GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

GLP10-01-02: Interim Report 16 - Analysis of PFBS. PFHS. and PFOS in Groundwater 

Samples Collected as Part of the Avenue A investigation Area in Decatur. AL in January 

2011 

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, MM 55144 

Project Identification 

GLP10-01-02-16 

Total Number of Pages 

61 

^•• ^ |H[^ Tlie testing reported herein meet the requirements of ISO/IEC 17025-2005 "General Requirements for the 

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

[ACCH^ii^T EPJ Testing that complies with this International Standard also operate In accordance with ISO 9001:2000. 

Testing Cert #2052.01 

Page 1 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

This page has been reserved for specific country requirements. 

Page 2 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

GLP COMPLIANCE STATEMENT 

Report Title: Interim Report 16 Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Collected as Part of the Avenue A Investigation Area in Decatur, AL in January 2011. 

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

Perfluorobutane Sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 

Site-Related Monitoring Program. 

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

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

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

system and no dosing of a test system. 

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

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

Gary Hohemstein, Sponsor Representative Date 

% M( 

Jaisimha Kesari, P.E., DEE, Study Director J i J Date 

Page 3 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

QUALITY ASSURANCE STATEMENT 

Report Title: Interim Report 16 Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Collected as Part of the Avenue A Investigation Area in Decatur, AL in January 2011. 

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

Perfluorobutane Sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 

Site-Related Monitoring Program. 

This analytical phase was audited by the 3M Environmental Laboratory Quality Assurance Unit (QAU), 

as indicated in the following table. The findings were reported to the principal investigator (P.I.), 

laboratory management and study director. 

Inspection Dates 

3/18/11 

Phase 

Data and Interim Report 

Date Reported to 

Testing Facility 

Management 

3/29/11 

Study Director 

3/29/11 

^-^-( f 

QAU Representative 

Page 4 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

TABLE OF CONTENTS 

GLP Compliance statement 3 

Quality Assurance Statement 4 

Table of Contents 5 

List of Tables 6 

1 Study Information 7 

2 Summary 8 

3 Introduction 8 

4 Test & Control Substances 9 

5 Reference Substances 9 

6 Test System 1 

7 Method Summary 1 

7.1 Methods 1 

7.2 Sample Collection 1 

7.3 Sample Preparation 1 

7.4 Analysis 12 

8 Analytical Results 13 

8.1 Calibration 13 

8.2 System Suitability 13 

8.3 Limit of Quantitation (LOQ) 14 

8.4 Continuing Calibration 14 

8.5 Blanks 14 

8.6 . Lab Control Spikes (LCSs) 14 

8.7 Analytical Method Uncertainty 17 

8.9 Field Matrix Spikes (FMS) 18 

9 Data Summary and Discussion 18 

Page 5 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

10 Conclusion 22 

11 Data/Sample Retention 22 

12 /attachments 22 

13 Signatures 23 

LIST OF TABLES 

Table 1. Summarized PFBS, PFHS, and PFOS Results (Avenue A Investigation, Jan 2011) 8 

Table 2. Sample Description Key Code 11 

Table 3. Instmment Parameters 12 

Table 4. Liquid Chromatography Conditions 12 

Tables. Mass Transitions 13 

Table 6. Limit of Quantitation (LOQ) 14 

Table 7. Laboratory Control Spike Recovery 16 

Table 8. Analytical Uncertainty 18 

Table 9. DAL GW SS22 270111 19 

Table 10. DAL GW SS24 270111 19 

Table 11. DAL GW 21 OR 280111 20 

Table 12. Trip Blank 20 

Table 13. Rinseate Blank 21 

Page 6 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

1 Study Information 

Sponsor 

3M Company 

Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

Study Director 

Jaisimha Kesari, P.E., DEE 

Weston Solutions, Inc. 

Westchester, PA 19380 

Phone:(610)701-3761 

Fax:(610)701-7401 

j.kesari(gwestonsolutions.com 

Study Location 

Testing Facility 

3M EHS Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55106 

Study Personnel 

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

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

Susan Wolf, 3M Analyst 

Chelsie Grochow; Analyst 

Jon Steege; Analyst 

Kevin Eich; Analyst 

Study Dates 

Study Initiation: March 8,2010 

Interim Report 16 Experimental Termination: March 11, 2011 

Interim Report Completion: Date of Interim Report Signing 

Location of Archives 

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

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

standard retain samples are archived at the 3M Environmental Laboratory according to 40 CFR 

Part 792 

Page 7 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS In Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

2 Summary 

The 3M Environmental Laboratory received water samples collected as part of the Avenue A 

Investigation area in Decatur, AL from three sampling locations. A total of twenty-one sample bottles 

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

perfluorohexane sulfonate (PFHS) and perfluorobutane sulfonate (PFBS), and included duplicate water 

samples from each sampling location, as well as three field matrix spike (FMS) samples for each 

location. Samples also included one trip blank containing Milli-QTM water and appropriate trip blank 

spikes, and one equipment rinseate. The equipment rinseate blank did not have FMS samples 

prepared for determination of PFBS, PFHS, and PFOS recovery. 

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

February 1,2011. All water samples for this project were logged under GLP10-01-01-16. 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-10-01-02-16. 

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

equipment rinseate and trip blank were below the lower limit of quantitation (LLOQ) collected with the 

water samples for GLP10-01-02-16, indicating adequate control of sample contamination during 

shipping and sample collections. The PFBS concentration results ranged from 3.39 ng/mL to 43.2 

ng/mL. The PFHS concentration ranged from 1.84 ng/mL to 309 ng/mL. The PFOS concentration 

results ranged from 8.62 ng/mL to 539 ng/mL. 

Table 1. Summarized PFBS, PFHS, and PFOS Results (Avenue A Investigation, Jan 2011). 

Sampling Location 

DAL GW SS22 270111 

DAL GW SS24 270111 

DALGW210R280111 

Trip Blank (Milli-QTM Water) 

Equipment rinseate blank 

PFBS 

Avg. Cone. 

(ng/mL) ± RPD 

3.39 ± 5.3% 

19.2 ±3.1 % 

43.2 ± 2.8% 

<0.0250 

<0.0250 

PFHS 

Avg. Cone. 

(ng/mL) ± RPD 

1.84 ±6.5% 

143 ±2.8% 

309 ±1.9% 

<0.0250 

<0.0250 

PFOS 

Avg. Cone. 

(ng/mL) ± RPD 

8.62 ±1.2% 

500 ± 5.8% '^' 

539 ± 6.3% '^' 

<0.0300 

<0.0300 

The analytical method uncertainties associated with the reported results are as follows: PFBS ± 20%, PFHS ± 22%, and PFOS ± 

33%. 

(1) Sampling location did not have an appropriate FMS spike level for PFOS to accurately assess analyte recovery. 

(2) Sample field matrix spike recovery did not meet acceptance criteria of 100 ± 30% with a recovery of 68.1%. The FMS 

recovery is within the analytical method uncertainty. 

3 Introduction 

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

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

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

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

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

Page 8 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

conducted to analyze ground water samples collected as part of the Avenue A Investigation in Decatur, 

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

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

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

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

spike samples. Each empty container was 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 (linear), PFHS (linear), and PFOS (linear) prior to being sent to 

the field for sample collection. See section 8.8 of the report for field matrix spike levels. 

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

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

Peri'ormance Liquid Chromatography/Mass Spectrometry Direct Injection Analysis". 

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

collected, trip blank, and groundwater-equipment rinseate sample. Tables 9-13 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 r' . .'.: ' = 

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

was purely analytical in nature. 

[5 Reference Substances, ' ^ 

Reference Substance 

Chemical Name 

Chemical Fomiula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFBS 

(predominantly linear) 

Perfluorobutane sulfonate 

C4F9SO3" 

Potassium Salt 

3M 

1/10/2017 

Frozen 

41-2600-8442-5 

TCR-121 

White Powder 

96.7% 

PFHS 

(linear) 

Perfluorohexane sulfonate 

CeF-isSOa 

Sodium Salt 

Wellington 

3/25/18 

Frozen 

LPFHxSAMOS 

TCR08-0018 

Crystalline 

98% 

Page 9 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Chemical Name 

Chemical Formula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFOS 

(linear) 

Perfluorooctane sulfonate 

CflFiySOs 

Potassium Salt 

CAS #2795-39-3 

Wellington 

10/18/2013 

Frozen 

LPFOSKBM06 

TCR08-0001 

Crystalline 

98% 

PFOS 

Perfluorooctane sulfonate 

CsFiySOs 

Potassium Salt 

CAS #2795-39-3 

3M 

12/14/2016 

Frozen 

171 

TCR-696 

White Powder 

86.4% 

Reference Substance 

Chemical Name 

Chemical Formula 

Identifier 

Source 

Expirat'on Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

"C,-PFOS 

Perfluorooctane sulfonate 

CsFiy SO3 

Sodium Salt 

Wellington 

9/28/13 

Frozen 

092310 

TCR10-0048 

Liquid 

98% 

Page 10 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

6 Test System 

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

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

not dosed with a specific lot of test substance. 

Table 2. Sample Description Key Code. 

String Number 

Example 

1 

2 

3 

4 

5 

String Descriptor Example 

DAL SWSS24 0270111 

Sample Location 

Sample Type 

Location ID 

Sampling Date 

Sample Type 

DAL=Decatur, Alabama 

GW=Gmun(lwater 

Example: SS24 

270111-January 27,2011 

0=primary sample 

DB=duplicate sample 

LS = low spike 

IVIS = mid spike 

HS = high spike 

RB = Rinseate Blank 

7 Method Summary 

7.1 Methods 

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

"Determination of Perfluorinated Compounds In Water by High Performance Liquid 

Chromatography/Mass Spectrometry Direct Injection Analysis". 

7.2 Sample Collection 

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

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

February 1, 2011. Samples were stored refrigerated at the laboratory after receipt. The laboratory 

prepared Trip Blank and Trip Blank fleld matrix spikes were received with the sample collection bottles. 

7.3 Sample Preparation 

All groundwater samples were initiall prepared by diluting ImL sample with 9 mLs of Milli-Q water 

(dilution 1:10). Sampling locations DAL GWSS24 and DAL GW210R required further dilution for PFOS 

and were prepared by diluting 0.1 mL of sample with 9.9 mLs of Milli Q water (dilution 1:100). 

Trip Blank and Rinseate Samples: Samples were prepared by removing an aliquot of the well mixed 

sample and placing it in an autovial for analysis. 

Sampling location DAL GW SS22 was analyzed for PFOS by removing a measured volume of sample, 

adding internal standard, and placing an aliquot of the preapred sample into an autovial for analysis. 

Page 11 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

7.4 Analysis 

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

perfomnance liquid chromatography/ tandem mass spectrometry (HPLC/MS/MS). Detailed instrument 

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

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

Table 3. Instrument Parameters. 

Instrument Name 

Analytical Method Followed 

Analysis Date 

Liquid Chromatograph 

Guard column 

Analytical column 

Injection Volume 

Mass Spectrometer 

Ion Source 

Electrode 

Polarity 

Software 

ETS Ginger 

ETS-8-044.0 

2/11/11,2/28/11 

Agilent 1100 

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

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

2or10nL 

Applied Biosystems API 5000 

Turbo Spray 

Turbo Ion electrode 

Negative 

Analyst 1.4.2 

ETS Buster 

ETS-8-044.0 

3/10/11 

Agilent 1100 

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

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

5|iL 

Applied Biosystems API 4000 

Turbo Spray 

Turbo ion electrode 

Negative 

Analyst 1.4.2 

Table 4. Liquid Chromatography Conditions. 

step 

Number 

Total Time 

(min) 

Flow Rate 

(fiUmin) 

Percent A 

(2 mM ammonium acetate) 

Percent B 

(Methanol} 

ETS-8-044.0 Analysis (ETS Ginger) 

0 

1 

2 

3 

4 

5 

0 

2.0 

11.0 

14.0 

14.5 

17.0 

300 

300 

300 

300 

300 

300 

ETS-8-044.0 Anah 

0 

1 

2 

3 

4 

5 

0 

2.0 

11.0 

13.5 

14.0 

17.0 

300 

300 

300 

300 

300 

300 

97.0 

97.0 

5.0 

5.0 

97.0 

97.0 

3.0 

3.0 

95.0 

95.0 

3.0 

3.0 

/sis (ETS Buster) 

97.0 

97.0 

5.0 

5.0 

97.0 

97.0 

3.0 

3.0 

95.0 

95.0 

3.0 

3.0 

Page 12 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Table 5. IVIass Transitions. 

Analyte 

PFBS 

PFHS 

PFOS 

Mass Transition 

Q1/Q3 

299/80 

299/99 

399/80 

399/99 

499/80 

499/99 

499/130 

Reference Material 

Structure 

Linear 

Linear 

Unear 

Intemal Standard 

NA 

NA 

t"CJPFOS"> 

Mass Transition 

Q1/Q3 

NA 

NA 

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. 

NA = Not Applicable; internal standard not used for quantitation. 

(1) PFOS intemal standard only used for 3/10/11 analysis. 

8 Analytical Results 

8.1 Calibration 

2/11/11 and 2/28/11 Analysis: Samples were analyzed against an external standard calibration curve. 

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

target analytes into prepared in Milli Q water or Synthetic Groundwater. A total of sixteen spiked 

standards ranging from 0.025 ng/mL to 100 ng/mL (nominal) were analyzed. Low curve points were 

disabled as needed to meet calibration acceptance criteria. A quadratic, 1/x weighted, calibration curve 

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

zero during the fitting process. Calculating the standard concentrations using the peak area confinned 

accuracy of each curve point. 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) and a correlation coefficient (r) greater than 0.995, were met for PFBS, PFHS, and 

PFOS. 

3/10/11 Analysis: Sampling location DAL GW SS22 was analyzed against a stable isotope intemal 

standard calibration curve for PFOS. Calibration standards were prepared by spiking known amounts 

of the stock solution containing the target analytes into a laboratory-prepared synthetic groundwater 

containing calcium and magnesium. A separate intemal standard spiking solution was prepared and 

an aliquot was added at the same level to all calibration standards and laboratory control samples at a 

nominal concentration of 1 ng/mL. A calibration curve ranging from 0.025 ng/mL to 100 ng/mL 

(nominal) was analyzed. Low curve points were disabled for PFOS to meet method accuracy or 

method blank criteria. The data were not forced through zero during the fitting process. Calculating the 

standard concentrations using the peak area ratios and the resultant calibration curve 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) and a correlation coeflicient (r) greater than 0.995, were met for PFOS. 

8.2 System Suitability 

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

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

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

met for PFBS, PFHS, and PFOS. 

Page 13 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

8.3 Limit of Quantitation (LOQ) 

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

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

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

Table 6. Limit of Quantitation (LOQ). 

Analysis Date 

2/11/11 

2/28/11 

3/10/11 

Dilutiort 

1 

10 

100 

1 

PFBS 

LOQ, ng/mL 

0.0250 

0.250 

NA 

NA 

PFHS 

LOQ, ng/mL 

0.0250 

0.250 

NA 

NA 

PFOS 

LOQ, ng/mL 

0.0300 

0.300 

2.50 

0.250 

NA = Not Applicable 

8.4 Continuing Calibration 

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

analyzed to confirm that the instrument 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: procedural blanks, field/trip blank, 

and equipment blank. Procedural blank results were reviewed and used to evaluate method 

performance and to determine the LOQ for each analyte. 

8.6 Lab Control Spikes (LCSs) 

Lab control spikes were prepared and analyzed in triplicate with each preparation set. LCSs were 

prepared by spiking known amounts of the analyte into 10 mL of Milli Q water to produce the desired 

concentration. The spiked water samples were then prepared and analyzed in the same manner as the 

samples. The method acceptance criteria states that the average of LCS at each level should be within 

100% ± 20% with an RSD ^20%. 

2/11/11 Analysis: Three spike levels were prepared and met method acceptance criteria for PFBS, 

PFHS, and PFOS (linear). 

2/28/11 Analysis: Three spike levels were prepared and met method acceptance criteria for PFOS 

(linear). 

3/10/11 Analysis: Two spike levels were prepared and met method acceptance criteria for PFOS 

(linear). 

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

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

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

2/11/11 Analysis: Three spike levels LCS (linear + branched) were prepared. The low and mid set of 

LCS met method acceptance criteria, while the high set of LCS did not meet method acceptance criteria 

with an average recovery of 133%. 

2/28/11 Analysis: Three spike levels LCS (linear + branched) were prepared. The low and mid set of 

LCS (linear + branched) met method acceptance criteria, while the high set of LCS did not meet method 

acceptance criteria with an average recovery of 125%. 

Page 14 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

3/10/11 Analysis: Two spike levels LCS (linear + branched) were prepared and met method acceptance 

criteria for PFOS. 

The average recovery of the high set of linear and branched LCS at 125% and 133% suggests a slight 

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

Therefore, the method uncertainty for this study has been set of ± 33%. A method deviation is included 

with the raw data. 

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

, oo D . n Calculated Concentration .,... , 

LCS Percent Recovery = 100% 

Spike Concentration 

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

average LCS recovery 

Page 15 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS In Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Table 7. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Analyzed 2/11/11 

Lab ID 

LCS-110210-1 

LCS-110210-2 

LCS-110210-3 

Average ±%RSD 

LCS-110210-4 

LCS-110210-5 

LCS-110210-6 

Average ±%RSD 

LCS-110210-7 

LCS-110210-8 

LCS-110210-9 

Average ±%RSD 

PFBS 

Spiked 

Concentration 

(ng/mL) 

0.498 

0.498 

0.498 

Calculated 

Concentration 

(ng/mL) 

0.563 

0.542 

0.581 

'/oRecovery 

113 

109 

117 

113% ±3.5% 

4.98 

4.98 

4.98 

5.37 

5.52 

5.58 

108 

111 

112 

110% ±1.9% 

29.9 

29.9 

29.9 

29.8 

31.1 

32.0 

99.5 

104 

107 

104% ±3.6% 

PFHS 

Spiked 

Concentration 

(ng/mL) 

0.498 

0.498 

0.498 

Calculated 

Concentration 

(ng/mL) 

0.603 

0.594 

0.599 

VoRecovery 

121 

119 

120 

120% ±0.83% 

4.98 

4.98 

4.98 

5.61 

5.36 

5.96 

113 

108 

120 

114% ±5.3% 

29.9 

29.9 

29.9 

30.7 

30.8 

32.7 

103 

103 

109 

105% ±3.3% 

ETS-8-044.0 

Analyzed 2/11/11 

Lab ID 

LCS-110210-1 

LCS-110210-2 

LCS-110210-3 

Average ±%RSD 

LCS-110210-4 

LCS-110210-5 

LCS-110210-6 

Average ±%RSD 

LCS-110210-7 

LCS-110210-8 

LCS-110210-9 

Average ±%RSD 

PFOS (linear) 

Spiked 

Concentration 

(ng/mL) 

0.498 

0.498 

0.498 

Calculated 

Concentration 

(ng/mL) 

0.650 

0.587 

0.540 

VoRecovery 

130 

118 

108 

119% ±9.3% 

4.98 

4.98 

4.98 

5.43 

4.93 

5.86 

109 

99.1 

118 

109% ±8.7% 

29.9 

29.9 

29.9 

30.8 

30.7 

32.4 

103 

103 

108 

105% ±2.8% 

Lab ID 

LCS-110210-10 

LCS-110210-11 

LCS-110210-12 

Average ±%RSD 

LCS-110210-13 

LCS-110210-14 

LCS-110210-15 

Average ±%RSD 

LCS-110210-16 

LCS-110210-17 

LCS-110210-18 

Average ±%RSD 

PFOS (linear + branched) 

Spiked 

Concentration 

(ng/mL) 

0.502 

0.502 

0.502 

Calculated 

Concentration 

(ng/mL) 

0.539 

0.585 

0.541 

VoRecovery 

107 

117 

108 

111% ±5.0% 

5.04 

5.04 

5.04 

6.15 

5.38 

5.44 

122 

107 

108 

112% ±7.5% 

30.2 

30.2 

30.2 

40.7 

40.4 

39.6 

135 

134 

131 

133% ±1.6%'^' 

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

Page 16 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Table 7 continued. Laboratory Control Spike Recovery. 

ETS-8-044.0 

^alyzed 2/28/11 

Lab ID 

LCS-110228-1 

LCS-110228-2 

LCS-110228-3 

Average ±%RSD 

LCS-110228-4 

LCS-110228-5 

LCS-110228-6 

Average ±%RSD 

LCS-110228-7 

LCS-110228-8 

LCS-110228-9 

Average ±%RSD 

Spiked 

Concentration 

(ng/mL) 

0.498 

0.498 

0.498 

PFOS (linear) 

Calculated 

Concentration 

(ng/mL) 

0.483 

0.487 

0.427 

VoRecovery 

97.0 

97.7 

85.6 

93.4% ±7.3% 

4.98 

4.98 

4.98 

5.27 

5.17 

5.34 

106 

104 

107 

106% ±1.4% 

29.9 

29.9 

29.9 

31.3 

31.7 

31.9 

105 

106 

107 

106% ±0.94% 

Lab ID 

LCS-110228-10 

LCS-110228-11 

LCS-110228-12 

Average ±%RSD 

LCS-110228-13 

LCS-110228-14 

LCS-110228-15 

Average ±%RSD 

LCS-110228-16 

LCS-110228-17 

LCS-110228-18 

Average ± %RSD 

PFOS (linear + branciied) 

Spiked 

Concentration 

(ng/mL) 

0.502 

0.502 

0.502 

Calculated 

Concentration 

(ng/mL) 

0.467 

0.475 

0.493 

VoRecovery 

93.1 

94.6 

98.2 

95.3% ±2.8% 

5.04 

5.04 

5.04 

4.88 

5.10 

4.72 

96.7 

101 

93.6 

97.1% ±3.8% 

30.2 

30.2 

30.2 

40.4 

36.1 

36.8 

134 

119 

122 

125% ±6.3%''' 

ETS-8-044.0 

Analyzed 3/10/11 

Lab ID 

LCS-110307-4 

LCS-110307-5 

LCS-110307-6 

Average ±%RSD 

LCS-110307-7 

LCS-110307-8 

LCS-110307-9 

Average ±%RSD 

Spiked 

Concentration 

(ng/mL) 

1.99 

1.99 

1.99 

PFOS (linear) 

Calculated 

Concentration 

(ng/mL) 

2.22 

2.05 

2.26 

VoRecovery 

111 

103 

114 

109% ±5.2% 

9.94 

9.94 

9.94 

11.1 

10.7 

10.2 

112 

107 

103 

107% ±4.2% 

Lab ID 

LCS-110307-13 

LCS-110307-14 

LCS-110307-15 

Average ±%RSD 

LCS-110307-16 

LCS-110307-17 

LCS-110307-18 

Average ±%RSD 

PFOS (linear + branched) 

Spiked 

Concentration 

(ng/mL) 

2.01 

2.01 

2.01 

Calculated 

Concentration 

(ng/mL) 

2.24 

2.23 

2.40 

VoRecovery 

111 

111 

120 

114% ±4.6% 

10.0 

10.0 

10.0 

11.2 

11.6 

11.0 

112 

116 

110 

113% ±2.7% 

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

8.7 Analytical IVIethod Uncertainty 

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

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

standard deviation is calculated for the set of accuracy results (in %) obtained for the most recent fifty 

QC samples. The expanded uncertainty is calculated by multiplying the standard deviation by a factor 

of 2, which con-esponds to a confidence level of 95%. The method uncertainty for PFOS by ETS-12-

012-2 was found to be ± 17%, however, since the high set of linear and branched LCS had an average 

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

uncertainty values are listed in Table 8. 

Page 17 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Table 8. Analytical Uncertainty. 

Analyte 

PFBS 

PFHS 

PFOS 

Standard Deviation 

10.1 

11.0 

NA'^' 

Method 

Uncertainty 

±20% 

±22% 

±33% 

(1) See section 8.6 for a discussion regarding the method uncertainty for PFOS. 

8.8 Field Matrix Spikes (FMS) 

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

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

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

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

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

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

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

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

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

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

^, ,_„ (SampleConcentration 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 Blank and rinseate blank. Results and average values are rounded to 

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

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

of ± 30%, demonstrate that the method(s) were appropriate for the given matrix and their respective 

quantitative ranges 

DAL GW 21 OR 280111; The recovery of the HS sample, the only appropriate FMS concentration level 

for PFOS, was 68.1%. The recovery was within the method uncertainty for PFOS. 

DAL GW SS24 270111 ; The HS at 97.8 ng/mL was not sufficient to accurately assess recovery for 

PFOS. 

Page 18 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Tables. DAL GWSS22 270111 

3M LIMS ID 

GLP 10-01-02-16-006 

GLP10-01-02-16-007 

GLP 10-01-02-16-008 

GLP10-01-02-16-009 

GLP10-01-02-16-010 

Description 

DAL GWSS22 0 270111 

DALGWSS22DB270111 

DALGWSS22LS270111 

DALGWSS22IVIS270111 

DALGWSS22HS270111 

Average Concentration (ng/mL) ± %RPD 

PFBS 

Concentration 

(ng/mL) 

3.30 

3.48 

4.45 

12.8 

99.5 

VoRecovery 

NA 

NA 

106 

94.1 

98.9 

3.39 ng/mL ±5.3% 

PFHS 

Concentration 

(ng/mL) 

1.78 

1.90 

3.13 

12.0 

104 

VoRecovery 

NA 

NA 

129 

102 

106 

1.84 ng/mL ±6.5% 

PFOS 

Concentration 

(ng/mL) 

8.57 

8.67 

NA<^' 

16.5 

NA'^' 

%Recovery 

NA 

NA 

NA'^> 

78.8 

NA'^> 

8.62 ng/mL ±1.2% 

NA = Not Applicatjie 

NO = Not Calculated; Endogenous concentration greater than 2x spike level. 

PFBS and PFHS were analyzed by external standard calibration on 2/11/11. PFOS was analyzed by intemal standard calibration on 3/10/11. 

(1) The sample was not analyzed. 

Table 10. DALGWSS24 270111 

3MLIIVISID 

GLP10-01-02-16-012 

GLP10-01-02-16-013 

GLP10-01-02-16-014 

GLP10-01-02-16-015 

GLP10-01-02-16-016 

Average Concer 

Description 

DAL GWSS24 0 270111 

DALGWSS24DB270111 

DALGWSS24LS270111 

DALGWSS24MS270111 

DALGWSS24HS270111 

rtration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

18.9 

19.5 

20.0 

28.6 

116 

%Recovery 

NA 

NA 

NC 

94.0 

99.6 

19.2 ng/mL ±3.1% 

PFHS 

Concentration 

(ng/mL) 

141 

145 

146 

154 

234 

VoRecovery 

NA 

NA 

NC 

NC 

94.7 

143 ng/mL ±2.8% 

PFOS 

Concentration 

(ng/mL) 

514 

485 

NA<^> 

NA<^' 

548 

VoRecovery 

NA 

NA 

NA<^' 

NA<^' 

NC 

500 ng/mL ±5.8%' ^ 

NA= Not Applicable 

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

PFBS and PFHS were analyzed 2/11/11. PFOS was analyzed 2/28/11. 

(1) The sample was not analyzed. 

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

Page 19 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Table 11. DAL GW 21 OR 280111 

3M LIMS ID 

GLP10-01-02-16-017 

GLP10-01-02-16-018 

GLP10-01-02-16-019 

GLP10-01-02-16-020 

GLP10-01-02-16-021 

Average Concer 

Description 

DAL GW210R 0 280111 

DAL GW210RDB 280111 

DAL GW210RLS 280111 

DAL GW210R MS 280111 

DAL GW210RHS 280111 

rtration (ng/mL) ± VoRPD 

PFBS 

Concerrtration 

(ng/mL) 

43.8 

42.6 

52.5 

136 

947 

VoRecovery 

NA 

NA 

NC 

95.5 

90.4 

43.2 ng/mL ±2.8% 

PFHS 

Concentration 

(ng/mL) 

312 

306 

324 

402 

1280 

VoRecovery 

NA 

NA 

NC 

NC 

97.1 

309 ng/mL ±1.9% 

PFOS 

Concerrtration 

(ng/mL) 

556 

522 

NA'^' 

NA'^> 

1220 

VoRecovery 

NA 

NA 

NA'^> 

NA'^> 

68.1 <^' 

539 ng/mL ±6.3% 

NA= Not Applicable 

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

PFBS and PFHS were analyzed 2/11/11. PFOS was analyzed 2/28/11. 

(1) The sample was not analyzed. 

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

Table 12. Trip Blank 

3M LIMS ID 

GLP10-01-02-16-001 

GLP10-01-02-16-002 

GLP10-01-02-16-003 

GLP10-01-02-16-004 

GLP10-01-02-16-005 

Description 

DAL GWTRIP 0 270111 

DAL GWTRIP LS 270111 

DAL GWTRIP MS 270111 

DAL GWTRIP MH 270111 

DAL GW TRIP HS 270111 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

1.04 

9.88 

101 

982 

VoRecovery 

NA 

104 

98.8 

104 

98.2 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

1.18 

10.3 

108 

1040 

%Recovery 

NA 

118 

103 

112 

104 

PFOS 

Concentration 

(ng/mL) 

<0.0300 

1.03 

9.37 

92.8 

950 

VoRecovery 

NA 

103 

93.7 

94.9 

95.0 

NA = Not Applicable 

Page 20 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Table 13. Rinseate Blank 

3M LIMS ID 

GLP10-01-02-16-011 

Description 

DALGWSS24RB270111 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

VoRecovery 

NA 

PFHS 

Concerrtration 

(ng/mL) 

<0.0250 

VoRecovery 

NA 

PFOS 

Concentration 

(ng/mL) 

<0.0300 

VoRecovery 

NA 

NA = Not /Applicable 

Page 21 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

10. Cohclusipn.' ;'; . -^y ''•-' ••' ^"^^y';: ty'J; (Vf:'''': 

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. 

' ItjDatwSampimRetention^,, - ^T^:f:i~'e-:'"^-'' ^'^'j-.-'-** • -*- -;' 

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

to 3M Environmental Laboratory standard operating procedures. 

Attachment A: Protocol Amendment 16 (General Project Outline) 

Attachment B: Representative Chromatograms and Calibration Curves 

Attachment C: Analytical Method 

Attachment D: Method Deviation 

Page 22 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

,13 Signatures 

'Z^)i 

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

P /f/^/ :k}7( 

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

U 

Gary Hohenstein, Sponsor Representative 

Oi^i^'i. 

Date 

m 

Jaisimha Kesari, Study Director Date 

Page 23 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

ATTACHMENT A: PROTOCOL AMENDMENT 

Page 24 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Analytical Protocol: GLP10-01-02 

Amendment 16 

Study Title 

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

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

Decatur Phase 3 Site-Related Monitoring Program 

PROTOCOL AMENDMENT NO. 16 

Amendment Date: 

January 25, 2011 

Performing Laboratory 

3M Environmental, Health, and Safety Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55144-1000 

Laboratory Project Identification 

GLP10-01-02 

Sampling Event 

Avenue A Investigation - Groundwater Sampling 

Exact Copy of Original 

initial Date 

t Page 1 of 6 

Page 25 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Analytical Protocol: GLP10-01-02 

Amendment 16 

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 the week of January 

24, 2011. The groundwater samples for this sampling event will be entered into the 3M Environmental 

Laboratory LIMS as project GLP10-01-02-16 and reported as interim report GLP10-01-02-06, (reflecting 

study GLP10-01-02 and amendment -16). 

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 6 

Page 26 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Analytical Protocol: GLP10-01-02 

Amendment 16 

Amendment Approval 

y// 

' {iMi " -^i fffm^^^ — H 

Gary Hohenstein, Sponsor Representative 

77 

'IL 

Date 

Cleston C. Lange, Principal Analytical Investigator fDat e ^ ^ 

;i.r.j7p^ s>o'// 

William Reagen/EHS Opns Environmental Lab Management 

fklMMj.: 

Date 

SL 

Jaisimha Kbsari P.E., DEE, Study Director Date 

Page 3 of 6 

Page 27 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Analytical Protocol: GLP10-01-02 

Amendment 16 

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 

Jai Kesari, Weston Solutions 

Charies Young, Weston Solutions 

Tim Frinak, Weston Solutions 

Date: January 25, 2011 

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 16 - Additional Avenue A 

Sampling; January 2011 

1 General Project Information 

Contacts 

Lab Request Number 

Six Digit Department Number 

Project Schedule/Test Dates 

3M Sponsor Representative 

Gary Hotienstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul. MN 55144-1000 

Phone:(651)737-3570 

aatiohenstein(5)mmm.com 

3IVI Environmental Laboratory Management 

William K. Reagen 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9739 

wkreaaen®mmnn.com 

Principal Analytical Investigator 

Cleston Lange 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9860 

cclanae(a)mmm.com 

Sampling Coordinator 

Timottiy Frinak 

Weston Solutions 

Timothv.frlnak(5)westonsolutions.com 

Ptione; (334)-332-9123 

GLP10-01-02-16 

Dept #530711, Project #0022674449 1 

Sampling sctieduled for the week of January 24, 2011 

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

Page 4 of 6 

Page 28 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Analytical Protocol: GLP10-01-02 

Amendment 16 

2 Background Information and Project Objective{s) 

The 3M EHS Operations Laboratory (3IV1 Environmental Lab) will receive and analyze groundwater 

samples collected from three 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 

January 24, 2011. 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-

01-02-16, 

3 Project Schedule . 

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

24,2011. Sample bottles will be shipped in coolers overnight to 3M Decatur for amval on Friday, January 21, 

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

Martin Smith \ Weston Trailer 

3M Decatur Plant 

1400 State Docks Road 

Decatur, Alabama 35601 

4 Test Parameters 

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

A total of three sampling locations have been specified. Sampling location descriptions were not available at the 

time of sample bottle preparation. For each sampling location, a total of five sample bottles will be collected 

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

spike). The "fill to here" line on each 250 mL Nalgene bottle will be 200 mL. One set of trip blanks consisting of 

reagent-grade water, a low-level trip blank spike, mid-level field spike, mid-high level field spike, and a high-level 

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

other bottles. One additional bottle will be prepared to be used for the preparation of the equipment rinseate 

blank. A total of twenty-one sample bottles will be prepared. 

5 Test Methods 

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

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

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

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

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

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

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

Chromatography/Mass Spectrometry". 

Page 5 of 6 

Page 29 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Analytical Protocol: GLP10-01-02 

Amendment 16 

6 Reporting Requirements 

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

field matrix spikes. 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 detemnine 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 6 

Page 30 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

ATTACHMENT B: SAMPLE CHROMATOGRAMS AND CALIBRATION CURVE 

Page 31 of 61 
**• Ginger AG01330509 

GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samp)<^uits Name: 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

gll0211a.rdb 

g11021 la.rdb (PFHS): "Quadratic" Regression ("1 / x" weighting): y = -8.76e+003 x'^2 + 1.24e+006 x + 4.17e+003 (r = 0.9995) 

4.2e7 

4.1e7 

4.0e7 

3.9e7 

3.8e7 

3.7e7 

3.6e7 

3.5e7 

3.4e7 

3.3e7 

3.2e7 

3.1e7 

3.0e7 

2.9e7-

2.8e7-

2.7e7-

2.6e7-

2.5e7 

2.4e7 

2.3e7 

2.2e7-

2.1e7-

2.0e7 

1.9e7 

1.8e7-

1.7e7-

1.6e7-

1.5e7-

1.4e7-

1.3e7 

1.2e7-| 

1.1e7 

1.0e7H 

9.0e6 

S.OeS 

7.0e6 

6.0e6 

5.0e6- / 

4.0e6 

3.0e6 

2.0e6 

I.OeS 

0.0 

-1.0e6 

/ 

/ 

10 12 14 16 18 20 22 24 26 28 30 32 

Concentration, ng/mL 

34 36 38 40 

Page 

42 44 46 48 50 

:^?nffi1 

Printing Time: 10:21:13 AM 

Printing Date: Thursday, March 17, 2011 

Page 1 of 1 
Ginge r AG01330509 

GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samp*^uits Name: gii02iia.rdb 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

g11021 la.rdb (PFBS): "Quadratic" Regression ("1 / x" weighting): y = -3.35e+003 x'^2 + 6.88e+005 x + 3.41e+003 (r = 0.9997) 

2.7e7-

2.6e7-

2.5e7-

2.4e7-

2.3e7-

2.2e7-

2.1e7-

2.0e7-

1.9e7-

1.8e7-

1.7e7-

1.6e7-

1.5e7-

1.4e7-

1.3e7-

1.2e7-

1.1e7-

1.0e7-

9.0e6-

8.0e6-

7.0e6-

e.oes5.0e6-

4.0e6-

3.0e6-

2.0e6-

1.0e6-

0.0-

/' 

/ 

' 

/ 

/ 

I ' 

/ 

/' 

I • I 

/ / 

' 1 

/ 

/ 

/ 

/ 

/ 

[ ' 1 

/' 

/ 

/ 

/ 

'' 

1 ' 1 

/ 

/ / / / / / / 

/ • 

/ / / 

/ 

/ / 

/ 

. 1 > 1 > 1 i 1 ' 1 

/ 

/ 

/ 

/ 

/ 

/ 

' 1 • 1 • 1 ' 1 '-

/ / 

/ 

/ 

1 ' I ' 1 

/ 

/ 

/ 

1 1 < 1 1 1 1 1 

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

Concentration, ng/mL P^Q^r^r^nfRi 

Printing Time: 10:20:40 AM 

Printing Date: Thursday, March 17, 2011 

Page 1 of 1 
Ginge r AG01330509 

I

Sample Name: "g110211a019" Sample ID: -10007'27-S' File: 'g110211a.wifr 

Peak Name: TFBS" Mass(es): "299.0/99.0 amu,299.0/80.0 amu" 

Connment '1.0 ng/mL FC std in Mili Q vratei' Annotatkin:" 

Sample Index; IS 

Sample Type: Standard 

Cancentration: 1.00 ng/mL 

Calculated Ccnc: 1.05 nij/rnL 

Acq. Date: 2/12/2011 

Acq. Time: 2:20:55 AM 

GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Results Name: gll0211a.rdb 

RT Window: 30.0 si 

Expected RT: 10-6 m: 

Vs^ Relative RT: No 

Int. Type: Hanual 

Kenention Time: 10.6 m: 

Ares: 733521 ciounl 

Height: 165000. ^-ps 

1.6e5 

1.6e5' 

1.S«5 

1.5«5 

1.4e5-

1.4«5-

1.3*5-

1.3e5-

1.2e5' 

1.2eS 

l.leS 

l.1e5 

1.0e5 

9.5e4 

9.0e4 

§• 6.Se4-

I e.0e4 

7.5e4 

7.0*4 

6.5e4 

6.0e4 

5.5e4 

5.0e4 

4.5e4 

4.0e4 

3.5e4 

3.0e4 

2.5e4-

2.0e4 

10 n 12 13 14 15 16 

Sample Name: "g110211aO11* Sample ID: "Solvent Blank" File; "g11021 la.vuifr 

•

Peak Name: "PFBS" Ma*«(es): -299.Dffl9.0 amu,299.0/80.0 amu" 

Comment •MilliQ\ftfaterTN11-00S2" Annotation:"" 

Sample Index : 11 

Sample Type: 

Data printed by CJG 

Printing Time: 10:16:01 AM 

Page 1 of 6 
^* Ginger AG01330509 

I

Sample Name: "gl 10211«032- Sample ID: "LCS-11021[M" File: "g11021 la.wiT 

Peak Name; 'PFBS* Maaafes): "299.0^.0 amu,299.0/80.0 Amu" 

Comment "5ppb LCS" Annotation: " 

Sample Index: 32 

Sample Type: QC 

Csncant cation: A.9? ng/mL 

Calculated Cone; 5,31 ng/mL 

Acq. Date: 2/12/2011 

GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur. AL - Jan 2011 

Results Name: gll0211a.rdb 

Acq. Tim 

I Rela 

6:14:52 nM 

! RT: No 

Inc. Type: Manual 

Retention Time: 10.6 

Area: 3603869 c. 

Height: 817000. 

Start Time: 10.5 

End Time: 11.2 

S.DeS 

7.8e5 

7.6e5 

7.4e5 

7.2e5 

7.0e5 

6.8e5 

6.6e5-

6.4e5 

6.2e5-

6.0e5 

5.8e5-

5.6e5 

5.4eS 

5.2e5 

S.OeS 

4.8a5 

4.6eS 

4.4e5 

4.2e5 

4.0e5 

3.8e5-

3.6eS 

3.4e5 

3.2e5 

3.0e5 

2.6e5 

2.6e5-

2.4e5-

2.2e5-

Z0e5' 

1.Se5 

1.6e5 

1.4e5 

1.2e5 

1.0e5 

B.0e4 

6.0e4 

4.0e4 

Tim^, mif) 

SamptoName:"g1102nfl068" SamptelD:"GLP1(M)1-02-1B-006" File: •g110211a.Mr 

•

Peak Name: "PFBS" Ma««(e«): "299.0/99.0 amu,299.0ffi0.0 amu" 

Comment" DALGWSS22 0 270111 (dil1:10)" Annotation: " 

Sample Index: 69 

Sample Type: Unknown 

Concentration: M/A 

Calculated Cone: 3.30 ng/mL 52*4 

Acq. Date: 2/12/2011 

Acq. Time: 5:03:11 PM 5^ ^ 

Modi fi«d: 

Base. Sub, window: 

p.-ak-Split. Factor 

R^po^t Largast paal 

Hin. Peak Height: 

Mln. Peak Width: 

Sooothing Width: 

RT Window: 

EKparted RT: 

Use Relative RT: 

alliC'jai 

90 

1,00 

5,0e4-

4.9e4-

4.ee4-

4.7e4-

4.6e4-

4.Se4' 

4.4e4' 

4.3e4 

4.2e4 

4.1e4 

4.0e4 

3.9e4 

3.8e4 

3.7e4 

3.6e4 

3.5e4 

3.4e4 

3.3e4 

3.2e4 

3.1 e4 

3.0e4 

Z9s4 

2.8e4 

2.7e4 

2.6e4 

2.5e4 

2.4e4 

2.3e4 

2.2e4 

2.1 e4 

2.0e4 

1.9*4 

1,8*4 

1.7e4-

1.6e4-

1.Se4 

1.4e4 

1.3e4 

1.2e4 

1.1e4 

1.0e4 

9000.0 

8000.0 

7000.0 

6000,0 

S000.D 

4000.0 

3000.0 

2000.0 

1000.0 

0.0 '-<v_-, 

Data printe d by CJG 

Printing Time: 10:16:01 AM 

Page 2 of 6 

TiTM.min Pagp :^R nf fi1 
Ginge r AG01330509 

• Sample Name:-g110211a07r Sample ID: "GLP1(H)1-02-16-012" File:-g110211a.<Mfr 

I Peak Name: "PFBS* Mass<es): -239.0i«9.0 amu,299.W80.0 

• Comment*D/U.GWSS240270111 {dil1;10)" Annotation: 

Samplfl Index: 77 

GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Results Name: gll0211a.rd b 

Sample Tvpe: 

Csncar^tration: 

Calculated Cone: 

Acq. Date: 

Acq. Tirae: 

Hidified; 

Proc. Algorithm: 

Ncise Percentage 

Base. Sub. Windo 

Unknown 

N/A 

IS.6 

2/12/2011 

7:<5:32 PH 

Yes 

InteiliQua 

95 

*: 1.00 

Peak-Split. Factor: 4 

Ksport Largest Peak: N". 

Min. Peak Height 

Hin. Peak Width: 

Smoothing Width: 

RT Window: 

Expflcted RT: 

Us^ Relative RT: 

Int, Type: 

Retention Tin.e: 

0.00 

0.00 

i 

30.0 

10.6 

No 

Base To Ba 

10.5 

Area: 12540<£ cou 

Height: 

Start Time: 

End Time: 

77000. cp 

10.t 

U . 2 

Concentratlo 

Calculated C 

Acq. [?at«: 

Acq. Tim?: 

Modified: 

n: H/A 

one: 4 3,6 

2/U/2011 

10:r-:i5S 

Ves 

Sample Name: •g110211aOee- Sample ID: "GLP10-01-02-lW)17- File: "g110211a.wr 

Peak Name: "PFBS" Ma«c(e«): "2S9.0/99.0 amu,299.0/80.0 a -

Comment'DALGW210R0280111 (dil1:10r Annotation:"' 

Samplp Index : 96 

6.4e5 

6.3e5 

6.2e5-

6.1 eS 

B.OeS 

5.9e5 

5.ee5 

5.7e5 

S.6e5 

5.5e5 

5.4e5 

S.3e5 

5.2e5 

5.1 e5 

S.OeS 

4.9e5 

4.8e5 

4.7e5 

4.6e5 

4.5eS 

4.4e5-

Data printed by CJG 

Printing Time: 10:16:01 AM 

Page 

Time-'"'" Pagg -^R nf fij_ 
Ginger AG01330509 

• SampleNarTM:'g110211a019" Satr^te ID: 

I Peak Name:-PFHS* Maea(e»): "399.0/99.0 

I Comment '1.0 ng/mL FC std tn UiB Q water" 

Sample Index: 19 

Sample Type: Standard 

Concentration: 1,00 ntj/mL 

Calculated Cone: 1.OS ny/mL 

Acq. Date: 2/12/2011 

Acq. Time: 2:20:55 AM 

fiei 

Report Large: 

m: Intel litiuan - MQIl 

Min. Peak Haiuh': 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

U=- Relative RT: 

lr,t. Type: 

Retention Tini«: 

: 0 

J 

30.0 

11.7 

No 

Baaa To 

11,7 

Area: 129527C 

Height: •&6000. 

00 

00 

Ba 

:ou 

cp 

'10007-27-8" FUe:"g110211a.wir 

amu,399.0/80.0 amiT 

Arviotation: ~ 

3.1 eS 

3.0e5 

3.0eS 

Z9e5 

2.9e5i 

2.8eS 

2.8eS 

Z7e5 

2.7e5 

ZSeS 

Z6e5 

ZSe5 

ZSeS: 

Z4e5 

Z4e5 

2.3e5 

2.3eS 

2.2e5 

2,2e5 

ZleS 

ZleSr 

ZOeSZOeS 

1.9e5 

GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS. and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur. AL - Jan 2011 

Results Name: gll0211a.rdb 

1.7e5-

1.7e5-

1.6e5-

1.6e5-

1.5e5 

1.5e5 

1.4e5 

1.4e5 

1.3e5 

1.3e5 

1.2e5 

^2t>S 

1,1e5 

l.leS1.0e5 

9.Se4 

9.0e4 

8.5e4-

S.0e4 

7.5e4 

7.0e4 

6.5e4 

6.0e4 

5.5e4 

5.0e4 

4.5e4 

4.0e4 

3.5e4 

3.0e4 

2.5e4 

2,0e4 

1.5e4 

1.0e4 

5000.0 

0.0 

Sample Name: "g110211a011" Sample ID: "Solvent Kank" File: "gl 1021 la.wfT 

Peak Name: "PFHS* Masa(es): "399.0/99.0 amu.399.(V80.0 amu' 

Comment 'Mill) Q Water TN11-0052" Annotation: 

Sample Index: 11 

Sample Type: Unt:j 

Calculated Cone: 

Acq. L'ate: 

Acq. Time: 

Modified: 

Proc. Algcrithm: 

Moisa Percentage 

Base. Sub. Windo 

< c, 

2/11/2011 

11:57:15 P 

No 

InteiliQua 

50 

• i : 1,0 0 

P-ak-Split. Factor: 2 

R-.pc.rt Largest Peak: No 

Min. Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Type: 

Retention Time: 

Area: 

Height: 

Start Time: 

0.00 

0.00 

3 

30.0 

11.7 

No 

valley 

11.7 

1567 cou 

26J. cp 

11,6 

Data printed by CJG 

Printing Time: 10:16:01 AM 

Page 4 of 6 
'^** Ginge r AG01330509 

I

Sampte Name: "g110211a03r Sample 10: "LCS-110210-4" 

Peak Name: "PFHS* Ma»»(e«): -399.Q«9.0 amu.399.0/80.0 

Comment 'Sppb LCS" Annotation: ~ 

GLP10-01-02; Interim Report 16 

Analysis of PFBS. PFHS. and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur. AL - Jan 2011 

Results Name: gll0211a.rdb 

Indej 32 

Sampl e Type : QC 

Concentration : 4.9B ng/mL 

Calculate d Cone : 5.6 1 ny/mL 

Acq. Date : 2/12/201 1 

Acq . Time : 6: H : 52 AM 

M:jdified: Yes 

Proc . Algorithm : IntelliQua n - MQ! 

Base , Sub . Window: 

Peak-Split , Facto r 

Repor t Largest Pea 

Hin , Peak Height : 

Min , Peak Width ; 

Smoothin g Width : 

RT Window: 

Expecte d RT: 

Us^ Relativ e RT: 

Int . Type : 

Retentio n Time : 

1.00 ra 

1 

0,0 0 c 

0,0 0 s 

i 

30. 0 38C 

11. 7 min 

No 

'alle y 

11. 7 min 

Area : 66^165 1 counts 

H«ight : 1610000 . cpu 

Star t Tine : 

End Time : 

11. 5 rain 

12. 1 rain 

ps 

point s 

1.5e6 

1,4e6 

1.4e6 

1.3e6 

Samptof4ame;"gl10211a068- Sample ID: "GLP1(W1-02-1&O06" Fite: •gll0211a.Mr 

Peak Name: "PFHS" Masc(es): "399.0/99.0 amu,399.0/80,0 amu' 

Comment'DALGWSS22 0 270111 ((SI1:10)" Annotation:-

sample Index : 6^ 

Sample Type: Unknown 

4.ae4 

4.7e4-

4.6e4 

4.Se4-

4.4e4 

4.3e4' 

4Ze4 

4.1 e4 

4.0e4 

3.9e4 

3.8e4 

3.7e4 

3.6a4 

3.5e4 

3.4e4 

3.3e4 

3.2e4 

3.1e4 

3.0e4 

Z9e4 

ZSe4' 

Z7e4 

Z6e4 

2.Se4 

2.4e4 

Z3e4-

2.2e4 

Zle4 -

Z0e4 

1.ge4 

1.8e4 

1.7e4 

1.6e4 

1.5e4-

1.4 

1.3*4' 

1.2*4-

1.1*4-

1.0e4-

9000.0-

B000.0-

7000.0-

6000.0-

5000.0 

4000.0 

3000.0-

2000.0 

1000.0 

0.0 

J\^^-^^' ^ 

.^,)A» 

10 11 12 13 14 15 18 17 

Data printe d by CJG 

Printing Time: 10:16:02 AM 

Page 5 of 6 
Ginge r AG01330509 

1

Sample Name: "91102118077" Sample ID: 'GLPI0-01-02-16-01 r File: "811021 la.wiT 

Peak Mame: "PFHS" Mass<es): "399.0/99.0 amu,399.0/80.0 amu" 

Comment "DAL GW SS24 0 270111 (dil 1:10r Annotation: "" 

Sample Index : 77 

GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Results Name: gll0211a.rd b 

Unki 

N/A 

Acq. Date: 

Acq. Time: 

Modified: 

KT Window: 

E.xpected RT: 

Use Relative 

Int. Type: 

Retention Ti 

Area: 

Height: 

KT 

me: 

2/12/2011 

7:^5:32 PM 

Yes 

30,0 

11.7 n 

No 

Manual 

11.7 ti 

15-'6S4:8 :o 

3050000. c 

3.0*6 

3.0*6 

Z9*6 

Z9*6 

Z8e6 

2.B«6 

2.7*6 

2.7*6 

2.6*6 

2.6e6 

2.5e8 

2.5e6 

2.4e6: 

Z4e6 

2.3*6-

Z3e8 

2.2e6 

Z2e6 

Z1e6 

Z1e6 

2.0e6 

2.0*6 

1.9*6 

1.9*6 

1.8e6 

1.3e6 

1.7*6 

1.7e6 

1.6*6 

1.6e6 

l.Se6 

1.5*6 

1.4*6 

1.4*6 

1.3*6-

1.3e6 

1.2e6-

1.2e6 

1.1e6 

1.1e6-

1.0e6-

9.5*5 

9.0*5 

8.5*5 

8.0*5 

7.5e5 

7.0e5 

6.5eS 

e.OeS 

5.5e5 

S.OeS 

4.5eS 

4.0e5 

3.5*5-

3.0*5 

2.5*5 

ZOeS 

I.SeS1.0*5 

5.0*4 

0.0 mI Sample Name: "gl 10211 aOSff- Sample ID: 'GLP 1(MH-02-1B-01 r File: "g110211a.wifr 

i Peak Name: "PFHS" MaM(*s): "399.0/99.0 amu,3g9.0/80.0 amu' 

I Comment" DALGW210R0280111 (di!1:10)" Annotation: ~ 

imple Type: 

mcantrati o 

Unkf 

N/A 

Calculated Cone 

Acq. fate : 

Acq. Time: 

l1odiii«d: 

RT Window: 

E:<pacted RT: 

U36 Relative 

Int. Type: 

Retention Ti 

Area: 

Height: 

Start Tin,e: 

End Time: 

RT 

312. 

2/12/20! 

10:27:£B 

Yes 

30,0 

11.7 

Ho 

Manual 

11.7 

30135E93 

5370000, 

11.3 

12.4 

1 

PM 

s 

m 

CO-J 

m 

m 

5,3*6-

5.2*6 

5.1*6 

5.0*6 

4.9*6' 

4.8*6-

4.7*6 

4.6*6 

4.5*6 

4.4*6 

4.3*6 

4.2*6 

4.1*6 

4.0*6 

3.9*6 

3.6*6 

3.7*6 

3.6e6 

3.5*6 

3.4*6 

3.3*6 

3.2*6 

3.1*6 

3.0*6 

Z9*6 

Z8e6 

Z7*6 

Z6*6 

Z5e6 

Z4*6 

Z3*6' 

2.2*6 

Z1*6-

Z0*6-

1.9*6 

1.6*6-

1.7*6 

1.6e6 

1.5e6 

1.4e6-

1.3e6' 

1,2e6 

1.1*6-

1.0*6-

9.0eS 

6.0*5 

7.0*5 

6.0*5 

S.OeS 

4.0eS 

3,0*5 

Z0*5 

1.0*5 

0.0 

Data printed by CJG 

Printing Time: 10:16:02 AM 

Page 6 of 6 

-IJiaSJDiQ Parj g -^Q n f R 1 
»** Ginger AG01330509 

GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Sampt^uits Name: 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

gll0228a.r<ab 

• g110228a.rdb (PFOS): "Quadratic" Regression ("1 / x" weighting): y = -6.87e-H003 x'^2 + 1.12e-H006 x -K -4.99e-t-003 (r = 0.9998) 

4.0e7-

3.9e7-

3.8e7-

3.7e7-

3.6e7-

3.5e7-

3.4e7-

3.3e7-

3.2e7-

3.1e7-

3.0e7-

2.9e7-

2.8e7-

2.7e7-

2.6e7-

2.5e7-

2.4e7-

2.3e7-

2.2e7-

2.1e7-

2.0e7-

1.9e7-

1.8e7-

1.7e7-

1.6e7-

1.5e7-

1.4e7-

1.3e7-

1.2e7-

1.1e7-

1.0e7-

9.0e6-

8.0e6-

7.0e6-

6.0e6-

5.0e6-

4.0e6-

3.0e6-

2.0e6-

1.0e6-

0.0-

• 

/ 

fi 

i 

/ 

/ 

/ / 

/ 

,-• 

/ 

/ 

/ 

/ / 

/' 

/ / / 

• / 

/ 

/ 

/ / / 

/ 

/ 

/ 

/ 

/ 

/ 

/ 

/ 

/ / / 

/ / / / 

/ / 

/ 

/ / 

/ 

/ 

/ 

/ / / / 

/ 

/ 

/ 

/ 

/ 

/ 

/ 

/ 

,.-• 

^-'' 

8 10 12 14 16 18 20 22 24 26 28 30 

Concentration, ng/mL 

32 34 36 38 40 

Pagp 

42 44 46 

4nnffi1 

48 50 

Printing Time: 10:24:13 AM 

Printing Date: Thursday, March 17, 2011 

Page 1 of 1 
** Ginger AG01330509 

•

Sample Name; •a110228a019' Sample ID: "10007-27-8" File; "g110228a.wifr 

Peak Name: "PFOS" Maac{*s): '49S.O/S9.0 amu.499.0/BO.O amu.499.0/130.0 amu" 

Comment '1,0 ng/mL FC std in Mifli Q water" /Annotation: " 

Sample Index: 19 

GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Results Name: gll0228a.rdb 

impla Type! 

1.00 ng/mL 

Calculated Cone: 

Acq. Date: 

Acq. Time: 

Hodilied: 

Proc. Algorithm: 

Nc-ise Petcencage; 

Base. Sub. Window 

Peak-Split. Facto 

Report Largest Pe 

Min. Peak Hei^iht: 

Min. Peak Width: 

Smoorliing WiJth: 

KT Window: 

Expscted RT: 

0.951 

2/28/2011 

9:40:20 P 

No 

ntelllQu 

50 

1.00 

r: 2 

ak: N::. 

0.0 

0.0 

0 

30.0 

12.5 

3.2*5 

3.1*5-

3.1*5-

3.0*5-

3.0*5 

Z9*5-

2.9*5 

2.6*5 

2.8*5-

Z7*5 

Z765 

2.6*5 

2.6*5 

2.5*5 

2.5*5 

2.4*5 

2,4*5 

2.3*5 

2,3*5-

2.2*5 

2.2*5 

ZleSZ1*5 

2.0*5 

2.0*5 

1.9*5 

Sample Nam*: "gl 10228a011' Sample ID: 'Solvent B 

Peak Name: "PFOS" Ma«*{ee); *4£* ' "" 

Comment "MilU Q V\bterTN11-007r Annotation: ~ 

Data printed by CJG 

Printing Time: 10:23:17 7U4 

Page 1 of 3 

limsjm] pRgp41 nf f>1 
*** Ginge r AG01330509 

•

Sample Name; -g11022Sa03r Sample ID: "LCS-11022&4" 

Peak Name: "PFOS" Ma»s(es): "499.0/99.0 an)u.499.0/BO.0 

Comment *5ppb LCS* Annotation: " 

Sampl e Index : 32 

Sampl e Type : QC 

Concentration : 4.9B ng/mL 

Calculate d Cone : 5.2 7 ny/mL 

Acq. Date : 3/1/201 1 

Acq. Tine : !2:? 4 •.2i AH 

GLP10-01-02; Interim Report 16 

Analysis of PFBS. PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Results Name: gll0228a.rdb 

llDdilied : No 

Proc . Algorithm : IntalliQua n - MQl! 

Ntis B PeLcentaqo : 50 

Base . Sub . Window: 1.00 min 

Peak-Split . Factor ; 2 

Report Larges t P«ak: NcHin . Peak Height : 0.0 0 cp a 

Hin. Peak Width: 0.00 sec 

Sn-aothin g width : 0 point ; 

RT Windov : 30. 0 se c 

Expecte d RT: 12. 5 min 

\}c^ Relativ e RT: Ho 

1.7*6 

1.6*6 

t . Type : alle y 

1.6*6 

1.5*6-

1.5*6 

1.4*6 

1.4e6 

1.3e6 

1.3e6-

1.2e6 

1.2*6 

1.1e6< 

l.leS1.0e6 

9.5e5 

9.0e5 

i 

" 8.0e5 

7.5e5 

7.0e5 

S.Se5 

6.0*5 

5.5*5 

5.0*5 

4.Se5 

4.0*5 

3.5*5 

3.0*5 

2.5*5 

ZO*S 

1.5*5 

1.0*5 

5.0*4 

0.0 

J

Sampte Name: "g11022Ba041- Sample ID: "LCS-110228-13- File: -g110228a.<Mr 

Peak Name: "PFOS" Uaaa{ea): "499.0/99.0 amu,499.0/80.0 amu,499.0/130.0 amu" 

Comment "Sppb LCS ECF" Annotation:"" 

:ample 

Sampl * Type : 

Calculate d Coi 

Acq. L'ate : 

Acq. Time : 

Modified : 

RT Windo-v: 

E:;pect8 d RT: 

Use Relativ e I 

Hfliyht: 

Star t T: 

End Timi 

CC 

5.0 4 1.02*6-

1.00*6-

9.80*5 

9.60*5 

9.40*5 

9.20*5 

9.00*5 

8.B0e5 

8.60e5 

8.40e5 

8.20e5-

8.00*5 

7.80*5 

7.60*5-

7.40e5 

7.20e5 

7.00*5 

6.80*5 

6.60*5 

6.40*5-

6.20*5 

6.00*5 

5.80*5 

5.60*5 

5.40*5 

5.20*5 

5.00*5 

4.80*5 

4.60*5 

4.40*5 

4.20*5-

4.00*5 

3.80*5 

3.60*5 

3.40*5-

3.20*5 

3.00*5 

2,80*5-

2.60e5 

2.40e5 

2.20e5 

2.00*5 

1,80*5 

1.60*5 

1.40*5 

1.20e5 

1,00e5 

8.00*4 

6,00*4 

4.00*4 

Z00*4 

0.00 

Data printed by CJG 

Printing Time: 10:23:18 AM 

Page 2 of 3 

agp4?nffi1 
*** Ginge r AG01330509 

T Sanple Name: "gl 10228a066- Sample ID:"GLP10-01-02-1fr0ir File: "gl 10228a.wrT 

Peak Name; 'PFOS' Mass(**): "49S.0/99.0 amu.499.0/80.0 amu,499.0/130.0 amu" 

Comm*nt "DAL GWSS24 0 270111 (da 1:100)" Awiotalion: " 

GLPI 0-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur. AL - Jan 2011 

Results Name: gll0228a.rdb 

Sampl e Type : Unknown 

Concentration : N/A 

Calculate d Cone : 51'). ng/mL 

Acq, Date : J/1/201 1 

Acq, Time : 10:47:2 5 AM 

Modified : 

RT window-: 

E.tpecta d RT: 

Vm Relativ e 

Heigh t 

Star t : 

End Tir 

Yes 

IBEOOO. cp s 

12, 1 mil 

IZ.-J mil 

1 i 

1 

7.8*5 

7.6*5 

7.*,5 

7Ze 5 

7.0*5 

6.8*5 

6.6*5 

6.4*5 

6.2*5 

6.0*5 

5,8*5 

5,6*5 

5,4*5 

5.2*5 

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-

Z8e5 -

Z6e 5 

Z4*5 -

2.2e5 -

Z0e 5 

1.8e5 

1.6*5 

1.4*5 

1.2*5 

1.0*5 

8.0*4 

6,0*4 

4.0*4 

2.0*4 

OD 

12 

1Z40 ^ 

12.30^ 

52 

h---n . 

Sample Index 

Sample Type: 

Concantrati o 

Calculate d Cone 

Acq. Dace: 

Acq. Time: 

Hodified : 

RT Window: 

E;:pocted RT: 

Use Relativ e 

Int . Type: 

Retentio n T i 

Haiulit : 

Star t Tin,«: 

RT 

70 

Unkno^-n 

N/A 

556. 

3/1/20 1 

11:59: J 

Yes 

30,0 

12.5 

No 

Manual 

12.5 

601B601 

1110000. 

12.2 

I

SampI* Name: 'gl10228a070- Sample ID: 'GLPI 001-02-16-017" File: "gl 10228a.wtfr 

Peak Mame; "PFOS" Massfee): "499.0/99.0 amu,499.0/80.0 amu,499.0/130.0 amu" 

Comment "DAL GW210R 0 280111 (dU 1:100)" Annotation;-

1,10*6-

1.08*6-

1.06*6 

1.04*6 

1.02*6-

1.00*6 

9.80*5 

9.60*5 

9.40*5 

9.20*5-

9.00*5 

8.80*5-

8.60*5 

8.40*5 

8.20*5 

8.00*5 

7.80*5 

7.60*5 

7.40*5 

7.20*5 

7.00*5 

6.80*5 

6.60*5 

6.40*5 

6.20*5 

6.00*5 

^ 5.60*5 

^ 5.60*5 

I 5.40*5 

5.20*5 

5.00*5 

4.80*5 

4.60*5 

4.40*5 

4.20*5-

4.00*5 

3.80*5 

3.60*5-

3.40*5-

3.20*5-

3.00*5 

Z80e 5 

Z60e 5 

Z40*5 

220* 5 

200* 5 

1.80*5 

I.eOeS 

1.40e5 

1.20*5 

1.00*5 

8.00*4 

6.00e4 

4.00*4 

2.00*4 

0.00 

Data printe d by CJG 

Printing Time: 10:23:18 /\M 

Page 3 of 3 

TiT^e.min Pgjg il'^ nf R1 
Buster J2930203 

GLPI 0-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 Batch Name: bll0310a.dab 

b110310a.rdb (PFOS): "Quadratic" Regression ("1 /x " weighting): y = -0.00048 x'^2 -H.34 x •^ 0.0514 (r = 0.9998) 

(D 

< 

W 

< 

(0 

135-

130-

125-

120-

115-

110-

105-

100-

95-

90-

85-

80-

75-

70^ 

65-

60-

. 

• 

55: 

. 50 J 

] 

45-

40-

35-

30: 

25: 

20-

15-

10-

5-

0-

,.•'' 

,' ,-•' ^ 

,*/"' 

,' ,-''' 

/.•-"" 

/ ' ' 

./' 

,' 

y " 

• • 

,x'' 

/ ' -'' 

_-•• • 

^'' 

,^' ^x 

,.-4 ^,-'' 

y ' 

/'' 

,/^'' 

^z' ' 

''' 

^ ^ 

y''' ' 

•,." 

,,-''' 

X 

/ 

,,---' 

'-•'' 

^ y ' 

/ " • 

,,•''' 

10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 

Analyte Cone. / IS Cone. 

85 90 95 100 

Data printed by STW 

Printing Time: 9:46:17 AM 

Printing Date: Thursday, March 17, 2011 

Page 1 of 1 

Page 44 of 61 
'• Buster J2930203 

Proc . Algorithm : 

Nois e Pei-centage : 

Base . Sub . Hindc v 

Peak-Split . Fact o 

Report Larges t Pe 

M m. Peak Heiyht : 

Hin . Peak Width : 

Smootliing Widtli : 

KT Windov: 

Expecte d RT: 

ntelUQu a 

k: 

JU 

12 

50 

1.00 

1 

Nt. 

0.0 0 

0.0 0 

0 

0 

•9 

T : •^as 

V3lU y 

: 12. 7 

301727 c< 

12. 7 

• Sample Name: "61103103022* Sample ID: "10007-32-10" Fil*: "b110310a.wifr 

I Peak Name: "PFOS" Mau(*c): "499.0/130.0 amu.499.0/99.0 amu,499.0/80.0 amu" 

I Comm*nt "5.0 ng/mL FC Md in Synth. Water" Annotation; ~ 

Sample Index : 22 

Sampl e Type : Standar d 

Concentration : 5.0 0 ng/mL 

Calculate d Cone : A.' l mj/mL 84* 4 

Acq. Date : 3/10/201 1 

Acq. Time : 11:11:0 2 PM 

8.2*4 

7.8*4 

7.6e4-

7.4*4 

7.2e4 

7.0e4 

6.8*4 

6.6*4 

6.4*4 

6Z*4 -

6.0*4-

5.6*4-

5.6*4 

5,4*4 

5.2*4 

5,0*4 

4.8*4 

4.6*4 

^ 4.4*4 

I 4,2*4 

I 

4.0e4-

3.8*4-

3.6e4' 

3.4e4 

3.2*4 

3.0*4 

Z8e4-

ZSe4 

Z4*4 

Z2*4 

2.0*4 

1.8*4 

1.6*4' 

1.0*4 

6000.0 

6000.0 

4000.0 

2000.0 

0.0-1-

GLP10-01-02; Interim Report 16 

Analysis of PFBS. PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur. AL - Jan 2011 

Batch Name: bll0310a.dab 

Jk: 

Printing Time: 10:27:27 7VM 

Printing Date: Thursday, March 17, 2011 

SampI* Nam*: "51103103012" Sanple ID: "10010-213* File: "bl 10310a.*rtr 

I

P*ak Nam*: 'PFOS* llrtaea(**); "499.0/130.0 amu,499.0/99.0 amu,499.0/80.0 amu" 

Comment "Method BbnlT Annotation: ~ 

Sampl e Index : 12 

Unkni 

N/A 

0.01S 9 n<j/mL 

3/10/201 1 

Sampl e Type : 

tio i 

Calcu l d Ci 

Acq. L' 

Acq. T 

Base. Sub. Window: 

P-?ak-Split, Factor: 

B-iport Larges t Paak 

Min . peak Height : 

Min . Peak Width : 

Smoorhinq Width : 

RT Window: 

Expected RT: 

Use Relativ e RT: 

1.00 

2 

No 

0,00 

0.00 

0 

30.0 

12.e 

¥ 3 3 

Int . Type: Valle y 

Retentio n Time: 

Area : 36 

H-iight : 1.1 

Star t Time: 

End Time: 

12.B 

10 cou 

i-e»0O:« 

12.7 

12.e 

Page 1 of 3 
'* Buster J2930203 

I Sampte Name; -bl10310a038" Sample ID:"LCS-110307-r Fil*; 'bl10310a.vflfr 

I P*»k Nam*: "PFOS" Mau(*s}: "499.0/130.0 amu.499.0/99.0 amu.499.0/80.0 amu" 

I ConuTwnt "lOppbLCS" Annotation:' 

Sample Index : 35 

GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Sampl e Type : QC 

Concentration : 9.9 4 ng/mL 

Calculate d Cone : 11. 1 na/mL 

Acq. Date : 3/11/201 1 

Acq. Time : 3:59:3 6 AM 

Hoditied : No 

Proc . Alqorithm : IntelliOua n - MOH 

Nois e Peicentage : 50 

Base . Sub . Window: 1.00 min 

Peak-Split . Factor : 1 

Report Larges t Peak : Nf. 

Hin . Pea k Heioht : 0.0 0 cp s 

Hin . Peak Width : 0.0 0 se e 

Smootliing Width : 0 point s 

RT Window: 30. 0 se c 

Expecte d RT: 12. 8 min 

Usfl Relativ e RT: Yes 

Int . Type : Valle-/ 

Retsntio n Tims: 12. 7 min 

Area : 596555 count s 

Height : ?.01e*00 5 cp s 

Star t Tirae : 12. 5 min 

End Time : 12. 6 min 

3.0*5 

3.0*5 

2.9*5 

Z9e 5 

2.6*5 

2.8*5 

Z7e 5 

2.7*5 

2.6*5 

2.6*5 

2.5*5 

Z5e 5 

Z4* 5 

24e 5 

Z3e 5 

23* 5 

2.2e5 

2.2*5 

Z1e 5 

Z1e5 -

ZOeS 

Z0* 5 

SampI* Nam*: "bn0310a048" Sarr ^ 10: "LC&-110307-

P*ak Name: "PFOS" Mas*(es): "499.0/130.0 anui,499.0/5 

Comment "lOppb LCS ECF" Annotalion:"" 

Sample Index : J9 

10. 0 ng/mL 

Calculate d 

Acq, L'ate: 

Acq, Time: 

Modified : 

RT Windo-^: 

Expected RT 

Cone ! 11.2 

3/11/201 1 

7:00:0 6 AM 

V9S 

30.0 

12.e 

Batch Name: bll0310a.dab 

i r File:"b110310a.wfr 

19.0 amu.499.0/a0.0 amu" 

1.26*5-

1.24*5-

1.22*5-

1.20e5-

1.18*5-

1.16*5-

1.14*5-

1.12*5-

1.10*5-

1.08*5-

1.06*5-

1.04*5-

1.02*5-

1.00*5-

9.80*4-

9.60*4-

9.40*4-

9.20*4-

9.00*4-

8.80*4-

8.60*4-

8.40*4-

8.20*4-

8.00*4-

7.80*4-

7.60*4-

7.40*4-

7.20*4-

7.00*4-

6.80*4-

!. 6.60*4-

^ 6.40*4-

j 6.20*4-

' 6.00*4-

5.80*4 

5.60*4-

5.40*4-

5.20*4-

5.00*4-

4.80*4-

4.60*4-

4.40*4-

4.20*4-

4.00*4-

3,60*4-

3,60*4-

3.40*4-

3.20*4-

3.00*4-

Z80*4-

2,60*4-

Z40e4-

Z20*4-

2.00*4-

1.80*4 

1.60*4-

1.40*4 

1.20*4 

1.00*4 

8000.00 

6000.00 

4000.00 

2000.00 

0.00 Jk^ 

Printing Time: 10:27:27 AM 

Printing Date: Thursday, March 17, 

Page 2 of 3 

Tim, min Pajo^Rnf R1 
Buster J2930203 

I Sample Nam*: "b110310a055" Sample ID: "GLP1(>O1-O2-16-006" File: "bllOaiOa.wifr 

I Peak Name: "PFOS" Mass(*«): "499.0/1300 amu.499.0/99.0 amu.4d9.OQ0.0 amu" 

• Comment"D/U.GWSS220270111 w/IS" Annotation:-

Sample Index : 55 

Sample Type : 

GLP10-01-02: Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

Batch Name: bll0310a.dab 

N/A 

Calculate d Cone 

Acq. Date: 

Acq. Time: 

: ?-57 

3/11/201 1 

9:0£:2 1 AM 

: 12.7 

7 0 4 7 0 7 Ci 

9.eSetOOJ 

9.8*4 

9.2*4 

9.0*4 

8.8*4 

8.6*4 

6.4*4 

8.2*4 

8.0*4 

7.8*4 

7.6*4 

7.4*4 

7.2*4 

7.0B 4 

6.8*4 

6.6*4-

6.4*4 

6.2*4 

6.0*4 

5.8e4-

S.6e4 

5.4*4 

5.2*4 

5.0*4 

4.8*4 

4.6*4-

4.4*4 

4.2*4 

4.0*4 

3.8*4 

3.6*4 

3.4*4 

3.2*4 

3.0*4-

Z8e 4 

Z6* 4 

2.4*4 

Z2* 4 

Z0* 4 

1.8*4 

1.6*4 

1.4*4-

1.2*4 

1.0e4 

eooo.o 

6000.0 

4000.0 

2000.0 

I nMniiiiiidi^i.. 

10 11 12 13 14 IS 16 17 

Printing Time: 10:27:27 AM 

Printing Date: Thursday, March 17, 2011 

Page 3 of 3 

Page 47 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

ATTACHMENT C: ANALYTICAL METHOD 

Page 48 of 61 
Ana^Js°S°pi^BsW^®S'pF0§f,>3teSh<^^^^^^ for 14 days from 04/04/2011 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

3M Environmental LaboiafxNy 

l\/lethod 

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 Da te: Q U 1(1 f o 7 

Approved By: 

^///^/ o • > 

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 49 of ei 
GLP10-01-02; Interim Report 16. , . ., * c .< ^ i s n^/Az-znA^-i 

Analysis of PFBs}^WismPvo§^^G}^m^siLf\mer)l for 14 days from 04/04/2011 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

1 Scope and Application 

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

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

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

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

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

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

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

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

Performance Liquid Chromatography/Mass Spectrometry". 

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

defined QC elements are satisfied. 

Sample collection is not covered under this analytical procedure. 

2 IVIetliod 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 determined using field matrix spikes to verify that the method is applicable to 

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

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

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

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

accuracy for analytical results. 

3 Definitions 

3.1 Calibration Standard 

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

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

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

concentration. 

3.2 Laboratory Duplicate Sample (LDS, or Lab Dup) 

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

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

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

preservation, or storage procedures. 

3.3 Field Blank (FB)/Trip Blank 

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

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

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

other interferences are present in the field environment. This sample is also 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 50 of 61 
AZlisl!'pFBsWMlm%6^%]Gh§^^^^^ for 14 days from 04/04/2011 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

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 (FIVIS) 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

3.7 Laboratory Control Sample (LCS) 

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

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

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

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

each day samples are extracted. 

3.8 Laboratory Matrix Spike (LMS) 

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

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

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

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

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

3.9 Laboratory Sample 

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

3.10 Limit of Quantitation (LOQ) 

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

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

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

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

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

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

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

ETS-8-044.0 Page 3 of 11 

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

Injection Analysis 

Page 51 of 61 
^!^sl!?F^^M!mkm^^^<ii^si^m^en t for 14 days from 04/04/2011 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

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 normally 

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 current awareness of local 

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

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

4.2 Cautions 

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

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

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

5 Interferences 

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

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

conditions of analysis by running method blanks. 

ETS-8-044.0 Page 4 of 11 

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

Injection Analysis 

Page 52 of 61 
GLPI0-01-02; Interim Report 16^ , , ., . x: ^ j^ , r. r\M/yA I'-sr^^ A 

Analysis of PFBs,LpRTsJg?,SPFdr:?i?.>3fe§i(i^%fe^safn^fc^^ for 14 days from 04/04/2011 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

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

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

(LC/MS/MS). I 

Analytical balance capable of reading to 0.0001 g 

A device to collect raw data for peak integration and quantitation 

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

Gas tight syringes, 25pL, 50pL, lOOpL, 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 \xm 

Analytical Column: Betasil C18,4.6 mm x 100 mm, 5 pm 

Temperature: 10°C 

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

Mobile Phase (B): Methanol 

Gradient Program: 

Time (min) 

0.0 

0.5 

11.0 

13.5 

13.6 

17.0 

%A 

97 

97 

5 

5 

97 

97 

%B 

3 

3 

95 

95 

3 

3 

Flow Rate 

(mL/min) 

1.0 

1.0 

1.0 

1.0 

1.0 

1.0 

Injection Volume: 100 pL. 

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

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 53 of 61 
GLPI0-01-02; Interim Report 16, , , ., ,. i: A ji i r nAinAi'-.nAi 

Analysis of PFBs.Lr^Fi-TsJ^iS^PTO^iPtefeSncJ^^fefisafn^^^^^ for 14 days from 04/04/201 1 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

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 information is intended as a guide, alternate instmments and equipment may be used. 

7 Reagents and Standards 

7.1 Chemicals 

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

Methanol - HPLC grade 

Ammonium Acetate -A. C.S. Reagent Grade 

7.2 Standards 

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

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

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

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

Products, Inc 

Perfiuorooctanoic Acid (PFOA - C8 acid); 3M 

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

Perfluorodecanoic Acid (PFDA-C10 acid); Oakwood Products, Inc 

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

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

Perfluorobutanesulfonate (PFBS - C4 sulfonate); 3M 

Perfluorohexanesulfonate (PFHS - C6 sulfonate); 3M 

Perfluorooctanesulfonate (PFOS - C8 sulfonate); 3M 

ETS-8-044.0 Page 6 of 11 

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

Analysis 

Page 54 of 61 
GLP10-01-02; Interim Report 16. , , ., x r .< ^ i ^ n A tr^ A m^A A 

Analysis of PFBS,lr>FfW@?,Sii#6T§f,)Gte§i(i^1.fe^s^fnpl;^rrent, for 14 days from 04/04/2011 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

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

used. 

7.3 Reagent Preparation 

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

water. 

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

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

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

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

when diluting stock solutions to appropriate levels. 

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

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

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

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

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

,^ ^- r ^ molecular weight of anion 

salt correction factor = = 

moclecular weight of salt 

4gQ PFOS (K^- )salt correction factor = ^^ ^ = 0.9275 

538 

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

5 Mg/mL (5000 ng/mL) mixed working standard—^Add 0.5mL each of the 100pg/mL SSSs to a 10mL volumetric 

flask and bring up to volume with solvent. 

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

volumetric flask and bring up to volume with solvent. 

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

flask and bring up to volume with solvent. 

Storage Conditions—Store all SSSs and wor1<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 55 of 61 
GLP10-01-02; Interim Report 16^ , , ., ^ r ^ j , x- njiir^Ai-^n^A 

Analysis of PFBS,Lp?i-T^JS'iS>pF%1?f,tefefncJiafef^sa'fe¥rent, for 14 days from 04/04/2011 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

7.5 Calibration Standards 

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

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

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

than those listed below can be prepared as needed. 

Concentration 

of WS, ng/mL 

125 

125 

125 

125 

250 

250 

250 

250 

5000 

5000 

5000 

Volume of WS,/J. 

10 

15 

20 

30 

20 

50 

100 

200 

25 

50 

100 

Final Volume of 

Calibration Standard (mL 

of ASTM Type 1 Water, or 

other suitable water) 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

Final Concentration of 

Calibration Standard, ng/mL 

(ppb) in ASTM Type 1 Water, 

or other suitable water 

0.025 

0.0375 

0.050 

0.075 

0.100 

0.250 

0.500 

1.00 

2.50 

5.00 

10.0 

8 Sample Handling 

8.1 Water Sample Preparation 

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

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

sample aliquot, or filtered. 

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

prefen-ed over the use of glass autovials, to prevent the possibly of fluorochemical sticking to the glass. 

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

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

Prepare at least five method blanks. 

9 Sample Analysi s - LC/MS/MS 

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

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

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

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

thoroughly documented in the raw data. 

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

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

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

The coefficient of detemnination (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 56 of 61 
Al^Bi°s\so°SsWMimkoS^^^ for 14 days from 04/04/2011 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

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

points will be used to construct the calibration curve. 

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

curve (if necessary) and reanalyze. 

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

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

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

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

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

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

curve should be further diluted and reanalyzed. 

10 Quality Control 

10.1 Data Quality Objectives 

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

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

the raw data and footnoted in the final report. 

10.2 Method Blanks 

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

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

method blank. At a minimum, method blanks are analyzed prior to instalment 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 determine outliers, or technical justification to eliminate one or more results should be made. 

10.3 Sample Replicates 

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

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

replicates excludes field blanks. 

10.4 Surrogate Spikes 

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

10.5 Lab Control Sample 

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

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

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

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

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

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

ETS-8-044.0 Page 9 of 11 

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

Analysis 

Page 57 of 61 
GLP10-01-02; Interim Report 16. , ,. ^ ,. t ^ yi ^ K n>i/n/i/TA^ ^ 

Analysis of PFBs,ir-Ft-Tsief',^i5r6'§f.>3feSh(j^%fe0safniSi6i«'ren for 14 days from 04/04/2011 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

10.6 Field Matrix Spikes / Lab Matrix Spikes 

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

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

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

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

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

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

11 Data Analysis and Calculations 

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

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

A .X r J / , .X (Peak Area-Intercept) ^ ^ Analyte found (ng/mL) = -^^ ^--^ x DF 

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

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

percent recovery. 

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

Analyte added (ng/mL) 

12 Method Performance 

Any method perfomriance 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 performance section are not met, maintenance may be perfonned 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 

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

calit)ration curve and are repeated injections from one autosampler vial. The system suitability injections must 

have area counts with an RSD of 55% and a retention time RSD of 52% to be compliant. 

12.2 Quantitation 

Calibration Curve: 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 be within ±30%. 

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

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

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

bracketed by CCVs not meeting these criteria must be reanalyzed. 

ETS-8-044.0 Page 10 of 11 

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

Analysis 

Page 58 of 61 
GLP10-01-02; Interim Report 16,, , .. . . r A j, , r n.Ai^Ai'-^r^AA 

Analysis of PFBS,k5i?i-TsJg?,S:pFGl§fi>3feg-ici4%fe?Ssa".ti^t|rrent, for 14 days from 04/04/2011 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

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

standard) and the mass spectral response of unique ions. 

12.3 Sensitivity 

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

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

to Section 10 for additional details. 

12.4 Accurac y 

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

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

spikes and laboratory matrix spikes. 

12.5 Precision 

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

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

requirement for replicates excludes field blanks or rinse blanks. 

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

13 Pollution Prevention and Waste Management 

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

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

14 Records 

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

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

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

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

15 Affected Document s 

None. 

16 Revisions 

Revision 

Number Summary of Changes 

ETS-8-044.0 Page 11 of 11 

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

Analysis 

Page 59 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Avenue A Investigation Area; Decatur, AL - Jan 2011 

ATTACHMENT D: DEVIATION(S) 

Page 60 of 61 
GLP10-01-02; Interim Report 16 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

REC0*frcJfi^tl'imW^/W6^SSS^0RMANCE 

/. Identification 

Study / Project No. 

GLP10-01-02-16 

Date(s) of Occurrence: 

g110228a and g110211a 

Document Number: 

ETS-8-044.0 

Deviation type D SOP D Equipment Procedure 0 Method 

(Check one) D Protocol D GPO D Other: 

//. Description (attach extra pages as needed) 

Method Requirements: 

1. LCS average recoveries within ±20% (section 10.5). 

2. FMS recovery within ±30% (section 10.6). 

Actual procedure/process: 

1. The average PFOS recovery for the 30 ppb LCS (linear-^ branched) was 133% (g11021 la). The average 

PFOS recovery for the 30 ppb LCS (linear •^ branched) was 125% (gl 10228a). 

2. Sampling location 210R; the recovery of the FMS High sample for PFOS was 68.1% (gl 10228a). 

///. Actions Taken 

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

Corrective Action (D Yes 0 No) Reference: 

Acceptability of the nonconforming work: 

1. The recoveries for the 30 ppb LCS (linear + branched) at 133% and 125% will be flagged In the final report. 

The last fifty LCSs for PFOS, including the LCS prepared with this study, were evaluated by ETS-12-012 to 

determine the method analytical uncertainty. The analytical uncertainty when evaluated by ETS-12-012 

was determined to be ± 17% for PFOS. However, the analytical uncertainty for this study will be set at ± 

33%, based on the recovery of the high sets of linear + branched LCS. 

2. The FMS High recovery for PFOS will be flagged in the final report. The recovery is within the method 

uncertainty of ± 33%. 

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

0 Other: Deviations will be noted in final report. 

Project Lead/PAI Approval: Date: 

Study Director (if GLP): Date: 

Sponsor Approval (for (StP protocol deviations): NA 

f echnicai Reviewer (optional): NA 

Date: 

Date: NA 

Laboratory DepartmentJ^dafvager Approval: Date: 

IV. Authorization to Resume Work 

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

Laboratory Department Manager Approval: NA Date: NA 

Deviation No. 

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

ETS-4-008.7 Page 1„of 1 

Documentation of Deviations and Control of Nonconforming Testin& Page 61 of 61