

0.198 

Calculated 

Concentration 

(ng/mL) 

0.212 

0.207 

0.220 

%Recovery 

107 

105 

111 

108% ±2.8% 

1.99 

1.99 

1.99 

1.96 

1.91 

1.97 

98.6 

95.9 

98.8 

97.8% ±1.7% 

ETS-8-044.0 

^alyzed 11/08/10 

Lab ID 

LCS-101105-1 

LCS-101105-2 

LCS-101105-3 

Average ±%RSD 

LCS-101105-4 

LCS-101105-5 

LCS-101105-6 

Average ±%RSD 

PFOS (linear) 

Spiked 

Concentration 

(ng/mL) 

0.198 

0.198 

0.198 

Calculated 

Concentration 

(ng/mL) 

0.189 

0.208 

0.218 

YoRecovery 

95.6 

105 

110 

104% ±7.1% 

1.98 

1.98 

1.98 

1.97 

1.89 

2.09 

99.3 

95.4 

106 

100% ±5.3% 

Lab ID 

LCS-101105-7 

LCS-101105-8 

LCS-101105-9 

Average ±%RSD 

LCS-101105-10 

LCS-101105-11 

LCS-101105-12 

Average ±%RSD 

PFOS (linear* branched) 

Spiked 

Concentration 

(ng/mL) 

0.196 

0.196 

0.196 

Calculated 

Concentration 

(ng/mL) 

0.256 

0.234 

0.250 

%Recovery 

131 

119 

128 

126% ±5.0%"' 

1.97 

1.97 

1.97 

2.52 

2.42 

2.29 

128 

123 

116 

122% ±4.9%'^' 

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

Page 16 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS In Groundwater from Decatur, AL 

October 2010 

8.7 Analytical Method Uncertainty 

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

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

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

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

corresponds to a confidence level of 95%. 

Table 7. Analytical Uncertainty. 

Analyte 

PFBS 

PFHS 

PFOS 

Standard Deviation 

8.06 

7.99 

10.7 

Method 

Uncertainty 

100%±16% 

100%±16% 

100%±21% 

8.8 Field Matrix Spikes (FMS) 

A field matrix spike sample was collected at each sampling point to verify that the analytical method is 

applicable to the collec:ted 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% c^nfimri that "unknown" components in the sample matrix do not 

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

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

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

Table 8. Field IVIatrix Spike Levels. 

Sampling Location 

All sampling locations 

PFBS, ng/mL 

0.999 

PFHS, ng/mL 

1.00 

PFOS, ng/mL 

0.999 

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

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

Spike Concentraton 

9 Data Summary and Discussion 

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

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

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

from those listed in the raw data. 

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

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

Page 17 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

Tables. DAL GW602L 101029 

3M LIMS ID 

GLP10-01-01-10-024 

GLP10-01-01-10-025 

GLP10-01-01-10-026 

Description 

DAL GW602L 0 101029 

DAL GW602LDB 101029 

DAL GW602LLS 101029 

Average Concentration (ng/mL) ± %RPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.0815 

0.0811 

1.02 

XRecovery 

NA 

NA 

94.0 

0.0813 ng/mL i 0.49% 

PFHS 

Concentration 

(ng/mL) 

0.329 

0.252 

1.33 

VoRecovery 

NA 

NA 

104 

0.291 ng/mL ±17%^^> 

PFOS 

Concentration 

(ng/mL) 

0.712 

0.776 

1.81 

%Recovery 

NA 

NA 

107 

0.744 ng/mL ±8.6% 

NA = Not /Applicable 

(1) The sample/sample duplicate RPD was 220%. 

Table 10. DAL GW 602S 101029 

3MUIVISID 

GLP10-01-01-10-028 

GLP10-01-01-10-029 

GLP10-01-01-10-030 

Description 

DAL GW602S 0 101029 

DAL GW602SDB 101029 

DAL GW602SLS 101029 

Average Concentration (ng/mL) ± %RPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.224 

0.253 

1.48 

XRecovery 

NA 

NA 

124 

0.239 ng/mL ±12% 

PFHS 

Concentration 

(ng/mL) 

0.123 

0.131 

0.944 

%Recovery 

NA 

NA 

81.7 

0.127 ng/mL ±6.3% 

PFOS 

Concentration 

(ng/mL) 

0.648 

0.772 

1.49 

%Recovery 

NA 

NA 

78.1 

0.710 ng/mL ±17% 

NA = Not /Applicable 

Page 18 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

Table 11. DAL GW603L 101029 

3M LIMS ID 

GLP10-01-01-10-034 

GLP10-01-01-10-035 

GLP10-01-01-10-036 

Description 

DAL GW603L 0 101029 

DAL GW603LDB 101029 

DAL GW603LLS 101029 

Average Concentration (ng/mL) ± %RPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.101 

0.122 

1.16 

%Recovery 

NA 

NA 

105 

0.112 ng/mL±19% 

PFHS 

Concentration 

(ng/mL) 

0.101 

0.116 

1.04 

%Recovery 

NA 

NA 

93.2 

0.109 ng/mL ±14% 

PFOS 

Concentration 

(ng/mL) 

0.105 

0.0997 

1.02 

%Recovery 

NA 

NA 

91.9 

0.102 ng/mL ±5.2% 

\ih = Not Applicable 

Table 12. DAL GW 603S 101028 

3I\IIUMSID 

GLP10-01-01-10-021 

GLP10-01-01-10-022 

GLP10-01-01-10-023 

Description 

DAL GW603S 0 101028 

DALGW603SDB 101028 

DAL GW603SLS 101028 

Average Concentration (ng/mL) ± "ARPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.164 

0.152 

1.12 

%Recovery 

NA 

NA 

96.3 

0.158 ng/mL ± 7.6% 

PFHS 

Concentration 

(ng/mL) 

0.124 

0.120 

0.952 

%Recovery 

NA 

NA 

83.0 

0.122 ng/mL ±3.3% 

PFOS 

Concentration 

(ng/mL) 

0.212 

0.227 

0.997 

%Recovery 

NA 

NA 

77.8 

0.220 ng/mL ±6.8% 

NA = Not Applicable 

Page 19 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

Table 13. DAL GW 604L 101029 

3M LIMS ID 

GLP10-01-01-10-037 

GLP10-01-01-10-038 

GLP10-01-01-10-039 

Description 

DAL GW604L 0 101029 

DAL GW604LDB 101029 

DAL GW604LLS 101029 

Average Concentration (ng/mL) ± %RPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.255 

0.302 

1.27 

%Recovery 

NA 

NA 

99.2 

0.279 ng/mL±17% 

PFHS 

Concentration 

(ng/mL) 

0.200 

0.229 

1.29 

%Recovery 

NA 

NA 

108 

0.215 ng/mL ±14% 

PFOS 

Concentration 

(ng/mL) 

1.48 

1.43 

2.32 

%Recovery 

NA 

NA 

86.6 

1.46 ng/mL ±3.4% 

NA = Not Applicable 

Table 14. DAL GW 604S 101029 

3M LIMS ID 

GLP10-01-01-10-040 

GLP10-01-01-10-041 

GLP10-01-01-10-042 

Description 

DAL GW604S 0 101029 

DAL GW604SDB 101029 

DALGW604SLS 101029 

Average Concentration (ng/mL) ± %RPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.324 

0.282 

1.31 

%Recovery 

NA 

NA 

101 

0.303 ng/mL ±14% 

PFHS 

Concentration 

(ng/mL) 

0.214 

0.233 

1.07 

%Recovery 

NA 

NA 

84.7 

0.224 ng/mL ±8.5% 

PFOS 

Concentration 

(ng/mL) 

0.493 

0.451 

1.33 

VoRecovery 

NA 

NA 

85.9 

0.472 ng/mL ±8.9% 

NA = Not Applicable 

Page 20 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

Table 15. DAL GW 605R 101029 

3MUMSID 

GLP10-01-01-10-043 

GLP10-01-01-10-044 

GLP10-01-01-10-045 

Description 

DAL GW605R 0 101029 

DAL GW605RDB 101029 

DAL GW605RLS 101029 

Average Concentration (ng/mL) ± %RPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.105 

0.132 

1.14 

%Recovery 

NA 

NA 

102 

0.119 ng/mL±23%''> 

PFHS 

Concentration 

(ng/mL) 

0.0671 

0.0650 

0.931 

%Recovery 

NA 

NA 

86.5 

0.0661 ng/mL ±3.2% 

PFOS 

Concentration 

(ng/mL) 

<0.0400 

0.0403 

0.952 

%Recovery 

NA 

NA 

91.3 

0.0403 ng/mL^ 

NA = Not Applicable 

(1) Tfie sample/sample duplicate RPD was 220%. 

(2) A RPD could not be calculated as one sample replicate was <LOQ. 

Table 16. DAL GW605L 101029 

3M LIMS ID 

GLP10-01-01-10-031 

GLP10-01-01-10-032 

GLP10-01-01-10-033 

Description 

DAL GW605L 0 101029 

DALGW605LDB 101029 

DAL GW605LLS 101029 

Average Concentration (ng/mL) ± %RPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.407 

0.405 

1.53 

%Recovery 

NA 

NA 

113 

0.406 ng/mL ±0.49% 

PFHS 

Concentration 

(ng/mL) 

0.693 

0.551 

1.89 

%Recovery 

NA 

NA 

127 

0.622 ng/mL ± 23% f^' 

PFOS 

Concentration 

(ng/mL) 

0.528 

0.515 

1.42 

%Recovery 

NA 

NA 

89.9 

0.522 ng/mL ±2.5% 

NA = Not Applicable 

(1) The sample/sample duplicate RPD was 220%. 

Page 21 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

Table 17. DAL GW 607R 101028 

3M LIMS ID 

GLP10-01-01-10-004 

GLP10-01-01-10-005 

GLP10-01-01-10-006 

Description 

DAL GW607R 0 101028 

DALGW607RDB 101028 

DAL GW607RLS 101028 

Average Concentration (ng/mL) ± %RPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.0870 

0.0869 

1.16 

%Recovery 

NA 

NA 

107 

0.0870 ng/mL ±0.12% 

PFHS 

Concentration 

(ng/mL) 

0.0661 

0.0753 

1.11 

VoRecovery 

NA 

NA 

104 

0.0707 ng/mL ±13% 

PFOS 

Concentration 

(ng/mL) 

0.0625 

0.0597 

1.02 

VoRecovery 

NA 

NA 

96.0 

0.0611 ng/mL ±4.6% 

NA = Not Applicable 

Table 18. DAL GW607L 101028 

3M LIMS ID 

GLP10-01-01-10-001 

GLP10-01-01-10-002 

GLP10-01-01-10-003 

Description 

DAL GW607L 0 101028 

DAL GW607LDB 101028 

DAL GW607LLS 101028 

Average Concentration (ng/mL) ± %RPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.0606 

0.0623 

1.12 

VoRecovery 

NA 

NA 

106 

0.0615 ng/mL ±2.8% 

PFHS 

Concentration 

(ng/mL) 

0.0665 

0.0980 

1.04 

VoRecovery 

NA 

NA 

95.8 

0.0823 ng/mL±38Vo^' 

PFOS 

Concentration 

(ng/mL) 

0.0882 

0.0957 

1.06 

VoRecovery 

. NA 

NA 

96.9 

0.0920 ng/mL ±8.2% 

NA = Not Applicable 

(1) The sample/sample duplicate RPD was 220%. 

Page 22 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

Table 19. DAL GW609R 101027 

3M LIMS ID 

GLP10-01-01-10-010 

GLP10-01-01-10-011 

GLP10-01-01-10-012 

Description 

DAL GW609R 0 101027 

DALGW609RDB 101027 

DAL GW609RLS 101027 

Average Concentration (ng/mL) ± %RPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.446 

0.513 

1.71 

VoRecovery 

NA 

NA 

123 

0.480 ng/mL ±14% 

PFHS 

Concentration 

(ng/mL) 

0.125 

0.182 

1.06 

VoRecovery 

NA 

NA 

90.7 

0.154ng/mL ±3r/o^^ 

PFOS 

Concentration 

(ng/mL) 

0.132 

0.196 

1.09 

VoRecovery 

NA 

NA 

92.7 

0.164 ng/mL ±39%^^^ 

NA = Not Applicable 

(1) The sample/sample duplicate RPD was >20%. 

Table 20. DAL GW609L101027 

3MUMSID 

GLP 10-01-01-10-007 

GLP10-01-01-10-008 

GLP 10-01-01-10-009 

Description 

DAL GW609L 0 101027 

DAL GW609LDB 101027 

DALGW609LLS 101027 

Average Concentration (ng/mL) ± %RPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.270 

0.247 

1.36 

%Recovery 

NA 

NA 

110 

0.259 ng/mL ±8.9% 

PFHS 

Concentration 

(ng/mL) 

0.479 

0.474 

1.56 

VoRecovery 

. NA 

NA 

108 

0.477 ng/mL ±1.0% 

PFOS 

Concentration 

(ng/mL) 

2.47 

2.35 

3.55 

VoRecovery 

NA 

NA 

NC 

2.41 ng/mL ±5.0%'^' 

NA = Not Applicable 

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

(1) The sampling location did not have an appropriate FI\/IS to sufficiently evaluate PFOS recovery. 

Page 23 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS In Groundwater from Decatur, AL 

October 2010 

Table 21. DAL GW 61 IR 101027 

3M LIMS ID 

GLP10-01-01-10-013 

GLP10-01-01-10-014 

GLP10-01-01-10-015 

Description 

DAL GW611R 0 101027 

DAL GW611RDB 101027 

DALGW611R LS 101027 

Average Concentration (ng/mL) ± VoRPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.185 

0.197 

1.23 

VoRecovery 

NA 

NA 

104 

0.191 ng/mL ±6.3% 

PFHS 

Concentration 

(ng/mL) 

0.0333 

0.0459 

1.04 

VoRecovery 

NA 

NA 

100 

0.0396 ng/mL ± 32% f^' 

PFOS 

Concentration 

(ng/mL) 

0.559 

0.601 

1.60 

VoRecovery 

NA 

NA 

102 

0.580 ng/mL ±7.2% 

NA = Not Applicable 

(1) The sample/sample duplicate RPD was 220%. 

Table 22. DAL GW 611L 101027 

3M LIMS ID 

GLP10-01-01-10-016 

GLP10-01-01-10-017 

GLP10-01-01-10-018 

Description 

DAL GW611L0 101027 

DALGW611LDB 101027 

DALGW611L LS 101027 

Average Concentration (ng/mL) ± VoRPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.315 

0.319 

1.36 

VoRecovery 

NA 

NA 

104 

0.317 ng/mL ±1.3% 

PFHS 

Concentration 

(ng/mL) 

0.167 

0.166 

1.06 

VoRecovery 

NA 

NA 

89.4 

0.167 ng/mL ±0.60% 

PFOS 

Concentration 

(ng/mL) 

0.957 

0.909 

1.85 

VoRecovery 

NA 

NA 

91.8 

0.933 ng/mL ±5.1% 

NA = Not Applicable 

Page 24 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

Table 23. Trip Blank 

3M LIMS ID 

GLP10-01-01-10-019 

GLP10-01-01-10-020 

Description 

TRIP BLANK SAMPLE 

TRIP BLANK FMS 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

1.05 

VoRecovery 

NA 

105 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

0.932 

%Recovery 

NA 

93.2 

PFOS 

Concentration 

(ng/mL) 

<0.0400 

0.933 

%Recovery 

NA 

93.4 

NA = Not Applicable 

Table 24. DAL GW 602S RB 101029 

3M LIMS ID 

GLP10-01-01-10-027 

Description 

DAL GW602SRB 101029 

PFBS 

Concerttration 

(ng/mL) 

<0.0250 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

PFOS 

Concentration 

(ng/mL) 

<0.0400 

NA = Not Applicable 

Page 25 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

10..emtlusion .{^'MV-: ..^:n?5U., \^?^^'^ " ' :1^^^iC 

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

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

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

11 Data/Sample Retention 

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

to 3M Environmental Laboratory standard operating procedures. 

12 Attachments 

Attachment A: Protocol Amendment 10 (General Project Outline) 

Attachment B: Representative Chromatograms and Calibration Curves 

Attachment C: Analytical Method 

Attachment D: Method Deviation 

Page 26 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS In Groundwater from Decatur, AL 

October 2010 

13 Signatures 

^4)21" I 

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

^^JTT^^O/ / 

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

Gary Hohenitein,/^!^! Sponsor Representative 

// 

l\ 

ou^ 

Date 

ML 

I /Date 

Jaisimha Kes^i^tudy Director 

Page 27 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS In Groundwater from Decatur, AL 

AttachmentA October2010 ^ ,...• , r, .. , ^ . n../, r,.< oo 

Analytical Protocol: GLP10-01-02 

Amendment 10 

Study Title 

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

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

Decatur Phase 3 Site-Related Monitoring Progrann 

PROTOCOL AMENDMENT NO. 10 

Amendment Date: 

October 19, 2010 

Performing Laboratory 

3M Environmental, Health, and Safety Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55144-1000 

Laboratory Project Identification 

GLP10-01-02 

Sampling Event 

Off-Site Phase 3 New Monitoring Wells 

Page 1 of 7 

Page 28 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

Attachment A October 2010 

Analytical Protocol: GLP10-01-02 

Amendment 10 

This amendment modifies the following portion of protocol: 

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

Decatur Phase 3 Site-Related Monitoring Program" 

PROTOCOL READS: 

No changes to the wording of the protocol are required. 

AMEND TO READ: 

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

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

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

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

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

LIMS as project GLPlO-01-02-10 and reported as interim report GLPlO-01-02-10, (reflecting study 

GLP10-01-02 and amendment -10). 

Reason: 

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

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

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

Page 2 of 7 

Page 20 of 57 
Attachment A 

GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 Analytical Protocol: GLP10-01-02 

Amendment 10 

Amendment Approval 

ifti-u w/m^/jj. "A '0 

Gary Hohenstein, Sponsor Representative Date 

Cleston C. Lange, Principal Analytical Investigator ^ D3te 

/ o / '^ o yj>cy a 

William Reagenl EHS Opns Environmental Lab Management 

(M>v// 

Date 

\\kk_ 

I Date Jaisimha Kfesari P.E., DEE, Study Director 

Page 3 of 7 

Page 30 of 57 
Attachment A 

GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

Analytical Protocol: GLP10-01-02 

Amendment 10 

Environmental Health & Safety Operations, Environmental Laboratory 

General Project Outline 

To: Gary Hohenstein, 3M EHS&Opns 

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

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

Cliffton Jacoby, 3M EHS&Opns; Environmental Lab 

Jai Kesari, Weston Solutions 

Charles Young, Weston Solutions 

Tim Frinak, Weston Solutions 

Date: Ocotber 19,2010 

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 10 - Off-Site Phase 3 New 

Monitoring Wells 

1 General Project Information 

Contacts 

Lab Request Number 

Six Digit Department Number 

Project Schedulerrest Dates 

3M Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

Qahohenstein(a)mmm.com 

3M Environmental Laboratory Management 

William K. Reagen 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9739 

wkreaaen(S)mmm.com 

Principal Analytical Investigator 

Cleston Lange 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9860 

cclanaeOmmm.com 

Sampling Coordinator 

Timothy Frinak 

Weston Solutions 

Timothv.frinakiawestonsolutions.com 

Phone: (334)-332-9123 

GLP10-01-02-10 

Dept #530711, Project #0022674449 

Sampling scheduled for the week of October 25, 2010 

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

Page 4 of 7 

Page 31 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

Attachment A October 2010 Analytical Protocol: GLP10-01-02 

Amendment 10 

2 Background Information and Project Objective(s) 

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

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

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

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

Practice Standards 40 CFR 792. 

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

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

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

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

01-02-10. 

3 Project Schedule 

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

25,2010. Sample bottles will be shipped in coolers overnight to 3M Decatur for arrival on Friday, October 22, 

2010. Sample bottles should be stored refrigerated on-site until sample collection. 

Martin Smith \ Weston Trailer 

3M Decatur Plant 

1400 State Docks Road 

Decatur, Alabama 35601 

Page 5 of 7 

Page 32 of 57 
GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

AttachmentA October2010 , .-, ow,^ n.. /in 

Analytical Protocol: GLP10-01-02 

Amendment 10 

4Th Test Parameters e 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. See attachment A for a list of the sampling 

locations that will be collected for this sampling event. For each sampling location, a total of three sample 

bottles will be collected (sample, sample duplicate, and a 1 ng/mL field matrix spike). The "fill to here" line on 

each 250 mL Nalgene bottle will be 200 mL. Two sets of trip blanks consisting of reagent-grade water and a 1 

ng/mL trip blank spike will be prepared at the 3M Environmental Laboratory and sent to the sampling location 

with the other bottles. All sample bottles will include the addition of ^^Oz-PFBS, ^^OrPFHS, and "Ca-PFOS 

(internal standard) at a nominal concentration of 1 ng/mL. All sample bottles will also include the addition of 

^C4-PF0S (surrogate spike) at a nominal concentration of 0.1 ng/mL. One additional bottle will be prepared to 

be used for the preparation of the equipment rinseate blank. A 500mL bottle of laboratory reagent water will be 

sent with the sample bottles to be used to generate the rinseate blank sample. A total of 56 sample bottles will 

be prepared. 

5 Test Methods 

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

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

Analysis". Altemately, samples may be analyzed by ETS 8-154.3 "Determination of Perfluorinated Acids, 

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

Chromatography/Mass Spectrometry". 

The data quality objectives for these studies are quantitative results for the target analytes with an analytical 

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

report and the final accuracy statement may be adjusted accordingly. 

Where applicable, samples will be analyzed against an internal standard calibration curve. Each curve point will 

contain isotopically-labeled perfluorocarboxylic acids and perfluorosulfonic acids at a nominal concentration of 1 

ng/mL. The calibration curve will be generated by taking the ratio of the standard peak area counts over the 

intemal standard peak area counts to fit the data for each analyte. 

6 Reporting Requirements 

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

matrix spike. Trip blank and trip blank spikes will be reported for the sampling event as will any 

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

of sample 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. For those sampling locations where the field matrix spike level was not appropriate, due to 

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

the final report. 

Page 6 of 7 

Page 33 of 57 
Attachment A 

Attachment A 

GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 Analytical Protocol: GLP10-01-02 

Amendment 10 

Bottle Request 

Phase 3 Investigation 

Off-site Phase 3 New Monitoring Wells 

02181.129.108.0001 

DATE REQUESTED: 18 October 2010 

October 2010 

DATE REQUIRED: 25 

This request addresses the bottle requirements for the following wells: 

602R 

602S 

602L 

603R 

603S 

603L 

604R 

604S 

604L 

605R 

605L 

607S 

607L 

609R 

609L 

611R 

611L 

Total Wells: 17 

Sample Summary 

No. of Samples 

17 

1 

2 

Sample Type 

Groundwater 

Rinseate Sample 

Trip Blanks 

Comment 

Will need HPLC water 

Anticipate 1 per cooler 

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

SHIPPING INFORMATION 

Please ship to the following address: 

Martin Smith \ Weston Field Office 

3M Decatur Plant 

1400 State Docks Road 

Decatur, AL 35601 

256-552-6189 

Page 7 of 7 

Page 34 of 57 
Ginge r AG01330509 

Attachment B 

GLP10-01-02; Interim Report 10 

Analysis for PFg^% j?|y^^ ^ P^pgjij^roy^water from Decatur, AL 

October 2010 

g101108a.rdb (PFBS): "Quadratic" Regression ("1 /x " weighting): y = -0.0836 x''2 + 3.58 x + 0.00792 (r = 0.9996) 

0) 

< 

W 

<u 

< 

ra 

28-

27-

26-

25-

24-

23-

22-

2 1 -

20-

19-

18-

17-

16-

15-

14-

13-

12-

1 1-

10-

9-

8-

7-

6-

5-

4-

3-

2-

1-

0-

y 

* ^ 

/ 

/ 

y 

y 

y 

y 

.y 

y 

X 

y ^ 

. - ^ 

^ / " 

,-^'' 

^.-- ^ 

^ 

^/-" ^ 

• ^ 

--• 

-.--•^^'' ^ 

0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 

Analyte Cone. / IS Cone. 

6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 

Data worked up by STW 

Printing Time: 1:35:45 PM 

Printing Date: Monday, January 03, 2011 

Page 1 of 1 

Page 35 of 57 
Ginge r AG01330509 

Attachment B 

GLP10-01-02; Interim Report 10 

Analysis for PFJ^,%J?|y^^^ P|p§ irj^rojjj^water from Decatur, AL 

October 2010 

Data worked up by STW 

Printing Time: 1:36:03 PM 

Printing Date: Monday, January 03, 2011 

Page 1 of 1 

Page 36 of 57 
Ginger AG01330509 

Attachment B 

GLP10-01-02; Interim Report 10 

Analysis for PFj^^S^J^^yq,^. Pffig jij^roy^water from Decatur, AL 

October 2010 

g101108a.rdb (PFOS): "Quadratic" Regression ("1 / x" weighting): y = -0.0313 x*2 -H.6 x -H 0.00885 (r = 0.9996) 

14 

13 

13 

12 

12-: 

till: 

10 

10 

9 

9 

8^ 

8: 

7 

7-

6-i 

6: 

5 

5 

4 

4 

3 

3^ , / 

2 

2 

Ir 

IT 

0: 

./ 

,/ 

0.0 o!5 l.'o l!5 2!o 2^5 3!o 3.5 4.0 4.5 5.0 5.5 6.0 

Analyte Cone. / IS Cone. 

6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 

Data worked up by STW 

Printing Time: 1:36:21 PM 

Printing Date: Monday, January 03, 2011 

Page 1 of 1 

Page 37 of 57 
Ginger AG01330509 

Attachment B 

GLP10-01-02; Interim Report 10 

Analysis for PFg^%J?|yq,^,Pfpgirj^royj^waterfrom Decatur, AL 

October 2010 

I Sample N»m«:-g101108a0ir Sampto ID:-08008-191-r Fito; "glOIIOSa.wifl" 

I P«ak Nama: *MePFOS{IS)' Mass<aB}: -507.0/80.0 amiT 

I Commant'1.0 ng/mL FCstd in Synth. VAbtar* Anrtotation: 

Sample Type : Standard 

Concentration : 0.960 ng/mL 

Calculaca d Cone: N/A 2.8«5 

Acq. Date : ll/S/ZOl O 

Acq. Time: 1:0S:37 PH 

2.6»5 

HDJitiad : 

Froc . ;,lgorUhm : 

Min . PaaK Heigh t 

Min . Peak Vlidth : 

5inootliin<3 Vlidrh : 

RT Vindav : 

EKpei:ted RT: 

Use Relativ e RT: 

Inc . Type : 

Retentio n Time; 

Area : 3 

Height ; 

Star t Tima: 

End Timi : 

Ve-1 

IntelliQ L 

0.00 

0.00 

0 

30.0 

H . 5 

No 

Valle y 

lA. i 

'•1719 cc 

2.866+005 

14.3 

14.e 

cps 

poi n 

nil . 

min 

unt s 

cps 

min 

mm 

lOA 

1 

2.4»5 

2.2e5 

2.0o5 

1.Be5 

1.6e5 

1.4«S 

e.004 

6.0«4 

13.6 13.8 14.2 14.4 14.6 14.8 15.0 15.2 1S.4 

• Sampl«Natna:-g101108aO30- Sampie ID: 

• PaakNamo:-M8PFOS(IS)' Mass(0s) 

Sample Indet : 

Sample Type: 

Concentration : 

Calculata d Cone: 

Acq. L'aca: 

Acq. Tine : 

HodiCisd : 

Proc . Algorithm : 

Mill . Paak Heigh t 

Mir,. Peak Width : 

Sraoothiny Width : 

RT Window: 

Expected BT: 

Use Relativ e RT: 

Int . Type: 

Retentio n Time; 

Haiglit ; 

Star t Time: 

End Timu: 

30 

OC 

LCS-101105-

•507.W80.I 

0.953 nq/mL 

N/A 

11/8/2010 

1:2^XAA PM 

Ya? 

Int^lliQua n -

0.00 sec 

0 pci n 

30.0 sac 

IJ. S min 

No 

Valle v 

H . 5 min 

86930 counts 

3.12e+005 cps 

14.4 min 

14.7 min 

lOA 

3 

1 

' Fila:'fl101108a.Mfr 

amu' 

3.0e5 

2.8e5 

2.6*5 

2.4«5 

2.2«5 

2.0*5 

1.8a5 

1.6«5 

1.4rt 

1.2e5 

l.OoS 

a.Oirf 

6.0»4 

14.4 14.6 14.8 15.0 15.2 15.4 

I

Sampla Name: -glOllOSaOSS" Sampto ID: 'LCS-101105-10' Fila; 'glOl lOSa.wifr 

Paak Namo: 'MSPFOSftSr Mass(es): '507.080.0 amu' 

Commant "Tppb LCS ECP Anrwtstion:" 

Sample Irjctex: 3? 

Sample Typo : OC 

Concentration : 0.S55 nq/mL 

Calculacart Cone: N/A *-*5 ' 

Acq. DaCH: 11/8/2010 

Acq. Time; 10:09:10 PM 3.Be5 

HC'Jifi. 

Hin . peak Width : 

.'Smoothing Hidth : 

RT Window: 

ExpactaiJ RT: 

.telllgua n -

0 . 0 0 cp ! 

0.0 0 se< 

OTe+OOS cp s 

3.6e5 

3.4«5 

3.2e5 

3.0e5 

2.8*5 

2.6*5 

2.4*5 

2.2*5 

2.0*5 

1.8*5 

1.6*5-

1.4*5-

1.2*5 

1.0*5 

8.0*4 

6.0*4 

4.0*4 

2.0*4 

0.O 

I

Sampla Nam*: 'glOl 108a063* SampI* ID: 'GLP1CM)l-02-

Paak Nam*: -M8PF0S(tSr Mass{*s): '507.0/80.0 amu* 

Commant 'DAL GW611L0 101027' Arwotation: " 

Sample Index ; 63 

Sample Type: Unknown 

Concentration : 0.960 nq/mL 

Calculate d Cone: N/A 

Acq. Date : 11/9/2010 

Acq. Time; 5:25:14 AM 

Hodififad : Ves 

Proc- Algorithm : IntelliQua n - IQJ 

Win. Peak Height : 0,00 cps 

Min . Peak Width : 0.00 aec 

Snioothinci Width : 0 point s 

RT Kindov : 30, 0 sec 

E.-pacted RT: It . 5 min 

L'se e l a ! RT: 

14.2 14.4 14.6 14.8 15.0 15.2 15.4 

Data worked up by STW 

Printin g Time: 1:35:20 PM 

Printin g Date : Monday, Januar y 03 , 

Page 1 of 

Page 38 of 57 
Ginge r AG01330509 

Attachment B 

GLP10-01-02; Interim Report 10 

Analysis for PFg,%Ji^y^M':PfP§i'J&?yfi^water from Decatur, AL 

October 2010 

Sampl e Tvpe : 

Concentration : 

Calculate d Cone : 

Acq. Dace : 

Acq. Time : 

Modified : 

Proc . Algorithm ; 

Min. Peak Height : 

Min. Peak Hidth : 

Smoothin g Vlidth : 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time : 

Area : 13! 

Height : 4 

.'n known 

0.36 0 

N/A 

11/9/201 0 

7:32:3 4 Al 

Yes 

IntelliC u 

0.0 0 

0.0 0 

0 

30. 0 

IA. 5 

No 

Valle y 

14. 4 

1636 CO 

.97«+00 5 

I

Sampl* Nam*: 'gl01108a07or San^ * ID: -M*thod BlantT Fda: 'g101108a.Mr 

Paak Nam*: 'MSPFOStlS)' Mass(8s): -507.0/80.0 amu' 

Commant '10 005-181' Annotation: ~ 

4.8*5 

4.6*5-

4.4*5-

4.2*5-

4.0*5 

3.8*5-

3.6*5 

3,4*5 

3.2a5 

3.0*5-

2.8*5 

2.6*5 

2.4*5 

2.2*5-

2.0*5 

1.8*5 

1.6*5 

1.4*5 

1.2*5 

1.0*5 

8.0*4 

6.0*4 

4.0*4 

2.0*4 

0.0 

13.6 13.8 14.2 14.4 14.6 14.8 15.0 15.2 15.4 

I

Sampla Nam«: "glOl lOSaOlS- Sarrvil* ID: -08008-191-8" 

Paak Nama: -MPFBSOSr Mass(M): "303.0/84.0 amu' 

Commant '1.0 ngAnL FC std in Synlh. WMer* Annotation: 

Sampiii Index : 19 

Sampl e Type : Standar d 

Concentration : 0.91 5 nq/mL 

Calculate d Cone : N/A 

Acq. Data : ll/'!/201 0 

Acq. Time : <:05:3 7 PM 

M-Jxiitiod: VflS 

Proc , Algcriclim; IntelliQua n - IQA 

Min. Pnalc Height ; 0.0 0 ep s 

Min, Peak Width : 0,0 0 sa c 

Smijothinrj Width ; 0 pcint s 

RT Window: 30. 0 se c 

Expecte d RT: 12. 1 min 

Use Relativ e RT: No 

Int . Type : Valle y 

Retentio n Time : 12. 1 min 

Area : 251447 counts 

Height : ' .T'^-OOA cp s 

Star t Time : 12. 0 min 

Enrt Time ; 12. 3 min 

11.2 11.4 11.6 11.8 12.0 12.2 1Z4 

I

San^ * Nam*: "glOt 108*030- SampI* ID: 'LCS-IOl 105-4- Fil*: 'glOl lOSa.MfT 

Paak NMtm: -MPFBS(tSr Massfss): "303.0/84.0 amu" 

Commant '2ppb LCS' Annotation: " 

Sampl e Index : 30 

Sampl e Type : yC 

Concentration : 0. 9 63 nq/mL 

Calculate d Cone : N/A 

Acq. Date : 11/8/201 0 

Acq. Time : 1:35:4 4 PM 

MoJifisd : 

Min. Peak Heig! 

Hin. Peak Widtl 

Smoothing Hidtl 

RT Window: 

Expected RT: 

Intel:iQ i 

: 0.0 0 

0.0 0 

Height : 

Star t Tir 

End Time ; 

24796 1 Ci 

9. 12e + 004 

8.0*4 

7.5*4 

7,0*4 

6.5*4-

6.0*4 

5.5*4 

5.0*4 

4.5*4 

f -• 

I 

.0*4 

3.5*4 

3.0*4 

2.5*4 

2,0*4 

1.5*4 

1.0*4 

5000.0 

I

SampI* Nam*: "glOl 108a039- SampI* ID: "LCS-lOl 105-10- Fil*: 'glOllOSa.vwT 

P*ak Nam*: -MPFBS(IS)- Mass(*a): "303.0/84.0 amu' 

Comm*nt "2ppb LCS ECF" Annotation: ~ 

Sampl e Index : 39 

Sampl e Type : QC 

Concentration : 0.97 0 ng/mL 

Calculate d Cone : N/A , 

Acq. Date ; n/?/201 0 7.0*4-

Acq. Time ; 10:09:1 0 PH 

6.5*4 

6.0M 

5.5*4 

5.0*4-

4.5*4 

I 4.0*4 

Modified : 

Proc. Algorith m 

Min . Peak Heigh 

Hin . Peak Width 

5»oothin q Width 

RT Kindo-.*: 

E-pectad BT: 

Use Relativ e RT 

Int . Type: 

R-atention Time ; 

Yea 

IntelliQ . 

: 0.00 

0.00 

0 

30.0 

12. 1 

No 

7a1 le i 

12.1 

Area : 2507^3 ec 

Height : 

3tjr t Time: 

7.30e-004 

12.0 

an -

cps 

sec 

poin t 

min 

unrs 

cps 

min 

11.8 1Z0 12.2 12.4 12.6 12.8 13.0 

Data worked up by STW 

Printin g Time: 1:35:2 1 PM 

Printin g Date : Monday, Januar y 03 , 2011 

Page 2 of 

Page 39 of 57 
Ginge r AG01330509 

Attachment B 

GLP10-01-02; Interim Report 10 

Analysis for PFg^S^J=i|y^^,Pfp§i.jgroy^waterfrom Decatur. AL 

October 2010 

I

SampI* Name: 'g101108a063" Sample ID: "GLP1(M)l-02-1 

P*ak Namo: "MPFBS(IS)" Ma«»(ea): "303.0/84.0 ami/ 

Conim8nt"DALGW611L010102r Annotation:-

Sample Tvpe: 

Calculate d Cone: 

Acq. Dace: 

Acq. Time: 

McdiEied : 

Proc. Algorithm : 

Miri. Peak Height 

Min . PeaK HiJth : 

Srocothing Hidth : 

BT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type: 

Vnknown 

0.975 

N/A 

11/9/2010 

5:25:14 AM 

No 

IntellUju a 

0.00 

0.00 

0 • p 

30.0 

12.1 

No 

Valle y 

End Time: 

I

SampI* Name: -gl01108a0l9' Sample ID:-08008-191-6- Fil«; "glOHOSa.wifr 

Peak Nam*: -MPFHS(IS)- Man{*a): '403.0/84.0 amiT 

Comm*nt -1.0 ng/mL FC std in Synth. Water' Annotation: 

Sample Index : 19 

Sample Type: Standard 

Concenrrari'jn : 0.9-J5 ng/mL 

Calculate d Cone: N/A 

Acq. Date : lI/a/201 0 

Acq. Time: J:05:37 PH 

I

SampI* Nam*: •g101108a070" SampI* ID: "Method Blank- File: -glOl 108a.wifr 

Paak Nam*: -MPFBS(IS)- Ma$s(*s): "303.0/84.0 amu" 

Comm«nt "10 005-181" Annotation:"" 

Sample Inde.'t: 70 

Sampl>* Type : Unknown 

Concentration: 

CaleulatBd C 

Acq, Date: 

Acq. Time: 

H.3diried: 

Ptoc. Alrjcri 

Min. Peak He 

hm: 

qhl 

Min. Peak Width 

.•Jmoothinq Width 

RT Window: 

Expected RT: 

Uae Relative 

Int. Type: 

Retention Ti 

Area; 

H•^ight: 

Start Tin,e! 

End Time: 

RT 

Un known 

0.975 

N/A 

11/9/2010 

7:32:34 AN 

Ye s 

InteliiQua 

! 0.00 

0.00 

0 p 

30.0 

12.1 

rio 

Valley 

12.1 

2363C2 COM 

B.27atO04 

12.0 

12.4 

11.6 12.0 122 12.4 12.6 1Z8 13.0 

Modified: 

Min. Peak Height: 

Min. Peak VFldrh; 

RT Window; 

E.tpectsd RT: 

Use Relativ e RT: 

Int. T\pe: 

No 

SampI* Nam*: "g10l108a030' SampI* ID: "LCS-101105-4- FUe: "g101108a.wir 

Peak Nam*: 'MPFHSOSf Mas»(es): "403.0/84.0 amuComm*nt '2ppb LCS' Annotation:" 

2.5*5 

2.4*5 

2.3*5 

2.2*5 

2.1*5 

2.0*5 

Height: 

Stsrt Tir 

End Time: 

599050 C( 

I.B9e*005 

13 . .5 

Calculated Cone 

Acq. Oaf.: 

Acq. Time: 

Modified: 

proc- Algerichm 

Min. Peak Heigh 

Min- Peak Width 

Smoothing Width 

RT Windo-j: 

E:^peetad RT: 

vaa Relative RT 

Int. Type: 

Retention Time: 

N/ft 

11/9/2010 

7:25:44 P 

No 

IntelliQu 

: 0.00 

0.00 

0 

30.0 

13.6 

No 

Valley 

13.6 

Area: 692646 co 

Haiqhr: 

oCArt Time: 

End Time: 

2.59e-'005 

13.4 

13.8 

1.8*5 

1.7*5-

1.4*5 

1.3*5 

1.2*5-

1.1*5 

1.0*5 

9.0*4 

6,0*4 

7.0*4 

6.0*4 

5.0*4 

4,0*4 

3.0*4 

2.0e4 

1.0*4 

0.0 

13.2 13.4 13.6 13.6 14.0 14.2 14.4 

Data worked up by STW 

Printin g Time: 1:35:2 1 PM 

Printin g Date : Monday, Januar y 03 , 2011 

Page 3 of 

Page 40 of 57 
Ginge r AG01330509 

Attachment B 

GLP10-01-02; Interim Report 10 

Analysis for PFg^%Ji|y^^,P^pgitjgrop^waterfrom Decatur, AL 

October 2010 

1 Sample Nam*:"gl01108a039- Sampto ID:'LCS-101 lOS-lff" File: "gl01108a.v«r 

I Peak Nam*:'MPFHSOSr Ma««(*a):-4O3.Q«4,0 amu" 

I Comm*nt-2ppb LCS ECF- Ajmotation:-

Sample Indax : 39 

Sample Type: QC ,35 g 

Concentration : 0.940 ng/mL 2.2*5 

Calculate d Cone: N/A 

Acq. Data: 11/^/201 0 2.1*5 

Acq. Time: 10:09:10 PH 

2,0*5 

MOslifled: Ves 

Proc . Algorithm : IncelliOua n - lOA 1.9*5 

Hin . Peak Height : 0.00 cps 

Min . Peak Vfidth: 0.00 sec 1.8*5 

Smoothing Width : 0 point s 

RT Window: 30.0 set- 1.7*5 

Expected RT; 13.S min 

Use Relativ e RT: No 1-6*5 

Int . Type: Valle y 1-5*5 

Retentio n Time: 13.S n.in 

Area : 657BS3 count s 1.4«5 

Height : 2.21e-f005 cps 

Star t Time: 13.5 min 1-3«5 

End Time: 13.8 rain ^ ^^^ ^ 

§• 1.1*5 

1 1,0*5 

9,0*4 

8.0 -

7.0*4 

6,0*4 

5,0M 

4,0*4 

3.0*4 

2,0*4 

1,0*4 J 

12.6 12,6 13.0 13.2 13.4 

^ 

13.6 13.8 14.0 14JZ 14.4 

1 Time, min 

I SampI* Name: "g101108a070- SampI* ID:-M.thod Blank- Fil*:"a101108a.Mfr 

I P*ak Name:-UPFHS(1S}" IUUs$(es):-403,0/84.0 amu" 

• Comm*nt-10 005-181- Annotafion:" 

Sample Index : 70 

[ Sample Type: Unknown lis: i 

Concentration : 0.945 ng/mL 

Calculate d Cone: N/A 

Acq. Date: 11/9/2010 3^«5 

Acq. Tliae: 7:32:34 AM 

Modified ; No ^,0*5 

Proc. Algorithm ; IntelliQua n - IQA 

Min . peak Height : 0.00 cps 2 8*5 

Hin . Peak width : 0.00 see 

Smooching Width : 0 point s 

RT Window: 30.0 sec 2.6*5 

Expected RT: 13.5 min 

Use Relativ e RT: No j 4e5 

Ir,t . Type: Valle y 

Retentio n Time: 13,5 min 2.2*5 

Area : 682B05 count s 

Height : 3.37e»005 cps _„ , 

Star t Time: 13.4 min 2.0*5 

End Time: 13.8 min . 

1 1.8*5 

1.6*5 

1.4*5 

1.2*5 

1.0*5 

8.0*4 

6.0*4 

4.0*4 

2.0*4 

l i 6 li e 13.0 13.2 13.4 

1—__ n 

1 

I 13.6 13.8 14.0 14.2 14.4 

1 1 sampto Nam*:-gl01l08a063- Sample ID:"GLPltM)l-02-10^16" File: "glOllOBa.wir 

I Peak Name: -MPrHS<lsr Ma«c<es): "403.0^.0 amu" 

Sampie Inde.t: 53 

Sarnpie Type: Unknown 

Concentration s 0.945 ng/mL 

Calculate d Cone: H/A 25e5 

Acq. Date: 11/9/2010 

Acq. Timet 5:25:14 AM 2.4*5 

Modified : Ye.- 2-3»5 

Proc . Algerithm : Inte l llO'ian - lUA , JBS 

Min . P«ak Height ; 0.00 cps 

Hin . Peak Width : 0.00 sec 2.1*5 

Smoothing Width : 0 pc.lnts 

RT Window: 30.0 sec 2.0*5 

Expected RT: 13.6 min ,- 5 

Use Relativ e RT: tlo 

1.6*5 

Int . Type: Valle y 

Retentio n Tin.e: 13.5 min 1.'"5 

Area : 662912 counts 

H-iight: 2.59et00 5 cps ^'^ ^ 

Star t Time; 13.4 min i.5»5 

End Time: 13.9 min , 

& 1.4.5 

t 1-3*5 Inter 

it 

1.0*5 

9.0e4 

8.0*4 

7.0*4 

6-0*4 

5.0*4 

4.0*4 

3.0*4 

2.0*4 

1.0*4 

1Z6 12.8 13.0 13.: 

1 SamptoNam*:-g101108a019- Sampto ID: "08008-191-8- Fito: "gl01108a.Mr 

I Peak Nam*:-PFBS" Maas(*s):-299.W99.0 amu,299.0/80.0 amu" 

• Comment "I.Oi^j/mLFC std in Synth. Water Annotation: "" 

Sample Index : l<i 

Sample Type; Standar d 

Concentration : 0.969 ng/mL 2.5*5 

Calculate d Cone; 0.944 t.q/mi 

Acq. Date: 11/5/2010 ^,4*5 

Acq. Time: 4:05:3 7 PM 2,3*5 

Modified ; Yes 22*5-

RT Kindo--J; 30.0 sec 

Expected RT: 12. 1 min 2.1*5 

Use Relativ e RT: No „ , 

2.0*5 

Int . Type: Manual ASmS 

Retentio n Time: 12, 1 min ^'^ ^ 

Area : 354206 count s 1.8*5 

Height : 2.51e-'005 cps 

Star t Time: 11.9 min 1-7*5 

End Time: 12.4 min ^ ^ ^ 

1.5*5 

» 1.4*5 

3-

^ 1.3*5 

1 1.2*5 

- 1.1*5 

1.0*5 

9.0*4 

8-0*4 

7.0*4 

6.0*4 

5.0*4 

4,0*4 

3.0*4 

i0* 4 

1.0*4 

11.2 11.4 11.6 

13.54 

I 

• 

13-4 13. m 6 13.8 14.C 

1210 

• 1 As 1.8 1Z0 12.2 12.4 

Time, min 

14.2 14.4 

1Z6 1Z8 13-0 

Data worked up by STW 

Printin g Time: 1:35:22 PM 

Printin g Date ; Monday, Januar y 03 , 2011 

Page 4 of 

Page 41 of 57 
Ginge r AG01330509 

Attachment B 

GLP10-01-02; Interim Report 10 

Analysis for PFj^^^J^^y^^ ^ PfPSl-J^ro^i^water from Decatur, AL 

October 2010 

Sampto Nama:-g101108a030' Sampto 10: "LCS'101105-4" Fito:'gl01108a.Mr 

Peak Nam*: "PFBS" Masses): "299.0/99.0 amu,299.0/80,0 amu* 

Comment "2ppb LCS" Annotation:" 

.<!ample Index : 30 

e Type: QC 

ng/mL 

Manual 

te: 12. : 

mj2T 7 

12.0 12.2 12.4 12.6 12.8 13.0 

I

San»pto Nam*: "g101108a039" Sampto ID; "LCS-IOl 105-10" Fito: "glOl lOea.wiT 

Paak Name: "PFBS" Mass<*s); •299.0ra9.0 amu,299.0/80.0 amu" 

Comment "2ppb LCS ECP Annotation: " 

Sample Type: QC 

Concentratio 

Calculated C 

Acq. Date: 

Acq. Time: 

Modified: 

RT h-indow: 

Expected RT; 

Use Relative 

Int. Type: 

Retention Ti 

Area: 

Height; 

Start Time; 

End Time: 

: 0.00 

nc: 0.0241 

11/9/2D10 

10:09:10 

Ves 

30.0 

12.1 

RT: No 

Manual 

ne: 12-1 

24276 cc 

6.55e*003 

12.0 

12.2 

ng/ 

ng/ 

PH 

min 

cps 

min 

mL 

mL 

1 

6500 

6000 

5500 

5000 

4500 

4000 

3500 

3000 

2500 

2000 

1500 

I

Sample Nam*: •g10110ea063" Sampto ID:"GLPlCK>1-02-ltM)16" FiJ«: 'g101108a.wr 

Paak Nam*: "PFBS' Mass(as}: "299.0/99.0 amu,299-0/80.0 amu" 

Comment-DALGW611L0101027" Annotaton:" 

lample Ir,. 63 

Sample Type; Unknown 

Concentration: N/A 

Calculated Cone: 0.315 ng/mL 

Acq, Date: 11/9/3010 

Acq. Time: 5:25:14 AM 

Mcdifiad: 

Proc. Algorit 

Naise Percent 

Ba?e, Sub. Wi 

Peak-Split. F 

Min. Paak Hel 

Min. Peak Wld 

Pmoorhing Wid 

RT Window: 

Expected RT: 

Heiijht: 

.•^tart Tim. 

End Tim-?: 

No 

8.5*4 

8.0*4 

7.5*4 

7.0*4 

6.5*4-

6.0*4 

5.5*4 

5.0*4 

4.5*4-

4-0*4 

3.5*4 

3.0*4 

2.5*4-

Z0ft4 

1.5*4 

1.0*4 

5000.0 

0.0 

I

Sampto Nam*: "glOl 108a070' Sampto ID: "Mathod Btonk" Fito: "g10l108a.wir 

Paak Nam*: "PFBS" Ma«8(*s): "299.0/99.0 

CortOTwnt "10 005-181" Annotation: " 

Sample Index: 70 

Sample Type: Unknown 

Concentration: N/A 

Calculated Cone: 0.00202 

Acq. Date: 11/9/2010 

7:32:34 AM Acq Time: 

Modified: 

RT Window: 

Exp 

Use 

Int 

Ret 

Helc 

Sta 

End 

cted R 

Relatl 

Type: 

ntion 

ht: 

t Time 

Time: 

12.0 12.2 1Z4 12.6 12.8 13.0 

Tim*, min 

Data worked up by STW 

Printing Time: 1:35:22 PM 

Printing Date: Monday, January 03, 

Page 5 of 

2011 Page 42 of 57 
Ginger AG01330509 

Attachment B 

GLP10-01-02; Interim Report 10 

Analysis for PFg^%J?|y^^^ Pf fig jijgroy^water from Decatur. AL 

October 2010 

I

SampI* Name: "glOIIOSaOl?' Sampto ID: "OeOOS-igi-a" 

Peak Name: "PFHS" Mass{es}: "399.0/99.0 amu,399.0/80.0 

Commant "1.0 nglml FC std in Synth. Water" Annotation: "" 

Sample Tvpe: 

Concentration: 

Calculated Cone 

Ac!!. Date; 

Acq. Time: 

MoJifled: 

Proc. Algorithm 

Min. Peak Heigh 

Min. Peak Width 

Smooching Hidth 

RT Window: 

Expected RT: 

Use Relative RT 

int. Type: 

Retention Time; 

Standard 

1.00 

1.03 

ll/e/2010 

J:05;37 p 

No 

Intellit'u 

: 0.00 

0.00 

0 

30.0 

13.3 

No 

Valley 

13.S 

Area; 144)535 co 

Height: 

Start Tine: 

End Time; 

5.03e-'005 

13.4 

13.e 

5,0*5 

4.8*5 

4,6*5 

4,4*5-

4.2*5 

4.0*5 

3.8*5 

3.6*5 

3.4*5 

3.2*5 

3.0*5 

2.8*5 

2.6*5 

2.4*5 

2.2*5 

2.0e5 

1.8*5 

1.6eS 

1.4*5 

1.2e5 

1.0e5 

8.0*4 

6.0*4 

4.0»4 

2.0*4 

0.0 

1Z6 iza 

_J4^03 

14.0 

I

Sampto Nam*; "glOl 108*030^ Sampto ID: "LCS-10110&4" Fio: "glOllOSa.Mr 

Peak Nam*: "PFHS" Mass<*a}: "399,0/99.0 amu,399.0/80.0 amu" 

Comment "2ppb LCS" Annotation: " 

Saraple Index : 30 

sample Type: QC 

Concentration ; 1.99 nq/mL 

Calculate d Cone: 1.56 ng/mL 

Ac:^. Datu: 11/^/2010 

Acq. Time: 7:25:44 PM 

Proc. Algerithm: 

Min. P.*ak H-iight 

Min. Peak Width: 

Sraccthlng Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

IntelllO 

0.00 

0.00 

0 

•0.0 

n.e No 

Valley 

13.C 

Area: 3137601 = 

I

SampI* Nam*: "g101108a039' Sampto ID: "LCS-IOI105-10* FHe: *gl0110ea.wir 

Peak Name: "PFHS" Mass(es): "399.0/99.0 amu,399.0/80.0 amuComment "2ppb LCS ECF" Annotation: " 

Sample Index : 35 

Sample Type: uC 

Concentration : 0.0 0 ng/mL 

Calculate d Cone: 0-135 ng/mL 

Acq. 

Modified ; 

RT window: 

EKpeeted RT: 

Use Relativ e 

11/8/2010 

10:09:1 0 pr 

Modified : Yea 

BT Kindov : 30.0 

Expected RT: 13. 6 

Use Relativ e RT: No 

Int . Type: Manual 

Retentio n Time: 13.5 

Area : 2T5a44 zi 

Height ; S.36e'0'}4 

Star t Time: 13.3 

End Time: 13.7 

I

Sampto Name:-gl01108a063- Sampto ID: "GLP10-01-02-l(H}ir Fito:-g10ll08a.wir 

Peak Name: "PFHS" Mass{ea): -399.0/99.0 amu,399.0/80.0 anuT 

Comment "OALGW611L0101027* • -

8.0*4 

7.5*4 

7.0e4 

6.5*4 

6.0*4 

5.5*4 

5.0*4 

8. 4.5*4 

2^ 

I 4.0*4 

3.5*4 

3.0*4 

2.5*4 

2.0*4 

1.5*4 

1.0*4 

5000.0 

0.0 

Data worked up by STW 

Printing Time: 1:35:24 PM 

Printing Date: Monday, January 03, 2011 

Page 6 of 

Page 43 of 57 
Ginge r AG01330509 

Attachment B 

GLP10-01-02; Interim Report 10 

Analysis for PFl?e%ii?y^M^:Pfft§i'J&?y<5^w3*^'' ^^ ^ ^^^^ur. AL 

October 2010 

• SampI* Nam*:'g101108a07O- Sampto ID: "Mathod Blank- Fito: -g101108a.wir 

I Paak Nam*: "PFHS" Mas«(es}: "399.0/99.0 Bmu,399.0/80.0 amu" 

m Commant •10005-181- Annotation:"" 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 0.000595 

Acq. Data: 11/9/2010 

Acq- Time: 7:32:34 AM 

I

Sampla Name: 'glOl 108aOig- Sampto ID: -08008-191-6- Fito: 'g101106a.\Mfr 

Peak Narrw: "PFOS" MaM<es}: "499.0/99.0 amu,499,0/80,0 amu.499.0/130.0 amu" 

Comment '1.0 ng/mL FC std In Synth. V^tater' Annotation: "" 

Sampl e Index : 19 

Sampl e Type : Standar d 

Concentration : 0.9 9 3 ng/mL 

Calculate d Cone : 1.0 3 ng/mL 

Acq. Date : 11/8/201 0 

.cq. Ti : 1:05:3 7 PH 

5.0*5 

4.8*5 

4.6*5 

4.4*5 

4.2*5 

4.0*5 

3.6*5 

3.6*5-

3-4*5 

3.2*5 

3.0*5 

28* 5 

I Z6*5 

I 2.4*5 

22* 5 

Z0e5 

1-8*5 

1.6*5 

1.4*5 

1,2*5 

1.0*5 

8.0*4 

6,0*4 

4.0*4 

20* 4 

0.0 

13.6 13.6 14.0 14.2 14.4 14.6 14.6 

I Sampto Nama: -g101108a030' Sampto ID: "LCS-101105-4' Fito: "glOIIOea.wiT 

I Paak Nama:-PFOS" Uass(*a): "499.0/99.0 

1 Comment "2ppb LCS- Annotation: "" 

Sample Index 

Sample Tvpe: 

Concentratl o 

Calculate d C 

Acq. Date : 

Acq. Time; 

h i Window: 

Expected RT: 

Us6 Relativ e 

int . Type: 

Ratantio n T i 

Height.: 

Star t Time; 

End Tim^•: 

30 

y c 

: 1.9B ng/mL 

3nc: 1.97 ng/mL 

11/9/2010 

7:25:44 PH 

30.0 sec 

14.5 min 

RT: No 

Manual 

ae: 14.5 min 

3139568 count s 

l-lletOO e eps 

14.4 min 

14.S min 

arru 

1 

J.499.CV80.0 ar 

1.05*6 

1.00*6 

9.50*5 

9.00*5 

6.50*5 

8.00eS 

7.50e5 

7-00e5 

6.50e5 

6.00e5 

5.S0e5 

5.00e5 

4.50*5 

4.00*5 

3.50*5 

3.00*5 

250*5 

Z00*5 

1.50*5 

1.00*5 

5.00*4 

1 

nu,499.0/130.0 amu" I

Sampto Nam*: "glOl lD8a039- Sampto tD: "LCS-101 lOS-lQ- Fito: "glOl 106a.Mfr 

Paak Name: "PFOS" Mass(*s): "499.0/99.0 amu.499.0/80.0 amu.499.0/130.0 amu" 

Convnant "2ppb LCS ECF" Annobtion: " 

2.5 2 nc 

11/9/201 0 

10!09;1 0 PH 

9.5*5 

9.0*5-

8.5*5 

aOe5 

7.5*5 

7-0*5 

6.5*5 

6.0*5 

^ 5,0*5 

I 4.5*5-

13-6 14.0 14.2 14.4 14.6 14.8 13.6 13.8 14.0 14.2 14.4 14.6 

Data worked up by STW 

Printing Time: 1:35:24 PM 

Printing Date: Monday, January 03, 

Page 7 of 

2011 Page 44 of 57 
*•** Ginge r AG01330509 

Attachment B 

GLP10-01-02; Interim Report 10 

Analysis for PFge%Ji^y^M^:P^ft8i'J&?!J<5^water from Decatur. AL 

October 2010 

1

Sample Nam*: "gl0110aa063" Sampto ID: "GLP1CM)1-02-10-016" Fito:-gl011O8a.w 

Paak Nama: "PFOS" Ma«s(es): "499.0/99.0 amu.499.ora0.0 amu,499.0/130.0 amu" 

Comment" DALGW611L010102r Annotation:-

Sample Index : 63 

j Sampto Name: "glQl 108a070- Sampto ID: -Method StanlT Fito: "g 101108a.wifr 

Sample Tvpe: 

Concentration ; 

Calculate d Cone; 

Acq. Date : 

Acq. Time: 

Modified ; 

RT Window: 

Expected RT: 

Unknown 

N/A 

0.957 

11/9/2010 

5:25:14 At 

Yes 

30.0 

14.5 

Height: 

Stact Tlmi 

End Tlmei 

I Peak Name: "PFOS" Mass(et): "499^0/99.0 

I Comment "10 005-181* Annotation: 

Sample Index: 70 

Sample Type: Unknown 

Concentration: N/A 

Calculated Cone: 0.00517 ni 

Acq. Date: 11/9/2010 

Acq- Time: 7;i2:34 AH 

Height: 

Start 1 

End Tir 

Data worked up by STW 

Printing Time: 1:35:24 PM 

Printing Date: Monday/ January 03, 

Page 

2011 Page 45 of 57 
DocuKgwmdi-efin-a^ib&iWRgiL^rtifocurrent, for 14 days from 01/03/2011 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

Attachment C October 2010 

3M Environmental Laiioratoiy 

Method 

Method of Analysis for the Determination of Perfluorinated Compounds in Water 

by LC/MS/MS; Direct Injection Analysis 

Method Number: ETS-8-044.0 

Adoption Date: Upon Signing 

Effective Date: Q^/f^/o ^ 

Approved By: 

^/>j/o -y 

William K. Reagen, Laboratory Manager Date 

ETS-8-044.0 Page 1 of 11 

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

Injection Analysis Page 46 of 57 
DocuBw?iirt-(ni-02f ifesririj88f)^3rtifocurrent, for 14 days from 01/03/2011 

Analysis for PFBS, PFHS, and PFOS In Groundwater from Decatur, AL 

Attachment C October 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), 

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

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

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

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

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

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

Performance Liquid Chromatography/Mass Spectrometry". 

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

defined QC elements are satisfied. 

Sample collection is not covered under this analytical procedure. 

2 IVIethod Summar y 

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

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

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

This is a performance-based method. Method accuracy is determined for each sample set using multiple 

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

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

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

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

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

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

accuracy for analytical results. 

3 Definitions 

3.1 Calibration Standard 

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

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

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

concentration. 

3.2 Laboratory Duplicate Sample (LDS, or Lab Dup) 

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

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

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

preservation, or storage procedures. 

3.3 Field Blank (FB)/Trip Blank 

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

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

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

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

ETS-8-044.0 Page 2 of 11 

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

Injection Analysis 

Page 47 of 57 
DocusGupii'd-omS'zrite-iftisefirtifocurrent, for 14 days from 01/03/2011 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

Attachment C October 2010 

3.4 Field Duplicate Sample (FDS, Field Dup) 

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

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

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

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

3.5 Field Matrix Spike (FMS) 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

3.7 Laboratory Control Sample (LCS) 

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

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

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

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

each day samples are extracted. 

3.8 Laboratory Matrix Spike (LMS) 

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

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

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

sample matrix must be detennined in a separate aliquot and the measured values in the LMS con-ected 

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 
Docus(Siwrt-(ma2/iteffirM8«f8i)rtifocurrent, for 14 days from 01/03/2011 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

Attachment C October 2010 

3.11 Method Blank 

An aliquot of control matrix that is treated exactly like a laboratory sample including exposure to all 

glassware, equipment, solvents, and reagents that are used with other laboratory samples. The method 

blank is used to detennine if test substances or other interferences are present in the laboratory 

environment, the reagents, or the apparatus. 

3.12 Sample 

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

material. 

3.13 Stock Standard Solution (SSS) 

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

compound. 

3.14 Surrogate 

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

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

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

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

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

quality control measure and is NOT required. 

3.15 Working Standard (WS) 

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

calibration standards and other required analyte solutions. 

4 Warnings and Cautions 

4.1 Health and Safety 

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

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

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

The laboratory is responsible for maintaining a safe wori< environment and a cun-ent awareness of local 

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

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

4.2 Cautions 

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

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

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

5 Interferences 

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

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

conditions of analysis by mnning method blanks. 

ETS-8-044.0 Page 4 of 11 

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

Injection Analysis 

Page 49 of 57 
Attachment C 

DocuBtiie'iirt-OT>s2ritesri«8eiii)rtifocurrent, for 14 days from 01/03/201 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

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

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

caps, autovial caps, HPLC parts, etc. 

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

calibration standards and matrix spikes. 

6 Instrumentation, Supplies, and Equipment 

6.1 Instrumentation and Equipment 

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

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

(LC/MS/MS). I 

Analytical balance capable of reading to 0.0001 g 

A device to collect raw data for peak integration and quantitation 

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

Gas tight syringes, 25pL, 50[JL, lOOpL, 250|JL, 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 ijm 

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

Temperature: 10°C 

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

Mobile Phase (B): Methanol 

Gradient Program: 

Time (min) 

0.0 

0.5 

11.0 

13.5 

13.6 

17.0 

%A 

97 

97 

5 

5 

97 

97 

%B 

3 

3 

95 

95 

3 

3 

Flow Rate 

(mL/min) 

1.0 

1.0 

1.0 

1.0 

1.0 

1.0 

Injection Volume: 100 pL 

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

Run Time: ~ 17 minutes. 

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

provided that data quality objectives are met. 

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 
Attachment C 

Docui(iniE'irt-OT>e2iite8'i«gs#,rtffocurrent, for 14 days from 01/03/2011 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

6.3 MS/MS System 

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

Analyte 

PFBA 

PFPeA 

PFHA 

PFHpA 

PFOA 

PFNA 

PFDA 

PFUnA 

PFDoA 

PFBS 

PFHS 

PFOS 

Transition Monitored 

213^169 

263^219 

313 ^269 and 313 ^119 

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

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

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

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

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

613 -> 569, 613 -^ 169 and 613 ^ 319 

299 -^ 80 and 299 -^ 99 

399 ^ 80 and 399 -> 99 

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

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

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

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

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

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

7 Reagents and Standards 

7.1 Chemicals 

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

Methanol - HPLC grade 

Ammonium Acetate -A.C.S. Reagent Grade 

7.2 Standards 

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

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

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

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

Products, Inc 

Perfluorooctanoic Acid (PFOA - C8 acid); 3M 

Perfiuorononanoic 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 
Docui(iiia?iiKl-0m82/itea-i«K^rtif6current, for 14 days from 01703/2011 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

Attachment C October 2010 

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

used. 

7.3 Reagent Preparation 

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

water. 

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

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

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

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

when diluting stock solutions to appropriate levels. 

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

purity^ and dilute to lOOmL with methanol or other suitable solvent, in a lOOmL volumetric flask. Transfer to a 

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

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

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

^. , ^ molecular weight of anion 

salt correction factor = = 

moclecular weight of salt 

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

538 

10 mg CaFiySOa'lC with purity 90% = 8.35mg C8F17SO3' (10 mg*0.90*0.9275=8.35 mg) 

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

flask and bring up to volume with solvent. 

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

volumetric flask and bring up to volume with solvent. 

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

flask and bring up to volume with solvent. 

Storage Conditions—Store all SSSs and wori<ing standards in accordance with laboratory standard operating 

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

ETS-8-044.0 Page 7 of 11 

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

Analysis 

Page 52 of 57 
Attachment C 

Docu;Giii!?iiid(-0ii-e2nk»i«8aiil)rtifocurrent, for 14 days from 0 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

1/03/2011 

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.fiL 

10 

15 

20 

30 

20 

50 

100 

200 

25 

50 

100 

Final Volume of 

Calibration Standard (mL 

of ASTM Type 1 Water, or 

other suitable water) 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

Final Concentration of 

Calibration Standard, ng/mL 

(ppb) in ASTIVI Type 1 Water, 

or other suitable water 

0.025 

0.0375 

0.050 

0.075 

0.100 

0.250 

0.500 

1.00 

2.50 

5,00 

10.0 

8 Sample Handling 

8.1 Water Sample Preparation 

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

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

sample aliquot, or filtered. 

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

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

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

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

Prepare at least five method blanks. 

9 Sampie Analysis-LC/MS/MS 

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

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

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

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

thoroughly documented in the raw data. 

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

appropriate to the data or because they did not meet the pre-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 Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection 

Analysis 

Page 53 of 57 
Docimwxtl-9TSBj\kmm'mi4>miccmient for 14 days from 01/03/2011 

Analysis for PFBS, PFHS, and PFOS In Groundwater from Decatur, AL 

Attachment C October 2010 

be within ±30%. Justification for exclusion of calibration curve points will be noted in the raw data. A minimum of 6 

points will be used to constmct the calibration curve. 

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

curve (if necessary) and reanalyze. 

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

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

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

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

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

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

curve should be further diluted and reanalyzed. 

10 Quality Control 

10.1 Data Quality Objectives 

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

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

the raw data and footnoted in the final report. 

10.2 Method Blanks 

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

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

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

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

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

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

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

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

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

10.3 Sample Replicates 

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

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

replicates excludes field blanks. 

10.4 Surrogate Spikes 

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

10.5 Lab Control Sample 

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

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

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

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

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

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

ETS-8-044.0 Page 9 of 11 

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

Analysis 

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Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

Attachment C October 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 determine 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 iDy an appropriate software program: 

A 11 r J/ , ,x (Peak Area-Intercept) ^rAnalyte 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. 

P _ 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. 

Nonconfonnance 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 performed on the system and 

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

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

discussed in the text of the report. 

12.1 System Suitability 

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

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

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

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

have area counts with an RSD of 25% and a retention time RSD of S2% to be compliant. 

12.2 Quantitation 

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

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

the LLOQ, which may be within ±30%. 

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

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

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

bracketed by CCVs not meeting these criteria must be reanalyzed. 

ETS-8-044.0 Page 10 of 11 

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

Analysis 

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Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

Attachment C October 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 Accuracy 

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

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

spikes and laboratory matrix spikes. 

12.5 Precision 

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

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

requirement for replicates excludes field blanks or rinse blanks. 

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

13 Pollution Prevention and Waste Management 

Waste generated when perfomriing 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 information for reconstruction of the data. 

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

sample and standard prep sheets/records, instmment run 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 
^McfffflS^l^ntial 

GLP10-01-02; Interim Report 10 

Analysis for PFBS, PFHS, and PFOS in Groundwater from Decatur, AL 

October 2010 

RECORD OF DEVIATION/NONCONFORMANCE 

/. Identification 

Study / Project No. 

GLPlO-01-02-10 

Date(s) of Occurrence: 

11/8/10-g101108a 

I Document 

! ETS-8-044 

Number: 

0 

Deviation type 0 SOP D Equipment Procedure IZi Method 

(Check one) D Protocol D GPO D Other: 

//. Description (attach extra pages as needed) 

Method Requirements: 

(1) System suitability area count RSD <5%, retention time RSD <2% 

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

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

Actual procedure/p^^^^^^^ 

(1) Area ratios were used in place of area counts since the calibration curve was generated using Internal 

standard area ratios. The area ratio RSD for PFHS was just outside method acceptance criteria at 

5.9%. 

(2) LCS average recovery for both sets of linear and branched PFOS were outside method acceptance 

criteria with average recoveries of 126% and 122%. 

(3) The RPD value for several sampling locations were >20% 

IIL Actions Taken 

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

Corrective Action (D Yes 0 No) Reference: 

Acceptability of the nonconforming work: 

1) System suitability - Other QC items were used to assess data accuracy for PFHS, which had area ratio 

RSDs outside method acceptance criteria - calibration curve point accuracy, curve fit criteria, CCV, and 

LCS and FMS recoveries, all meeting method acceptance criteria. 

2) In general, the ECF LCS for PFOA and PFOS have been running 1.5-20% higher when quantitated using 

linear PFOA and PFOS. LCS recoveries <130% for ECF PFOA and PFOS are within FMS acceptance 

criteria of 100% ± 30% for ETS-8-044.0. All LCS were used in the determination of method uncertainty. 

3) Sampling locations with RPD values >20% will be footnoted in the data tables. 

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

IZI Other: Deviations will be noted in final report 

Ml 

Project Lead/PA! Approval: S 

Study Director (if GLP): 

Date ^ 1 1 

Date: 

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

Technical Reviewer (optional): NA Date: NA 

Laboratory Department Manager Approval: Date: 

ly. Authorization to Resume Work 

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

Laboratory Department Manager Approval: NA I 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 l^ofj 

Documentation of Deviations and Control of Nonconforming Testing, 

Page 57 of 57